# Electronic Supplementary Material (ESI) for ChemComm. # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_date 2014-01-09 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _shelxl_version_number 2013-4 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H59 N3 Ni O, 2(C7 H8)' _chemical_formula_sum 'C55 H75 N3 Ni O' _chemical_formula_weight 852.89 _chemical_melting_point ? _chemical_oxdiff_formula 'C41 H59 N3 Ni O' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1354(8) _cell_length_b 12.2243(5) _cell_length_c 17.8241(7) _cell_angle_alpha 87.524(4) _cell_angle_beta 85.065(5) _cell_angle_gamma 87.053(5) _cell_volume 2412.2(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7676 _cell_measurement_temperature 123.00(10) _cell_measurement_theta_max 72.8750 _cell_measurement_theta_min 3.5820 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour 'clear pink' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 924 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.957 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 21977 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.957 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.763 _diffrn_reflns_theta_min 3.623 _diffrn_ambient_temperature 123.00(10) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0370497000 _diffrn_orient_matrix_UB_12 -0.1090627000 _diffrn_orient_matrix_UB_13 -0.0377391000 _diffrn_orient_matrix_UB_21 -0.1325819000 _diffrn_orient_matrix_UB_22 -0.0321764000 _diffrn_orient_matrix_UB_23 0.0084786000 _diffrn_orient_matrix_UB_31 -0.0194097000 _diffrn_orient_matrix_UB_32 0.0549415000 _diffrn_orient_matrix_UB_33 -0.0777265000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7547 _reflns_number_total 9329 _reflns_odcompleteness_completeness 99.23 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL-2013 (Sheldrick, 2008)' _computing_structure_solution 'ShelXS-2013 (Sheldrick, 2008)' _refine_diff_density_max 0.646 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.057 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 561 _refine_ls_number_reflns 9329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0476 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.6711P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1224 _refine_ls_wR_factor_ref 0.1354 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C15(H15), C18(H18), C27(H27), C30(H30) 2.b Secondary CH2 refined with riding coordinates: C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B) 2.c Me refined with riding coordinates: C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B, H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A, H32B,H32C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C106(H10A,H10B,H10C), C206(H20D,H20E,H20F) 2.d Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C11(H11), C12(H12), C13(H13), C23(H23), C24(H24), C25(H25), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), C201(H201), C202(H202), C203(H203), C204(H204), C205(H205) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.37046(17) 0.23324(15) 0.21754(11) 0.0189(4) Uani 1 1 d . . . . . C2 C 0.21219(19) 0.12092(16) 0.22073(12) 0.0250(4) Uani 1 1 d . . . . . H2 H 0.1579 0.0680 0.2374 0.030 Uiso 1 1 calc R . . . . C3 C 0.21519(19) 0.17957(16) 0.15482(12) 0.0261(4) Uani 1 1 d . . . . . H3 H 0.1630 0.1749 0.1172 0.031 Uiso 1 1 calc R . . . . C4 C 0.62240(19) 0.25318(16) 0.15673(11) 0.0242(4) Uani 1 1 d . . . . . C5 C 0.6337(2) 0.13355(17) 0.15944(12) 0.0278(4) Uani 1 1 d . . . . . C6 C 0.7489(2) 0.10046(19) 0.17267(13) 0.0325(5) Uani 1 1 d . . . . . C7 C 0.8178(2) 0.1960(2) 0.17611(14) 0.0325(5) Uani 1 1 d . . . . . C8 C 0.7438(2) 0.28656(18) 0.16405(12) 0.0273(4) Uani 1 1 d . . . . . C9 C 0.32683(17) 0.11405(16) 0.33400(11) 0.0211(4) Uani 1 1 d . . . . . C10 C 0.28348(17) 0.17767(16) 0.39514(11) 0.0220(4) Uani 1 1 d . . . . . C11 C 0.2986(2) 0.13314(18) 0.46713(12) 0.0282(4) Uani 1 1 d . . . . . H11 H 0.2719 0.1735 0.5089 0.034 Uiso 1 1 calc R . . . . C12 C 0.3528(2) 0.02946(19) 0.47758(13) 0.0318(5) Uani 1 1 d . . . . . H12 H 0.3618 0.0010 0.5261 0.038 Uiso 1 1 calc R . . . . C13 C 0.3934(2) -0.03149(17) 0.41656(13) 0.0298(5) Uani 1 1 d . . . . . H13 H 0.4290 -0.1010 0.4245 0.036 Uiso 1 1 calc R . . . . C14 C 0.38196(18) 0.00906(16) 0.34275(12) 0.0243(4) Uani 1 1 d . . . . . C15 C 0.21659(18) 0.28750(16) 0.38460(12) 0.0236(4) Uani 1 1 d . . . . . H15 H 0.2504 0.3227 0.3376 0.028 Uiso 1 1 calc R . . . . C16 C 0.2275(2) 0.36516(19) 0.44858(14) 0.0329(5) Uani 1 1 d . . . . . H16A H 0.1833 0.4330 0.4387 0.049 Uiso 1 1 calc R . . . . H16B H 0.3110 0.3791 0.4518 0.049 Uiso 1 1 calc R . . . . H16C H 0.1952 0.3321 0.4953 0.049 Uiso 1 1 calc R . . . . C17 C 0.08259(19) 0.27049(19) 0.37701(14) 0.0320(5) Uani 1 1 d . . . . . H17A H 0.0407 0.3404 0.3702 0.048 Uiso 1 1 calc R . . . . H17B H 0.0483 0.2335 0.4218 0.048 Uiso 1 1 calc R . . . . H17C H 0.0749 0.2270 0.3343 0.048 Uiso 1 1 calc R . . . . C18 C 0.4254(2) -0.06158(17) 0.27703(14) 0.0307(5) Uani 1 1 d . . . . . H18 H 0.4207 -0.0161 0.2306 0.037 Uiso 1 1 calc R . . . . C19 C 0.3444(3) -0.1576(2) 0.27241(17) 0.0438(6) Uani 1 1 d . . . . . H19A H 0.3736 -0.2007 0.2303 0.066 Uiso 1 1 calc R . . . . H19B H 0.2635 -0.1302 0.2660 0.066 Uiso 1 1 calc R . . . . H19C H 0.3453 -0.2023 0.3180 0.066 Uiso 1 1 calc R . . . . C20 C 0.5571(2) -0.1018(2) 0.28136(17) 0.0427(6) Uani 1 1 d . . . . . H20A H 0.5822 -0.1460 0.2390 0.064 Uiso 1 1 calc R . . . . H20B H 0.5648 -0.1448 0.3272 0.064 Uiso 1 1 calc R . . . . H20C H 0.6070 -0.0400 0.2806 0.064 Uiso 1 1 calc R . . . . C21 C 0.33136(18) 0.33113(16) 0.09389(11) 0.0219(4) Uani 1 1 d . . . . . C22 C 0.28647(19) 0.43947(16) 0.10720(12) 0.0246(4) Uani 1 1 d . . . . . C23 C 0.3014(2) 0.51562(17) 0.04674(13) 0.0295(5) Uani 1 1 d . . . . . H23 H 0.2734 0.5879 0.0532 0.035 Uiso 1 1 calc R . . . . C24 C 0.3564(2) 0.48634(18) -0.02196(13) 0.0340(5) Uani 1 1 d . . . . . H24 H 0.3657 0.5390 -0.0610 0.041 Uiso 1 1 calc R . . . . C25 C 0.3980(2) 0.37958(19) -0.03354(12) 0.0312(5) Uani 1 1 d . . . . . H25 H 0.4347 0.3611 -0.0805 0.037 Uiso 1 1 calc R . . . . C26 C 0.38594(19) 0.29893(17) 0.02424(12) 0.0256(4) Uani 1 1 d . . . . . C27 C 0.2207(2) 0.47165(17) 0.18141(13) 0.0308(5) Uani 1 1 d . . . . . H27 H 0.2620 0.4334 0.2220 0.037 Uiso 1 1 calc R . . . . C28 C 0.2202(3) 0.59531(19) 0.19375(15) 0.0409(6) Uani 1 1 d . . . . . H28A H 0.1777 0.6110 0.2415 0.061 Uiso 1 1 calc R . . . . H28B H 0.1809 0.6347 0.1542 0.061 Uiso 1 1 calc R . . . . H28C H 0.3018 0.6174 0.1932 0.061 Uiso 1 1 calc R . . . . C29 C 0.0898(2) 0.4367(2) 0.18793(15) 0.0411(6) Uani 1 1 d . . . . . H29A H 0.0505 0.4580 0.2355 0.062 Uiso 1 1 calc R . . . . H29B H 0.0889 0.3586 0.1846 0.062 Uiso 1 1 calc R . . . . H29C H 0.0480 0.4716 0.1478 0.062 Uiso 1 1 calc R . . . . C30 C 0.4265(2) 0.18071(18) 0.00769(13) 0.0326(5) Uani 1 1 d . . . . . H30 H 0.4270 0.1390 0.0559 0.039 Uiso 1 1 calc R . . . . C31 C 0.5539(3) 0.1709(2) -0.03208(15) 0.0454(6) Uani 1 1 d . . . . . H31A H 0.5753 0.0953 -0.0413 0.068 Uiso 1 1 calc R . . . . H31B H 0.6102 0.1989 -0.0007 0.068 Uiso 1 1 calc R . . . . H31C H 0.5562 0.2124 -0.0791 0.068 Uiso 1 1 calc R . . . . C32 C 0.3355(3) 0.1303(2) -0.03920(15) 0.0451(6) Uani 1 1 d . . . . . H32A H 0.3614 0.0559 -0.0495 0.068 Uiso 1 1 calc R . . . . H32B H 0.3306 0.1719 -0.0859 0.068 Uiso 1 1 calc R . . . . H32C H 0.2575 0.1315 -0.0116 0.068 Uiso 1 1 calc R . . . . C33 C 0.65357(18) 0.31483(16) 0.37840(11) 0.0225(4) Uani 1 1 d . . . . . C34 C 0.78574(18) 0.34418(17) 0.36358(12) 0.0259(4) Uani 1 1 d . . . . . H34A H 0.8314 0.3089 0.4026 0.031 Uiso 1 1 calc R . . . . H34B H 0.8179 0.3152 0.3158 0.031 Uiso 1 1 calc R . . . . C35 C 0.80389(19) 0.46675(18) 0.36166(14) 0.0310(5) Uani 1 1 d . . . . . H35A H 0.8890 0.4803 0.3519 0.037 Uiso 1 1 calc R . . . . H35B H 0.7754 0.4966 0.4099 0.037 Uiso 1 1 calc R . . . . C36 C 0.73362(19) 0.52168(17) 0.29965(13) 0.0273(4) Uani 1 1 d . . . . . H36A H 0.7666 0.4946 0.2514 0.033 Uiso 1 1 calc R . . . . H36B H 0.7443 0.6000 0.2986 0.033 Uiso 1 1 calc R . . . . C37 C 0.59796(18) 0.50134(16) 0.30988(11) 0.0226(4) Uani 1 1 d . . . . . C38 C 0.64420(19) 0.19296(17) 0.36500(13) 0.0280(4) Uani 1 1 d . . . . . H38A H 0.5615 0.1737 0.3740 0.042 Uiso 1 1 calc R . . . . H38B H 0.6924 0.1503 0.3987 0.042 Uiso 1 1 calc R . . . . H38C H 0.6728 0.1783 0.3139 0.042 Uiso 1 1 calc R . . . . C39 C 0.6058(2) 0.3360(2) 0.45999(12) 0.0305(5) Uani 1 1 d . . . . . H39A H 0.6109 0.4122 0.4694 0.046 Uiso 1 1 calc R . . . . H39B H 0.6534 0.2926 0.4938 0.046 Uiso 1 1 calc R . . . . H39C H 0.5232 0.3162 0.4679 0.046 Uiso 1 1 calc R . . . . C40 C 0.5353(2) 0.56685(18) 0.37482(13) 0.0308(5) Uani 1 1 d . . . . . H40A H 0.5703 0.5447 0.4208 0.046 Uiso 1 1 calc R . . . . H40B H 0.4508 0.5533 0.3799 0.046 Uiso 1 1 calc R . . . . H40C H 0.5457 0.6437 0.3644 0.046 Uiso 1 1 calc R . . . . C41 C 0.5407(2) 0.53868(17) 0.23782(13) 0.0301(5) Uani 1 1 d . . . . . H41A H 0.4560 0.5260 0.2437 0.045 Uiso 1 1 calc R . . . . H41B H 0.5781 0.4981 0.1965 0.045 Uiso 1 1 calc R . . . . H41C H 0.5519 0.6155 0.2279 0.045 Uiso 1 1 calc R . . . . C100 C 1.0366(2) 0.7681(2) 0.39882(13) 0.0339(5) Uani 1 1 d . . . . . C101 C 0.9406(2) 0.7820(2) 0.35508(15) 0.0443(6) Uani 1 1 d . . . . . H101 H 0.9062 0.7213 0.3375 0.053 Uiso 1 1 calc R . . . . C102 C 0.8947(3) 0.8881(3) 0.33711(17) 0.0568(8) Uani 1 1 d . . . . . H102 H 0.8296 0.8978 0.3077 0.068 Uiso 1 1 calc R . . . . C103 C 0.9466(3) 0.9787(2) 0.36329(18) 0.0506(7) Uani 1 1 d . . . . . H103 H 0.9170 1.0492 0.3512 0.061 Uiso 1 1 calc R . . . . C104 C 1.0414(3) 0.9628(2) 0.40685(19) 0.0514(7) Uani 1 1 d . . . . . H104 H 1.0765 1.0230 0.4246 0.062 Uiso 1 1 calc R . . . . C105 C 1.0855(2) 0.8584(2) 0.42469(16) 0.0420(6) Uani 1 1 d . . . . . H105 H 1.1497 0.8490 0.4549 0.050 Uiso 1 1 calc R . . . . C106 C 1.0879(3) 0.6546(2) 0.41823(17) 0.0466(6) Uani 1 1 d . . . . . H10A H 1.1540 0.6601 0.4489 0.070 Uiso 1 1 calc R . . . . H10B H 1.1160 0.6187 0.3727 0.070 Uiso 1 1 calc R . . . . H10C H 1.0264 0.6130 0.4454 0.070 Uiso 1 1 calc R . . . . C200 C 1.0263(3) 0.8315(2) 0.08228(18) 0.0472(7) Uani 1 1 d . . . . . C201 C 0.9395(3) 0.7780(3) 0.13219(17) 0.0639(10) Uani 1 1 d . . . . . H201 H 0.9146 0.8059 0.1790 0.077 Uiso 1 1 calc R . . . . C202 C 0.8909(3) 0.6789(3) 0.10822(17) 0.0514(7) Uani 1 1 d . . . . . H202 H 0.8333 0.6417 0.1389 0.062 Uiso 1 1 calc R . . . . C203 C 0.9321(3) 0.6419(2) 0.03966(17) 0.0469(6) Uani 1 1 d . . . . . H203 H 0.9012 0.5787 0.0234 0.056 Uiso 1 1 calc R . . . . C204 C 1.0159(3) 0.6932(3) -0.00554(18) 0.0508(7) Uani 1 1 d . . . . . H204 H 1.0424 0.6649 -0.0520 0.061 Uiso 1 1 calc R . . . . C205 C 1.0618(3) 0.7858(3) 0.01622(17) 0.0499(7) Uani 1 1 d . . . . . H205 H 1.1205 0.8194 -0.0159 0.060 Uiso 1 1 calc R . . . . C206 C 1.0771(4) 0.9348(4) 0.1056(3) 0.1053(18) Uani 1 1 d . . . . . H20D H 1.0404 0.9536 0.1544 0.158 Uiso 1 1 calc R . . . . H20E H 1.0607 0.9932 0.0696 0.158 Uiso 1 1 calc R . . . . H20F H 1.1627 0.9238 0.1078 0.158 Uiso 1 1 calc R . . . . N1 N 0.58027(14) 0.37950(13) 0.32217(9) 0.0187(3) Uani 1 1 d . . . . . N2 N 0.30616(15) 0.15537(13) 0.25865(9) 0.0199(3) Uani 1 1 d . . . . . N3 N 0.31053(15) 0.24798(13) 0.15371(9) 0.0210(3) Uani 1 1 d . . . . . O1 O 0.45751(12) 0.36045(11) 0.33676(8) 0.0216(3) Uani 1 1 d . . . . . Ni1 Ni 0.50842(3) 0.29723(3) 0.24692(2) 0.01851(10) Uani 1 1 d . . . . . H7 H 0.892(3) 0.195(2) 0.1841(16) 0.037(7) Uiso 1 1 d . . . . . H4 H 0.572(2) 0.292(2) 0.1234(15) 0.032(7) Uiso 1 1 d . . . . . H8 H 0.771(2) 0.360(2) 0.1615(15) 0.033(7) Uiso 1 1 d . . . . . H5 H 0.572(2) 0.087(2) 0.1528(15) 0.031(7) Uiso 1 1 d . . . . . H6 H 0.779(2) 0.033(2) 0.1772(15) 0.031(7) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0214(9) 0.0154(8) 0.0190(9) 0.0030(7) -0.0003(7) 0.0006(7) C2 0.0281(10) 0.0207(9) 0.0271(11) 0.0038(8) -0.0067(8) -0.0054(7) C3 0.0308(11) 0.0234(10) 0.0253(10) 0.0021(8) -0.0091(8) -0.0039(8) C4 0.0320(11) 0.0207(9) 0.0187(9) 0.0020(8) 0.0012(8) 0.0014(8) C5 0.0367(12) 0.0220(10) 0.0239(10) -0.0003(8) 0.0003(9) -0.0005(8) C6 0.0363(12) 0.0257(11) 0.0325(12) 0.0029(9) 0.0060(9) 0.0082(9) C7 0.0241(11) 0.0393(12) 0.0324(12) -0.0010(10) 0.0051(9) 0.0018(9) C8 0.0312(11) 0.0272(10) 0.0222(10) -0.0008(8) 0.0064(8) -0.0028(8) C9 0.0224(9) 0.0210(9) 0.0195(10) 0.0072(7) -0.0036(7) 0.0004(7) C10 0.0186(9) 0.0242(9) 0.0229(10) 0.0053(8) -0.0018(7) -0.0016(7) C11 0.0294(11) 0.0333(11) 0.0213(10) 0.0059(9) -0.0009(8) -0.0043(8) C12 0.0317(11) 0.0369(12) 0.0264(11) 0.0163(9) -0.0072(9) -0.0053(9) C13 0.0297(11) 0.0230(10) 0.0360(12) 0.0143(9) -0.0065(9) -0.0009(8) C14 0.0220(9) 0.0201(9) 0.0300(11) 0.0066(8) -0.0015(8) -0.0020(7) C15 0.0219(9) 0.0234(9) 0.0244(10) 0.0037(8) 0.0017(8) 0.0010(7) C16 0.0330(11) 0.0308(11) 0.0337(12) -0.0041(9) 0.0029(9) 0.0033(9) C17 0.0232(10) 0.0323(11) 0.0398(13) 0.0044(10) -0.0033(9) 0.0028(8) C18 0.0359(12) 0.0191(9) 0.0355(12) 0.0048(9) 0.0008(9) 0.0010(8) C19 0.0553(16) 0.0263(11) 0.0493(16) -0.0052(11) 0.0021(12) -0.0056(11) C20 0.0394(13) 0.0277(11) 0.0570(17) 0.0098(11) 0.0089(12) 0.0077(10) C21 0.0264(10) 0.0198(9) 0.0201(10) 0.0038(7) -0.0075(8) -0.0010(7) C22 0.0301(10) 0.0211(9) 0.0234(10) 0.0022(8) -0.0092(8) -0.0004(8) C23 0.0403(12) 0.0185(9) 0.0305(12) 0.0045(8) -0.0110(9) -0.0003(8) C24 0.0463(13) 0.0273(11) 0.0287(12) 0.0138(9) -0.0092(10) -0.0072(9) C25 0.0396(12) 0.0341(11) 0.0192(10) 0.0061(9) -0.0022(9) -0.0006(9) C26 0.0324(11) 0.0242(10) 0.0204(10) 0.0028(8) -0.0058(8) -0.0005(8) C27 0.0437(13) 0.0236(10) 0.0249(11) -0.0008(8) -0.0079(9) 0.0088(9) C28 0.0521(15) 0.0294(12) 0.0420(14) -0.0081(10) -0.0152(12) 0.0141(10) C29 0.0453(14) 0.0347(12) 0.0407(14) 0.0015(11) 0.0064(11) 0.0049(10) C30 0.0489(14) 0.0270(11) 0.0211(10) 0.0012(8) -0.0048(9) 0.0068(9) C31 0.0585(17) 0.0461(14) 0.0282(12) 0.0002(11) 0.0025(11) 0.0175(12) C32 0.0733(19) 0.0293(12) 0.0346(13) -0.0066(10) -0.0152(13) 0.0023(12) C33 0.0219(9) 0.0270(10) 0.0184(9) 0.0040(8) -0.0029(7) 0.0002(7) C34 0.0205(9) 0.0299(10) 0.0270(11) 0.0028(8) -0.0034(8) -0.0009(8) C35 0.0232(10) 0.0330(11) 0.0379(12) -0.0018(9) -0.0057(9) -0.0048(8) C36 0.0289(11) 0.0233(10) 0.0294(11) 0.0007(8) 0.0004(8) -0.0053(8) C37 0.0255(10) 0.0195(9) 0.0227(10) 0.0008(8) -0.0006(8) -0.0035(7) C38 0.0272(10) 0.0274(10) 0.0289(11) 0.0101(9) -0.0061(8) 0.0001(8) C39 0.0289(11) 0.0431(12) 0.0192(10) 0.0033(9) -0.0027(8) -0.0018(9) C40 0.0341(11) 0.0269(10) 0.0310(12) -0.0062(9) -0.0016(9) 0.0024(8) C41 0.0426(12) 0.0203(9) 0.0277(11) 0.0037(8) -0.0073(9) -0.0007(8) C100 0.0340(12) 0.0383(12) 0.0283(11) 0.0016(9) 0.0041(9) -0.0048(9) C101 0.0432(14) 0.0517(15) 0.0389(14) -0.0019(12) -0.0079(11) -0.0048(11) C102 0.0426(15) 0.087(2) 0.0391(15) 0.0123(15) -0.0056(12) 0.0054(15) C103 0.0538(17) 0.0395(14) 0.0532(17) 0.0119(13) 0.0124(14) 0.0082(12) C104 0.0536(17) 0.0397(14) 0.0597(18) 0.0029(13) 0.0049(14) -0.0104(12) C105 0.0377(13) 0.0437(14) 0.0445(15) 0.0022(11) -0.0015(11) -0.0083(10) C106 0.0512(16) 0.0406(14) 0.0475(16) 0.0009(12) -0.0047(12) -0.0004(11) C200 0.0427(14) 0.0386(13) 0.0630(19) -0.0076(13) -0.0212(13) 0.0038(11) C201 0.069(2) 0.087(2) 0.0342(15) -0.0128(15) -0.0153(14) 0.0419(19) C202 0.0431(15) 0.0583(17) 0.0493(17) 0.0197(14) 0.0008(12) 0.0046(13) C203 0.0418(14) 0.0426(14) 0.0565(17) -0.0021(13) -0.0076(13) 0.0012(11) C204 0.0479(16) 0.0587(18) 0.0464(16) -0.0042(14) -0.0084(13) 0.0012(13) C205 0.0463(15) 0.0550(17) 0.0475(16) 0.0017(13) -0.0040(13) 0.0026(12) C206 0.095(3) 0.068(3) 0.164(5) -0.044(3) -0.056(3) -0.004(2) N1 0.0186(7) 0.0199(7) 0.0174(8) 0.0022(6) -0.0009(6) -0.0012(6) N2 0.0233(8) 0.0169(7) 0.0192(8) 0.0045(6) -0.0032(6) -0.0005(6) N3 0.0277(8) 0.0167(7) 0.0188(8) 0.0033(6) -0.0047(6) -0.0011(6) O1 0.0171(6) 0.0270(7) 0.0205(7) 0.0009(5) 0.0000(5) -0.0019(5) Ni1 0.02037(17) 0.01771(17) 0.01720(18) 0.00231(12) -0.00188(12) -0.00034(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.369(2) . ? C1 N3 1.369(3) . ? C1 Ni1 1.8824(19) . ? C2 C3 1.348(3) . ? C2 N2 1.386(3) . ? C3 N3 1.383(3) . ? C4 C5 1.460(3) . ? C4 C8 1.450(3) . ? C4 Ni1 2.034(2) . ? C5 C6 1.362(3) . ? C6 C7 1.436(3) . ? C7 C8 1.366(3) . ? C9 C10 1.403(3) . ? C9 C14 1.402(3) . ? C9 N2 1.447(2) . ? C10 C11 1.392(3) . ? C10 C15 1.514(3) . ? C11 C12 1.388(3) . ? C12 C13 1.376(3) . ? C13 C14 1.399(3) . ? C14 C18 1.516(3) . ? C15 C16 1.532(3) . ? C15 C17 1.535(3) . ? C18 C19 1.525(3) . ? C18 C20 1.530(3) . ? C21 C22 1.414(3) . ? C21 C26 1.398(3) . ? C21 N3 1.453(2) . ? C22 C23 1.398(3) . ? C22 C27 1.513(3) . ? C23 C24 1.375(3) . ? C24 C25 1.380(3) . ? C25 C26 1.397(3) . ? C26 C30 1.525(3) . ? C27 C28 1.537(3) . ? C27 C29 1.533(4) . ? C30 C31 1.532(4) . ? C30 C32 1.536(4) . ? C33 C34 1.531(3) . ? C33 C38 1.529(3) . ? C33 C39 1.533(3) . ? C33 N1 1.517(2) . ? C34 C35 1.521(3) . ? C35 C36 1.522(3) . ? C36 C37 1.538(3) . ? C37 C40 1.533(3) . ? C37 C41 1.525(3) . ? C37 N1 1.517(2) . ? C100 C101 1.376(4) . ? C100 C105 1.370(4) . ? C100 C106 1.510(4) . ? C101 C102 1.403(4) . ? C102 C103 1.391(5) . ? C103 C104 1.364(5) . ? C104 C105 1.379(4) . ? C200 C201 1.422(5) . ? C200 C205 1.345(4) . ? C200 C206 1.499(4) . ? C201 C202 1.447(5) . ? C202 C203 1.356(4) . ? C203 C204 1.341(4) . ? C204 C205 1.351(4) . ? N1 O1 1.399(2) . ? N1 Ni1 1.9581(16) . ? O1 Ni1 1.8408(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 Ni1 125.51(14) . . ? N3 C1 N2 102.98(16) . . ? N3 C1 Ni1 131.51(14) . . ? C3 C2 N2 106.23(17) . . ? C2 C3 N3 107.10(18) . . ? C5 C4 Ni1 106.81(14) . . ? C8 C4 C5 104.20(18) . . ? C8 C4 Ni1 111.29(15) . . ? C6 C5 C4 109.3(2) . . ? C5 C6 C7 108.5(2) . . ? C8 C7 C6 108.3(2) . . ? C7 C8 C4 109.53(19) . . ? C10 C9 N2 118.48(17) . . ? C14 C9 C10 123.02(18) . . ? C14 C9 N2 118.36(18) . . ? C9 C10 C15 122.15(18) . . ? C11 C10 C9 117.22(19) . . ? C11 C10 C15 120.54(19) . . ? C12 C11 C10 121.1(2) . . ? C13 C12 C11 120.4(2) . . ? C12 C13 C14 121.31(19) . . ? C9 C14 C18 123.30(19) . . ? C13 C14 C9 117.0(2) . . ? C13 C14 C18 119.71(18) . . ? C10 C15 C16 113.50(18) . . ? C10 C15 C17 109.85(17) . . ? C16 C15 C17 109.15(18) . . ? C14 C18 C19 111.16(19) . . ? C14 C18 C20 111.3(2) . . ? C19 C18 C20 110.96(19) . . ? C22 C21 N3 118.08(18) . . ? C26 C21 C22 123.04(18) . . ? C26 C21 N3 118.68(17) . . ? C21 C22 C27 122.48(18) . . ? C23 C22 C21 116.4(2) . . ? C23 C22 C27 121.05(19) . . ? C24 C23 C22 121.6(2) . . ? C23 C24 C25 120.6(2) . . ? C24 C25 C26 120.9(2) . . ? C21 C26 C30 123.42(18) . . ? C25 C26 C21 117.34(19) . . ? C25 C26 C30 119.2(2) . . ? C22 C27 C28 113.0(2) . . ? C22 C27 C29 111.33(19) . . ? C29 C27 C28 108.6(2) . . ? C26 C30 C31 112.6(2) . . ? C26 C30 C32 109.81(19) . . ? C31 C30 C32 110.6(2) . . ? C34 C33 C39 111.20(17) . . ? C38 C33 C34 108.79(17) . . ? C38 C33 C39 108.29(17) . . ? N1 C33 C34 108.61(15) . . ? N1 C33 C38 107.89(16) . . ? N1 C33 C39 111.96(16) . . ? C35 C34 C33 113.67(17) . . ? C34 C35 C36 108.73(18) . . ? C35 C36 C37 113.16(17) . . ? C40 C37 C36 110.99(17) . . ? C41 C37 C36 108.98(17) . . ? C41 C37 C40 108.12(17) . . ? N1 C37 C36 109.55(16) . . ? N1 C37 C40 111.61(16) . . ? N1 C37 C41 107.48(16) . . ? C101 C100 C106 120.6(2) . . ? C105 C100 C101 119.3(2) . . ? C105 C100 C106 120.1(2) . . ? C100 C101 C102 119.8(3) . . ? C103 C102 C101 119.9(3) . . ? C104 C103 C102 119.3(3) . . ? C103 C104 C105 120.5(3) . . ? C100 C105 C104 121.2(3) . . ? C201 C200 C206 119.2(4) . . ? C205 C200 C201 118.4(3) . . ? C205 C200 C206 122.4(4) . . ? C200 C201 C202 118.3(3) . . ? C203 C202 C201 117.9(3) . . ? C204 C203 C202 122.4(3) . . ? C203 C204 C205 120.2(3) . . ? C200 C205 C204 122.8(3) . . ? C33 N1 Ni1 117.53(12) . . ? C37 N1 C33 118.79(15) . . ? C37 N1 Ni1 120.74(12) . . ? O1 N1 C33 110.52(14) . . ? O1 N1 C37 110.16(14) . . ? O1 N1 Ni1 63.99(8) . . ? C1 N2 C2 112.03(16) . . ? C1 N2 C9 126.11(16) . . ? C2 N2 C9 121.83(16) . . ? C1 N3 C3 111.65(16) . . ? C1 N3 C21 126.72(16) . . ? C3 N3 C21 121.35(16) . . ? N1 O1 Ni1 72.94(9) . . ? C1 Ni1 C4 97.10(9) . . ? C1 Ni1 N1 147.56(8) . . ? N1 Ni1 C4 115.33(8) . . ? O1 Ni1 C1 104.50(7) . . ? O1 Ni1 C4 158.38(8) . . ? O1 Ni1 N1 43.07(6) . . ? _shelx_res_file ; TITL tP-1 in P-1 CELL 1.54178 11.1354 12.2243 17.8241 87.524 85.065 87.053 ZERR 2.00 0.0008 0.0005 0.0007 0.004 0.005 0.005 LATT 1 SFAC C H N O NI UNIT 110 150 6 2 2 MERG 2 FMAP 2 PLAN 25 ACTA L.S. 20 WGHT 0.065300 0.671100 FVAR 0.17102 C1 1 0.370459 0.233241 0.217543 11.00000 0.02143 0.01540 = 0.01902 0.00299 -0.00034 0.00059 C2 1 0.212189 0.120925 0.220730 11.00000 0.02809 0.02072 = 0.02709 0.00379 -0.00672 -0.00541 AFIX 43 H2 2 0.157936 0.067977 0.237402 11.00000 -1.20000 AFIX 0 C3 1 0.215188 0.179572 0.154816 11.00000 0.03076 0.02339 = 0.02531 0.00214 -0.00909 -0.00386 AFIX 43 H3 2 0.162979 0.174904 0.117186 11.00000 -1.20000 AFIX 0 C4 1 0.622402 0.253176 0.156730 11.00000 0.03201 0.02073 = 0.01867 0.00205 0.00118 0.00143 C5 1 0.633710 0.133553 0.159438 11.00000 0.03674 0.02201 = 0.02390 -0.00031 0.00032 -0.00048 C6 1 0.748898 0.100460 0.172668 11.00000 0.03635 0.02573 = 0.03249 0.00290 0.00602 0.00818 C7 1 0.817786 0.196015 0.176112 11.00000 0.02412 0.03935 = 0.03236 -0.00097 0.00512 0.00179 C8 1 0.743810 0.286563 0.164055 11.00000 0.03121 0.02723 = 0.02217 -0.00076 0.00636 -0.00275 C9 1 0.326834 0.114046 0.334002 11.00000 0.02239 0.02102 = 0.01948 0.00719 -0.00360 0.00043 C10 1 0.283477 0.177669 0.395144 11.00000 0.01863 0.02417 = 0.02287 0.00534 -0.00184 -0.00161 C11 1 0.298585 0.133137 0.467128 11.00000 0.02937 0.03335 = 0.02128 0.00590 -0.00088 -0.00430 AFIX 43 H11 2 0.271893 0.173525 0.508895 11.00000 -1.20000 AFIX 0 C12 1 0.352830 0.029458 0.477576 11.00000 0.03167 0.03691 = 0.02642 0.01625 -0.00722 -0.00525 AFIX 43 H12 2 0.361836 0.001010 0.526116 11.00000 -1.20000 AFIX 0 C13 1 0.393357 -0.031486 0.416556 11.00000 0.02967 0.02298 = 0.03599 0.01431 -0.00653 -0.00087 AFIX 43 H13 2 0.429037 -0.101013 0.424515 11.00000 -1.20000 AFIX 0 C14 1 0.381963 0.009059 0.342746 11.00000 0.02204 0.02010 = 0.03002 0.00657 -0.00148 -0.00199 C15 1 0.216591 0.287502 0.384596 11.00000 0.02189 0.02338 = 0.02439 0.00369 0.00168 0.00104 AFIX 13 H15 2 0.250386 0.322703 0.337576 11.00000 -1.20000 AFIX 0 C16 1 0.227548 0.365155 0.448581 11.00000 0.03297 0.03080 = 0.03366 -0.00410 0.00286 0.00331 AFIX 33 H16A 2 0.183315 0.432983 0.438672 11.00000 -1.50000 H16B 2 0.310966 0.379077 0.451845 11.00000 -1.50000 H16C 2 0.195229 0.332076 0.495330 11.00000 -1.50000 AFIX 0 C17 1 0.082586 0.270495 0.377012 11.00000 0.02319 0.03229 = 0.03983 0.00439 -0.00325 0.00283 AFIX 33 H17A 2 0.040705 0.340367 0.370203 11.00000 -1.50000 H17B 2 0.048334 0.233523 0.421816 11.00000 -1.50000 H17C 2 0.074929 0.226960 0.334276 11.00000 -1.50000 AFIX 0 C18 1 0.425391 -0.061584 0.277029 11.00000 0.03590 0.01913 = 0.03553 0.00476 0.00077 0.00103 AFIX 13 H18 2 0.420663 -0.016090 0.230642 11.00000 -1.20000 AFIX 0 C19 1 0.344444 -0.157598 0.272405 11.00000 0.05531 0.02627 = 0.04926 -0.00521 0.00205 -0.00561 AFIX 33 H19A 2 0.373613 -0.200693 0.230273 11.00000 -1.50000 H19B 2 0.263451 -0.130217 0.266037 11.00000 -1.50000 H19C 2 0.345322 -0.202309 0.317995 11.00000 -1.50000 AFIX 0 C20 1 0.557133 -0.101847 0.281363 11.00000 0.03937 0.02765 = 0.05701 0.00976 0.00890 0.00767 AFIX 33 H20A 2 0.582192 -0.145982 0.239036 11.00000 -1.50000 H20B 2 0.564801 -0.144816 0.327221 11.00000 -1.50000 H20C 2 0.607044 -0.039998 0.280551 11.00000 -1.50000 AFIX 0 C21 1 0.331357 0.331127 0.093894 11.00000 0.02638 0.01983 = 0.02013 0.00382 -0.00754 -0.00104 C22 1 0.286467 0.439473 0.107205 11.00000 0.03013 0.02113 = 0.02344 0.00225 -0.00915 -0.00042 C23 1 0.301373 0.515620 0.046740 11.00000 0.04030 0.01849 = 0.03045 0.00448 -0.01104 -0.00027 AFIX 43 H23 2 0.273361 0.587880 0.053154 11.00000 -1.20000 AFIX 0 C24 1 0.356405 0.486343 -0.021960 11.00000 0.04629 0.02726 = 0.02866 0.01381 -0.00915 -0.00722 AFIX 43 H24 2 0.365675 0.538968 -0.061017 11.00000 -1.20000 AFIX 0 C25 1 0.398045 0.379581 -0.033538 11.00000 0.03959 0.03412 = 0.01918 0.00608 -0.00218 -0.00061 AFIX 43 H25 2 0.434667 0.361064 -0.080450 11.00000 -1.20000 AFIX 0 C26 1 0.385943 0.298932 0.024243 11.00000 0.03239 0.02420 = 0.02038 0.00278 -0.00578 -0.00054 C27 1 0.220689 0.471652 0.181414 11.00000 0.04369 0.02365 = 0.02490 -0.00080 -0.00788 0.00885 AFIX 13 H27 2 0.261951 0.433368 0.222042 11.00000 -1.20000 AFIX 0 C28 1 0.220238 0.595308 0.193750 11.00000 0.05209 0.02942 = 0.04202 -0.00805 -0.01515 0.01408 AFIX 33 H28A 2 0.177732 0.611046 0.241524 11.00000 -1.50000 H28B 2 0.180900 0.634699 0.154247 11.00000 -1.50000 H28C 2 0.301800 0.617435 0.193186 11.00000 -1.50000 AFIX 0 C29 1 0.089798 0.436677 0.187927 11.00000 0.04529 0.03471 = 0.04073 0.00151 0.00642 0.00494 AFIX 33 H29A 2 0.050466 0.457957 0.235488 11.00000 -1.50000 H29B 2 0.088945 0.358552 0.184604 11.00000 -1.50000 H29C 2 0.048037 0.471628 0.147767 11.00000 -1.50000 AFIX 0 C30 1 0.426496 0.180714 0.007685 11.00000 0.04891 0.02697 = 0.02106 0.00120 -0.00481 0.00683 AFIX 13 H30 2 0.426993 0.139021 0.055879 11.00000 -1.20000 AFIX 0 C31 1 0.553949 0.170920 -0.032081 11.00000 0.05848 0.04615 = 0.02823 0.00017 0.00254 0.01753 AFIX 33 H31A 2 0.575300 0.095313 -0.041307 11.00000 -1.50000 H31B 2 0.610247 0.198937 -0.000723 11.00000 -1.50000 H31C 2 0.556154 0.212373 -0.079128 11.00000 -1.50000 AFIX 0 C32 1 0.335480 0.130282 -0.039205 11.00000 0.07333 0.02926 = 0.03458 -0.00655 -0.01519 0.00234 AFIX 33 H32A 2 0.361424 0.055916 -0.049468 11.00000 -1.50000 H32B 2 0.330608 0.171906 -0.085855 11.00000 -1.50000 H32C 2 0.257536 0.131510 -0.011591 11.00000 -1.50000 AFIX 0 C33 1 0.653570 0.314827 0.378400 11.00000 0.02190 0.02704 = 0.01836 0.00402 -0.00294 0.00016 C34 1 0.785744 0.344178 0.363577 11.00000 0.02048 0.02995 = 0.02703 0.00285 -0.00345 -0.00089 AFIX 23 H34A 2 0.831433 0.308906 0.402597 11.00000 -1.20000 H34B 2 0.817879 0.315190 0.315750 11.00000 -1.20000 AFIX 0 C35 1 0.803895 0.466750 0.361655 11.00000 0.02321 0.03298 = 0.03789 -0.00183 -0.00572 -0.00478 AFIX 23 H35A 2 0.888991 0.480303 0.351901 11.00000 -1.20000 H35B 2 0.775447 0.496572 0.409895 11.00000 -1.20000 AFIX 0 C36 1 0.733623 0.521675 0.299653 11.00000 0.02890 0.02328 = 0.02944 0.00066 0.00040 -0.00531 AFIX 23 H36A 2 0.766622 0.494555 0.251449 11.00000 -1.20000 H36B 2 0.744272 0.599998 0.298644 11.00000 -1.20000 AFIX 0 C37 1 0.597955 0.501344 0.309884 11.00000 0.02546 0.01948 = 0.02269 0.00075 -0.00062 -0.00352 C38 1 0.644197 0.192960 0.365001 11.00000 0.02722 0.02745 = 0.02890 0.01011 -0.00609 0.00014 AFIX 33 H38A 2 0.561540 0.173739 0.373964 11.00000 -1.50000 H38B 2 0.692405 0.150291 0.398744 11.00000 -1.50000 H38C 2 0.672762 0.178342 0.313884 11.00000 -1.50000 AFIX 0 C39 1 0.605825 0.335951 0.459990 11.00000 0.02893 0.04306 = 0.01916 0.00327 -0.00267 -0.00178 AFIX 33 H39A 2 0.610943 0.412224 0.469438 11.00000 -1.50000 H39B 2 0.653404 0.292645 0.493753 11.00000 -1.50000 H39C 2 0.523226 0.316216 0.467880 11.00000 -1.50000 AFIX 0 C40 1 0.535350 0.566854 0.374816 11.00000 0.03413 0.02695 = 0.03104 -0.00624 -0.00159 0.00242 AFIX 33 H40A 2 0.570267 0.544666 0.420810 11.00000 -1.50000 H40B 2 0.450835 0.553263 0.379891 11.00000 -1.50000 H40C 2 0.545747 0.643651 0.364405 11.00000 -1.50000 AFIX 0 C41 1 0.540694 0.538684 0.237821 11.00000 0.04256 0.02033 = 0.02774 0.00367 -0.00731 -0.00070 AFIX 33 H41A 2 0.455966 0.526041 0.243724 11.00000 -1.50000 H41B 2 0.578141 0.498058 0.196454 11.00000 -1.50000 H41C 2 0.551923 0.615459 0.227915 11.00000 -1.50000 AFIX 0 C100 1 1.036569 0.768054 0.398818 11.00000 0.03399 0.03827 = 0.02833 0.00165 0.00415 -0.00483 C101 1 0.940586 0.782012 0.355077 11.00000 0.04319 0.05171 = 0.03894 -0.00193 -0.00792 -0.00481 AFIX 43 H101 2 0.906234 0.721339 0.337466 11.00000 -1.20000 AFIX 0 C102 1 0.894661 0.888093 0.337110 11.00000 0.04265 0.08691 = 0.03913 0.01225 -0.00555 0.00535 AFIX 43 H102 2 0.829567 0.897825 0.307728 11.00000 -1.20000 AFIX 0 C103 1 0.946599 0.978657 0.363290 11.00000 0.05381 0.03949 = 0.05320 0.01192 0.01243 0.00822 AFIX 43 H103 2 0.917034 1.049191 0.351243 11.00000 -1.20000 AFIX 0 C104 1 1.041408 0.962849 0.406845 11.00000 0.05361 0.03974 = 0.05968 0.00293 0.00494 -0.01036 AFIX 43 H104 2 1.076533 1.022989 0.424624 11.00000 -1.20000 AFIX 0 C105 1 1.085524 0.858368 0.424694 11.00000 0.03767 0.04372 = 0.04446 0.00219 -0.00155 -0.00828 AFIX 43 H105 2 1.149690 0.849014 0.454851 11.00000 -1.20000 AFIX 0 C106 1 1.087905 0.654630 0.418225 11.00000 0.05120 0.04064 = 0.04753 0.00088 -0.00470 -0.00043 AFIX 33 H10A 2 1.154003 0.660114 0.448853 11.00000 -1.50000 H10B 2 1.115968 0.618704 0.372715 11.00000 -1.50000 H10C 2 1.026383 0.612959 0.445448 11.00000 -1.50000 AFIX 0 C200 1 1.026336 0.831500 0.082279 11.00000 0.04269 0.03863 = 0.06304 -0.00759 -0.02116 0.00383 C201 1 0.939524 0.777957 0.132189 11.00000 0.06874 0.08687 = 0.03424 -0.01284 -0.01533 0.04185 AFIX 43 H201 2 0.914622 0.805871 0.179012 11.00000 -1.20000 AFIX 0 C202 1 0.890910 0.678860 0.108218 11.00000 0.04314 0.05825 = 0.04932 0.01966 0.00080 0.00456 AFIX 43 H202 2 0.833254 0.641728 0.138869 11.00000 -1.20000 AFIX 0 C203 1 0.932109 0.641901 0.039662 11.00000 0.04180 0.04260 = 0.05654 -0.00211 -0.00756 0.00116 AFIX 43 H203 2 0.901156 0.578655 0.023368 11.00000 -1.20000 AFIX 0 C204 1 1.015862 0.693178 -0.005536 11.00000 0.04792 0.05868 = 0.04637 -0.00423 -0.00836 0.00119 AFIX 43 H204 2 1.042399 0.664889 -0.051999 11.00000 -1.20000 AFIX 0 C205 1 1.061815 0.785818 0.016221 11.00000 0.04627 0.05498 = 0.04750 0.00167 -0.00399 0.00264 AFIX 43 H205 2 1.120462 0.819401 -0.015852 11.00000 -1.20000 AFIX 0 C206 1 1.077109 0.934806 0.105626 11.00000 0.09549 0.06766 = 0.16417 -0.04417 -0.05611 -0.00441 AFIX 33 H20D 2 1.040370 0.953599 0.154376 11.00000 -1.50000 H20E 2 1.060739 0.993167 0.069604 11.00000 -1.50000 H20F 2 1.162734 0.923814 0.107848 11.00000 -1.50000 AFIX 0 N1 3 0.580265 0.379498 0.322166 11.00000 0.01858 0.01994 = 0.01739 0.00220 -0.00087 -0.00121 N2 3 0.306161 0.155369 0.258649 11.00000 0.02329 0.01690 = 0.01922 0.00452 -0.00315 -0.00047 N3 3 0.310531 0.247979 0.153707 11.00000 0.02770 0.01670 = 0.01884 0.00332 -0.00469 -0.00105 O1 4 0.457507 0.360445 0.336759 11.00000 0.01710 0.02702 = 0.02046 0.00087 -0.00005 -0.00187 NI1 5 0.508419 0.297233 0.246918 11.00000 0.02037 0.01771 = 0.01720 0.00231 -0.00188 -0.00034 H7 2 0.892119 0.194721 0.184141 11.00000 0.03652 H4 2 0.571790 0.291605 0.123368 11.00000 0.03184 H8 2 0.770766 0.360234 0.161470 11.00000 0.03336 H5 2 0.572450 0.086984 0.152782 11.00000 0.03081 H6 2 0.778571 0.032865 0.177199 11.00000 0.03132 HKLF 4 REM tP-1 in P-1 REM R1 = 0.0476 for 7547 Fo > 4sig(Fo) and 0.0606 for all 9329 data REM 561 parameters refined using 0 restraints END WGHT 0.0653 0.6716 REM Highest difference peak 0.646, deepest hole -0.347, 1-sigma level 0.057 Q1 1 1.1213 0.9238 0.0426 11.00000 0.05 0.65 Q2 1 0.8904 0.7350 0.1646 11.00000 0.05 0.60 Q3 1 0.9772 0.8317 0.1445 11.00000 0.05 0.49 Q4 1 0.4314 0.2760 0.2233 11.00000 0.05 0.42 Q5 1 1.0049 0.7573 0.0179 11.00000 0.05 0.40 Q6 1 1.0452 0.5999 0.3892 11.00000 0.05 0.32 Q7 1 0.8538 0.8245 0.3312 11.00000 0.05 0.32 Q8 1 0.3351 0.1582 0.3615 11.00000 0.05 0.29 Q9 1 0.1559 0.2728 0.3789 11.00000 0.05 0.29 Q10 1 1.1881 0.6510 0.3992 11.00000 0.05 0.28 Q11 1 0.5981 0.5836 0.4150 11.00000 0.05 0.27 Q12 1 0.1432 0.6254 0.1740 11.00000 0.05 0.26 Q13 1 0.3201 0.1407 0.2926 11.00000 0.05 0.25 Q14 1 0.3090 0.6349 0.1611 11.00000 0.05 0.25 Q15 1 1.0688 0.6402 0.4756 11.00000 0.05 0.25 Q16 1 0.2892 0.0772 0.4697 11.00000 0.05 0.24 Q17 1 1.1371 0.7213 0.4177 11.00000 0.05 0.23 Q18 1 0.5541 0.1527 0.3971 11.00000 0.05 0.23 Q19 1 0.7157 0.3327 0.3615 11.00000 0.05 0.23 Q20 1 0.8542 0.9581 0.3390 11.00000 0.05 0.23 Q21 1 0.4523 0.5192 0.4033 11.00000 0.05 0.23 Q22 1 0.3848 0.3173 0.0661 11.00000 0.05 0.23 Q23 1 0.2522 0.2210 0.3876 11.00000 0.05 0.23 Q24 1 0.3410 0.4076 0.1078 11.00000 0.05 0.22 Q25 1 0.5838 0.2641 0.2321 11.00000 0.05 0.22 ; _shelx_res_checksum 59663 _database_code_depnum_ccdc_archive 'CCDC 995931' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6-S _audit_creation_date 2013-10-29 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C64 H82 N4 Ni2 S2' _chemical_formula_sum 'C64 H82 N4 Ni2 S2' _chemical_formula_weight 1088.88 _chemical_melting_point ? _chemical_oxdiff_formula 'C64 H82 N4 Ni2 S2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 13.0231(5) _cell_length_b 14.2423(6) _cell_length_c 18.1147(5) _cell_angle_alpha 100.585(3) _cell_angle_beta 95.676(3) _cell_angle_gamma 114.757(4) _cell_volume 2940.41(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11760 _cell_measurement_temperature 123.01(10) _cell_measurement_theta_max 73.6810 _cell_measurement_theta_min 3.7720 _exptl_absorpt_coefficient_mu 1.766 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour_lustre ? _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1164 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_unetI/netI 0.0299 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 21454 _diffrn_reflns_theta_full 66.97 _diffrn_reflns_theta_max 73.66 _diffrn_reflns_theta_min 3.53 _diffrn_ambient_temperature 123.01(10) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9908 _diffrn_measured_fraction_theta_max 0.9552 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0843600000 _diffrn_orient_matrix_UB_12 -0.0500490000 _diffrn_orient_matrix_UB_13 -0.0041758000 _diffrn_orient_matrix_UB_21 -0.0815799000 _diffrn_orient_matrix_UB_22 -0.0862048000 _diffrn_orient_matrix_UB_23 -0.0717429000 _diffrn_orient_matrix_UB_31 0.0623087000 _diffrn_orient_matrix_UB_32 0.0720489000 _diffrn_orient_matrix_UB_33 -0.0512135000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9816 _reflns_number_total 11356 _reflns_odcompleteness_completeness 99.08 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2\s(I) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.281 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.046 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 649 _refine_ls_number_reflns 11356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0302 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.0071P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.0782 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.029) H3(0.028) H4(0.036) H5(0.034) H6(0.036) H7(0.039) H8(0.039) H11(0.035) H12(0.041) H13(0.036) H15(0.031) H16A(0.082) H16B(0.082) H16C(0.082) H17A(0.093) H17B(0.093) H17C(0.093) H18(0.031) H19A(0.051) H19B(0.051) H19C(0.051) H20A(0.057) H20B(0.057) H20C(0.057) H23(0.032) H24(0.038) H25(0.034) H27(0.028) H28A(0.047) H28B(0.047) H28C(0.047) H29A(0.054) H29B(0.054) H29C(0.054) H30(0.03) H31A(0.06) H31B(0.06) H31C(0.06) H32A(0.067) H32B(0.067) H32C(0.067) H34(0.027) H35(0.028) H36(0.035) H37(0.03) H38(0.03) H39(0.034) H40(0.036) H43(0.039) H44(0.047) H45(0.04) H47(0.035) H48A(0.055) H48B(0.055) H48C(0.055) H49A(0.066) H49B(0.066) H49C(0.066) H50(0.035) H51A(0.065) H51B(0.065) H51C(0.065) H52A(0.057) H52B(0.057) H52C(0.057) H55(0.044) H56(0.053) H57(0.046) H59(0.031) H60A(0.069) H60B(0.069) H60C(0.069) H61A(0.068) H61B(0.068) H61C(0.068) H62(0.039) H63A(0.072) H63B(0.072) H63C(0.072) H64A(0.072) H64B(0.072) H64C(0.072) Fixed X: H2(0.8044) H3(0.6422) H4(0.4591) H5(0.3736) H6(0.5366) H7(0.7193) H8(0.669) H11(0.8301) H12(0.9813) H13(1.0128) H15(0.6104) H16A(0.5508) H16B(0.6667) H16C(0.5783) H17A(0.655) H17B(0.7455) H17C(0.7766) H18(0.8357) H19A(0.945) H19B(0.8647) H19C(0.9961) H20A(1.0209) H20B(1.0728) H20C(0.9873) H23(0.2349) H24(0.2207) H25(0.3529) H27(0.4452) H28A(0.2757) H28B(0.2528) H28C(0.2111) H29A(0.4222) H29B(0.3633) H29C(0.4939) H30(0.5719) H31A(0.5561) H31B(0.4655) H31C(0.4354) H32A(0.7036) H32B(0.6837) H32C(0.6246) H34(0.0057) H35(-0.1549) H36(-0.0533) H37(0.1327) H38(0.2936) H39(0.2052) H40(-0.0074) H43(0.4207) H44(0.4392) H45(0.3012) H47(0.2) H48A(0.364) H48B(0.3904) H48C(0.4358) H49A(0.2256) H49B(0.2894) H49C(0.158) H50(0.0698) H51A(0.0763) H51B(0.1716) H51C(0.1987) H52A(-0.0602) H52B(-0.0314) H52C(0.0264) H55(- 0.2047) H56(-0.3491) H57(-0.3631) H59(0.0313) H60A(0.0847) H60B(-0.0345) H60C(0.0539) H61A(-0.1036) H61B(-0.1283) H61C(-0.007) H62(-0.163) H63A(- 0.2683) H63B(-0.2006) H63C(-0.3332) H64A(-0.3356) H64B(-0.4032) H64C(-0.3113) Fixed Y: H2(0.4191) H3(0.4637) H4(0.161) H5(-0.0182) H6(-0.0513) H7(0.1134) H8(0.2502) H11(0.051) H12(0.1225) H13(0.272) H15(0.1343) H16A(-0.0341) H16B(- 0.0345) H16C(-0.0365) H17A(0.1311) H17B(0.2355) H17C(0.1415) H18(0.4074) H19A(0.451) H19B(0.3278) H19C(0.3721) H20A(0.5531) H20B(0.4771) H20C(0.498) H23(0.3359) H24(0.4063) H25(0.4317) H27(0.2478) H28A(0.1475) H28B(0.1246) H28C(0.2004) H29A(0.3207) H29B(0.3814) H29C(0.4124) H30(0.3499) H31A(0.4091) H31B(0.4457) H31C(0.3241) H32A(0.5231) H32B(0.5138) H32C(0.5679) H34(-0.4446) H35(-0.4314) H36(0.0043) H37(0.1225) H38(0.1459) H39(0.0543) H40(-0.0502) H43(- 0.2865) H44(-0.2262) H45(-0.1862) H47(-0.3112) H48A(-0.2858) H48B(-0.1843) H48C(-0.2659) H49A(-0.4638) H49B(-0.4515) H49C(-0.4793) H50(-0.1735) H51A(- 0.1223) H51B(-0.1595) H51C(-0.0621) H52A(-0.2993) H52B(-0.3566) H52C(-0.3481) H55(-0.1407) H56(-0.1455) H57(-0.2036) H59(-0.1899) H60A(-0.0772) H60B(- 0.0737) H60C(-0.0228) H61A(-0.3443) H61B(-0.2738) H61C(-0.2731) H62(-0.273) H63A(-0.2312) H63B(-0.1322) H63C(-0.2026) H64A(-0.4128) H64B(-0.3938) H64C(- 0.4353) Fixed Z: H2(0.4913) H3(0.4795) H4(0.1218) H5(0.1507) H6(0.2072) H7(0.2251) H8(0.182) H11(0.4198) H12(0.359) H13(0.3154) H15(0.4409) H16A(0.4645) H16B(0.4484) H16C(0.382) H17A(0.5692) H17B(0.5526) H17C(0.5574) H18(0.322) H19A(0.2272) H19B(0.206) H19C(0.2405) H20A(0.361) H20B(0.3802) H20C(0.4282) H23(0.4203) H24(0.3177) H25(0.2388) H27(0.4718) H28A(0.5127) H28B(0.4231) H28C(0.4712) H29A(0.5924) H29B(0.5552) H29C(0.5553) H30(0.2446) H31A(0.1338) H31B(0.1618) H31C(0.141) H32A(0.246) H32B(0.3288) H32C(0.2836) H34(0.1053) H35(0.1585) H36(0.2022) H37(0.2925) H38(0.2197) H39(0.0817) H40(0.0737) H43(0.1239) H44(0.0143) H45(-0.0413) H47(0.2316) H48A(0.3152) H48B(0.2838) H48C(0.2503) H49A(0.2378) H49B(0.1686) H49C(0.1565) H50(0.0329) H51A(-0.083) H51B(-0.098) H51C(-0.0295) H52A(-0.077) H52B(-0.0178) H52C(-0.0898) H55(0.362) H56(0.2755) H57(0.1465) H59(0.3177) H60A(0.4403) H60B(0.4305) H60C(0.3796) H61A(0.3451) H61B(0.4114) H61C(0.4178) H62(0.0586) H63A(-0.0315) H63B(0.0386) H63C(0.0306) H64A(-0.0167) H64B(0.0468) H64C(0.0631) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.60278(12) 0.26139(11) 0.35061(8) 0.0166(3) Uani 1 1 d . . . C2 C 0.73708(14) 0.38348(13) 0.45413(9) 0.0246(3) Uani 1 1 d . . . H2 H 0.8044 0.4191 0.4913 0.029 Uiso 1 1 calc R . . C3 C 0.64823(13) 0.40778(13) 0.44770(8) 0.0235(3) Uani 1 1 d . . . H3 H 0.6422 0.4637 0.4795 0.028 Uiso 1 1 calc R . . C4 C 0.49874(15) 0.13127(15) 0.14716(9) 0.0298(4) Uani 1 1 d . . . H4 H 0.4591 0.1610 0.1218 0.036 Uiso 1 1 calc R . . C5 C 0.45155(14) 0.02945(14) 0.16124(9) 0.0280(4) Uani 1 1 d . . . H5 H 0.3736 -0.0182 0.1507 0.034 Uiso 1 1 calc R . . C6 C 0.54389(16) 0.01134(14) 0.19462(9) 0.0299(4) Uani 1 1 d . . . H6 H 0.5366 -0.0513 0.2072 0.036 Uiso 1 1 calc R . . C7 C 0.64594(15) 0.10330(15) 0.20493(9) 0.0322(4) Uani 1 1 d . . . H7 H 0.7193 0.1134 0.2251 0.039 Uiso 1 1 calc R . . C8 C 0.61749(15) 0.17985(14) 0.17873(9) 0.0322(4) Uani 1 1 d . . . H8 H 0.6690 0.2502 0.1820 0.039 Uiso 1 1 calc R . . C9 C 0.78539(12) 0.24601(13) 0.38412(8) 0.0202(3) Uani 1 1 d . . . C10 C 0.76506(13) 0.15624(13) 0.41229(8) 0.0226(3) Uani 1 1 d . . . C11 C 0.84108(15) 0.11108(15) 0.40196(10) 0.0293(4) Uani 1 1 d . . . H11 H 0.8301 0.0510 0.4198 0.035 Uiso 1 1 calc R . . C12 C 0.93222(16) 0.15417(16) 0.36574(11) 0.0342(4) Uani 1 1 d . . . H12 H 0.9813 0.1225 0.3590 0.041 Uiso 1 1 calc R . . C13 C 0.95094(14) 0.24382(15) 0.33953(10) 0.0298(4) Uani 1 1 d . . . H13 H 1.0128 0.2720 0.3154 0.036 Uiso 1 1 calc R . . C14 C 0.87847(13) 0.29302(13) 0.34866(9) 0.0235(3) Uani 1 1 d . . . C15 C 0.66884(14) 0.11131(14) 0.45570(9) 0.0260(3) Uani 1 1 d . . . H15 H 0.6104 0.1343 0.4409 0.031 Uiso 1 1 calc R . . C16 C 0.6108(2) -0.00951(17) 0.43582(16) 0.0548(6) Uani 1 1 d . . . H16A H 0.5508 -0.0341 0.4645 0.082 Uiso 1 1 calc R . . H16B H 0.6667 -0.0345 0.4484 0.082 Uiso 1 1 calc R . . H16C H 0.5783 -0.0365 0.3820 0.082 Uiso 1 1 calc R . . C17 C 0.71583(19) 0.1593(3) 0.54173(11) 0.0623(8) Uani 1 1 d . . . H17A H 0.6550 0.1311 0.5692 0.093 Uiso 1 1 calc R . . H17B H 0.7455 0.2355 0.5526 0.093 Uiso 1 1 calc R . . H17C H 0.7766 0.1415 0.5574 0.093 Uiso 1 1 calc R . . C18 C 0.90380(14) 0.39421(13) 0.32217(9) 0.0262(3) Uani 1 1 d . . . H18 H 0.8357 0.4074 0.3220 0.031 Uiso 1 1 calc R . . C19 C 0.92983(16) 0.38548(15) 0.24147(10) 0.0339(4) Uani 1 1 d . . . H19A H 0.9450 0.4510 0.2272 0.051 Uiso 1 1 calc R . . H19B H 0.8647 0.3278 0.2060 0.051 Uiso 1 1 calc R . . H19C H 0.9961 0.3721 0.2405 0.051 Uiso 1 1 calc R . . C20 C 1.00574(17) 0.48951(15) 0.37813(11) 0.0382(4) Uani 1 1 d . . . H20A H 1.0209 0.5531 0.3610 0.057 Uiso 1 1 calc R . . H20B H 1.0728 0.4771 0.3802 0.057 Uiso 1 1 calc R . . H20C H 0.9873 0.4980 0.4282 0.057 Uiso 1 1 calc R . . C21 C 0.46316(12) 0.34298(11) 0.36040(8) 0.0182(3) Uani 1 1 d . . . C22 C 0.38096(13) 0.32234(12) 0.40752(9) 0.0204(3) Uani 1 1 d . . . C23 C 0.29027(14) 0.34750(13) 0.38975(10) 0.0265(3) Uani 1 1 d . . . H23 H 0.2349 0.3359 0.4203 0.032 Uiso 1 1 calc R . . C24 C 0.28116(14) 0.38909(14) 0.32798(11) 0.0313(4) Uani 1 1 d . . . H24 H 0.2207 0.4063 0.3177 0.038 Uiso 1 1 calc R . . C25 C 0.36139(14) 0.40539(13) 0.28116(10) 0.0282(3) Uani 1 1 d . . . H25 H 0.3529 0.4317 0.2388 0.034 Uiso 1 1 calc R . . C26 C 0.45498(13) 0.38320(12) 0.29621(9) 0.0209(3) Uani 1 1 d . . . C27 C 0.38620(14) 0.27330(13) 0.47467(9) 0.0237(3) Uani 1 1 d . . . H27 H 0.4452 0.2478 0.4718 0.028 Uiso 1 1 calc R . . C28 C 0.27066(15) 0.17751(14) 0.46997(10) 0.0313(4) Uani 1 1 d . . . H28A H 0.2757 0.1475 0.5127 0.047 Uiso 1 1 calc R . . H28B H 0.2528 0.1246 0.4231 0.047 Uiso 1 1 calc R . . H28C H 0.2111 0.2004 0.4712 0.047 Uiso 1 1 calc R . . C29 C 0.41951(18) 0.35450(15) 0.55150(10) 0.0360(4) Uani 1 1 d . . . H29A H 0.4222 0.3207 0.5924 0.054 Uiso 1 1 calc R . . H29B H 0.3633 0.3814 0.5552 0.054 Uiso 1 1 calc R . . H29C H 0.4939 0.4124 0.5553 0.054 Uiso 1 1 calc R . . C30 C 0.54455(14) 0.40457(13) 0.24573(9) 0.0248(3) Uani 1 1 d . . . H30 H 0.5719 0.3499 0.2446 0.030 Uiso 1 1 calc R . . C31 C 0.49584(19) 0.39500(17) 0.16290(10) 0.0403(4) Uani 1 1 d . . . H31A H 0.5561 0.4091 0.1338 0.060 Uiso 1 1 calc R . . H31B H 0.4655 0.4457 0.1618 0.060 Uiso 1 1 calc R . . H31C H 0.4354 0.3241 0.1410 0.060 Uiso 1 1 calc R . . C32 C 0.64870(17) 0.51229(17) 0.27911(11) 0.0448(5) Uani 1 1 d . . . H32A H 0.7036 0.5231 0.2460 0.067 Uiso 1 1 calc R . . H32B H 0.6837 0.5138 0.3288 0.067 Uiso 1 1 calc R . . H32C H 0.6246 0.5679 0.2836 0.067 Uiso 1 1 calc R . . C33 C 0.04939(12) -0.20516(11) 0.16646(8) 0.0169(3) Uani 1 1 d . . . C34 C 0.00094(13) -0.38209(12) 0.12605(9) 0.0226(3) Uani 1 1 d . . . H34 H 0.0057 -0.4446 0.1053 0.027 Uiso 1 1 calc R . . C35 C -0.08705(14) -0.37500(12) 0.15520(9) 0.0231(3) Uani 1 1 d . . . H35 H -0.1549 -0.4314 0.1585 0.028 Uiso 1 1 calc R . . C36 C 0.01982(15) 0.02614(13) 0.19052(10) 0.0293(4) Uani 1 1 d . . . H36 H -0.0533 0.0043 0.2022 0.035 Uiso 1 1 calc R . . C37 C 0.12375(14) 0.09258(12) 0.24073(9) 0.0252(3) Uani 1 1 d . . . H37 H 0.1327 0.1225 0.2925 0.030 Uiso 1 1 calc R . . C38 C 0.21514(14) 0.10722(12) 0.19906(10) 0.0251(3) Uani 1 1 d . . . H38 H 0.2936 0.1459 0.2197 0.030 Uiso 1 1 calc R . . C39 C 0.16607(16) 0.05336(13) 0.12207(10) 0.0284(3) Uani 1 1 d . . . H39 H 0.2052 0.0543 0.0817 0.034 Uiso 1 1 calc R . . C40 C 0.04594(15) -0.00258(13) 0.11727(10) 0.0301(4) Uani 1 1 d . . . H40 H -0.0074 -0.0502 0.0737 0.036 Uiso 1 1 calc R . . C41 C 0.18710(13) -0.25824(12) 0.10176(9) 0.0207(3) Uani 1 1 d . . . C42 C 0.27069(14) -0.28140(12) 0.13732(9) 0.0241(3) Uani 1 1 d . . . C43 C 0.36453(15) -0.26992(15) 0.10232(11) 0.0327(4) Uani 1 1 d . . . H43 H 0.4207 -0.2865 0.1239 0.039 Uiso 1 1 calc R . . C44 C 0.37541(16) -0.23442(16) 0.03631(11) 0.0392(4) Uani 1 1 d . . . H44 H 0.4392 -0.2262 0.0143 0.047 Uiso 1 1 calc R . . C45 C 0.29211(16) -0.21103(15) 0.00277(10) 0.0336(4) Uani 1 1 d . . . H45 H 0.3012 -0.1862 -0.0413 0.040 Uiso 1 1 calc R . . C46 C 0.19475(15) -0.22395(12) 0.03367(9) 0.0249(3) Uani 1 1 d . . . C47 C 0.26215(14) -0.32077(14) 0.21000(10) 0.0288(4) Uani 1 1 d . . . H47 H 0.2000 -0.3112 0.2316 0.035 Uiso 1 1 calc R . . C48 C 0.37344(16) -0.25839(16) 0.27047(11) 0.0366(4) Uani 1 1 d . . . H48A H 0.3640 -0.2858 0.3152 0.055 Uiso 1 1 calc R . . H48B H 0.3904 -0.1843 0.2838 0.055 Uiso 1 1 calc R . . H48C H 0.4358 -0.2659 0.2503 0.055 Uiso 1 1 calc R . . C49 C 0.23088(18) -0.43995(16) 0.19151(13) 0.0443(5) Uani 1 1 d . . . H49A H 0.2256 -0.4638 0.2378 0.066 Uiso 1 1 calc R . . H49B H 0.2894 -0.4515 0.1686 0.066 Uiso 1 1 calc R . . H49C H 0.1580 -0.4793 0.1565 0.066 Uiso 1 1 calc R . . C50 C 0.09937(16) -0.20617(14) -0.00666(9) 0.0295(4) Uani 1 1 d . . . H50 H 0.0698 -0.1735 0.0329 0.035 Uiso 1 1 calc R . . C51 C 0.1403(2) -0.13045(16) -0.05918(11) 0.0433(5) Uani 1 1 d . . . H51A H 0.0763 -0.1223 -0.0830 0.065 Uiso 1 1 calc R . . H51B H 0.1716 -0.1595 -0.0980 0.065 Uiso 1 1 calc R . . H51C H 0.1987 -0.0621 -0.0295 0.065 Uiso 1 1 calc R . . C52 C -0.00080(17) -0.31245(16) -0.05208(10) 0.0380(4) Uani 1 1 d . . . H52A H -0.0602 -0.2993 -0.0770 0.057 Uiso 1 1 calc R . . H52B H -0.0314 -0.3566 -0.0178 0.057 Uiso 1 1 calc R . . H52C H 0.0264 -0.3481 -0.0898 0.057 Uiso 1 1 calc R . . C53 C -0.13697(13) -0.23008(12) 0.20723(9) 0.0210(3) Uani 1 1 d . . . C54 C -0.12583(13) -0.19359(13) 0.28608(9) 0.0245(3) Uani 1 1 d . . . C55 C -0.20843(15) -0.16361(16) 0.30990(11) 0.0366(4) Uani 1 1 d . . . H55 H -0.2047 -0.1407 0.3620 0.044 Uiso 1 1 calc R . . C56 C -0.29561(16) -0.16703(18) 0.25807(13) 0.0444(5) Uani 1 1 d . . . H56 H -0.3491 -0.1455 0.2755 0.053 Uiso 1 1 calc R . . C57 C -0.30405(15) -0.20203(16) 0.18080(12) 0.0386(4) Uani 1 1 d . . . H57 H -0.3631 -0.2036 0.1465 0.046 Uiso 1 1 calc R . . C58 C -0.22533(14) -0.23522(13) 0.15308(10) 0.0271(3) Uani 1 1 d . . . C59 C -0.02890(14) -0.18570(13) 0.34458(9) 0.0257(3) Uani 1 1 d . . . H59 H 0.0313 -0.1899 0.3177 0.031 Uiso 1 1 calc R . . C60 C 0.0236(2) -0.08021(16) 0.40420(12) 0.0459(5) Uani 1 1 d . . . H60A H 0.0847 -0.0772 0.4403 0.069 Uiso 1 1 calc R . . H60B H -0.0345 -0.0737 0.4305 0.069 Uiso 1 1 calc R . . H60C H 0.0539 -0.0228 0.3796 0.069 Uiso 1 1 calc R . . C61 C -0.07083(18) -0.27776(16) 0.38332(13) 0.0456(5) Uani 1 1 d . . . H61A H -0.1036 -0.3443 0.3451 0.068 Uiso 1 1 calc R . . H61B H -0.1283 -0.2738 0.4114 0.068 Uiso 1 1 calc R . . H61C H -0.0070 -0.2731 0.4178 0.068 Uiso 1 1 calc R . . C62 C -0.23662(15) -0.27447(15) 0.06750(10) 0.0324(4) Uani 1 1 d . . . H62 H -0.1630 -0.2730 0.0586 0.039 Uiso 1 1 calc R . . C63 C -0.26205(18) -0.20351(18) 0.02206(13) 0.0481(5) Uani 1 1 d . . . H63A H -0.2683 -0.2312 -0.0315 0.072 Uiso 1 1 calc R . . H63B H -0.2006 -0.1322 0.0386 0.072 Uiso 1 1 calc R . . H63C H -0.3332 -0.2026 0.0306 0.072 Uiso 1 1 calc R . . C64 C -0.33044(19) -0.38990(17) 0.03733(12) 0.0477(5) Uani 1 1 d . . . H64A H -0.3356 -0.4128 -0.0167 0.072 Uiso 1 1 calc R . . H64B H -0.4032 -0.3938 0.0468 0.072 Uiso 1 1 calc R . . H64C H -0.3113 -0.4353 0.0631 0.072 Uiso 1 1 calc R . . N1 N 0.70947(10) 0.29519(10) 0.39474(7) 0.0184(2) Uani 1 1 d . . . N2 N 0.56700(10) 0.33361(10) 0.38453(7) 0.0172(2) Uani 1 1 d . . . N3 N 0.08350(11) -0.27875(10) 0.13275(7) 0.0181(2) Uani 1 1 d . . . N4 N -0.05711(10) -0.26735(10) 0.17932(7) 0.0183(2) Uani 1 1 d . . . S1 S 0.39253(3) 0.07194(3) 0.333021(19) 0.01997(8) Uani 1 1 d . . . S2 S 0.25682(3) -0.07030(3) 0.27452(2) 0.01976(8) Uani 1 1 d . . . Ni1 Ni 0.52530(2) 0.14010(2) 0.267707(13) 0.01742(6) Uani 1 1 d . . . Ni2 Ni 0.13115(2) -0.055433(19) 0.194645(14) 0.01697(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0147(6) 0.0197(7) 0.0162(6) 0.0065(5) 0.0057(5) 0.0070(6) C2 0.0200(7) 0.0292(8) 0.0181(7) -0.0047(6) -0.0014(6) 0.0104(6) C3 0.0217(7) 0.0243(8) 0.0192(7) -0.0038(6) 0.0000(6) 0.0099(6) C4 0.0345(9) 0.0406(10) 0.0137(7) 0.0047(6) 0.0077(6) 0.0165(8) C5 0.0230(8) 0.0300(9) 0.0190(7) -0.0060(6) 0.0056(6) 0.0054(7) C6 0.0370(9) 0.0278(8) 0.0244(8) -0.0016(6) 0.0106(7) 0.0163(7) C7 0.0224(8) 0.0432(10) 0.0258(8) -0.0057(7) 0.0080(6) 0.0148(8) C8 0.0311(9) 0.0307(9) 0.0245(8) 0.0011(7) 0.0171(7) 0.0041(7) C9 0.0153(7) 0.0283(8) 0.0173(7) 0.0017(6) 0.0019(5) 0.0120(6) C10 0.0193(7) 0.0312(8) 0.0187(7) 0.0047(6) 0.0027(6) 0.0134(7) C11 0.0288(9) 0.0365(9) 0.0325(9) 0.0132(7) 0.0094(7) 0.0212(8) C12 0.0301(9) 0.0467(11) 0.0407(10) 0.0139(8) 0.0142(8) 0.0283(9) C13 0.0204(8) 0.0416(10) 0.0324(9) 0.0105(7) 0.0124(7) 0.0164(7) C14 0.0185(7) 0.0304(8) 0.0202(7) 0.0030(6) 0.0037(6) 0.0111(6) C15 0.0228(8) 0.0371(9) 0.0244(8) 0.0123(7) 0.0079(6) 0.0167(7) C16 0.0515(13) 0.0408(12) 0.0952(19) 0.0351(12) 0.0460(13) 0.0281(11) C17 0.0353(11) 0.115(2) 0.0243(10) 0.0199(12) 0.0116(8) 0.0198(13) C18 0.0206(8) 0.0306(9) 0.0267(8) 0.0074(7) 0.0070(6) 0.0100(7) C19 0.0314(9) 0.0381(10) 0.0302(9) 0.0122(7) 0.0110(7) 0.0112(8) C20 0.0340(10) 0.0336(10) 0.0380(10) 0.0015(8) 0.0057(8) 0.0100(8) C21 0.0147(7) 0.0174(7) 0.0208(7) 0.0020(5) 0.0016(5) 0.0071(6) C22 0.0188(7) 0.0167(7) 0.0246(7) 0.0042(6) 0.0057(6) 0.0072(6) C23 0.0188(7) 0.0250(8) 0.0389(9) 0.0105(7) 0.0110(7) 0.0106(6) C24 0.0207(8) 0.0297(9) 0.0498(10) 0.0165(8) 0.0057(7) 0.0148(7) C25 0.0244(8) 0.0274(8) 0.0352(9) 0.0156(7) 0.0027(7) 0.0114(7) C26 0.0184(7) 0.0176(7) 0.0237(7) 0.0050(6) 0.0029(6) 0.0055(6) C27 0.0258(8) 0.0263(8) 0.0249(8) 0.0089(6) 0.0113(6) 0.0148(7) C28 0.0329(9) 0.0313(9) 0.0371(9) 0.0168(7) 0.0195(8) 0.0153(8) C29 0.0478(11) 0.0371(10) 0.0265(9) 0.0057(7) 0.0125(8) 0.0220(9) C30 0.0267(8) 0.0262(8) 0.0213(7) 0.0076(6) 0.0062(6) 0.0105(7) C31 0.0501(12) 0.0486(12) 0.0245(9) 0.0159(8) 0.0076(8) 0.0214(10) C32 0.0362(10) 0.0418(11) 0.0352(10) 0.0029(8) 0.0186(8) -0.0023(9) C33 0.0156(7) 0.0199(7) 0.0141(6) 0.0046(5) 0.0030(5) 0.0065(6) C34 0.0246(8) 0.0169(7) 0.0245(7) 0.0060(6) 0.0064(6) 0.0070(6) C35 0.0214(7) 0.0187(7) 0.0255(7) 0.0068(6) 0.0060(6) 0.0045(6) C36 0.0233(8) 0.0265(8) 0.0423(10) 0.0099(7) 0.0066(7) 0.0145(7) C37 0.0306(8) 0.0203(7) 0.0277(8) 0.0037(6) 0.0072(7) 0.0147(7) C38 0.0222(8) 0.0166(7) 0.0353(9) 0.0089(6) 0.0061(6) 0.0065(6) C39 0.0402(10) 0.0259(8) 0.0271(8) 0.0138(7) 0.0126(7) 0.0181(7) C40 0.0350(9) 0.0252(8) 0.0296(8) 0.0053(7) -0.0051(7) 0.0160(7) C41 0.0205(7) 0.0171(7) 0.0230(7) 0.0029(6) 0.0086(6) 0.0070(6) C42 0.0233(8) 0.0198(7) 0.0292(8) 0.0042(6) 0.0085(6) 0.0096(6) C43 0.0247(8) 0.0357(10) 0.0389(10) 0.0043(8) 0.0105(7) 0.0156(7) C44 0.0316(10) 0.0457(11) 0.0395(10) 0.0052(8) 0.0221(8) 0.0154(9) C45 0.0381(10) 0.0348(9) 0.0257(8) 0.0065(7) 0.0180(7) 0.0122(8) C46 0.0310(8) 0.0203(7) 0.0208(7) 0.0022(6) 0.0099(6) 0.0091(7) C47 0.0242(8) 0.0318(9) 0.0369(9) 0.0144(7) 0.0083(7) 0.0157(7) C48 0.0309(9) 0.0458(11) 0.0381(10) 0.0133(8) 0.0042(8) 0.0212(9) C49 0.0406(11) 0.0344(10) 0.0639(13) 0.0218(10) 0.0073(10) 0.0193(9) C50 0.0427(10) 0.0319(9) 0.0189(7) 0.0062(6) 0.0107(7) 0.0203(8) C51 0.0734(15) 0.0410(11) 0.0285(9) 0.0154(8) 0.0198(9) 0.0330(11) C52 0.0418(11) 0.0462(11) 0.0234(8) 0.0078(8) 0.0048(7) 0.0178(9) C53 0.0144(7) 0.0217(7) 0.0248(7) 0.0063(6) 0.0067(6) 0.0052(6) C54 0.0187(7) 0.0246(8) 0.0253(8) 0.0036(6) 0.0071(6) 0.0057(6) C55 0.0267(9) 0.0433(11) 0.0349(9) -0.0011(8) 0.0113(7) 0.0144(8) C56 0.0261(9) 0.0530(12) 0.0578(13) 0.0044(10) 0.0136(9) 0.0236(9) C57 0.0204(8) 0.0469(11) 0.0487(11) 0.0111(9) 0.0022(8) 0.0164(8) C58 0.0180(7) 0.0282(8) 0.0317(9) 0.0097(7) 0.0038(6) 0.0064(6) C59 0.0205(7) 0.0307(9) 0.0211(7) 0.0032(6) 0.0065(6) 0.0078(7) C60 0.0541(13) 0.0298(10) 0.0377(10) 0.0000(8) -0.0143(9) 0.0120(9) C61 0.0349(10) 0.0336(10) 0.0615(13) 0.0164(9) -0.0008(9) 0.0093(9) C62 0.0245(8) 0.0380(10) 0.0292(9) 0.0131(7) 0.0004(7) 0.0079(7) C63 0.0381(11) 0.0513(13) 0.0460(12) 0.0243(10) -0.0061(9) 0.0098(10) C64 0.0478(12) 0.0423(12) 0.0339(10) 0.0084(9) -0.0068(9) 0.0058(10) N1 0.0147(6) 0.0237(6) 0.0163(6) 0.0022(5) 0.0030(5) 0.0091(5) N2 0.0155(6) 0.0193(6) 0.0157(6) 0.0018(5) 0.0030(5) 0.0077(5) N3 0.0184(6) 0.0170(6) 0.0189(6) 0.0047(5) 0.0060(5) 0.0073(5) N4 0.0160(6) 0.0182(6) 0.0183(6) 0.0052(5) 0.0047(5) 0.0047(5) S1 0.01690(17) 0.02148(17) 0.01615(16) 0.00222(13) 0.00441(13) 0.00430(14) S2 0.01739(17) 0.01829(17) 0.02128(17) 0.00606(13) 0.00167(13) 0.00581(14) Ni1 0.01529(12) 0.01913(13) 0.01458(12) 0.00113(9) 0.00400(9) 0.00565(10) Ni2 0.01569(12) 0.01607(12) 0.01795(12) 0.00440(9) 0.00335(9) 0.00590(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3711(18) . ? C1 N2 1.3706(19) . ? C1 Ni1 1.8828(14) . ? C2 C3 1.340(2) . ? C2 N1 1.3840(19) . ? C3 N2 1.3875(19) . ? C4 C5 1.402(3) . ? C4 C8 1.407(3) . ? C4 Ni1 2.1487(16) . ? C5 C6 1.432(2) . ? C5 Ni1 2.0916(15) . ? C6 C7 1.386(3) . ? C6 Ni1 2.1720(16) . ? C7 C8 1.430(3) . ? C7 Ni1 2.2046(16) . ? C8 Ni1 2.1233(16) . ? C9 C10 1.396(2) . ? C9 C14 1.401(2) . ? C9 N1 1.4399(18) . ? C10 C11 1.398(2) . ? C10 C15 1.519(2) . ? C11 C12 1.381(3) . ? C12 C13 1.378(3) . ? C13 C14 1.397(2) . ? C14 C18 1.518(2) . ? C15 C16 1.514(3) . ? C15 C17 1.530(3) . ? C18 C19 1.528(2) . ? C18 C20 1.533(2) . ? C21 C22 1.404(2) . ? C21 C26 1.401(2) . ? C21 N2 1.4467(18) . ? C22 C23 1.396(2) . ? C22 C27 1.519(2) . ? C23 C24 1.376(2) . ? C24 C25 1.382(3) . ? C25 C26 1.396(2) . ? C26 C30 1.518(2) . ? C27 C28 1.531(2) . ? C27 C29 1.527(2) . ? C30 C31 1.528(2) . ? C30 C32 1.521(2) . ? C33 N3 1.3700(19) . ? C33 N4 1.3686(18) . ? C33 Ni2 1.8795(15) . ? C34 C35 1.341(2) . ? C34 N3 1.3857(19) . ? C35 N4 1.383(2) . ? C36 C37 1.386(2) . ? C36 C40 1.432(3) . ? C36 Ni2 2.2088(16) . ? C37 C38 1.434(2) . ? C37 Ni2 2.1656(15) . ? C38 C39 1.401(2) . ? C38 Ni2 2.0884(15) . ? C39 C40 1.412(3) . ? C39 Ni2 2.1477(16) . ? C40 Ni2 2.1312(16) . ? C41 C42 1.396(2) . ? C41 C46 1.405(2) . ? C41 N3 1.4494(19) . ? C42 C43 1.395(2) . ? C42 C47 1.519(2) . ? C43 C44 1.379(3) . ? C44 C45 1.380(3) . ? C45 C46 1.392(2) . ? C46 C50 1.514(2) . ? C47 C48 1.530(2) . ? C47 C49 1.531(3) . ? C50 C51 1.532(2) . ? C50 C52 1.532(3) . ? C53 C54 1.398(2) . ? C53 C58 1.404(2) . ? C53 N4 1.4447(19) . ? C54 C55 1.391(2) . ? C54 C59 1.517(2) . ? C55 C56 1.378(3) . ? C56 C57 1.374(3) . ? C57 C58 1.395(3) . ? C58 C62 1.518(2) . ? C59 C60 1.513(2) . ? C59 C61 1.524(3) . ? C62 C63 1.530(3) . ? C62 C64 1.533(3) . ? S1 S2 2.0476(5) . ? S1 Ni1 2.1800(4) . ? S2 Ni2 2.1797(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 126.98(11) . . ? N2 C1 N1 102.87(12) . . ? N2 C1 Ni1 130.06(11) . . ? C3 C2 N1 106.82(13) . . ? C2 C3 N2 106.89(13) . . ? C5 C4 C8 106.94(16) . . ? C5 C4 Ni1 68.50(9) . . ? C8 C4 Ni1 69.79(9) . . ? C4 C5 C6 108.36(15) . . ? C4 C5 Ni1 72.91(9) . . ? C6 C5 Ni1 73.43(9) . . ? C5 C6 Ni1 67.36(9) . . ? C7 C6 C5 108.17(16) . . ? C7 C6 Ni1 72.83(9) . . ? C6 C7 C8 107.31(15) . . ? C6 C7 Ni1 70.27(9) . . ? C8 C7 Ni1 67.66(9) . . ? C4 C8 C7 108.83(16) . . ? C4 C8 Ni1 71.75(9) . . ? C7 C8 Ni1 73.82(10) . . ? C10 C9 C14 123.28(14) . . ? C10 C9 N1 118.31(13) . . ? C14 C9 N1 118.37(14) . . ? C9 C10 C11 116.97(15) . . ? C9 C10 C15 122.46(14) . . ? C11 C10 C15 120.51(15) . . ? C12 C11 C10 121.13(16) . . ? C13 C12 C11 120.50(15) . . ? C12 C13 C14 121.05(16) . . ? C9 C14 C18 122.94(14) . . ? C13 C14 C9 117.05(15) . . ? C13 C14 C18 119.99(15) . . ? C10 C15 C17 109.46(15) . . ? C16 C15 C10 112.49(14) . . ? C16 C15 C17 111.98(19) . . ? C14 C18 C19 112.48(14) . . ? C14 C18 C20 110.11(14) . . ? C19 C18 C20 109.40(14) . . ? C22 C21 N2 117.97(13) . . ? C26 C21 C22 122.95(14) . . ? C26 C21 N2 118.70(13) . . ? C21 C22 C27 123.08(13) . . ? C23 C22 C21 117.07(14) . . ? C23 C22 C27 119.84(14) . . ? C24 C23 C22 121.29(15) . . ? C23 C24 C25 120.35(15) . . ? C24 C25 C26 121.29(15) . . ? C21 C26 C30 122.18(14) . . ? C25 C26 C21 116.99(14) . . ? C25 C26 C30 120.81(14) . . ? C22 C27 C28 110.66(13) . . ? C22 C27 C29 111.95(14) . . ? C29 C27 C28 109.87(14) . . ? C26 C30 C31 113.22(14) . . ? C26 C30 C32 111.61(13) . . ? C32 C30 C31 110.52(15) . . ? N3 C33 Ni2 129.09(11) . . ? N4 C33 N3 103.02(12) . . ? N4 C33 Ni2 127.78(11) . . ? C35 C34 N3 107.07(13) . . ? C34 C35 N4 106.61(13) . . ? C37 C36 C40 107.30(15) . . ? C37 C36 Ni2 69.84(9) . . ? C40 C36 Ni2 67.83(9) . . ? C36 C37 C38 108.23(14) . . ? C36 C37 Ni2 73.22(9) . . ? C38 C37 Ni2 67.42(8) . . ? C37 C38 Ni2 73.23(9) . . ? C39 C38 C37 108.40(15) . . ? C39 C38 Ni2 73.00(9) . . ? C38 C39 C40 107.01(15) . . ? C38 C39 Ni2 68.42(9) . . ? C40 C39 Ni2 70.10(9) . . ? C36 C40 Ni2 73.70(9) . . ? C39 C40 C36 108.71(15) . . ? C39 C40 Ni2 71.36(9) . . ? C42 C41 C46 122.77(14) . . ? C42 C41 N3 118.65(13) . . ? C46 C41 N3 118.38(14) . . ? C41 C42 C47 123.27(14) . . ? C43 C42 C41 117.37(15) . . ? C43 C42 C47 119.34(15) . . ? C44 C43 C42 121.10(17) . . ? C43 C44 C45 120.34(16) . . ? C44 C45 C46 121.25(17) . . ? C41 C46 C50 121.85(14) . . ? C45 C46 C41 117.12(16) . . ? C45 C46 C50 120.97(15) . . ? C42 C47 C48 112.41(14) . . ? C42 C47 C49 110.29(15) . . ? C48 C47 C49 109.84(15) . . ? C46 C50 C51 113.37(16) . . ? C46 C50 C52 110.94(14) . . ? C52 C50 C51 109.91(15) . . ? C54 C53 C58 122.75(14) . . ? C54 C53 N4 119.46(14) . . ? C58 C53 N4 117.76(14) . . ? C53 C54 C59 122.82(14) . . ? C55 C54 C53 117.00(15) . . ? C55 C54 C59 120.18(15) . . ? C56 C55 C54 121.53(17) . . ? C57 C56 C55 120.41(17) . . ? C56 C57 C58 120.99(17) . . ? C53 C58 C62 122.48(15) . . ? C57 C58 C53 117.29(16) . . ? C57 C58 C62 120.23(16) . . ? C54 C59 C61 111.19(14) . . ? C60 C59 C54 111.16(15) . . ? C60 C59 C61 110.01(16) . . ? C58 C62 C63 112.40(17) . . ? C58 C62 C64 111.13(15) . . ? C63 C62 C64 109.49(15) . . ? C1 N1 C2 111.80(12) . . ? C1 N1 C9 125.95(12) . . ? C2 N1 C9 122.23(12) . . ? C1 N2 C3 111.60(12) . . ? C1 N2 C21 128.60(12) . . ? C3 N2 C21 119.72(12) . . ? C33 N3 C34 111.41(12) . . ? C33 N3 C41 127.35(12) . . ? C34 N3 C41 121.12(12) . . ? C33 N4 C35 111.88(12) . . ? C33 N4 C53 126.12(12) . . ? C35 N4 C53 121.73(12) . . ? S2 S1 Ni1 114.63(2) . . ? S1 S2 Ni2 114.40(2) . . ? C1 Ni1 C4 128.99(7) . . ? C1 Ni1 C5 167.53(7) . . ? C1 Ni1 C6 143.56(7) . . ? C1 Ni1 C7 112.04(6) . . ? C1 Ni1 C8 104.50(6) . . ? C1 Ni1 S1 89.34(4) . . ? C4 Ni1 C6 64.27(7) . . ? C4 Ni1 C7 64.00(7) . . ? C4 Ni1 S1 126.56(5) . . ? C5 Ni1 C4 38.59(7) . . ? C5 Ni1 C6 39.20(7) . . ? C5 Ni1 C7 64.12(6) . . ? C5 Ni1 C8 64.77(6) . . ? C5 Ni1 S1 100.64(5) . . ? C6 Ni1 C7 36.90(7) . . ? C6 Ni1 S1 108.81(5) . . ? C8 Ni1 C4 38.47(7) . . ? C8 Ni1 C6 63.72(7) . . ? C8 Ni1 C7 38.52(7) . . ? C8 Ni1 S1 164.52(5) . . ? S1 Ni1 C7 141.50(5) . . ? C33 Ni2 C36 113.77(6) . . ? C33 Ni2 C37 145.57(6) . . ? C33 Ni2 C38 166.92(6) . . ? C33 Ni2 C39 128.36(6) . . ? C33 Ni2 C40 105.13(6) . . ? C33 Ni2 S2 88.33(4) . . ? C37 Ni2 C36 36.94(6) . . ? C37 Ni2 S2 108.51(5) . . ? C38 Ni2 C36 64.19(6) . . ? C38 Ni2 C37 39.36(6) . . ? C38 Ni2 C39 38.59(7) . . ? C38 Ni2 C40 64.80(6) . . ? C38 Ni2 S2 100.86(5) . . ? C39 Ni2 C36 64.06(7) . . ? C39 Ni2 C37 64.43(6) . . ? C39 Ni2 S2 127.08(5) . . ? C40 Ni2 C36 38.48(7) . . ? C40 Ni2 C37 63.78(6) . . ? C40 Ni2 C39 38.53(7) . . ? C40 Ni2 S2 164.98(5) . . ? S2 Ni2 C36 141.04(5) . . ? _database_code_depnum_ccdc_archive 'CCDC 995932' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6-Se _audit_creation_date 2013-12-04 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _shelxl_version_number 2013-4 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C64 H82 N4 Ni2 Se2, C6 H14' _chemical_formula_sum 'C70 H96 N4 Ni2 Se2' _chemical_formula_weight 1268.84 _chemical_melting_point ? _chemical_oxdiff_formula 'C64 H82 N4 Ni2 Se2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.5580(3) _cell_length_b 20.1611(2) _cell_length_c 16.7962(2) _cell_angle_alpha 90 _cell_angle_beta 96.1920(10) _cell_angle_gamma 90 _cell_volume 6584.28(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 18301 _cell_measurement_temperature 123.01(10) _cell_measurement_theta_max 73.4600 _cell_measurement_theta_min 3.1520 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.282 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour_lustre ? _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2672 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_unetI/netI 0.0302 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 32467 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.481 _diffrn_reflns_theta_min 3.158 _diffrn_ambient_temperature 123.01(10) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9918 _diffrn_measured_fraction_theta_max 0.9636 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0762822000 _diffrn_orient_matrix_UB_12 0.0415948000 _diffrn_orient_matrix_UB_13 0.0040683000 _diffrn_orient_matrix_UB_21 0.0395762000 _diffrn_orient_matrix_UB_22 0.0589568000 _diffrn_orient_matrix_UB_23 -0.0333559000 _diffrn_orient_matrix_UB_31 -0.0336252000 _diffrn_orient_matrix_UB_32 -0.0252191000 _diffrn_orient_matrix_UB_33 -0.0716979000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 10916 _reflns_number_total 12810 _reflns_odcompleteness_completeness 99.18 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.379 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 703 _refine_ls_number_reflns 12810 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0296 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+3.4382P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.0759 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.023) H3(0.022) H4(0.029) H5(0.029) H6(0.03) H7(0.029) H8(0.03) H11(0.027) H12(0.028) H13(0.026) H15(0.025) H16A(0.041) H16B(0.041) H16C(0.041) H17A(0.046) H17B(0.046) H17C(0.046) H18(0.027) H19A(0.045) H19B(0.045) H19C(0.045) H20A(0.052) H20B(0.052) H20C(0.052) H23(0.027) H24(0.031) H25(0.028) H27(0.029) H28A(0.055) H28B(0.055) H28C(0.055) H29A(0.05) H29B(0.05) H29C(0.05) H30(0.024) H31A(0.044) H31B(0.044) H31C(0.044) H32A(0.04) H32B(0.04) H32C(0.04) H34(0.028) H35(0.026) H36(0.028) H37(0.03) H38(0.027) H39(0.027) H40(0.028) H43(0.034) H44(0.038) H45(0.035) H47(0.034) H48A(0.072) H48B(0.072) H48C(0.072) H49A(0.066) H49B(0.066) H49C(0.066) H50(0.034) H51A(0.059) H51B(0.059) H51C(0.059) H52A(0.064) H52B(0.064) H52C(0.064) H55(0.036) H56(0.041) H57(0.038) H59(0.033) H60A(0.054) H60B(0.054) H60C(0.054) H61A(0.072) H61B(0.072) H61C(0.072) H62(0.041) H63A(0.079) H63B(0.079) H63C(0.079) H64A(0.072) H64B(0.072) H64C(0.072) H10A(0.11) H10B(0.11) H10C(0.11) H10D(0.072) H10E(0.072) H10F(0.071) H10G(0.071) H10H(0.077) H10I(0.077) H10J(0.11) H10K(0.11) H10L(0.157) H10M(0.157) H10N(0.157) Fixed X: H2(0.8183) H3(0.764) H4(0.9349) H5(0.8451) H6(0.8135) H7(0.891) H8(0.9579) H11(0.8716) H12(0.9882) H13(1.0347) H15(0.7467) H16A(0.7002) H16B(0.7706) H16C(0.7649) H17A(0.6925) H17B(0.751) H17C(0.7633) H18(0.9448) H19A(1.0631) H19B(1.0387) H19C(1.0784) H20A(1.0085) H20B(1.0194) H20C(0.9455) H23(0.8296) H24(0.7155) H25(0.6316) H27(0.8963) H28A(0.9854) H28B(0.9345) H28C(0.9252) H29A(0.963) H29B(0.8885) H29C(0.9089) H30(0.6561) H31A(0.5426) H31B(0.5939) H31C(0.5574) H32A(0.5732) H32B(0.5912) H32C(0.6458) H34(0.5598) H35(0.6816) H36(0.7196) H37(0.5905) H38(0.5604) H39(0.6705) H40(0.7699) H43(0.3825) H44(0.3485) H45(0.4228) H47(0.5477) H48A(0.4874) H48B(0.493) H48C(0.424) H49A(0.4851) H49B(0.4225) H49C(0.4915) H50(0.599) H51A(0.5842) H51B(0.5071) H51C(0.5659) H52A(0.5699) H52B(0.5417) H52C(0.4917) H55(0.8789) H56(0.9524) H57(0.9108) H59(0.6956) H60A(0.73) H60B(0.8075) H60C(0.7614) H61A(0.7085) H61B(0.7229) H61C(0.7844) H62(0.7362) H63A(0.8055) H63B(0.8255) H63C(0.8717) H64A(0.762) H64B(0.8242) H64C(0.7488) H10A(0.5983) H10B(0.6341) H10C(0.632) H10D(0.7045) H10E(0.7023) H10F(0.7647) H10G(0.7604) H10H(0.8331) H10I(0.8346) H10J(0.8896) H10K(0.8923) H10L(0.9987) H10M(0.9668) H10N(0.9642) Fixed Y: H2(-0.2749) H3(-0.2802) H4(-0.0187) H5(0.0684) H6(0.0848) H7(0.0137) H8(-0.0585) H11(-0.0731) H12(-0.0899) H13(-0.1487) H15(-0.1206) H16A(-0.0352) H16B(-0.0268) H16C(-0.0093) H17A(-0.153) H17B(-0.2031) H17C(-0.1502) H18(- 0.2037) H19A(-0.2019) H19B(-0.1307) H19C(-0.1752) H20A(-0.3008) H20B(-0.2783) H20C(-0.2963) H23(-0.1417) H24(-0.1463) H25(-0.1617) H27(-0.1448) H28A(- 0.1237) H28B(-0.1332) H28C(-0.0731) H29A(-0.2356) H29B(-0.2583) H29C(-0.2514) H30(-0.1787) H31A(-0.1432) H31B(-0.0883) H31C(-0.1345) H32A(-0.2611) H32B(- 0.2576) H32C(-0.284) H34(0.2589) H35(0.2475) H36(0.092) H37(0.1039) H38(0.2184) H39(0.2766) H40(0.2026) H43(0.135) H44(0.2363) H45(0.325) H47(0.0957) H48A(-0.0028) H48B(0.0388) H48C(0.0379) H49A(0.052) H49B(0.0974) H49C(0.1292) H50(0.3203) H51A(0.4078) H51B(0.3875) H51C(0.3399) H52A(0.4248) H52B(0.3686) H52C(0.4057) H55(0.0911) H56(0.1638) H57(0.2534) H59(0.094) H60A(- 0.0125) H60B(0.0082) H60C(0.0041) H61A(0.075) H61B(0.1497) H61C(0.1011) H62(0.2917) H63A(0.3645) H63B(0.2911) H63C(0.3329) H64A(0.3951) H64B(0.3631) H64C(0.3417) H10A(-0.0312) H10B(-0.1003) H10C(-0.0495) H10D(-0.0292) H10E(0.0216) H10F(-0.103) H10G(-0.0546) H10H(0.018) H10I(-0.0264) H10J(- 0.0645) H10K(-0.1075) H10L(-0.057) H10M(-0.0297) H10N(0.0133) Fixed Z: H2(-0.02) H3(0.1049) H4(-0.0184) H5(-0.0222) H6(0.1183) H7(0.2106) H8(0.1248) H11(-0.2213) H12(-0.1985) H13(-0.0881) H15(-0.0928) H16A(-0.1762) H16B(-0.2118) H16C(-0.1218) H17A(-0.2186) H17B(-0.1888) H17C(-0.2542) H18(0.0729) H19A(0.1154) H19B(0.0877) H19C(0.0315) H20A(0.0552) H20B(-0.0318) H20C(-0.0107) H23(0.3759) H24(0.3983) H25(0.2936) H27(0.1897) H28A(0.2912) H28B(0.3563) H28C(0.2969) H29A(0.2393) H29B(0.2067) H29C(0.2992) H30(0.0878) H31A(0.0947) H31B(0.1302) H31C(0.1877) H32A(0.1044) H32B(0.1976) H32C(0.1435) H34(0.3008) H35(0.3506) H36(-0.0425) H37(-0.0669) H38(-0.0289) H39(0.0238) H40(-0.0014) H43(0.0931) H44(0.0401) H45(0.0488) H47(0.1906) H48A(0.1595) H48B(0.0816) H48C(0.121) H49A(0.2902) H49B(0.2602) H49C(0.2983) H50(0.1297) H51A(0.0369) H51B(0.0153) H51C(-0.0058) H52A(0.1771) H52B(0.2293) H52C(0.1649) H55(0.3392) H56(0.2871) H57(0.2128) H59(0.304) H60A(0.3478) H60B(0.3503) H60C(0.2681) H61A(0.4432) H61B(0.4251) H61C(0.4487) H62(0.155) H63A(0.0914) H63B(0.0738) H63C(0.1373) H64A(0.2162) H64B(0.2694) H64C(0.2806) H10A(0.5734) H10B(0.5666) H10C(0.4957) H10D(0.6463) H10E(0.5757) H10F(0.5764) H10G(0.5034) H10H(0.5739) H10I(0.6504) H10J(0.5114) H10K(0.5892) H10L(0.5822) H10M(0.6574) H10N(0.5794) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.81343(9) -0.13517(9) 0.06648(11) 0.0150(4) Uani 1 1 d . . . . . C2 C 0.81199(10) -0.23980(9) 0.01447(12) 0.0192(4) Uani 1 1 d . . . . . H2 H 0.8183 -0.2749 -0.0200 0.023 Uiso 1 1 calc R U . . . C3 C 0.78218(10) -0.24261(9) 0.08291(11) 0.0187(4) Uani 1 1 d . . . . . H3 H 0.7640 -0.2802 0.1049 0.022 Uiso 1 1 calc R U . . . C4 C 0.91420(10) -0.00285(10) 0.02518(12) 0.0242(4) Uani 1 1 d . . . . . H4 H 0.9349 -0.0187 -0.0184 0.029 Uiso 1 1 calc R U . . . C5 C 0.86425(11) 0.04597(10) 0.02323(13) 0.0245(4) Uani 1 1 d . . . . . H5 H 0.8451 0.0684 -0.0222 0.029 Uiso 1 1 calc R U . . . C6 C 0.84699(11) 0.05593(10) 0.10328(13) 0.0249(4) Uani 1 1 d . . . . . H6 H 0.8135 0.0848 0.1183 0.030 Uiso 1 1 calc R U . . . C7 C 0.88910(10) 0.01489(10) 0.15501(13) 0.0242(4) Uani 1 1 d . . . . . H7 H 0.8910 0.0137 0.2106 0.029 Uiso 1 1 calc R U . . . C8 C 0.92818(10) -0.02442(10) 0.10670(13) 0.0247(4) Uani 1 1 d . . . . . H8 H 0.9579 -0.0585 0.1248 0.030 Uiso 1 1 calc R U . . . C9 C 0.87496(9) -0.15228(9) -0.05419(11) 0.0160(4) Uani 1 1 d . . . . . C10 C 0.84525(10) -0.11901(10) -0.12212(11) 0.0184(4) Uani 1 1 d . . . . . C11 C 0.88960(10) -0.09597(10) -0.17566(12) 0.0223(4) Uani 1 1 d . . . . . H11 H 0.8716 -0.0731 -0.2213 0.027 Uiso 1 1 calc R U . . . C12 C 0.95965(10) -0.10635(10) -0.16236(12) 0.0233(4) Uani 1 1 d . . . . . H12 H 0.9882 -0.0899 -0.1985 0.028 Uiso 1 1 calc R U . . . C13 C 0.98759(10) -0.14108(10) -0.09575(12) 0.0218(4) Uani 1 1 d . . . . . H13 H 1.0347 -0.1487 -0.0881 0.026 Uiso 1 1 calc R U . . . C14 C 0.94566(10) -0.16494(10) -0.03967(11) 0.0189(4) Uani 1 1 d . . . . . C15 C 0.76843(10) -0.10984(10) -0.14117(11) 0.0205(4) Uani 1 1 d . . . . . H15 H 0.7467 -0.1206 -0.0928 0.025 Uiso 1 1 calc R U . . . C16 C 0.74923(11) -0.03867(11) -0.16492(13) 0.0273(5) Uani 1 1 d . . . . . H16A H 0.7002 -0.0352 -0.1762 0.041 Uiso 1 1 calc R U . . . H16B H 0.7706 -0.0268 -0.2118 0.041 Uiso 1 1 calc R U . . . H16C H 0.7649 -0.0093 -0.1218 0.041 Uiso 1 1 calc R U . . . C17 C 0.74129(11) -0.15857(11) -0.20677(14) 0.0305(5) Uani 1 1 d . . . . . H17A H 0.6925 -0.1530 -0.2186 0.046 Uiso 1 1 calc R U . . . H17B H 0.7510 -0.2031 -0.1888 0.046 Uiso 1 1 calc R U . . . H17C H 0.7633 -0.1502 -0.2542 0.046 Uiso 1 1 calc R U . . . C18 C 0.97731(10) -0.20414(10) 0.03238(12) 0.0226(4) Uani 1 1 d . . . . . H18 H 0.9448 -0.2037 0.0729 0.027 Uiso 1 1 calc R U . . . C19 C 1.04576(11) -0.17525(11) 0.07030(13) 0.0299(5) Uani 1 1 d . . . . . H19A H 1.0631 -0.2019 0.1154 0.045 Uiso 1 1 calc R U . . . H19B H 1.0387 -0.1307 0.0877 0.045 Uiso 1 1 calc R U . . . H19C H 1.0784 -0.1752 0.0315 0.045 Uiso 1 1 calc R U . . . C20 C 0.98873(12) -0.27667(11) 0.00910(15) 0.0348(5) Uani 1 1 d . . . . . H20A H 1.0085 -0.3008 0.0552 0.052 Uiso 1 1 calc R U . . . H20B H 1.0194 -0.2783 -0.0318 0.052 Uiso 1 1 calc R U . . . H20C H 0.9455 -0.2963 -0.0107 0.052 Uiso 1 1 calc R U . . . C21 C 0.76365(10) -0.16558(9) 0.19359(11) 0.0161(4) Uani 1 1 d . . . . . C22 C 0.81603(10) -0.15679(9) 0.25649(11) 0.0189(4) Uani 1 1 d . . . . . C23 C 0.79618(11) -0.14876(10) 0.33305(12) 0.0227(4) Uani 1 1 d . . . . . H23 H 0.8296 -0.1417 0.3759 0.027 Uiso 1 1 calc R U . . . C24 C 0.72761(11) -0.15111(10) 0.34661(12) 0.0255(5) Uani 1 1 d . . . . . H24 H 0.7155 -0.1463 0.3983 0.031 Uiso 1 1 calc R U . . . C25 C 0.67748(11) -0.16047(10) 0.28371(12) 0.0231(4) Uani 1 1 d . . . . . H25 H 0.6316 -0.1617 0.2936 0.028 Uiso 1 1 calc R U . . . C26 C 0.69371(10) -0.16815(9) 0.20543(11) 0.0183(4) Uani 1 1 d . . . . . C27 C 0.89165(10) -0.16108(10) 0.24376(12) 0.0239(4) Uani 1 1 d . . . . . H27 H 0.8963 -0.1448 0.1897 0.029 Uiso 1 1 calc R U . . . C28 C 0.93855(12) -0.11881(13) 0.30250(14) 0.0367(6) Uani 1 1 d . . . . . H28A H 0.9854 -0.1237 0.2912 0.055 Uiso 1 1 calc R U . . . H28B H 0.9345 -0.1332 0.3563 0.055 Uiso 1 1 calc R U . . . H28C H 0.9252 -0.0731 0.2969 0.055 Uiso 1 1 calc R U . . . C29 C 0.91521(11) -0.23330(12) 0.24760(15) 0.0332(5) Uani 1 1 d . . . . . H29A H 0.9630 -0.2356 0.2393 0.050 Uiso 1 1 calc R U . . . H29B H 0.8885 -0.2583 0.2067 0.050 Uiso 1 1 calc R U . . . H29C H 0.9089 -0.2514 0.2992 0.050 Uiso 1 1 calc R U . . . C30 C 0.63666(10) -0.18193(10) 0.13902(12) 0.0199(4) Uani 1 1 d . . . . . H30 H 0.6561 -0.1787 0.0878 0.024 Uiso 1 1 calc R U . . . C31 C 0.57706(10) -0.13237(11) 0.13781(14) 0.0291(5) Uani 1 1 d . . . . . H31A H 0.5426 -0.1432 0.0947 0.044 Uiso 1 1 calc R U . . . H31B H 0.5939 -0.0883 0.1302 0.044 Uiso 1 1 calc R U . . . H31C H 0.5574 -0.1345 0.1877 0.044 Uiso 1 1 calc R U . . . C32 C 0.60913(11) -0.25282(11) 0.14687(13) 0.0270(5) Uani 1 1 d . . . . . H32A H 0.5732 -0.2611 0.1044 0.040 Uiso 1 1 calc R U . . . H32B H 0.5912 -0.2576 0.1976 0.040 Uiso 1 1 calc R U . . . H32C H 0.6458 -0.2840 0.1435 0.040 Uiso 1 1 calc R U . . . C33 C 0.64714(9) 0.19011(9) 0.17495(11) 0.0155(4) Uani 1 1 d . . . . . C34 C 0.59416(10) 0.24025(10) 0.27362(12) 0.0230(4) Uani 1 1 d . . . . . H34 H 0.5598 0.2589 0.3008 0.028 Uiso 1 1 calc R U . . . C35 C 0.66078(10) 0.23402(10) 0.30088(11) 0.0218(4) Uani 1 1 d . . . . . H35 H 0.6816 0.2475 0.3506 0.026 Uiso 1 1 calc R U . . . C36 C 0.69489(11) 0.13046(11) -0.03497(11) 0.0234(4) Uani 1 1 d . . . . . H36 H 0.7196 0.0920 -0.0425 0.028 Uiso 1 1 calc R U . . . C37 C 0.62136(11) 0.13677(11) -0.04758(12) 0.0246(4) Uani 1 1 d . . . . . H37 H 0.5905 0.1039 -0.0669 0.030 Uiso 1 1 calc R U . . . C38 C 0.60450(11) 0.20062(10) -0.02588(11) 0.0227(4) Uani 1 1 d . . . . . H38 H 0.5604 0.2184 -0.0289 0.027 Uiso 1 1 calc R U . . . C39 C 0.66720(11) 0.23422(10) 0.00199(11) 0.0228(4) Uani 1 1 d . . . . . H39 H 0.6705 0.2766 0.0238 0.027 Uiso 1 1 calc R U . . . C40 C 0.72346(11) 0.19188(11) -0.00934(11) 0.0233(4) Uani 1 1 d . . . . . H40 H 0.7699 0.2026 -0.0014 0.028 Uiso 1 1 calc R U . . . C41 C 0.52113(9) 0.21780(10) 0.14786(11) 0.0186(4) Uani 1 1 d . . . . . C42 C 0.47744(10) 0.16267(10) 0.14243(12) 0.0221(4) Uani 1 1 d . . . . . C43 C 0.41255(11) 0.17085(12) 0.09948(13) 0.0285(5) Uani 1 1 d . . . . . H43 H 0.3825 0.1350 0.0931 0.034 Uiso 1 1 calc R U . . . C44 C 0.39253(11) 0.23139(12) 0.06644(13) 0.0320(5) Uani 1 1 d . . . . . H44 H 0.3485 0.2363 0.0401 0.038 Uiso 1 1 calc R U . . . C45 C 0.43702(11) 0.28469(12) 0.07193(12) 0.0290(5) Uani 1 1 d . . . . . H45 H 0.4228 0.3250 0.0488 0.035 Uiso 1 1 calc R U . . . C46 C 0.50325(10) 0.27894(10) 0.11187(11) 0.0218(4) Uani 1 1 d . . . . . C47 C 0.49737(11) 0.09724(11) 0.18261(14) 0.0282(5) Uani 1 1 d . . . . . H47 H 0.5477 0.0957 0.1906 0.034 Uiso 1 1 calc R U . . . C48 C 0.47319(14) 0.03717(12) 0.13140(19) 0.0482(7) Uani 1 1 d . . . . . H48A H 0.4874 -0.0028 0.1595 0.072 Uiso 1 1 calc R U . . . H48B H 0.4930 0.0388 0.0816 0.072 Uiso 1 1 calc R U . . . H48C H 0.4240 0.0379 0.1210 0.072 Uiso 1 1 calc R U . . . C49 C 0.47173(14) 0.09362(13) 0.26558(16) 0.0440(7) Uani 1 1 d . . . . . H49A H 0.4851 0.0520 0.2902 0.066 Uiso 1 1 calc R U . . . H49B H 0.4225 0.0974 0.2602 0.066 Uiso 1 1 calc R U . . . H49C H 0.4915 0.1292 0.2983 0.066 Uiso 1 1 calc R U . . . C50 C 0.55254(12) 0.33746(11) 0.11452(13) 0.0282(5) Uani 1 1 d . . . . . H50 H 0.5990 0.3203 0.1297 0.034 Uiso 1 1 calc R U . . . C51 C 0.55243(13) 0.37132(12) 0.03253(15) 0.0392(6) Uani 1 1 d . . . . . H51A H 0.5842 0.4078 0.0369 0.059 Uiso 1 1 calc R U . . . H51B H 0.5071 0.3875 0.0153 0.059 Uiso 1 1 calc R U . . . H51C H 0.5659 0.3399 -0.0058 0.059 Uiso 1 1 calc R U . . . C52 C 0.53756(14) 0.38893(12) 0.17729(16) 0.0425(6) Uani 1 1 d . . . . . H52A H 0.5699 0.4248 0.1771 0.064 Uiso 1 1 calc R U . . . H52B H 0.5417 0.3686 0.2293 0.064 Uiso 1 1 calc R U . . . H52C H 0.4917 0.4057 0.1649 0.064 Uiso 1 1 calc R U . . . C53 C 0.76574(10) 0.19051(10) 0.25026(11) 0.0179(4) Uani 1 1 d . . . . . C54 C 0.78979(10) 0.13523(10) 0.29517(11) 0.0214(4) Uani 1 1 d . . . . . C55 C 0.86102(11) 0.12688(11) 0.30877(13) 0.0302(5) Uani 1 1 d . . . . . H55 H 0.8789 0.0911 0.3392 0.036 Uiso 1 1 calc R U . . . C56 C 0.90517(11) 0.17072(12) 0.27797(14) 0.0338(5) Uani 1 1 d . . . . . H56 H 0.9524 0.1638 0.2871 0.041 Uiso 1 1 calc R U . . . C57 C 0.88018(11) 0.22463(12) 0.23383(14) 0.0319(5) Uani 1 1 d . . . . . H57 H 0.9108 0.2534 0.2128 0.038 Uiso 1 1 calc R U . . . C58 C 0.80984(11) 0.23684(11) 0.22002(12) 0.0238(4) Uani 1 1 d . . . . . C59 C 0.74190(12) 0.08805(10) 0.33188(12) 0.0278(5) Uani 1 1 d . . . . . H59 H 0.6956 0.0940 0.3040 0.033 Uiso 1 1 calc R U . . . C60 C 0.76207(14) 0.01519(11) 0.32374(14) 0.0359(5) Uani 1 1 d . . . . . H60A H 0.7300 -0.0125 0.3478 0.054 Uiso 1 1 calc R U . . . H60B H 0.8075 0.0082 0.3503 0.054 Uiso 1 1 calc R U . . . H60C H 0.7614 0.0041 0.2681 0.054 Uiso 1 1 calc R U . . . C61 C 0.73917(16) 0.10505(13) 0.42049(14) 0.0478(7) Uani 1 1 d . . . . . H61A H 0.7085 0.0750 0.4432 0.072 Uiso 1 1 calc R U . . . H61B H 0.7229 0.1497 0.4251 0.072 Uiso 1 1 calc R U . . . H61C H 0.7844 0.1011 0.4487 0.072 Uiso 1 1 calc R U . . . C62 C 0.78300(12) 0.30022(12) 0.17987(14) 0.0339(5) Uani 1 1 d . . . . . H62 H 0.7362 0.2917 0.1550 0.041 Uiso 1 1 calc R U . . . C63 C 0.82533(16) 0.32440(15) 0.11454(16) 0.0527(8) Uani 1 1 d . . . . . H63A H 0.8055 0.3645 0.0914 0.079 Uiso 1 1 calc R U . . . H63B H 0.8255 0.2911 0.0738 0.079 Uiso 1 1 calc R U . . . H63C H 0.8717 0.3329 0.1373 0.079 Uiso 1 1 calc R U . . . C64 C 0.77913(15) 0.35520(13) 0.24235(17) 0.0480(7) Uani 1 1 d . . . . . H64A H 0.7620 0.3951 0.2162 0.072 Uiso 1 1 calc R U . . . H64B H 0.8242 0.3631 0.2694 0.072 Uiso 1 1 calc R U . . . H64C H 0.7488 0.3417 0.2806 0.072 Uiso 1 1 calc R U . . . C100 C 0.6357(2) -0.05410(17) 0.5529(2) 0.0730(10) Uani 1 1 d . . . . . H10A H 0.5983 -0.0312 0.5734 0.110 Uiso 1 1 calc R U . . . H10B H 0.6341 -0.1003 0.5666 0.110 Uiso 1 1 calc R U . . . H10C H 0.6320 -0.0495 0.4957 0.110 Uiso 1 1 calc R U . . . C101 C 0.70200(18) -0.02528(16) 0.58854(17) 0.0597(8) Uani 1 1 d . . . . . H10D H 0.7045 -0.0292 0.6463 0.072 Uiso 1 1 calc R U . . . H10E H 0.7023 0.0216 0.5757 0.072 Uiso 1 1 calc R U . . . C102 C 0.76447(18) -0.05652(15) 0.56139(19) 0.0593(8) Uani 1 1 d . . . . . H10F H 0.7647 -0.1030 0.5764 0.071 Uiso 1 1 calc R U . . . H10G H 0.7604 -0.0546 0.5034 0.071 Uiso 1 1 calc R U . . . C103 C 0.83175(19) -0.02754(16) 0.59241(19) 0.0644(9) Uani 1 1 d . . . . . H10H H 0.8331 0.0180 0.5739 0.077 Uiso 1 1 calc R U . . . H10I H 0.8346 -0.0264 0.6504 0.077 Uiso 1 1 calc R U . . . C104 C 0.8929(2) -0.0623(2) 0.5694(3) 0.0918(13) Uani 1 1 d . . . . . H10J H 0.8896 -0.0645 0.5114 0.110 Uiso 1 1 calc R U . . . H10K H 0.8923 -0.1075 0.5892 0.110 Uiso 1 1 calc R U . . . C105 C 0.9621(2) -0.0310(2) 0.6000(3) 0.1043(15) Uani 1 1 d . . . . . H10L H 0.9987 -0.0570 0.5822 0.157 Uiso 1 1 calc R U . . . H10M H 0.9668 -0.0297 0.6574 0.157 Uiso 1 1 calc R U . . . H10N H 0.9642 0.0133 0.5794 0.157 Uiso 1 1 calc R U . . . N1 N 0.83154(8) -0.17431(8) 0.00536(9) 0.0156(3) Uani 1 1 d . . . . . N2 N 0.78359(8) -0.17914(8) 0.11443(9) 0.0148(3) Uani 1 1 d . . . . . N3 N 0.58625(8) 0.21358(8) 0.19703(9) 0.0171(3) Uani 1 1 d . . . . . N4 N 0.69264(8) 0.20363(8) 0.24068(9) 0.0167(3) Uani 1 1 d . . . . . Ni1 Ni 0.82236(2) -0.04301(2) 0.07487(2) 0.01536(7) Uani 1 1 d . . . . . Ni2 Ni 0.66204(2) 0.15101(2) 0.07678(2) 0.01535(7) Uani 1 1 d . . . . . Se1 Se 0.70512(2) -0.03244(2) 0.04625(2) 0.01823(5) Uani 1 1 d . . . . . Se2 Se 0.66518(2) 0.04650(2) 0.13193(2) 0.02007(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0104(9) 0.0204(9) 0.0145(9) 0.0010(7) 0.0020(7) -0.0006(7) C2 0.0189(10) 0.0166(9) 0.0226(10) -0.0035(7) 0.0051(8) -0.0016(7) C3 0.0171(10) 0.0165(9) 0.0231(10) -0.0002(7) 0.0049(8) -0.0025(7) C4 0.0189(10) 0.0261(11) 0.0297(11) -0.0050(8) 0.0119(9) -0.0089(8) C5 0.0216(11) 0.0206(10) 0.0313(11) 0.0054(8) 0.0029(9) -0.0085(8) C6 0.0192(10) 0.0186(10) 0.0381(12) -0.0079(9) 0.0084(9) -0.0042(8) C7 0.0222(11) 0.0258(11) 0.0247(11) -0.0065(8) 0.0036(8) -0.0094(8) C8 0.0143(10) 0.0217(10) 0.0376(12) -0.0012(9) 0.0007(9) -0.0035(8) C9 0.0151(9) 0.0186(9) 0.0152(9) -0.0028(7) 0.0064(7) -0.0034(7) C10 0.0188(10) 0.0201(10) 0.0168(9) -0.0034(7) 0.0046(8) -0.0027(8) C11 0.0230(11) 0.0277(11) 0.0169(10) 0.0004(8) 0.0046(8) -0.0030(8) C12 0.0235(11) 0.0279(11) 0.0203(10) -0.0032(8) 0.0104(8) -0.0085(8) C13 0.0152(10) 0.0273(11) 0.0240(10) -0.0075(8) 0.0069(8) -0.0042(8) C14 0.0170(10) 0.0207(10) 0.0195(10) -0.0041(8) 0.0037(8) -0.0019(8) C15 0.0165(10) 0.0280(11) 0.0173(9) -0.0010(8) 0.0030(7) 0.0004(8) C16 0.0268(12) 0.0293(11) 0.0263(11) 0.0011(9) 0.0052(9) 0.0055(9) C17 0.0222(11) 0.0327(12) 0.0357(13) -0.0088(10) -0.0013(9) -0.0005(9) C18 0.0169(10) 0.0284(11) 0.0228(10) -0.0004(8) 0.0036(8) -0.0007(8) C19 0.0250(12) 0.0341(12) 0.0295(12) 0.0012(9) -0.0025(9) -0.0009(9) C20 0.0335(13) 0.0265(12) 0.0429(14) 0.0002(10) -0.0021(11) 0.0018(10) C21 0.0186(10) 0.0154(9) 0.0151(9) 0.0020(7) 0.0051(7) 0.0001(7) C22 0.0210(10) 0.0157(9) 0.0198(10) 0.0039(7) 0.0012(8) -0.0017(7) C23 0.0306(11) 0.0200(10) 0.0168(10) 0.0013(8) -0.0007(8) -0.0031(8) C24 0.0383(13) 0.0238(10) 0.0159(10) 0.0011(8) 0.0104(9) -0.0002(9) C25 0.0240(11) 0.0234(10) 0.0237(11) 0.0021(8) 0.0113(8) 0.0001(8) C26 0.0177(10) 0.0179(9) 0.0201(10) 0.0021(7) 0.0055(8) -0.0006(7) C27 0.0176(10) 0.0298(11) 0.0232(10) 0.0064(8) -0.0022(8) -0.0031(8) C28 0.0267(12) 0.0439(14) 0.0369(13) 0.0061(11) -0.0081(10) -0.0100(10) C29 0.0217(11) 0.0389(13) 0.0387(13) 0.0046(10) 0.0011(10) 0.0057(10) C30 0.0140(9) 0.0255(10) 0.0206(10) 0.0020(8) 0.0041(8) -0.0017(8) C31 0.0158(10) 0.0333(12) 0.0391(13) 0.0056(10) 0.0074(9) 0.0018(9) C32 0.0225(11) 0.0290(11) 0.0295(12) 0.0027(9) 0.0029(9) -0.0058(9) C33 0.0139(9) 0.0165(9) 0.0164(9) 0.0021(7) 0.0028(7) 0.0002(7) C34 0.0224(11) 0.0292(11) 0.0183(10) -0.0061(8) 0.0060(8) 0.0032(8) C35 0.0248(11) 0.0266(10) 0.0143(9) -0.0056(8) 0.0033(8) 0.0023(8) C36 0.0286(11) 0.0281(11) 0.0147(9) -0.0002(8) 0.0082(8) 0.0062(9) C37 0.0276(11) 0.0303(11) 0.0159(10) -0.0035(8) 0.0019(8) -0.0026(9) C38 0.0222(10) 0.0306(11) 0.0152(9) 0.0044(8) 0.0015(8) 0.0050(8) C39 0.0327(12) 0.0217(10) 0.0146(9) 0.0033(8) 0.0057(8) 0.0004(8) C40 0.0213(10) 0.0327(11) 0.0170(10) 0.0063(8) 0.0073(8) -0.0002(9) C41 0.0131(9) 0.0260(10) 0.0170(9) -0.0043(8) 0.0034(7) 0.0043(8) C42 0.0162(10) 0.0281(11) 0.0233(10) -0.0062(8) 0.0075(8) 0.0012(8) C43 0.0161(10) 0.0374(12) 0.0323(12) -0.0108(10) 0.0039(9) -0.0009(9) C44 0.0190(11) 0.0519(15) 0.0246(11) -0.0079(10) 0.0001(9) 0.0090(10) C45 0.0266(12) 0.0385(13) 0.0223(11) 0.0018(9) 0.0042(9) 0.0139(10) C46 0.0207(10) 0.0282(11) 0.0177(10) -0.0003(8) 0.0073(8) 0.0061(8) C47 0.0174(10) 0.0249(11) 0.0435(13) -0.0026(9) 0.0090(9) -0.0001(8) C48 0.0330(14) 0.0302(13) 0.082(2) -0.0169(13) 0.0075(14) -0.0028(11) C49 0.0446(15) 0.0367(14) 0.0543(16) 0.0164(12) 0.0220(13) 0.0120(12) C50 0.0287(12) 0.0249(11) 0.0328(12) 0.0028(9) 0.0115(9) 0.0053(9) C51 0.0431(15) 0.0337(13) 0.0438(15) 0.0120(11) 0.0183(12) 0.0094(11) C52 0.0500(16) 0.0325(13) 0.0485(15) -0.0068(11) 0.0216(13) -0.0033(11) C53 0.0155(9) 0.0234(10) 0.0142(9) -0.0049(7) -0.0006(7) 0.0013(8) C54 0.0243(11) 0.0239(10) 0.0150(9) -0.0059(8) -0.0017(8) 0.0052(8) C55 0.0291(12) 0.0326(12) 0.0266(11) -0.0093(9) -0.0076(9) 0.0127(10) C56 0.0184(11) 0.0443(14) 0.0374(13) -0.0182(11) -0.0038(9) 0.0040(10) C57 0.0209(11) 0.0439(14) 0.0310(12) -0.0089(10) 0.0033(9) -0.0077(10) C58 0.0215(11) 0.0306(11) 0.0192(10) -0.0050(8) 0.0011(8) -0.0049(9) C59 0.0375(13) 0.0237(11) 0.0228(11) 0.0043(8) 0.0065(9) 0.0060(9) C60 0.0514(16) 0.0245(12) 0.0312(13) 0.0048(9) 0.0014(11) 0.0068(11) C61 0.080(2) 0.0404(15) 0.0255(13) 0.0063(11) 0.0183(13) 0.0133(14) C62 0.0297(12) 0.0360(13) 0.0338(13) 0.0093(10) -0.0057(10) -0.0128(10) C63 0.0642(19) 0.0560(18) 0.0362(15) 0.0111(13) -0.0023(13) -0.0302(15) C64 0.0589(18) 0.0284(13) 0.0560(17) 0.0068(12) 0.0040(14) 0.0013(12) C100 0.096(3) 0.053(2) 0.070(2) -0.0028(17) 0.007(2) -0.0223(19) C101 0.086(2) 0.0539(18) 0.0366(16) 0.0041(13) -0.0043(15) -0.0077(17) C102 0.087(3) 0.0363(15) 0.0526(19) -0.0040(13) 0.0003(17) 0.0015(15) C103 0.095(3) 0.0505(18) 0.0434(17) -0.0004(14) -0.0141(17) 0.0097(18) C104 0.094(3) 0.070(3) 0.108(3) -0.022(2) -0.005(3) 0.020(2) C105 0.098(4) 0.098(3) 0.110(4) 0.005(3) -0.023(3) 0.007(3) N1 0.0140(8) 0.0181(8) 0.0151(8) -0.0007(6) 0.0039(6) -0.0021(6) N2 0.0124(8) 0.0175(8) 0.0153(8) -0.0004(6) 0.0042(6) -0.0017(6) N3 0.0150(8) 0.0213(8) 0.0152(8) -0.0020(6) 0.0024(6) 0.0010(6) N4 0.0153(8) 0.0202(8) 0.0144(8) -0.0007(6) 0.0012(6) 0.0018(6) Ni1 0.01205(16) 0.01566(16) 0.01895(17) -0.00119(12) 0.00430(12) -0.00124(12) Ni2 0.01533(16) 0.01813(16) 0.01303(16) -0.00013(12) 0.00358(12) 0.00135(12) Se1 0.01343(10) 0.01842(10) 0.02313(11) -0.00341(8) 0.00330(8) 0.00016(8) Se2 0.02236(11) 0.01907(11) 0.02052(11) 0.00167(8) 0.01026(8) 0.00335(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.371(2) . ? C1 N2 1.370(2) . ? C1 Ni1 1.8701(19) . ? C2 C3 1.345(3) . ? C2 N1 1.388(2) . ? C3 N2 1.384(2) . ? C4 C5 1.385(3) . ? C4 C8 1.435(3) . ? C4 Ni1 2.2140(19) . ? C5 C6 1.435(3) . ? C5 Ni1 2.1896(19) . ? C6 C7 1.401(3) . ? C6 Ni1 2.095(2) . ? C7 C8 1.416(3) . ? C7 Ni1 2.121(2) . ? C8 Ni1 2.115(2) . ? C9 C10 1.395(3) . ? C9 C14 1.401(3) . ? C9 N1 1.450(2) . ? C10 C11 1.395(3) . ? C10 C15 1.513(3) . ? C11 C12 1.380(3) . ? C12 C13 1.382(3) . ? C13 C14 1.399(3) . ? C14 C18 1.520(3) . ? C15 C16 1.525(3) . ? C15 C17 1.528(3) . ? C18 C19 1.534(3) . ? C18 C20 1.536(3) . ? C21 C22 1.401(3) . ? C21 C26 1.404(3) . ? C21 N2 1.451(2) . ? C22 C23 1.392(3) . ? C22 C27 1.519(3) . ? C23 C24 1.385(3) . ? C24 C25 1.375(3) . ? C25 C26 1.394(3) . ? C26 C30 1.516(3) . ? C27 C28 1.532(3) . ? C27 C29 1.526(3) . ? C30 C31 1.534(3) . ? C30 C32 1.538(3) . ? C33 N3 1.369(2) . ? C33 N4 1.369(2) . ? C33 Ni2 1.8784(18) . ? C34 C35 1.340(3) . ? C34 N3 1.387(2) . ? C35 N4 1.386(2) . ? C36 C37 1.437(3) . ? C36 C40 1.407(3) . ? C36 Ni2 2.0900(18) . ? C37 C38 1.387(3) . ? C37 Ni2 2.173(2) . ? C38 C39 1.435(3) . ? C38 Ni2 2.196(2) . ? C39 C40 1.421(3) . ? C39 Ni2 2.1048(19) . ? C40 Ni2 2.1422(19) . ? C41 C42 1.399(3) . ? C41 C46 1.401(3) . ? C41 N3 1.444(2) . ? C42 C43 1.400(3) . ? C42 C47 1.514(3) . ? C43 C44 1.380(3) . ? C44 C45 1.379(3) . ? C45 C46 1.398(3) . ? C46 C50 1.521(3) . ? C47 C48 1.530(3) . ? C47 C49 1.533(3) . ? C50 C51 1.537(3) . ? C50 C52 1.530(3) . ? C53 C54 1.398(3) . ? C53 C58 1.403(3) . ? C53 N4 1.446(2) . ? C54 C55 1.397(3) . ? C54 C59 1.512(3) . ? C55 C56 1.375(3) . ? C56 C57 1.375(3) . ? C57 C58 1.392(3) . ? C58 C62 1.512(3) . ? C59 C60 1.531(3) . ? C59 C61 1.534(3) . ? C62 C63 1.524(3) . ? C62 C64 1.534(4) . ? C100 C101 1.486(5) . ? C101 C102 1.489(4) . ? C102 C103 1.482(5) . ? C103 C104 1.474(5) . ? C104 C105 1.531(6) . ? Ni1 Se1 2.3013(4) . ? Ni2 Se2 2.2998(4) . ? Se1 Se2 2.3361(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 126.77(13) . . ? N2 C1 N1 103.21(15) . . ? N2 C1 Ni1 129.86(13) . . ? C3 C2 N1 106.50(16) . . ? C2 C3 N2 107.19(16) . . ? C5 C4 C8 107.42(18) . . ? C5 C4 Ni1 70.72(11) . . ? C8 C4 Ni1 66.94(11) . . ? C4 C5 C6 108.30(19) . . ? C4 C5 Ni1 72.63(11) . . ? C6 C5 Ni1 66.91(11) . . ? C5 C6 Ni1 74.03(11) . . ? C7 C6 C5 108.44(18) . . ? C7 C6 Ni1 71.60(12) . . ? C6 C7 C8 107.02(19) . . ? C6 C7 Ni1 69.58(12) . . ? C8 C7 Ni1 70.22(11) . . ? C4 C8 Ni1 74.44(12) . . ? C7 C8 C4 108.55(19) . . ? C7 C8 Ni1 70.73(11) . . ? C10 C9 C14 123.09(16) . . ? C10 C9 N1 119.23(16) . . ? C14 C9 N1 117.68(16) . . ? C9 C10 C15 123.23(16) . . ? C11 C10 C9 117.03(18) . . ? C11 C10 C15 119.69(18) . . ? C12 C11 C10 121.38(19) . . ? C11 C12 C13 120.45(18) . . ? C12 C13 C14 120.67(19) . . ? C9 C14 C18 122.86(16) . . ? C13 C14 C9 117.34(18) . . ? C13 C14 C18 119.79(17) . . ? C10 C15 C16 112.40(17) . . ? C10 C15 C17 109.49(16) . . ? C16 C15 C17 111.08(17) . . ? C14 C18 C19 113.28(17) . . ? C14 C18 C20 110.49(17) . . ? C19 C18 C20 108.83(18) . . ? C22 C21 C26 122.83(17) . . ? C22 C21 N2 117.88(16) . . ? C26 C21 N2 119.00(17) . . ? C21 C22 C27 122.02(17) . . ? C23 C22 C21 117.19(18) . . ? C23 C22 C27 120.62(18) . . ? C24 C23 C22 121.28(19) . . ? C25 C24 C23 120.09(18) . . ? C24 C25 C26 121.60(19) . . ? C21 C26 C30 123.61(16) . . ? C25 C26 C21 116.99(18) . . ? C25 C26 C30 119.33(17) . . ? C22 C27 C28 113.71(18) . . ? C22 C27 C29 110.01(17) . . ? C29 C27 C28 110.27(18) . . ? C26 C30 C31 112.86(17) . . ? C26 C30 C32 110.12(16) . . ? C31 C30 C32 109.50(16) . . ? N3 C33 Ni2 127.19(14) . . ? N4 C33 N3 102.79(15) . . ? N4 C33 Ni2 130.00(13) . . ? C35 C34 N3 106.72(16) . . ? C34 C35 N4 106.81(17) . . ? C37 C36 Ni2 73.44(11) . . ? C40 C36 C37 108.99(18) . . ? C40 C36 Ni2 72.60(11) . . ? C36 C37 Ni2 67.23(11) . . ? C38 C37 C36 107.82(19) . . ? C38 C37 Ni2 72.39(12) . . ? C37 C38 C39 107.75(18) . . ? C37 C38 Ni2 70.58(12) . . ? C39 C38 Ni2 67.12(11) . . ? C38 C39 Ni2 73.97(11) . . ? C40 C39 C38 108.63(18) . . ? C40 C39 Ni2 71.87(11) . . ? C36 C40 C39 106.39(18) . . ? C36 C40 Ni2 68.59(11) . . ? C39 C40 Ni2 69.03(11) . . ? C42 C41 C46 123.28(18) . . ? C42 C41 N3 119.04(17) . . ? C46 C41 N3 117.56(18) . . ? C41 C42 C43 116.96(19) . . ? C41 C42 C47 122.49(18) . . ? C43 C42 C47 120.52(19) . . ? C44 C43 C42 120.9(2) . . ? C45 C44 C43 120.8(2) . . ? C44 C45 C46 120.9(2) . . ? C41 C46 C50 122.82(18) . . ? C45 C46 C41 117.1(2) . . ? C45 C46 C50 120.09(19) . . ? C42 C47 C48 112.9(2) . . ? C42 C47 C49 110.67(17) . . ? C48 C47 C49 111.2(2) . . ? C46 C50 C51 112.2(2) . . ? C46 C50 C52 112.24(17) . . ? C52 C50 C51 109.53(19) . . ? C54 C53 C58 122.79(18) . . ? C54 C53 N4 118.49(17) . . ? C58 C53 N4 118.49(17) . . ? C53 C54 C59 122.28(18) . . ? C55 C54 C53 117.1(2) . . ? C55 C54 C59 120.52(19) . . ? C56 C55 C54 121.1(2) . . ? C55 C56 C57 120.6(2) . . ? C56 C57 C58 121.1(2) . . ? C53 C58 C62 121.78(19) . . ? C57 C58 C53 117.2(2) . . ? C57 C58 C62 120.9(2) . . ? C54 C59 C60 112.98(18) . . ? C54 C59 C61 110.06(19) . . ? C60 C59 C61 109.72(18) . . ? C58 C62 C63 113.7(2) . . ? C58 C62 C64 110.23(19) . . ? C63 C62 C64 109.4(2) . . ? C100 C101 C102 114.8(3) . . ? C103 C102 C101 116.9(3) . . ? C104 C103 C102 115.8(3) . . ? C103 C104 C105 115.4(4) . . ? C1 N1 C2 111.64(15) . . ? C1 N1 C9 123.91(15) . . ? C2 N1 C9 123.80(15) . . ? C1 N2 C3 111.44(15) . . ? C1 N2 C21 126.18(15) . . ? C3 N2 C21 121.89(15) . . ? C33 N3 C34 111.83(16) . . ? C33 N3 C41 127.21(15) . . ? C34 N3 C41 120.72(15) . . ? C33 N4 C35 111.85(15) . . ? C33 N4 C53 127.04(15) . . ? C35 N4 C53 121.10(16) . . ? C1 Ni1 C4 114.07(8) . . ? C1 Ni1 C5 145.09(8) . . ? C1 Ni1 C6 168.65(9) . . ? C1 Ni1 C7 129.84(8) . . ? C1 Ni1 C8 106.02(8) . . ? C1 Ni1 Se1 89.62(6) . . ? C4 Ni1 Se1 135.89(6) . . ? C5 Ni1 C4 36.65(8) . . ? C5 Ni1 Se1 104.38(6) . . ? C6 Ni1 C4 64.01(8) . . ? C6 Ni1 C5 39.06(8) . . ? C6 Ni1 C7 38.82(8) . . ? C6 Ni1 C8 65.10(8) . . ? C6 Ni1 Se1 99.14(6) . . ? C7 Ni1 C4 64.49(8) . . ? C7 Ni1 C5 64.51(8) . . ? C7 Ni1 Se1 127.78(6) . . ? C8 Ni1 C4 38.62(8) . . ? C8 Ni1 C5 63.71(8) . . ? C8 Ni1 C7 39.06(8) . . ? C8 Ni1 Se1 164.24(6) . . ? C33 Ni2 C36 164.44(8) . . ? C33 Ni2 C37 145.49(8) . . ? C33 Ni2 C38 112.54(8) . . ? C33 Ni2 C39 102.20(8) . . ? C33 Ni2 C40 125.64(8) . . ? C33 Ni2 Se2 91.77(6) . . ? C36 Ni2 C37 39.33(8) . . ? C36 Ni2 C38 64.29(8) . . ? C36 Ni2 C39 65.34(8) . . ? C36 Ni2 C40 38.80(8) . . ? C36 Ni2 Se2 100.52(6) . . ? C37 Ni2 C38 37.03(8) . . ? C37 Ni2 Se2 104.91(6) . . ? C38 Ni2 Se2 136.28(6) . . ? C39 Ni2 C37 64.39(8) . . ? C39 Ni2 C38 38.90(8) . . ? C39 Ni2 C40 39.10(8) . . ? C39 Ni2 Se2 165.86(6) . . ? C40 Ni2 C37 64.88(8) . . ? C40 Ni2 C38 64.64(8) . . ? C40 Ni2 Se2 129.18(6) . . ? Ni1 Se1 Se2 109.039(12) . . ? Ni2 Se2 Se1 111.858(12) . . ? _shelx_res_file ; TITL mp21c in P2(1)/c CELL 1.54178 19.5580 20.1611 16.7962 90.000 96.192 90.000 ZERR 4.00 0.0003 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N NI SE UNIT 280 384 16 8 8 MERG 2 FMAP 2 PLAN 25 ACTA L.S. 20 WGHT 0.034500 3.438200 FVAR 0.06616 C1 1 0.813428 -0.135168 0.066478 11.00000 0.01039 0.02043 = 0.01448 0.00098 0.00204 -0.00060 C2 1 0.811992 -0.239805 0.014467 11.00000 0.01895 0.01660 = 0.02257 -0.00348 0.00508 -0.00163 AFIX 43 H2 2 0.818268 -0.274867 -0.019983 11.00000 -1.20000 AFIX 0 C3 1 0.782184 -0.242606 0.082912 11.00000 0.01712 0.01648 = 0.02307 -0.00025 0.00489 -0.00252 AFIX 43 H3 2 0.764026 -0.280171 0.104936 11.00000 -1.20000 AFIX 0 C4 1 0.914198 -0.002855 0.025177 11.00000 0.01892 0.02613 = 0.02965 -0.00497 0.01191 -0.00888 AFIX 43 H4 2 0.934879 -0.018742 -0.018366 11.00000 -1.20000 AFIX 0 C5 1 0.864246 0.045965 0.023234 11.00000 0.02157 0.02061 = 0.03130 0.00543 0.00286 -0.00850 AFIX 43 H5 2 0.845147 0.068443 -0.022165 11.00000 -1.20000 AFIX 0 C6 1 0.846994 0.055935 0.103279 11.00000 0.01925 0.01861 = 0.03809 -0.00790 0.00836 -0.00425 AFIX 43 H6 2 0.813535 0.084756 0.118276 11.00000 -1.20000 AFIX 0 C7 1 0.889101 0.014890 0.155014 11.00000 0.02221 0.02579 = 0.02469 -0.00651 0.00356 -0.00943 AFIX 43 H7 2 0.891013 0.013697 0.210561 11.00000 -1.20000 AFIX 0 C8 1 0.928185 -0.024423 0.106698 11.00000 0.01426 0.02171 = 0.03763 -0.00118 0.00073 -0.00353 AFIX 43 H8 2 0.957934 -0.058509 0.124780 11.00000 -1.20000 AFIX 0 C9 1 0.874958 -0.152279 -0.054192 11.00000 0.01505 0.01862 = 0.01522 -0.00279 0.00640 -0.00335 C10 1 0.845254 -0.119012 -0.122121 11.00000 0.01881 0.02008 = 0.01675 -0.00340 0.00463 -0.00266 C11 1 0.889596 -0.095968 -0.175659 11.00000 0.02302 0.02766 = 0.01690 0.00038 0.00459 -0.00300 AFIX 43 H11 2 0.871586 -0.073126 -0.221273 11.00000 -1.20000 AFIX 0 C12 1 0.959651 -0.106353 -0.162365 11.00000 0.02352 0.02791 = 0.02033 -0.00315 0.01044 -0.00854 AFIX 43 H12 2 0.988248 -0.089863 -0.198499 11.00000 -1.20000 AFIX 0 C13 1 0.987586 -0.141077 -0.095746 11.00000 0.01517 0.02734 = 0.02397 -0.00750 0.00694 -0.00422 AFIX 43 H13 2 1.034740 -0.148668 -0.088096 11.00000 -1.20000 AFIX 0 C14 1 0.945659 -0.164938 -0.039675 11.00000 0.01698 0.02066 = 0.01950 -0.00407 0.00369 -0.00192 C15 1 0.768435 -0.109838 -0.141167 11.00000 0.01655 0.02797 = 0.01731 -0.00103 0.00305 0.00043 AFIX 13 H15 2 0.746702 -0.120553 -0.092849 11.00000 -1.20000 AFIX 0 C16 1 0.749233 -0.038670 -0.164918 11.00000 0.02676 0.02927 = 0.02626 0.00106 0.00524 0.00553 AFIX 33 H16A 2 0.700191 -0.035165 -0.176172 11.00000 -1.50000 H16B 2 0.770557 -0.026752 -0.211765 11.00000 -1.50000 H16C 2 0.764865 -0.009302 -0.121764 11.00000 -1.50000 AFIX 0 C17 1 0.741286 -0.158573 -0.206773 11.00000 0.02220 0.03267 = 0.03568 -0.00884 -0.00132 -0.00051 AFIX 33 H17A 2 0.692499 -0.152976 -0.218551 11.00000 -1.50000 H17B 2 0.750999 -0.203126 -0.188807 11.00000 -1.50000 H17C 2 0.763305 -0.150232 -0.254176 11.00000 -1.50000 AFIX 0 C18 1 0.977310 -0.204143 0.032385 11.00000 0.01691 0.02837 = 0.02278 -0.00045 0.00364 -0.00069 AFIX 13 H18 2 0.944849 -0.203654 0.072939 11.00000 -1.20000 AFIX 0 C19 1 1.045762 -0.175249 0.070298 11.00000 0.02495 0.03415 = 0.02951 0.00116 -0.00250 -0.00089 AFIX 33 H19A 2 1.063077 -0.201853 0.115429 11.00000 -1.50000 H19B 2 1.038652 -0.130658 0.087687 11.00000 -1.50000 H19C 2 1.078395 -0.175153 0.031505 11.00000 -1.50000 AFIX 0 C20 1 0.988729 -0.276672 0.009096 11.00000 0.03350 0.02655 = 0.04293 0.00022 -0.00208 0.00184 AFIX 33 H20A 2 1.008461 -0.300788 0.055243 11.00000 -1.50000 H20B 2 1.019380 -0.278267 -0.031821 11.00000 -1.50000 H20C 2 0.945480 -0.296285 -0.010688 11.00000 -1.50000 AFIX 0 C21 1 0.763647 -0.165584 0.193591 11.00000 0.01865 0.01539 = 0.01507 0.00203 0.00514 0.00009 C22 1 0.816034 -0.156789 0.256490 11.00000 0.02096 0.01567 = 0.01978 0.00395 0.00115 -0.00171 C23 1 0.796182 -0.148762 0.333050 11.00000 0.03057 0.02002 = 0.01683 0.00129 -0.00068 -0.00309 AFIX 43 H23 2 0.829612 -0.141688 0.375927 11.00000 -1.20000 AFIX 0 C24 1 0.727608 -0.151109 0.346605 11.00000 0.03828 0.02385 = 0.01593 0.00111 0.01040 -0.00021 AFIX 43 H24 2 0.715467 -0.146341 0.398330 11.00000 -1.20000 AFIX 0 C25 1 0.677480 -0.160473 0.283709 11.00000 0.02398 0.02343 = 0.02371 0.00214 0.01135 0.00006 AFIX 43 H25 2 0.631623 -0.161715 0.293616 11.00000 -1.20000 AFIX 0 C26 1 0.693712 -0.168155 0.205427 11.00000 0.01773 0.01790 = 0.02010 0.00213 0.00554 -0.00064 C27 1 0.891651 -0.161076 0.243757 11.00000 0.01763 0.02980 = 0.02321 0.00636 -0.00218 -0.00308 AFIX 13 H27 2 0.896338 -0.144765 0.189651 11.00000 -1.20000 AFIX 0 C28 1 0.938551 -0.118813 0.302498 11.00000 0.02673 0.04386 = 0.03694 0.00606 -0.00805 -0.00999 AFIX 33 H28A 2 0.985367 -0.123689 0.291191 11.00000 -1.50000 H28B 2 0.934458 -0.133176 0.356271 11.00000 -1.50000 H28C 2 0.925227 -0.073083 0.296852 11.00000 -1.50000 AFIX 0 C29 1 0.915207 -0.233297 0.247598 11.00000 0.02171 0.03886 = 0.03866 0.00464 0.00110 0.00574 AFIX 33 H29A 2 0.962956 -0.235572 0.239318 11.00000 -1.50000 H29B 2 0.888531 -0.258347 0.206710 11.00000 -1.50000 H29C 2 0.908947 -0.251392 0.299181 11.00000 -1.50000 AFIX 0 C30 1 0.636663 -0.181932 0.139024 11.00000 0.01400 0.02548 = 0.02063 0.00205 0.00408 -0.00175 AFIX 13 H30 2 0.656063 -0.178661 0.087753 11.00000 -1.20000 AFIX 0 C31 1 0.577062 -0.132372 0.137809 11.00000 0.01577 0.03332 = 0.03909 0.00557 0.00740 0.00183 AFIX 33 H31A 2 0.542552 -0.143207 0.094725 11.00000 -1.50000 H31B 2 0.593883 -0.088341 0.130210 11.00000 -1.50000 H31C 2 0.557449 -0.134548 0.187733 11.00000 -1.50000 AFIX 0 C32 1 0.609126 -0.252817 0.146870 11.00000 0.02248 0.02901 = 0.02950 0.00265 0.00293 -0.00576 AFIX 33 H32A 2 0.573190 -0.261109 0.104448 11.00000 -1.50000 H32B 2 0.591226 -0.257567 0.197583 11.00000 -1.50000 H32C 2 0.645773 -0.284023 0.143478 11.00000 -1.50000 AFIX 0 C33 1 0.647143 0.190113 0.174945 11.00000 0.01387 0.01647 = 0.01640 0.00206 0.00280 0.00024 C34 1 0.594157 0.240252 0.273617 11.00000 0.02240 0.02918 = 0.01828 -0.00615 0.00605 0.00315 AFIX 43 H34 2 0.559849 0.258854 0.300769 11.00000 -1.20000 AFIX 0 C35 1 0.660777 0.234024 0.300880 11.00000 0.02481 0.02657 = 0.01435 -0.00564 0.00328 0.00227 AFIX 43 H35 2 0.681644 0.247499 0.350625 11.00000 -1.20000 AFIX 0 C36 1 0.694894 0.130457 -0.034972 11.00000 0.02859 0.02814 = 0.01466 -0.00022 0.00815 0.00616 AFIX 43 H36 2 0.719620 0.091983 -0.042531 11.00000 -1.20000 AFIX 0 C37 1 0.621361 0.136768 -0.047581 11.00000 0.02761 0.03027 = 0.01590 -0.00354 0.00186 -0.00259 AFIX 43 H37 2 0.590547 0.103905 -0.066860 11.00000 -1.20000 AFIX 0 C38 1 0.604501 0.200618 -0.025876 11.00000 0.02222 0.03062 = 0.01520 0.00435 0.00150 0.00501 AFIX 43 H38 2 0.560442 0.218443 -0.028855 11.00000 -1.20000 AFIX 0 C39 1 0.667204 0.234224 0.001989 11.00000 0.03271 0.02166 = 0.01460 0.00334 0.00572 0.00044 AFIX 43 H39 2 0.670498 0.276641 0.023825 11.00000 -1.20000 AFIX 0 C40 1 0.723455 0.191880 -0.009342 11.00000 0.02131 0.03272 = 0.01704 0.00629 0.00726 -0.00019 AFIX 43 H40 2 0.769928 0.202647 -0.001389 11.00000 -1.20000 AFIX 0 C41 1 0.521132 0.217800 0.147858 11.00000 0.01310 0.02596 = 0.01701 -0.00434 0.00341 0.00428 C42 1 0.477437 0.162672 0.142430 11.00000 0.01620 0.02809 = 0.02331 -0.00616 0.00754 0.00125 C43 1 0.412551 0.170846 0.099482 11.00000 0.01605 0.03738 = 0.03227 -0.01076 0.00387 -0.00087 AFIX 43 H43 2 0.382544 0.134990 0.093133 11.00000 -1.20000 AFIX 0 C44 1 0.392525 0.231393 0.066443 11.00000 0.01896 0.05190 = 0.02462 -0.00794 0.00009 0.00895 AFIX 43 H44 2 0.348481 0.236327 0.040149 11.00000 -1.20000 AFIX 0 C45 1 0.437017 0.284685 0.071931 11.00000 0.02660 0.03850 = 0.02233 0.00181 0.00421 0.01394 AFIX 43 H45 2 0.422764 0.324955 0.048762 11.00000 -1.20000 AFIX 0 C46 1 0.503249 0.278941 0.111865 11.00000 0.02066 0.02823 = 0.01773 -0.00034 0.00729 0.00606 C47 1 0.497374 0.097239 0.182613 11.00000 0.01744 0.02488 = 0.04353 -0.00258 0.00899 -0.00005 AFIX 13 H47 2 0.547728 0.095651 0.190610 11.00000 -1.20000 AFIX 0 C48 1 0.473186 0.037173 0.131404 11.00000 0.03304 0.03022 = 0.08164 -0.01685 0.00750 -0.00278 AFIX 33 H48A 2 0.487404 -0.002832 0.159456 11.00000 -1.50000 H48B 2 0.493030 0.038792 0.081596 11.00000 -1.50000 H48C 2 0.423951 0.037883 0.121037 11.00000 -1.50000 AFIX 0 C49 1 0.471732 0.093622 0.265580 11.00000 0.04455 0.03669 = 0.05433 0.01640 0.02196 0.01196 AFIX 33 H49A 2 0.485070 0.051961 0.290227 11.00000 -1.50000 H49B 2 0.422520 0.097407 0.260180 11.00000 -1.50000 H49C 2 0.491546 0.129231 0.298295 11.00000 -1.50000 AFIX 0 C50 1 0.552539 0.337459 0.114522 11.00000 0.02868 0.02491 = 0.03279 0.00283 0.01148 0.00528 AFIX 13 H50 2 0.599010 0.320318 0.129687 11.00000 -1.20000 AFIX 0 C51 1 0.552427 0.371317 0.032531 11.00000 0.04312 0.03375 = 0.04378 0.01205 0.01829 0.00941 AFIX 33 H51A 2 0.584212 0.407753 0.036883 11.00000 -1.50000 H51B 2 0.507067 0.387458 0.015258 11.00000 -1.50000 H51C 2 0.565933 0.339890 -0.005764 11.00000 -1.50000 AFIX 0 C52 1 0.537564 0.388926 0.177288 11.00000 0.05004 0.03248 = 0.04852 -0.00676 0.02162 -0.00326 AFIX 33 H52A 2 0.569873 0.424759 0.177116 11.00000 -1.50000 H52B 2 0.541696 0.368586 0.229264 11.00000 -1.50000 H52C 2 0.491727 0.405729 0.164871 11.00000 -1.50000 AFIX 0 C53 1 0.765736 0.190506 0.250263 11.00000 0.01555 0.02342 = 0.01425 -0.00492 -0.00056 0.00126 C54 1 0.789793 0.135235 0.295171 11.00000 0.02430 0.02394 = 0.01504 -0.00592 -0.00174 0.00523 C55 1 0.861017 0.126877 0.308770 11.00000 0.02907 0.03263 = 0.02662 -0.00934 -0.00764 0.01266 AFIX 43 H55 2 0.878857 0.091072 0.339155 11.00000 -1.20000 AFIX 0 C56 1 0.905168 0.170719 0.277970 11.00000 0.01841 0.04426 = 0.03736 -0.01819 -0.00378 0.00405 AFIX 43 H56 2 0.952385 0.163849 0.287075 11.00000 -1.20000 AFIX 0 C57 1 0.880183 0.224629 0.233829 11.00000 0.02095 0.04395 = 0.03103 -0.00889 0.00331 -0.00773 AFIX 43 H57 2 0.910794 0.253414 0.212849 11.00000 -1.20000 AFIX 0 C58 1 0.809838 0.236838 0.220024 11.00000 0.02150 0.03064 = 0.01917 -0.00496 0.00110 -0.00493 C59 1 0.741904 0.088046 0.331882 11.00000 0.03753 0.02367 = 0.02278 0.00430 0.00648 0.00604 AFIX 13 H59 2 0.695647 0.094015 0.304038 11.00000 -1.20000 AFIX 0 C60 1 0.762065 0.015194 0.323740 11.00000 0.05138 0.02453 = 0.03119 0.00479 0.00143 0.00678 AFIX 33 H60A 2 0.729989 -0.012455 0.347755 11.00000 -1.50000 H60B 2 0.807464 0.008218 0.350291 11.00000 -1.50000 H60C 2 0.761387 0.004131 0.268069 11.00000 -1.50000 AFIX 0 C61 1 0.739171 0.105049 0.420495 11.00000 0.08043 0.04040 = 0.02545 0.00634 0.01831 0.01328 AFIX 33 H61A 2 0.708501 0.075008 0.443212 11.00000 -1.50000 H61B 2 0.722932 0.149679 0.425054 11.00000 -1.50000 H61C 2 0.784370 0.101102 0.448678 11.00000 -1.50000 AFIX 0 C62 1 0.783001 0.300215 0.179865 11.00000 0.02971 0.03605 = 0.03384 0.00933 -0.00566 -0.01281 AFIX 13 H62 2 0.736160 0.291685 0.155030 11.00000 -1.20000 AFIX 0 C63 1 0.825333 0.324397 0.114538 11.00000 0.06425 0.05601 = 0.03618 0.01115 -0.00234 -0.03019 AFIX 33 H63A 2 0.805522 0.364490 0.091441 11.00000 -1.50000 H63B 2 0.825474 0.291054 0.073752 11.00000 -1.50000 H63C 2 0.871667 0.332877 0.137275 11.00000 -1.50000 AFIX 0 C64 1 0.779127 0.355198 0.242349 11.00000 0.05895 0.02844 = 0.05602 0.00681 0.00402 0.00133 AFIX 33 H64A 2 0.762011 0.395130 0.216184 11.00000 -1.50000 H64B 2 0.824179 0.363145 0.269357 11.00000 -1.50000 H64C 2 0.748767 0.341730 0.280609 11.00000 -1.50000 AFIX 0 C100 1 0.635745 -0.054101 0.552931 11.00000 0.09554 0.05332 = 0.06990 -0.00282 0.00739 -0.02235 AFIX 33 H10A 2 0.598317 -0.031214 0.573424 11.00000 -1.50000 H10B 2 0.634086 -0.100262 0.566618 11.00000 -1.50000 H10C 2 0.632021 -0.049455 0.495744 11.00000 -1.50000 AFIX 0 C101 1 0.702001 -0.025275 0.588539 11.00000 0.08633 0.05385 = 0.03661 0.00410 -0.00426 -0.00773 AFIX 23 H10D 2 0.704471 -0.029178 0.646339 11.00000 -1.20000 H10E 2 0.702349 0.021616 0.575662 11.00000 -1.20000 AFIX 0 C102 1 0.764470 -0.056519 0.561386 11.00000 0.08735 0.03627 = 0.05263 -0.00400 0.00028 0.00153 AFIX 23 H10F 2 0.764711 -0.102989 0.576374 11.00000 -1.20000 H10G 2 0.760440 -0.054587 0.503364 11.00000 -1.20000 AFIX 0 C103 1 0.831751 -0.027535 0.592413 11.00000 0.09467 0.05049 = 0.04336 -0.00036 -0.01413 0.00971 AFIX 23 H10H 2 0.833134 0.017967 0.573892 11.00000 -1.20000 H10I 2 0.834572 -0.026408 0.650410 11.00000 -1.20000 AFIX 0 C104 1 0.892931 -0.062329 0.569410 11.00000 0.09350 0.07030 = 0.10821 -0.02177 -0.00466 0.01954 AFIX 23 H10J 2 0.889616 -0.064469 0.511428 11.00000 -1.20000 H10K 2 0.892283 -0.107502 0.589192 11.00000 -1.20000 AFIX 0 C105 1 0.962121 -0.031012 0.599983 11.00000 0.09754 0.09838 = 0.10959 0.00462 -0.02336 0.00712 AFIX 33 H10L 2 0.998747 -0.056951 0.582231 11.00000 -1.50000 H10M 2 0.966806 -0.029739 0.657449 11.00000 -1.50000 H10N 2 0.964198 0.013294 0.579441 11.00000 -1.50000 AFIX 0 N1 3 0.831536 -0.174312 0.005365 11.00000 0.01402 0.01809 = 0.01512 -0.00073 0.00385 -0.00210 N2 3 0.783588 -0.179139 0.114431 11.00000 0.01236 0.01748 = 0.01526 -0.00036 0.00417 -0.00173 N3 3 0.586248 0.213577 0.197031 11.00000 0.01497 0.02129 = 0.01518 -0.00196 0.00239 0.00103 N4 3 0.692637 0.203629 0.240682 11.00000 0.01533 0.02023 = 0.01438 -0.00069 0.00116 0.00183 NI1 4 0.822358 -0.043009 0.074867 11.00000 0.01205 0.01566 = 0.01895 -0.00119 0.00430 -0.00124 NI2 4 0.662039 0.151013 0.076780 11.00000 0.01533 0.01813 = 0.01303 -0.00013 0.00358 0.00135 SE1 5 0.705122 -0.032444 0.046247 11.00000 0.01343 0.01842 = 0.02313 -0.00341 0.00330 0.00016 SE2 5 0.665182 0.046505 0.131929 11.00000 0.02236 0.01907 = 0.02052 0.00167 0.01026 0.00335 HKLF 4 REM mp21c in P2(1)/c REM R1 = 0.0296 for 10916 Fo > 4sig(Fo) and 0.0382 for all 12810 data REM 703 parameters refined using 0 restraints END WGHT 0.0344 3.4597 REM Highest difference peak 0.379, deepest hole -0.578, 1-sigma level 0.058 Q1 1 0.7339 0.0479 0.1254 11.00000 0.05 0.38 Q2 1 0.8072 -0.0815 0.6032 11.00000 0.05 0.35 Q3 1 0.7166 -0.0749 0.5775 11.00000 0.05 0.35 Q4 1 0.9630 -0.1537 -0.0667 11.00000 0.05 0.29 Q5 1 0.9063 -0.0077 0.5902 11.00000 0.05 0.28 Q6 1 0.7619 0.1132 0.3064 11.00000 0.05 0.27 Q7 1 0.5421 0.3244 -0.0266 11.00000 0.05 0.26 Q8 1 0.7297 0.1577 0.0738 11.00000 0.05 0.26 Q9 1 0.9588 -0.1411 0.3562 11.00000 0.05 0.25 Q10 1 0.5199 0.4091 0.0217 11.00000 0.05 0.25 Q11 1 0.6724 0.2012 0.2022 11.00000 0.05 0.25 Q12 1 0.6581 0.0294 0.0522 11.00000 0.05 0.24 Q13 1 0.7791 0.1613 0.2777 11.00000 0.05 0.24 Q14 1 0.9107 -0.0542 0.3194 11.00000 0.05 0.24 Q15 1 0.8514 -0.1598 0.2476 11.00000 0.05 0.24 Q16 1 0.5505 0.2190 0.1743 11.00000 0.05 0.24 Q17 1 0.6692 -0.1816 0.1758 11.00000 0.05 0.23 Q18 1 0.5389 -0.1575 0.1851 11.00000 0.05 0.23 Q19 1 1.0476 -0.1304 0.0691 11.00000 0.05 0.23 Q20 1 0.5143 0.2502 0.1318 11.00000 0.05 0.23 Q21 1 0.8211 -0.2078 0.0083 11.00000 0.05 0.23 Q22 1 0.7132 0.1070 0.1118 11.00000 0.05 0.22 Q23 1 0.8702 0.3515 0.1398 11.00000 0.05 0.22 Q24 1 0.8450 0.2832 0.0925 11.00000 0.05 0.22 Q25 1 0.8271 -0.1526 0.0373 11.00000 0.05 0.22 ; _shelx_res_checksum 88440 _database_code_depnum_ccdc_archive 'CCDC 995933' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6-Te _audit_creation_date 2014-01-23 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _shelxl_version_number 2013-4 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C64 H82 N4 Ni2 Te2, C6 H14' _chemical_formula_sum 'C70 H96 N4 Ni2 Te2' _chemical_formula_weight 1366.12 _chemical_melting_point ? _chemical_oxdiff_formula 'C64 H82 N4 Ni2 Te2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.1759 6.3531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.69630(10) _cell_length_b 20.47330(10) _cell_length_c 16.93030(10) _cell_angle_alpha 90 _cell_angle_beta 98.0580(10) _cell_angle_gamma 90 _cell_volume 6759.71(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 45790 _cell_measurement_temperature 123.01(10) _cell_measurement_theta_max 73.5530 _cell_measurement_theta_min 3.8400 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 7.667 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour 'dark brown' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2816 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 88776 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.632 _diffrn_reflns_theta_min 3.129 _diffrn_ambient_temperature 123.01(10) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0059040000 _diffrn_orient_matrix_UB_12 -0.0618503000 _diffrn_orient_matrix_UB_13 0.0448797000 _diffrn_orient_matrix_UB_21 -0.0079702000 _diffrn_orient_matrix_UB_22 0.0421157000 _diffrn_orient_matrix_UB_23 0.0635014000 _diffrn_orient_matrix_UB_31 -0.0914252000 _diffrn_orient_matrix_UB_32 -0.0076789000 _diffrn_orient_matrix_UB_33 -0.0138185000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 12622 _reflns_number_total 13479 _reflns_odcompleteness_completeness 99.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL-2013 (Sheldrick, 2008)' _computing_structure_solution 'SIR97 (Burla et al., 2007)' _refine_diff_density_max 2.469 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.070 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 703 _refine_ls_number_reflns 13479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0277 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+5.4258P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.0735 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.027) H3(0.03) H4(0.029) H5(0.028) H6(0.027) H7(0.028) H8(0.03) H11(0.037) H12(0.042) H13(0.037) H15(0.037) H16A(0.071) H16B(0.071) H16C(0.071) H17A(0.065) H17B(0.065) H17C(0.065) H18(0.033) H19A(0.056) H19B(0.056) H19C(0.056) H20A(0.068) H20B(0.068) H20C(0.068) H23(0.035) H24(0.039) H25(0.035) H27(0.035) H28A(0.063) H28B(0.063) H28C(0.063) H29A(0.065) H29B(0.065) H29C(0.065) H30(0.033) H31A(0.057) H31B(0.057) H31C(0.057) H32A(0.061) H32B(0.061) H32C(0.061) H34(0.024) H35(0.025) H36(0.032) H37(0.032) H38(0.032) H39(0.032) H40(0.033) H43(0.029) H44(0.034) H45(0.031) H47(0.03) H48A(0.053) H48B(0.053) H48C(0.053) H49A(0.055) H49B(0.055) H49C(0.055) H50(0.026) H51A(0.044) H51B(0.044) H51C(0.044) H52A(0.048) H52B(0.048) H52C(0.048) H55(0.028) H56(0.03) H57(0.027) H59(0.029) H60A(0.059) H60B(0.059) H60C(0.059) H61A(0.048) H61B(0.048) H61C(0.048) H62(0.026) H63A(0.049) H63B(0.049) H63C(0.049) H64A(0.045) H64B(0.045) H64C(0.045) H10A(0.126) H10B(0.126) H10C(0.126) H10D(0.101) H10E(0.101) H10F(0.102) H10G(0.102) H10H(0.104) H10I(0.104) H10J(0.156) H10K(0.156) H10L(0.165) H10M(0.165) H10N(0.165) Fixed X: H2(0.3112) H3(0.4346) H4(0.2737) H5(0.228) H6(0.3297) H7(0.4371) H8(0.403) H11(0.0955) H12(0.0443) H13(0.107) H15(0.273) H16A(0.2136) H16B(0.1434) H16C(0.1921) H17A(0.2478) H17B(0.2523) H17C(0.1806) H18(0.2884) H19A(0.244) H19B(0.2225) H19C(0.1694) H20A(0.2592) H20B(0.1862) H20C(0.2513) H23(0.5765) H24(0.652) H25(0.6186) H27(0.4) H28A(0.4179) H28B(0.4382) H28C(0.4954) H29A(0.4271) H29B(0.505) H29C(0.4524) H30(0.4528) H31A(0.5159) H31B(0.5787) H31C(0.5108) H32A(0.5149) H32B(0.5068) H32C(0.5765) H34(0.2355) H35(0.1805) H36(0.0398) H37(0.1079) H38(0.1851) H39(0.1511) H40(0.0611) H43(0.1758) H44(0.2906) H45(0.3719) H47(0.1042) H48A(0.0395) H48B(0.0952) H48C(0.1132) H49A(0.0177) H49B(0.0774) H49C(0.0704) H50(0.3439) H51A(0.4215) H51B(0.3479) H51C(0.404) H52A(0.4594) H52B(0.4458) H52C(0.4122) H55(-0.0359) H56(0.0103) H57(0.1271) H59(0.0534) H60A(-0.0106) H60B(0.0523) H60C(-0.0212) H61A(-0.0645) H61B(-0.0795) H61C(-0.0393) H62(0.2516) H63A(0.3044) H63B(0.2335) H63C(0.2453) H64A(0.2997) H64B(0.2361) H64C(0.2294) H10A(0.4026) H10B(0.3698) H10C(0.3699) H10D(0.3001) H10E(0.3002) H10F(0.2415) H10G(0.2438) H10H(0.1685) H10I(0.1702) H10J(0.1127) H10K(0.1148) H10L(0.006) H10M(0.0381) H10N(0.036) Fixed Y: H2(-0.2442) H3(-0.2514) H4(-0.1104) H5(-0.2193) H6(-0.2893) H7(- 0.2307) H8(-0.1191) H11(-0.2694) H12(-0.1762) H13(-0.1002) H15(-0.3035) H16A(- 0.3861) H16B(-0.3549) H16C(-0.3176) H17A(-0.3998) H17B(-0.3403) H17C(-0.3678) H18(-0.0976) H19A(0.0051) H19B(-0.0119) H19C(-0.0192) H20A(-0.0817) H20B(- 0.111) H20C(-0.1555) H23(-0.326) H24(-0.2398) H25(-0.1401) H27(-0.3203) H28A(- 0.4106) H28B(-0.3459) H28C(-0.3914) H29A(-0.4205) H29B(-0.4014) H29C(-0.3622) H30(-0.0988) H31A(-0.0029) H31B(-0.0443) H31C(-0.0433) H32A(-0.058) H32B(- 0.134) H32C(-0.1037) H34(0.2794) H35(0.2742) H36(0.0604) H37(-0.0111) H38(- 0.0799) H39(-0.0626) H40(0.0228) H43(0.1356) H44(0.138) H45(0.159) H47(0.1437) H48A(0.2337) H48B(0.2488) H48C(0.2558) H49A(0.1241) H49B(0.0737) H49C(0.1332) H50(0.1819) H51A(0.2674) H51B(0.2854) H51C(0.2617) H52A(0.1538) H52B(0.1434) H52C(0.0964) H55(0.1488) H56(0.0908) H57(0.0755) H59(0.2031) H60A(0.2984) H60B(0.2945) H60C(0.2765) H61A(0.2001) H61B(0.1739) H61C(0.1304) H62(0.1221) H63A(0.1621) H63B(0.1608) H63C(0.2089) H64A(0.0437) H64B(0.0142) H64C(0.0366) H10A(0.0319) H10B(0.0492) H10C(0.101) H10D(-0.0153) H10E(0.0362) H10F(0.1076) H10G(0.0587) H10H(0.0391) H10I(-0.009) H10J(0.1132) H10K(0.0655) H10L(0.0651) H10M(-0.0046) H10N(0.0436) Fixed Z: H2(0.1301) H3(0.1763) H4(0.5239) H5(0.4743) H6(0.4553) H7(0.5172) H8(0.5558) H11(0.2887) H12(0.2323) H13(0.1745) H15(0.3218) H16A(0.3789) H16B(0.3426) H16C(0.4088) H17A(0.248) H17B(0.1907) H17C(0.2043) H18(0.1819) H19A(0.1401) H19B(0.2234) H19C(0.1457) H20A(0.0434) H20B(0.0474) H20C(0.065) H23(0.4306) H24(0.4401) H25(0.3846) H27(0.3486) H28A(0.4341) H28B(0.4812) H28C(0.4558) H29A(0.2931) H29B(0.305) H29C(0.2447) H30(0.2867) H31A(0.3181) H31B(0.3573) H31C(0.3957) H32A(0.1886) H32B(0.1812) H32C(0.2203) H34(0.4071) H35(0.5279) H36(0.3758) H37(0.2948) H38(0.3921) H39(0.5292) H40(0.5185) H43(0.1361) H44(0.1219) H45(0.2301) H47(0.3141) H48A(0.26) H48B(0.2049) H48C(0.2977) H49A(0.2072) H49B(0.2056) H49C(0.1467) H50(0.4307) H51A(0.4153) H51B(0.3729) H51C(0.3223) H52A(0.43) H52B(0.3374) H52C(0.3939) H55(0.5864) H56(0.6974) H57(0.7254) H59(0.4302) H60A(0.4445) H60B(0.5122) H60C(0.5307) H61A(0.3834) H61B(0.4662) H61C(0.4123) H62(0.6028) H63A(0.7268) H63B(0.7589) H63C(0.69) H64A(0.6952) H64B(0.6408) H64C(0.728) H10A(-0.0594) H10B(0.0171) H10C(-0.0511) H10D(-0.0659) H10E(-0.134) H10F(-0.0666) H10G(0.0042) H10H(- 0.1444) H10I(-0.0727) H10J(-0.079) H10K(-0.0069) H10L(-0.0799) H10M(-0.0845) H10N(-0.1568) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.35113(11) -0.19534(10) 0.30835(13) 0.0166(4) Uani 1 1 d . . . . . C2 C 0.33349(12) -0.23246(11) 0.18012(14) 0.0224(5) Uani 1 1 d . . . . . H2 H 0.3112 -0.2442 0.1301 0.027 Uiso 1 1 calc R U . . . C3 C 0.40105(12) -0.23648(12) 0.20553(14) 0.0246(5) Uani 1 1 d . . . . . H3 H 0.4346 -0.2514 0.1763 0.030 Uiso 1 1 calc R U . . . C4 C 0.29973(12) -0.14724(12) 0.51645(14) 0.0243(5) Uani 1 1 d . . . . . H4 H 0.2737 -0.1104 0.5239 0.029 Uiso 1 1 calc R U . . . C5 C 0.27394(12) -0.20776(12) 0.48650(14) 0.0235(5) Uani 1 1 d . . . . . H5 H 0.2280 -0.2193 0.4743 0.028 Uiso 1 1 calc R U . . . C6 C 0.33150(12) -0.24797(11) 0.47833(14) 0.0222(5) Uani 1 1 d . . . . . H6 H 0.3297 -0.2893 0.4553 0.027 Uiso 1 1 calc R U . . . C7 C 0.39274(12) -0.21417(12) 0.51154(14) 0.0232(5) Uani 1 1 d . . . . . H7 H 0.4371 -0.2307 0.5172 0.028 Uiso 1 1 calc R U . . . C8 C 0.37348(13) -0.15186(12) 0.53375(14) 0.0252(5) Uani 1 1 d . . . . . H8 H 0.4030 -0.1191 0.5558 0.030 Uiso 1 1 calc R U . . . C9 C 0.23034(11) -0.19870(11) 0.23931(13) 0.0177(4) Uani 1 1 d . . . . . C10 C 0.19224(12) -0.24829(12) 0.27026(14) 0.0233(5) Uani 1 1 d . . . . . C11 C 0.12198(13) -0.23825(13) 0.26723(16) 0.0306(5) Uani 1 1 d . . . . . H11 H 0.0955 -0.2694 0.2887 0.037 Uiso 1 1 calc R U . . . C12 C 0.09114(13) -0.18256(14) 0.23275(18) 0.0350(6) Uani 1 1 d . . . . . H12 H 0.0443 -0.1762 0.2323 0.042 Uiso 1 1 calc R U . . . C13 C 0.12898(13) -0.13654(13) 0.19920(16) 0.0306(6) Uani 1 1 d . . . . . H13 H 0.1070 -0.1002 0.1745 0.037 Uiso 1 1 calc R U . . . C14 C 0.19969(12) -0.14305(11) 0.20139(14) 0.0209(4) Uani 1 1 d . . . . . C15 C 0.22544(14) -0.31258(12) 0.29900(16) 0.0309(6) Uani 1 1 d . . . . . H15 H 0.2730 -0.3035 0.3218 0.037 Uiso 1 1 calc R U . . . C16 C 0.19037(18) -0.34588(16) 0.36329(19) 0.0472(8) Uani 1 1 d . . . . . H16A H 0.2136 -0.3861 0.3789 0.071 Uiso 1 1 calc R U . . . H16B H 0.1434 -0.3549 0.3426 0.071 Uiso 1 1 calc R U . . . H16C H 0.1921 -0.3176 0.4088 0.071 Uiso 1 1 calc R U . . . C17 C 0.22666(18) -0.35947(14) 0.2290(2) 0.0433(7) Uani 1 1 d . . . . . H17A H 0.2478 -0.3998 0.2480 0.065 Uiso 1 1 calc R U . . . H17B H 0.2523 -0.3403 0.1907 0.065 Uiso 1 1 calc R U . . . H17C H 0.1806 -0.3678 0.2043 0.065 Uiso 1 1 calc R U . . . C18 C 0.23999(14) -0.09436(11) 0.15903(15) 0.0274(5) Uani 1 1 d . . . . . H18 H 0.2884 -0.0976 0.1819 0.033 Uiso 1 1 calc R U . . . C19 C 0.21680(17) -0.02347(13) 0.16789(19) 0.0375(6) Uani 1 1 d . . . . . H19A H 0.2440 0.0051 0.1401 0.056 Uiso 1 1 calc R U . . . H19B H 0.2225 -0.0119 0.2234 0.056 Uiso 1 1 calc R U . . . H19C H 0.1694 -0.0192 0.1457 0.056 Uiso 1 1 calc R U . . . C20 C 0.2336(2) -0.11228(15) 0.07041(17) 0.0456(8) Uani 1 1 d . . . . . H20A H 0.2592 -0.0817 0.0434 0.068 Uiso 1 1 calc R U . . . H20B H 0.1862 -0.1110 0.0474 0.068 Uiso 1 1 calc R U . . . H20C H 0.2513 -0.1555 0.0650 0.068 Uiso 1 1 calc R U . . . C21 C 0.47774(11) -0.21952(11) 0.33168(14) 0.0208(4) Uani 1 1 d . . . . . C22 C 0.49578(12) -0.28002(12) 0.36695(15) 0.0238(5) Uani 1 1 d . . . . . C23 C 0.56245(13) -0.28625(13) 0.40726(15) 0.0290(5) Uani 1 1 d . . . . . H23 H 0.5765 -0.3260 0.4306 0.035 Uiso 1 1 calc R U . . . C24 C 0.60781(13) -0.23453(14) 0.41312(16) 0.0321(6) Uani 1 1 d . . . . . H24 H 0.6520 -0.2398 0.4401 0.039 Uiso 1 1 calc R U . . . C25 C 0.58794(12) -0.17483(13) 0.37906(16) 0.0293(5) Uani 1 1 d . . . . . H25 H 0.6186 -0.1401 0.3846 0.035 Uiso 1 1 calc R U . . . C26 C 0.52250(11) -0.16598(12) 0.33649(14) 0.0227(5) Uani 1 1 d . . . . . C27 C 0.44660(13) -0.33765(12) 0.36172(17) 0.0295(5) Uani 1 1 d . . . . . H27 H 0.4000 -0.3203 0.3486 0.035 Uiso 1 1 calc R U . . . C28 C 0.44982(16) -0.37485(14) 0.4406(2) 0.0418(7) Uani 1 1 d . . . . . H28A H 0.4179 -0.4106 0.4341 0.063 Uiso 1 1 calc R U . . . H28B H 0.4382 -0.3459 0.4812 0.063 Uiso 1 1 calc R U . . . H28C H 0.4954 -0.3914 0.4558 0.063 Uiso 1 1 calc R U . . . C29 C 0.45894(17) -0.38486(15) 0.2949(2) 0.0436(7) Uani 1 1 d . . . . . H29A H 0.4271 -0.4205 0.2931 0.065 Uiso 1 1 calc R U . . . H29B H 0.5050 -0.4014 0.3050 0.065 Uiso 1 1 calc R U . . . H29C H 0.4524 -0.3622 0.2447 0.065 Uiso 1 1 calc R U . . . C30 C 0.50302(12) -0.10135(12) 0.29548(16) 0.0272(5) Uani 1 1 d . . . . . H30 H 0.4528 -0.0988 0.2867 0.033 Uiso 1 1 calc R U . . . C31 C 0.52960(14) -0.04249(13) 0.3464(2) 0.0381(7) Uani 1 1 d . . . . . H31A H 0.5159 -0.0029 0.3181 0.057 Uiso 1 1 calc R U . . . H31B H 0.5787 -0.0443 0.3573 0.057 Uiso 1 1 calc R U . . . H31C H 0.5108 -0.0433 0.3957 0.057 Uiso 1 1 calc R U . . . C32 C 0.52758(16) -0.09904(15) 0.21381(19) 0.0406(7) Uani 1 1 d . . . . . H32A H 0.5149 -0.0580 0.1886 0.061 Uiso 1 1 calc R U . . . H32B H 0.5068 -0.1340 0.1812 0.061 Uiso 1 1 calc R U . . . H32C H 0.5765 -0.1037 0.2203 0.061 Uiso 1 1 calc R U . . . C33 C 0.18494(10) 0.13687(10) 0.44227(13) 0.0165(4) Uani 1 1 d . . . . . C34 C 0.21698(11) 0.24241(11) 0.42780(14) 0.0204(4) Uani 1 1 d . . . . . H34 H 0.2355 0.2794 0.4071 0.024 Uiso 1 1 calc R U . . . C35 C 0.18678(11) 0.23971(11) 0.49399(14) 0.0207(4) Uani 1 1 d . . . . . H35 H 0.1805 0.2742 0.5279 0.025 Uiso 1 1 calc R U . . . C36 C 0.06953(12) 0.02708(11) 0.39563(17) 0.0270(5) Uani 1 1 d . . . . . H36 H 0.0398 0.0604 0.3758 0.032 Uiso 1 1 calc R U . . . C37 C 0.10927(12) -0.01177(12) 0.34988(16) 0.0267(5) Uani 1 1 d . . . . . H37 H 0.1079 -0.0111 0.2948 0.032 Uiso 1 1 calc R U . . . C38 C 0.15120(12) -0.05158(11) 0.40448(17) 0.0266(5) Uani 1 1 d . . . . . H38 H 0.1851 -0.0799 0.3921 0.032 Uiso 1 1 calc R U . . . C39 C 0.13263(13) -0.04102(11) 0.48274(16) 0.0269(5) Uani 1 1 d . . . . . H39 H 0.1511 -0.0626 0.5292 0.032 Uiso 1 1 calc R U . . . C40 C 0.08250(12) 0.00680(12) 0.47688(16) 0.0272(5) Uani 1 1 d . . . . . H40 H 0.0611 0.0228 0.5185 0.033 Uiso 1 1 calc R U . . . C41 C 0.23740(11) 0.16576(10) 0.31972(13) 0.0173(4) Uani 1 1 d . . . . . C42 C 0.18655(12) 0.15486(10) 0.25405(14) 0.0199(4) Uani 1 1 d . . . . . C43 C 0.20819(13) 0.14396(11) 0.18036(14) 0.0241(5) Uani 1 1 d . . . . . H43 H 0.1758 0.1356 0.1361 0.029 Uiso 1 1 calc R U . . . C44 C 0.27714(14) 0.14537(12) 0.17171(15) 0.0283(5) Uani 1 1 d . . . . . H44 H 0.2906 0.1380 0.1219 0.034 Uiso 1 1 calc R U . . . C45 C 0.32590(13) 0.15775(12) 0.23683(15) 0.0257(5) Uani 1 1 d . . . . . H45 H 0.3719 0.1590 0.2301 0.031 Uiso 1 1 calc R U . . . C46 C 0.30766(11) 0.16839(10) 0.31241(14) 0.0197(4) Uani 1 1 d . . . . . C47 C 0.11056(12) 0.15973(12) 0.26111(15) 0.0247(5) Uani 1 1 d . . . . . H47 H 0.1042 0.1437 0.3141 0.030 Uiso 1 1 calc R U . . . C48 C 0.08749(14) 0.23117(14) 0.25539(19) 0.0355(6) Uani 1 1 d . . . . . H48A H 0.0395 0.2337 0.2600 0.053 Uiso 1 1 calc R U . . . H48B H 0.0952 0.2488 0.2049 0.053 Uiso 1 1 calc R U . . . H48C H 0.1132 0.2558 0.2977 0.053 Uiso 1 1 calc R U . . . C49 C 0.06477(14) 0.11888(14) 0.19942(18) 0.0365(6) Uani 1 1 d . . . . . H49A H 0.0177 0.1241 0.2072 0.055 Uiso 1 1 calc R U . . . H49B H 0.0774 0.0737 0.2056 0.055 Uiso 1 1 calc R U . . . H49C H 0.0704 0.1332 0.1467 0.055 Uiso 1 1 calc R U . . . C50 C 0.36331(11) 0.18563(11) 0.38070(15) 0.0220(5) Uani 1 1 d . . . . . H50 H 0.3439 0.1819 0.4307 0.026 Uiso 1 1 calc R U . . . C51 C 0.38634(13) 0.25674(12) 0.37198(16) 0.0292(5) Uani 1 1 d . . . . . H51A H 0.4215 0.2674 0.4153 0.044 Uiso 1 1 calc R U . . . H51B H 0.3479 0.2854 0.3729 0.044 Uiso 1 1 calc R U . . . H51C H 0.4040 0.2617 0.3223 0.044 Uiso 1 1 calc R U . . . C52 C 0.42606(12) 0.14056(14) 0.38601(18) 0.0317(6) Uani 1 1 d . . . . . H52A H 0.4594 0.1538 0.4300 0.048 Uiso 1 1 calc R U . . . H52B H 0.4458 0.1434 0.3374 0.048 Uiso 1 1 calc R U . . . H52C H 0.4122 0.0964 0.3939 0.048 Uiso 1 1 calc R U . . . C53 C 0.12340(11) 0.15389(10) 0.55930(13) 0.0174(4) Uani 1 1 d . . . . . C54 C 0.05255(11) 0.16552(11) 0.54200(14) 0.0198(4) Uani 1 1 d . . . . . C55 C 0.01116(11) 0.14164(12) 0.59583(15) 0.0231(5) Uani 1 1 d . . . . . H55 H -0.0359 0.1488 0.5864 0.028 Uiso 1 1 calc R U . . . C56 C 0.03889(12) 0.10746(12) 0.66304(15) 0.0247(5) Uani 1 1 d . . . . . H56 H 0.0103 0.0908 0.6974 0.030 Uiso 1 1 calc R U . . . C57 C 0.10902(12) 0.09794(11) 0.67947(14) 0.0226(5) Uani 1 1 d . . . . . H57 H 0.1271 0.0755 0.7254 0.027 Uiso 1 1 calc R U . . . C58 C 0.15309(11) 0.12138(11) 0.62820(14) 0.0188(4) Uani 1 1 d . . . . . C59 C 0.02092(12) 0.20358(12) 0.46907(15) 0.0241(5) Uani 1 1 d . . . . . H59 H 0.0534 0.2031 0.4302 0.029 Uiso 1 1 calc R U . . . C60 C 0.00926(16) 0.27490(13) 0.4912(2) 0.0392(6) Uani 1 1 d . . . . . H60A H -0.0106 0.2984 0.4445 0.059 Uiso 1 1 calc R U . . . H60B H 0.0523 0.2945 0.5122 0.059 Uiso 1 1 calc R U . . . H60C H -0.0212 0.2765 0.5307 0.059 Uiso 1 1 calc R U . . . C61 C -0.04693(13) 0.17425(13) 0.42901(17) 0.0319(6) Uani 1 1 d . . . . . H61A H -0.0645 0.2001 0.3834 0.048 Uiso 1 1 calc R U . . . H61B H -0.0795 0.1739 0.4662 0.048 Uiso 1 1 calc R U . . . H61C H -0.0393 0.1304 0.4123 0.048 Uiso 1 1 calc R U . . . C62 C 0.23011(11) 0.11421(11) 0.65074(14) 0.0214(4) Uani 1 1 d . . . . . H62 H 0.2516 0.1221 0.6028 0.026 Uiso 1 1 calc R U . . . C63 C 0.25572(13) 0.16636(13) 0.71233(17) 0.0325(6) Uani 1 1 d . . . . . H63A H 0.3044 0.1621 0.7268 0.049 Uiso 1 1 calc R U . . . H63B H 0.2335 0.1608 0.7589 0.049 Uiso 1 1 calc R U . . . H63C H 0.2453 0.2089 0.6900 0.049 Uiso 1 1 calc R U . . . C64 C 0.25075(14) 0.04582(13) 0.68155(17) 0.0301(5) Uani 1 1 d . . . . . H64A H 0.2997 0.0437 0.6952 0.045 Uiso 1 1 calc R U . . . H64B H 0.2361 0.0142 0.6408 0.045 Uiso 1 1 calc R U . . . H64C H 0.2294 0.0366 0.7280 0.045 Uiso 1 1 calc R U . . . C100 C 0.3663(3) 0.0553(2) -0.0395(3) 0.0842(15) Uani 1 1 d . . . . . H10A H 0.4026 0.0319 -0.0594 0.126 Uiso 1 1 calc R U . . . H10B H 0.3698 0.0492 0.0171 0.126 Uiso 1 1 calc R U . . . H10C H 0.3699 0.1010 -0.0511 0.126 Uiso 1 1 calc R U . . . C101 C 0.3019(3) 0.0312(3) -0.0768(3) 0.0840(15) Uani 1 1 d . . . . . H10D H 0.3001 -0.0153 -0.0659 0.101 Uiso 1 1 calc R U . . . H10E H 0.3002 0.0362 -0.1340 0.101 Uiso 1 1 calc R U . . . C102 C 0.2402(3) 0.0616(2) -0.0534(3) 0.0847(16) Uani 1 1 d . . . . . H10F H 0.2415 0.1076 -0.0666 0.102 Uiso 1 1 calc R U . . . H10G H 0.2438 0.0587 0.0042 0.102 Uiso 1 1 calc R U . . . C103 C 0.1719(3) 0.0369(3) -0.0867(3) 0.0865(16) Uani 1 1 d . . . . . H10H H 0.1685 0.0391 -0.1444 0.104 Uiso 1 1 calc R U . . . H10I H 0.1702 -0.0090 -0.0727 0.104 Uiso 1 1 calc R U . . . C104 C 0.1115(4) 0.0675(3) -0.0645(5) 0.130(3) Uani 1 1 d . . . . . H10J H 0.1127 0.1132 -0.0790 0.156 Uiso 1 1 calc R U . . . H10K H 0.1148 0.0655 -0.0069 0.156 Uiso 1 1 calc R U . . . C105 C 0.0414(3) 0.0404(3) -0.0997(4) 0.110(2) Uani 1 1 d . . . . . H10L H 0.0060 0.0651 -0.0799 0.165 Uiso 1 1 calc R U . . . H10M H 0.0381 -0.0046 -0.0845 0.165 Uiso 1 1 calc R U . . . H10N H 0.0360 0.0436 -0.1568 0.165 Uiso 1 1 calc R U . . . N1 N 0.30342(9) -0.20737(9) 0.24299(11) 0.0170(3) Uani 1 1 d . . . . . N2 N 0.41137(9) -0.21420(9) 0.28364(11) 0.0185(4) Uani 1 1 d . . . . . N3 N 0.21557(9) 0.17995(9) 0.39600(11) 0.0167(3) Uani 1 1 d . . . . . N4 N 0.16674(9) 0.17529(9) 0.50200(11) 0.0171(4) Uani 1 1 d . . . . . Ni1 Ni 0.33820(2) -0.16293(2) 0.40863(2) 0.01632(8) Uani 1 1 d . . . . . Ni2 Ni 0.17438(2) 0.04616(2) 0.43384(2) 0.01696(8) Uani 1 1 d . . . . . Te1 Te 0.33963(2) -0.04859(2) 0.36110(2) 0.02275(5) Uani 1 1 d . . . . . Te2 Te 0.29917(2) 0.03114(2) 0.47319(2) 0.01887(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0187(10) 0.0137(9) 0.0170(11) 0.0023(8) 0.0010(8) -0.0014(7) C2 0.0250(11) 0.0277(11) 0.0144(11) -0.0060(9) 0.0022(9) 0.0013(9) C3 0.0243(11) 0.0324(12) 0.0179(11) -0.0084(9) 0.0060(9) 0.0024(9) C4 0.0305(12) 0.0280(11) 0.0159(11) 0.0028(9) 0.0089(9) 0.0079(9) C5 0.0246(11) 0.0282(11) 0.0187(11) 0.0062(9) 0.0060(9) -0.0019(9) C6 0.0305(12) 0.0209(10) 0.0158(11) 0.0030(8) 0.0053(9) -0.0003(9) C7 0.0231(11) 0.0293(11) 0.0170(11) 0.0044(9) 0.0021(9) 0.0034(9) C8 0.0308(12) 0.0310(12) 0.0134(11) -0.0018(9) 0.0011(9) -0.0018(10) C9 0.0181(10) 0.0215(10) 0.0131(10) -0.0042(8) 0.0006(8) -0.0009(8) C10 0.0244(11) 0.0272(12) 0.0177(11) -0.0029(9) 0.0005(9) -0.0062(9) C11 0.0248(12) 0.0375(13) 0.0303(14) -0.0099(11) 0.0062(10) -0.0114(10) C12 0.0183(11) 0.0423(15) 0.0439(16) -0.0200(13) 0.0028(11) -0.0007(10) C13 0.0266(12) 0.0297(12) 0.0328(14) -0.0110(11) -0.0051(10) 0.0080(10) C14 0.0240(11) 0.0214(10) 0.0160(11) -0.0054(8) -0.0014(8) 0.0025(8) C15 0.0335(13) 0.0273(12) 0.0293(14) 0.0069(10) -0.0043(11) -0.0109(10) C16 0.063(2) 0.0419(16) 0.0352(16) 0.0111(13) -0.0001(15) -0.0227(15) C17 0.0556(18) 0.0260(13) 0.0475(18) 0.0009(12) 0.0045(15) 0.0013(12) C18 0.0388(13) 0.0206(11) 0.0233(12) 0.0048(9) 0.0063(10) 0.0063(10) C19 0.0535(17) 0.0212(12) 0.0376(16) 0.0044(11) 0.0062(13) 0.0091(11) C20 0.078(2) 0.0364(15) 0.0241(15) 0.0043(12) 0.0137(14) 0.0129(15) C21 0.0181(10) 0.0272(11) 0.0173(11) -0.0025(9) 0.0034(8) 0.0027(8) C22 0.0230(11) 0.0280(11) 0.0213(12) -0.0023(9) 0.0058(9) 0.0038(9) C23 0.0272(12) 0.0352(13) 0.0244(13) 0.0009(10) 0.0027(10) 0.0119(10) C24 0.0202(11) 0.0479(15) 0.0265(13) -0.0074(11) -0.0028(10) 0.0078(10) C25 0.0189(11) 0.0374(13) 0.0309(14) -0.0105(11) 0.0012(10) -0.0001(9) C26 0.0199(10) 0.0278(11) 0.0212(12) -0.0054(9) 0.0055(9) 0.0009(9) C27 0.0309(12) 0.0244(11) 0.0343(14) 0.0013(10) 0.0089(11) 0.0033(10) C28 0.0464(16) 0.0315(14) 0.0503(19) 0.0120(13) 0.0162(14) 0.0091(12) C29 0.0477(17) 0.0330(14) 0.0528(19) -0.0103(13) 0.0164(15) -0.0034(12) C30 0.0215(11) 0.0261(12) 0.0349(14) -0.0029(10) 0.0068(10) 0.0000(9) C31 0.0298(13) 0.0302(13) 0.0543(19) -0.0086(12) 0.0061(13) -0.0062(10) C32 0.0431(15) 0.0381(15) 0.0437(17) 0.0091(13) 0.0172(13) 0.0089(12) C33 0.0116(9) 0.0208(10) 0.0169(10) 0.0011(8) 0.0010(8) -0.0013(7) C34 0.0229(10) 0.0169(10) 0.0217(11) 0.0004(8) 0.0039(9) -0.0045(8) C35 0.0234(10) 0.0159(10) 0.0231(12) -0.0025(8) 0.0051(9) -0.0033(8) C36 0.0172(10) 0.0220(11) 0.0415(15) -0.0011(10) 0.0034(10) -0.0043(8) C37 0.0263(11) 0.0258(11) 0.0282(13) -0.0059(10) 0.0043(10) -0.0097(9) C38 0.0225(11) 0.0179(10) 0.0410(15) -0.0064(10) 0.0103(10) -0.0041(8) C39 0.0278(12) 0.0217(11) 0.0316(14) 0.0053(10) 0.0050(10) -0.0099(9) C40 0.0233(11) 0.0262(11) 0.0345(14) -0.0069(10) 0.0129(10) -0.0117(9) C41 0.0199(10) 0.0152(9) 0.0176(11) 0.0016(8) 0.0049(8) -0.0016(7) C42 0.0248(11) 0.0149(9) 0.0197(11) 0.0033(8) 0.0023(9) -0.0029(8) C43 0.0338(12) 0.0209(10) 0.0170(11) -0.0001(9) 0.0013(9) -0.0043(9) C44 0.0409(14) 0.0260(11) 0.0201(12) -0.0028(9) 0.0120(10) -0.0026(10) C45 0.0274(12) 0.0256(11) 0.0264(13) 0.0000(9) 0.0115(10) -0.0016(9) C46 0.0213(10) 0.0168(9) 0.0222(12) 0.0023(8) 0.0069(9) -0.0029(8) C47 0.0212(11) 0.0288(12) 0.0227(12) 0.0047(9) -0.0017(9) -0.0031(9) C48 0.0283(13) 0.0344(14) 0.0427(16) 0.0037(12) 0.0013(11) 0.0043(10) C49 0.0306(13) 0.0405(15) 0.0349(15) 0.0031(12) -0.0079(11) -0.0081(11) C50 0.0187(10) 0.0248(11) 0.0232(12) 0.0030(9) 0.0052(9) -0.0039(8) C51 0.0275(12) 0.0294(12) 0.0295(13) 0.0014(10) 0.0005(10) -0.0113(10) C52 0.0186(11) 0.0382(14) 0.0393(15) 0.0070(12) 0.0075(10) -0.0015(10) C53 0.0195(10) 0.0172(9) 0.0165(11) -0.0033(8) 0.0061(8) -0.0044(8) C54 0.0194(10) 0.0208(10) 0.0195(11) -0.0038(8) 0.0035(8) -0.0030(8) C55 0.0173(10) 0.0273(11) 0.0255(12) -0.0048(9) 0.0063(9) -0.0050(8) C56 0.0254(11) 0.0279(11) 0.0229(12) -0.0026(9) 0.0110(9) -0.0085(9) C57 0.0266(11) 0.0246(11) 0.0174(11) 0.0014(9) 0.0053(9) -0.0026(9) C58 0.0195(10) 0.0192(10) 0.0186(11) -0.0029(8) 0.0054(8) -0.0014(8) C59 0.0209(11) 0.0277(11) 0.0236(12) 0.0021(9) 0.0022(9) -0.0015(9) C60 0.0419(15) 0.0270(13) 0.0460(17) 0.0010(12) -0.0032(13) 0.0003(11) C61 0.0244(12) 0.0360(13) 0.0329(14) 0.0036(11) -0.0036(10) -0.0027(10) C62 0.0210(10) 0.0258(11) 0.0180(11) 0.0005(9) 0.0044(9) 0.0007(8) C63 0.0230(11) 0.0360(14) 0.0376(15) -0.0101(12) 0.0005(11) -0.0008(10) C64 0.0327(13) 0.0310(13) 0.0273(14) 0.0060(10) 0.0067(11) 0.0065(10) C100 0.109(4) 0.055(2) 0.090(4) -0.007(2) 0.020(3) -0.022(3) C101 0.109(4) 0.086(3) 0.055(3) -0.009(2) 0.003(3) -0.012(3) C102 0.135(5) 0.049(2) 0.064(3) 0.000(2) -0.006(3) 0.036(3) C103 0.128(5) 0.090(3) 0.036(2) 0.000(2) -0.006(3) 0.018(3) C104 0.171(7) 0.084(4) 0.125(6) -0.030(4) -0.011(5) 0.063(5) C105 0.100(4) 0.120(5) 0.100(5) 0.009(4) -0.020(4) 0.020(4) N1 0.0184(8) 0.0187(8) 0.0138(9) -0.0014(7) 0.0014(7) 0.0003(7) N2 0.0178(8) 0.0221(9) 0.0157(9) -0.0032(7) 0.0030(7) 0.0007(7) N3 0.0163(8) 0.0175(8) 0.0165(9) 0.0004(7) 0.0032(7) -0.0022(6) N4 0.0174(8) 0.0164(8) 0.0182(9) -0.0009(7) 0.0052(7) -0.0034(6) Ni1 0.01914(17) 0.01793(17) 0.01224(18) -0.00052(13) 0.00338(14) 0.00011(13) Ni2 0.01544(17) 0.01444(17) 0.0216(2) -0.00110(14) 0.00465(14) -0.00266(13) Te1 0.03152(8) 0.01750(7) 0.02204(8) 0.00029(5) 0.01360(6) 0.00243(5) Te2 0.01704(7) 0.01767(7) 0.02217(8) -0.00469(5) 0.00368(5) -0.00022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.370(3) . ? C1 N2 1.368(3) . ? C1 Ni1 1.873(2) . ? C2 C3 1.342(3) . ? C2 N1 1.387(3) . ? C3 N2 1.387(3) . ? C4 C5 1.406(3) . ? C4 C8 1.444(3) . ? C4 Ni1 2.097(2) . ? C5 C6 1.423(3) . ? C5 Ni1 2.156(2) . ? C6 C7 1.435(3) . ? C6 Ni1 2.118(2) . ? C7 C8 1.397(3) . ? C7 Ni1 2.183(2) . ? C8 Ni1 2.147(2) . ? C9 C10 1.407(3) . ? C9 C14 1.402(3) . ? C9 N1 1.443(3) . ? C10 C11 1.393(3) . ? C10 C15 1.519(3) . ? C11 C12 1.382(4) . ? C12 C13 1.373(4) . ? C13 C14 1.394(3) . ? C14 C18 1.516(3) . ? C15 C16 1.529(4) . ? C15 C17 1.528(4) . ? C18 C19 1.535(3) . ? C18 C20 1.533(4) . ? C21 C22 1.399(3) . ? C21 C26 1.402(3) . ? C21 N2 1.444(3) . ? C22 C23 1.398(3) . ? C22 C27 1.521(3) . ? C23 C24 1.380(4) . ? C24 C25 1.384(4) . ? C25 C26 1.398(3) . ? C26 C30 1.518(3) . ? C27 C28 1.531(4) . ? C27 C29 1.533(4) . ? C30 C31 1.531(4) . ? C30 C32 1.528(4) . ? C33 N3 1.374(3) . ? C33 N4 1.368(3) . ? C33 Ni2 1.872(2) . ? C34 C35 1.341(3) . ? C34 N3 1.386(3) . ? C35 N4 1.389(3) . ? C36 C37 1.420(4) . ? C36 C40 1.425(4) . ? C36 Ni2 2.112(2) . ? C37 C38 1.410(4) . ? C37 Ni2 2.136(2) . ? C38 C39 1.439(4) . ? C38 Ni2 2.097(2) . ? C39 C40 1.384(4) . ? C39 Ni2 2.177(2) . ? C40 Ni2 2.197(2) . ? C41 C42 1.406(3) . ? C41 C46 1.408(3) . ? C41 N3 1.447(3) . ? C42 C43 1.392(3) . ? C42 C47 1.521(3) . ? C43 C44 1.386(4) . ? C44 C45 1.380(4) . ? C45 C46 1.394(3) . ? C46 C50 1.519(3) . ? C47 C48 1.531(4) . ? C47 C49 1.530(3) . ? C50 C51 1.538(3) . ? C50 C52 1.535(3) . ? C53 C54 1.405(3) . ? C53 C58 1.398(3) . ? C53 N4 1.447(3) . ? C54 C55 1.394(3) . ? C54 C59 1.518(3) . ? C55 C56 1.382(4) . ? C56 C57 1.384(3) . ? C57 C58 1.396(3) . ? C58 C62 1.519(3) . ? C59 C60 1.533(4) . ? C59 C61 1.534(3) . ? C62 C63 1.528(3) . ? C62 C64 1.529(3) . ? C100 C101 1.424(7) . ? C101 C102 1.469(7) . ? C102 C103 1.473(8) . ? C103 C104 1.439(8) . ? C104 C105 1.530(9) . ? Ni1 Te1 2.4769(4) . ? Ni2 Te2 2.4741(4) . ? Te1 Te2 2.70633(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 129.11(16) . . ? N2 C1 N1 103.20(18) . . ? N2 C1 Ni1 127.67(16) . . ? C3 C2 N1 106.7(2) . . ? C2 C3 N2 107.0(2) . . ? C5 C4 C8 108.5(2) . . ? C5 C4 Ni1 72.99(14) . . ? C8 C4 Ni1 71.98(13) . . ? C4 C5 C6 107.0(2) . . ? C4 C5 Ni1 68.42(13) . . ? C6 C5 Ni1 69.08(13) . . ? C5 C6 C7 108.7(2) . . ? C5 C6 Ni1 72.02(13) . . ? C7 C6 Ni1 72.99(13) . . ? C6 C7 Ni1 68.06(13) . . ? C8 C7 C6 107.5(2) . . ? C8 C7 Ni1 69.78(14) . . ? C4 C8 Ni1 68.25(13) . . ? C7 C8 C4 108.0(2) . . ? C7 C8 Ni1 72.58(14) . . ? C10 C9 N1 118.4(2) . . ? C14 C9 C10 122.6(2) . . ? C14 C9 N1 118.86(19) . . ? C9 C10 C15 121.1(2) . . ? C11 C10 C9 117.3(2) . . ? C11 C10 C15 121.4(2) . . ? C12 C11 C10 120.9(2) . . ? C13 C12 C11 120.6(2) . . ? C12 C13 C14 121.4(2) . . ? C9 C14 C18 122.0(2) . . ? C13 C14 C9 117.0(2) . . ? C13 C14 C18 120.8(2) . . ? C10 C15 C16 113.4(3) . . ? C10 C15 C17 110.4(2) . . ? C17 C15 C16 109.3(2) . . ? C14 C18 C19 113.1(2) . . ? C14 C18 C20 109.2(2) . . ? C20 C18 C19 109.7(2) . . ? C22 C21 C26 123.2(2) . . ? C22 C21 N2 117.6(2) . . ? C26 C21 N2 119.1(2) . . ? C21 C22 C27 122.7(2) . . ? C23 C22 C21 117.0(2) . . ? C23 C22 C27 120.3(2) . . ? C24 C23 C22 121.3(2) . . ? C23 C24 C25 120.3(2) . . ? C24 C25 C26 121.0(2) . . ? C21 C26 C30 122.6(2) . . ? C25 C26 C21 117.1(2) . . ? C25 C26 C30 120.3(2) . . ? C22 C27 C28 112.8(2) . . ? C22 C27 C29 111.5(2) . . ? C28 C27 C29 109.8(2) . . ? C26 C30 C31 112.6(2) . . ? C26 C30 C32 110.4(2) . . ? C32 C30 C31 111.0(2) . . ? N3 C33 Ni2 130.26(16) . . ? N4 C33 N3 103.53(18) . . ? N4 C33 Ni2 126.08(16) . . ? C35 C34 N3 107.41(19) . . ? C34 C35 N4 106.63(19) . . ? C37 C36 C40 109.0(2) . . ? C37 C36 Ni2 71.37(13) . . ? C40 C36 Ni2 73.92(14) . . ? C36 C37 Ni2 69.59(14) . . ? C38 C37 C36 106.5(2) . . ? C38 C37 Ni2 69.06(14) . . ? C37 C38 C39 108.4(2) . . ? C37 C38 Ni2 72.05(13) . . ? C39 C38 Ni2 73.35(13) . . ? C38 C39 Ni2 67.34(13) . . ? C40 C39 C38 108.1(2) . . ? C40 C39 Ni2 72.33(14) . . ? C36 C40 Ni2 67.51(13) . . ? C39 C40 C36 107.8(2) . . ? C39 C40 Ni2 70.77(13) . . ? C42 C41 C46 122.5(2) . . ? C42 C41 N3 118.03(19) . . ? C46 C41 N3 119.3(2) . . ? C41 C42 C47 121.8(2) . . ? C43 C42 C41 117.4(2) . . ? C43 C42 C47 120.6(2) . . ? C44 C43 C42 121.3(2) . . ? C45 C44 C43 120.1(2) . . ? C44 C45 C46 121.5(2) . . ? C41 C46 C50 123.7(2) . . ? C45 C46 C41 117.2(2) . . ? C45 C46 C50 118.9(2) . . ? C42 C47 C48 110.14(19) . . ? C42 C47 C49 113.8(2) . . ? C49 C47 C48 109.7(2) . . ? C46 C50 C51 109.74(19) . . ? C46 C50 C52 113.2(2) . . ? C52 C50 C51 109.19(19) . . ? C54 C53 N4 118.1(2) . . ? C58 C53 C54 122.8(2) . . ? C58 C53 N4 119.10(19) . . ? C53 C54 C59 122.6(2) . . ? C55 C54 C53 117.3(2) . . ? C55 C54 C59 120.1(2) . . ? C56 C55 C54 121.1(2) . . ? C55 C56 C57 120.3(2) . . ? C56 C57 C58 121.1(2) . . ? C53 C58 C62 122.82(19) . . ? C57 C58 C53 117.3(2) . . ? C57 C58 C62 119.8(2) . . ? C54 C59 C60 110.4(2) . . ? C54 C59 C61 113.0(2) . . ? C60 C59 C61 109.3(2) . . ? C58 C62 C63 109.06(19) . . ? C58 C62 C64 112.5(2) . . ? C63 C62 C64 111.1(2) . . ? C100 C101 C102 116.9(5) . . ? C101 C102 C103 119.7(4) . . ? C104 C103 C102 119.5(5) . . ? C103 C104 C105 118.3(6) . . ? C1 N1 C2 111.59(18) . . ? C1 N1 C9 125.45(18) . . ? C2 N1 C9 122.89(18) . . ? C1 N2 C3 111.53(18) . . ? C1 N2 C21 127.21(19) . . ? C3 N2 C21 120.84(18) . . ? C33 N3 C34 110.92(18) . . ? C33 N3 C41 126.11(18) . . ? C34 N3 C41 122.66(18) . . ? C33 N4 C35 111.49(18) . . ? C33 N4 C53 124.18(18) . . ? C35 N4 C53 123.74(18) . . ? C1 Ni1 C4 162.72(10) . . ? C1 Ni1 C5 124.71(9) . . ? C1 Ni1 C6 103.93(9) . . ? C1 Ni1 C7 116.04(9) . . ? C1 Ni1 C8 149.93(9) . . ? C1 Ni1 Te1 91.79(6) . . ? C4 Ni1 C5 38.59(9) . . ? C4 Ni1 C6 65.33(9) . . ? C4 Ni1 C7 64.93(9) . . ? C4 Ni1 C8 39.77(9) . . ? C4 Ni1 Te1 99.21(7) . . ? C5 Ni1 C7 64.71(9) . . ? C5 Ni1 Te1 129.44(7) . . ? C6 Ni1 C5 38.89(9) . . ? C6 Ni1 C7 38.95(9) . . ? C6 Ni1 C8 64.78(9) . . ? C6 Ni1 Te1 164.26(7) . . ? C7 Ni1 Te1 133.37(7) . . ? C8 Ni1 C5 65.06(9) . . ? C8 Ni1 C7 37.65(9) . . ? C8 Ni1 Te1 101.77(7) . . ? C33 Ni2 C36 107.47(9) . . ? C33 Ni2 C37 130.67(10) . . ? C33 Ni2 C38 169.44(10) . . ? C33 Ni2 C39 145.92(10) . . ? C33 Ni2 C40 115.25(9) . . ? C33 Ni2 Te2 90.41(6) . . ? C36 Ni2 C37 39.04(10) . . ? C36 Ni2 C39 63.87(10) . . ? C36 Ni2 C40 38.57(10) . . ? C36 Ni2 Te2 162.05(7) . . ? C37 Ni2 C39 64.80(10) . . ? C37 Ni2 C40 64.61(10) . . ? C37 Ni2 Te2 126.26(7) . . ? C38 Ni2 C36 65.15(9) . . ? C38 Ni2 C37 38.89(10) . . ? C38 Ni2 C39 39.31(10) . . ? C38 Ni2 C40 64.30(9) . . ? C38 Ni2 Te2 96.91(7) . . ? C39 Ni2 C40 36.90(10) . . ? C39 Ni2 Te2 102.10(7) . . ? C40 Ni2 Te2 134.32(7) . . ? Ni1 Te1 Te2 108.927(10) . . ? Ni2 Te2 Te1 105.377(10) . . ? _shelx_res_file ; TITL mp21 in P2(1)/c CELL 1.54178 19.6963 20.4733 16.9303 90.000 98.058 90.000 ZERR 4.00 0.0001 0.0001 0.0001 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N NI TE UNIT 280 384 16 8 8 MERG 2 FMAP 2 ACTA PLAN 20 L.S. 30 WGHT 0.040500 5.425800 FVAR 0.17493 C1 1 0.351128 -0.195340 0.308352 11.00000 0.01867 0.01370 = 0.01698 0.00226 0.00104 -0.00138 C2 1 0.333488 -0.232464 0.180123 11.00000 0.02501 0.02772 = 0.01445 -0.00603 0.00221 0.00127 AFIX 43 H2 2 0.311168 -0.244227 0.130071 11.00000 -1.20000 AFIX 0 C3 1 0.401048 -0.236481 0.205535 11.00000 0.02434 0.03240 = 0.01789 -0.00845 0.00602 0.00239 AFIX 43 H3 2 0.434557 -0.251373 0.176312 11.00000 -1.20000 AFIX 0 C4 1 0.299729 -0.147241 0.516450 11.00000 0.03054 0.02803 = 0.01592 0.00282 0.00892 0.00787 AFIX 43 H4 2 0.273669 -0.110442 0.523866 11.00000 -1.20000 AFIX 0 C5 1 0.273945 -0.207759 0.486498 11.00000 0.02458 0.02823 = 0.01865 0.00619 0.00600 -0.00187 AFIX 43 H5 2 0.228004 -0.219315 0.474338 11.00000 -1.20000 AFIX 0 C6 1 0.331503 -0.247965 0.478325 11.00000 0.03055 0.02094 = 0.01575 0.00299 0.00533 -0.00028 AFIX 43 H6 2 0.329723 -0.289277 0.455285 11.00000 -1.20000 AFIX 0 C7 1 0.392741 -0.214169 0.511543 11.00000 0.02308 0.02929 = 0.01696 0.00436 0.00213 0.00345 AFIX 43 H7 2 0.437132 -0.230717 0.517246 11.00000 -1.20000 AFIX 0 C8 1 0.373484 -0.151856 0.533754 11.00000 0.03076 0.03096 = 0.01343 -0.00183 0.00113 -0.00182 AFIX 43 H8 2 0.402969 -0.119122 0.555797 11.00000 -1.20000 AFIX 0 C9 1 0.230344 -0.198700 0.239309 11.00000 0.01807 0.02149 = 0.01307 -0.00425 0.00064 -0.00095 C10 1 0.192241 -0.248290 0.270257 11.00000 0.02437 0.02715 = 0.01769 -0.00291 0.00050 -0.00622 C11 1 0.121984 -0.238245 0.267235 11.00000 0.02476 0.03750 = 0.03033 -0.00991 0.00623 -0.01144 AFIX 43 H11 2 0.095482 -0.269414 0.288698 11.00000 -1.20000 AFIX 0 C12 1 0.091138 -0.182559 0.232753 11.00000 0.01827 0.04227 = 0.04388 -0.01997 0.00278 -0.00072 AFIX 43 H12 2 0.044329 -0.176209 0.232276 11.00000 -1.20000 AFIX 0 C13 1 0.128979 -0.136537 0.199202 11.00000 0.02655 0.02967 = 0.03282 -0.01104 -0.00513 0.00795 AFIX 43 H13 2 0.106976 -0.100225 0.174476 11.00000 -1.20000 AFIX 0 C14 1 0.199691 -0.143054 0.201390 11.00000 0.02396 0.02145 = 0.01603 -0.00544 -0.00142 0.00248 C15 1 0.225440 -0.312577 0.299005 11.00000 0.03348 0.02731 = 0.02930 0.00689 -0.00429 -0.01093 AFIX 13 H15 2 0.273018 -0.303492 0.321807 11.00000 -1.20000 AFIX 0 C16 1 0.190373 -0.345878 0.363289 11.00000 0.06264 0.04191 = 0.03516 0.01106 -0.00010 -0.02275 AFIX 33 H16A 2 0.213560 -0.386066 0.378906 11.00000 -1.50000 H16B 2 0.143412 -0.354861 0.342550 11.00000 -1.50000 H16C 2 0.192127 -0.317620 0.408780 11.00000 -1.50000 AFIX 0 C17 1 0.226656 -0.359470 0.229006 11.00000 0.05561 0.02602 = 0.04749 0.00085 0.00449 0.00129 AFIX 33 H17A 2 0.247839 -0.399790 0.248034 11.00000 -1.50000 H17B 2 0.252316 -0.340277 0.190730 11.00000 -1.50000 H17C 2 0.180578 -0.367806 0.204275 11.00000 -1.50000 AFIX 0 C18 1 0.239994 -0.094356 0.159034 11.00000 0.03879 0.02059 = 0.02327 0.00476 0.00630 0.00634 AFIX 13 H18 2 0.288407 -0.097647 0.181924 11.00000 -1.20000 AFIX 0 C19 1 0.216801 -0.023469 0.167889 11.00000 0.05352 0.02118 = 0.03763 0.00439 0.00620 0.00910 AFIX 33 H19A 2 0.244044 0.005080 0.140104 11.00000 -1.50000 H19B 2 0.222452 -0.011911 0.223377 11.00000 -1.50000 H19C 2 0.169404 -0.019247 0.145722 11.00000 -1.50000 AFIX 0 C20 1 0.233582 -0.112283 0.070414 11.00000 0.07807 0.03637 = 0.02415 0.00432 0.01373 0.01290 AFIX 33 H20A 2 0.259189 -0.081651 0.043396 11.00000 -1.50000 H20B 2 0.186210 -0.110956 0.047356 11.00000 -1.50000 H20C 2 0.251331 -0.155473 0.064976 11.00000 -1.50000 AFIX 0 C21 1 0.477737 -0.219521 0.331684 11.00000 0.01811 0.02718 = 0.01733 -0.00250 0.00342 0.00275 C22 1 0.495779 -0.280019 0.366950 11.00000 0.02296 0.02798 = 0.02134 -0.00228 0.00578 0.00385 C23 1 0.562451 -0.286253 0.407256 11.00000 0.02718 0.03523 = 0.02443 0.00086 0.00265 0.01190 AFIX 43 H23 2 0.576502 -0.326030 0.430566 11.00000 -1.20000 AFIX 0 C24 1 0.607811 -0.234529 0.413122 11.00000 0.02025 0.04787 = 0.02650 -0.00744 -0.00279 0.00779 AFIX 43 H24 2 0.651956 -0.239808 0.440093 11.00000 -1.20000 AFIX 0 C25 1 0.587938 -0.174827 0.379064 11.00000 0.01894 0.03738 = 0.03092 -0.01048 0.00122 -0.00008 AFIX 43 H25 2 0.618619 -0.140055 0.384603 11.00000 -1.20000 AFIX 0 C26 1 0.522499 -0.165983 0.336491 11.00000 0.01991 0.02782 = 0.02118 -0.00538 0.00550 0.00089 C27 1 0.446600 -0.337648 0.361719 11.00000 0.03092 0.02438 = 0.03432 0.00134 0.00890 0.00332 AFIX 13 H27 2 0.400001 -0.320325 0.348584 11.00000 -1.20000 AFIX 0 C28 1 0.449819 -0.374854 0.440585 11.00000 0.04638 0.03148 = 0.05027 0.01199 0.01615 0.00915 AFIX 33 H28A 2 0.417931 -0.410561 0.434140 11.00000 -1.50000 H28B 2 0.438180 -0.345912 0.481238 11.00000 -1.50000 H28C 2 0.495366 -0.391423 0.455837 11.00000 -1.50000 AFIX 0 C29 1 0.458937 -0.384865 0.294889 11.00000 0.04765 0.03301 = 0.05277 -0.01032 0.01644 -0.00344 AFIX 33 H29A 2 0.427136 -0.420549 0.293067 11.00000 -1.50000 H29B 2 0.504957 -0.401369 0.305025 11.00000 -1.50000 H29C 2 0.452444 -0.362241 0.244730 11.00000 -1.50000 AFIX 0 C30 1 0.503022 -0.101354 0.295485 11.00000 0.02148 0.02608 = 0.03487 -0.00294 0.00684 0.00004 AFIX 13 H30 2 0.452846 -0.098778 0.286688 11.00000 -1.20000 AFIX 0 C31 1 0.529597 -0.042485 0.346400 11.00000 0.02982 0.03016 = 0.05435 -0.00857 0.00615 -0.00619 AFIX 33 H31A 2 0.515931 -0.002931 0.318104 11.00000 -1.50000 H31B 2 0.578722 -0.044315 0.357293 11.00000 -1.50000 H31C 2 0.510805 -0.043290 0.395735 11.00000 -1.50000 AFIX 0 C32 1 0.527581 -0.099041 0.213810 11.00000 0.04310 0.03812 = 0.04373 0.00906 0.01722 0.00893 AFIX 33 H32A 2 0.514860 -0.057980 0.188605 11.00000 -1.50000 H32B 2 0.506761 -0.133996 0.181202 11.00000 -1.50000 H32C 2 0.576547 -0.103694 0.220320 11.00000 -1.50000 AFIX 0 C33 1 0.184936 0.136870 0.442268 11.00000 0.01160 0.02080 = 0.01693 0.00113 0.00095 -0.00132 C34 1 0.216981 0.242414 0.427804 11.00000 0.02286 0.01694 = 0.02166 0.00039 0.00392 -0.00455 AFIX 43 H34 2 0.235467 0.279394 0.407066 11.00000 -1.20000 AFIX 0 C35 1 0.186781 0.239706 0.493993 11.00000 0.02343 0.01595 = 0.02313 -0.00254 0.00510 -0.00329 AFIX 43 H35 2 0.180489 0.274240 0.527908 11.00000 -1.20000 AFIX 0 C36 1 0.069528 0.027084 0.395626 11.00000 0.01720 0.02200 = 0.04149 -0.00115 0.00339 -0.00434 AFIX 43 H36 2 0.039829 0.060391 0.375788 11.00000 -1.20000 AFIX 0 C37 1 0.109266 -0.011771 0.349878 11.00000 0.02630 0.02583 = 0.02824 -0.00595 0.00431 -0.00972 AFIX 43 H37 2 0.107902 -0.011096 0.294753 11.00000 -1.20000 AFIX 0 C38 1 0.151197 -0.051575 0.404480 11.00000 0.02253 0.01790 = 0.04096 -0.00641 0.01028 -0.00411 AFIX 43 H38 2 0.185101 -0.079858 0.392052 11.00000 -1.20000 AFIX 0 C39 1 0.132634 -0.041017 0.482741 11.00000 0.02777 0.02166 = 0.03157 0.00528 0.00500 -0.00989 AFIX 43 H39 2 0.151112 -0.062574 0.529170 11.00000 -1.20000 AFIX 0 C40 1 0.082503 0.006797 0.476881 11.00000 0.02331 0.02622 = 0.03448 -0.00686 0.01285 -0.01172 AFIX 43 H40 2 0.061114 0.022819 0.518504 11.00000 -1.20000 AFIX 0 C41 1 0.237398 0.165763 0.319716 11.00000 0.01990 0.01515 = 0.01757 0.00165 0.00488 -0.00158 C42 1 0.186549 0.154862 0.254050 11.00000 0.02478 0.01492 = 0.01972 0.00328 0.00229 -0.00293 C43 1 0.208193 0.143958 0.180359 11.00000 0.03378 0.02086 = 0.01702 -0.00013 0.00129 -0.00430 AFIX 43 H43 2 0.175787 0.135563 0.136075 11.00000 -1.20000 AFIX 0 C44 1 0.277143 0.145373 0.171707 11.00000 0.04087 0.02597 = 0.02012 -0.00277 0.01202 -0.00259 AFIX 43 H44 2 0.290561 0.137973 0.121949 11.00000 -1.20000 AFIX 0 C45 1 0.325901 0.157746 0.236827 11.00000 0.02742 0.02561 = 0.02639 -0.00002 0.01153 -0.00160 AFIX 43 H45 2 0.371947 0.159007 0.230126 11.00000 -1.20000 AFIX 0 C46 1 0.307662 0.168394 0.312411 11.00000 0.02131 0.01679 = 0.02218 0.00229 0.00693 -0.00289 C47 1 0.110561 0.159727 0.261112 11.00000 0.02120 0.02884 = 0.02273 0.00475 -0.00172 -0.00307 AFIX 13 H47 2 0.104210 0.143685 0.314120 11.00000 -1.20000 AFIX 0 C48 1 0.087487 0.231165 0.255390 11.00000 0.02828 0.03442 = 0.04269 0.00372 0.00131 0.00427 AFIX 33 H48A 2 0.039538 0.233704 0.260033 11.00000 -1.50000 H48B 2 0.095222 0.248819 0.204882 11.00000 -1.50000 H48C 2 0.113228 0.255780 0.297668 11.00000 -1.50000 AFIX 0 C49 1 0.064765 0.118875 0.199421 11.00000 0.03061 0.04049 = 0.03486 0.00306 -0.00794 -0.00810 AFIX 33 H49A 2 0.017723 0.124111 0.207205 11.00000 -1.50000 H49B 2 0.077412 0.073687 0.205602 11.00000 -1.50000 H49C 2 0.070420 0.133190 0.146742 11.00000 -1.50000 AFIX 0 C50 1 0.363311 0.185630 0.380703 11.00000 0.01875 0.02483 = 0.02323 0.00302 0.00524 -0.00392 AFIX 13 H50 2 0.343867 0.181941 0.430721 11.00000 -1.20000 AFIX 0 C51 1 0.386337 0.256735 0.371980 11.00000 0.02755 0.02941 = 0.02949 0.00141 0.00047 -0.01125 AFIX 33 H51A 2 0.421454 0.267438 0.415276 11.00000 -1.50000 H51B 2 0.347893 0.285409 0.372918 11.00000 -1.50000 H51C 2 0.404036 0.261740 0.322303 11.00000 -1.50000 AFIX 0 C52 1 0.426058 0.140563 0.386005 11.00000 0.01865 0.03825 = 0.03932 0.00700 0.00750 -0.00146 AFIX 33 H52A 2 0.459379 0.153773 0.430000 11.00000 -1.50000 H52B 2 0.445796 0.143376 0.337390 11.00000 -1.50000 H52C 2 0.412247 0.096352 0.393942 11.00000 -1.50000 AFIX 0 C53 1 0.123401 0.153891 0.559299 11.00000 0.01954 0.01724 = 0.01650 -0.00330 0.00613 -0.00443 C54 1 0.052550 0.165516 0.542000 11.00000 0.01940 0.02076 = 0.01952 -0.00382 0.00347 -0.00295 C55 1 0.011160 0.141643 0.595833 11.00000 0.01732 0.02734 = 0.02545 -0.00485 0.00634 -0.00504 AFIX 43 H55 2 -0.035899 0.148840 0.586355 11.00000 -1.20000 AFIX 0 C56 1 0.038895 0.107462 0.663044 11.00000 0.02538 0.02790 = 0.02293 -0.00256 0.01096 -0.00853 AFIX 43 H56 2 0.010295 0.090766 0.697424 11.00000 -1.20000 AFIX 0 C57 1 0.109018 0.097939 0.679473 11.00000 0.02660 0.02457 = 0.01742 0.00142 0.00530 -0.00261 AFIX 43 H57 2 0.127080 0.075547 0.725445 11.00000 -1.20000 AFIX 0 C58 1 0.153095 0.121380 0.628202 11.00000 0.01949 0.01924 = 0.01860 -0.00287 0.00543 -0.00140 C59 1 0.020922 0.203582 0.469075 11.00000 0.02090 0.02768 = 0.02360 0.00214 0.00223 -0.00152 AFIX 13 H59 2 0.053386 0.203060 0.430190 11.00000 -1.20000 AFIX 0 C60 1 0.009265 0.274902 0.491199 11.00000 0.04189 0.02696 = 0.04598 0.00102 -0.00318 0.00027 AFIX 33 H60A 2 -0.010632 0.298360 0.444535 11.00000 -1.50000 H60B 2 0.052322 0.294476 0.512189 11.00000 -1.50000 H60C 2 -0.021196 0.276540 0.530731 11.00000 -1.50000 AFIX 0 C61 1 -0.046929 0.174245 0.429011 11.00000 0.02442 0.03602 = 0.03295 0.00362 -0.00364 -0.00273 AFIX 33 H61A 2 -0.064503 0.200106 0.383396 11.00000 -1.50000 H61B 2 -0.079486 0.173905 0.466230 11.00000 -1.50000 H61C 2 -0.039265 0.130364 0.412333 11.00000 -1.50000 AFIX 0 C62 1 0.230110 0.114208 0.650743 11.00000 0.02098 0.02580 = 0.01799 0.00051 0.00443 0.00074 AFIX 13 H62 2 0.251645 0.122149 0.602845 11.00000 -1.20000 AFIX 0 C63 1 0.255720 0.166362 0.712332 11.00000 0.02297 0.03601 = 0.03755 -0.01006 0.00048 -0.00084 AFIX 33 H63A 2 0.304414 0.162111 0.726810 11.00000 -1.50000 H63B 2 0.233526 0.160848 0.758884 11.00000 -1.50000 H63C 2 0.245313 0.208897 0.690001 11.00000 -1.50000 AFIX 0 C64 1 0.250748 0.045818 0.681554 11.00000 0.03268 0.03102 = 0.02733 0.00603 0.00675 0.00645 AFIX 33 H64A 2 0.299678 0.043700 0.695196 11.00000 -1.50000 H64B 2 0.236074 0.014212 0.640837 11.00000 -1.50000 H64C 2 0.229449 0.036608 0.727974 11.00000 -1.50000 AFIX 0 C100 1 0.366319 0.055289 -0.039514 11.00000 0.10908 0.05514 = 0.09033 -0.00655 0.02037 -0.02199 AFIX 33 H10A 2 0.402641 0.031925 -0.059406 11.00000 -1.50000 H10B 2 0.369837 0.049246 0.017143 11.00000 -1.50000 H10C 2 0.369909 0.100951 -0.051143 11.00000 -1.50000 AFIX 0 C101 1 0.301890 0.031177 -0.076805 11.00000 0.10904 0.08568 = 0.05494 -0.00899 0.00334 -0.01205 AFIX 23 H10D 2 0.300063 -0.015259 -0.065924 11.00000 -1.20000 H10E 2 0.300169 0.036222 -0.134019 11.00000 -1.20000 AFIX 0 C102 1 0.240155 0.061596 -0.053378 11.00000 0.13544 0.04889 = 0.06423 0.00013 -0.00575 0.03607 AFIX 23 H10F 2 0.241517 0.107632 -0.066610 11.00000 -1.20000 H10G 2 0.243766 0.058696 0.004245 11.00000 -1.20000 AFIX 0 C103 1 0.171895 0.036863 -0.086730 11.00000 0.12760 0.09046 = 0.03629 -0.00020 -0.00618 0.01823 AFIX 23 H10H 2 0.168522 0.039094 -0.144378 11.00000 -1.20000 H10I 2 0.170214 -0.008993 -0.072725 11.00000 -1.20000 AFIX 0 C104 1 0.111540 0.067457 -0.064532 11.00000 0.17149 0.08410 = 0.12487 -0.03004 -0.01109 0.06262 AFIX 23 H10J 2 0.112735 0.113246 -0.078992 11.00000 -1.20000 H10K 2 0.114757 0.065463 -0.006885 11.00000 -1.20000 AFIX 0 C105 1 0.041390 0.040379 -0.099711 11.00000 0.09997 0.12047 = 0.10036 0.00873 -0.01984 0.02013 AFIX 33 H10L 2 0.005979 0.065147 -0.079903 11.00000 -1.50000 H10M 2 0.038139 -0.004558 -0.084484 11.00000 -1.50000 H10N 2 0.036031 0.043556 -0.156820 11.00000 -1.50000 AFIX 0 N1 3 0.303416 -0.207365 0.242992 11.00000 0.01838 0.01866 = 0.01379 -0.00140 0.00140 0.00026 N2 3 0.411369 -0.214202 0.283641 11.00000 0.01780 0.02206 = 0.01574 -0.00316 0.00305 0.00068 N3 3 0.215570 0.179947 0.395996 11.00000 0.01633 0.01753 = 0.01651 0.00037 0.00320 -0.00224 N4 3 0.166743 0.175286 0.502004 11.00000 0.01740 0.01636 = 0.01820 -0.00094 0.00516 -0.00337 NI1 4 0.338198 -0.162930 0.408631 11.00000 0.01914 0.01793 = 0.01224 -0.00052 0.00338 0.00011 NI2 4 0.174380 0.046161 0.433836 11.00000 0.01544 0.01444 = 0.02158 -0.00110 0.00465 -0.00266 TE1 5 0.339627 -0.048587 0.361101 11.00000 0.03152 0.01750 = 0.02204 0.00029 0.01360 0.00243 TE2 5 0.299175 0.031141 0.473188 11.00000 0.01704 0.01767 = 0.02217 -0.00469 0.00368 -0.00022 HKLF 4 REM mp21 in P2(1)/c REM R1 = 0.0277 for 12622 Fo > 4sig(Fo) and 0.0302 for all 13479 data REM 703 parameters refined using 0 restraints END WGHT 0.0404 5.4436 REM Highest difference peak 2.469, deepest hole -0.752, 1-sigma level 0.070 Q1 1 0.2992 -0.0138 0.3797 11.00000 0.05 2.47 Q2 1 0.2836 0.0861 -0.0702 11.00000 0.05 0.88 Q3 1 0.3180 -0.1299 0.4215 11.00000 0.05 0.79 Q4 1 0.1845 0.0172 0.3997 11.00000 0.05 0.67 Q5 1 0.0992 0.0197 -0.0840 11.00000 0.05 0.66 Q6 1 0.2781 0.0392 0.3889 11.00000 0.05 0.50 Q7 1 0.3164 -0.0538 0.2761 11.00000 0.05 0.48 Q8 1 0.3133 0.0385 0.5596 11.00000 0.05 0.47 Q9 1 0.1611 0.0738 -0.0767 11.00000 0.05 0.39 Q10 1 0.3553 -0.0574 0.4452 11.00000 0.05 0.38 Q11 1 0.3305 -0.1637 0.3206 11.00000 0.05 0.36 Q12 1 0.0481 0.0025 -0.0477 11.00000 0.05 0.36 Q13 1 0.3503 -0.1527 0.5040 11.00000 0.05 0.34 Q14 1 0.3359 0.0093 0.5464 11.00000 0.05 0.34 Q15 1 0.2375 0.0428 0.4296 11.00000 0.05 0.33 Q16 1 0.2207 -0.1216 0.1793 11.00000 0.05 0.33 Q17 1 0.2394 0.0248 0.4734 11.00000 0.05 0.32 Q18 1 0.2697 0.1629 0.3154 11.00000 0.05 0.31 Q19 1 0.2534 0.0019 0.4080 11.00000 0.05 0.31 Q20 1 0.2070 0.1506 0.2849 11.00000 0.05 0.30 ; _shelx_res_checksum 27842 _database_code_depnum_ccdc_archive 'CCDC 995934' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7-S _audit_creation_date 2013-11-11 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C64 H82 N4 Ni2 S3)' _chemical_formula_sum 'C128 H164 N8 Ni4 S6' _chemical_formula_weight 2241.87 _chemical_melting_point ? _chemical_oxdiff_formula 'C64 H82 N4 Ni S2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6760(4) _cell_length_b 18.4118(5) _cell_length_c 38.8467(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.027(2) _cell_angle_gamma 90.00 _cell_volume 11861.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 18037 _cell_measurement_temperature 123.00(10) _cell_measurement_theta_max 73.4800 _cell_measurement_theta_min 3.2610 _exptl_absorpt_coefficient_mu 2.086 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary purple _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4784 _exptl_crystal_size_max 0.0873 _exptl_crystal_size_mid 0.0823 _exptl_crystal_size_min 0.0742 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_unetI/netI 0.0386 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_number 47574 _diffrn_reflns_theta_full 66.97 _diffrn_reflns_theta_max 73.76 _diffrn_reflns_theta_min 3.32 _diffrn_ambient_temperature 123.00(10) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9870 _diffrn_measured_fraction_theta_max 0.9517 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0003307000 _diffrn_orient_matrix_UB_12 0.0658794000 _diffrn_orient_matrix_UB_13 -0.0244127000 _diffrn_orient_matrix_UB_21 0.0037180000 _diffrn_orient_matrix_UB_22 -0.0515834000 _diffrn_orient_matrix_UB_23 -0.0310309000 _diffrn_orient_matrix_UB_31 -0.0928244000 _diffrn_orient_matrix_UB_32 -0.0018963000 _diffrn_orient_matrix_UB_33 -0.0055073000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 19041 _reflns_number_total 22844 _reflns_odcompleteness_completeness 98.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2\s(I) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.717 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.051 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1315 _refine_ls_number_reflns 22844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0367 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+3.8796P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.0961 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.032) H3(0.033) H4(0.038) H5(0.038) H6(0.037) H7(0.039) H8(0.04) H11(0.042) H12(0.042) H13(0.034) H15(0.041) H16A(0.068) H16B(0.068) H16C(0.068) H17A(0.073) H17B(0.073) H17C(0.073) H18(0.032) H19A(0.05) H19B(0.05) H19C(0.05) H20A(0.058) H20B(0.058) H20C(0.058) H23(0.049) H24(0.05) H25(0.043) H27(0.052) H28A(0.09) H28B(0.09) H28C(0.09) H29A(0.088) H29B(0.088) H29C(0.088) H30(0.034) H31A(0.053) H31B(0.053) H31C(0.053) H32A(0.057) H32B(0.057) H32C(0.057) H34(0.031) H35(0.03) H36(0.042) H37(0.042) H38(0.039) H39(0.039) H40(0.04) H43(0.052) H44(0.059) H45(0.052) H47(0.047) H48A(0.094) H48B(0.094) H48C(0.094) H49A(0.069) H49B(0.069) H49C(0.069) H50(0.042) H51A(0.071) H51B(0.071) H51C(0.071) H52A(0.066) H52B(0.066) H52C(0.066) H55(0.039) H56(0.043) H57(0.041) H59(0.037) H60A(0.093) H60B(0.093) H60C(0.093) H61A(0.09) H61B(0.09) H61C(0.09) H62(0.04) H63A(0.072) H63B(0.072) H63C(0.072) H64A(0.066) H64B(0.066) H64C(0.066) H66(0.034) H67(0.037) H68(0.046) H69(0.049) H70(0.047) H71(0.041) H72(0.043) H75(0.043) H76(0.047) H77(0.041) H79(0.039) H80A(0.076) H80B(0.076) H80C(0.076) H81A(0.069) H81B(0.069) H81C(0.069) H82(0.038) H83A(0.059) H83B(0.059) H83C(0.059) H84A(0.065) H84B(0.065) H84C(0.065) H87(0.055) H88(0.061) H89(0.054) H91(0.043) H92A(0.07) H92B(0.07) H92C(0.07) H93A(0.067) H93B(0.067) H93C(0.067) H94(0.048) H95A(0.09) H95B(0.09) H95C(0.09) H96A(0.089) H96B(0.089) H96C(0.089) H98(0.031) H99(0.031) H100(0.044) H101(0.043) H102(0.038) H103(0.036) H104(0.041) H107(0.041) H108(0.045) H109(0.04) H111(0.039) H11A(0.068) H11B(0.068) H11C(0.068) H11D(0.064) H11E(0.064) H11F(0.064) H114(0.034) H11G(0.058) H11H(0.058) H11I(0.058) H11J(0.057) H11K(0.057) H11L(0.057) H119(0.042) H120(0.046) H121(0.041) H123(0.037) H12A(0.07) H12B(0.07) H12C(0.07) H12D(0.062) H12E(0.062) H12F(0.062) H126(0.039) H12G(0.062) H12H(0.062) H12I(0.062) H12J(0.072) H12K(0.072) H12L(0.072) Fixed X: H2(-0.0726) H3(-0.1177) H4(-0.0874) H5(0.0351) H6(0.1459) H7(0.0868) H8(-0.0589) H11(-0.0113) H12(0.1115) H13(0.1804) H15(-0.1079) H16A(-0.1685) H16B(-0.1091) H16C(-0.0763) H17A(-0.2197) H17B(-0.1621) H17C(-0.1619) H18(0.1275) H19A(0.2595) H19B(0.2514) H19C(0.2522) H20A(0.1453) H20B(0.1295) H20C(0.0601) H23(-0.2169) H24(-0.1268) H25(-0.0018) H27(-0.1811) H28A(-0.2823) H28B(-0.2014) H28C(-0.27) H29A(-0.3149) H29B(-0.3033) H29C(-0.2545) H30(0.0846) H31A(0.1045) H31B(0.0169) H31C(0.0316) H32A(0.1781) H32B(0.1108) H32C(0.1387) H34(0.4227) H35(0.4276) H36(0.4842) H37(0.3749) H38(0.4027) H39(0.5346) H40(0.5763) H43(0.5573) H44(0.4449) H45(0.3239) H47(0.5622) H48A(0.6891) H48B(0.6229) H48C(0.6604) H49A(0.6608) H49B(0.6283) H49C(0.5743) H50(0.2815) H51A(0.1595) H51B(0.2059) H51C(0.2133) H52A(0.2209) H52B(0.3148) H52C(0.2729) H55(0.3594) H56(0.4893) H57(0.591) H59(0.2958) H60A(0.1945) H60B(0.275) H60C(0.2465) H61A(0.2774) H61B(0.1959) H61C(0.2435) H62(0.5734) H63A(0.7095) H63B(0.6869) H63C(0.6581) H64A(0.6513) H64B(0.5608) H64C(0.6242) H66(0.5142) H67(0.4726) H68(0.4374) H69(0.4854) H70(0.6298) H71(0.6694) H72(0.5463) H75(0.4998) H76(0.6137) H77(0.6989) H79(0.4436) H80A(0.3563) H80B(0.3982) H80C(0.446) H81A(0.3202) H81B(0.3861) H81C(0.3624) H82(0.6787) H83A(0.8158) H83B(0.7867) H83C(0.7973) H84A(0.7213) H84B(0.6983) H84C(0.6308) H87(0.5372) H88(0.4072) H89(0.3213) H91(0.6345) H92A(0.731) H92B(0.663) H92C(0.6815) H93A(0.6693) H93B(0.5803) H93C(0.5972) H94(0.3766) H95A(0.2525) H95B(0.3178) H95C(0.2544) H96A(0.2589) H96B(0.2633) H96C(0.3304) H98(0.9883) H99(1.0143) H100(1.09) H101(0.9669) H102(0.8801) H103(0.9551) H104(1.0909) H107(0.78) H108(0.8737) H109(1.0072) H111(0.8134) H11A(0.6748) H11B(0.7172) H11C(0.6907) H11D(0.7426) H11E(0.7645) H11F(0.8326) H114(1.0957) H11G(1.1971) H11H(1.1331) H11I(1.1329) H11J(1.1584) H11K(1.0695) H11L(1.0908) H119(0.917) H120(1.0448) H121(1.1476) H123(0.8462) H12A(0.8032) H12B(0.8954) H12C(0.8674) H12D(0.7378) H12E(0.7974) H12F(0.7881) H126(1.1283) H12G(1.2468) H12H(1.1726) H12I(1.2269) H12J(1.245) H12K(1.2212) H12L(1.1677) Fixed Y: H2(1.006) H3(1.0132) H4(0.7249) H5(0.6794) H6(0.6704) H7(0.6915) H8(0.7206) H11(0.7995) H12(0.8465) H13(0.9224) H15(0.8194) H16A(0.7237) H16B(0.7354) H16C(0.7081) H17A(0.8468) H17B(0.9141) H17C(0.8657) H18(0.9629) H19A(1.0026) H19B(0.92) H19C(0.9783) H20A(1.0849) H20B(1.0647) H20C(1.0571) H23(0.8407) H24(0.8646) H25(0.9123) H27(0.8663) H28A(0.7788) H28B(0.7497) H28C(0.7777) H29A(0.908) H29B(0.9141) H29C(0.9651) H30(0.9337) H31A(1.0579) H31B(1.0437) H31C(1.0577) H32A(0.9654) H32B(0.9605) H32C(0.8903) H34(0.464) H35(0.5074) H36(0.8077) H37(0.8692) H38(0.8523) H39(0.7884) H40(0.7485) H43(0.5783) H44(0.5523) H45(0.5318) H47(0.624) H48A(0.6429) H48B(0.681) H48C(0.6071) H49A(0.5341) H49B(0.4919) H49C(0.4997) H50(0.5458) H51A(0.5503) H51B(0.5496) H51C(0.6167) H52A(0.4334) H52B(0.4251) H52C(0.4291) H55(0.759) H56(0.7656) H57(0.7017) H59(0.6801) H60A(0.7534) H60B(0.7976) H60C(0.7688) H61A(0.5828) H61B(0.6236) H61C(0.6365) H62(0.5981) H63A(0.6285) H63B(0.6741) H63C(0.6995) H64A(0.5187) H64B(0.5163) H64C(0.5598) H66(0.019) H67(-0.0197) H68(0.2844) H69(0.2398) H70(0.2752) H71(0.3464) H72(0.3635) H75(0.2892) H76(0.2622) H77(0.1717) H79(0.2198) H80A(0.3141) H80B(0.32) H80C(0.3404) H81A(0.1877) H81B(0.1286) H81C(0.1843) H82(0.0645) H83A(0.0675) H83B(0.1456) H83C(0.1251) H84A(-0.02) H84B(0.0346) H84C(0.0008) H87(0.0709) H88(0.1097) H89(0.1306) H91(0.0578) H92A(0.0502) H92B(0.0561) H92C(0.1223) H93A(-0.0591) H93B(-0.058) H93C(-0.0576) H94(0.1338) H95A(0.1924) H95B(0.2299) H95C(0.1773) H96A(0.0637) H96B(0.0403) H96C(0.0151) H98(0.5096) H99(0.5422) H100(0.2579) H101(0.21) H102(0.1515) H103(0.1529) H104(0.207) H107(0.2981) H108(0.256) H109(0.2886) H111(0.375) H11A(0.3666) H11B(0.2944) H11C(0.3515) H11D(0.4821) H11E(0.4729) H11F(0.4886) H114(0.3853) H11G(0.3194) H11H(0.2843) H11I(0.2651) H11J(0.4398) H11K(0.4679) H11L(0.409) H119(0.4502) H120(0.4247) H121(0.4058) H123(0.4493) H12A(0.5685) H12B(0.5676) H12C(0.5747) H12D(0.4627) H12E(0.4657) H12F(0.3938) H126(0.4037) H12G(0.3413) H12H(0.2997) H12I(0.3479) H12J(0.4746) H12K(0.4852) H12L(0.5191) Fixed Z: H2(0.183) H3(0.1209) H4(0.1458) H5(0.1825) H6(0.1444) H7(0.0827) H8(0.0831) H11(0.2717) H12(0.2927) H13(0.259) H15(0.1863) H16A(0.2135) H16B(0.2471) H16C(0.213) H17A(0.2161) H17B(0.2161) H17C(0.2493) H18(0.1705) H19A(0.187) H19B(0.1958) H19C(0.2253) H20A(0.187) H20B(0.2249) H20C(0.1946) H23(0.0276) H24(-0.0117) H25(0.0061) H27(0.1195) H28A(0.1095) H28B(0.0975) H28C(0.07) H29A(0.1077) H29B(0.0682) H29C(0.0952) H30(0.0914) H31A(0.0817) H31B(0.0913) H31C(0.0527) H32A(0.0532) H32B(0.022) H32C(0.0427) H34(0.1454) H35(0.2051) H36(0.1954) H37(0.1578) H38(0.0956) H39(0.0953) H40(0.1562) H43(0.0382) H44(0.0013) H45(0.022) H47(0.1264) H48A(0.1079) H48B(0.0825) H48C(0.0721) H49A(0.139) H49B(0.1053) H49C(0.1358) H50(0.1094) H51A(0.0738) H51B(0.0408) H51C(0.0657) H52A(0.0929) H52B(0.0996) H52C(0.0616) H55(0.2671) H56(0.2936) H57(0.2716) H59(0.1863) H60A(0.2037) H60B(0.2043) H60C(0.239) H61A(0.2235) H61B(0.2132) H61C(0.2497) H62(0.1937) H63A(0.208) H63B(0.2397) H63C(0.2019) H64A(0.2308) H64B(0.2384) H64C(0.263) H66(0.0384) H67(0.094) H68(0.1127) H69(0.1727) H70(0.1852) H71(0.1342) H72(0.0923) H75(-0.0173) H76(- 0.0434) H77(-0.0216) H79(0.0606) H80A(0.0411) H80B(0.0069) H80C(0.0425) H81A(0.0295) H81B(0.0251) H81C(-0.0047) H82(0.0533) H83A(0.0442) H83B(0.0532) H83C(0.0148) H84A(0.0137) H84B(-0.0167) H84C(0.0035) H87(0.2272) H88(0.2308) H89(0.1815) H91(0.1502) H92A(0.1984) H92B(0.2232) H92C(0.1999) H93A(0.1709) H93B(0.1533) H93C(0.1937) H94(0.0958) H95A(0.0967) H95B(0.1228) H95C(0.1365) H96A(0.0835) H96B(0.1224) H96C(0.0997) H98(0.0619) H99(0.1234) H100(0.0952) H101(0.0589) H102(0.099) H103(0.1591) H104(0.1552) H107(0.0052) H108(-0.0293) H109(-0.0178) H111(0.086) H11A(0.0696) H11B(0.0601) H11C(0.0312) H11D(0.0697) H11E(0.0317) H11F(0.0617) H114(0.056) H11G(0.0325) H11H(0.0049) H11I(0.0442) H11J(0.0108) H11K(0.0104) H11L(-0.0163) H119(0.2405) H120(0.2652) H121(0.2311) H123(0.1518) H12A(0.1615) H12B(0.1567) H12C(0.1938) H12D(0.185) H12E(0.219) H12F(0.1973) H126(0.1384) H12G(0.1577) H12H(0.1698) H12I(0.1961) H12J(0.1524) H12K(0.1901) H12L(0.1586) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.00485(10) 0.87740(11) 0.14020(4) 0.0218(4) Uani 1 1 d . . . C2 C -0.05972(11) 0.97398(11) 0.16591(5) 0.0271(4) Uani 1 1 d . . . H2 H -0.0726 1.0060 0.1830 0.032 Uiso 1 1 calc R . . C3 C -0.08441(11) 0.97790(11) 0.13199(5) 0.0272(4) Uani 1 1 d . . . H3 H -0.1177 1.0132 0.1209 0.033 Uiso 1 1 calc R . . C4 C -0.03879(12) 0.71156(12) 0.13786(6) 0.0319(4) Uani 1 1 d . . . H4 H -0.0874 0.7249 0.1458 0.038 Uiso 1 1 calc R . . C5 C 0.03090(13) 0.68836(12) 0.15882(6) 0.0318(4) Uani 1 1 d . . . H5 H 0.0351 0.6794 0.1825 0.038 Uiso 1 1 calc R . . C6 C 0.09232(13) 0.68144(11) 0.13722(6) 0.0312(4) Uani 1 1 d . . . H6 H 0.1459 0.6704 0.1444 0.037 Uiso 1 1 calc R . . C7 C 0.05894(13) 0.69418(12) 0.10218(6) 0.0324(4) Uani 1 1 d . . . H7 H 0.0868 0.6915 0.0827 0.039 Uiso 1 1 calc R . . C8 C -0.02231(13) 0.71122(12) 0.10232(6) 0.0334(4) Uani 1 1 d . . . H8 H -0.0589 0.7206 0.0831 0.040 Uiso 1 1 calc R . . C9 C 0.02495(11) 0.89164(11) 0.20446(4) 0.0232(4) Uani 1 1 d . . . C10 C -0.01894(12) 0.84582(12) 0.22433(5) 0.0277(4) Uani 1 1 d . . . C11 C 0.01584(13) 0.82985(13) 0.25772(5) 0.0347(5) Uani 1 1 d . . . H11 H -0.0113 0.7995 0.2717 0.042 Uiso 1 1 calc R . . C12 C 0.08945(13) 0.85807(13) 0.27038(5) 0.0346(5) Uani 1 1 d . . . H12 H 0.1115 0.8465 0.2927 0.042 Uiso 1 1 calc R . . C13 C 0.13080(12) 0.90362(12) 0.25010(5) 0.0284(4) Uani 1 1 d . . . H13 H 0.1804 0.9224 0.2590 0.034 Uiso 1 1 calc R . . C14 C 0.09956(11) 0.92191(11) 0.21647(5) 0.0240(4) Uani 1 1 d . . . C15 C -0.10202(13) 0.81741(13) 0.21160(5) 0.0341(5) Uani 1 1 d . . . H15 H -0.1079 0.8194 0.1863 0.041 Uiso 1 1 calc R . . C16 C -0.11520(15) 0.73888(14) 0.22231(7) 0.0451(6) Uani 1 1 d . . . H16A H -0.1685 0.7237 0.2135 0.068 Uiso 1 1 calc R . . H16B H -0.1091 0.7354 0.2471 0.068 Uiso 1 1 calc R . . H16C H -0.0763 0.7081 0.2130 0.068 Uiso 1 1 calc R . . C17 C -0.16755(14) 0.86549(16) 0.22448(7) 0.0484(6) Uani 1 1 d . . . H17A H -0.2197 0.8468 0.2161 0.073 Uiso 1 1 calc R . . H17B H -0.1621 0.9141 0.2161 0.073 Uiso 1 1 calc R . . H17C H -0.1619 0.8657 0.2493 0.073 Uiso 1 1 calc R . . C18 C 0.14313(12) 0.97443(11) 0.19489(5) 0.0270(4) Uani 1 1 d . . . H18 H 0.1275 0.9629 0.1705 0.032 Uiso 1 1 calc R . . C19 C 0.23514(12) 0.96825(12) 0.20135(6) 0.0334(4) Uani 1 1 d . . . H19A H 0.2595 1.0026 0.1870 0.050 Uiso 1 1 calc R . . H19B H 0.2514 0.9200 0.1958 0.050 Uiso 1 1 calc R . . H19C H 0.2522 0.9783 0.2253 0.050 Uiso 1 1 calc R . . C20 C 0.11707(14) 1.05257(12) 0.20094(6) 0.0384(5) Uani 1 1 d . . . H20A H 0.1453 1.0849 0.1870 0.058 Uiso 1 1 calc R . . H20B H 0.1295 1.0647 0.2249 0.058 Uiso 1 1 calc R . . H20C H 0.0601 1.0571 0.1946 0.058 Uiso 1 1 calc R . . C21 C -0.07057(11) 0.90223(11) 0.08046(5) 0.0259(4) Uani 1 1 d . . . C22 C -0.14695(13) 0.87379(12) 0.07051(6) 0.0335(4) Uani 1 1 d . . . C23 C -0.16657(14) 0.85994(13) 0.03524(6) 0.0407(5) Uani 1 1 d . . . H23 H -0.2169 0.8407 0.0276 0.049 Uiso 1 1 calc R . . C24 C -0.11267(15) 0.87432(14) 0.01168(6) 0.0416(5) Uani 1 1 d . . . H24 H -0.1268 0.8646 -0.0117 0.050 Uiso 1 1 calc R . . C25 C -0.03766(14) 0.90310(13) 0.02238(5) 0.0356(5) Uani 1 1 d . . . H25 H -0.0018 0.9123 0.0061 0.043 Uiso 1 1 calc R . . C26 C -0.01499(12) 0.91853(11) 0.05714(5) 0.0269(4) Uani 1 1 d . . . C27 C -0.20852(13) 0.86078(15) 0.09605(6) 0.0434(6) Uani 1 1 d . . . H27 H -0.1811 0.8663 0.1195 0.052 Uiso 1 1 calc R . . C28 C -0.24381(17) 0.78473(18) 0.09296(9) 0.0598(8) Uani 1 1 d . . . H28A H -0.2823 0.7788 0.1095 0.090 Uiso 1 1 calc R . . H28B H -0.2014 0.7497 0.0975 0.090 Uiso 1 1 calc R . . H28C H -0.2700 0.7777 0.0700 0.090 Uiso 1 1 calc R . . C29 C -0.27668(16) 0.91729(19) 0.09133(8) 0.0587(7) Uani 1 1 d . . . H29A H -0.3149 0.9080 0.1077 0.088 Uiso 1 1 calc R . . H29B H -0.3033 0.9141 0.0682 0.088 Uiso 1 1 calc R . . H29C H -0.2545 0.9651 0.0952 0.088 Uiso 1 1 calc R . . C30 C 0.06476(11) 0.95459(12) 0.06894(5) 0.0287(4) Uani 1 1 d . . . H30 H 0.0846 0.9337 0.0914 0.034 Uiso 1 1 calc R . . C31 C 0.05340(13) 1.03600(13) 0.07415(6) 0.0355(5) Uani 1 1 d . . . H31A H 0.1045 1.0579 0.0817 0.053 Uiso 1 1 calc R . . H31B H 0.0169 1.0437 0.0913 0.053 Uiso 1 1 calc R . . H31C H 0.0316 1.0577 0.0527 0.053 Uiso 1 1 calc R . . C32 C 0.12907(13) 0.94148(13) 0.04443(6) 0.0377(5) Uani 1 1 d . . . H32A H 0.1781 0.9654 0.0532 0.057 Uiso 1 1 calc R . . H32B H 0.1108 0.9605 0.0220 0.057 Uiso 1 1 calc R . . H32C H 0.1387 0.8903 0.0427 0.057 Uiso 1 1 calc R . . C33 C 0.42522(10) 0.63574(10) 0.15072(5) 0.0212(3) Uani 1 1 d . . . C34 C 0.42389(11) 0.51216(11) 0.15260(5) 0.0256(4) Uani 1 1 d . . . H34 H 0.4227 0.4640 0.1454 0.031 Uiso 1 1 calc R . . C35 C 0.42659(11) 0.53591(11) 0.18532(5) 0.0253(4) Uani 1 1 d . . . H35 H 0.4276 0.5074 0.2051 0.030 Uiso 1 1 calc R . . C36 C 0.47916(13) 0.80982(12) 0.17133(6) 0.0350(5) Uani 1 1 d . . . H36 H 0.4842 0.8077 0.1954 0.042 Uiso 1 1 calc R . . C37 C 0.41859(13) 0.84451(12) 0.15031(6) 0.0350(5) Uani 1 1 d . . . H37 H 0.3749 0.8692 0.1578 0.042 Uiso 1 1 calc R . . C38 C 0.43503(13) 0.83576(11) 0.11493(6) 0.0328(4) Uani 1 1 d . . . H38 H 0.4027 0.8523 0.0956 0.039 Uiso 1 1 calc R . . C39 C 0.50772(12) 0.79816(12) 0.11453(6) 0.0321(4) Uani 1 1 d . . . H39 H 0.5346 0.7884 0.0953 0.039 Uiso 1 1 calc R . . C40 C 0.53234(12) 0.77794(12) 0.14902(6) 0.0337(5) Uani 1 1 d . . . H40 H 0.5763 0.7485 0.1562 0.040 Uiso 1 1 calc R . . C41 C 0.42842(12) 0.56849(10) 0.09467(5) 0.0254(4) Uani 1 1 d . . . C42 C 0.50411(13) 0.57935(11) 0.08280(6) 0.0321(4) Uani 1 1 d . . . C43 C 0.50807(16) 0.57193(14) 0.04710(6) 0.0437(6) Uani 1 1 d . . . H43 H 0.5573 0.5783 0.0382 0.052 Uiso 1 1 calc R . . C44 C 0.44099(18) 0.55549(15) 0.02495(6) 0.0489(6) Uani 1 1 d . . . H44 H 0.4449 0.5523 0.0013 0.059 Uiso 1 1 calc R . . C45 C 0.36857(16) 0.54373(14) 0.03735(6) 0.0436(6) Uani 1 1 d . . . H45 H 0.3239 0.5318 0.0220 0.052 Uiso 1 1 calc R . . C46 C 0.36024(13) 0.54936(12) 0.07270(5) 0.0311(4) Uani 1 1 d . . . C47 C 0.57847(13) 0.59395(13) 0.10752(7) 0.0389(5) Uani 1 1 d . . . H47 H 0.5622 0.6240 0.1264 0.047 Uiso 1 1 calc R . . C48 C 0.64374(16) 0.63500(16) 0.09096(10) 0.0625(9) Uani 1 1 d . . . H48A H 0.6891 0.6429 0.1079 0.094 Uiso 1 1 calc R . . H48B H 0.6229 0.6810 0.0825 0.094 Uiso 1 1 calc R . . H48C H 0.6604 0.6071 0.0721 0.094 Uiso 1 1 calc R . . C49 C 0.61377(14) 0.52333(14) 0.12338(7) 0.0461(6) Uani 1 1 d . . . H49A H 0.6608 0.5341 0.1390 0.069 Uiso 1 1 calc R . . H49B H 0.6283 0.4919 0.1053 0.069 Uiso 1 1 calc R . . H49C H 0.5743 0.4997 0.1358 0.069 Uiso 1 1 calc R . . C50 C 0.28054(12) 0.52953(12) 0.08536(6) 0.0348(5) Uani 1 1 d . . . H50 H 0.2815 0.5458 0.1094 0.042 Uiso 1 1 calc R . . C51 C 0.20807(15) 0.56479(15) 0.06447(7) 0.0476(6) Uani 1 1 d . . . H51A H 0.1595 0.5503 0.0738 0.071 Uiso 1 1 calc R . . H51B H 0.2059 0.5496 0.0408 0.071 Uiso 1 1 calc R . . H51C H 0.2133 0.6167 0.0657 0.071 Uiso 1 1 calc R . . C52 C 0.27142(15) 0.44649(14) 0.08480(7) 0.0438(5) Uani 1 1 d . . . H52A H 0.2209 0.4334 0.0929 0.066 Uiso 1 1 calc R . . H52B H 0.3148 0.4251 0.0996 0.066 Uiso 1 1 calc R . . H52C H 0.2729 0.4291 0.0616 0.066 Uiso 1 1 calc R . . C53 C 0.44379(11) 0.65521(11) 0.21491(5) 0.0243(4) Uani 1 1 d . . . C54 C 0.38036(12) 0.69254(12) 0.22799(5) 0.0269(4) Uani 1 1 d . . . C55 C 0.39999(13) 0.73341(13) 0.25773(5) 0.0329(4) Uani 1 1 d . . . H55 H 0.3594 0.7590 0.2671 0.039 Uiso 1 1 calc R . . C56 C 0.47799(14) 0.73728(13) 0.27382(5) 0.0361(5) Uani 1 1 d . . . H56 H 0.4893 0.7656 0.2936 0.043 Uiso 1 1 calc R . . C57 C 0.53876(13) 0.69925(13) 0.26056(5) 0.0338(5) Uani 1 1 d . . . H57 H 0.5910 0.7017 0.2716 0.041 Uiso 1 1 calc R . . C58 C 0.52309(11) 0.65700(12) 0.23075(5) 0.0276(4) Uani 1 1 d . . . C59 C 0.29406(12) 0.68922(13) 0.21104(5) 0.0306(4) Uani 1 1 d . . . H59 H 0.2958 0.6801 0.1863 0.037 Uiso 1 1 calc R . . C60 C 0.24839(17) 0.75852(16) 0.21484(9) 0.0617(8) Uani 1 1 d . . . H60A H 0.1945 0.7534 0.2037 0.093 Uiso 1 1 calc R . . H60B H 0.2750 0.7976 0.2043 0.093 Uiso 1 1 calc R . . H60C H 0.2465 0.7688 0.2390 0.093 Uiso 1 1 calc R . . C61 C 0.24857(15) 0.62736(17) 0.22570(9) 0.0599(8) Uani 1 1 d . . . H61A H 0.2774 0.5828 0.2235 0.090 Uiso 1 1 calc R . . H61B H 0.1959 0.6236 0.2132 0.090 Uiso 1 1 calc R . . H61C H 0.2435 0.6365 0.2497 0.090 Uiso 1 1 calc R . . C62 C 0.59116(12) 0.61364(13) 0.21738(5) 0.0334(5) Uani 1 1 d . . . H62 H 0.5734 0.5981 0.1937 0.040 Uiso 1 1 calc R . . C63 C 0.66864(13) 0.65809(17) 0.21668(7) 0.0480(6) Uani 1 1 d . . . H63A H 0.7095 0.6285 0.2080 0.072 Uiso 1 1 calc R . . H63B H 0.6869 0.6741 0.2397 0.072 Uiso 1 1 calc R . . H63C H 0.6581 0.6995 0.2019 0.072 Uiso 1 1 calc R . . C64 C 0.60845(13) 0.54585(15) 0.23944(7) 0.0437(6) Uani 1 1 d . . . H64A H 0.6513 0.5187 0.2308 0.066 Uiso 1 1 calc R . . H64B H 0.5608 0.5163 0.2384 0.066 Uiso 1 1 calc R . . H64C H 0.6242 0.5598 0.2630 0.066 Uiso 1 1 calc R . . C65 C 0.54313(10) 0.14003(11) 0.09609(5) 0.0214(4) Uani 1 1 d . . . C66 C 0.51717(11) 0.04639(11) 0.05861(5) 0.0282(4) Uani 1 1 d . . . H66 H 0.5142 0.0190 0.0384 0.034 Uiso 1 1 calc R . . C67 C 0.49440(12) 0.02508(12) 0.08906(5) 0.0304(4) Uani 1 1 d . . . H67 H 0.4726 -0.0197 0.0940 0.037 Uiso 1 1 calc R . . C68 C 0.48779(13) 0.29319(13) 0.12461(6) 0.0381(5) Uani 1 1 d . . . H68 H 0.4374 0.2844 0.1127 0.046 Uiso 1 1 calc R . . C69 C 0.51557(14) 0.26613(14) 0.15824(6) 0.0412(6) Uani 1 1 d . . . H69 H 0.4854 0.2398 0.1727 0.049 Uiso 1 1 calc R . . C70 C 0.59624(14) 0.28650(14) 0.16531(6) 0.0388(5) Uani 1 1 d . . . H70 H 0.6298 0.2752 0.1852 0.047 Uiso 1 1 calc R . . C71 C 0.61834(13) 0.32789(12) 0.13649(6) 0.0340(5) Uani 1 1 d . . . H71 H 0.6694 0.3464 0.1342 0.041 Uiso 1 1 calc R . . C72 C 0.55010(13) 0.33576(12) 0.11242(6) 0.0362(5) Uani 1 1 d . . . H72 H 0.5463 0.3635 0.0923 0.043 Uiso 1 1 calc R . . C73 C 0.56780(11) 0.16016(11) 0.03403(4) 0.0236(4) Uani 1 1 d . . . C74 C 0.51431(12) 0.21466(11) 0.02080(5) 0.0275(4) Uani 1 1 d . . . C75 C 0.53380(13) 0.25229(13) -0.00824(5) 0.0357(5) Uani 1 1 d . . . H75 H 0.4998 0.2892 -0.0173 0.043 Uiso 1 1 calc R . . C76 C 0.60216(14) 0.23637(14) -0.02395(5) 0.0388(5) Uani 1 1 d . . . H76 H 0.6137 0.2622 -0.0434 0.047 Uiso 1 1 calc R . . C77 C 0.65300(13) 0.18226(14) -0.01080(5) 0.0340(5) Uani 1 1 d . . . H77 H 0.6989 0.1717 -0.0216 0.041 Uiso 1 1 calc R . . C78 C 0.63728(11) 0.14265(12) 0.01847(5) 0.0274(4) Uani 1 1 d . . . C79 C 0.43519(12) 0.22967(13) 0.03565(5) 0.0321(4) Uani 1 1 d . . . H79 H 0.4436 0.2198 0.0606 0.039 Uiso 1 1 calc R . . C80 C 0.40624(16) 0.30840(16) 0.03109(7) 0.0505(6) Uani 1 1 d . . . H80A H 0.3563 0.3141 0.0411 0.076 Uiso 1 1 calc R . . H80B H 0.3982 0.3200 0.0069 0.076 Uiso 1 1 calc R . . H80C H 0.4460 0.3404 0.0425 0.076 Uiso 1 1 calc R . . C81 C 0.36990(13) 0.17772(16) 0.01992(7) 0.0460(6) Uani 1 1 d . . . H81A H 0.3202 0.1877 0.0295 0.069 Uiso 1 1 calc R . . H81B H 0.3861 0.1286 0.0251 0.069 Uiso 1 1 calc R . . H81C H 0.3624 0.1843 -0.0047 0.069 Uiso 1 1 calc R . . C82 C 0.69388(12) 0.08161(13) 0.03102(5) 0.0315(4) Uani 1 1 d . . . H82 H 0.6787 0.0645 0.0533 0.038 Uiso 1 1 calc R . . C83 C 0.78163(12) 0.10735(15) 0.03630(6) 0.0392(5) Uani 1 1 d . . . H83A H 0.8158 0.0675 0.0442 0.059 Uiso 1 1 calc R . . H83B H 0.7867 0.1456 0.0532 0.059 Uiso 1 1 calc R . . H83C H 0.7973 0.1251 0.0148 0.059 Uiso 1 1 calc R . . C84 C 0.68528(14) 0.01841(14) 0.00550(6) 0.0434(6) Uani 1 1 d . . . H84A H 0.7213 -0.0200 0.0137 0.065 Uiso 1 1 calc R . . H84B H 0.6983 0.0346 -0.0167 0.065 Uiso 1 1 calc R . . H84C H 0.6308 0.0008 0.0035 0.065 Uiso 1 1 calc R . . C85 C 0.48075(12) 0.08684(12) 0.14542(5) 0.0282(4) Uani 1 1 d . . . C86 C 0.53329(13) 0.07132(13) 0.17495(5) 0.0339(5) Uani 1 1 d . . . C87 C 0.50370(15) 0.08037(16) 0.20700(6) 0.0461(6) Uani 1 1 d . . . H87 H 0.5372 0.0709 0.2272 0.055 Uiso 1 1 calc R . . C88 C 0.42546(16) 0.10319(17) 0.20919(6) 0.0510(7) Uani 1 1 d . . . H88 H 0.4072 0.1097 0.2308 0.061 Uiso 1 1 calc R . . C89 C 0.37419(14) 0.11636(16) 0.17961(6) 0.0447(6) Uani 1 1 d . . . H89 H 0.3213 0.1306 0.1815 0.054 Uiso 1 1 calc R . . C90 C 0.40064(12) 0.10865(13) 0.14696(6) 0.0341(5) Uani 1 1 d . . . C91 C 0.61746(12) 0.04200(14) 0.17237(5) 0.0361(5) Uani 1 1 d . . . H91 H 0.6345 0.0578 0.1502 0.043 Uiso 1 1 calc R . . C92 C 0.67897(14) 0.07026(16) 0.20113(6) 0.0467(6) Uani 1 1 d . . . H92A H 0.7310 0.0502 0.1984 0.070 Uiso 1 1 calc R . . H92B H 0.6630 0.0561 0.2232 0.070 Uiso 1 1 calc R . . H92C H 0.6815 0.1223 0.1999 0.070 Uiso 1 1 calc R . . C93 C 0.61589(15) -0.04088(15) 0.17259(6) 0.0444(6) Uani 1 1 d . . . H93A H 0.6693 -0.0591 0.1709 0.067 Uiso 1 1 calc R . . H93B H 0.5803 -0.0580 0.1533 0.067 Uiso 1 1 calc R . . H93C H 0.5972 -0.0576 0.1937 0.067 Uiso 1 1 calc R . . C94 C 0.34368(12) 0.12249(15) 0.11454(6) 0.0400(5) Uani 1 1 d . . . H94 H 0.3766 0.1338 0.0958 0.048 Uiso 1 1 calc R . . C95 C 0.28682(15) 0.18646(19) 0.11797(9) 0.0601(8) Uani 1 1 d . . . H95A H 0.2525 0.1924 0.0967 0.090 Uiso 1 1 calc R . . H95B H 0.3178 0.2299 0.1228 0.090 Uiso 1 1 calc R . . H95C H 0.2544 0.1773 0.1365 0.090 Uiso 1 1 calc R . . C96 C 0.29445(16) 0.05398(19) 0.10404(8) 0.0591(8) Uani 1 1 d . . . H96A H 0.2589 0.0637 0.0835 0.089 Uiso 1 1 calc R . . H96B H 0.2633 0.0403 0.1224 0.089 Uiso 1 1 calc R . . H96C H 0.3304 0.0151 0.0997 0.089 Uiso 1 1 calc R . . C97 C 0.96601(10) 0.37673(10) 0.11173(4) 0.0189(3) Uani 1 1 d . . . C98 C 0.98483(11) 0.47888(11) 0.08066(5) 0.0260(4) Uani 1 1 d . . . H98 H 0.9883 0.5096 0.0619 0.031 Uiso 1 1 calc R . . C99 C 0.99910(11) 0.49680(11) 0.11437(5) 0.0256(4) Uani 1 1 d . . . H99 H 1.0143 0.5422 0.1234 0.031 Uiso 1 1 calc R . . C100 C 1.04986(13) 0.22928(13) 0.10313(6) 0.0370(5) Uani 1 1 d . . . H100 H 1.0900 0.2579 0.0952 0.044 Uiso 1 1 calc R . . C101 C 0.97876(14) 0.20451(12) 0.08264(5) 0.0360(5) Uani 1 1 d . . . H101 H 0.9669 0.2100 0.0589 0.043 Uiso 1 1 calc R . . C102 C 0.93110(13) 0.17088(11) 0.10498(5) 0.0318(4) Uani 1 1 d . . . H102 H 0.8801 0.1515 0.0990 0.038 Uiso 1 1 calc R . . C103 C 0.97424(12) 0.17113(11) 0.13917(5) 0.0297(4) Uani 1 1 d . . . H103 H 0.9551 0.1529 0.1591 0.036 Uiso 1 1 calc R . . C104 C 1.04929(12) 0.20330(12) 0.13734(6) 0.0339(5) Uani 1 1 d . . . H104 H 1.0909 0.2070 0.1552 0.041 Uiso 1 1 calc R . . C105 C 0.93886(11) 0.36710(11) 0.04765(4) 0.0229(4) Uani 1 1 d . . . C106 C 0.85608(11) 0.35221(12) 0.03978(5) 0.0272(4) Uani 1 1 d . . . C107 C 0.83401(13) 0.31000(13) 0.01068(5) 0.0346(5) Uani 1 1 d . . . H107 H 0.7800 0.2981 0.0052 0.041 Uiso 1 1 calc R . . C108 C 0.88997(14) 0.28526(14) -0.01027(5) 0.0375(5) Uani 1 1 d . . . H108 H 0.8737 0.2560 -0.0293 0.045 Uiso 1 1 calc R . . C109 C 0.97010(13) 0.30387(13) -0.00305(5) 0.0334(5) Uani 1 1 d . . . H109 H 1.0072 0.2886 -0.0178 0.040 Uiso 1 1 calc R . . C110 C 0.99643(11) 0.34547(11) 0.02613(5) 0.0260(4) Uani 1 1 d . . . C111 C 0.79349(11) 0.38235(14) 0.06158(5) 0.0329(5) Uani 1 1 d . . . H111 H 0.8134 0.3750 0.0860 0.039 Uiso 1 1 calc R . . C112 C 0.71145(13) 0.34528(16) 0.05505(6) 0.0450(6) Uani 1 1 d . . . H11A H 0.6748 0.3666 0.0696 0.068 Uiso 1 1 calc R . . H11B H 0.7172 0.2944 0.0601 0.068 Uiso 1 1 calc R . . H11C H 0.6907 0.3515 0.0312 0.068 Uiso 1 1 calc R . . C113 C 0.78225(14) 0.46412(15) 0.05560(6) 0.0425(5) Uani 1 1 d . . . H11D H 0.7426 0.4821 0.0697 0.064 Uiso 1 1 calc R . . H11E H 0.7645 0.4729 0.0317 0.064 Uiso 1 1 calc R . . H11F H 0.8326 0.4886 0.0617 0.064 Uiso 1 1 calc R . . C114 C 1.08493(11) 0.36632(12) 0.03241(5) 0.0287(4) Uani 1 1 d . . . H114 H 1.0957 0.3853 0.0560 0.034 Uiso 1 1 calc R . . C115 C 1.14236(13) 0.30288(14) 0.02811(6) 0.0388(5) Uani 1 1 d . . . H11G H 1.1971 0.3194 0.0325 0.058 Uiso 1 1 calc R . . H11H H 1.1331 0.2843 0.0049 0.058 Uiso 1 1 calc R . . H11I H 1.1329 0.2651 0.0442 0.058 Uiso 1 1 calc R . . C116 C 1.10256(13) 0.42638(14) 0.00694(6) 0.0383(5) Uani 1 1 d . . . H11J H 1.1584 0.4398 0.0108 0.057 Uiso 1 1 calc R . . H11K H 1.0695 0.4679 0.0104 0.057 Uiso 1 1 calc R . . H11L H 1.0908 0.4090 -0.0163 0.057 Uiso 1 1 calc R . . C117 C 1.00209(11) 0.43082(10) 0.17033(4) 0.0216(4) Uani 1 1 d . . . C118 C 0.93933(11) 0.44563(11) 0.19062(5) 0.0256(4) Uani 1 1 d . . . C119 C 0.95764(14) 0.44209(13) 0.22631(5) 0.0353(5) Uani 1 1 d . . . H119 H 0.9170 0.4502 0.2405 0.042 Uiso 1 1 calc R . . C120 C 1.03435(15) 0.42692(13) 0.24122(5) 0.0383(5) Uani 1 1 d . . . H120 H 1.0448 0.4247 0.2652 0.046 Uiso 1 1 calc R . . C121 C 1.09574(13) 0.41494(13) 0.22075(5) 0.0338(5) Uani 1 1 d . . . H121 H 1.1476 0.4058 0.2311 0.041 Uiso 1 1 calc R . . C122 C 1.08105(11) 0.41631(11) 0.18460(5) 0.0256(4) Uani 1 1 d . . . C123 C 0.85629(12) 0.47036(12) 0.17500(6) 0.0306(4) Uani 1 1 d . . . H123 H 0.8462 0.4493 0.1518 0.037 Uiso 1 1 calc R . . C124 C 0.85548(14) 0.55296(14) 0.17142(8) 0.0470(6) Uani 1 1 d . . . H12A H 0.8032 0.5685 0.1615 0.070 Uiso 1 1 calc R . . H12B H 0.8954 0.5676 0.1567 0.070 Uiso 1 1 calc R . . H12C H 0.8674 0.5747 0.1938 0.070 Uiso 1 1 calc R . . C125 C 0.78858(13) 0.44586(14) 0.19603(6) 0.0411(5) Uani 1 1 d . . . H12D H 0.7378 0.4627 0.1850 0.062 Uiso 1 1 calc R . . H12E H 0.7974 0.4657 0.2190 0.062 Uiso 1 1 calc R . . H12F H 0.7881 0.3938 0.1973 0.062 Uiso 1 1 calc R . . C126 C 1.15043(11) 0.40879(13) 0.16263(5) 0.0328(5) Uani 1 1 d . . . H126 H 1.1283 0.4037 0.1384 0.039 Uiso 1 1 calc R . . C127 C 1.20415(13) 0.34336(15) 0.17248(6) 0.0416(5) Uani 1 1 d . . . H12G H 1.2468 0.3413 0.1577 0.062 Uiso 1 1 calc R . . H12H H 1.1726 0.2997 0.1698 0.062 Uiso 1 1 calc R . . H12I H 1.2269 0.3479 0.1961 0.062 Uiso 1 1 calc R . . C128 C 1.20078(14) 0.47840(16) 0.16626(7) 0.0477(6) Uani 1 1 d . . . H12J H 1.2450 0.4746 0.1524 0.072 Uiso 1 1 calc R . . H12K H 1.2212 0.4852 0.1901 0.072 Uiso 1 1 calc R . . H12L H 1.1677 0.5191 0.1586 0.072 Uiso 1 1 calc R . . N1 N -0.01133(9) 0.91288(9) 0.17053(4) 0.0224(3) Uani 1 1 d . . . N2 N -0.05066(9) 0.91920(9) 0.11665(4) 0.0234(3) Uani 1 1 d . . . N3 N 0.42315(9) 0.57317(9) 0.13161(4) 0.0218(3) Uani 1 1 d . . . N4 N 0.42766(9) 0.61116(9) 0.18402(4) 0.0221(3) Uani 1 1 d . . . N5 N 0.54616(9) 0.11697(9) 0.06280(4) 0.0213(3) Uani 1 1 d . . . N6 N 0.50961(9) 0.08275(9) 0.11167(4) 0.0245(3) Uani 1 1 d . . . N7 N 0.96401(9) 0.40599(9) 0.07929(4) 0.0206(3) Uani 1 1 d . . . N8 N 0.98673(8) 0.43433(9) 0.13297(4) 0.0200(3) Uani 1 1 d . . . S1 S 0.16977(3) 0.84279(3) 0.133250(13) 0.02824(10) Uani 1 1 d . . . S2 S 0.23302(3) 0.80124(3) 0.095058(12) 0.02679(10) Uani 1 1 d . . . S3 S 0.29592(3) 0.70955(3) 0.111357(12) 0.02581(10) Uani 1 1 d . . . S4 S 0.70679(3) 0.17628(3) 0.115721(12) 0.02700(10) Uani 1 1 d . . . S5 S 0.78444(3) 0.20370(3) 0.158552(12) 0.03045(11) Uani 1 1 d . . . S6 S 0.84513(3) 0.29802(3) 0.150512(12) 0.02658(10) Uani 1 1 d . . . Ni1 Ni 0.051527(18) 0.790267(18) 0.132474(8) 0.02277(7) Uani 1 1 d . . . Ni2 Ni 0.416627(18) 0.732813(17) 0.135698(8) 0.02110(7) Uani 1 1 d . . . Ni3 Ni 0.587141(18) 0.222856(19) 0.118968(8) 0.02380(7) Uani 1 1 d . . . Ni4 Ni 0.949694(18) 0.278352(17) 0.122690(8) 0.02057(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0201(8) 0.0259(9) 0.0188(8) 0.0030(7) -0.0002(6) -0.0032(7) C2 0.0309(9) 0.0278(10) 0.0225(9) -0.0005(8) 0.0033(7) 0.0038(8) C3 0.0285(9) 0.0274(10) 0.0252(9) 0.0017(8) 0.0004(7) 0.0055(8) C4 0.0307(10) 0.0303(11) 0.0357(11) -0.0030(9) 0.0085(8) -0.0047(8) C5 0.0378(11) 0.0251(10) 0.0330(10) 0.0056(8) 0.0057(8) -0.0012(8) C6 0.0336(10) 0.0220(10) 0.0384(11) 0.0009(9) 0.0053(8) 0.0010(8) C7 0.0414(11) 0.0257(10) 0.0317(10) -0.0073(8) 0.0117(8) -0.0039(9) C8 0.0377(11) 0.0314(11) 0.0300(10) -0.0065(9) -0.0012(8) -0.0082(9) C9 0.0293(9) 0.0241(9) 0.0160(8) 0.0018(7) 0.0020(7) 0.0036(8) C10 0.0315(9) 0.0297(10) 0.0228(9) 0.0009(8) 0.0066(7) 0.0003(8) C11 0.0398(11) 0.0418(13) 0.0234(9) 0.0084(9) 0.0080(8) -0.0030(10) C12 0.0405(11) 0.0430(13) 0.0196(9) 0.0073(9) 0.0001(8) 0.0064(10) C13 0.0300(9) 0.0336(11) 0.0208(9) -0.0003(8) -0.0010(7) 0.0037(8) C14 0.0293(9) 0.0226(9) 0.0201(8) -0.0009(7) 0.0027(7) 0.0042(8) C15 0.0353(10) 0.0395(12) 0.0281(10) -0.0008(9) 0.0066(8) -0.0061(9) C16 0.0472(13) 0.0425(14) 0.0486(14) -0.0041(11) 0.0199(11) -0.0109(11) C17 0.0324(11) 0.0501(15) 0.0629(16) -0.0022(13) 0.0057(10) -0.0026(11) C18 0.0318(10) 0.0260(10) 0.0228(9) 0.0012(8) 0.0012(7) -0.0017(8) C19 0.0319(10) 0.0335(11) 0.0352(11) -0.0010(9) 0.0054(8) -0.0029(9) C20 0.0412(11) 0.0263(11) 0.0459(12) 0.0031(10) -0.0035(9) 0.0007(9) C21 0.0294(9) 0.0261(10) 0.0205(9) -0.0011(7) -0.0060(7) 0.0041(8) C22 0.0360(10) 0.0310(11) 0.0314(10) 0.0017(9) -0.0069(8) -0.0017(9) C23 0.0424(12) 0.0379(13) 0.0372(12) -0.0031(10) -0.0180(9) -0.0046(10) C24 0.0563(14) 0.0397(13) 0.0251(10) -0.0077(9) -0.0130(9) 0.0041(11) C25 0.0456(12) 0.0391(12) 0.0211(9) -0.0044(9) -0.0018(8) 0.0071(10) C26 0.0335(10) 0.0245(10) 0.0218(9) -0.0012(7) -0.0025(7) 0.0091(8) C27 0.0343(11) 0.0531(16) 0.0411(12) 0.0051(11) -0.0047(9) -0.0118(11) C28 0.0464(14) 0.0597(19) 0.0709(19) 0.0127(15) -0.0054(13) -0.0183(13) C29 0.0416(13) 0.073(2) 0.0613(17) 0.0062(16) 0.0071(12) -0.0003(14) C30 0.0286(9) 0.0338(11) 0.0239(9) 0.0017(8) 0.0028(7) 0.0058(8) C31 0.0362(11) 0.0355(12) 0.0356(11) -0.0059(9) 0.0075(8) 0.0003(9) C32 0.0399(11) 0.0393(13) 0.0360(11) 0.0054(10) 0.0135(9) 0.0108(10) C33 0.0181(8) 0.0240(9) 0.0212(8) 0.0002(7) 0.0011(6) -0.0006(7) C34 0.0264(9) 0.0204(9) 0.0298(9) 0.0015(8) 0.0022(7) -0.0024(7) C35 0.0243(9) 0.0246(10) 0.0267(9) 0.0053(8) 0.0010(7) -0.0004(7) C36 0.0453(12) 0.0293(11) 0.0291(10) -0.0042(9) -0.0015(8) -0.0144(9) C37 0.0355(11) 0.0202(10) 0.0508(13) -0.0055(9) 0.0109(9) -0.0060(8) C38 0.0361(10) 0.0213(10) 0.0397(11) 0.0067(9) -0.0031(8) -0.0077(8) C39 0.0301(10) 0.0297(11) 0.0377(11) 0.0017(9) 0.0087(8) -0.0094(8) C40 0.0254(9) 0.0267(10) 0.0472(12) 0.0015(9) -0.0044(8) -0.0065(8) C41 0.0335(10) 0.0191(9) 0.0241(9) -0.0002(7) 0.0061(7) 0.0026(8) C42 0.0395(11) 0.0221(10) 0.0368(11) 0.0000(8) 0.0144(9) 0.0032(8) C43 0.0586(14) 0.0347(12) 0.0429(13) 0.0039(10) 0.0291(11) 0.0078(11) C44 0.0794(18) 0.0417(14) 0.0274(11) -0.0016(10) 0.0145(11) 0.0127(13) C45 0.0621(15) 0.0410(13) 0.0263(10) -0.0072(10) -0.0017(10) 0.0062(12) C46 0.0441(11) 0.0242(10) 0.0241(9) -0.0033(8) -0.0004(8) 0.0051(9) C47 0.0303(10) 0.0296(11) 0.0588(14) -0.0042(11) 0.0142(10) -0.0011(9) C48 0.0401(13) 0.0388(15) 0.113(3) 0.0118(16) 0.0280(15) -0.0041(11) C49 0.0323(11) 0.0402(14) 0.0663(16) 0.0047(12) 0.0074(10) 0.0003(10) C50 0.0335(10) 0.0324(11) 0.0365(11) -0.0100(9) -0.0055(8) -0.0002(9) C51 0.0426(12) 0.0415(14) 0.0543(15) -0.0163(12) -0.0162(11) 0.0049(11) C52 0.0417(12) 0.0371(13) 0.0502(14) -0.0087(11) -0.0060(10) -0.0041(10) C53 0.0269(9) 0.0263(10) 0.0192(8) 0.0017(7) 0.0009(7) -0.0013(8) C54 0.0304(9) 0.0303(10) 0.0196(8) 0.0040(8) 0.0015(7) 0.0017(8) C55 0.0390(11) 0.0372(12) 0.0223(9) -0.0039(9) 0.0022(8) 0.0055(9) C56 0.0472(12) 0.0385(12) 0.0207(9) -0.0035(9) -0.0051(8) -0.0013(10) C57 0.0325(10) 0.0409(12) 0.0259(9) 0.0024(9) -0.0069(8) -0.0025(9) C58 0.0272(9) 0.0309(10) 0.0237(9) 0.0035(8) -0.0015(7) -0.0003(8) C59 0.0276(9) 0.0434(12) 0.0203(9) -0.0007(8) 0.0008(7) 0.0068(9) C60 0.0485(15) 0.0449(16) 0.086(2) 0.0049(15) -0.0219(14) 0.0181(13) C61 0.0343(12) 0.0503(16) 0.090(2) 0.0188(16) -0.0168(13) -0.0050(11) C62 0.0244(9) 0.0446(13) 0.0308(10) 0.0040(9) 0.0000(7) 0.0037(9) C63 0.0284(11) 0.0690(18) 0.0463(13) 0.0095(13) 0.0027(9) -0.0038(11) C64 0.0315(11) 0.0513(15) 0.0481(13) 0.0099(12) 0.0028(9) 0.0109(10) C65 0.0184(8) 0.0253(9) 0.0201(8) 0.0009(7) 0.0003(6) -0.0014(7) C66 0.0306(9) 0.0259(10) 0.0268(9) -0.0060(8) -0.0035(7) -0.0038(8) C67 0.0284(9) 0.0264(10) 0.0350(10) -0.0019(9) -0.0035(8) -0.0070(8) C68 0.0325(10) 0.0404(13) 0.0428(12) -0.0176(10) 0.0110(9) -0.0042(9) C69 0.0457(12) 0.0459(14) 0.0354(11) -0.0183(10) 0.0202(10) -0.0114(11) C70 0.0472(12) 0.0427(13) 0.0268(10) -0.0170(10) 0.0055(9) -0.0089(10) C71 0.0356(10) 0.0289(11) 0.0386(11) -0.0122(9) 0.0084(8) -0.0069(9) C72 0.0393(11) 0.0293(11) 0.0406(12) -0.0071(10) 0.0075(9) 0.0007(9) C73 0.0268(9) 0.0271(10) 0.0160(8) -0.0026(7) -0.0014(6) -0.0040(7) C74 0.0313(9) 0.0292(10) 0.0209(8) -0.0020(8) -0.0025(7) -0.0001(8) C75 0.0413(11) 0.0374(12) 0.0271(10) 0.0063(9) -0.0027(8) 0.0021(10) C76 0.0487(13) 0.0459(14) 0.0219(9) 0.0040(9) 0.0041(9) -0.0082(11) C77 0.0339(10) 0.0472(13) 0.0213(9) -0.0041(9) 0.0052(7) -0.0042(9) C78 0.0280(9) 0.0334(11) 0.0204(8) -0.0045(8) 0.0001(7) -0.0039(8) C79 0.0296(10) 0.0384(12) 0.0271(9) -0.0012(9) -0.0028(8) 0.0053(9) C80 0.0477(14) 0.0492(16) 0.0544(15) 0.0049(13) 0.0048(11) 0.0181(12) C81 0.0295(11) 0.0601(17) 0.0464(13) -0.0101(12) -0.0056(9) -0.0015(11) C82 0.0291(10) 0.0397(12) 0.0255(9) -0.0066(9) 0.0020(7) 0.0028(9) C83 0.0270(10) 0.0603(16) 0.0302(10) -0.0112(11) 0.0022(8) 0.0041(10) C84 0.0422(12) 0.0431(14) 0.0442(13) -0.0139(11) 0.0011(10) 0.0062(10) C85 0.0282(9) 0.0313(11) 0.0253(9) 0.0041(8) 0.0040(7) -0.0112(8) C86 0.0334(10) 0.0403(12) 0.0279(10) 0.0085(9) 0.0024(8) -0.0129(9) C87 0.0497(13) 0.0614(17) 0.0273(11) 0.0107(11) 0.0047(9) -0.0169(12) C88 0.0540(14) 0.0704(19) 0.0319(11) 0.0032(12) 0.0203(10) -0.0153(13) C89 0.0367(11) 0.0564(16) 0.0438(13) 0.0038(12) 0.0177(10) -0.0104(11) C90 0.0274(10) 0.0401(12) 0.0357(11) 0.0020(9) 0.0077(8) -0.0109(9) C91 0.0321(10) 0.0462(13) 0.0289(10) 0.0123(10) -0.0028(8) -0.0109(10) C92 0.0415(12) 0.0550(16) 0.0404(12) 0.0155(12) -0.0106(10) -0.0191(12) C93 0.0432(12) 0.0483(15) 0.0405(12) 0.0082(11) -0.0011(10) -0.0067(11) C94 0.0246(10) 0.0557(15) 0.0399(12) 0.0062(11) 0.0044(8) -0.0057(10) C95 0.0339(12) 0.078(2) 0.0701(19) 0.0090(17) 0.0130(12) 0.0081(13) C96 0.0372(13) 0.080(2) 0.0574(16) -0.0034(16) -0.0064(11) -0.0178(14) C97 0.0166(7) 0.0235(9) 0.0162(7) 0.0001(7) -0.0003(6) 0.0021(7) C98 0.0299(9) 0.0258(10) 0.0213(9) 0.0044(8) -0.0016(7) -0.0036(8) C99 0.0292(9) 0.0224(9) 0.0245(9) 0.0013(8) -0.0010(7) -0.0048(8) C100 0.0360(11) 0.0313(11) 0.0455(12) 0.0047(10) 0.0126(9) 0.0108(9) C101 0.0552(13) 0.0272(11) 0.0258(10) -0.0015(8) 0.0051(9) 0.0144(10) C102 0.0406(11) 0.0212(10) 0.0313(10) -0.0034(8) -0.0076(8) 0.0043(8) C103 0.0367(10) 0.0220(10) 0.0293(10) 0.0042(8) -0.0024(8) 0.0032(8) C104 0.0303(10) 0.0301(11) 0.0393(11) 0.0044(9) -0.0052(8) 0.0077(9) C105 0.0266(9) 0.0267(10) 0.0144(8) 0.0021(7) -0.0024(6) -0.0039(7) C106 0.0266(9) 0.0344(11) 0.0196(8) 0.0061(8) -0.0025(7) -0.0043(8) C107 0.0335(10) 0.0448(13) 0.0237(9) 0.0031(9) -0.0052(8) -0.0136(9) C108 0.0470(12) 0.0429(13) 0.0208(9) -0.0043(9) -0.0045(8) -0.0136(10) C109 0.0386(11) 0.0407(12) 0.0212(9) -0.0050(9) 0.0047(8) -0.0036(9) C110 0.0292(9) 0.0301(10) 0.0182(8) 0.0015(8) 0.0000(7) -0.0028(8) C111 0.0242(9) 0.0508(14) 0.0233(9) 0.0069(9) 0.0011(7) -0.0023(9) C112 0.0273(10) 0.0620(17) 0.0455(13) 0.0173(12) 0.0024(9) -0.0069(11) C113 0.0326(11) 0.0510(15) 0.0446(13) -0.0034(11) 0.0074(9) 0.0022(10) C114 0.0263(9) 0.0369(11) 0.0227(9) -0.0019(8) 0.0015(7) -0.0008(8) C115 0.0348(11) 0.0436(13) 0.0383(12) -0.0066(10) 0.0056(9) 0.0052(10) C116 0.0355(11) 0.0442(13) 0.0352(11) 0.0031(10) 0.0040(8) -0.0077(10) C117 0.0284(9) 0.0215(9) 0.0142(8) -0.0017(7) -0.0012(6) -0.0030(7) C118 0.0300(9) 0.0225(9) 0.0247(9) -0.0040(8) 0.0043(7) -0.0018(8) C119 0.0468(12) 0.0373(12) 0.0230(9) -0.0068(9) 0.0101(8) -0.0015(10) C120 0.0570(13) 0.0405(13) 0.0165(9) -0.0038(9) -0.0010(8) -0.0005(11) C121 0.0390(11) 0.0362(12) 0.0232(9) -0.0008(9) -0.0107(8) 0.0001(9) C122 0.0279(9) 0.0264(10) 0.0212(9) -0.0016(7) -0.0033(7) -0.0012(8) C123 0.0289(10) 0.0270(10) 0.0366(11) -0.0056(9) 0.0060(8) 0.0004(8) C124 0.0349(11) 0.0310(12) 0.0751(18) -0.0049(12) 0.0054(11) 0.0027(10) C125 0.0340(11) 0.0460(14) 0.0456(13) -0.0119(11) 0.0148(9) -0.0027(10) C126 0.0239(9) 0.0442(13) 0.0295(10) -0.0004(9) -0.0015(7) -0.0003(9) C127 0.0299(10) 0.0499(14) 0.0437(12) -0.0056(11) -0.0022(9) 0.0060(10) C128 0.0353(12) 0.0530(16) 0.0547(15) 0.0057(13) 0.0040(10) -0.0071(11) N1 0.0244(7) 0.0251(8) 0.0175(7) 0.0019(6) 0.0008(5) 0.0021(6) N2 0.0238(7) 0.0259(8) 0.0200(7) 0.0006(6) -0.0002(6) 0.0017(6) N3 0.0222(7) 0.0212(8) 0.0217(7) 0.0012(6) 0.0016(5) -0.0012(6) N4 0.0220(7) 0.0224(8) 0.0216(7) 0.0019(6) 0.0012(5) -0.0002(6) N5 0.0217(7) 0.0220(8) 0.0197(7) -0.0019(6) 0.0001(5) -0.0023(6) N6 0.0208(7) 0.0275(8) 0.0244(7) 0.0013(7) -0.0010(6) -0.0068(6) N7 0.0220(7) 0.0227(8) 0.0166(7) 0.0010(6) -0.0008(5) -0.0015(6) N8 0.0206(7) 0.0223(8) 0.0167(7) -0.0001(6) -0.0005(5) -0.0012(6) S1 0.0234(2) 0.0252(2) 0.0356(2) -0.0060(2) 0.00082(17) 0.00179(18) S2 0.0242(2) 0.0313(2) 0.0242(2) 0.00470(19) -0.00032(16) 0.00358(18) S3 0.0216(2) 0.0231(2) 0.0320(2) -0.00375(19) -0.00058(16) 0.00080(17) S4 0.0252(2) 0.0303(2) 0.0254(2) -0.00535(19) 0.00172(16) -0.00753(18) S5 0.0315(2) 0.0358(3) 0.0232(2) 0.0052(2) -0.00153(17) -0.0129(2) S6 0.0259(2) 0.0275(2) 0.0267(2) -0.00503(19) 0.00466(16) -0.00793(18) Ni1 0.02323(15) 0.02222(16) 0.02246(15) -0.00056(13) 0.00047(11) 0.00137(12) Ni2 0.02110(14) 0.01945(16) 0.02248(15) 0.00041(12) 0.00102(11) -0.00111(12) Ni3 0.02576(15) 0.02623(17) 0.01984(15) -0.00589(13) 0.00450(12) -0.00746(13) Ni4 0.02255(15) 0.01997(16) 0.01847(14) 0.00073(12) -0.00128(11) -0.00029(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.361(2) . ? C1 N2 1.366(2) . ? C1 Ni1 1.899(2) . ? C2 C3 1.341(3) . ? C2 N1 1.385(3) . ? C3 N2 1.382(3) . ? C4 C5 1.413(3) . ? C4 C8 1.436(3) . ? C4 Ni1 2.116(2) . ? C5 C6 1.396(3) . ? C5 Ni1 2.182(2) . ? C6 C7 1.435(3) . ? C6 Ni1 2.118(2) . ? C7 C8 1.391(3) . ? C7 Ni1 2.135(2) . ? C8 Ni1 2.169(2) . ? C9 C10 1.400(3) . ? C9 C14 1.398(3) . ? C9 N1 1.445(2) . ? C10 C11 1.395(3) . ? C10 C15 1.514(3) . ? C11 C12 1.375(3) . ? C12 C13 1.383(3) . ? C13 C14 1.396(3) . ? C14 C18 1.515(3) . ? C15 C16 1.527(3) . ? C15 C17 1.531(3) . ? C18 C19 1.533(3) . ? C18 C20 1.528(3) . ? C21 C22 1.394(3) . ? C21 C26 1.395(3) . ? C21 N2 1.444(2) . ? C22 C23 1.398(3) . ? C22 C27 1.520(3) . ? C23 C24 1.374(4) . ? C24 C25 1.382(3) . ? C25 C26 1.393(3) . ? C26 C30 1.514(3) . ? C27 C28 1.519(4) . ? C27 C29 1.538(4) . ? C30 C31 1.527(3) . ? C30 C32 1.526(3) . ? C33 N3 1.369(2) . ? C33 N4 1.367(2) . ? C33 Ni2 1.8809(19) . ? C34 C35 1.340(3) . ? C34 N3 1.387(2) . ? C35 N4 1.387(3) . ? C36 C37 1.386(3) . ? C36 C40 1.429(3) . ? C36 Ni2 2.170(2) . ? C37 C38 1.439(3) . ? C37 Ni2 2.133(2) . ? C38 C39 1.397(3) . ? C38 Ni2 2.095(2) . ? C39 C40 1.410(3) . ? C39 Ni2 2.167(2) . ? C40 Ni2 2.115(2) . ? C41 C42 1.403(3) . ? C41 C46 1.393(3) . ? C41 N3 1.450(2) . ? C42 C43 1.402(3) . ? C42 C47 1.511(3) . ? C43 C44 1.372(4) . ? C44 C45 1.364(4) . ? C45 C46 1.399(3) . ? C46 C50 1.510(3) . ? C47 C48 1.522(3) . ? C47 C49 1.530(3) . ? C50 C51 1.528(3) . ? C50 C52 1.536(3) . ? C53 C54 1.401(3) . ? C53 C58 1.399(3) . ? C53 N4 1.450(2) . ? C54 C55 1.389(3) . ? C54 C59 1.520(3) . ? C55 C56 1.384(3) . ? C56 C57 1.376(3) . ? C57 C58 1.397(3) . ? C58 C62 1.523(3) . ? C59 C60 1.501(3) . ? C59 C61 1.513(4) . ? C62 C63 1.532(3) . ? C62 C64 1.524(3) . ? C65 N5 1.367(2) . ? C65 N6 1.365(2) . ? C65 Ni3 1.8755(19) . ? C66 C67 1.339(3) . ? C66 N5 1.390(3) . ? C67 N6 1.385(3) . ? C68 C69 1.429(4) . ? C68 C72 1.422(3) . ? C68 Ni3 2.132(2) . ? C69 C70 1.396(3) . ? C69 Ni3 2.184(2) . ? C70 C71 1.434(3) . ? C70 Ni3 2.140(2) . ? C71 C72 1.402(3) . ? C71 Ni3 2.098(2) . ? C72 Ni3 2.176(2) . ? C73 C74 1.404(3) . ? C73 C78 1.400(3) . ? C73 N5 1.448(2) . ? C74 C75 1.391(3) . ? C74 C79 1.520(3) . ? C75 C76 1.380(3) . ? C76 C77 1.372(3) . ? C77 C78 1.398(3) . ? C78 C82 1.515(3) . ? C79 C80 1.532(3) . ? C79 C81 1.528(3) . ? C82 C83 1.531(3) . ? C82 C84 1.526(3) . ? C85 C86 1.398(3) . ? C85 C90 1.402(3) . ? C85 N6 1.445(2) . ? C86 C87 1.396(3) . ? C86 C91 1.517(3) . ? C87 C88 1.382(4) . ? C88 C89 1.380(4) . ? C89 C90 1.393(3) . ? C90 C94 1.517(3) . ? C91 C92 1.527(3) . ? C91 C93 1.526(4) . ? C94 C95 1.527(4) . ? C94 C96 1.536(4) . ? C97 N7 1.367(2) . ? C97 N8 1.366(2) . ? C97 Ni4 1.8870(19) . ? C98 C99 1.347(3) . ? C98 N7 1.386(3) . ? C99 N8 1.385(2) . ? C100 C101 1.431(3) . ? C100 C104 1.413(3) . ? C100 Ni4 2.109(2) . ? C101 C102 1.383(3) . ? C101 Ni4 2.159(2) . ? C102 C103 1.443(3) . ? C102 Ni4 2.107(2) . ? C103 C104 1.393(3) . ? C103 Ni4 2.102(2) . ? C104 Ni4 2.189(2) . ? C105 C106 1.409(3) . ? C105 C110 1.395(3) . ? C105 N7 1.446(2) . ? C106 C107 1.389(3) . ? C106 C111 1.517(3) . ? C107 C108 1.379(3) . ? C108 C109 1.379(3) . ? C109 C110 1.400(3) . ? C110 C114 1.520(3) . ? C111 C112 1.526(3) . ? C111 C113 1.532(4) . ? C114 C115 1.531(3) . ? C114 C116 1.533(3) . ? C117 C118 1.402(3) . ? C117 C122 1.400(3) . ? C117 N8 1.448(2) . ? C118 C119 1.390(3) . ? C118 C123 1.522(3) . ? C119 C120 1.376(3) . ? C120 C121 1.378(3) . ? C121 C122 1.400(3) . ? C122 C126 1.514(3) . ? C123 C124 1.527(3) . ? C123 C125 1.530(3) . ? C126 C127 1.526(3) . ? C126 C128 1.531(3) . ? S1 S2 2.0561(7) . ? S1 Ni1 2.1936(6) . ? S2 S3 2.0522(7) . ? S3 Ni2 2.1748(5) . ? S4 S5 2.0610(7) . ? S4 Ni3 2.1875(6) . ? S5 S6 2.0503(7) . ? S6 Ni4 2.1761(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 102.68(16) . . ? N1 C1 Ni1 128.88(13) . . ? N2 C1 Ni1 128.42(14) . . ? C3 C2 N1 106.59(17) . . ? C2 C3 N2 106.54(17) . . ? C5 C4 C8 108.89(18) . . ? C5 C4 Ni1 73.34(12) . . ? C8 C4 Ni1 72.41(12) . . ? C4 C5 Ni1 68.31(12) . . ? C6 C5 C4 106.98(19) . . ? C6 C5 Ni1 68.58(12) . . ? C5 C6 C7 108.61(19) . . ? C5 C6 Ni1 73.55(12) . . ? C7 C6 Ni1 70.95(12) . . ? C6 C7 Ni1 69.63(12) . . ? C8 C7 C6 108.32(18) . . ? C8 C7 Ni1 72.44(12) . . ? C4 C8 Ni1 68.46(12) . . ? C7 C8 C4 106.83(19) . . ? C7 C8 Ni1 69.85(12) . . ? C10 C9 N1 118.20(17) . . ? C14 C9 C10 123.68(17) . . ? C14 C9 N1 117.98(16) . . ? C9 C10 C15 122.77(18) . . ? C11 C10 C9 116.67(19) . . ? C11 C10 C15 120.49(19) . . ? C12 C11 C10 121.4(2) . . ? C11 C12 C13 120.31(19) . . ? C12 C13 C14 121.32(19) . . ? C9 C14 C18 122.12(16) . . ? C13 C14 C9 116.60(18) . . ? C13 C14 C18 121.23(18) . . ? C10 C15 C16 113.0(2) . . ? C10 C15 C17 110.71(19) . . ? C16 C15 C17 109.30(19) . . ? C14 C18 C19 113.08(17) . . ? C14 C18 C20 110.80(17) . . ? C20 C18 C19 109.92(17) . . ? C22 C21 C26 123.43(18) . . ? C22 C21 N2 117.47(18) . . ? C26 C21 N2 119.01(17) . . ? C21 C22 C23 117.0(2) . . ? C21 C22 C27 122.58(19) . . ? C23 C22 C27 120.4(2) . . ? C24 C23 C22 121.0(2) . . ? C23 C24 C25 120.6(2) . . ? C24 C25 C26 121.0(2) . . ? C21 C26 C30 121.36(17) . . ? C25 C26 C21 117.03(19) . . ? C25 C26 C30 121.55(19) . . ? C22 C27 C29 110.9(2) . . ? C28 C27 C22 112.1(2) . . ? C28 C27 C29 109.8(2) . . ? C26 C30 C31 110.70(16) . . ? C26 C30 C32 113.23(17) . . ? C32 C30 C31 110.06(18) . . ? N3 C33 Ni2 129.40(13) . . ? N4 C33 N3 103.36(16) . . ? N4 C33 Ni2 127.00(14) . . ? C35 C34 N3 106.88(17) . . ? C34 C35 N4 106.91(17) . . ? C37 C36 C40 107.00(19) . . ? C37 C36 Ni2 69.75(12) . . ? C40 C36 Ni2 68.43(12) . . ? C36 C37 C38 108.11(19) . . ? C36 C37 Ni2 72.68(13) . . ? C38 C37 Ni2 68.71(12) . . ? C37 C38 Ni2 71.52(12) . . ? C39 C38 C37 108.59(19) . . ? C39 C38 Ni2 73.65(12) . . ? C38 C39 C40 106.65(19) . . ? C38 C39 Ni2 68.11(11) . . ? C40 C39 Ni2 68.80(11) . . ? C36 C40 Ni2 72.63(12) . . ? C39 C40 C36 109.29(19) . . ? C39 C40 Ni2 72.77(12) . . ? C42 C41 N3 117.85(18) . . ? C46 C41 C42 122.63(19) . . ? C46 C41 N3 119.41(17) . . ? C41 C42 C47 121.55(19) . . ? C43 C42 C41 116.7(2) . . ? C43 C42 C47 121.7(2) . . ? C44 C43 C42 121.5(2) . . ? C45 C44 C43 120.5(2) . . ? C44 C45 C46 121.2(2) . . ? C41 C46 C45 117.5(2) . . ? C41 C46 C50 123.45(18) . . ? C45 C46 C50 118.9(2) . . ? C42 C47 C48 113.3(2) . . ? C42 C47 C49 111.11(19) . . ? C48 C47 C49 109.3(2) . . ? C46 C50 C51 113.5(2) . . ? C46 C50 C52 108.99(19) . . ? C51 C50 C52 110.10(19) . . ? C54 C53 N4 119.55(16) . . ? C58 C53 C54 122.94(18) . . ? C58 C53 N4 117.50(17) . . ? C53 C54 C59 122.68(18) . . ? C55 C54 C53 116.52(18) . . ? C55 C54 C59 120.80(18) . . ? C56 C55 C54 122.1(2) . . ? C57 C56 C55 119.9(2) . . ? C56 C57 C58 120.86(19) . . ? C53 C58 C62 122.80(18) . . ? C57 C58 C53 117.62(19) . . ? C57 C58 C62 119.56(18) . . ? C60 C59 C54 113.0(2) . . ? C60 C59 C61 108.9(2) . . ? C61 C59 C54 110.90(18) . . ? C58 C62 C63 112.7(2) . . ? C58 C62 C64 109.96(18) . . ? C64 C62 C63 109.72(19) . . ? N5 C65 Ni3 130.49(14) . . ? N6 C65 N5 103.73(16) . . ? N6 C65 Ni3 125.18(13) . . ? C67 C66 N5 107.32(17) . . ? C66 C67 N6 106.61(18) . . ? C69 C68 Ni3 72.63(14) . . ? C72 C68 C69 108.6(2) . . ? C72 C68 Ni3 72.40(13) . . ? C68 C69 Ni3 68.72(12) . . ? C70 C69 C68 107.4(2) . . ? C70 C69 Ni3 69.48(12) . . ? C69 C70 C71 108.1(2) . . ? C69 C70 Ni3 72.87(12) . . ? C71 C70 Ni3 68.63(12) . . ? C70 C71 Ni3 71.82(12) . . ? C72 C71 C70 108.56(19) . . ? C72 C71 Ni3 73.89(13) . . ? C68 C72 Ni3 69.07(14) . . ? C71 C72 C68 106.9(2) . . ? C71 C72 Ni3 67.85(13) . . ? C74 C73 N5 118.35(16) . . ? C78 C73 C74 121.98(18) . . ? C78 C73 N5 119.45(17) . . ? C73 C74 C79 122.32(18) . . ? C75 C74 C73 117.34(19) . . ? C75 C74 C79 120.22(19) . . ? C76 C75 C74 121.8(2) . . ? C77 C76 C75 119.8(2) . . ? C76 C77 C78 121.3(2) . . ? C73 C78 C82 123.22(18) . . ? C77 C78 C73 117.74(19) . . ? C77 C78 C82 119.01(18) . . ? C74 C79 C80 113.8(2) . . ? C74 C79 C81 110.17(18) . . ? C81 C79 C80 110.1(2) . . ? C78 C82 C83 111.6(2) . . ? C78 C82 C84 110.11(17) . . ? C84 C82 C83 110.26(18) . . ? C86 C85 C90 122.78(19) . . ? C86 C85 N6 119.61(18) . . ? C90 C85 N6 117.58(18) . . ? C85 C86 C91 121.53(19) . . ? C87 C86 C85 117.2(2) . . ? C87 C86 C91 121.2(2) . . ? C88 C87 C86 121.0(2) . . ? C89 C88 C87 120.6(2) . . ? C88 C89 C90 120.8(2) . . ? C85 C90 C94 121.94(19) . . ? C89 C90 C85 117.5(2) . . ? C89 C90 C94 120.5(2) . . ? C86 C91 C92 112.7(2) . . ? C86 C91 C93 109.82(18) . . ? C93 C91 C92 110.3(2) . . ? C90 C94 C95 113.4(2) . . ? C90 C94 C96 110.7(2) . . ? C95 C94 C96 109.7(2) . . ? N7 C97 Ni4 126.58(13) . . ? N8 C97 N7 103.36(15) . . ? N8 C97 Ni4 129.96(13) . . ? C99 C98 N7 107.00(16) . . ? C98 C99 N8 106.44(17) . . ? C101 C100 Ni4 72.29(12) . . ? C104 C100 C101 109.1(2) . . ? C104 C100 Ni4 73.89(12) . . ? C100 C101 Ni4 68.54(12) . . ? C102 C101 C100 106.91(19) . . ? C102 C101 Ni4 69.06(12) . . ? C101 C102 C103 108.20(19) . . ? C101 C102 Ni4 73.13(13) . . ? C103 C102 Ni4 69.77(12) . . ? C102 C103 Ni4 70.15(11) . . ? C104 C103 C102 108.56(19) . . ? C104 C103 Ni4 74.48(12) . . ? C100 C104 Ni4 67.78(12) . . ? C103 C104 C100 106.65(19) . . ? C103 C104 Ni4 67.70(11) . . ? C106 C105 N7 118.08(16) . . ? C110 C105 C106 122.31(17) . . ? C110 C105 N7 119.61(16) . . ? C105 C106 C111 121.59(18) . . ? C107 C106 C105 117.07(19) . . ? C107 C106 C111 121.33(18) . . ? C108 C107 C106 121.83(19) . . ? C107 C108 C109 119.94(19) . . ? C108 C109 C110 121.0(2) . . ? C105 C110 C109 117.66(18) . . ? C105 C110 C114 123.32(17) . . ? C109 C110 C114 119.01(18) . . ? C106 C111 C112 113.6(2) . . ? C106 C111 C113 110.82(17) . . ? C112 C111 C113 108.72(19) . . ? C110 C114 C115 113.44(18) . . ? C110 C114 C116 109.12(16) . . ? C115 C114 C116 108.38(18) . . ? C118 C117 N8 119.40(16) . . ? C122 C117 C118 122.78(16) . . ? C122 C117 N8 117.74(16) . . ? C117 C118 C123 122.40(17) . . ? C119 C118 C117 116.95(18) . . ? C119 C118 C123 120.47(18) . . ? C120 C119 C118 121.76(19) . . ? C119 C120 C121 120.24(18) . . ? C120 C121 C122 120.89(19) . . ? C117 C122 C121 117.31(18) . . ? C117 C122 C126 122.48(16) . . ? C121 C122 C126 119.99(17) . . ? C118 C123 C124 109.47(17) . . ? C118 C123 C125 113.00(18) . . ? C124 C123 C125 110.03(19) . . ? C122 C126 C127 113.21(18) . . ? C122 C126 C128 108.41(19) . . ? C127 C126 C128 109.64(18) . . ? C1 N1 C2 112.07(15) . . ? C1 N1 C9 126.58(16) . . ? C2 N1 C9 121.34(15) . . ? C1 N2 C3 112.11(15) . . ? C1 N2 C21 125.81(16) . . ? C3 N2 C21 121.75(16) . . ? C33 N3 C34 111.39(15) . . ? C33 N3 C41 125.88(16) . . ? C34 N3 C41 122.40(16) . . ? C33 N4 C35 111.46(16) . . ? C33 N4 C53 125.62(16) . . ? C35 N4 C53 122.08(16) . . ? C65 N5 C66 110.76(16) . . ? C65 N5 C73 126.63(16) . . ? C66 N5 C73 122.31(15) . . ? C65 N6 C67 111.55(16) . . ? C65 N6 C85 123.59(17) . . ? C67 N6 C85 124.01(16) . . ? C97 N7 C98 111.37(15) . . ? C97 N7 C105 124.41(16) . . ? C98 N7 C105 124.13(15) . . ? C97 N8 C99 111.81(14) . . ? C97 N8 C117 125.30(16) . . ? C99 N8 C117 122.64(15) . . ? S2 S1 Ni1 110.77(3) . . ? S3 S2 S1 111.58(3) . . ? S2 S3 Ni2 113.07(3) . . ? S5 S4 Ni3 110.92(3) . . ? S6 S5 S4 111.27(3) . . ? S5 S6 Ni4 111.64(3) . . ? C1 Ni1 C4 101.16(8) . . ? C1 Ni1 C5 123.18(8) . . ? C1 Ni1 C6 160.95(8) . . ? C1 Ni1 C7 147.69(8) . . ? C1 Ni1 C8 112.94(8) . . ? C1 Ni1 S1 94.86(6) . . ? C4 Ni1 C5 38.36(8) . . ? C4 Ni1 C6 64.47(8) . . ? C4 Ni1 C7 64.55(8) . . ? C4 Ni1 C8 39.13(8) . . ? C4 Ni1 S1 161.55(6) . . ? C5 Ni1 S1 123.95(6) . . ? C6 Ni1 C5 37.87(8) . . ? C6 Ni1 C7 39.42(8) . . ? C6 Ni1 C8 64.60(9) . . ? C6 Ni1 S1 97.81(6) . . ? C7 Ni1 C5 64.35(8) . . ? C7 Ni1 C8 37.71(9) . . ? C7 Ni1 S1 105.59(6) . . ? C8 Ni1 C5 64.39(8) . . ? C8 Ni1 S1 139.62(6) . . ? C33 Ni2 C36 114.02(8) . . ? C33 Ni2 C37 146.63(9) . . ? C33 Ni2 C38 165.84(8) . . ? C33 Ni2 C39 127.72(8) . . ? C33 Ni2 C40 105.04(8) . . ? C33 Ni2 S3 89.12(5) . . ? C36 Ni2 S3 140.06(7) . . ? C37 Ni2 C36 37.57(9) . . ? C37 Ni2 C39 64.77(8) . . ? C37 Ni2 S3 107.05(6) . . ? C38 Ni2 C36 64.82(8) . . ? C38 Ni2 C37 39.77(9) . . ? C38 Ni2 C39 38.24(9) . . ? C38 Ni2 C40 64.66(8) . . ? C38 Ni2 S3 100.20(6) . . ? C39 Ni2 C36 64.55(8) . . ? C39 Ni2 S3 126.74(6) . . ? C40 Ni2 C36 38.94(9) . . ? C40 Ni2 C37 64.40(8) . . ? C40 Ni2 C39 38.43(8) . . ? C40 Ni2 S3 164.35(6) . . ? C65 Ni3 C68 105.84(8) . . ? C65 Ni3 C69 114.35(8) . . ? C65 Ni3 C70 146.47(9) . . ? C65 Ni3 C71 167.13(9) . . ? C65 Ni3 C72 128.99(8) . . ? C65 Ni3 S4 88.16(6) . . ? C68 Ni3 C69 38.65(10) . . ? C68 Ni3 C70 64.42(9) . . ? C68 Ni3 C72 38.52(9) . . ? C68 Ni3 S4 165.31(7) . . ? C69 Ni3 S4 138.77(7) . . ? C70 Ni3 C69 37.65(9) . . ? C70 Ni3 C72 64.50(9) . . ? C70 Ni3 S4 106.18(7) . . ? C71 Ni3 C68 64.89(9) . . ? C71 Ni3 C69 64.66(9) . . ? C71 Ni3 C70 39.55(9) . . ? C71 Ni3 C72 38.26(9) . . ? C71 Ni3 S4 100.57(6) . . ? C72 Ni3 C69 64.14(9) . . ? C72 Ni3 S4 128.11(6) . . ? C97 Ni4 C100 101.04(8) . . ? C97 Ni4 C101 113.15(8) . . ? C97 Ni4 C102 147.93(8) . . ? C97 Ni4 C103 160.40(8) . . ? C97 Ni4 C104 122.76(8) . . ? C97 Ni4 S6 95.42(5) . . ? C100 Ni4 C101 39.16(9) . . ? C100 Ni4 C104 38.34(9) . . ? C100 Ni4 S6 162.98(7) . . ? C101 Ni4 C104 64.43(8) . . ? C101 Ni4 S6 135.63(7) . . ? C102 Ni4 C100 64.86(9) . . ? C102 Ni4 C101 37.80(9) . . ? C102 Ni4 C104 64.77(8) . . ? C102 Ni4 S6 102.73(6) . . ? C103 Ni4 C100 64.61(9) . . ? C103 Ni4 C101 64.96(8) . . ? C103 Ni4 C102 40.08(8) . . ? C103 Ni4 C104 37.82(8) . . ? C103 Ni4 S6 98.37(6) . . ? S6 Ni4 C104 126.97(6) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -8 -7 -4 0.0492 -7.9891 -6.9873 -4.0448 -0.3642 0.4562 0.7771 7 9 4 0.0383 6.9921 8.9870 4.0349 0.4959 -0.5628 -0.6883 4 -11 -5 0.0477 3.9887 -10.9962 -4.9561 -0.6021 0.7358 -0.3221 8 -9 -3 0.0395 7.9823 -9.0016 -2.9315 -0.5188 0.5850 -0.7077 -7 8 -6 0.0487 -6.9795 8.0024 -6.0601 0.6728 -0.2507 0.6661 -7 -9 6 0.0325 -6.9978 -8.9882 5.9650 -0.7401 0.2525 0.6338 7 -8 6 0.0452 6.9795 -8.0024 6.0601 -0.6728 0.2507 -0.6661 -10 -2 12 0.0368 -9.9915 -1.9905 11.9339 -0.4258 -0.3048 0.8655 3 -3 22 0.0396 2.9805 -3.0036 22.0250 -0.7346 -0.5174 -0.3923 -3 -4 24 0.0348 -3.0113 -3.9974 23.9851 -0.8499 -0.5493 0.1550 -7 9 4 0.0328 -6.9845 9.0005 3.9383 0.4945 -0.6125 0.6096 1 -1 25 0.0322 0.9835 -1.0033 25.0082 -0.6763 -0.7206 -0.2271 10 -3 -12 0.0414 9.9881 -3.0063 -11.9265 0.0964 0.5623 -0.8558 6 -8 -14 0.0382 5.9925 -7.9990 -13.9467 -0.1845 0.8677 -0.4643 3 -5 -23 0.0482 3.0046 -4.9969 -22.9718 0.2326 0.9818 -0.1429 -5 -4 -19 0.0587 -4.9836 -3.9903 -19.0284 0.2000 0.7778 0.5750 3 6 -21 0.0501 3.0109 5.9958 -20.9881 0.9084 0.3532 -0.1753 -5 5 -19 0.0568 -4.9775 5.0039 -19.0418 0.7929 0.3143 0.5574 0 0 -25 0.0464 0.0142 0.0030 -24.9999 0.6105 0.7757 0.1364 10 1 -13 0.0391 9.9913 0.9913 -12.9324 0.3843 0.3873 -0.8581 _database_code_depnum_ccdc_archive 'CCDC 995935' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7-Se _audit_creation_date 2014-01-23 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _shelxl_version_number 2013-4 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C64 H82 N4 Ni2 Se3' _chemical_formula_sum 'C64 H82 N4 Ni2 Se3' _chemical_formula_weight 1261.63 _chemical_melting_point ? _chemical_oxdiff_formula 'C64 H82 N4 Ni2 Se' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.8208(6) _cell_length_b 18.4669(10) _cell_length_c 39.0547(10) _cell_angle_alpha 90 _cell_angle_beta 96.196(3) _cell_angle_gamma 90 _cell_volume 12060.6(8) _cell_formula_units_Z 8 _cell_measurement_reflns_used 15684 _cell_measurement_temperature 123.01(10) _cell_measurement_theta_max 73.2610 _cell_measurement_theta_min 3.5170 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 3.152 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour 'dark red' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 5216 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.953 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 43761 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.985 _diffrn_reflns_theta_min 3.566 _diffrn_ambient_temperature 123.01(10) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.953 _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0461342000 _diffrn_orient_matrix_UB_12 0.0412242000 _diffrn_orient_matrix_UB_13 -0.0301845000 _diffrn_orient_matrix_UB_21 -0.0418310000 _diffrn_orient_matrix_UB_22 -0.0708341000 _diffrn_orient_matrix_UB_23 -0.0126389000 _diffrn_orient_matrix_UB_31 -0.0677460000 _diffrn_orient_matrix_UB_32 0.0156714000 _diffrn_orient_matrix_UB_33 0.0225073000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 19930 _reflns_number_total 23312 _reflns_odcompleteness_completeness 98.55 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL-2013 (Sheldrick, 2008)' _computing_structure_solution 'SIR97 (Burla et al., 2007)' _refine_diff_density_max 2.756 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.078 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1315 _refine_ls_number_reflns 23312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0409 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+12.6020P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.1040 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.034) H3(0.033) H4(0.04) H5(0.041) H6(0.04) H7(0.041) H8(0.042) H11(0.044) H12(0.045) H13(0.037) H15(0.042) H16A(0.067) H16B(0.067) H16C(0.067) H17A(0.075) H17B(0.075) H17C(0.075) H18(0.033) H19A(0.054) H19B(0.054) H19C(0.054) H20A(0.058) H20B(0.058) H20C(0.058) H23(0.064) H24(0.069) H25(0.058) H27(0.061) H28A(0.101) H28B(0.101) H28C(0.101) H29A(0.098) H29B(0.098) H29C(0.098) H30(0.045) H31A(0.065) H31B(0.065) H31C(0.065) H32A(0.076) H32B(0.076) H32C(0.076) H34(0.033) H35(0.033) H36(0.047) H37(0.048) H38(0.043) H39(0.045) H40(0.047) H43(0.052) H44(0.059) H45(0.054) H47(0.044) H48A(0.085) H48B(0.085) H48C(0.085) H49A(0.065) H49B(0.065) H49C(0.065) H50(0.046) H51A(0.076) H51B(0.076) H51C(0.076) H52A(0.079) H52B(0.079) H52C(0.079) H55(0.044) H56(0.047) H57(0.042) H59(0.042) H60A(0.069) H60B(0.069) H60C(0.069) H61A(0.067) H61B(0.067) H61C(0.067) H62(0.039) H63A(0.099) H63B(0.099) H63C(0.099) H64A(0.089) H64B(0.089) H64C(0.089) H66(0.036) H67(0.036) H68(0.041) H69(0.042) H70(0.048) H71(0.051) H72(0.048) H75(0.05) H76(0.055) H77(0.047) H79(0.045) H80A(0.077) H80B(0.077) H80C(0.077) H81A(0.069) H81B(0.069) H81C(0.069) H82(0.038) H83A(0.067) H83B(0.067) H83C(0.067) H84A(0.059) H84B(0.059) H84C(0.059) H87(0.05) H88(0.053) H89(0.045) H91(0.04) H92A(0.065) H92B(0.065) H92C(0.065) H93A(0.074) H93B(0.074) H93C(0.074) H94(0.048) H95A(0.07) H95B(0.07) H95C(0.07) H96A(0.089) H96B(0.089) H96C(0.089) H98(0.046) H99(0.05) H100(0.046) H101(0.049) H102(0.044) H103(0.043) H104(0.042) H107(0.056) H108(0.059) H109(0.05) H111(0.056) H11A(0.103) H11B(0.103) H11C(0.103) H11D(0.098) H11E(0.098) H11F(0.098) H114(0.04) H11G(0.077) H11H(0.077) H11I(0.077) H11J(0.08) H11K(0.08) H11L(0.08) H119(0.065) H120(0.075) H121(0.067) H123(0.053) H12A(0.077) H12B(0.077) H12C(0.077) H12D(0.077) H12E(0.077) H12F(0.077) H126(0.062) H12G(0.12) H12H(0.12) H12I(0.12) H12J(0.105) H12K(0.105) H12L(0.105) Fixed X: H2(1.0711) H3(1.1217) H4(1.086) H5(0.9609) H6(0.8532) H7(0.9176) H8(1.0625) H11(1.0126) H12(0.8925) H13(0.8239) H15(1.1066) H16A(1.169) H16B(1.1116) H16C(1.0774) H17A(1.2196) H17B(1.1622) H17C(1.164) H18(0.8759) H19A(0.7453) H19B(0.7538) H19C(0.753) H20A(0.8591) H20B(0.8747) H20C(0.9435) H23(1.2379) H24(1.16) H25(1.0346) H27(1.1823) H28A(1.282) H28B(1.2052) H28C(1.279) H29A(1.3161) H29B(1.3147) H29C(1.2618) H30(0.9293) H31A(0.9156) H31B(0.9977) H31C(0.9944) H32A(0.849) H32B(0.9227) H32C(0.8885) H34(0.5752) H35(0.5684) H36(0.5165) H37(0.622) H38(0.5878) H39(0.456) H40(0.4203) H43(0.4533) H44(0.5665) H45(0.6829) H47(0.439) H48A(0.3149) H48B(0.3826) H48C(0.347) H49A(0.3406) H49B(0.3755) H49C(0.4261) H50(0.7157) H51A(0.7737) H51B(0.6802) H51C(0.7263) H52A(0.8403) H52B(0.7981) H52C(0.7904) H55(0.4065) H56(0.5065) H57(0.6346) H59(0.4236) H60A(0.2886) H60B(0.311) H60C(0.3386) H61A(0.3478) H61B(0.4376) H61C(0.3746) H62(0.697) H63A(0.7145) H63B(0.7958) H63C(0.7496) H64A(0.7997) H64B(0.7207) H64C(0.7493) H66(0.9936) H67(1.0215) H68(0.959) H69(0.8809) H70(0.967) H71(1.0921) H72(1.0946) H75(0.7793) H76(0.8693) H77(1.0022) H79(0.8205) H80A(0.6829) H80B(0.695) H80C(0.7245) H81A(0.749) H81B(0.8371) H81C(0.7672) H82(1.0968) H83A(1.1935) H83B(1.129) H83C(1.1274) H84A(1.1581) H84B(1.0892) H84C(1.0709) H87(0.9188) H88(1.0425) H89(1.1451) H91(0.852) H92A(0.7437) H92B(0.7903) H92C(0.8021) H93A(0.8124) H93B(0.8755) H93C(0.9039) H94(1.1309) H95A(1.2454) H95B(1.2234) H95C(1.1693) H96A(1.2481) H96B(1.1724) H96C(1.2227) H98(0.5045) H99(0.458) H100(0.6213) H101(0.4766) H102(0.4362) H103(0.5509) H104(0.6687) H107(0.6976) H108(0.6183) H109(0.5032) H111(0.6708) H11A(0.7029) H11B(0.6147) H11C(0.6826) H11D(0.8046) H11E(0.7893) H11F(0.7843) H114(0.4389) H11G(0.3562) H11H(0.4459) H11I(0.4008) H11J(0.319) H11K(0.3641) H11L(0.3841) H119(0.5147) H120(0.3859) H121(0.3056) H123(0.6194) H12A(0.6504) H12B(0.5755) H12C(0.5642) H12D(0.7097) H12E(0.6612) H12F(0.6394) H126(0.3657) H12G(0.2452) H12H(0.3128) H12I(0.2475) H12J(0.2475) H12K(0.2476) H12L(0.3147) Fixed Y: H2(0.5176) H3(0.5214) H4(0.2305) H5(0.1876) H6(0.1844) H7(0.2062) H8(0.2302) H11(0.3026) H12(0.3499) H13(0.4293) H15(0.3266) H16A(0.2319) H16B(0.2435) H16C(0.2159) H17A(0.355) H17B(0.4219) H17C(0.3745) H18(0.478) H19A(0.5156) H19B(0.4323) H19C(0.4868) H20A(0.5979) H20B(0.5726) H20C(0.5683) H23(0.336) H24(0.3531) H25(0.4009) H27(0.3733) H28A(0.2837) H28B(0.2538) H28C(0.2782) H29A(0.4124) H29B(0.4136) H29C(0.4682) H30(0.4363) H31A(0.5596) H31B(0.5451) H31C(0.556) H32A(0.4655) H32B(0.4573) H32C(0.3894) H34(-0.0336) H35(0.0125) H36(0.3108) H37(0.3705) H38(0.3519) H39(0.2891) H40(0.2507) H43(0.08) H44(0.0491) H45(0.0261) H47(0.1302) H48A(0.1452) H48B(0.1804) H48C(0.105) H49A(0.0412) H49B(-0.0046) H49C(0.0071) H50(0.0413) H51A(-0.0727) H51B(-0.0788) H51C(-0.0761) H52A(0.0418) H52B(0.0413) H52C(0.1091) H55(0.2051) H56(0.2704) H57(0.2666) H59(0.1002) H60A(0.1293) H60B(0.1763) H60C(0.2005) H61A(0.0212) H61B(0.02) H61C(0.0636) H62(0.1943) H63A(0.0884) H63B(0.1295) H63C(0.1341) H64A(0.2602) H64B(0.3059) H64C(0.268) H66(-0.0117) H67(-0.0459) H68(0.3411) H69(0.3415) H70(0.2833) H71(0.2389) H72(0.2914) H75(0.1944) H76(0.2375) H77(0.2071) H79(0.1196) H80A(0.1282) H80B(0.1442) H80C(0.2002) H81A(0.0132) H81B(0.0067) H81C(0.0222) H82(0.113) H83A(0.182) H83B(0.2338) H83C(0.2159) H84A(0.0607) H84B(0.0902) H84C(0.0307) H87(0.0328) H88(0.0636) H89(0.0901) H91(0.0412) H92A(0.0186) H92B(0.0874) H92C(0.0132) H93A(-0.0801) H93B(-0.0894) H93C(-0.076) H94(0.1012) H95A(0.165) H95B(0.152) H95C(0.2018) H96A(0.0329) H96B(-0.0148) H96C(0.0162) H98(0.482) H99(0.5156) H100(0.2242) H101(0.2514) H102(0.2069) H103(0.1359) H104(0.1565) H107(0.3331) H108(0.2401) H109(0.2104) H111(0.4401) H11A(0.529) H11B(0.5027) H11C(0.4746) H11D(0.448) H11E(0.3915) H11F(0.3675) H114(0.281) H11G(0.1851) H11H(0.1606) H11I(0.1798) H11J(0.3109) H11K(0.3137) H11L(0.3704) H119(0.4091) H120(0.3697) H121(0.3548) H123(0.4327) H12A(0.5489) H12B(0.5465) H12C(0.5472) H12D(0.44) H12E(0.3675) H12F(0.4322) H126(0.37) H12G(0.4345) H12H(0.4826) H12I(0.448) H12J(0.3034) H12K(0.3077) H12L(0.2642) Fixed Z: H2(0.8166) H3(0.8779) H4(0.8526) H5(0.8177) H6(0.8575) H7(0.9181) H8(0.9155) H11(0.7301) H12(0.7078) H13(0.7394) H15(0.8148) H16A(0.7883) H16B(0.7544) H16C(0.7878) H17A(0.7867) H17B(0.7864) H17C(0.7532) H18(0.8264) H19A(0.8086) H19B(0.8021) H19C(0.7713) H20A(0.8063) H20B(0.7693) H20C(0.7997) H23(0.9613) H24(1.0048) H25(0.9943) H27(0.8724) H28A(0.876) H28B(0.8906) H28C(0.9159) H29A(0.8796) H29B(0.9196) H29C(0.8964) H30(0.9139) H31A(0.9271) H31B(0.9127) H31C(0.9524) H32A(0.9573) H32B(0.9853) H32C(0.9646) H34(0.8559) H35(0.797) H36(0.8078) H37(0.8474) H38(0.9084) H39(0.9058) H40(0.8446) H43(0.9667) H44(1.001) H45(0.9779) H47(0.88) H48A(0.9012) H48B(0.9266) H48C(0.9353) H49A(0.8664) H49B(0.8984) H49C(0.8674) H50(0.8898) H51A(0.9046) H51B(0.8999) H51C(0.937) H52A(0.9231) H52B(0.957) H52C(0.9328) H55(0.7317) H56(0.7104) H57(0.7376) H59(0.8084) H60A(0.7938) H60B(0.7628) H60C(0.8006) H61A(0.7705) H61B(0.7633) H61C(0.7389) H62(0.8184) H63A(0.7874) H63B(0.7957) H63C(0.7587) H64A(0.7979) H64B(0.7943) H64C(0.7619) H66(1.0612) H67(1.1221) H68(1.159) H69(1.0995) H70(1.0592) H71(1.0947) H72(1.154) H75(1.0072) H76(0.9718) H77(0.9818) H79(1.088) H80A(1.0742) H80B(1.0356) H80C(1.0644) H81A(1.073) H81B(1.0637) H81C(1.0347) H82(1.0545) H83A(1.0303) H83B(1.043) H83C(1.0037) H84A(1.009) H84B(0.9824) H84C(1.0091) H87(1.2381) H88(1.2641) H89(1.2318) H91(1.1495) H92A(1.1813) H92B(1.1959) H92C(1.2153) H93A(1.155) H93B(1.1873) H93C(1.1509) H94(1.1403) H95A(1.1631) H95B(1.2006) H95C(1.1752) H96A(1.1535) H96B(1.1572) H96C(1.1901) H98(1.0423) H99(1.0974) H100(1.1861) H101(1.1717) H102(1.1114) H103(1.0921) H104(1.1358) H107(0.9839) H108(0.962) H109(0.9864) H111(1.0573) H11A(1.0177) H11B(1.0083) H11C(0.9872) H11D(1.0463) H11E(1.0164) H11F(1.0546) H114(1.0617) H11G(1.0413) H11H(1.0443) H11I(1.0082) H11J(1.0284) H11K(0.9954) H11L(1.0249) H119(1.2291) H120(1.229) H121(1.1784) H123(1.1555) H12A(1.1772) H12B(1.1978) H12C(1.1574) H12D(1.205) H12E(1.2049) H12F(1.2281) H126(1.0941) H12G(1.0849) H12H(1.104) H12I(1.1247) H12J(1.0907) H12K(1.1308) H12L(1.1148) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.00954(17) 0.38644(16) 0.85864(7) 0.0228(5) Uani 1 1 d . . . . . C2 C 1.06035(19) 0.48440(17) 0.83340(7) 0.0283(6) Uani 1 1 d . . . . . H2 H 1.0711 0.5176 0.8166 0.034 Uiso 1 1 calc R U . . . C3 C 1.08805(18) 0.48661(17) 0.86695(7) 0.0276(6) Uani 1 1 d . . . . . H3 H 1.1217 0.5214 0.8779 0.033 Uiso 1 1 calc R U . . . C4 C 1.0380(2) 0.21926(18) 0.86122(9) 0.0334(7) Uani 1 1 d . . . . . H4 H 1.0860 0.2305 0.8526 0.040 Uiso 1 1 calc R U . . . C5 C 0.9670(2) 0.19753(18) 0.84120(8) 0.0340(7) Uani 1 1 d . . . . . H5 H 0.9609 0.1876 0.8177 0.041 Uiso 1 1 calc R U . . . C6 C 0.9071(2) 0.19378(17) 0.86380(9) 0.0330(7) Uani 1 1 d . . . . . H6 H 0.8532 0.1844 0.8575 0.040 Uiso 1 1 calc R U . . . C7 C 0.9436(2) 0.20697(17) 0.89822(8) 0.0338(7) Uani 1 1 d . . . . . H7 H 0.9176 0.2062 0.9181 0.041 Uiso 1 1 calc R U . . . C8 C 1.0245(2) 0.22117(18) 0.89686(8) 0.0349(7) Uani 1 1 d . . . . . H8 H 1.0625 0.2302 0.9155 0.042 Uiso 1 1 calc R U . . . C9 C 0.97685(18) 0.40089(16) 0.79499(7) 0.0241(6) Uani 1 1 d . . . . . C10 C 1.02037(19) 0.35305(17) 0.77615(7) 0.0290(6) Uani 1 1 d . . . . . C11 C 0.9860(2) 0.3347(2) 0.74326(8) 0.0366(7) Uani 1 1 d . . . . . H11 H 1.0126 0.3026 0.7301 0.044 Uiso 1 1 calc R U . . . C12 C 0.9140(2) 0.3630(2) 0.72988(8) 0.0376(7) Uani 1 1 d . . . . . H12 H 0.8925 0.3499 0.7078 0.045 Uiso 1 1 calc R U . . . C13 C 0.8728(2) 0.41071(18) 0.74884(7) 0.0305(6) Uani 1 1 d . . . . . H13 H 0.8239 0.4293 0.7394 0.037 Uiso 1 1 calc R U . . . C14 C 0.90392(18) 0.43116(16) 0.78204(7) 0.0242(6) Uani 1 1 d . . . . . C15 C 1.1023(2) 0.32495(19) 0.78963(8) 0.0351(7) Uani 1 1 d . . . . . H15 H 1.1066 0.3266 0.8148 0.042 Uiso 1 1 calc R U . . . C16 C 1.1164(2) 0.2468(2) 0.77906(10) 0.0448(9) Uani 1 1 d . . . . . H16A H 1.1690 0.2319 0.7883 0.067 Uiso 1 1 calc R U . . . H16B H 1.1116 0.2435 0.7544 0.067 Uiso 1 1 calc R U . . . H16C H 1.0774 0.2159 0.7878 0.067 Uiso 1 1 calc R U . . . C17 C 1.1682(2) 0.3737(2) 0.77786(11) 0.0501(9) Uani 1 1 d . . . . . H17A H 1.2196 0.3550 0.7867 0.075 Uiso 1 1 calc R U . . . H17B H 1.1622 0.4219 0.7864 0.075 Uiso 1 1 calc R U . . . H17C H 1.1640 0.3745 0.7532 0.075 Uiso 1 1 calc R U . . . C18 C 0.86052(19) 0.48644(17) 0.80184(7) 0.0276(6) Uani 1 1 d . . . . . H18 H 0.8759 0.4780 0.8264 0.033 Uiso 1 1 calc R U . . . C19 C 0.7697(2) 0.4797(2) 0.79538(8) 0.0362(7) Uani 1 1 d . . . . . H19A H 0.7453 0.5156 0.8086 0.054 Uiso 1 1 calc R U . . . H19B H 0.7538 0.4323 0.8021 0.054 Uiso 1 1 calc R U . . . H19C H 0.7530 0.4868 0.7713 0.054 Uiso 1 1 calc R U . . . C20 C 0.8869(2) 0.56353(19) 0.79351(9) 0.0388(7) Uani 1 1 d . . . . . H20A H 0.8591 0.5979 0.8063 0.058 Uiso 1 1 calc R U . . . H20B H 0.8747 0.5726 0.7693 0.058 Uiso 1 1 calc R U . . . H20C H 0.9435 0.5683 0.7997 0.058 Uiso 1 1 calc R U . . . C21 C 1.0839(2) 0.40501(17) 0.91691(7) 0.0301(6) Uani 1 1 d . . . . . C22 C 1.1599(2) 0.3750(2) 0.92269(9) 0.0408(8) Uani 1 1 d . . . . . C23 C 1.1872(3) 0.3560(2) 0.95648(11) 0.0535(11) Uani 1 1 d . . . . . H23 H 1.2379 0.3360 0.9613 0.064 Uiso 1 1 calc R U . . . C24 C 1.1406(3) 0.3662(2) 0.98243(10) 0.0577(12) Uani 1 1 d . . . . . H24 H 1.1600 0.3531 1.0048 0.069 Uiso 1 1 calc R U . . . C25 C 1.0658(3) 0.3955(2) 0.97617(8) 0.0483(10) Uani 1 1 d . . . . . H25 H 1.0346 0.4009 0.9943 0.058 Uiso 1 1 calc R U . . . C26 C 1.0348(2) 0.41775(18) 0.94294(7) 0.0343(7) Uani 1 1 d . . . . . C27 C 1.2142(2) 0.3651(2) 0.89456(11) 0.0510(10) Uani 1 1 d . . . . . H27 H 1.1823 0.3733 0.8724 0.061 Uiso 1 1 calc R U . . . C28 C 1.2483(3) 0.2880(3) 0.89426(15) 0.0674(13) Uani 1 1 d . . . . . H28A H 1.2820 0.2837 0.8760 0.101 Uiso 1 1 calc R U . . . H28B H 1.2052 0.2538 0.8906 0.101 Uiso 1 1 calc R U . . . H28C H 1.2790 0.2782 0.9159 0.101 Uiso 1 1 calc R U . . . C29 C 1.2832(3) 0.4200(3) 0.89785(14) 0.0650(12) Uani 1 1 d . . . . . H29A H 1.3161 0.4124 0.8796 0.098 Uiso 1 1 calc R U . . . H29B H 1.3147 0.4136 0.9196 0.098 Uiso 1 1 calc R U . . . H29C H 1.2618 0.4682 0.8964 0.098 Uiso 1 1 calc R U . . . C30 C 0.9551(2) 0.4549(2) 0.93587(8) 0.0371(8) Uani 1 1 d . . . . . H30 H 0.9293 0.4363 0.9139 0.045 Uiso 1 1 calc R U . . . C31 C 0.9668(2) 0.5365(2) 0.93161(9) 0.0434(8) Uani 1 1 d . . . . . H31A H 0.9156 0.5596 0.9271 0.065 Uiso 1 1 calc R U . . . H31B H 0.9977 0.5451 0.9127 0.065 Uiso 1 1 calc R U . . . H31C H 0.9944 0.5560 0.9524 0.065 Uiso 1 1 calc R U . . . C32 C 0.8985(3) 0.4404(2) 0.96331(10) 0.0505(10) Uani 1 1 d . . . . . H32A H 0.8490 0.4655 0.9573 0.076 Uiso 1 1 calc R U . . . H32B H 0.9227 0.4573 0.9853 0.076 Uiso 1 1 calc R U . . . H32C H 0.8885 0.3894 0.9646 0.076 Uiso 1 1 calc R U . . . C33 C 0.57136(17) 0.13787(16) 0.85226(7) 0.0229(5) Uani 1 1 d . . . . . C34 C 0.57352(18) 0.01476(16) 0.84921(8) 0.0276(6) Uani 1 1 d . . . . . H34 H 0.5752 -0.0336 0.8559 0.033 Uiso 1 1 calc R U . . . C35 C 0.56971(18) 0.04005(17) 0.81696(8) 0.0279(6) Uani 1 1 d . . . . . H35 H 0.5684 0.0125 0.7970 0.033 Uiso 1 1 calc R U . . . C36 C 0.5193(2) 0.31225(19) 0.83174(9) 0.0396(8) Uani 1 1 d . . . . . H36 H 0.5165 0.3108 0.8078 0.047 Uiso 1 1 calc R U . . . C37 C 0.5777(2) 0.34596(18) 0.85380(10) 0.0397(8) Uani 1 1 d . . . . . H37 H 0.6220 0.3705 0.8474 0.048 Uiso 1 1 calc R U . . . C38 C 0.5574(2) 0.33615(18) 0.88845(9) 0.0360(7) Uani 1 1 d . . . . . H38 H 0.5878 0.3519 0.9084 0.043 Uiso 1 1 calc R U . . . C39 C 0.4847(2) 0.29908(19) 0.88730(9) 0.0378(7) Uani 1 1 d . . . . . H39 H 0.4560 0.2891 0.9058 0.045 Uiso 1 1 calc R U . . . C40 C 0.4635(2) 0.27977(19) 0.85266(10) 0.0388(7) Uani 1 1 d . . . . . H40 H 0.4203 0.2507 0.8446 0.047 Uiso 1 1 calc R U . . . C41 C 0.57321(18) 0.06810(16) 0.90776(7) 0.0261(6) Uani 1 1 d . . . . . C42 C 0.5003(2) 0.08010(17) 0.92111(8) 0.0306(6) Uani 1 1 d . . . . . C43 C 0.5004(2) 0.0721(2) 0.95679(9) 0.0433(8) Uani 1 1 d . . . . . H43 H 0.4533 0.0800 0.9667 0.052 Uiso 1 1 calc R U . . . C44 C 0.5680(3) 0.0530(2) 0.97738(9) 0.0490(9) Uani 1 1 d . . . . . H44 H 0.5665 0.0491 1.0010 0.059 Uiso 1 1 calc R U . . . C45 C 0.6376(3) 0.0397(2) 0.96351(9) 0.0447(9) Uani 1 1 d . . . . . H45 H 0.6829 0.0261 0.9779 0.054 Uiso 1 1 calc R U . . . C46 C 0.6423(2) 0.04597(18) 0.92808(8) 0.0328(7) Uani 1 1 d . . . . . C47 C 0.4247(2) 0.09764(19) 0.89817(9) 0.0367(7) Uani 1 1 d . . . . . H47 H 0.4390 0.1302 0.8800 0.044 Uiso 1 1 calc R U . . . C48 C 0.3614(3) 0.1356(2) 0.91711(13) 0.0566(11) Uani 1 1 d . . . . . H48A H 0.3149 0.1452 0.9012 0.085 Uiso 1 1 calc R U . . . H48B H 0.3826 0.1804 0.9266 0.085 Uiso 1 1 calc R U . . . H48C H 0.3470 0.1050 0.9353 0.085 Uiso 1 1 calc R U . . . C49 C 0.3883(2) 0.0289(2) 0.88097(10) 0.0435(8) Uani 1 1 d . . . . . H49A H 0.3406 0.0412 0.8664 0.065 Uiso 1 1 calc R U . . . H49B H 0.3755 -0.0046 0.8984 0.065 Uiso 1 1 calc R U . . . H49C H 0.4261 0.0071 0.8674 0.065 Uiso 1 1 calc R U . . . C50 C 0.7188(2) 0.0246(2) 0.91368(9) 0.0385(7) Uani 1 1 d . . . . . H50 H 0.7157 0.0413 0.8898 0.046 Uiso 1 1 calc R U . . . C51 C 0.7254(3) -0.0586(2) 0.91381(11) 0.0503(9) Uani 1 1 d . . . . . H51A H 0.7737 -0.0727 0.9046 0.076 Uiso 1 1 calc R U . . . H51B H 0.6802 -0.0788 0.8999 0.076 Uiso 1 1 calc R U . . . H51C H 0.7263 -0.0761 0.9370 0.076 Uiso 1 1 calc R U . . . C52 C 0.7939(2) 0.0573(2) 0.93350(12) 0.0527(10) Uani 1 1 d . . . . . H52A H 0.8403 0.0418 0.9231 0.079 Uiso 1 1 calc R U . . . H52B H 0.7981 0.0413 0.9570 0.079 Uiso 1 1 calc R U . . . H52C H 0.7904 0.1091 0.9328 0.079 Uiso 1 1 calc R U . . . C53 C 0.55175(18) 0.15976(17) 0.78861(7) 0.0260(6) Uani 1 1 d . . . . . C54 C 0.47354(19) 0.16039(18) 0.77232(7) 0.0301(6) Uani 1 1 d . . . . . C55 C 0.4581(2) 0.2031(2) 0.74285(8) 0.0367(7) Uani 1 1 d . . . . . H55 H 0.4065 0.2051 0.7317 0.044 Uiso 1 1 calc R U . . . C56 C 0.5179(2) 0.2423(2) 0.73008(8) 0.0396(8) Uani 1 1 d . . . . . H56 H 0.5065 0.2704 0.7104 0.047 Uiso 1 1 calc R U . . . C57 C 0.5948(2) 0.23993(19) 0.74651(8) 0.0346(7) Uani 1 1 d . . . . . H57 H 0.6346 0.2666 0.7376 0.042 Uiso 1 1 calc R U . . . C58 C 0.61425(19) 0.19879(17) 0.77609(7) 0.0288(6) Uani 1 1 d . . . . . C59 C 0.40629(19) 0.1163(2) 0.78488(8) 0.0348(7) Uani 1 1 d . . . . . H59 H 0.4236 0.1002 0.8084 0.042 Uiso 1 1 calc R U . . . C60 C 0.3289(2) 0.1596(2) 0.78557(10) 0.0459(9) Uani 1 1 d . . . . . H60A H 0.2886 0.1293 0.7938 0.069 Uiso 1 1 calc R U . . . H60B H 0.3110 0.1763 0.7628 0.069 Uiso 1 1 calc R U . . . H60C H 0.3386 0.2005 0.8006 0.069 Uiso 1 1 calc R U . . . C61 C 0.3901(2) 0.0490(2) 0.76227(10) 0.0446(8) Uani 1 1 d . . . . . H61A H 0.3478 0.0212 0.7705 0.067 Uiso 1 1 calc R U . . . H61B H 0.4376 0.0200 0.7633 0.067 Uiso 1 1 calc R U . . . H61C H 0.3746 0.0636 0.7389 0.067 Uiso 1 1 calc R U . . . C62 C 0.69946(19) 0.19704(19) 0.79352(8) 0.0326(7) Uani 1 1 d . . . . . H62 H 0.6970 0.1943 0.8184 0.039 Uiso 1 1 calc R U . . . C63 C 0.7439(2) 0.1313(3) 0.78286(15) 0.0660(14) Uani 1 1 d . . . . . H63A H 0.7145 0.0884 0.7874 0.099 Uiso 1 1 calc R U . . . H63B H 0.7958 0.1295 0.7957 0.099 Uiso 1 1 calc R U . . . H63C H 0.7496 0.1341 0.7587 0.099 Uiso 1 1 calc R U . . . C64 C 0.7466(3) 0.2639(2) 0.78621(12) 0.0596(12) Uani 1 1 d . . . . . H64A H 0.7997 0.2602 0.7979 0.089 Uiso 1 1 calc R U . . . H64B H 0.7207 0.3059 0.7943 0.089 Uiso 1 1 calc R U . . . H64C H 0.7493 0.2680 0.7619 0.089 Uiso 1 1 calc R U . . . C65 C 0.97106(16) 0.11839(16) 1.11189(7) 0.0230(5) Uani 1 1 d . . . . . C66 C 0.99012(19) 0.01824(17) 1.08008(7) 0.0296(6) Uani 1 1 d . . . . . H66 H 0.9936 -0.0117 1.0612 0.036 Uiso 1 1 calc R U . . . C67 C 1.00543(19) -0.00067(17) 1.11348(8) 0.0301(6) Uani 1 1 d . . . . . H67 H 1.0215 -0.0459 1.1221 0.036 Uiso 1 1 calc R U . . . C68 C 0.9773(2) 0.32349(18) 1.13899(9) 0.0343(7) Uani 1 1 d . . . . . H68 H 0.9590 0.3411 1.1590 0.041 Uiso 1 1 calc R U . . . C69 C 0.9321(2) 0.32296(17) 1.10513(8) 0.0353(7) Uani 1 1 d . . . . . H69 H 0.8809 0.3415 1.0995 0.042 Uiso 1 1 calc R U . . . C70 C 0.9797(2) 0.28961(19) 1.08278(9) 0.0399(8) Uani 1 1 d . . . . . H70 H 0.9670 0.2833 1.0592 0.048 Uiso 1 1 calc R U . . . C71 C 1.0520(2) 0.2668(2) 1.10274(10) 0.0427(8) Uani 1 1 d . . . . . H71 H 1.0921 0.2389 1.0947 0.051 Uiso 1 1 calc R U . . . C72 C 1.0523(2) 0.2935(2) 1.13657(10) 0.0401(8) Uani 1 1 d . . . . . H72 H 1.0946 0.2914 1.1540 0.048 Uiso 1 1 calc R U . . . C73 C 0.94092(18) 0.12880(17) 1.04807(7) 0.0263(6) Uani 1 1 d . . . . . C74 C 0.8584(2) 0.14278(19) 1.04128(7) 0.0318(7) Uani 1 1 d . . . . . C75 C 0.8334(2) 0.1837(2) 1.01219(8) 0.0421(8) Uani 1 1 d . . . . . H75 H 0.7793 0.1944 1.0072 0.050 Uiso 1 1 calc R U . . . C76 C 0.8871(2) 0.2088(2) 0.99067(8) 0.0456(9) Uani 1 1 d . . . . . H76 H 0.8693 0.2375 0.9718 0.055 Uiso 1 1 calc R U . . . C77 C 0.9670(2) 0.1915(2) 0.99700(8) 0.0395(8) Uani 1 1 d . . . . . H77 H 1.0022 0.2071 0.9818 0.047 Uiso 1 1 calc R U . . . C78 C 0.99599(19) 0.15105(18) 1.02582(7) 0.0299(6) Uani 1 1 d . . . . . C79 C 0.79837(19) 0.1124(2) 1.06401(8) 0.0374(8) Uani 1 1 d . . . . . H79 H 0.8205 0.1196 1.0880 0.045 Uiso 1 1 calc R U . . . C80 C 0.7179(2) 0.1497(3) 1.05910(11) 0.0517(10) Uani 1 1 d . . . . . H80A H 0.6829 0.1282 1.0742 0.077 Uiso 1 1 calc R U . . . H80B H 0.6950 0.1442 1.0356 0.077 Uiso 1 1 calc R U . . . H80C H 0.7245 0.2002 1.0644 0.077 Uiso 1 1 calc R U . . . C81 C 0.7868(2) 0.0311(2) 1.05830(10) 0.0459(9) Uani 1 1 d . . . . . H81A H 0.7490 0.0132 1.0730 0.069 Uiso 1 1 calc R U . . . H81B H 0.8371 0.0067 1.0637 0.069 Uiso 1 1 calc R U . . . H81C H 0.7672 0.0222 1.0347 0.069 Uiso 1 1 calc R U . . . C82 C 1.08436(19) 0.13192(19) 1.03111(8) 0.0314(6) Uani 1 1 d . . . . . H82 H 1.0968 0.1130 1.0545 0.038 Uiso 1 1 calc R U . . . C83 C 1.1386(2) 0.1969(2) 1.02659(10) 0.0445(8) Uani 1 1 d . . . . . H83A H 1.1935 0.1820 1.0303 0.067 Uiso 1 1 calc R U . . . H83B H 1.1290 0.2338 1.0430 0.067 Uiso 1 1 calc R U . . . H83C H 1.1274 0.2159 1.0037 0.067 Uiso 1 1 calc R U . . . C84 C 1.1023(2) 0.0729(2) 1.00552(9) 0.0397(8) Uani 1 1 d . . . . . H84A H 1.1581 0.0607 1.0090 0.059 Uiso 1 1 calc R U . . . H84B H 1.0892 0.0902 0.9824 0.059 Uiso 1 1 calc R U . . . H84C H 1.0709 0.0307 1.0091 0.059 Uiso 1 1 calc R U . . . C85 C 1.00593(19) 0.06224(17) 1.16977(7) 0.0269(6) Uani 1 1 d . . . . . C86 C 0.9429(2) 0.04266(17) 1.18863(8) 0.0317(6) Uani 1 1 d . . . . . C87 C 0.9592(2) 0.0443(2) 1.22457(8) 0.0413(8) Uani 1 1 d . . . . . H87 H 0.9188 0.0328 1.2381 0.050 Uiso 1 1 calc R U . . . C88 C 1.0335(2) 0.0625(2) 1.24018(8) 0.0438(9) Uani 1 1 d . . . . . H88 H 1.0425 0.0636 1.2641 0.053 Uiso 1 1 calc R U . . . C89 C 1.0947(2) 0.0793(2) 1.22087(8) 0.0378(7) Uani 1 1 d . . . . . H89 H 1.1451 0.0901 1.2318 0.045 Uiso 1 1 calc R U . . . C90 C 1.0818(2) 0.08018(18) 1.18504(8) 0.0311(6) Uani 1 1 d . . . . . C91 C 0.8623(2) 0.01719(18) 1.17196(8) 0.0337(7) Uani 1 1 d . . . . . H91 H 0.8520 0.0412 1.1495 0.040 Uiso 1 1 calc R U . . . C92 C 0.7931(2) 0.0359(2) 1.19311(10) 0.0437(8) Uani 1 1 d . . . . . H92A H 0.7437 0.0186 1.1813 0.065 Uiso 1 1 calc R U . . . H92B H 0.7903 0.0874 1.1959 0.065 Uiso 1 1 calc R U . . . H92C H 0.8021 0.0132 1.2153 0.065 Uiso 1 1 calc R U . . . C93 C 0.8636(2) -0.0647(2) 1.16569(12) 0.0493(9) Uani 1 1 d . . . . . H93A H 0.8124 -0.0801 1.1550 0.074 Uiso 1 1 calc R U . . . H93B H 0.8755 -0.0894 1.1873 0.074 Uiso 1 1 calc R U . . . H93C H 0.9039 -0.0760 1.1509 0.074 Uiso 1 1 calc R U . . . C94 C 1.1517(2) 0.0933(2) 1.16439(8) 0.0396(8) Uani 1 1 d . . . . . H94 H 1.1309 0.1012 1.1403 0.048 Uiso 1 1 calc R U . . . C95 C 1.2022(2) 0.1592(2) 1.17699(10) 0.0469(9) Uani 1 1 d . . . . . H95A H 1.2454 0.1650 1.1631 0.070 Uiso 1 1 calc R U . . . H95B H 1.2234 0.1520 1.2006 0.070 Uiso 1 1 calc R U . . . H95C H 1.1693 0.2018 1.1752 0.070 Uiso 1 1 calc R U . . . C96 C 1.2035(3) 0.0257(3) 1.16649(12) 0.0592(11) Uani 1 1 d . . . . . H96A H 1.2481 0.0329 1.1535 0.089 Uiso 1 1 calc R U . . . H96B H 1.1724 -0.0148 1.1572 0.089 Uiso 1 1 calc R U . . . H96C H 1.2227 0.0162 1.1901 0.089 Uiso 1 1 calc R U . . . C97 C 0.53481(17) 0.35877(16) 1.09821(7) 0.0249(6) Uani 1 1 d . . . . . C98 C 0.5074(2) 0.45362(18) 1.06202(9) 0.0382(7) Uani 1 1 d . . . . . H98 H 0.5045 0.4820 1.0423 0.046 Uiso 1 1 calc R U . . . C99 C 0.4819(2) 0.47216(19) 1.09220(10) 0.0417(8) Uani 1 1 d . . . . . H99 H 0.4580 0.5156 1.0974 0.050 Uiso 1 1 calc R U . . . C100 C 0.5901(2) 0.2117(2) 1.16582(8) 0.0381(8) Uani 1 1 d . . . . . H100 H 0.6213 0.2242 1.1861 0.046 Uiso 1 1 calc R U . . . C101 C 0.5094(2) 0.2275(2) 1.15764(9) 0.0406(8) Uani 1 1 d . . . . . H101 H 0.4766 0.2514 1.1717 0.049 Uiso 1 1 calc R U . . . C102 C 0.4861(2) 0.20056(19) 1.12382(9) 0.0370(7) Uani 1 1 d . . . . . H102 H 0.4362 0.2069 1.1114 0.044 Uiso 1 1 calc R U . . . C103 C 0.5514(2) 0.16244(18) 1.11232(9) 0.0354(7) Uani 1 1 d . . . . . H103 H 0.5509 0.1359 1.0921 0.043 Uiso 1 1 calc R U . . . C104 C 0.6168(2) 0.17247(18) 1.13732(9) 0.0354(7) Uani 1 1 d . . . . . H104 H 0.6687 0.1565 1.1358 0.042 Uiso 1 1 calc R U . . . C105 C 0.56332(18) 0.34270(17) 1.03702(7) 0.0271(6) Uani 1 1 d . . . . . C106 C 0.6331(2) 0.3618(2) 1.02250(8) 0.0366(7) Uani 1 1 d . . . . . C107 C 0.6517(2) 0.3217(3) 0.99406(9) 0.0467(9) Uani 1 1 d . . . . . H107 H 0.6976 0.3331 0.9839 0.056 Uiso 1 1 calc R U . . . C108 C 0.6043(3) 0.2661(3) 0.98085(9) 0.0492(10) Uani 1 1 d . . . . . H108 H 0.6183 0.2401 0.9620 0.059 Uiso 1 1 calc R U . . . C109 C 0.5351(2) 0.2484(2) 0.99555(9) 0.0416(8) Uani 1 1 d . . . . . H109 H 0.5032 0.2104 0.9864 0.050 Uiso 1 1 calc R U . . . C110 C 0.51284(19) 0.28648(18) 1.02366(7) 0.0304(6) Uani 1 1 d . . . . . C111 C 0.6851(2) 0.4250(2) 1.03469(9) 0.0464(9) Uani 1 1 d . . . . . H111 H 0.6708 0.4401 1.0573 0.056 Uiso 1 1 calc R U . . . C112 C 0.6699(3) 0.4888(3) 1.00964(12) 0.0686(15) Uani 1 1 d . . . . . H11A H 0.7029 0.5290 1.0177 0.103 Uiso 1 1 calc R U . . . H11B H 0.6147 0.5027 1.0083 0.103 Uiso 1 1 calc R U . . . H11C H 0.6826 0.4746 0.9872 0.103 Uiso 1 1 calc R U . . . C113 C 0.7741(2) 0.4063(3) 1.03834(11) 0.0653(15) Uani 1 1 d . . . . . H11D H 0.8046 0.4480 1.0463 0.098 Uiso 1 1 calc R U . . . H11E H 0.7893 0.3915 1.0164 0.098 Uiso 1 1 calc R U . . . H11F H 0.7843 0.3675 1.0546 0.098 Uiso 1 1 calc R U . . . C114 C 0.43314(19) 0.27056(19) 1.03700(8) 0.0331(7) Uani 1 1 d . . . . . H114 H 0.4389 0.2810 1.0617 0.040 Uiso 1 1 calc R U . . . C115 C 0.4065(3) 0.1917(2) 1.03227(11) 0.0516(10) Uani 1 1 d . . . . . H11G H 0.3562 0.1851 1.0413 0.077 Uiso 1 1 calc R U . . . H11H H 0.4459 0.1606 1.0443 0.077 Uiso 1 1 calc R U . . . H11I H 0.4008 0.1798 1.0082 0.077 Uiso 1 1 calc R U . . . C116 C 0.3692(2) 0.3211(3) 1.01985(11) 0.0536(10) Uani 1 1 d . . . . . H11J H 0.3190 0.3109 1.0284 0.080 Uiso 1 1 calc R U . . . H11K H 0.3641 0.3137 0.9954 0.080 Uiso 1 1 calc R U . . . H11L H 0.3841 0.3704 1.0249 0.080 Uiso 1 1 calc R U . . . C117 C 0.4662(2) 0.4055(2) 1.14692(9) 0.0382(7) Uani 1 1 d . . . . . C118 C 0.5157(2) 0.4175(2) 1.17732(9) 0.0421(8) Uani 1 1 d . . . . . C119 C 0.4832(3) 0.4028(3) 1.20826(10) 0.0543(11) Uani 1 1 d . . . . . H119 H 0.5147 0.4091 1.2291 0.065 Uiso 1 1 calc R U . . . C120 C 0.4060(3) 0.3793(3) 1.20824(12) 0.0627(13) Uani 1 1 d . . . . . H120 H 0.3859 0.3697 1.2290 0.075 Uiso 1 1 calc R U . . . C121 C 0.3582(3) 0.3699(3) 1.17793(11) 0.0561(11) Uani 1 1 d . . . . . H121 H 0.3056 0.3548 1.1784 0.067 Uiso 1 1 calc R U . . . C122 C 0.3871(2) 0.3827(2) 1.14627(10) 0.0447(9) Uani 1 1 d . . . . . C123 C 0.5997(2) 0.4477(2) 1.17711(9) 0.0444(9) Uani 1 1 d . . . . . H123 H 0.6194 0.4327 1.1555 0.053 Uiso 1 1 calc R U . . . C124 C 0.5972(3) 0.5302(2) 1.17741(10) 0.0511(10) Uani 1 1 d . . . . . H12A H 0.6504 0.5489 1.1772 0.077 Uiso 1 1 calc R U . . . H12B H 0.5755 0.5465 1.1978 0.077 Uiso 1 1 calc R U . . . H12C H 0.5642 0.5472 1.1574 0.077 Uiso 1 1 calc R U . . . C125 C 0.6578(3) 0.4192(2) 1.20646(10) 0.0513(10) Uani 1 1 d . . . . . H12D H 0.7097 0.4400 1.2050 0.077 Uiso 1 1 calc R U . . . H12E H 0.6612 0.3675 1.2049 0.077 Uiso 1 1 calc R U . . . H12F H 0.6394 0.4322 1.2281 0.077 Uiso 1 1 calc R U . . . C126 C 0.3318(2) 0.3739(3) 1.11296(11) 0.0514(10) Uani 1 1 d . . . . . H126 H 0.3657 0.3700 1.0941 0.062 Uiso 1 1 calc R U . . . C127 C 0.2795(3) 0.4410(4) 1.10599(15) 0.0798(17) Uani 1 1 d . . . . . H12G H 0.2452 0.4345 1.0849 0.120 Uiso 1 1 calc R U . . . H12H H 0.3128 0.4826 1.1040 0.120 Uiso 1 1 calc R U . . . H12I H 0.2475 0.4480 1.1247 0.120 Uiso 1 1 calc R U . . . C128 C 0.2807(3) 0.3061(3) 1.11225(14) 0.0703(14) Uani 1 1 d . . . . . H12J H 0.2475 0.3034 1.0907 0.105 Uiso 1 1 calc R U . . . H12K H 0.2476 0.3077 1.1308 0.105 Uiso 1 1 calc R U . . . H12L H 0.3147 0.2642 1.1148 0.105 Uiso 1 1 calc R U . . . N1 N 1.01264(14) 0.42329(13) 0.82863(6) 0.0233(5) Uani 1 1 d . . . . . N2 N 1.05659(15) 0.42675(14) 0.88196(6) 0.0244(5) Uani 1 1 d . . . . . N3 N 0.57451(14) 0.07446(13) 0.87074(6) 0.0234(5) Uani 1 1 d . . . . . N4 N 0.56814(14) 0.11462(13) 0.81888(6) 0.0240(5) Uani 1 1 d . . . . . N5 N 0.96830(14) 0.09030(14) 1.07920(6) 0.0239(5) Uani 1 1 d . . . . . N6 N 0.99242(15) 0.06079(14) 1.13245(6) 0.0245(5) Uani 1 1 d . . . . . N7 N 0.53907(15) 0.38440(14) 1.06571(6) 0.0274(5) Uani 1 1 d . . . . . N8 N 0.49818(16) 0.41363(15) 1.11407(7) 0.0311(5) Uani 1 1 d . . . . . Ni1 Ni 0.95308(3) 0.30082(3) 0.86670(2) 0.02328(10) Uani 1 1 d . . . . . Ni2 Ni 0.57696(3) 0.23409(3) 0.86785(2) 0.02324(10) Uani 1 1 d . . . . . Ni3 Ni 0.95627(3) 0.21617(3) 1.12351(2) 0.02443(10) Uani 1 1 d . . . . . Ni4 Ni 0.57984(3) 0.27582(3) 1.11977(2) 0.02473(11) Uani 1 1 d . . . . . Se1 Se 0.83284(2) 0.36125(2) 0.86577(2) 0.02863(7) Uani 1 1 d . . . . . Se2 Se 0.76699(2) 0.31974(2) 0.91159(2) 0.02768(7) Uani 1 1 d . . . . . Se3 Se 0.70099(2) 0.21186(2) 0.89572(2) 0.02769(7) Uani 1 1 d . . . . . Se4 Se 0.85411(2) 0.19475(2) 1.15627(2) 0.02871(7) Uani 1 1 d . . . . . Se5 Se 0.78725(2) 0.30219(2) 1.16552(2) 0.03238(8) Uani 1 1 d . . . . . Se6 Se 0.70236(2) 0.32909(2) 1.11587(2) 0.02926(7) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0245(14) 0.0272(14) 0.0168(12) 0.0008(10) 0.0027(10) 0.0044(11) C2 0.0345(16) 0.0278(15) 0.0233(13) 0.0026(11) 0.0053(12) -0.0020(12) C3 0.0279(15) 0.0283(15) 0.0261(14) -0.0009(11) 0.0008(11) -0.0037(12) C4 0.0314(16) 0.0319(16) 0.0383(17) 0.0038(13) 0.0098(13) 0.0029(13) C5 0.0381(18) 0.0317(16) 0.0330(16) -0.0058(12) 0.0073(13) 0.0010(13) C6 0.0320(16) 0.0278(15) 0.0399(17) -0.0018(13) 0.0065(13) -0.0037(12) C7 0.0427(18) 0.0292(15) 0.0307(15) 0.0090(12) 0.0088(13) 0.0018(13) C8 0.0383(18) 0.0326(16) 0.0328(16) 0.0061(13) -0.0010(13) 0.0065(13) C9 0.0328(15) 0.0249(14) 0.0149(12) 0.0007(10) 0.0044(11) -0.0016(11) C10 0.0355(16) 0.0305(15) 0.0222(13) 0.0024(11) 0.0088(12) 0.0037(13) C11 0.0456(19) 0.0428(18) 0.0224(14) -0.0083(13) 0.0082(13) 0.0057(15) C12 0.048(2) 0.0451(19) 0.0185(13) -0.0057(13) 0.0004(13) -0.0017(16) C13 0.0338(16) 0.0366(16) 0.0202(13) -0.0004(12) -0.0019(11) -0.0019(13) C14 0.0306(15) 0.0249(14) 0.0171(12) 0.0018(10) 0.0021(11) -0.0016(11) C15 0.0374(18) 0.0415(18) 0.0276(15) 0.0027(13) 0.0089(13) 0.0096(14) C16 0.052(2) 0.044(2) 0.0416(19) 0.0048(15) 0.0186(16) 0.0159(17) C17 0.041(2) 0.050(2) 0.060(2) 0.0075(18) 0.0118(18) 0.0067(17) C18 0.0318(16) 0.0290(15) 0.0212(13) -0.0003(11) -0.0013(11) 0.0016(12) C19 0.0345(17) 0.0408(18) 0.0332(16) 0.0016(13) 0.0031(13) 0.0070(14) C20 0.047(2) 0.0307(17) 0.0374(17) -0.0004(13) -0.0013(15) 0.0008(14) C21 0.0361(17) 0.0301(15) 0.0222(13) 0.0047(11) -0.0060(12) -0.0056(13) C22 0.0392(19) 0.0355(18) 0.0434(19) 0.0077(14) -0.0144(15) -0.0040(15) C23 0.053(2) 0.047(2) 0.054(2) 0.0164(18) -0.0257(19) -0.0082(18) C24 0.076(3) 0.053(2) 0.036(2) 0.0213(17) -0.030(2) -0.025(2) C25 0.071(3) 0.050(2) 0.0217(15) 0.0061(14) -0.0044(16) -0.027(2) C26 0.049(2) 0.0324(16) 0.0198(13) 0.0007(12) -0.0017(13) -0.0175(14) C27 0.0328(19) 0.056(2) 0.062(2) 0.0045(19) -0.0066(17) 0.0106(17) C28 0.041(2) 0.059(3) 0.100(4) -0.002(3) -0.003(2) 0.012(2) C29 0.044(2) 0.066(3) 0.085(3) 0.011(3) 0.006(2) 0.000(2) C30 0.0416(18) 0.048(2) 0.0232(14) -0.0054(13) 0.0084(13) -0.0166(15) C31 0.053(2) 0.045(2) 0.0344(17) 0.0033(15) 0.0160(16) -0.0024(17) C32 0.061(3) 0.057(2) 0.0375(18) -0.0139(17) 0.0233(18) -0.026(2) C33 0.0211(13) 0.0267(14) 0.0205(12) -0.0003(10) 0.0003(10) 0.0017(11) C34 0.0274(15) 0.0240(14) 0.0316(15) -0.0013(11) 0.0047(12) 0.0002(11) C35 0.0275(15) 0.0278(15) 0.0284(14) -0.0053(11) 0.0035(11) 0.0006(12) C36 0.050(2) 0.0324(17) 0.0347(17) 0.0044(13) -0.0034(15) 0.0161(15) C37 0.044(2) 0.0225(15) 0.053(2) 0.0052(14) 0.0057(16) 0.0001(14) C38 0.0367(18) 0.0277(15) 0.0421(17) -0.0079(13) -0.0025(14) 0.0077(13) C39 0.0348(17) 0.0330(17) 0.0472(19) -0.0034(14) 0.0118(15) 0.0091(14) C40 0.0287(16) 0.0306(16) 0.055(2) -0.0038(14) -0.0067(14) 0.0064(13) C41 0.0313(15) 0.0236(14) 0.0236(13) 0.0007(10) 0.0037(11) -0.0017(11) C42 0.0343(16) 0.0246(14) 0.0345(15) 0.0001(12) 0.0103(13) -0.0041(12) C43 0.054(2) 0.0382(18) 0.0415(19) 0.0001(15) 0.0230(17) -0.0066(16) C44 0.070(3) 0.049(2) 0.0287(16) 0.0074(15) 0.0100(17) -0.0094(19) C45 0.055(2) 0.047(2) 0.0297(16) 0.0099(15) -0.0063(15) -0.0075(17) C46 0.0362(17) 0.0291(15) 0.0320(16) 0.0072(12) -0.0011(13) -0.0032(13) C47 0.0281(16) 0.0330(17) 0.0505(19) 0.0015(14) 0.0115(14) 0.0012(13) C48 0.040(2) 0.042(2) 0.091(3) -0.011(2) 0.020(2) 0.0032(17) C49 0.0268(17) 0.046(2) 0.058(2) -0.0082(17) 0.0056(15) -0.0007(15) C50 0.0310(17) 0.0369(18) 0.0458(19) 0.0133(14) -0.0033(14) 0.0016(14) C51 0.044(2) 0.042(2) 0.063(2) 0.0144(18) -0.0017(18) 0.0088(17) C52 0.0299(18) 0.050(2) 0.074(3) 0.023(2) -0.0122(17) -0.0010(16) C53 0.0302(15) 0.0300(15) 0.0174(12) -0.0029(11) 0.0001(11) 0.0006(12) C54 0.0298(16) 0.0364(16) 0.0233(13) -0.0034(12) -0.0005(11) 0.0027(13) C55 0.0338(17) 0.0468(19) 0.0271(15) -0.0014(13) -0.0080(13) 0.0030(14) C56 0.049(2) 0.0449(19) 0.0225(14) 0.0043(13) -0.0048(13) 0.0002(16) C57 0.0438(19) 0.0385(17) 0.0210(14) 0.0000(12) 0.0016(13) -0.0068(14) C58 0.0304(16) 0.0331(16) 0.0224(13) -0.0026(11) -0.0002(11) -0.0021(12) C59 0.0271(16) 0.0451(19) 0.0319(15) -0.0051(14) 0.0018(12) 0.0002(14) C60 0.0302(18) 0.060(2) 0.047(2) -0.0086(17) 0.0015(15) 0.0032(17) C61 0.0331(18) 0.052(2) 0.049(2) -0.0120(17) 0.0059(15) -0.0084(16) C62 0.0300(16) 0.0440(18) 0.0233(14) 0.0003(12) -0.0002(12) -0.0067(14) C63 0.029(2) 0.054(3) 0.111(4) -0.021(3) -0.013(2) 0.0007(18) C64 0.054(3) 0.050(2) 0.069(3) 0.006(2) -0.019(2) -0.022(2) C65 0.0199(13) 0.0312(14) 0.0176(12) 0.0000(10) 0.0006(10) -0.0019(11) C66 0.0334(16) 0.0314(15) 0.0232(13) -0.0055(11) -0.0011(12) 0.0012(12) C67 0.0348(16) 0.0258(14) 0.0288(15) -0.0010(11) -0.0006(12) 0.0037(12) C68 0.0376(17) 0.0292(16) 0.0348(16) -0.0066(12) -0.0025(13) -0.0049(13) C69 0.0446(19) 0.0249(15) 0.0346(16) 0.0046(12) -0.0050(14) -0.0036(13) C70 0.058(2) 0.0323(17) 0.0291(16) 0.0039(13) 0.0047(15) -0.0131(16) C71 0.0371(19) 0.0378(18) 0.055(2) -0.0041(16) 0.0144(16) -0.0107(15) C72 0.0327(17) 0.0362(18) 0.049(2) -0.0070(15) -0.0058(15) -0.0093(14) C73 0.0301(15) 0.0318(15) 0.0161(12) -0.0036(11) -0.0011(11) 0.0015(12) C74 0.0320(16) 0.0432(18) 0.0197(13) -0.0061(12) -0.0002(11) 0.0060(13) C75 0.0380(19) 0.062(2) 0.0245(15) -0.0032(15) -0.0037(13) 0.0172(17) C76 0.053(2) 0.059(2) 0.0232(15) 0.0073(15) -0.0028(14) 0.0190(18) C77 0.046(2) 0.052(2) 0.0212(14) 0.0064(14) 0.0050(13) 0.0059(16) C78 0.0320(16) 0.0377(17) 0.0195(13) -0.0028(12) -0.0003(11) -0.0001(13) C79 0.0269(16) 0.058(2) 0.0267(15) -0.0104(14) 0.0017(12) 0.0016(15) C80 0.0330(19) 0.070(3) 0.053(2) -0.018(2) 0.0096(16) 0.0073(18) C81 0.0331(18) 0.059(2) 0.047(2) -0.0018(17) 0.0100(15) -0.0030(17) C82 0.0286(16) 0.0411(18) 0.0239(14) 0.0022(12) 0.0000(11) -0.0025(13) C83 0.042(2) 0.049(2) 0.0425(19) 0.0030(16) 0.0085(16) -0.0062(17) C84 0.0341(18) 0.049(2) 0.0358(17) -0.0001(15) 0.0035(14) 0.0041(15) C85 0.0314(15) 0.0298(15) 0.0189(13) 0.0029(11) 0.0001(11) 0.0010(12) C86 0.0388(17) 0.0295(15) 0.0271(14) 0.0070(12) 0.0052(13) -0.0025(13) C87 0.050(2) 0.047(2) 0.0275(16) 0.0094(14) 0.0085(14) -0.0095(16) C88 0.058(2) 0.052(2) 0.0202(14) 0.0073(14) -0.0011(14) -0.0075(18) C89 0.0429(19) 0.0436(19) 0.0243(15) 0.0038(13) -0.0084(13) -0.0018(15) C90 0.0333(16) 0.0345(16) 0.0242(14) 0.0024(12) -0.0023(12) 0.0021(13) C91 0.0362(17) 0.0305(16) 0.0347(16) 0.0073(13) 0.0057(13) -0.0049(13) C92 0.041(2) 0.049(2) 0.0426(19) 0.0079(16) 0.0103(15) -0.0076(16) C93 0.042(2) 0.0349(19) 0.071(3) 0.0018(18) 0.0052(18) -0.0064(16) C94 0.0272(16) 0.062(2) 0.0289(15) 0.0001(15) 0.0002(12) 0.0023(15) C95 0.0320(18) 0.068(3) 0.0404(19) 0.0105(18) 0.0006(14) -0.0052(17) C96 0.043(2) 0.075(3) 0.058(2) -0.013(2) -0.0025(19) 0.015(2) C97 0.0209(13) 0.0302(15) 0.0223(13) -0.0003(11) -0.0036(10) -0.0022(11) C98 0.046(2) 0.0278(16) 0.0373(17) 0.0074(13) -0.0124(14) -0.0003(14) C99 0.047(2) 0.0277(16) 0.047(2) -0.0016(14) -0.0100(16) 0.0123(15) C100 0.0431(19) 0.0469(19) 0.0245(15) 0.0156(14) 0.0049(13) 0.0059(15) C101 0.045(2) 0.0435(19) 0.0366(17) 0.0149(15) 0.0210(15) 0.0070(16) C102 0.0325(17) 0.0399(18) 0.0399(17) 0.0113(14) 0.0099(14) -0.0001(14) C103 0.0384(18) 0.0301(16) 0.0386(17) 0.0058(13) 0.0077(14) 0.0027(13) C104 0.0365(17) 0.0345(17) 0.0363(16) 0.0124(13) 0.0087(13) 0.0077(14) C105 0.0296(15) 0.0323(15) 0.0183(12) 0.0058(11) -0.0032(11) 0.0005(12) C106 0.0335(17) 0.051(2) 0.0244(14) 0.0156(14) -0.0021(12) -0.0049(15) C107 0.041(2) 0.073(3) 0.0273(16) 0.0120(17) 0.0100(14) -0.0011(19) C108 0.055(2) 0.067(3) 0.0268(16) 0.0024(16) 0.0114(16) 0.009(2) C109 0.049(2) 0.047(2) 0.0284(16) -0.0054(14) 0.0016(14) -0.0026(17) C110 0.0324(16) 0.0356(16) 0.0220(13) 0.0028(12) -0.0026(11) -0.0010(13) C111 0.0357(19) 0.066(3) 0.0343(17) 0.0227(17) -0.0084(14) -0.0182(17) C112 0.067(3) 0.073(3) 0.059(3) 0.034(2) -0.022(2) -0.037(3) C113 0.036(2) 0.117(4) 0.042(2) 0.029(2) -0.0001(16) -0.024(2) C114 0.0296(16) 0.0387(17) 0.0296(15) -0.0008(13) -0.0034(12) -0.0077(13) C115 0.051(2) 0.052(2) 0.051(2) -0.0063(18) 0.0029(18) -0.0206(19) C116 0.035(2) 0.068(3) 0.056(2) 0.006(2) -0.0079(17) 0.0011(19) C117 0.0385(18) 0.0417(19) 0.0342(16) -0.0090(14) 0.0036(14) 0.0137(15) C118 0.044(2) 0.046(2) 0.0355(17) -0.0120(15) 0.0020(15) 0.0148(16) C119 0.057(3) 0.072(3) 0.0351(19) -0.0172(18) 0.0066(17) 0.019(2) C120 0.057(3) 0.085(3) 0.050(2) -0.013(2) 0.025(2) 0.021(2) C121 0.042(2) 0.075(3) 0.055(2) -0.012(2) 0.0198(18) 0.013(2) C122 0.0323(18) 0.052(2) 0.050(2) -0.0121(17) 0.0075(15) 0.0141(16) C123 0.042(2) 0.059(2) 0.0298(16) -0.0164(15) -0.0045(14) 0.0168(17) C124 0.048(2) 0.062(3) 0.042(2) -0.0089(18) -0.0048(16) 0.0100(19) C125 0.048(2) 0.060(2) 0.043(2) -0.0178(18) -0.0096(17) 0.0180(19) C126 0.0295(18) 0.068(3) 0.057(2) -0.013(2) 0.0046(16) 0.0094(18) C127 0.053(3) 0.099(4) 0.083(4) -0.011(3) -0.016(3) 0.029(3) C128 0.031(2) 0.097(4) 0.084(3) -0.017(3) 0.014(2) -0.006(2) N1 0.0265(12) 0.0259(12) 0.0177(10) 0.0004(9) 0.0026(9) 0.0014(9) N2 0.0255(12) 0.0281(12) 0.0185(11) 0.0032(9) -0.0025(9) -0.0013(10) N3 0.0218(11) 0.0246(12) 0.0237(11) 0.0001(9) 0.0019(9) 0.0007(9) N4 0.0236(12) 0.0263(12) 0.0220(11) -0.0010(9) 0.0018(9) 0.0014(9) N5 0.0243(12) 0.0291(12) 0.0178(10) -0.0027(9) 0.0000(9) 0.0005(10) N6 0.0259(12) 0.0303(13) 0.0166(10) -0.0008(9) -0.0009(9) 0.0001(10) N7 0.0285(13) 0.0277(13) 0.0241(12) 0.0045(10) -0.0056(9) -0.0009(10) N8 0.0315(14) 0.0310(13) 0.0293(13) -0.0047(10) -0.0038(10) 0.0067(11) Ni1 0.0250(2) 0.0252(2) 0.0195(2) 0.00157(18) 0.00134(18) -0.00115(19) Ni2 0.0235(2) 0.0226(2) 0.0232(2) -0.00052(18) 0.00069(18) 0.00050(19) Ni3 0.0273(3) 0.0257(2) 0.0197(2) -0.00195(18) -0.00034(18) -0.0005(2) Ni4 0.0238(2) 0.0307(3) 0.0202(2) 0.00523(19) 0.00425(18) 0.0054(2) Se1 0.02504(15) 0.03109(16) 0.02948(15) 0.00690(12) 0.00174(12) -0.00114(12) Se2 0.02620(15) 0.03311(16) 0.02336(14) -0.00248(12) 0.00100(11) -0.00551(12) Se3 0.02404(15) 0.02649(15) 0.03176(16) 0.00333(12) -0.00063(12) -0.00169(12) Se4 0.02781(16) 0.03198(16) 0.02652(15) 0.00257(12) 0.00384(12) 0.00662(12) Se5 0.03147(17) 0.03972(18) 0.02493(15) -0.00626(13) -0.00159(12) 0.01145(14) Se6 0.02450(15) 0.03744(17) 0.02563(15) 0.00610(12) 0.00176(11) 0.00430(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.361(4) . ? C1 N2 1.362(4) . ? C1 Ni1 1.888(3) . ? C2 C3 1.343(4) . ? C2 N1 1.386(4) . ? C3 N2 1.383(4) . ? C4 C5 1.414(5) . ? C4 C8 1.435(5) . ? C4 Ni1 2.103(3) . ? C5 C6 1.411(5) . ? C5 Ni1 2.176(3) . ? C6 C7 1.437(5) . ? C6 Ni1 2.121(3) . ? C7 C8 1.392(5) . ? C7 Ni1 2.142(3) . ? C8 Ni1 2.165(3) . ? C9 C10 1.405(4) . ? C9 C14 1.393(4) . ? C9 N1 1.445(4) . ? C10 C11 1.392(5) . ? C10 C15 1.513(5) . ? C11 C12 1.370(5) . ? C12 C13 1.385(5) . ? C13 C14 1.397(4) . ? C14 C18 1.515(4) . ? C15 C16 1.527(5) . ? C15 C17 1.537(5) . ? C18 C19 1.526(5) . ? C18 C20 1.537(5) . ? C21 C22 1.391(5) . ? C21 C26 1.396(5) . ? C21 N2 1.449(4) . ? C22 C23 1.394(5) . ? C22 C27 1.513(6) . ? C23 C24 1.359(7) . ? C24 C25 1.368(7) . ? C25 C26 1.406(5) . ? C26 C30 1.506(5) . ? C27 C28 1.535(6) . ? C27 C29 1.536(6) . ? C30 C31 1.531(5) . ? C30 C32 1.531(4) . ? C33 N3 1.374(4) . ? C33 N4 1.368(4) . ? C33 Ni2 1.877(3) . ? C34 C35 1.339(4) . ? C34 N3 1.385(4) . ? C35 N4 1.380(4) . ? C36 C37 1.383(5) . ? C36 C40 1.440(5) . ? C36 Ni2 2.172(3) . ? C37 C38 1.442(5) . ? C37 Ni2 2.138(3) . ? C38 C39 1.398(5) . ? C38 Ni2 2.089(3) . ? C39 C40 1.407(5) . ? C39 Ni2 2.164(3) . ? C40 Ni2 2.113(3) . ? C41 C42 1.402(4) . ? C41 C46 1.396(5) . ? C41 N3 1.453(4) . ? C42 C43 1.401(5) . ? C42 C47 1.509(5) . ? C43 C44 1.366(6) . ? C44 C45 1.366(6) . ? C45 C46 1.399(5) . ? C46 C50 1.511(5) . ? C47 C48 1.531(5) . ? C47 C49 1.532(5) . ? C50 C51 1.540(5) . ? C50 C52 1.533(5) . ? C53 C54 1.398(4) . ? C53 C58 1.405(4) . ? C53 N4 1.448(4) . ? C54 C55 1.396(5) . ? C54 C59 1.517(5) . ? C55 C56 1.375(5) . ? C56 C57 1.381(5) . ? C57 C58 1.392(4) . ? C58 C62 1.519(4) . ? C59 C60 1.530(5) . ? C59 C61 1.532(5) . ? C62 C63 1.508(6) . ? C62 C64 1.511(5) . ? C65 N5 1.374(3) . ? C65 N6 1.357(4) . ? C65 Ni3 1.885(3) . ? C66 C67 1.348(4) . ? C66 N5 1.380(4) . ? C67 N6 1.386(4) . ? C68 C69 1.453(5) . ? C68 C72 1.390(5) . ? C68 Ni3 2.091(3) . ? C69 C70 1.390(5) . ? C69 Ni3 2.123(3) . ? C70 C71 1.435(6) . ? C70 Ni3 2.159(3) . ? C71 C72 1.410(5) . ? C71 Ni3 2.099(3) . ? C72 Ni3 2.175(3) . ? C73 C74 1.409(4) . ? C73 C78 1.399(4) . ? C73 N5 1.440(4) . ? C74 C75 1.392(5) . ? C74 C79 1.521(5) . ? C75 C76 1.378(6) . ? C76 C77 1.378(5) . ? C77 C78 1.394(5) . ? C78 C82 1.520(4) . ? C79 C80 1.513(5) . ? C79 C81 1.528(6) . ? C82 C83 1.530(5) . ? C82 C84 1.531(5) . ? C85 C86 1.403(4) . ? C85 C90 1.390(5) . ? C85 N6 1.451(3) . ? C86 C87 1.401(5) . ? C86 C91 1.514(5) . ? C87 C88 1.372(6) . ? C88 C89 1.375(5) . ? C89 C90 1.393(4) . ? C90 C94 1.515(5) . ? C91 C92 1.537(5) . ? C91 C93 1.533(5) . ? C94 C95 1.534(6) . ? C94 C96 1.519(6) . ? C97 N7 1.364(4) . ? C97 N8 1.368(4) . ? C97 Ni4 1.868(3) . ? C98 C99 1.342(5) . ? C98 N7 1.386(4) . ? C99 N8 1.387(4) . ? C100 C101 1.392(5) . ? C100 C104 1.439(5) . ? C100 Ni4 2.145(3) . ? C101 C102 1.427(5) . ? C101 Ni4 2.183(3) . ? C102 C103 1.418(5) . ? C102 Ni4 2.121(3) . ? C103 C104 1.403(5) . ? C103 Ni4 2.161(3) . ? C104 Ni4 2.099(3) . ? C105 C106 1.402(5) . ? C105 C110 1.406(5) . ? C105 N7 1.454(4) . ? C106 C107 1.399(5) . ? C106 C111 1.505(5) . ? C107 C108 1.365(6) . ? C108 C109 1.393(6) . ? C109 C110 1.389(5) . ? C110 C114 1.519(4) . ? C111 C112 1.535(5) . ? C111 C113 1.527(6) . ? C114 C115 1.529(5) . ? C114 C116 1.523(5) . ? C117 C118 1.392(5) . ? C117 C122 1.393(6) . ? C117 N8 1.451(4) . ? C118 C119 1.406(6) . ? C118 C123 1.519(6) . ? C119 C120 1.369(7) . ? C120 C121 1.369(7) . ? C121 C122 1.397(6) . ? C122 C126 1.524(6) . ? C123 C124 1.524(6) . ? C123 C125 1.518(5) . ? C126 C127 1.526(7) . ? C126 C128 1.518(7) . ? Ni1 Se1 2.3068(6) . ? Ni2 Se3 2.2838(6) . ? Ni3 Se4 2.2847(6) . ? Ni4 Se6 2.3034(6) . ? Se1 Se2 2.3335(4) . ? Se2 Se3 2.3318(5) . ? Se4 Se5 2.3282(5) . ? Se5 Se6 2.3341(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 103.3(2) . . ? N1 C1 Ni1 129.0(2) . . ? N2 C1 Ni1 127.8(2) . . ? C3 C2 N1 106.9(3) . . ? C2 C3 N2 106.3(3) . . ? C5 C4 C8 109.3(3) . . ? C5 C4 Ni1 73.55(19) . . ? C8 C4 Ni1 72.73(18) . . ? C4 C5 Ni1 67.92(18) . . ? C6 C5 C4 106.6(3) . . ? C6 C5 Ni1 68.74(18) . . ? C5 C6 C7 108.3(3) . . ? C5 C6 Ni1 72.94(19) . . ? C7 C6 Ni1 71.06(18) . . ? C6 C7 Ni1 69.54(18) . . ? C8 C7 C6 108.5(3) . . ? C8 C7 Ni1 72.07(18) . . ? C4 C8 Ni1 68.01(18) . . ? C7 C8 C4 106.9(3) . . ? C7 C8 Ni1 70.22(19) . . ? C10 C9 N1 117.8(3) . . ? C14 C9 C10 123.4(3) . . ? C14 C9 N1 118.7(2) . . ? C9 C10 C15 122.7(3) . . ? C11 C10 C9 116.6(3) . . ? C11 C10 C15 120.6(3) . . ? C12 C11 C10 121.4(3) . . ? C11 C12 C13 120.8(3) . . ? C12 C13 C14 120.6(3) . . ? C9 C14 C13 117.1(3) . . ? C9 C14 C18 122.6(3) . . ? C13 C14 C18 120.2(3) . . ? C10 C15 C16 113.1(3) . . ? C10 C15 C17 110.8(3) . . ? C16 C15 C17 109.5(3) . . ? C14 C18 C19 112.9(3) . . ? C14 C18 C20 110.5(3) . . ? C19 C18 C20 110.4(3) . . ? C22 C21 C26 123.7(3) . . ? C22 C21 N2 117.1(3) . . ? C26 C21 N2 119.2(3) . . ? C21 C22 C23 117.2(4) . . ? C21 C22 C27 123.2(3) . . ? C23 C22 C27 119.6(4) . . ? C24 C23 C22 120.9(4) . . ? C23 C24 C25 121.0(3) . . ? C24 C25 C26 121.5(4) . . ? C21 C26 C25 115.7(4) . . ? C21 C26 C30 121.9(3) . . ? C25 C26 C30 122.4(3) . . ? C22 C27 C28 111.9(4) . . ? C22 C27 C29 111.7(4) . . ? C28 C27 C29 109.5(4) . . ? C26 C30 C31 110.2(3) . . ? C26 C30 C32 113.6(3) . . ? C31 C30 C32 110.2(3) . . ? N3 C33 Ni2 129.7(2) . . ? N4 C33 N3 103.2(2) . . ? N4 C33 Ni2 127.0(2) . . ? C35 C34 N3 106.8(3) . . ? C34 C35 N4 107.2(3) . . ? C37 C36 C40 107.3(3) . . ? C37 C36 Ni2 69.9(2) . . ? C40 C36 Ni2 68.15(18) . . ? C36 C37 C38 107.7(3) . . ? C36 C37 Ni2 72.6(2) . . ? C38 C37 Ni2 68.25(18) . . ? C37 C38 Ni2 71.87(19) . . ? C39 C38 C37 109.0(3) . . ? C39 C38 Ni2 73.71(19) . . ? C38 C39 C40 106.6(3) . . ? C38 C39 Ni2 67.96(18) . . ? C40 C39 Ni2 68.85(19) . . ? C36 C40 Ni2 72.60(19) . . ? C39 C40 C36 109.1(3) . . ? C39 C40 Ni2 72.8(2) . . ? C42 C41 N3 117.7(3) . . ? C46 C41 C42 122.9(3) . . ? C46 C41 N3 119.2(3) . . ? C41 C42 C47 121.8(3) . . ? C43 C42 C41 116.5(3) . . ? C43 C42 C47 121.6(3) . . ? C44 C43 C42 121.6(3) . . ? C45 C44 C43 120.6(3) . . ? C44 C45 C46 121.3(4) . . ? C41 C46 C45 117.0(3) . . ? C41 C46 C50 123.7(3) . . ? C45 C46 C50 119.2(3) . . ? C42 C47 C48 113.4(3) . . ? C42 C47 C49 110.7(3) . . ? C48 C47 C49 109.0(3) . . ? C46 C50 C51 108.9(3) . . ? C46 C50 C52 113.4(3) . . ? C52 C50 C51 109.6(3) . . ? C54 C53 C58 122.7(3) . . ? C54 C53 N4 117.6(3) . . ? C58 C53 N4 119.7(3) . . ? C53 C54 C59 123.1(3) . . ? C55 C54 C53 117.5(3) . . ? C55 C54 C59 119.4(3) . . ? C56 C55 C54 121.2(3) . . ? C55 C56 C57 120.0(3) . . ? C56 C57 C58 121.8(3) . . ? C53 C58 C62 122.6(3) . . ? C57 C58 C53 116.8(3) . . ? C57 C58 C62 120.6(3) . . ? C54 C59 C60 113.0(3) . . ? C54 C59 C61 110.0(3) . . ? C60 C59 C61 109.6(3) . . ? C63 C62 C58 111.4(3) . . ? C63 C62 C64 108.7(4) . . ? C64 C62 C58 112.8(3) . . ? N5 C65 Ni3 126.4(2) . . ? N6 C65 N5 103.5(2) . . ? N6 C65 Ni3 129.9(2) . . ? C67 C66 N5 107.2(3) . . ? C66 C67 N6 106.3(3) . . ? C69 C68 Ni3 71.03(18) . . ? C72 C68 C69 109.0(3) . . ? C72 C68 Ni3 74.3(2) . . ? C68 C69 Ni3 68.65(18) . . ? C70 C69 C68 107.1(3) . . ? C70 C69 Ni3 72.5(2) . . ? C69 C70 C71 107.5(3) . . ? C69 C70 Ni3 69.66(18) . . ? C71 C70 Ni3 68.06(19) . . ? C70 C71 Ni3 72.6(2) . . ? C72 C71 C70 108.9(3) . . ? C72 C71 Ni3 73.7(2) . . ? C68 C72 C71 106.9(3) . . ? C68 C72 Ni3 67.74(19) . . ? C71 C72 Ni3 67.85(19) . . ? C74 C73 N5 117.9(3) . . ? C78 C73 C74 122.3(3) . . ? C78 C73 N5 119.8(3) . . ? C73 C74 C79 121.7(3) . . ? C75 C74 C73 117.3(3) . . ? C75 C74 C79 121.1(3) . . ? C76 C75 C74 121.4(3) . . ? C77 C76 C75 120.2(3) . . ? C76 C77 C78 121.2(3) . . ? C73 C78 C82 123.4(3) . . ? C77 C78 C73 117.5(3) . . ? C77 C78 C82 119.1(3) . . ? C74 C79 C81 111.1(3) . . ? C80 C79 C74 113.5(3) . . ? C80 C79 C81 109.3(3) . . ? C78 C82 C83 112.9(3) . . ? C78 C82 C84 109.6(3) . . ? C83 C82 C84 108.8(3) . . ? C86 C85 N6 118.5(3) . . ? C90 C85 C86 123.3(3) . . ? C90 C85 N6 118.2(3) . . ? C85 C86 C91 123.2(3) . . ? C87 C86 C85 116.3(3) . . ? C87 C86 C91 120.5(3) . . ? C88 C87 C86 121.4(3) . . ? C87 C88 C89 120.7(3) . . ? C88 C89 C90 120.6(3) . . ? C85 C90 C89 117.6(3) . . ? C85 C90 C94 122.7(3) . . ? C89 C90 C94 119.4(3) . . ? C86 C91 C92 113.2(3) . . ? C86 C91 C93 110.3(3) . . ? C93 C91 C92 109.4(3) . . ? C90 C94 C95 113.0(3) . . ? C90 C94 C96 108.3(3) . . ? C96 C94 C95 109.9(3) . . ? N7 C97 N8 103.6(3) . . ? N7 C97 Ni4 130.1(2) . . ? N8 C97 Ni4 125.7(2) . . ? C99 C98 N7 107.4(3) . . ? C98 C99 N8 106.3(3) . . ? C101 C100 C104 107.8(3) . . ? C101 C100 Ni4 72.72(18) . . ? C104 C100 Ni4 68.48(17) . . ? C100 C101 C102 107.7(3) . . ? C100 C101 Ni4 69.77(18) . . ? C102 C101 Ni4 68.33(18) . . ? C101 C102 Ni4 73.0(2) . . ? C103 C102 C101 108.7(3) . . ? C103 C102 Ni4 72.2(2) . . ? C102 C103 Ni4 69.2(2) . . ? C104 C103 C102 106.9(3) . . ? C104 C103 Ni4 68.4(2) . . ? C100 C104 Ni4 71.89(19) . . ? C103 C104 C100 108.5(3) . . ? C103 C104 Ni4 73.16(19) . . ? C106 C105 C110 122.3(3) . . ? C106 C105 N7 119.7(3) . . ? C110 C105 N7 118.0(3) . . ? C105 C106 C111 123.4(3) . . ? C107 C106 C105 117.2(3) . . ? C107 C106 C111 119.3(3) . . ? C108 C107 C106 121.7(3) . . ? C107 C108 C109 120.1(4) . . ? C110 C109 C108 121.0(4) . . ? C105 C110 C114 122.4(3) . . ? C109 C110 C105 117.7(3) . . ? C109 C110 C114 119.7(3) . . ? C106 C111 C112 110.0(3) . . ? C106 C111 C113 112.6(4) . . ? C113 C111 C112 109.1(3) . . ? C110 C114 C115 113.6(3) . . ? C110 C114 C116 109.8(3) . . ? C116 C114 C115 110.3(3) . . ? C118 C117 C122 123.1(3) . . ? C118 C117 N8 119.5(3) . . ? C122 C117 N8 117.3(3) . . ? C117 C118 C119 116.7(4) . . ? C117 C118 C123 121.7(3) . . ? C119 C118 C123 121.6(3) . . ? C120 C119 C118 121.2(4) . . ? C121 C120 C119 120.7(4) . . ? C120 C121 C122 121.0(4) . . ? C117 C122 C121 117.3(4) . . ? C117 C122 C126 122.8(4) . . ? C121 C122 C126 119.9(4) . . ? C118 C123 C124 109.9(3) . . ? C125 C123 C118 113.1(4) . . ? C125 C123 C124 110.9(3) . . ? C122 C126 C127 110.7(4) . . ? C128 C126 C122 113.3(4) . . ? C128 C126 C127 110.6(4) . . ? C1 N1 C2 111.5(2) . . ? C1 N1 C9 126.1(2) . . ? C2 N1 C9 122.3(2) . . ? C1 N2 C3 112.0(2) . . ? C1 N2 C21 125.5(2) . . ? C3 N2 C21 121.6(2) . . ? C33 N3 C34 111.2(2) . . ? C33 N3 C41 126.0(2) . . ? C34 N3 C41 122.6(2) . . ? C33 N4 C35 111.5(2) . . ? C33 N4 C53 125.6(2) . . ? C35 N4 C53 122.2(2) . . ? C65 N5 C66 111.0(2) . . ? C65 N5 C73 125.0(2) . . ? C66 N5 C73 123.8(2) . . ? C65 N6 C67 111.9(2) . . ? C65 N6 C85 125.6(2) . . ? C67 N6 C85 122.4(3) . . ? C97 N7 C98 111.0(3) . . ? C97 N7 C105 125.5(3) . . ? C98 N7 C105 123.0(3) . . ? C97 N8 C99 111.5(3) . . ? C97 N8 C117 123.5(3) . . ? C99 N8 C117 123.9(3) . . ? C1 Ni1 C4 102.91(12) . . ? C1 Ni1 C5 125.23(12) . . ? C1 Ni1 C6 163.43(12) . . ? C1 Ni1 C7 147.51(13) . . ? C1 Ni1 C8 113.59(13) . . ? C1 Ni1 Se1 92.76(9) . . ? C4 Ni1 C5 38.53(14) . . ? C4 Ni1 C6 64.84(13) . . ? C4 Ni1 C7 64.68(12) . . ? C4 Ni1 C8 39.26(13) . . ? C4 Ni1 Se1 161.63(10) . . ? C5 Ni1 Se1 123.65(10) . . ? C6 Ni1 C5 38.31(12) . . ? C6 Ni1 C7 39.39(13) . . ? C6 Ni1 C8 64.77(14) . . ? C6 Ni1 Se1 97.80(9) . . ? C7 Ni1 C5 64.66(13) . . ? C7 Ni1 C8 37.72(13) . . ? C7 Ni1 Se1 106.32(10) . . ? C8 Ni1 C5 64.71(13) . . ? C8 Ni1 Se1 140.46(9) . . ? C33 Ni2 C36 114.53(13) . . ? C33 Ni2 C37 146.40(13) . . ? C33 Ni2 C38 166.97(13) . . ? C33 Ni2 C39 128.76(13) . . ? C33 Ni2 C40 105.95(13) . . ? C33 Ni2 Se3 89.75(9) . . ? C36 Ni2 Se3 138.59(11) . . ? C37 Ni2 C36 37.42(15) . . ? C37 Ni2 C39 65.05(14) . . ? C37 Ni2 Se3 105.42(11) . . ? C38 Ni2 C36 64.70(13) . . ? C38 Ni2 C37 39.87(14) . . ? C38 Ni2 C39 38.33(14) . . ? C38 Ni2 C40 64.71(14) . . ? C38 Ni2 Se3 98.76(10) . . ? C39 Ni2 C36 64.68(14) . . ? C39 Ni2 Se3 125.83(10) . . ? C40 Ni2 C36 39.25(15) . . ? C40 Ni2 C37 64.66(14) . . ? C40 Ni2 C39 38.40(14) . . ? C40 Ni2 Se3 163.11(10) . . ? C65 Ni3 C68 162.74(13) . . ? C65 Ni3 C69 146.50(12) . . ? C65 Ni3 C70 112.64(13) . . ? C65 Ni3 C71 101.92(13) . . ? C65 Ni3 C72 124.84(13) . . ? C65 Ni3 Se4 95.50(8) . . ? C68 Ni3 C69 40.32(13) . . ? C68 Ni3 C70 65.10(13) . . ? C68 Ni3 C71 64.97(14) . . ? C68 Ni3 C72 37.98(14) . . ? C68 Ni3 Se4 96.68(10) . . ? C69 Ni3 C70 37.88(14) . . ? C69 Ni3 C72 65.15(14) . . ? C69 Ni3 Se4 102.83(10) . . ? C70 Ni3 C72 64.56(14) . . ? C70 Ni3 Se4 136.84(11) . . ? C71 Ni3 C69 65.33(15) . . ? C71 Ni3 C70 39.36(16) . . ? C71 Ni3 C72 38.48(15) . . ? C71 Ni3 Se4 161.47(11) . . ? C72 Ni3 Se4 124.53(10) . . ? C97 Ni4 C100 145.36(13) . . ? C97 Ni4 C101 114.65(13) . . ? C97 Ni4 C102 107.58(13) . . ? C97 Ni4 C103 131.34(13) . . ? C97 Ni4 C104 169.67(14) . . ? C97 Ni4 Se6 86.69(9) . . ? C100 Ni4 C101 37.51(14) . . ? C100 Ni4 C103 64.81(14) . . ? C100 Ni4 Se6 107.43(10) . . ? C101 Ni4 Se6 140.73(11) . . ? C102 Ni4 C100 64.47(14) . . ? C102 Ni4 C101 38.68(15) . . ? C102 Ni4 C103 38.67(13) . . ? C102 Ni4 Se6 164.30(10) . . ? C103 Ni4 C101 64.33(14) . . ? C103 Ni4 Se6 126.28(9) . . ? C104 Ni4 C100 39.63(13) . . ? C104 Ni4 C101 64.57(13) . . ? C104 Ni4 C102 64.94(14) . . ? C104 Ni4 C103 38.41(14) . . ? C104 Ni4 Se6 100.03(10) . . ? Ni1 Se1 Se2 108.480(19) . . ? Se3 Se2 Se1 109.177(17) . . ? Ni2 Se3 Se2 110.94(2) . . ? Ni3 Se4 Se5 110.15(2) . . ? Se4 Se5 Se6 108.352(17) . . ? Ni4 Se6 Se5 109.006(19) . . ? _shelx_res_file ; TITL mP21n in P2(1)/n CELL 1.54178 16.8208 18.4669 39.0547 90.000 96.196 90.000 ZERR 8.00 0.0006 0.0010 0.0010 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N NI SE UNIT 512 656 32 16 24 MERG 2 FMAP 2 PLAN 20 ACTA L.S. 30 WGHT 0.045700 12.602000 FVAR 0.09854 C1 1 1.009545 0.386440 0.858636 11.00000 0.02449 0.02715 = 0.01685 0.00077 0.00271 0.00442 C2 1 1.060353 0.484402 0.833403 11.00000 0.03446 0.02779 = 0.02326 0.00260 0.00532 -0.00202 AFIX 43 H2 2 1.071135 0.517556 0.816584 11.00000 -1.20000 AFIX 0 C3 1 1.088050 0.486607 0.866947 11.00000 0.02789 0.02826 = 0.02609 -0.00088 0.00082 -0.00372 AFIX 43 H3 2 1.121690 0.521448 0.877900 11.00000 -1.20000 AFIX 0 C4 1 1.037997 0.219257 0.861221 11.00000 0.03140 0.03187 = 0.03834 0.00376 0.00981 0.00295 AFIX 43 H4 2 1.085956 0.230544 0.852640 11.00000 -1.20000 AFIX 0 C5 1 0.966976 0.197529 0.841197 11.00000 0.03815 0.03167 = 0.03301 -0.00583 0.00726 0.00103 AFIX 43 H5 2 0.960908 0.187636 0.817712 11.00000 -1.20000 AFIX 0 C6 1 0.907076 0.193780 0.863805 11.00000 0.03195 0.02781 = 0.03989 -0.00182 0.00648 -0.00373 AFIX 43 H6 2 0.853163 0.184377 0.857506 11.00000 -1.20000 AFIX 0 C7 1 0.943601 0.206971 0.898218 11.00000 0.04265 0.02919 = 0.03074 0.00904 0.00875 0.00180 AFIX 43 H7 2 0.917590 0.206163 0.918053 11.00000 -1.20000 AFIX 0 C8 1 1.024492 0.221166 0.896863 11.00000 0.03828 0.03261 = 0.03276 0.00612 -0.00101 0.00652 AFIX 43 H8 2 1.062488 0.230160 0.915490 11.00000 -1.20000 AFIX 0 C9 1 0.976847 0.400892 0.794995 11.00000 0.03283 0.02493 = 0.01486 0.00069 0.00444 -0.00163 C10 1 1.020370 0.353051 0.776146 11.00000 0.03555 0.03047 = 0.02220 0.00241 0.00878 0.00366 C11 1 0.986020 0.334727 0.743263 11.00000 0.04563 0.04284 = 0.02237 -0.00833 0.00816 0.00570 AFIX 43 H11 2 1.012552 0.302617 0.730092 11.00000 -1.20000 AFIX 0 C12 1 0.913988 0.362958 0.729878 11.00000 0.04838 0.04515 = 0.01846 -0.00566 0.00036 -0.00169 AFIX 43 H12 2 0.892519 0.349905 0.707798 11.00000 -1.20000 AFIX 0 C13 1 0.872758 0.410709 0.748842 11.00000 0.03376 0.03664 = 0.02015 -0.00037 -0.00193 -0.00189 AFIX 43 H13 2 0.823883 0.429331 0.739390 11.00000 -1.20000 AFIX 0 C14 1 0.903921 0.431164 0.782045 11.00000 0.03060 0.02495 = 0.01706 0.00175 0.00210 -0.00157 C15 1 1.102268 0.324950 0.789632 11.00000 0.03735 0.04155 = 0.02757 0.00268 0.00889 0.00964 AFIX 13 H15 2 1.106571 0.326624 0.814845 11.00000 -1.20000 AFIX 0 C16 1 1.116379 0.246806 0.779061 11.00000 0.05206 0.04373 = 0.04162 0.00480 0.01856 0.01594 AFIX 33 H16A 2 1.169039 0.231907 0.788304 11.00000 -1.50000 H16B 2 1.111571 0.243471 0.754394 11.00000 -1.50000 H16C 2 1.077402 0.215900 0.787837 11.00000 -1.50000 AFIX 0 C17 1 1.168211 0.373662 0.777858 11.00000 0.04135 0.05027 = 0.05995 0.00754 0.01180 0.00672 AFIX 33 H17A 2 1.219622 0.354984 0.786701 11.00000 -1.50000 H17B 2 1.162201 0.421906 0.786366 11.00000 -1.50000 H17C 2 1.164009 0.374529 0.753151 11.00000 -1.50000 AFIX 0 C18 1 0.860523 0.486442 0.801841 11.00000 0.03184 0.02897 = 0.02118 -0.00034 -0.00132 0.00162 AFIX 13 H18 2 0.875899 0.478027 0.826441 11.00000 -1.20000 AFIX 0 C19 1 0.769734 0.479684 0.795376 11.00000 0.03449 0.04080 = 0.03318 0.00160 0.00313 0.00705 AFIX 33 H19A 2 0.745303 0.515629 0.808590 11.00000 -1.50000 H19B 2 0.753788 0.432335 0.802140 11.00000 -1.50000 H19C 2 0.752990 0.486836 0.771330 11.00000 -1.50000 AFIX 0 C20 1 0.886940 0.563531 0.793509 11.00000 0.04712 0.03069 = 0.03744 -0.00040 -0.00126 0.00083 AFIX 33 H20A 2 0.859138 0.597869 0.806319 11.00000 -1.50000 H20B 2 0.874688 0.572570 0.769308 11.00000 -1.50000 H20C 2 0.943497 0.568315 0.799694 11.00000 -1.50000 AFIX 0 C21 1 1.083855 0.405007 0.916912 11.00000 0.03607 0.03013 = 0.02217 0.00473 -0.00595 -0.00558 C22 1 1.159926 0.374957 0.922692 11.00000 0.03924 0.03552 = 0.04342 0.00769 -0.01443 -0.00397 C23 1 1.187152 0.355971 0.956483 11.00000 0.05258 0.04717 = 0.05401 0.01641 -0.02569 -0.00822 AFIX 43 H23 2 1.237876 0.336008 0.961333 11.00000 -1.20000 AFIX 0 C24 1 1.140627 0.366220 0.982433 11.00000 0.07634 0.05275 = 0.03633 0.02131 -0.02954 -0.02545 AFIX 43 H24 2 1.159962 0.353122 1.004783 11.00000 -1.20000 AFIX 0 C25 1 1.065751 0.395528 0.976169 11.00000 0.07089 0.05021 = 0.02173 0.00611 -0.00444 -0.02744 AFIX 43 H25 2 1.034618 0.400869 0.994291 11.00000 -1.20000 AFIX 0 C26 1 1.034832 0.417751 0.942937 11.00000 0.04941 0.03240 = 0.01985 0.00065 -0.00167 -0.01751 C27 1 1.214212 0.365065 0.894564 11.00000 0.03280 0.05594 = 0.06156 0.00450 -0.00662 0.01064 AFIX 13 H27 2 1.182340 0.373345 0.872392 11.00000 -1.20000 AFIX 0 C28 1 1.248314 0.287980 0.894264 11.00000 0.04095 0.05949 = 0.09956 -0.00157 -0.00257 0.01157 AFIX 33 H28A 2 1.282047 0.283692 0.876047 11.00000 -1.50000 H28B 2 1.205200 0.253831 0.890617 11.00000 -1.50000 H28C 2 1.279018 0.278215 0.915942 11.00000 -1.50000 AFIX 0 C29 1 1.283176 0.419972 0.897852 11.00000 0.04407 0.06601 = 0.08479 0.01082 0.00614 -0.00026 AFIX 33 H29A 2 1.316139 0.412398 0.879580 11.00000 -1.50000 H29B 2 1.314684 0.413628 0.919644 11.00000 -1.50000 H29C 2 1.261819 0.468215 0.896387 11.00000 -1.50000 AFIX 0 C30 1 0.955055 0.454937 0.935873 11.00000 0.04161 0.04755 = 0.02318 -0.00538 0.00842 -0.01662 AFIX 13 H30 2 0.929290 0.436279 0.913936 11.00000 -1.20000 AFIX 0 C31 1 0.966777 0.536517 0.931613 11.00000 0.05327 0.04502 = 0.03435 0.00331 0.01600 -0.00235 AFIX 33 H31A 2 0.915581 0.559586 0.927067 11.00000 -1.50000 H31B 2 0.997658 0.545134 0.912732 11.00000 -1.50000 H31C 2 0.994444 0.555993 0.952369 11.00000 -1.50000 AFIX 0 C32 1 0.898540 0.440431 0.963313 11.00000 0.06113 0.05678 = 0.03750 -0.01391 0.02330 -0.02632 AFIX 33 H32A 2 0.848985 0.465487 0.957317 11.00000 -1.50000 H32B 2 0.922670 0.457337 0.985257 11.00000 -1.50000 H32C 2 0.888525 0.389373 0.964571 11.00000 -1.50000 AFIX 0 C33 1 0.571361 0.137871 0.852258 11.00000 0.02108 0.02673 = 0.02049 -0.00030 0.00034 0.00173 C34 1 0.573518 0.014763 0.849215 11.00000 0.02740 0.02395 = 0.03164 -0.00132 0.00467 0.00017 AFIX 43 H34 2 0.575180 -0.033599 0.855895 11.00000 -1.20000 AFIX 0 C35 1 0.569705 0.040046 0.816957 11.00000 0.02755 0.02784 = 0.02841 -0.00526 0.00346 0.00061 AFIX 43 H35 2 0.568364 0.012481 0.796974 11.00000 -1.20000 AFIX 0 C36 1 0.519269 0.312247 0.831737 11.00000 0.04986 0.03239 = 0.03467 0.00444 -0.00336 0.01614 AFIX 43 H36 2 0.516545 0.310808 0.807836 11.00000 -1.20000 AFIX 0 C37 1 0.577661 0.345961 0.853802 11.00000 0.04401 0.02247 = 0.05270 0.00524 0.00566 0.00008 AFIX 43 H37 2 0.622032 0.370544 0.847440 11.00000 -1.20000 AFIX 0 C38 1 0.557391 0.336155 0.888449 11.00000 0.03673 0.02774 = 0.04206 -0.00793 -0.00252 0.00773 AFIX 43 H38 2 0.587788 0.351949 0.908352 11.00000 -1.20000 AFIX 0 C39 1 0.484681 0.299078 0.887300 11.00000 0.03476 0.03297 = 0.04724 -0.00335 0.01182 0.00909 AFIX 43 H39 2 0.455962 0.289120 0.905806 11.00000 -1.20000 AFIX 0 C40 1 0.463457 0.279775 0.852660 11.00000 0.02865 0.03058 = 0.05483 -0.00377 -0.00671 0.00635 AFIX 43 H40 2 0.420313 0.250713 0.844576 11.00000 -1.20000 AFIX 0 C41 1 0.573205 0.068103 0.907759 11.00000 0.03126 0.02360 = 0.02357 0.00066 0.00365 -0.00175 C42 1 0.500257 0.080098 0.921113 11.00000 0.03428 0.02459 = 0.03448 0.00007 0.01034 -0.00405 C43 1 0.500372 0.072139 0.956789 11.00000 0.05420 0.03820 = 0.04149 0.00007 0.02302 -0.00659 AFIX 43 H43 2 0.453275 0.080045 0.966699 11.00000 -1.20000 AFIX 0 C44 1 0.567970 0.053047 0.977383 11.00000 0.06986 0.04938 = 0.02866 0.00739 0.00998 -0.00937 AFIX 43 H44 2 0.566529 0.049136 1.001049 11.00000 -1.20000 AFIX 0 C45 1 0.637642 0.039659 0.963506 11.00000 0.05503 0.04688 = 0.02967 0.00993 -0.00629 -0.00746 AFIX 43 H45 2 0.682871 0.026083 0.977888 11.00000 -1.20000 AFIX 0 C46 1 0.642306 0.045966 0.928077 11.00000 0.03622 0.02907 = 0.03202 0.00720 -0.00114 -0.00321 C47 1 0.424743 0.097638 0.898166 11.00000 0.02813 0.03301 = 0.05051 0.00154 0.01147 0.00116 AFIX 13 H47 2 0.438953 0.130172 0.879959 11.00000 -1.20000 AFIX 0 C48 1 0.361391 0.135576 0.917105 11.00000 0.03952 0.04169 = 0.09133 -0.01149 0.02010 0.00318 AFIX 33 H48A 2 0.314922 0.145165 0.901242 11.00000 -1.50000 H48B 2 0.382565 0.180389 0.926634 11.00000 -1.50000 H48C 2 0.346958 0.104963 0.935316 11.00000 -1.50000 AFIX 0 C49 1 0.388345 0.028916 0.880971 11.00000 0.02681 0.04591 = 0.05797 -0.00823 0.00556 -0.00067 AFIX 33 H49A 2 0.340561 0.041185 0.866423 11.00000 -1.50000 H49B 2 0.375547 -0.004586 0.898355 11.00000 -1.50000 H49C 2 0.426120 0.007092 0.867362 11.00000 -1.50000 AFIX 0 C50 1 0.718761 0.024581 0.913677 11.00000 0.03103 0.03689 = 0.04584 0.01333 -0.00327 0.00162 AFIX 13 H50 2 0.715689 0.041271 0.889751 11.00000 -1.20000 AFIX 0 C51 1 0.725367 -0.058581 0.913813 11.00000 0.04417 0.04174 = 0.06346 0.01442 -0.00174 0.00884 AFIX 33 H51A 2 0.773707 -0.072701 0.904605 11.00000 -1.50000 H51B 2 0.680205 -0.078787 0.899924 11.00000 -1.50000 H51C 2 0.726306 -0.076106 0.936995 11.00000 -1.50000 AFIX 0 C52 1 0.793904 0.057272 0.933496 11.00000 0.02987 0.05049 = 0.07373 0.02298 -0.01216 -0.00103 AFIX 33 H52A 2 0.840274 0.041835 0.923133 11.00000 -1.50000 H52B 2 0.798078 0.041308 0.957015 11.00000 -1.50000 H52C 2 0.790417 0.109147 0.932752 11.00000 -1.50000 AFIX 0 C53 1 0.551748 0.159758 0.788613 11.00000 0.03019 0.02998 = 0.01743 -0.00292 0.00010 0.00064 C54 1 0.473538 0.160392 0.772315 11.00000 0.02979 0.03639 = 0.02334 -0.00340 -0.00049 0.00266 C55 1 0.458125 0.203098 0.742854 11.00000 0.03382 0.04678 = 0.02710 -0.00143 -0.00795 0.00303 AFIX 43 H55 2 0.406489 0.205082 0.731659 11.00000 -1.20000 AFIX 0 C56 1 0.517860 0.242284 0.730078 11.00000 0.04950 0.04486 = 0.02247 0.00434 -0.00478 0.00023 AFIX 43 H56 2 0.506494 0.270353 0.710388 11.00000 -1.20000 AFIX 0 C57 1 0.594763 0.239929 0.746511 11.00000 0.04385 0.03855 = 0.02099 0.00005 0.00161 -0.00679 AFIX 43 H57 2 0.634640 0.266581 0.737562 11.00000 -1.20000 AFIX 0 C58 1 0.614249 0.198787 0.776089 11.00000 0.03035 0.03309 = 0.02243 -0.00259 -0.00023 -0.00211 C59 1 0.406286 0.116326 0.784878 11.00000 0.02711 0.04511 = 0.03191 -0.00514 0.00177 0.00022 AFIX 13 H59 2 0.423611 0.100179 0.808407 11.00000 -1.20000 AFIX 0 C60 1 0.328907 0.159629 0.785574 11.00000 0.03022 0.05984 = 0.04693 -0.00855 0.00150 0.00325 AFIX 33 H60A 2 0.288625 0.129306 0.793759 11.00000 -1.50000 H60B 2 0.310973 0.176260 0.762754 11.00000 -1.50000 H60C 2 0.338584 0.200486 0.800647 11.00000 -1.50000 AFIX 0 C61 1 0.390052 0.048990 0.762274 11.00000 0.03313 0.05247 = 0.04864 -0.01203 0.00585 -0.00844 AFIX 33 H61A 2 0.347752 0.021218 0.770492 11.00000 -1.50000 H61B 2 0.437623 0.020006 0.763263 11.00000 -1.50000 H61C 2 0.374611 0.063561 0.738906 11.00000 -1.50000 AFIX 0 C62 1 0.699455 0.197041 0.793520 11.00000 0.02997 0.04403 = 0.02327 0.00025 -0.00017 -0.00674 AFIX 13 H62 2 0.697049 0.194336 0.818447 11.00000 -1.20000 AFIX 0 C63 1 0.743891 0.131273 0.782856 11.00000 0.02855 0.05431 = 0.11059 -0.02097 -0.01324 0.00066 AFIX 33 H63A 2 0.714508 0.088383 0.787375 11.00000 -1.50000 H63B 2 0.795832 0.129500 0.795705 11.00000 -1.50000 H63C 2 0.749618 0.134071 0.758700 11.00000 -1.50000 AFIX 0 C64 1 0.746605 0.263879 0.786212 11.00000 0.05438 0.04975 = 0.06910 0.00595 -0.01899 -0.02205 AFIX 33 H64A 2 0.799713 0.260200 0.797850 11.00000 -1.50000 H64B 2 0.720742 0.305945 0.794280 11.00000 -1.50000 H64C 2 0.749317 0.267961 0.761860 11.00000 -1.50000 AFIX 0 C65 1 0.971063 0.118388 1.111886 11.00000 0.01992 0.03117 = 0.01757 0.00003 0.00063 -0.00185 C66 1 0.990124 0.018240 1.080078 11.00000 0.03336 0.03137 = 0.02316 -0.00548 -0.00111 0.00121 AFIX 43 H66 2 0.993625 -0.011700 1.061152 11.00000 -1.20000 AFIX 0 C67 1 1.005426 -0.000672 1.113483 11.00000 0.03481 0.02584 = 0.02878 -0.00099 -0.00055 0.00367 AFIX 43 H67 2 1.021502 -0.045934 1.122080 11.00000 -1.20000 AFIX 0 C68 1 0.977302 0.323486 1.138991 11.00000 0.03761 0.02915 = 0.03476 -0.00662 -0.00250 -0.00491 AFIX 43 H68 2 0.959036 0.341055 1.159043 11.00000 -1.20000 AFIX 0 C69 1 0.932100 0.322964 1.105131 11.00000 0.04458 0.02488 = 0.03455 0.00463 -0.00504 -0.00359 AFIX 43 H69 2 0.880946 0.341460 1.099467 11.00000 -1.20000 AFIX 0 C70 1 0.979693 0.289613 1.082783 11.00000 0.05809 0.03234 = 0.02914 0.00392 0.00466 -0.01314 AFIX 43 H70 2 0.967001 0.283272 1.059204 11.00000 -1.20000 AFIX 0 C71 1 1.051976 0.266759 1.102740 11.00000 0.03710 0.03776 = 0.05514 -0.00415 0.01435 -0.01070 AFIX 43 H71 2 1.092065 0.238880 1.094672 11.00000 -1.20000 AFIX 0 C72 1 1.052296 0.293469 1.136573 11.00000 0.03268 0.03618 = 0.04931 -0.00700 -0.00581 -0.00933 AFIX 43 H72 2 1.094610 0.291404 1.153961 11.00000 -1.20000 AFIX 0 C73 1 0.940919 0.128801 1.048074 11.00000 0.03011 0.03175 = 0.01610 -0.00358 -0.00115 0.00153 C74 1 0.858357 0.142781 1.041281 11.00000 0.03199 0.04320 = 0.01968 -0.00606 -0.00020 0.00603 C75 1 0.833373 0.183745 1.012191 11.00000 0.03802 0.06222 = 0.02445 -0.00316 -0.00375 0.01718 AFIX 43 H75 2 0.779343 0.194429 1.007166 11.00000 -1.20000 AFIX 0 C76 1 0.887063 0.208812 0.990672 11.00000 0.05322 0.05893 = 0.02324 0.00734 -0.00277 0.01901 AFIX 43 H76 2 0.869286 0.237507 0.971818 11.00000 -1.20000 AFIX 0 C77 1 0.966976 0.191503 0.996999 11.00000 0.04589 0.05178 = 0.02118 0.00635 0.00502 0.00586 AFIX 43 H77 2 1.002231 0.207096 0.981761 11.00000 -1.20000 AFIX 0 C78 1 0.995992 0.151050 1.025816 11.00000 0.03200 0.03767 = 0.01947 -0.00283 -0.00028 -0.00011 C79 1 0.798374 0.112401 1.064009 11.00000 0.02686 0.05831 = 0.02671 -0.01042 0.00169 0.00159 AFIX 13 H79 2 0.820473 0.119581 1.088028 11.00000 -1.20000 AFIX 0 C80 1 0.717850 0.149665 1.059099 11.00000 0.03299 0.07006 = 0.05299 -0.01769 0.00955 0.00733 AFIX 33 H80A 2 0.682945 0.128249 1.074159 11.00000 -1.50000 H80B 2 0.695024 0.144177 1.035633 11.00000 -1.50000 H80C 2 0.724485 0.200216 1.064389 11.00000 -1.50000 AFIX 0 C81 1 0.786828 0.031061 1.058304 11.00000 0.03312 0.05855 = 0.04740 -0.00178 0.01004 -0.00299 AFIX 33 H81A 2 0.748957 0.013177 1.072968 11.00000 -1.50000 H81B 2 0.837055 0.006724 1.063685 11.00000 -1.50000 H81C 2 0.767218 0.022174 1.034676 11.00000 -1.50000 AFIX 0 C82 1 1.084362 0.131920 1.031111 11.00000 0.02863 0.04108 = 0.02387 0.00220 -0.00003 -0.00245 AFIX 13 H82 2 1.096825 0.112991 1.054518 11.00000 -1.20000 AFIX 0 C83 1 1.138619 0.196941 1.026589 11.00000 0.04247 0.04936 = 0.04250 0.00302 0.00850 -0.00621 AFIX 33 H83A 2 1.193537 0.181981 1.030254 11.00000 -1.50000 H83B 2 1.128991 0.233773 1.042991 11.00000 -1.50000 H83C 2 1.127376 0.215869 1.003685 11.00000 -1.50000 AFIX 0 C84 1 1.102296 0.072862 1.005521 11.00000 0.03413 0.04900 = 0.03576 -0.00008 0.00348 0.00413 AFIX 33 H84A 2 1.158064 0.060668 1.008989 11.00000 -1.50000 H84B 2 1.089156 0.090236 0.982436 11.00000 -1.50000 H84C 2 1.070912 0.030653 1.009092 11.00000 -1.50000 AFIX 0 C85 1 1.005926 0.062236 1.169775 11.00000 0.03144 0.02979 = 0.01894 0.00294 0.00012 0.00095 C86 1 0.942851 0.042657 1.188631 11.00000 0.03884 0.02948 = 0.02714 0.00698 0.00523 -0.00249 C87 1 0.959212 0.044308 1.224566 11.00000 0.05009 0.04731 = 0.02745 0.00938 0.00849 -0.00950 AFIX 43 H87 2 0.918832 0.032785 1.238129 11.00000 -1.20000 AFIX 0 C88 1 1.033477 0.062547 1.240182 11.00000 0.05823 0.05176 = 0.02020 0.00728 -0.00114 -0.00753 AFIX 43 H88 2 1.042543 0.063620 1.264092 11.00000 -1.20000 AFIX 0 C89 1 1.094687 0.079268 1.220873 11.00000 0.04293 0.04360 = 0.02428 0.00380 -0.00840 -0.00177 AFIX 43 H89 2 1.145131 0.090067 1.231846 11.00000 -1.20000 AFIX 0 C90 1 1.081843 0.080181 1.185036 11.00000 0.03325 0.03455 = 0.02425 0.00237 -0.00235 0.00206 C91 1 0.862276 0.017185 1.171957 11.00000 0.03622 0.03047 = 0.03467 0.00727 0.00565 -0.00491 AFIX 13 H91 2 0.851965 0.041177 1.149536 11.00000 -1.20000 AFIX 0 C92 1 0.793137 0.035857 1.193115 11.00000 0.04090 0.04870 = 0.04265 0.00787 0.01029 -0.00762 AFIX 33 H92A 2 0.743744 0.018599 1.181314 11.00000 -1.50000 H92B 2 0.790330 0.087406 1.195923 11.00000 -1.50000 H92C 2 0.802147 0.013229 1.215325 11.00000 -1.50000 AFIX 0 C93 1 0.863646 -0.064733 1.165692 11.00000 0.04209 0.03488 = 0.07069 0.00183 0.00516 -0.00636 AFIX 33 H93A 2 0.812351 -0.080131 1.155013 11.00000 -1.50000 H93B 2 0.875542 -0.089396 1.187276 11.00000 -1.50000 H93C 2 0.903904 -0.075971 1.150865 11.00000 -1.50000 AFIX 0 C94 1 1.151741 0.093285 1.164392 11.00000 0.02718 0.06209 = 0.02887 0.00008 0.00020 0.00225 AFIX 13 H94 2 1.130912 0.101204 1.140270 11.00000 -1.20000 AFIX 0 C95 1 1.202169 0.159182 1.176990 11.00000 0.03203 0.06762 = 0.04044 0.01048 0.00062 -0.00518 AFIX 33 H95A 2 1.245400 0.164986 1.163061 11.00000 -1.50000 H95B 2 1.223362 0.152000 1.200566 11.00000 -1.50000 H95C 2 1.169308 0.201805 1.175228 11.00000 -1.50000 AFIX 0 C96 1 1.203514 0.025677 1.166494 11.00000 0.04254 0.07500 = 0.05841 -0.01279 -0.00254 0.01469 AFIX 33 H96A 2 1.248137 0.032914 1.153488 11.00000 -1.50000 H96B 2 1.172439 -0.014765 1.157208 11.00000 -1.50000 H96C 2 1.222676 0.016165 1.190115 11.00000 -1.50000 AFIX 0 C97 1 0.534807 0.358766 1.098213 11.00000 0.02089 0.03016 = 0.02230 -0.00034 -0.00357 -0.00223 C98 1 0.507444 0.453620 1.062019 11.00000 0.04592 0.02781 = 0.03726 0.00744 -0.01239 -0.00027 AFIX 43 H98 2 0.504482 0.482005 1.042253 11.00000 -1.20000 AFIX 0 C99 1 0.481885 0.472160 1.092199 11.00000 0.04672 0.02774 = 0.04726 -0.00165 -0.01004 0.01234 AFIX 43 H99 2 0.457988 0.515626 1.097409 11.00000 -1.20000 AFIX 0 C100 1 0.590128 0.211670 1.165818 11.00000 0.04306 0.04692 = 0.02447 0.01560 0.00488 0.00590 AFIX 43 H100 2 0.621274 0.224172 1.186087 11.00000 -1.20000 AFIX 0 C101 1 0.509421 0.227530 1.157640 11.00000 0.04531 0.04348 = 0.03657 0.01491 0.02103 0.00698 AFIX 43 H101 2 0.476639 0.251403 1.171691 11.00000 -1.20000 AFIX 0 C102 1 0.486052 0.200565 1.123819 11.00000 0.03251 0.03987 = 0.03987 0.01130 0.00993 -0.00013 AFIX 43 H102 2 0.436217 0.206933 1.111371 11.00000 -1.20000 AFIX 0 C103 1 0.551375 0.162441 1.112317 11.00000 0.03840 0.03014 = 0.03856 0.00582 0.00775 0.00271 AFIX 43 H103 2 0.550913 0.135870 1.092068 11.00000 -1.20000 AFIX 0 C104 1 0.616812 0.172474 1.137321 11.00000 0.03646 0.03448 = 0.03626 0.01239 0.00871 0.00769 AFIX 43 H104 2 0.668721 0.156486 1.135750 11.00000 -1.20000 AFIX 0 C105 1 0.563321 0.342704 1.037021 11.00000 0.02960 0.03226 = 0.01826 0.00581 -0.00322 0.00053 C106 1 0.633053 0.361793 1.022496 11.00000 0.03346 0.05075 = 0.02437 0.01562 -0.00206 -0.00489 C107 1 0.651747 0.321658 0.994055 11.00000 0.04108 0.07306 = 0.02729 0.01204 0.01003 -0.00106 AFIX 43 H107 2 0.697649 0.333093 0.983880 11.00000 -1.20000 AFIX 0 C108 1 0.604349 0.266141 0.980853 11.00000 0.05484 0.06745 = 0.02677 0.00240 0.01136 0.00909 AFIX 43 H108 2 0.618347 0.240146 0.962009 11.00000 -1.20000 AFIX 0 C109 1 0.535065 0.248359 0.995554 11.00000 0.04853 0.04723 = 0.02842 -0.00537 0.00158 -0.00257 AFIX 43 H109 2 0.503211 0.210389 0.986413 11.00000 -1.20000 AFIX 0 C110 1 0.512841 0.286484 1.023658 11.00000 0.03236 0.03555 = 0.02200 0.00281 -0.00259 -0.00097 C111 1 0.685121 0.424992 1.034691 11.00000 0.03566 0.06641 = 0.03432 0.02266 -0.00844 -0.01820 AFIX 13 H111 2 0.670774 0.440126 1.057277 11.00000 -1.20000 AFIX 0 C112 1 0.669911 0.488786 1.009640 11.00000 0.06677 0.07345 = 0.05921 0.03351 -0.02170 -0.03732 AFIX 33 H11A 2 0.702910 0.529003 1.017727 11.00000 -1.50000 H11B 2 0.614662 0.502665 1.008302 11.00000 -1.50000 H11C 2 0.682649 0.474586 0.987223 11.00000 -1.50000 AFIX 0 C113 1 0.774082 0.406276 1.038339 11.00000 0.03576 0.11739 = 0.04167 0.02882 -0.00008 -0.02411 AFIX 33 H11D 2 0.804640 0.448043 1.046315 11.00000 -1.50000 H11E 2 0.789262 0.391504 1.016391 11.00000 -1.50000 H11F 2 0.784257 0.367518 1.054604 11.00000 -1.50000 AFIX 0 C114 1 0.433136 0.270557 1.037002 11.00000 0.02961 0.03873 = 0.02957 -0.00082 -0.00341 -0.00773 AFIX 13 H114 2 0.438904 0.281000 1.061748 11.00000 -1.20000 AFIX 0 C115 1 0.406536 0.191669 1.032268 11.00000 0.05099 0.05221 = 0.05108 -0.00632 0.00290 -0.02055 AFIX 33 H11G 2 0.356187 0.185139 1.041326 11.00000 -1.50000 H11H 2 0.445880 0.160575 1.044307 11.00000 -1.50000 H11I 2 0.400842 0.179772 1.008199 11.00000 -1.50000 AFIX 0 C116 1 0.369182 0.321069 1.019850 11.00000 0.03506 0.06751 = 0.05552 0.00577 -0.00788 0.00108 AFIX 33 H11J 2 0.318975 0.310945 1.028432 11.00000 -1.50000 H11K 2 0.364134 0.313699 0.995379 11.00000 -1.50000 H11L 2 0.384133 0.370396 1.024931 11.00000 -1.50000 AFIX 0 C117 1 0.466228 0.405494 1.146924 11.00000 0.03851 0.04170 = 0.03419 -0.00896 0.00357 0.01373 C118 1 0.515733 0.417517 1.177319 11.00000 0.04387 0.04647 = 0.03549 -0.01199 0.00201 0.01483 C119 1 0.483214 0.402790 1.208262 11.00000 0.05656 0.07167 = 0.03507 -0.01717 0.00661 0.01895 AFIX 43 H119 2 0.514711 0.409113 1.229123 11.00000 -1.20000 AFIX 0 C120 1 0.406004 0.379306 1.208238 11.00000 0.05722 0.08465 = 0.05041 -0.01263 0.02464 0.02088 AFIX 43 H120 2 0.385860 0.369654 1.229023 11.00000 -1.20000 AFIX 0 C121 1 0.358173 0.369893 1.177928 11.00000 0.04162 0.07514 = 0.05482 -0.01218 0.01982 0.01350 AFIX 43 H121 2 0.305576 0.354754 1.178417 11.00000 -1.20000 AFIX 0 C122 1 0.387123 0.382671 1.146270 11.00000 0.03235 0.05238 = 0.05013 -0.01208 0.00746 0.01411 C123 1 0.599669 0.447710 1.177111 11.00000 0.04221 0.05949 = 0.02975 -0.01642 -0.00450 0.01683 AFIX 13 H123 2 0.619386 0.432666 1.155493 11.00000 -1.20000 AFIX 0 C124 1 0.597237 0.530206 1.177407 11.00000 0.04803 0.06160 = 0.04170 -0.00890 -0.00481 0.01004 AFIX 33 H12A 2 0.650435 0.548887 1.177173 11.00000 -1.50000 H12B 2 0.575532 0.546541 1.197803 11.00000 -1.50000 H12C 2 0.564212 0.547152 1.157431 11.00000 -1.50000 AFIX 0 C125 1 0.657825 0.419215 1.206462 11.00000 0.04766 0.05978 = 0.04331 -0.01783 -0.00960 0.01802 AFIX 33 H12D 2 0.709697 0.439951 1.205031 11.00000 -1.50000 H12E 2 0.661171 0.367452 1.204859 11.00000 -1.50000 H12F 2 0.639373 0.432227 1.228053 11.00000 -1.50000 AFIX 0 C126 1 0.331815 0.373949 1.112962 11.00000 0.02947 0.06752 = 0.05713 -0.01280 0.00460 0.00944 AFIX 13 H126 2 0.365664 0.369964 1.094139 11.00000 -1.20000 AFIX 0 C127 1 0.279481 0.440982 1.105991 11.00000 0.05255 0.09872 = 0.08300 -0.01100 -0.01576 0.02860 AFIX 33 H12G 2 0.245180 0.434492 1.084926 11.00000 -1.50000 H12H 2 0.312832 0.482630 1.104010 11.00000 -1.50000 H12I 2 0.247514 0.447983 1.124652 11.00000 -1.50000 AFIX 0 C128 1 0.280724 0.306068 1.112246 11.00000 0.03123 0.09694 = 0.08438 -0.01735 0.01418 -0.00635 AFIX 33 H12J 2 0.247542 0.303371 1.090685 11.00000 -1.50000 H12K 2 0.247627 0.307699 1.130777 11.00000 -1.50000 H12L 2 0.314699 0.264218 1.114822 11.00000 -1.50000 AFIX 0 N1 3 1.012639 0.423289 0.828633 11.00000 0.02654 0.02585 = 0.01768 0.00035 0.00262 0.00135 N2 3 1.056588 0.426745 0.881964 11.00000 0.02554 0.02814 = 0.01851 0.00323 -0.00249 -0.00134 N3 3 0.574512 0.074456 0.870739 11.00000 0.02181 0.02458 = 0.02371 0.00005 0.00192 0.00069 N4 3 0.568137 0.114618 0.818883 11.00000 0.02363 0.02629 = 0.02204 -0.00101 0.00178 0.00140 N5 3 0.968297 0.090304 1.079204 11.00000 0.02428 0.02909 = 0.01782 -0.00270 -0.00001 0.00048 N6 3 0.992417 0.060794 1.132447 11.00000 0.02588 0.03027 = 0.01660 -0.00083 -0.00087 0.00013 N7 3 0.539072 0.384400 1.065713 11.00000 0.02853 0.02771 = 0.02413 0.00454 -0.00557 -0.00090 N8 3 0.498183 0.413633 1.114072 11.00000 0.03154 0.03102 = 0.02935 -0.00466 -0.00377 0.00665 NI1 4 0.953085 0.300823 0.866703 11.00000 0.02496 0.02516 = 0.01950 0.00157 0.00134 -0.00115 NI2 4 0.576957 0.234090 0.867846 11.00000 0.02350 0.02257 = 0.02325 -0.00052 0.00069 0.00050 NI3 4 0.956268 0.216171 1.123515 11.00000 0.02731 0.02567 = 0.01969 -0.00195 -0.00034 -0.00045 NI4 4 0.579838 0.275823 1.119774 11.00000 0.02376 0.03065 = 0.02018 0.00523 0.00425 0.00537 SE1 5 0.832845 0.361251 0.865771 11.00000 0.02504 0.03109 = 0.02948 0.00690 0.00174 -0.00114 SE2 5 0.766987 0.319742 0.911594 11.00000 0.02620 0.03311 = 0.02336 -0.00248 0.00100 -0.00551 SE3 5 0.700989 0.211862 0.895716 11.00000 0.02404 0.02649 = 0.03176 0.00333 -0.00063 -0.00169 SE4 5 0.854114 0.194748 1.156269 11.00000 0.02781 0.03198 = 0.02652 0.00257 0.00384 0.00662 SE5 5 0.787248 0.302194 1.165524 11.00000 0.03147 0.03972 = 0.02493 -0.00626 -0.00159 0.01145 SE6 5 0.702357 0.329091 1.115873 11.00000 0.02450 0.03744 = 0.02563 0.00610 0.00176 0.00430 HKLF 4 REM mP21n in P2(1)/n REM R1 = 0.0409 for 19930 Fo > 4sig(Fo) and 0.0495 for all 23312 data REM 1315 parameters refined using 0 restraints END WGHT 0.0457 12.6188 REM Highest difference peak 2.756, deepest hole -0.710, 1-sigma level 0.078 Q1 1 0.7959 0.2072 1.1439 11.00000 0.05 2.76 Q2 1 0.7166 0.2838 1.1125 11.00000 0.05 2.48 Q3 1 0.9069 0.2214 1.1229 11.00000 0.05 1.19 Q4 1 0.8125 0.3173 0.8687 11.00000 0.05 1.00 Q5 1 0.7418 0.2324 0.8901 11.00000 0.05 0.98 Q6 1 0.6224 0.2461 0.8666 11.00000 0.05 0.53 Q7 1 0.9839 0.2915 0.8630 11.00000 0.05 0.52 Q8 1 0.5853 0.2407 1.1142 11.00000 0.05 0.51 Q9 1 0.9444 0.2740 0.8674 11.00000 0.05 0.48 Q10 1 0.8023 0.0821 1.2062 11.00000 0.05 0.40 Q11 1 0.9813 0.1616 1.1179 11.00000 0.05 0.40 Q12 1 0.7237 0.1632 0.8935 11.00000 0.05 0.38 Q13 1 0.8152 0.2423 1.1724 11.00000 0.05 0.37 Q14 1 0.8161 0.1371 1.1528 11.00000 0.05 0.36 Q15 1 0.9896 0.3692 0.7872 11.00000 0.05 0.36 Q16 1 0.5767 0.1944 0.7883 11.00000 0.05 0.35 Q17 1 0.8895 0.4147 0.7640 11.00000 0.05 0.34 Q18 1 0.8786 0.3151 0.8797 11.00000 0.05 0.34 Q19 1 0.9387 0.1537 1.1171 11.00000 0.05 0.34 Q20 1 0.7972 0.2724 0.9103 11.00000 0.05 0.34 ; _shelx_res_checksum 61416 _database_code_depnum_ccdc_archive 'CCDC 995936' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mp21c _audit_creation_date 2013-08-20 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C64 H82 N4 Ni2 P4, 0.5(C4 H8 O)' _chemical_formula_sum 'C66 H86 N4 Ni2 O0.50 P4' _chemical_formula_weight 1184.69 _chemical_melting_point ? _chemical_oxdiff_formula 'C64 H84 N4 Ni2 P4' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 13.7371(2) _cell_length_b 23.6940(5) _cell_length_c 19.4754(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.093(2) _cell_angle_gamma 90.00 _cell_volume 6337.83(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11884 _cell_measurement_temperature 123.01(10) _cell_measurement_theta_max 73.5770 _cell_measurement_theta_min 3.7170 _exptl_absorpt_coefficient_mu 2.012 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_crystal_size_max 0.2598 _exptl_crystal_size_mid 0.074 _exptl_crystal_size_min 0.0434 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_unetI/netI 0.0402 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 27288 _diffrn_reflns_theta_full 66.97 _diffrn_reflns_theta_max 73.59 _diffrn_reflns_theta_min 3.22 _diffrn_ambient_temperature 123.01(10) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9893 _diffrn_measured_fraction_theta_max 0.9553 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -59.00 35.00 0.5000 7.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 37.0000 -90.0000 188 #__ type_ start__ end____ width___ exp.time_ 2 omega -97.00 -2.00 0.5000 7.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 125.0000 90.0000 190 #__ type_ start__ end____ width___ exp.time_ 3 omega 31.00 69.00 0.5000 40.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 30.0000 76 #__ type_ start__ end____ width___ exp.time_ 4 omega 47.00 156.00 0.5000 40.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 15.0000 -30.0000 218 #__ type_ start__ end____ width___ exp.time_ 5 omega 32.00 77.00 0.5000 40.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -45.0000 60.0000 90 #__ type_ start__ end____ width___ exp.time_ 6 omega 84.00 158.00 0.5000 40.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 30.0000 -150.0000 148 #__ type_ start__ end____ width___ exp.time_ 7 omega 29.00 63.00 0.5000 40.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 90.0000 68 #__ type_ start__ end____ width___ exp.time_ 8 omega 23.00 109.00 0.5000 40.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 -120.0000 172 #__ type_ start__ end____ width___ exp.time_ 9 omega 29.00 69.00 0.5000 40.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 0.0000 80 #__ type_ start__ end____ width___ exp.time_ 10 omega -115.00 -12.00 0.5000 7.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -57.0000 -90.0000 206 #__ type_ start__ end____ width___ exp.time_ 11 omega -120.00 -61.00 0.5000 7.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 150.0000 118 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0960033000 _diffrn_orient_matrix_UB_12 0.0113910000 _diffrn_orient_matrix_UB_13 -0.0398166000 _diffrn_orient_matrix_UB_21 -0.0541870000 _diffrn_orient_matrix_UB_22 -0.0395506000 _diffrn_orient_matrix_UB_23 0.0490049000 _diffrn_orient_matrix_UB_31 -0.0208814000 _diffrn_orient_matrix_UB_32 0.0503099000 _diffrn_orient_matrix_UB_33 0.0476717000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 10235 _reflns_number_total 12211 _reflns_odcompleteness_completeness 98.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.356 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.053 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 712 _refine_ls_number_reflns 12211 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0366 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+1.5462P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0925 _refine_ls_wR_factor_ref 0.0995 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One disordered THF solvent molecule (special position) was successfully refined. ; _olex2_refinement_description ; 1. Others Fixed Sof: O1(0.5) C101(0.5) H10A(0.5) H10B(0.5) C102(0.5) H10C(0.5) H10D(0.5) C103(0.5) H10E(0.5) H10F(0.5) C104(0.5) H10G(0.5) H10H(0.5) Fixed Uiso: H2(0.029) H3(0.029) H4(0.038) H5(0.04) H6(0.043) H7(0.043) H8(0.039) H11(0.029) H12(0.033) H13(0.033) H15(0.028) H16A(0.056) H16B(0.056) H16C(0.056) H17A(0.049) H17B(0.049) H17C(0.049) H18(0.034) H19A(0.065) H19B(0.065) H19C(0.065) H20A(0.062) H20B(0.062) H20C(0.062) H23(0.045) H24(0.05) H25(0.041) H27(0.037) H28A(0.06) H28B(0.06) H28C(0.06) H29A(0.061) H29B(0.061) H29C(0.061) H30(0.032) H31A(0.056) H31B(0.056) H31C(0.056) H32A(0.053) H32B(0.053) H32C(0.053) H34(0.034) H35(0.033) H36(0.053) H37(0.049) H38(0.046) H39(0.049) H40(0.055) H43(0.038) H44(0.04) H45(0.035) H47(0.036) H48A(0.069) H48B(0.069) H48C(0.069) H49A(0.078) H49B(0.078) H49C(0.078) H50(0.037) H51A(0.072) H51B(0.072) H51C(0.072) H52A(0.073) H52B(0.073) H52C(0.073) H55(0.035) H56(0.039) H57(0.038) H59(0.031) H60A(0.049) H60B(0.049) H60C(0.049) H61A(0.051) H61B(0.051) H61C(0.051) H62(0.041) H63A(0.078) H63B(0.078) H63C(0.078) H64A(0.093) H64B(0.093) H64C(0.093) H10A(0.105) H10B(0.105) H10C(0.156) H10D(0.156) H10E(0.14) H10F(0.14) H10G(0.105) H10H(0.105) Fixed X: H2(-0.0287) H3(-0.0591) H4(0.1136) H5(0.1053) H6(0.1985) H7(0.2632) H8(0.2243) H11(0.0359) H12(0.1907) H13(0.2669) H15(-0.1003) H16A(-0.2207) H16B(-0.1397) H16C(-0.1463) H17A(-0.1693) H17B(-0.0608) H17C(-0.0881) H18(0.1795) H19A(0.3471) H19B(0.352) H19C(0.3283) H20A(0.2289) H20B(0.1293) H20C(0.226) H23(-0.1372) H24(0.0114) H25(0.1531) H27(-0.1798) H28A(-0.3221) H28B(-0.2691) H28C(-0.2375) H29A(-0.2882) H29B(-0.1812) H29C(-0.2311) H30(0.1812) H31A(0.2493) H31B(0.1909) H31C(0.1353) H32A(0.3334) H32B(0.2773) H32C(0.2834) H34(-0.6336) H35(-0.6112) H36(-0.1281) H37(-0.1879) H38(-0.3538) H39(-0.396) H40(-0.2521) H43(-0.4) H44(-0.4953) H45(-0.5893) H47(-0.3692) H48A(-0.2402) H48B(-0.2403) H48C(-0.2804) H49A(-0.3921) H49B(-0.4415) H49C(- 0.4919) H50(-0.5879) H51A(-0.635) H51B(-0.6171) H51C(-0.5293) H52A(-0.7546) H52B(-0.7288) H52C(-0.744) H55(-0.3518) H56(-0.3555) H57(-0.4192) H59(-0.4098) H60A(-0.32) H60B(-0.3126) H60C(-0.2598) H61A(-0.4974) H61B(-0.5558) H61C(- 0.4986) H62(-0.4916) H63A(-0.3893) H63B(-0.468) H63C(-0.4894) H64A(-0.6411) H64B(-0.6207) H64C(-0.6359) H10A(-0.0619) H10B(0.0503) H10C(-0.0191) H10D(0.0816) H10E(-0.0019) H10F(-0.1022) H10G(-0.0882) H10H(0.0128) Fixed Y: H2(0.2623) H3(0.3337) H4(0.1215) H5(0.0544) H6(0.0964) H7(0.1901) H8(0.2011) H11(0.0343) H12(0.0445) H13(0.1313) H15(0.1397) H16A(0.1085) H16B(0.0828) H16C(0.1483) H17A(0.0516) H17B(0.0528) H17C(0.022) H18(0.2546) H19A(0.2651) H19B(0.2049) H19C(0.2115) H20A(0.2962) H20B(0.2648) H20C(0.237) H23(0.3582) H24(0.3817) H25(0.3634) H27(0.2796) H28A(0.2802) H28B(0.3148) H28C(0.2525) H29A(0.3555) H29B(0.3747) H29C(0.3915) H30(0.2788) H31A(0.3549) H31B(0.3974) H31C(0.3566) H32A(0.3128) H32B(0.2888) H32C(0.3542) H34(0.1566) H35(0.1112) H36(0.0274) H37(0.0875) H38(0.0548) H39(-0.0266) H40(-0.0477) H43(0.2163) H44(0.1629) H45(0.09) H47(0.1936) H48A(0.2499) H48B(0.192) H48C(0.2463) H49A(0.2917) H49B(0.289) H49C(0.2604) H50(0.0417) H51A(-0.0336) H51B(0.0035) H51C(-0.014) H52A(0.0318) H52B(0.0954) H52C(0.0733) H55(0.0593) H56(-0.0375) H57(-0.0803) H59(0.1573) H60A(0.2036) H60B(0.1474) H60C(0.1527) H61A(0.2011) H61B(0.1493) H61C(0.1442) H62(-0.0126) H63A(-0.0914) H63B(- 0.1208) H63C(-0.1095) H64A(-0.0589) H64B(-0.0638) H64C(-0.0043) H10A(0.5381) H10B(0.5393) H10C(0.4459) H10D(0.4625) H10E(0.4517) H10F(0.4656) H10G(0.5528) H10H(0.5393) Fixed Z: H2(-0.1127) H3(-0.0251) H4(0.2272) H5(0.127) H6(0.0317) H7(0.0721) H8(0.1965) H11(-0.1057) H12(-0.1468) H13(-0.1433) H15(-0.0181) H16A(-0.0972) H16B(-0.1434) H16C(-0.1332) H17A(0.0042) H17B(0.0306) H17C(-0.0383) H18(- 0.0588) H19A(-0.0753) H19B(-0.1084) H19C(-0.0304) H20A(-0.1623) H20B(-0.1734) H20C(-0.1983) H23(0.2259) H24(0.2743) H25(0.2167) H27(0.0728) H28A(0.1374) H28B(0.1956) H28C(0.1807) H29A(0.0539) H29B(0.0401) H29C(0.1088) H30(0.0723) H31A(0.0122) H31B(0.0574) H31C(0.0068) H32A(0.1088) H32B(0.1717) H32C(0.1602) H34(0.2655) H35(0.1536) H36(0.3044) H37(0.4018) H38(0.4309) H39(0.353) H40(0.2812) H43(0.4792) H44(0.5504) H45(0.5065) H47(0.2995) H48A(0.3403) H48B(0.3793) H48C(0.415) H49A(0.2969) H49B(0.3687) H49C(0.3047) H50(0.3324) H51A(0.4019) H51B(0.4677) H51C(0.422) H52A(0.3545) H52B(0.3419) H52C(0.4169) H55(-0.0131) H56(-0.0045) H57(0.0909) H59(0.1189) H60A(0.0348) H60B(-0.0073) H60C(0.0645) H61A(0.0282) H61B(0.0557) H61C(-0.0129) H62(0.2436) H63A(0.232) H63B(0.1849) H63C(0.2624) H64A(0.2268) H64B(0.148) H64C(0.1815) H10A(-0.0746) H10B(-0.0911) H10C(-0.0587) H10D(-0.0236) H10E(0.0722) H10F(0.035) H10G(0.0674) H10H(0.1028) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.03228(12) 0.22166(7) 0.03710(9) 0.0185(3) Uani 1 1 d . . . N1 N 0.02413(11) 0.21256(6) -0.03216(8) 0.0198(3) Uani 1 1 d . . . P1 P -0.07889(3) 0.16852(2) 0.14136(3) 0.02581(11) Uani 1 1 d . . . Ni1 Ni 0.07311(2) 0.170006(13) 0.106100(15) 0.01957(8) Uani 1 1 d . . . C2 C -0.01588(14) 0.25898(8) -0.06585(10) 0.0238(4) Uani 1 1 d . . . H2 H -0.0287 0.2623 -0.1127 0.029 Uiso 1 1 calc R . . N2 N -0.00248(11) 0.27545(6) 0.04478(8) 0.0204(3) Uani 1 1 d . . . P2 P -0.24053(3) 0.12331(2) 0.21664(3) 0.02538(11) Uani 1 1 d . . . Ni2 Ni -0.31049(2) 0.065054(13) 0.289336(16) 0.02073(8) Uani 1 1 d . . . C3 C -0.03247(14) 0.29810(8) -0.01785(10) 0.0243(4) Uani 1 1 d . . . H3 H -0.0591 0.3337 -0.0251 0.029 Uiso 1 1 calc R . . N3 N -0.49858(11) 0.12226(7) 0.29214(8) 0.0218(3) Uani 1 1 d . . . P3 P -0.08982(4) 0.14537(2) 0.25211(3) 0.02911(11) Uani 1 1 d . . . C4 C 0.14427(15) 0.12635(9) 0.18538(11) 0.0320(4) Uani 1 1 d . . . H4 H 0.1136 0.1215 0.2272 0.038 Uiso 1 1 calc R . . N4 N -0.47853(11) 0.08354(6) 0.19412(8) 0.0209(3) Uani 1 1 d . . . P4 P -0.11098(4) 0.08123(2) 0.17408(3) 0.02928(11) Uani 1 1 d . . . C5 C 0.13827(15) 0.08872(9) 0.12822(12) 0.0336(5) Uani 1 1 d . . . H5 H 0.1053 0.0544 0.1270 0.040 Uiso 1 1 calc R . . C6 C 0.19014(16) 0.11213(10) 0.07495(11) 0.0356(5) Uani 1 1 d . . . H6 H 0.1985 0.0964 0.0317 0.043 Uiso 1 1 calc R . . C7 C 0.22821(14) 0.16467(10) 0.09838(12) 0.0358(5) Uani 1 1 d . . . H7 H 0.2632 0.1901 0.0721 0.043 Uiso 1 1 calc R . . C8 C 0.20424(15) 0.17184(9) 0.16777(11) 0.0323(5) Uani 1 1 d . . . H8 H 0.2243 0.2011 0.1965 0.039 Uiso 1 1 calc R . . C9 C 0.06847(13) 0.16554(8) -0.06697(9) 0.0206(3) Uani 1 1 d . . . C10 C 0.01827(13) 0.11423(8) -0.07177(9) 0.0209(3) Uani 1 1 d . . . C11 C 0.06668(14) 0.06916(8) -0.10233(9) 0.0241(4) Uani 1 1 d . . . H11 H 0.0359 0.0343 -0.1057 0.029 Uiso 1 1 calc R . . C12 C 0.15927(15) 0.07528(9) -0.12765(10) 0.0276(4) Uani 1 1 d . . . H12 H 0.1907 0.0445 -0.1468 0.033 Uiso 1 1 calc R . . C13 C 0.20545(14) 0.12733(9) -0.12466(10) 0.0273(4) Uani 1 1 d . . . H13 H 0.2669 0.1313 -0.1433 0.033 Uiso 1 1 calc R . . C14 C 0.16126(13) 0.17377(8) -0.09425(9) 0.0233(4) Uani 1 1 d . . . C15 C -0.08601(13) 0.10814(8) -0.04876(10) 0.0231(4) Uani 1 1 d . . . H15 H -0.1003 0.1397 -0.0181 0.028 Uiso 1 1 calc R . . C16 C -0.15459(15) 0.11233(11) -0.11147(11) 0.0375(5) Uani 1 1 d . . . H16A H -0.2207 0.1085 -0.0972 0.056 Uiso 1 1 calc R . . H16B H -0.1397 0.0828 -0.1434 0.056 Uiso 1 1 calc R . . H16C H -0.1463 0.1483 -0.1332 0.056 Uiso 1 1 calc R . . C17 C -0.10260(16) 0.05359(9) -0.00945(11) 0.0325(4) Uani 1 1 d . . . H17A H -0.1693 0.0516 0.0042 0.049 Uiso 1 1 calc R . . H17B H -0.0608 0.0528 0.0306 0.049 Uiso 1 1 calc R . . H17C H -0.0881 0.0220 -0.0383 0.049 Uiso 1 1 calc R . . C18 C 0.21093(14) 0.23113(9) -0.09342(10) 0.0284(4) Uani 1 1 d . . . H18 H 0.1795 0.2546 -0.0588 0.034 Uiso 1 1 calc R . . C19 C 0.31973(16) 0.22786(12) -0.07518(13) 0.0433(6) Uani 1 1 d . . . H19A H 0.3471 0.2651 -0.0753 0.065 Uiso 1 1 calc R . . H19B H 0.3520 0.2049 -0.1084 0.065 Uiso 1 1 calc R . . H19C H 0.3283 0.2115 -0.0304 0.065 Uiso 1 1 calc R . . C20 C 0.19752(19) 0.25999(10) -0.16338(12) 0.0411(5) Uani 1 1 d . . . H20A H 0.2289 0.2962 -0.1623 0.062 Uiso 1 1 calc R . . H20B H 0.1293 0.2648 -0.1734 0.062 Uiso 1 1 calc R . . H20C H 0.2260 0.2370 -0.1983 0.062 Uiso 1 1 calc R . . C21 C 0.00034(13) 0.30663(8) 0.10872(10) 0.0224(4) Uani 1 1 d . . . C22 C -0.08694(14) 0.31993(8) 0.14083(10) 0.0267(4) Uani 1 1 d . . . C23 C -0.08043(17) 0.34885(10) 0.20323(12) 0.0377(5) Uani 1 1 d . . . H23 H -0.1372 0.3582 0.2259 0.045 Uiso 1 1 calc R . . C24 C 0.00859(18) 0.36381(11) 0.23188(12) 0.0418(5) Uani 1 1 d . . . H24 H 0.0114 0.3817 0.2743 0.050 Uiso 1 1 calc R . . C25 C 0.09378(16) 0.35216(10) 0.19749(11) 0.0338(5) Uani 1 1 d . . . H25 H 0.1531 0.3634 0.2167 0.041 Uiso 1 1 calc R . . C26 C 0.09226(14) 0.32397(8) 0.13492(10) 0.0245(4) Uani 1 1 d . . . C27 C -0.18696(14) 0.30831(9) 0.10849(11) 0.0305(4) Uani 1 1 d . . . H27 H -0.1798 0.2796 0.0728 0.037 Uiso 1 1 calc R . . C28 C -0.26079(16) 0.28694(10) 0.16037(13) 0.0397(5) Uani 1 1 d . . . H28A H -0.3221 0.2802 0.1374 0.060 Uiso 1 1 calc R . . H28B H -0.2691 0.3148 0.1956 0.060 Uiso 1 1 calc R . . H28C H -0.2375 0.2525 0.1807 0.060 Uiso 1 1 calc R . . C29 C -0.22546(17) 0.36257(10) 0.07467(13) 0.0408(5) Uani 1 1 d . . . H29A H -0.2882 0.3555 0.0539 0.061 Uiso 1 1 calc R . . H29B H -0.1812 0.3747 0.0401 0.061 Uiso 1 1 calc R . . H29C H -0.2311 0.3915 0.1088 0.061 Uiso 1 1 calc R . . C30 C 0.18464(14) 0.31601(8) 0.09421(10) 0.0264(4) Uani 1 1 d . . . H30 H 0.1812 0.2788 0.0723 0.032 Uiso 1 1 calc R . . C31 C 0.19060(16) 0.36036(10) 0.03734(12) 0.0376(5) Uani 1 1 d . . . H31A H 0.2493 0.3549 0.0122 0.056 Uiso 1 1 calc R . . H31B H 0.1909 0.3974 0.0574 0.056 Uiso 1 1 calc R . . H31C H 0.1353 0.3566 0.0068 0.056 Uiso 1 1 calc R . . C32 C 0.27840(15) 0.31816(10) 0.13779(12) 0.0351(5) Uani 1 1 d . . . H32A H 0.3334 0.3128 0.1088 0.053 Uiso 1 1 calc R . . H32B H 0.2773 0.2888 0.1717 0.053 Uiso 1 1 calc R . . H32C H 0.2834 0.3542 0.1602 0.053 Uiso 1 1 calc R . . C33 C -0.43377(13) 0.09013(7) 0.25692(9) 0.0197(3) Uani 1 1 d . . . C34 C -0.58051(14) 0.13509(9) 0.25231(10) 0.0284(4) Uani 1 1 d . . . H34 H -0.6336 0.1566 0.2655 0.034 Uiso 1 1 calc R . . C35 C -0.56803(14) 0.11040(9) 0.19097(10) 0.0278(4) Uani 1 1 d . . . H35 H -0.6112 0.1112 0.1536 0.033 Uiso 1 1 calc R . . C36 C -0.18707(17) 0.02319(12) 0.32656(12) 0.0444(6) Uani 1 1 d . . . H36 H -0.1281 0.0274 0.3044 0.053 Uiso 1 1 calc R . . C37 C -0.22161(17) 0.05787(11) 0.38100(11) 0.0407(5) Uani 1 1 d . . . H37 H -0.1879 0.0875 0.4018 0.049 Uiso 1 1 calc R . . C38 C -0.31414(17) 0.03955(11) 0.39744(11) 0.0380(5) Uani 1 1 d . . . H38 H -0.3538 0.0548 0.4309 0.046 Uiso 1 1 calc R . . C39 C -0.33743(18) -0.00694(10) 0.35387(12) 0.0406(5) Uani 1 1 d . . . H39 H -0.3960 -0.0266 0.3530 0.049 Uiso 1 1 calc R . . C40 C -0.2574(2) -0.01821(10) 0.31238(13) 0.0459(6) Uani 1 1 d . . . H40 H -0.2521 -0.0477 0.2812 0.055 Uiso 1 1 calc R . . C41 C -0.49487(13) 0.13327(8) 0.36487(10) 0.0232(4) Uani 1 1 d . . . C42 C -0.43677(13) 0.17755(8) 0.39001(10) 0.0254(4) Uani 1 1 d . . . C43 C -0.43810(15) 0.18747(9) 0.46060(11) 0.0319(4) Uani 1 1 d . . . H43 H -0.4000 0.2163 0.4792 0.038 Uiso 1 1 calc R . . C44 C -0.49495(15) 0.15519(10) 0.50358(11) 0.0332(4) Uani 1 1 d . . . H44 H -0.4953 0.1629 0.5504 0.040 Uiso 1 1 calc R . . C45 C -0.55144(14) 0.11140(9) 0.47716(10) 0.0294(4) Uani 1 1 d . . . H45 H -0.5893 0.0900 0.5065 0.035 Uiso 1 1 calc R . . C46 C -0.55211(13) 0.09907(8) 0.40691(10) 0.0256(4) Uani 1 1 d . . . C47 C -0.37675(15) 0.21410(9) 0.34275(11) 0.0301(4) Uani 1 1 d . . . H47 H -0.3692 0.1936 0.2995 0.036 Uiso 1 1 calc R . . C48 C -0.27493(18) 0.22674(12) 0.37207(14) 0.0458(6) Uani 1 1 d . . . H48A H -0.2402 0.2499 0.3403 0.069 Uiso 1 1 calc R . . H48B H -0.2403 0.1920 0.3793 0.069 Uiso 1 1 calc R . . H48C H -0.2804 0.2463 0.4150 0.069 Uiso 1 1 calc R . . C49 C -0.4305(2) 0.26885(11) 0.32678(16) 0.0522(7) Uani 1 1 d . . . H49A H -0.3921 0.2917 0.2969 0.078 Uiso 1 1 calc R . . H49B H -0.4415 0.2890 0.3687 0.078 Uiso 1 1 calc R . . H49C H -0.4919 0.2604 0.3047 0.078 Uiso 1 1 calc R . . C50 C -0.61103(15) 0.04975(9) 0.37865(11) 0.0308(4) Uani 1 1 d . . . H50 H -0.5879 0.0417 0.3324 0.037 Uiso 1 1 calc R . . C51 C -0.5968(2) -0.00350(11) 0.42153(14) 0.0482(6) Uani 1 1 d . . . H51A H -0.6350 -0.0336 0.4019 0.072 Uiso 1 1 calc R . . H51B H -0.6171 0.0035 0.4677 0.072 Uiso 1 1 calc R . . H51C H -0.5293 -0.0140 0.4220 0.072 Uiso 1 1 calc R . . C52 C -0.71979(17) 0.06391(12) 0.37239(15) 0.0484(6) Uani 1 1 d . . . H52A H -0.7546 0.0318 0.3545 0.073 Uiso 1 1 calc R . . H52B H -0.7288 0.0954 0.3419 0.073 Uiso 1 1 calc R . . H52C H -0.7440 0.0733 0.4169 0.073 Uiso 1 1 calc R . . C53 C -0.44282(13) 0.04964(8) 0.13826(10) 0.0227(4) Uani 1 1 d . . . C54 C -0.40726(13) 0.07690(8) 0.08001(10) 0.0240(4) Uani 1 1 d . . . C55 C -0.37550(14) 0.04267(9) 0.02640(10) 0.0288(4) Uani 1 1 d . . . H55 H -0.3518 0.0593 -0.0131 0.035 Uiso 1 1 calc R . . C56 C -0.37873(15) -0.01548(9) 0.03113(11) 0.0322(4) Uani 1 1 d . . . H56 H -0.3555 -0.0375 -0.0045 0.039 Uiso 1 1 calc R . . C57 C -0.41646(15) -0.04108(9) 0.08874(11) 0.0318(4) Uani 1 1 d . . . H57 H -0.4192 -0.0803 0.0909 0.038 Uiso 1 1 calc R . . C58 C -0.45034(14) -0.00937(8) 0.14345(10) 0.0262(4) Uani 1 1 d . . . C59 C -0.40753(14) 0.14089(8) 0.07276(10) 0.0260(4) Uani 1 1 d . . . H59 H -0.4098 0.1573 0.1189 0.031 Uiso 1 1 calc R . . C60 C -0.31653(15) 0.16323(10) 0.03796(11) 0.0326(4) Uani 1 1 d . . . H60A H -0.3200 0.2036 0.0348 0.049 Uiso 1 1 calc R . . H60B H -0.3126 0.1474 -0.0073 0.049 Uiso 1 1 calc R . . H60C H -0.2598 0.1527 0.0645 0.049 Uiso 1 1 calc R . . C61 C -0.49838(15) 0.16076(9) 0.03213(12) 0.0337(5) Uani 1 1 d . . . H61A H -0.4974 0.2011 0.0282 0.051 Uiso 1 1 calc R . . H61B H -0.5558 0.1493 0.0557 0.051 Uiso 1 1 calc R . . H61C H -0.4986 0.1442 -0.0129 0.051 Uiso 1 1 calc R . . C62 C -0.50065(17) -0.03731(9) 0.20362(12) 0.0344(5) Uani 1 1 d . . . H62 H -0.4916 -0.0126 0.2436 0.041 Uiso 1 1 calc R . . C63 C -0.4578(2) -0.09516(10) 0.22249(14) 0.0522(7) Uani 1 1 d . . . H63A H -0.3893 -0.0914 0.2320 0.078 Uiso 1 1 calc R . . H63B H -0.4680 -0.1208 0.1849 0.078 Uiso 1 1 calc R . . H63C H -0.4894 -0.1095 0.2624 0.078 Uiso 1 1 calc R . . C64 C -0.6097(2) -0.04144(15) 0.18858(16) 0.0620(8) Uani 1 1 d . . . H64A H -0.6411 -0.0589 0.2268 0.093 Uiso 1 1 calc R . . H64B H -0.6207 -0.0638 0.1480 0.093 Uiso 1 1 calc R . . H64C H -0.6359 -0.0043 0.1815 0.093 Uiso 1 1 calc R . . O1 O 0.0229(3) 0.56776(14) 0.0092(3) 0.0608(11) Uani 0.50 1 d PD A -1 C101 C 0.0031(8) 0.5315(4) -0.0560(6) 0.087(3) Uani 0.50 1 d PDU A -1 H10A H -0.0619 0.5381 -0.0746 0.105 Uiso 0.50 1 calc PR A -1 H10B H 0.0503 0.5393 -0.0911 0.105 Uiso 0.50 1 calc PR A -1 C102 C 0.0136(11) 0.4730(4) -0.0288(6) 0.130(5) Uani 0.50 1 d PDU A -1 H10C H -0.0191 0.4459 -0.0587 0.156 Uiso 0.50 1 calc PR A -1 H10D H 0.0816 0.4625 -0.0236 0.156 Uiso 0.50 1 calc PR A -1 C103 C -0.0342(10) 0.4763(4) 0.0390(6) 0.116(4) Uani 0.50 1 d PDU A -1 H10E H -0.0019 0.4517 0.0722 0.140 Uiso 0.50 1 calc PR A -1 H10F H -0.1022 0.4656 0.0350 0.140 Uiso 0.50 1 calc PR A -1 C104 C -0.0242(5) 0.5369(4) 0.0600(5) 0.088(4) Uani 0.50 1 d PDU A -1 H10G H -0.0882 0.5528 0.0674 0.105 Uiso 0.50 1 calc PR A -1 H10H H 0.0128 0.5393 0.1028 0.105 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0131(7) 0.0189(8) 0.0234(8) -0.0005(7) -0.0028(6) -0.0027(6) N1 0.0168(7) 0.0197(7) 0.0227(7) 0.0005(6) -0.0031(5) -0.0014(6) P1 0.0161(2) 0.0293(2) 0.0320(2) 0.0069(2) 0.00009(17) -0.00021(17) Ni1 0.01451(14) 0.02169(15) 0.02238(15) 0.00151(12) -0.00274(11) 0.00080(11) C2 0.0236(9) 0.0229(9) 0.0246(9) 0.0031(7) -0.0053(7) -0.0002(7) N2 0.0170(7) 0.0201(7) 0.0240(7) -0.0008(6) -0.0021(6) -0.0006(6) P2 0.0173(2) 0.0289(2) 0.0300(2) 0.0084(2) -0.00063(17) -0.00013(18) Ni2 0.01719(15) 0.02190(15) 0.02305(16) 0.00405(12) -0.00081(11) 0.00266(12) C3 0.0231(9) 0.0208(8) 0.0288(9) 0.0019(7) -0.0052(7) 0.0000(7) N3 0.0169(7) 0.0239(7) 0.0246(8) 0.0007(6) -0.0015(6) 0.0028(6) P3 0.0228(2) 0.0375(3) 0.0271(2) -0.0048(2) 0.00026(18) -0.0062(2) C4 0.0278(10) 0.0408(11) 0.0273(10) 0.0094(9) -0.0029(8) 0.0113(9) N4 0.0172(7) 0.0227(7) 0.0227(7) 0.0004(6) -0.0021(6) 0.0010(6) P4 0.0297(3) 0.0252(2) 0.0332(3) -0.0040(2) 0.0082(2) -0.00406(19) C5 0.0284(10) 0.0233(9) 0.0487(13) 0.0040(9) -0.0124(9) 0.0047(8) C6 0.0333(11) 0.0447(12) 0.0286(10) -0.0052(9) -0.0050(8) 0.0224(10) C7 0.0146(8) 0.0436(12) 0.0493(13) 0.0157(10) 0.0010(8) 0.0070(8) C8 0.0227(9) 0.0333(10) 0.0402(11) -0.0043(9) -0.0168(8) 0.0043(8) C9 0.0200(8) 0.0224(8) 0.0192(8) -0.0017(7) -0.0042(6) 0.0007(7) C10 0.0205(8) 0.0233(8) 0.0187(8) 0.0009(7) -0.0034(6) 0.0008(7) C11 0.0270(9) 0.0211(8) 0.0240(9) 0.0002(7) -0.0021(7) -0.0001(7) C12 0.0286(10) 0.0274(9) 0.0269(9) -0.0020(8) -0.0007(7) 0.0076(8) C13 0.0208(9) 0.0350(10) 0.0261(9) -0.0009(8) 0.0007(7) 0.0015(8) C14 0.0196(8) 0.0288(9) 0.0214(8) 0.0013(7) -0.0021(7) -0.0011(7) C15 0.0210(8) 0.0223(8) 0.0259(9) -0.0015(7) -0.0005(7) -0.0025(7) C16 0.0218(9) 0.0563(14) 0.0343(11) 0.0021(10) -0.0044(8) -0.0009(9) C17 0.0317(10) 0.0285(10) 0.0375(11) 0.0039(9) 0.0065(9) -0.0052(8) C18 0.0219(9) 0.0338(10) 0.0295(10) -0.0026(8) 0.0017(7) -0.0070(8) C19 0.0225(10) 0.0582(15) 0.0492(14) -0.0013(12) -0.0024(9) -0.0122(10) C20 0.0458(13) 0.0357(11) 0.0417(12) 0.0074(10) -0.0003(10) -0.0111(10) C21 0.0223(9) 0.0193(8) 0.0254(9) -0.0017(7) -0.0031(7) -0.0016(7) C22 0.0217(9) 0.0264(9) 0.0317(10) -0.0030(8) -0.0013(7) -0.0001(7) C23 0.0297(11) 0.0478(13) 0.0358(11) -0.0129(10) 0.0032(9) -0.0005(10) C24 0.0381(12) 0.0548(14) 0.0326(11) -0.0208(11) -0.0013(9) -0.0041(11) C25 0.0283(10) 0.0396(11) 0.0331(11) -0.0083(9) -0.0055(8) -0.0068(9) C26 0.0233(9) 0.0215(8) 0.0286(9) -0.0008(7) -0.0031(7) -0.0025(7) C27 0.0200(9) 0.0309(10) 0.0405(11) -0.0080(9) -0.0008(8) -0.0005(8) C28 0.0246(10) 0.0372(11) 0.0577(14) -0.0060(11) 0.0078(9) -0.0006(9) C29 0.0291(11) 0.0390(12) 0.0538(14) -0.0023(11) -0.0093(10) 0.0045(9) C30 0.0197(8) 0.0269(9) 0.0325(10) -0.0019(8) -0.0023(7) -0.0055(7) C31 0.0287(11) 0.0440(12) 0.0401(12) 0.0060(10) -0.0009(9) -0.0097(9) C32 0.0240(10) 0.0375(11) 0.0435(12) -0.0010(10) -0.0064(9) -0.0055(8) C33 0.0192(8) 0.0173(8) 0.0224(8) 0.0013(7) 0.0009(6) -0.0021(6) C34 0.0186(9) 0.0359(10) 0.0305(10) 0.0024(8) -0.0029(7) 0.0074(8) C35 0.0183(8) 0.0381(11) 0.0269(9) 0.0022(8) -0.0036(7) 0.0029(8) C36 0.0300(11) 0.0623(16) 0.0411(12) 0.0285(12) 0.0053(9) 0.0203(11) C37 0.0353(11) 0.0554(14) 0.0307(11) 0.0147(10) -0.0151(9) 0.0019(10) C38 0.0342(11) 0.0541(14) 0.0257(10) 0.0143(10) 0.0010(8) 0.0135(10) C39 0.0408(12) 0.0386(12) 0.0425(12) 0.0221(10) 0.0012(10) 0.0003(10) C40 0.0633(16) 0.0302(11) 0.0444(13) 0.0158(10) 0.0079(11) 0.0216(11) C41 0.0197(8) 0.0252(9) 0.0245(9) -0.0017(7) -0.0010(7) 0.0057(7) C42 0.0183(8) 0.0262(9) 0.0316(10) -0.0039(8) -0.0005(7) 0.0051(7) C43 0.0252(10) 0.0357(11) 0.0346(11) -0.0102(9) -0.0030(8) 0.0041(8) C44 0.0283(10) 0.0458(12) 0.0253(9) -0.0066(9) -0.0025(8) 0.0080(9) C45 0.0241(9) 0.0366(11) 0.0275(10) 0.0031(8) 0.0029(7) 0.0059(8) C46 0.0199(8) 0.0285(9) 0.0284(9) 0.0005(8) 0.0001(7) 0.0049(7) C47 0.0254(10) 0.0256(9) 0.0396(11) -0.0057(8) 0.0054(8) 0.0003(8) C48 0.0322(12) 0.0489(14) 0.0566(15) -0.0140(12) 0.0044(10) -0.0139(10) C49 0.0487(15) 0.0368(13) 0.0719(18) 0.0152(12) 0.0223(13) 0.0124(11) C50 0.0271(10) 0.0339(10) 0.0316(10) -0.0007(8) 0.0036(8) -0.0032(8) C51 0.0550(15) 0.0408(13) 0.0489(14) 0.0096(11) 0.0019(12) -0.0138(12) C52 0.0250(11) 0.0573(15) 0.0630(16) -0.0161(13) -0.0008(10) -0.0056(10) C53 0.0181(8) 0.0254(9) 0.0243(9) -0.0026(7) -0.0042(7) 0.0004(7) C54 0.0164(8) 0.0297(9) 0.0256(9) -0.0013(8) -0.0047(7) -0.0004(7) C55 0.0221(9) 0.0398(11) 0.0245(9) -0.0029(8) -0.0024(7) 0.0008(8) C56 0.0273(10) 0.0394(11) 0.0298(10) -0.0109(9) -0.0046(8) 0.0062(9) C57 0.0310(10) 0.0271(10) 0.0370(11) -0.0065(8) -0.0102(8) 0.0020(8) C58 0.0239(9) 0.0272(9) 0.0271(9) -0.0021(8) -0.0072(7) -0.0019(7) C59 0.0237(9) 0.0291(9) 0.0250(9) 0.0033(8) -0.0018(7) -0.0010(7) C60 0.0275(10) 0.0391(11) 0.0312(10) 0.0078(9) -0.0025(8) -0.0053(9) C61 0.0271(10) 0.0343(11) 0.0395(11) 0.0081(9) -0.0055(8) 0.0001(8) C62 0.0389(12) 0.0278(10) 0.0365(11) 0.0005(9) -0.0018(9) -0.0087(9) C63 0.081(2) 0.0264(11) 0.0489(15) 0.0038(10) 0.0048(13) -0.0053(12) C64 0.0410(15) 0.085(2) 0.0597(17) 0.0142(16) 0.0001(12) -0.0286(15) O1 0.056(2) 0.0235(17) 0.103(3) -0.0028(19) 0.009(2) -0.0011(16) C101 0.097(7) 0.050(5) 0.113(6) -0.012(4) -0.063(5) 0.022(4) C102 0.163(11) 0.062(6) 0.162(10) 0.000(7) -0.087(8) 0.001(7) C103 0.112(8) 0.046(5) 0.192(11) 0.021(7) 0.019(8) -0.010(6) C104 0.021(2) 0.082(6) 0.160(9) 0.068(6) 0.009(4) 0.011(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.368(2) . ? C1 Ni1 1.8946(17) . ? C1 N2 1.370(2) . ? N1 C2 1.389(2) . ? N1 C9 1.445(2) . ? P1 Ni1 2.2107(6) . ? P1 P3 2.2334(7) . ? P1 P4 2.2111(7) . ? Ni1 C4 2.0861(19) . ? Ni1 C5 2.164(2) . ? Ni1 C6 2.207(2) . ? Ni1 C7 2.143(2) . ? Ni1 C8 2.1463(18) . ? C2 C3 1.339(3) . ? N2 C3 1.388(2) . ? N2 C21 1.448(2) . ? P2 Ni2 2.2103(6) . ? P2 P3 2.2320(7) . ? P2 P4 2.2146(7) . ? Ni2 C33 1.8918(18) . ? Ni2 C36 2.083(2) . ? Ni2 C37 2.150(2) . ? Ni2 C38 2.192(2) . ? Ni2 C39 2.155(2) . ? Ni2 C40 2.148(2) . ? N3 C33 1.366(2) . ? N3 C34 1.388(2) . ? N3 C41 1.440(2) . ? P3 P4 2.1649(7) . ? C4 C5 1.427(3) . ? C4 C8 1.403(3) . ? N4 C33 1.367(2) . ? N4 C35 1.385(2) . ? N4 C53 1.446(2) . ? C5 C6 1.386(3) . ? C6 C7 1.422(3) . ? C7 C8 1.407(3) . ? C9 C10 1.400(3) . ? C9 C14 1.404(3) . ? C10 C11 1.397(3) . ? C10 C15 1.516(2) . ? C11 C12 1.381(3) . ? C12 C13 1.388(3) . ? C13 C14 1.394(3) . ? C14 C18 1.521(3) . ? C15 C16 1.531(3) . ? C15 C17 1.522(3) . ? C18 C19 1.532(3) . ? C18 C20 1.532(3) . ? C21 C22 1.399(3) . ? C21 C26 1.414(3) . ? C22 C23 1.397(3) . ? C22 C27 1.526(3) . ? C23 C24 1.381(3) . ? C24 C25 1.387(3) . ? C25 C26 1.390(3) . ? C26 C30 1.521(3) . ? C27 C28 1.531(3) . ? C27 C29 1.534(3) . ? C30 C31 1.530(3) . ? C30 C32 1.530(3) . ? C34 C35 1.344(3) . ? C36 C37 1.430(4) . ? C36 C40 1.401(4) . ? C37 C38 1.386(3) . ? C38 C39 1.423(4) . ? C39 C40 1.402(4) . ? C41 C42 1.401(3) . ? C41 C46 1.403(3) . ? C42 C43 1.395(3) . ? C42 C47 1.518(3) . ? C43 C44 1.386(3) . ? C44 C45 1.389(3) . ? C45 C46 1.399(3) . ? C46 C50 1.519(3) . ? C47 C48 1.530(3) . ? C47 C49 1.522(3) . ? C50 C51 1.523(3) . ? C50 C52 1.534(3) . ? C53 C54 1.401(3) . ? C53 C58 1.406(3) . ? C54 C55 1.399(3) . ? C54 C59 1.523(3) . ? C55 C56 1.382(3) . ? C56 C57 1.385(3) . ? C57 C58 1.391(3) . ? C58 C62 1.523(3) . ? C59 C60 1.528(3) . ? C59 C61 1.539(3) . ? C62 C63 1.534(3) . ? C62 C64 1.523(3) . ? O1 C101 1.552(10) . ? O1 C104 1.399(9) . ? C101 C102 1.491(8) . ? C102 C103 1.489(9) . ? C103 C104 1.497(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 127.94(13) . . ? N1 C1 N2 103.42(14) . . ? N2 C1 Ni1 128.50(13) . . ? C1 N1 C2 111.41(15) . . ? C1 N1 C9 123.84(14) . . ? C2 N1 C9 123.74(15) . . ? Ni1 P1 P3 112.66(2) . . ? Ni1 P1 P4 107.40(3) . . ? P4 P1 P3 58.30(2) . . ? C1 Ni1 P1 87.82(5) . . ? C1 Ni1 C4 166.77(8) . . ? C1 Ni1 C5 146.31(8) . . ? C1 Ni1 C6 114.44(8) . . ? C1 Ni1 C7 105.64(8) . . ? C1 Ni1 C8 128.15(8) . . ? C4 Ni1 P1 101.20(6) . . ? C4 Ni1 C5 39.20(9) . . ? C4 Ni1 C6 64.01(8) . . ? C4 Ni1 C7 64.54(8) . . ? C4 Ni1 C8 38.69(9) . . ? C5 Ni1 P1 108.27(6) . . ? C5 Ni1 C6 36.95(9) . . ? C6 Ni1 P1 140.61(7) . . ? C7 Ni1 P1 165.30(6) . . ? C7 Ni1 C5 63.47(8) . . ? C7 Ni1 C6 38.13(9) . . ? C7 Ni1 C8 38.31(9) . . ? C8 Ni1 P1 127.88(7) . . ? C8 Ni1 C5 64.34(8) . . ? C8 Ni1 C6 63.79(8) . . ? C3 C2 N1 106.83(16) . . ? C1 N2 C3 111.22(15) . . ? C1 N2 C21 124.39(15) . . ? C3 N2 C21 124.14(15) . . ? Ni2 P2 P3 111.10(3) . . ? Ni2 P2 P4 108.72(3) . . ? P4 P2 P3 58.27(2) . . ? C33 Ni2 P2 89.29(5) . . ? C33 Ni2 C36 169.55(10) . . ? C33 Ni2 C37 142.41(9) . . ? C33 Ni2 C38 111.74(8) . . ? C33 Ni2 C39 106.30(8) . . ? C33 Ni2 C40 131.03(10) . . ? C36 Ni2 P2 99.17(7) . . ? C36 Ni2 C37 39.44(10) . . ? C36 Ni2 C38 64.38(9) . . ? C36 Ni2 C39 64.38(9) . . ? C36 Ni2 C40 38.64(11) . . ? C37 Ni2 P2 109.53(7) . . ? C37 Ni2 C38 37.23(9) . . ? C37 Ni2 C39 63.53(10) . . ? C38 Ni2 P2 143.67(7) . . ? C39 Ni2 P2 161.71(7) . . ? C39 Ni2 C38 38.21(10) . . ? C40 Ni2 P2 123.88(7) . . ? C40 Ni2 C37 64.45(10) . . ? C40 Ni2 C38 63.89(9) . . ? C40 Ni2 C39 38.03(10) . . ? C2 C3 N2 107.11(16) . . ? C33 N3 C34 111.75(16) . . ? C33 N3 C41 125.70(15) . . ? C34 N3 C41 121.54(16) . . ? P2 P3 P1 80.66(2) . . ? P4 P3 P1 60.34(2) . . ? P4 P3 P2 60.46(2) . . ? C5 C4 Ni1 73.34(11) . . ? C8 C4 Ni1 72.98(11) . . ? C8 C4 C5 108.34(19) . . ? C33 N4 C35 111.77(15) . . ? C33 N4 C53 125.68(15) . . ? C35 N4 C53 122.40(15) . . ? P1 P4 P2 81.54(2) . . ? P3 P4 P1 61.37(2) . . ? P3 P4 P2 61.27(2) . . ? C4 C5 Ni1 67.46(11) . . ? C6 C5 Ni1 73.21(12) . . ? C6 C5 C4 108.12(19) . . ? C5 C6 Ni1 69.83(12) . . ? C5 C6 C7 107.55(19) . . ? C7 C6 Ni1 68.48(11) . . ? C6 C7 Ni1 73.38(12) . . ? C8 C7 Ni1 70.99(11) . . ? C8 C7 C6 108.8(2) . . ? C4 C8 Ni1 68.33(11) . . ? C4 C8 C7 106.93(19) . . ? C7 C8 Ni1 70.70(11) . . ? C10 C9 N1 119.30(16) . . ? C10 C9 C14 123.03(17) . . ? C14 C9 N1 117.67(16) . . ? C9 C10 C15 122.01(16) . . ? C11 C10 C9 117.02(17) . . ? C11 C10 C15 120.88(17) . . ? C12 C11 C10 121.41(18) . . ? C11 C12 C13 120.14(18) . . ? C12 C13 C14 121.11(18) . . ? C9 C14 C18 122.05(17) . . ? C13 C14 C9 117.19(17) . . ? C13 C14 C18 120.72(17) . . ? C10 C15 C16 109.17(16) . . ? C10 C15 C17 112.40(16) . . ? C17 C15 C16 111.13(17) . . ? C14 C18 C19 113.15(18) . . ? C14 C18 C20 110.07(16) . . ? C19 C18 C20 109.20(18) . . ? C22 C21 N2 119.36(16) . . ? C22 C21 C26 122.72(17) . . ? C26 C21 N2 117.89(17) . . ? C21 C22 C27 123.21(18) . . ? C23 C22 C21 117.28(18) . . ? C23 C22 C27 119.35(19) . . ? C24 C23 C22 121.3(2) . . ? C23 C24 C25 120.2(2) . . ? C24 C25 C26 121.36(19) . . ? C21 C26 C30 121.62(17) . . ? C25 C26 C21 117.04(18) . . ? C25 C26 C30 121.20(17) . . ? C22 C27 C28 112.95(19) . . ? C22 C27 C29 109.04(17) . . ? C28 C27 C29 109.46(18) . . ? C26 C30 C31 110.42(17) . . ? C26 C30 C32 114.13(17) . . ? C32 C30 C31 108.82(17) . . ? N3 C33 Ni2 126.54(13) . . ? N3 C33 N4 103.09(15) . . ? N4 C33 Ni2 130.32(13) . . ? C35 C34 N3 106.60(17) . . ? C34 C35 N4 106.78(16) . . ? C37 C36 Ni2 72.83(12) . . ? C40 C36 Ni2 73.19(13) . . ? C40 C36 C37 108.1(2) . . ? C36 C37 Ni2 67.73(12) . . ? C38 C37 Ni2 73.02(12) . . ? C38 C37 C36 108.1(2) . . ? C37 C38 Ni2 69.75(12) . . ? C37 C38 C39 107.5(2) . . ? C39 C38 Ni2 69.49(12) . . ? C38 C39 Ni2 72.30(13) . . ? C40 C39 Ni2 70.70(13) . . ? C40 C39 C38 108.7(2) . . ? C36 C40 Ni2 68.17(13) . . ? C36 C40 C39 107.4(2) . . ? C39 C40 Ni2 71.26(13) . . ? C42 C41 N3 119.24(17) . . ? C42 C41 C46 123.39(18) . . ? C46 C41 N3 117.36(17) . . ? C41 C42 C47 121.84(18) . . ? C43 C42 C41 116.89(19) . . ? C43 C42 C47 121.25(18) . . ? C44 C43 C42 121.4(2) . . ? C43 C44 C45 120.39(19) . . ? C44 C45 C46 120.8(2) . . ? C41 C46 C50 122.24(18) . . ? C45 C46 C41 117.18(18) . . ? C45 C46 C50 120.56(18) . . ? C42 C47 C48 112.86(19) . . ? C42 C47 C49 110.06(17) . . ? C49 C47 C48 110.2(2) . . ? C46 C50 C51 112.13(18) . . ? C46 C50 C52 111.84(18) . . ? C51 C50 C52 109.8(2) . . ? C54 C53 N4 118.80(17) . . ? C54 C53 C58 122.94(18) . . ? C58 C53 N4 118.17(17) . . ? C53 C54 C59 122.25(17) . . ? C55 C54 C53 117.11(18) . . ? C55 C54 C59 120.56(18) . . ? C56 C55 C54 121.2(2) . . ? C55 C56 C57 120.26(19) . . ? C56 C57 C58 121.3(2) . . ? C53 C58 C62 121.50(18) . . ? C57 C58 C53 117.14(19) . . ? C57 C58 C62 121.18(19) . . ? C54 C59 C60 112.68(17) . . ? C54 C59 C61 110.66(16) . . ? C60 C59 C61 109.16(16) . . ? C58 C62 C63 113.3(2) . . ? C58 C62 C64 109.80(19) . . ? C64 C62 C63 111.1(2) . . ? C104 O1 C101 102.3(7) . . ? C102 C101 O1 102.2(6) . . ? C103 C102 C101 102.9(6) . . ? C102 C103 C104 104.7(5) . . ? O1 C104 C103 110.5(7) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 12 8 0.0338 0.0023 12.0209 7.9881 -0.1813 -0.0841 0.9855 0 -12 -8 0.0402 -0.0023 -12.0209 -7.9881 0.1813 0.0841 -0.9855 9 -4 1 0.1032 9.0034 -4.0031 1.0114 -0.9502 -0.2800 -0.3412 -8 -1 -5 0.1041 -8.0039 -1.0055 -5.0062 0.9563 0.2281 -0.1221 -2 12 8 0.0557 -1.9986 12.0203 7.9869 0.0108 0.0243 1.0272 -1 10 -10 0.0394 -0.9991 10.0122 -10.0195 0.6089 -0.8329 0.0469 1 -9 10 0.0016 0.9993 -9.0106 10.0182 -0.5975 0.7932 0.0034 _database_code_depnum_ccdc_archive 'CCDC 995937' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_date 2013-05-06 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H41 N2 Ni' _chemical_formula_sum 'C32 H41 N2 Ni' _chemical_formula_weight 512.38 _chemical_melting_point ? _chemical_oxdiff_formula 'C32 H41 N2 Ni' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.1771(3) _cell_length_b 9.3242(3) _cell_length_c 18.2253(5) _cell_angle_alpha 92.783(2) _cell_angle_beta 90.158(2) _cell_angle_gamma 116.159(3) _cell_volume 1397.63(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 12154 _cell_measurement_temperature 123.00(16) _cell_measurement_theta_max 76.5000 _cell_measurement_theta_min 4.8480 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 550 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_unetI/netI 0.0188 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 14839 _diffrn_reflns_theta_full 70.93 _diffrn_reflns_theta_max 76.68 _diffrn_reflns_theta_min 4.86 _diffrn_ambient_temperature 123.00(16) _diffrn_detector_area_resol_mean 5.1773 _diffrn_measured_fraction_theta_full 0.9922 _diffrn_measured_fraction_theta_max 0.9677 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -27.00 67.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 -37.0000 -150.0000 94 #__ type_ start__ end____ width___ exp.time_ 2 omega 17.00 110.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 37.0000 30.0000 93 #__ type_ start__ end____ width___ exp.time_ 3 omega 4.00 98.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 -125.0000 150.0000 94 #__ type_ start__ end____ width___ exp.time_ 4 omega -77.00 -15.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 45.0000 -120.0000 62 #__ type_ start__ end____ width___ exp.time_ 5 omega 76.00 113.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 60.0000 37 #__ type_ start__ end____ width___ exp.time_ 6 omega 40.00 85.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 150.0000 45 #__ type_ start__ end____ width___ exp.time_ 7 omega 35.00 65.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 60.0000 30 #__ type_ start__ end____ width___ exp.time_ 8 omega 87.00 155.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 -60.0000 68 #__ type_ start__ end____ width___ exp.time_ 9 omega 42.00 68.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 10 omega 36.00 116.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 -30.0000 80 #__ type_ start__ end____ width___ exp.time_ 11 omega 40.00 77.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -45.0000 -90.0000 37 #__ type_ start__ end____ width___ exp.time_ 12 omega 52.00 114.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 150.0000 62 #__ type_ start__ end____ width___ exp.time_ 13 omega 35.00 60.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 90.0000 25 #__ type_ start__ end____ width___ exp.time_ 14 omega 39.00 143.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -61.0000 -30.0000 104 #__ type_ start__ end____ width___ exp.time_ 15 omega 41.00 69.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 120.0000 28 #__ type_ start__ end____ width___ exp.time_ 16 omega 113.00 147.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -77.0000 150.0000 34 #__ type_ start__ end____ width___ exp.time_ 17 omega 35.00 116.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -111.0000 -120.0000 81 #__ type_ start__ end____ width___ exp.time_ 18 omega 39.00 65.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 19 omega 27.00 154.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 0.0000 90.0000 127 #__ type_ start__ end____ width___ exp.time_ 20 omega -71.00 33.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 57.0000 30.0000 104 #__ type_ start__ end____ width___ exp.time_ 21 omega 12.00 115.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 57.0000 90.0000 103 #__ type_ start__ end____ width___ exp.time_ 22 omega 15.00 117.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 37.0000 -150.0000 102 #__ type_ start__ end____ width___ exp.time_ 23 omega 12.00 115.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 57.0000 -90.0000 103 #__ type_ start__ end____ width___ exp.time_ 24 omega 85.00 158.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 45.0000 120.0000 73 #__ type_ start__ end____ width___ exp.time_ 25 omega 83.00 158.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 61.0000 -120.0000 75 #__ type_ start__ end____ width___ exp.time_ 26 omega 82.00 158.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 30.0000 -150.0000 76 #__ type_ start__ end____ width___ exp.time_ 27 omega 79.00 158.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 77.0000 60.0000 79 #__ type_ start__ end____ width___ exp.time_ 28 omega 35.00 69.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 113.0000 -30.0000 -60.0000 34 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0584908000 _diffrn_orient_matrix_UB_12 -0.0263555000 _diffrn_orient_matrix_UB_13 0.0752293000 _diffrn_orient_matrix_UB_21 -0.1294080000 _diffrn_orient_matrix_UB_22 -0.1757536000 _diffrn_orient_matrix_UB_23 -0.0054795000 _diffrn_orient_matrix_UB_31 0.1218082000 _diffrn_orient_matrix_UB_32 -0.0490350000 _diffrn_orient_matrix_UB_33 -0.0384411000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5475 _reflns_number_total 5715 _reflns_odcompleteness_completeness 99.22 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 70.93 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 0.303 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.040 _refine_ls_extinction_coef 0.0014(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 325 _refine_ls_number_reflns 5715 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0293 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.6198P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.0745 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C121(H121), C161(H161), C221(H221), C261(H261) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25) 2.c Idealised Me refined as rotating group: C122(H12a,H12b,H12c), C123(H12d,H12e,H12f), C162(H16a,H16b,H16c), C163(H16d, H16e,H16f), C222(H22a,H22b,H22c), C223(H22d,H22e,H22f), C262(H26a,H26b,H26c), C263(H26d,H26e,H26f) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.98988(13) 0.25089(13) 0.25706(6) 0.0152(2) Uani 1 1 d . . . C2 C 1.03845(14) 0.04322(14) 0.29086(6) 0.0192(2) Uani 1 1 d . . . H2 H 1.0652 -0.0214 0.3199 0.023 Uiso 1 1 calc R . . C3 C 0.99699(14) 0.01687(14) 0.21895(7) 0.0193(2) Uani 1 1 d . . . H3 H 0.9893 -0.0695 0.1886 0.023 Uiso 1 1 calc R . . C4 C 1.10519(16) 0.65893(15) 0.20217(7) 0.0259(3) Uani 1 1 d . . . H4 H 1.2086 0.6914 0.1836 0.031 Uiso 1 1 calc R . . C5 C 0.95725(17) 0.56074(15) 0.16431(7) 0.0259(3) Uani 1 1 d . . . H5 H 0.9464 0.5146 0.1170 0.031 Uiso 1 1 calc R . . C6 C 0.82835(16) 0.54476(15) 0.21089(8) 0.0270(3) Uani 1 1 d . . . H6 H 0.7181 0.4890 0.1990 0.032 Uiso 1 1 calc R . . C7 C 0.89668(16) 0.62829(15) 0.27834(7) 0.0261(3) Uani 1 1 d . . . H7 H 0.8396 0.6359 0.3192 0.031 Uiso 1 1 calc R . . C8 C 1.06881(16) 0.69896(14) 0.27284(7) 0.0257(3) Uani 1 1 d . . . H8 H 1.1439 0.7607 0.3096 0.031 Uiso 1 1 calc R . . C11 C 0.91425(14) 0.16332(13) 0.12702(6) 0.0169(2) Uani 1 1 d . . . C12 C 0.74993(14) 0.12780(14) 0.11684(6) 0.0199(2) Uani 1 1 d . . . C13 C 0.70224(16) 0.15719(16) 0.04875(7) 0.0254(3) Uani 1 1 d . . . H13 H 0.5946 0.1365 0.0403 0.031 Uiso 1 1 calc R . . C14 C 0.81288(17) 0.21672(17) -0.00656(7) 0.0285(3) Uani 1 1 d . . . H14 H 0.7793 0.2374 -0.0513 0.034 Uiso 1 1 calc R . . C15 C 0.97275(16) 0.24563(16) 0.00422(7) 0.0259(3) Uani 1 1 d . . . H15 H 1.0448 0.2828 -0.0340 0.031 Uiso 1 1 calc R . . C16 C 1.02797(14) 0.21989(14) 0.07157(6) 0.0193(2) Uani 1 1 d . . . C21 C 1.07574(14) 0.26247(13) 0.38586(6) 0.0165(2) Uani 1 1 d . . . C22 C 0.96046(14) 0.20895(14) 0.44080(6) 0.0197(2) Uani 1 1 d . . . C23 C 1.00229(17) 0.29361(16) 0.50897(7) 0.0265(3) Uani 1 1 d . . . H23 H 0.9282 0.2622 0.5466 0.032 Uiso 1 1 calc R . . C24 C 1.15218(18) 0.42348(17) 0.52148(7) 0.0296(3) Uani 1 1 d . . . H24 H 1.1767 0.4799 0.5669 0.035 Uiso 1 1 calc R . . C25 C 1.26574(16) 0.46991(16) 0.46702(7) 0.0268(3) Uani 1 1 d . . . H25 H 1.3672 0.5554 0.4767 0.032 Uiso 1 1 calc R . . C26 C 1.23036(14) 0.39033(14) 0.39768(6) 0.0204(2) Uani 1 1 d . . . C121 C 0.62785(15) 0.05235(17) 0.17600(7) 0.0273(3) Uani 1 1 d . . . H121 H 0.6828 0.0959 0.2238 0.033 Uiso 1 1 calc R . . C122 C 0.57320(18) -0.12895(19) 0.17221(10) 0.0409(4) Uani 1 1 d . . . H12A H 0.5193 -0.1746 0.1257 0.061 Uiso 1 1 calc R . . H12B H 0.4999 -0.1761 0.2111 0.061 Uiso 1 1 calc R . . H12C H 0.6663 -0.1495 0.1774 0.061 Uiso 1 1 calc R . . C123 C 0.47977(17) 0.08678(18) 0.17180(9) 0.0347(3) Uani 1 1 d . . . H12D H 0.5152 0.2001 0.1709 0.052 Uiso 1 1 calc R . . H12E H 0.4144 0.0470 0.2139 0.052 Uiso 1 1 calc R . . H12F H 0.4168 0.0348 0.1279 0.052 Uiso 1 1 calc R . . C161 C 1.20582(15) 0.25846(15) 0.08360(7) 0.0226(2) Uani 1 1 d . . . H161 H 1.2116 0.1884 0.1207 0.027 Uiso 1 1 calc R . . C162 C 1.28328(18) 0.22829(18) 0.01403(8) 0.0335(3) Uani 1 1 d . . . H16A H 1.2187 0.1212 -0.0058 0.050 Uiso 1 1 calc R . . H16B H 1.3907 0.2418 0.0258 0.050 Uiso 1 1 calc R . . H16C H 1.2891 0.3030 -0.0216 0.050 Uiso 1 1 calc R . . C163 C 1.30254(17) 0.43144(18) 0.11360(9) 0.0341(3) Uani 1 1 d . . . H16D H 1.3006 0.5029 0.0778 0.051 Uiso 1 1 calc R . . H16E H 1.4128 0.4517 0.1238 0.051 Uiso 1 1 calc R . . H16F H 1.2549 0.4484 0.1580 0.051 Uiso 1 1 calc R . . C221 C 0.79456(15) 0.06793(15) 0.42660(7) 0.0235(3) Uani 1 1 d . . . H221 H 0.8037 0.0023 0.3849 0.028 Uiso 1 1 calc R . . C222 C 0.67020(17) 0.12701(19) 0.40497(9) 0.0359(3) Uani 1 1 d . . . H22A H 0.6539 0.1864 0.4460 0.054 Uiso 1 1 calc R . . H22B H 0.5691 0.0370 0.3909 0.054 Uiso 1 1 calc R . . H22C H 0.7094 0.1948 0.3644 0.054 Uiso 1 1 calc R . . C223 C 0.73750(18) -0.03801(18) 0.49212(9) 0.0373(3) Uani 1 1 d . . . H22D H 0.8175 -0.0735 0.5048 0.056 Uiso 1 1 calc R . . H22E H 0.6363 -0.1291 0.4794 0.056 Uiso 1 1 calc R . . H22F H 0.7229 0.0221 0.5333 0.056 Uiso 1 1 calc R . . C261 C 1.35804(15) 0.43372(16) 0.33917(7) 0.0249(3) Uani 1 1 d . . . H261 H 1.3018 0.4046 0.2910 0.030 Uiso 1 1 calc R . . C262 C 1.47437(19) 0.61212(18) 0.34156(10) 0.0414(4) Uani 1 1 d . . . H26A H 1.4131 0.6730 0.3406 0.062 Uiso 1 1 calc R . . H26B H 1.5429 0.6345 0.2998 0.062 Uiso 1 1 calc R . . H26C H 1.5402 0.6409 0.3858 0.062 Uiso 1 1 calc R . . C263 C 1.45345(17) 0.33579(17) 0.34657(8) 0.0319(3) Uani 1 1 d . . . H26D H 1.5092 0.3618 0.3935 0.048 Uiso 1 1 calc R . . H26E H 1.5311 0.3602 0.3083 0.048 Uiso 1 1 calc R . . H26F H 1.3800 0.2238 0.3426 0.048 Uiso 1 1 calc R . . N1 N 0.96782(11) 0.14444(11) 0.19876(5) 0.01574(19) Uani 1 1 d . . . N2 N 1.03365(11) 0.18535(11) 0.31344(5) 0.01572(19) Uani 1 1 d . . . Ni1 Ni 0.97593(2) 0.44597(2) 0.263007(10) 0.01805(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0142(5) 0.0162(5) 0.0146(5) 0.0022(4) 0.0006(4) 0.0061(4) C2 0.0237(6) 0.0172(5) 0.0203(5) 0.0028(4) 0.0000(4) 0.0122(5) C3 0.0229(6) 0.0155(5) 0.0215(6) -0.0002(4) 0.0002(4) 0.0105(4) C4 0.0255(6) 0.0203(6) 0.0330(7) 0.0107(5) 0.0095(5) 0.0101(5) C5 0.0388(7) 0.0235(6) 0.0191(6) 0.0083(5) 0.0022(5) 0.0162(5) C6 0.0236(6) 0.0231(6) 0.0373(7) 0.0097(5) -0.0016(5) 0.0123(5) C7 0.0342(7) 0.0234(6) 0.0299(6) 0.0071(5) 0.0099(5) 0.0205(5) C8 0.0313(7) 0.0156(5) 0.0314(7) 0.0007(5) -0.0025(5) 0.0116(5) C11 0.0208(5) 0.0161(5) 0.0140(5) -0.0001(4) -0.0016(4) 0.0086(4) C12 0.0202(6) 0.0200(5) 0.0178(5) -0.0024(4) -0.0015(4) 0.0077(5) C13 0.0235(6) 0.0301(6) 0.0232(6) -0.0019(5) -0.0064(5) 0.0127(5) C14 0.0345(7) 0.0351(7) 0.0180(6) 0.0037(5) -0.0052(5) 0.0170(6) C15 0.0315(7) 0.0300(6) 0.0174(6) 0.0060(5) 0.0032(5) 0.0142(5) C16 0.0228(6) 0.0185(5) 0.0175(5) 0.0010(4) 0.0015(4) 0.0098(5) C21 0.0206(5) 0.0180(5) 0.0138(5) 0.0020(4) -0.0011(4) 0.0110(4) C22 0.0217(6) 0.0215(6) 0.0187(5) 0.0035(4) 0.0016(4) 0.0120(5) C23 0.0314(7) 0.0317(7) 0.0177(6) 0.0023(5) 0.0057(5) 0.0151(6) C24 0.0384(7) 0.0308(7) 0.0174(6) -0.0039(5) -0.0036(5) 0.0140(6) C25 0.0265(6) 0.0257(6) 0.0219(6) 0.0000(5) -0.0056(5) 0.0059(5) C26 0.0212(6) 0.0226(6) 0.0183(5) 0.0046(4) -0.0010(4) 0.0101(5) C121 0.0175(6) 0.0378(7) 0.0204(6) 0.0000(5) -0.0005(5) 0.0066(5) C122 0.0245(7) 0.0419(8) 0.0551(10) 0.0238(7) 0.0087(6) 0.0115(6) C123 0.0229(6) 0.0372(8) 0.0403(8) -0.0066(6) 0.0041(6) 0.0107(6) C161 0.0222(6) 0.0260(6) 0.0216(6) 0.0044(5) 0.0048(5) 0.0121(5) C162 0.0332(7) 0.0387(8) 0.0335(7) -0.0003(6) 0.0092(6) 0.0205(6) C163 0.0230(6) 0.0345(7) 0.0413(8) -0.0081(6) 0.0008(6) 0.0104(6) C221 0.0213(6) 0.0247(6) 0.0233(6) 0.0029(5) 0.0049(5) 0.0090(5) C222 0.0234(7) 0.0382(8) 0.0452(9) 0.0068(7) -0.0015(6) 0.0124(6) C223 0.0332(8) 0.0337(7) 0.0395(8) 0.0150(6) 0.0064(6) 0.0084(6) C261 0.0190(6) 0.0319(7) 0.0192(6) 0.0060(5) -0.0001(5) 0.0066(5) C262 0.0337(8) 0.0330(8) 0.0566(10) 0.0187(7) 0.0152(7) 0.0121(6) C263 0.0283(7) 0.0328(7) 0.0336(7) 0.0019(6) 0.0080(6) 0.0125(6) N1 0.0183(5) 0.0152(4) 0.0143(4) 0.0011(3) -0.0003(3) 0.0079(4) N2 0.0189(5) 0.0159(4) 0.0144(4) 0.0022(3) 0.0001(3) 0.0095(4) Ni1 0.02532(12) 0.01561(11) 0.01645(12) 0.00269(7) 0.00156(8) 0.01179(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3690(14) . ? C1 N2 1.3659(14) . ? C1 Ni1 1.8770(11) . ? C2 H2 0.9300 . ? C2 C3 1.3440(17) . ? C2 N2 1.3879(15) . ? C3 H3 0.9300 . ? C3 N1 1.3945(14) . ? C4 H4 0.9300 . ? C4 C5 1.4124(19) . ? C4 C8 1.4055(19) . ? C4 Ni1 2.1734(12) . ? C5 H5 0.9300 . ? C5 C6 1.4158(19) . ? C5 Ni1 2.1810(12) . ? C6 H6 0.9300 . ? C6 C7 1.408(2) . ? C6 Ni1 2.1824(12) . ? C7 H7 0.9300 . ? C7 C8 1.4245(19) . ? C7 Ni1 2.1312(12) . ? C8 H8 0.9300 . ? C8 Ni1 2.1233(12) . ? C11 C12 1.4037(16) . ? C11 C16 1.4004(16) . ? C11 N1 1.4413(14) . ? C12 C13 1.3938(17) . ? C12 C121 1.5159(17) . ? C13 H13 0.9300 . ? C13 C14 1.3850(19) . ? C14 H14 0.9300 . ? C14 C15 1.3814(19) . ? C15 H15 0.9300 . ? C15 C16 1.3977(17) . ? C16 C161 1.5212(17) . ? C21 C22 1.3999(16) . ? C21 C26 1.4011(16) . ? C21 N2 1.4382(14) . ? C22 C23 1.3961(17) . ? C22 C221 1.5211(17) . ? C23 H23 0.9300 . ? C23 C24 1.383(2) . ? C24 H24 0.9300 . ? C24 C25 1.3815(19) . ? C25 H25 0.9300 . ? C25 C26 1.3955(17) . ? C26 C261 1.5179(17) . ? C121 H121 0.9800 . ? C121 C122 1.535(2) . ? C121 C123 1.5304(19) . ? C122 H12A 0.9600 . ? C122 H12B 0.9600 . ? C122 H12C 0.9600 . ? C123 H12D 0.9600 . ? C123 H12E 0.9600 . ? C123 H12F 0.9600 . ? C161 H161 0.9800 . ? C161 C162 1.5294(17) . ? C161 C163 1.5289(18) . ? C162 H16A 0.9600 . ? C162 H16B 0.9600 . ? C162 H16C 0.9600 . ? C163 H16D 0.9600 . ? C163 H16E 0.9600 . ? C163 H16F 0.9600 . ? C221 H221 0.9800 . ? C221 C222 1.5278(18) . ? C221 C223 1.5291(18) . ? C222 H22A 0.9600 . ? C222 H22B 0.9600 . ? C222 H22C 0.9600 . ? C223 H22D 0.9600 . ? C223 H22E 0.9600 . ? C223 H22F 0.9600 . ? C261 H261 0.9800 . ? C261 C262 1.5282(19) . ? C261 C263 1.5281(19) . ? C262 H26A 0.9600 . ? C262 H26B 0.9600 . ? C262 H26C 0.9600 . ? C263 H26D 0.9600 . ? C263 H26E 0.9600 . ? C263 H26F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 131.11(8) . . ? N2 C1 N1 103.15(9) . . ? N2 C1 Ni1 125.68(8) . . ? C3 C2 H2 126.6 . . ? C3 C2 N2 106.87(10) . . ? N2 C2 H2 126.6 . . ? C2 C3 H3 126.8 . . ? C2 C3 N1 106.50(10) . . ? N1 C3 H3 126.8 . . ? C5 C4 H4 126.0 . . ? C5 C4 Ni1 71.37(7) . . ? C8 C4 H4 126.0 . . ? C8 C4 C5 108.03(12) . . ? C8 C4 Ni1 68.99(7) . . ? Ni1 C4 H4 125.2 . . ? C4 C5 H5 125.9 . . ? C4 C5 C6 108.18(12) . . ? C4 C5 Ni1 70.78(7) . . ? C6 C5 H5 125.9 . . ? C6 C5 Ni1 71.12(7) . . ? Ni1 C5 H5 123.8 . . ? C5 C6 H6 126.1 . . ? C5 C6 Ni1 71.01(7) . . ? C7 C6 C5 107.89(12) . . ? C7 C6 H6 126.1 . . ? C7 C6 Ni1 68.99(7) . . ? Ni1 C6 H6 125.5 . . ? C6 C7 H7 126.1 . . ? C6 C7 C8 107.86(11) . . ? C6 C7 Ni1 72.93(7) . . ? C8 C7 H7 126.1 . . ? C8 C7 Ni1 70.14(7) . . ? Ni1 C7 H7 122.5 . . ? C4 C8 C7 107.99(12) . . ? C4 C8 H8 126.0 . . ? C4 C8 Ni1 72.85(7) . . ? C7 C8 H8 126.0 . . ? C7 C8 Ni1 70.74(7) . . ? Ni1 C8 H8 122.1 . . ? C12 C11 N1 117.87(10) . . ? C16 C11 C12 123.09(10) . . ? C16 C11 N1 119.02(10) . . ? C11 C12 C121 121.32(10) . . ? C13 C12 C11 117.22(11) . . ? C13 C12 C121 121.38(11) . . ? C12 C13 H13 119.5 . . ? C14 C13 C12 120.93(12) . . ? C14 C13 H13 119.5 . . ? C13 C14 H14 119.7 . . ? C15 C14 C13 120.57(11) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 119.5 . . ? C14 C15 C16 121.05(12) . . ? C16 C15 H15 119.5 . . ? C11 C16 C161 122.43(10) . . ? C15 C16 C11 117.08(11) . . ? C15 C16 C161 120.45(11) . . ? C22 C21 C26 123.00(11) . . ? C22 C21 N2 118.94(10) . . ? C26 C21 N2 118.05(10) . . ? C21 C22 C221 121.75(11) . . ? C23 C22 C21 117.12(11) . . ? C23 C22 C221 121.10(11) . . ? C22 C23 H23 119.5 . . ? C24 C23 C22 121.08(12) . . ? C24 C23 H23 119.5 . . ? C23 C24 H24 119.8 . . ? C25 C24 C23 120.48(12) . . ? C25 C24 H24 119.8 . . ? C24 C25 H25 119.5 . . ? C24 C25 C26 120.95(12) . . ? C26 C25 H25 119.5 . . ? C21 C26 C261 121.38(11) . . ? C25 C26 C21 117.30(11) . . ? C25 C26 C261 121.21(11) . . ? C12 C121 H121 107.8 . . ? C12 C121 C122 109.42(11) . . ? C12 C121 C123 113.78(12) . . ? C122 C121 H121 107.8 . . ? C123 C121 H121 107.8 . . ? C123 C121 C122 110.00(11) . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12B 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12E 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C16 C161 H161 107.7 . . ? C16 C161 C162 112.79(11) . . ? C16 C161 C163 110.59(10) . . ? C162 C161 H161 107.7 . . ? C163 C161 H161 107.7 . . ? C163 C161 C162 110.07(11) . . ? C161 C162 H16A 109.5 . . ? C161 C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16A C162 H16B 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C163 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16D C163 H16E 109.5 . . ? H16D C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C22 C221 H221 107.7 . . ? C22 C221 C222 110.21(11) . . ? C22 C221 C223 112.47(11) . . ? C222 C221 H221 107.7 . . ? C222 C221 C223 110.94(11) . . ? C223 C221 H221 107.7 . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22B 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22E 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C26 C261 H261 107.9 . . ? C26 C261 C262 113.26(12) . . ? C26 C261 C263 109.66(10) . . ? C262 C261 H261 107.9 . . ? C263 C261 H261 107.9 . . ? C263 C261 C262 110.03(11) . . ? C261 C262 H26A 109.5 . . ? C261 C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26A C262 H26B 109.5 . . ? H26A C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C263 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26D C263 H26E 109.5 . . ? H26D C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C1 N1 C3 111.64(9) . . ? C1 N1 C11 122.44(9) . . ? C3 N1 C11 125.87(10) . . ? C1 N2 C2 111.85(9) . . ? C1 N2 C21 122.29(9) . . ? C2 N2 C21 125.81(9) . . ? C1 Ni1 C4 129.36(5) . . ? C1 Ni1 C5 121.25(5) . . ? C1 Ni1 C6 136.33(5) . . ? C1 Ni1 C7 164.86(5) . . ? C1 Ni1 C8 155.35(5) . . ? C4 Ni1 C5 37.85(5) . . ? C4 Ni1 C6 63.46(5) . . ? C5 Ni1 C6 37.87(5) . . ? C7 Ni1 C4 64.26(5) . . ? C7 Ni1 C5 63.92(5) . . ? C7 Ni1 C6 38.09(5) . . ? C8 Ni1 C4 38.17(5) . . ? C8 Ni1 C5 63.96(5) . . ? C8 Ni1 C6 64.24(5) . . ? C8 Ni1 C7 39.12(5) . . ? _database_code_depnum_ccdc_archive 'CCDC 995938' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1-H _audit_creation_date 2013-07-03 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C32 H42 N2 Ni' _chemical_formula_sum 'C32 H42 N2 Ni' _chemical_formula_weight 513.39 _chemical_melting_point ? _chemical_oxdiff_formula 'C32 H42 N2 Ni' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4764(4) _cell_length_b 36.2568(10) _cell_length_c 12.7163(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.223(3) _cell_angle_gamma 90.00 _cell_volume 5752.2(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 11451 _cell_measurement_temperature 123.00(10) _cell_measurement_theta_max 31.0410 _cell_measurement_theta_min 3.5990 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.96541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear ? red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier ? _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2208 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 27792 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 3.20 _diffrn_ambient_temperature 123.00(10) _diffrn_detector ATLAS _diffrn_detector_area_resol_mean 7.9851 _diffrn_detector_type CCD _diffrn_measured_fraction_theta_full 0.9851 _diffrn_measured_fraction_theta_max 0.9076 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -46.00 54.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - 33.5453 -38.0000 -150.0000 200 #__ type_ start__ end____ width___ exp.time_ 2 omega 13.00 108.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - 33.5453 57.0000 0.0000 190 #__ type_ start__ end____ width___ exp.time_ 3 omega -120.00 -64.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - -33.8578 178.0000 -90.0000 112 #__ type_ start__ end____ width___ exp.time_ 4 omega -38.00 11.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - -33.8578 57.0000 90.0000 98 #__ type_ start__ end____ width___ exp.time_ 5 omega -109.00 -84.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - -33.8578 -54.0000 -176.0000 50 ; _diffrn_measurement_device SuperNova _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0093226000 _diffrn_orient_matrix_UB_12 0.0189521000 _diffrn_orient_matrix_UB_13 0.0104154000 _diffrn_orient_matrix_UB_21 0.0359143000 _diffrn_orient_matrix_UB_22 -0.0048358000 _diffrn_orient_matrix_UB_23 0.0411158000 _diffrn_orient_matrix_UB_31 0.0431200000 _diffrn_orient_matrix_UB_32 -0.0000779000 _diffrn_orient_matrix_UB_33 -0.0361899000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_source_target 'microfocus sealed X-ray tube' _diffrn_source_type 'Agilent microfocus 1st generation' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 10004 _reflns_number_total 11247 _reflns_odcompleteness_completeness 98.51 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.44 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 0.634 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.085 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 639 _refine_ls_number_reflns 11247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0627 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+30.8404P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1742 _refine_ls_wR_factor_ref 0.1771 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Others Fixed Uiso: H2A(0.028) H3(0.028) H4(0.035) H5(0.036) H6(0.037) H7(0.035) H8(0.032) H12(0.039) H13(0.042) H14(0.034) H22(0.037) H23(0.04) H24(0.036) H31(0.031) H32(0.032) H33(0.063) H34(0.058) H35(0.053) H36(0.051) H37(0.048) H42(0.041) H43(0.04) H44(0.036) H52(0.041) H53(0.041) H54(0.042) H111(0.039) H11A(0.09) H11B(0.09) H11C(0.09) H11D(0.112) H11E(0.112) H11F(0.112) H151(0.033) H15A(0.118) H15B(0.118) H15C(0.118) H15D(0.083) H15E(0.083) H15F(0.083) H211(0.035) H21A(0.079) H21B(0.079) H21C(0.079) H21D(0.073) H21E(0.073) H21F(0.073) H251(0.039) H25A(0.068) H25B(0.068) H25C(0.068) H25D(0.081) H25E(0.081) H25F(0.081) H411(0.042) H41A(0.121) H41B(0.121) H41C(0.121) H41D(0.103) H41E(0.103) H41F(0.103) H451(0.039) H45A(0.095) H45B(0.095) H45C(0.095) H45D(0.117) H45E(0.117) H45F(0.117) H511(0.043) H51A(0.101) H51B(0.101) H51C(0.101) H51D(0.102) H51E(0.102) H51F(0.102) H551(0.055) H55A(0.103) H55B(0.103) H55C(0.103) H55D(0.132) H55E(0.132) H55F(0.132) Fixed X: H2A(0.7767) H3(0.6053) H4(0.6459) H5(0.5692) H6(0.7159) H7(0.8853) H8(0.8391) H12(1.0968) H13(1.1001) H14(0.9623) H22(0.4292) H23(0.2771) H24(0.2782) H31(0.7065) H32(0.7946) H33(0.9168) H34(0.7594) H35(0.6294) H36(0.7178) H37(0.8897) H42(0.7423) H43(0.9243) H44(1.0402) H52(0.3886) H53(0.4686) H54(0.6514) H111(0.876) H11A(0.9616) H11B(1.0736) H11C(0.9965) H11D(0.98) H11E(1.0078) H11F(1.0849) H151(0.7416) H15A(0.8708) H15B(0.8488) H15C(0.7592) H15D(0.668) H15E(0.6337) H15F(0.7235) H211(0.6825) H21A(0.7196) H21B(0.5997) H21C(0.6724) H21D(0.5852) H21E(0.5506) H21F(0.6713) H251(0.5028) H25A(0.3955) H25B(0.4448) H25C(0.3249) H25D(0.3557) H25E(0.2852) H25F(0.3825) H411(0.6086) H41A(0.581) H41B(0.5712) H41C(0.4848) H41D(0.516) H41E(0.6103) H41F(0.6287) H451(0.9653) H45A(1.0458) H45B(1.1299) H45C(1.1285) H45D(1.1156) H45E(1.0162) H45F(1.1054) H511(0.5263) H51A(0.3539) H51B(0.331) H51C(0.4172) H51D(0.391) H51E(0.482) H51F(0.3734) H551(0.8387) H55A(0.9165) H55B(0.8074) H55C(0.8168) H55D(0.924) H55E(0.8283) H55F(0.8155) Fixed Y: H2A(0.118) H3(0.1093) H4(0.286) H5(0.3004) H6(0.2934) H7(0.2793) H8(0.2698) H12(0.2171) H13(0.2405) H14(0.2293) H22(0.1642) H23(0.1859) H24(0.1983) H31(0.3639) H32(0.3562) H33(0.5143) H34(0.5509) H35(0.5551) H36(0.5289) H37(0.5006) H42(0.4419) H43(0.4467) H44(0.4321) H52(0.4476) H53(0.4709) H54(0.4712) H111(0.17) H11A(0.2224) H11B(0.2044) H11C(0.1872) H11D(0.1237) H11E(0.1268) H11F(0.1439) H151(0.17) H15A(0.1655) H15B(0.2066) H15C(0.1768) H15D(0.2271) H15E(0.215) H15F(0.2448) H211(0.1483) H21A(0.1623) H21B(0.1736) H21C(0.1969) H21D(0.0939) H21E(0.1081) H21F(0.0992) H251(0.1887) H25A(0.2354) H25B(0.2482) H25C(0.2354) H25D(0.17) H25E(0.1667) H25F(0.14) H411(0.4268) H41A(0.4743) H41B(0.4452) H41C(0.4465) H41D(0.3808) H41E(0.378) H41F(0.3666) H451(0.4118) H45A(0.4688) H45B(0.4413) H45C(0.4493) H45D(0.3746) H45E(0.359) H45F(0.3808) H511(0.4131) H51A(0.4301) H51B(0.4463) H51C(0.4648) H51D(0.3682) H51E(0.363) H51F(0.3817) H551(0.4413) H55A(0.4206) H55B(0.4267) H55C(0.3963) H55D(0.4869) H55E(0.5044) H55F(0.4952) Fixed Z: H2A(0.1453) H3(0.2339) H4(0.1339) H5(0.3098) H6(0.4428) H7(0.3473) H8(0.1582) H12(0.2367) H13(0.0696) H14(-0.0457) H22(0.5719) H23(0.49) H24(0.3122) H31(0.1211) H32(0.2915) H33(0.213) H34(0.1487) H35(0.2984) H36(0.4582) H37(0.4037) H42(0.6463) H43(0.6707) H44(0.5367) H52(0.0069) H53(- 0.1412) H54(-0.1564) H111(0.3565) H11A(0.4252) H11B(0.4041) H11C(0.4879) H11D(0.2777) H11E(0.3977) H11F(0.3138) H151(0.0025) H15A(-0.1282) H15B(- 0.1602) H15C(-0.1753) H15D(0.0458) H15E(-0.0678) H15F(-0.0525) H211(0.4484) H21A(0.624) H21B(0.6412) H21C(0.5661) H21D(0.4758) H21E(0.5871) H21F(0.5646) H251(0.1401) H25A(0.0696) H25B(0.1771) H25C(0.1713) H25D(0.0367) H25E(0.1381) H25F(0.1218) H411(0.4044) H41A(0.5258) H41B(0.6164) H41C(0.5266) H41D(0.4948) H41E(0.5763) H41F(0.4588) H451(0.2718) H45A(0.3086) H45B(0.2619) H45C(0.383) H45D(0.3004) H45E(0.3608) H45F(0.4219) H511(0.2341) H51A(0.2861) H51B(0.1739) H51C(0.2468) H51D(0.2113) H51E(0.1278) H51F(0.0953) H551(0.0404) H55A(-0.1171) H55B(-0.1763) H55C(-0.0891) H55D(-0.0623) H55E(-0.0003) H55F(-0.1202) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6942(3) 0.19100(11) 0.2567(3) 0.0172(8) Uani 1 1 d . . . C2 C 0.7385(3) 0.13576(12) 0.1824(3) 0.0230(9) Uani 1 1 d . . . H2A H 0.7767 0.1180 0.1453 0.028 Uiso 1 1 calc R . . C3 C 0.6451(4) 0.13093(12) 0.2310(3) 0.0231(9) Uani 1 1 d . . . H3 H 0.6053 0.1093 0.2339 0.028 Uiso 1 1 calc R . . C4 C 0.6830(4) 0.28576(13) 0.1975(4) 0.0289(10) Uani 1 1 d . . . H4 H 0.6459 0.2860 0.1339 0.035 Uiso 1 1 calc R . . C5 C 0.6398(4) 0.29391(12) 0.2960(4) 0.0304(11) Uani 1 1 d . . . H5 H 0.5692 0.3004 0.3098 0.036 Uiso 1 1 calc R . . C6 C 0.7228(4) 0.29043(12) 0.3705(4) 0.0307(11) Uani 1 1 d . . . H6 H 0.7159 0.2934 0.4428 0.037 Uiso 1 1 calc R . . C7 C 0.8176(4) 0.28166(13) 0.3172(4) 0.0295(10) Uani 1 1 d . . . H7 H 0.8853 0.2793 0.3473 0.035 Uiso 1 1 calc R . . C8 C 0.7922(4) 0.27717(12) 0.2108(4) 0.0270(10) Uani 1 1 d . . . H8 H 0.8391 0.2698 0.1582 0.032 Uiso 1 1 calc R . . C10 C 0.8647(3) 0.18897(11) 0.1581(3) 0.0200(9) Uani 1 1 d . . . C11 C 0.9505(3) 0.19329(12) 0.2285(4) 0.0254(9) Uani 1 1 d . . . C12 C 1.0388(4) 0.21307(14) 0.1921(4) 0.0324(11) Uani 1 1 d . . . H12 H 1.0968 0.2171 0.2367 0.039 Uiso 1 1 calc R . . C13 C 1.0413(4) 0.22676(14) 0.0915(4) 0.0352(12) Uani 1 1 d . . . H13 H 1.1001 0.2405 0.0696 0.042 Uiso 1 1 calc R . . C14 C 0.9581(4) 0.22041(13) 0.0227(4) 0.0285(10) Uani 1 1 d . . . H14 H 0.9623 0.2293 -0.0457 0.034 Uiso 1 1 calc R . . C15 C 0.8678(3) 0.20080(12) 0.0541(3) 0.0235(9) Uani 1 1 d . . . C20 C 0.5224(3) 0.17061(11) 0.3364(3) 0.0182(8) Uani 1 1 d . . . C21 C 0.5245(3) 0.16310(12) 0.4439(3) 0.0225(9) Uani 1 1 d . . . C22 C 0.4304(4) 0.16909(14) 0.5001(4) 0.0311(11) Uani 1 1 d . . . H22 H 0.4292 0.1642 0.5719 0.037 Uiso 1 1 calc R . . C23 C 0.3392(4) 0.18210(15) 0.4512(4) 0.0333(11) Uani 1 1 d . . . H23 H 0.2771 0.1859 0.4900 0.040 Uiso 1 1 calc R . . C24 C 0.3401(4) 0.18945(14) 0.3444(4) 0.0304(11) Uani 1 1 d . . . H24 H 0.2782 0.1983 0.3122 0.036 Uiso 1 1 calc R . . C25 C 0.4319(3) 0.18391(12) 0.2838(3) 0.0234(9) Uani 1 1 d . . . C30 C 0.7315(3) 0.43925(11) 0.2449(3) 0.0198(9) Uani 1 1 d . . . C31 C 0.7219(4) 0.38242(12) 0.1695(4) 0.0261(10) Uani 1 1 d . . . H31 H 0.7065 0.3639 0.1211 0.031 Uiso 1 1 calc R . . C32 C 0.7697(4) 0.37821(12) 0.2627(4) 0.0269(10) Uani 1 1 d . . . H32 H 0.7946 0.3562 0.2915 0.032 Uiso 1 1 calc R . . C33 C 0.8580(5) 0.52135(17) 0.2529(6) 0.0523(16) Uani 1 1 d . . . H33 H 0.9168 0.5143 0.2130 0.063 Uiso 1 1 calc R . . C34 C 0.7690(5) 0.54149(14) 0.2160(5) 0.0486(15) Uani 1 1 d . . . H34 H 0.7594 0.5509 0.1487 0.058 Uiso 1 1 calc R . . C35 C 0.6973(5) 0.54454(14) 0.3011(5) 0.0445(15) Uani 1 1 d . . . H35 H 0.6294 0.5551 0.2984 0.053 Uiso 1 1 calc R . . C36 C 0.7459(4) 0.52893(15) 0.3906(5) 0.0425(13) Uani 1 1 d . . . H36 H 0.7178 0.5289 0.4582 0.051 Uiso 1 1 calc R . . C37 C 0.8429(4) 0.51362(14) 0.3605(5) 0.0404(13) Uani 1 1 d . . . H37 H 0.8897 0.5006 0.4037 0.048 Uiso 1 1 calc R . . C40 C 0.8180(3) 0.42080(11) 0.4118(3) 0.0213(9) Uani 1 1 d . . . C41 C 0.7445(4) 0.42705(13) 0.4938(4) 0.0274(10) Uani 1 1 d . . . C42 C 0.7880(4) 0.43694(15) 0.5905(4) 0.0345(11) Uani 1 1 d . . . H42 H 0.7423 0.4419 0.6463 0.041 Uiso 1 1 calc R . . C43 C 0.8973(4) 0.43952(14) 0.6056(4) 0.0337(11) Uani 1 1 d . . . H43 H 0.9243 0.4467 0.6707 0.040 Uiso 1 1 calc R . . C44 C 0.9667(4) 0.43147(13) 0.5247(4) 0.0296(10) Uani 1 1 d . . . H44 H 1.0402 0.4321 0.5367 0.036 Uiso 1 1 calc R . . C45 C 0.9280(4) 0.42242(12) 0.4252(4) 0.0252(9) Uani 1 1 d . . . C50 C 0.6353(3) 0.43449(12) 0.0733(4) 0.0233(9) Uani 1 1 d . . . C51 C 0.5247(4) 0.43339(12) 0.0846(4) 0.0272(10) Uani 1 1 d . . . C52 C 0.4629(4) 0.44760(14) 0.0018(4) 0.0341(11) Uani 1 1 d . . . H52 H 0.3886 0.4476 0.0069 0.041 Uiso 1 1 calc R . . C53 C 0.5108(4) 0.46155(13) -0.0868(4) 0.0345(11) Uani 1 1 d . . . H53 H 0.4686 0.4709 -0.1412 0.041 Uiso 1 1 calc R . . C54 C 0.6204(4) 0.46186(14) -0.0956(4) 0.0350(11) Uani 1 1 d . . . H54 H 0.6514 0.4712 -0.1564 0.042 Uiso 1 1 calc R . . C55 C 0.6865(4) 0.44848(13) -0.0150(4) 0.0297(10) Uani 1 1 d . . . C111 C 0.9503(4) 0.17532(14) 0.3369(4) 0.0324(11) Uani 1 1 d . . . H111 H 0.8760 0.1700 0.3565 0.039 Uiso 1 1 calc R . . C112 C 1.0001(6) 0.19955(18) 0.4213(5) 0.0597(18) Uani 1 1 d . . . H11A H 0.9616 0.2224 0.4252 0.090 Uiso 1 1 calc R . . H11B H 1.0736 0.2044 0.4041 0.090 Uiso 1 1 calc R . . H11C H 0.9965 0.1872 0.4879 0.090 Uiso 1 1 calc R . . C113 C 1.0114(8) 0.13908(18) 0.3310(5) 0.075(2) Uani 1 1 d . . . H11D H 0.9800 0.1237 0.2777 0.112 Uiso 1 1 calc R . . H11E H 1.0078 0.1268 0.3977 0.112 Uiso 1 1 calc R . . H11F H 1.0849 0.1439 0.3138 0.112 Uiso 1 1 calc R . . C151 C 0.7769(4) 0.19251(13) -0.0224(3) 0.0272(10) Uani 1 1 d . . . H151 H 0.7416 0.1700 0.0025 0.033 Uiso 1 1 calc R . . C152 C 0.8176(5) 0.1846(3) -0.1314(5) 0.079(3) Uani 1 1 d . . . H15A H 0.8708 0.1655 -0.1282 0.118 Uiso 1 1 calc R . . H15B H 0.8488 0.2066 -0.1602 0.118 Uiso 1 1 calc R . . H15C H 0.7592 0.1768 -0.1753 0.118 Uiso 1 1 calc R . . C153 C 0.6928(5) 0.22262(18) -0.0244(5) 0.0555(17) Uani 1 1 d . . . H15D H 0.6680 0.2271 0.0458 0.083 Uiso 1 1 calc R . . H15E H 0.6337 0.2150 -0.0678 0.083 Uiso 1 1 calc R . . H15F H 0.7235 0.2448 -0.0525 0.083 Uiso 1 1 calc R . . C211 C 0.6237(4) 0.14830(14) 0.4993(4) 0.0292(10) Uani 1 1 d . . . H211 H 0.6825 0.1483 0.4484 0.035 Uiso 1 1 calc R . . C212 C 0.6569(5) 0.17251(17) 0.5911(5) 0.0527(16) Uani 1 1 d . . . H21A H 0.7196 0.1623 0.6240 0.079 Uiso 1 1 calc R . . H21B H 0.5997 0.1736 0.6412 0.079 Uiso 1 1 calc R . . H21C H 0.6724 0.1969 0.5661 0.079 Uiso 1 1 calc R . . C213 C 0.6061(5) 0.10869(16) 0.5350(5) 0.0484(15) Uani 1 1 d . . . H21D H 0.5852 0.0939 0.4758 0.073 Uiso 1 1 calc R . . H21E H 0.5506 0.1081 0.5871 0.073 Uiso 1 1 calc R . . H21F H 0.6713 0.0992 0.5646 0.073 Uiso 1 1 calc R . . C251 C 0.4300(4) 0.19205(15) 0.1671(4) 0.0323(11) Uani 1 1 d . . . H251 H 0.5028 0.1887 0.1401 0.039 Uiso 1 1 calc R . . C252 C 0.3957(5) 0.23140(15) 0.1442(4) 0.0454(14) Uani 1 1 d . . . H25A H 0.3955 0.2354 0.0696 0.068 Uiso 1 1 calc R . . H25B H 0.4448 0.2482 0.1771 0.068 Uiso 1 1 calc R . . H25C H 0.3249 0.2354 0.1713 0.068 Uiso 1 1 calc R . . C253 C 0.3565(6) 0.16463(16) 0.1107(5) 0.0543(17) Uani 1 1 d . . . H25D H 0.3557 0.1700 0.0367 0.081 Uiso 1 1 calc R . . H25E H 0.2852 0.1667 0.1381 0.081 Uiso 1 1 calc R . . H25F H 0.3825 0.1400 0.1218 0.081 Uiso 1 1 calc R . . C411 C 0.6249(4) 0.42251(15) 0.4789(4) 0.0351(12) Uani 1 1 d . . . H411 H 0.6086 0.4268 0.4044 0.042 Uiso 1 1 calc R . . C412 C 0.5595(5) 0.4496(2) 0.5428(8) 0.081(3) Uani 1 1 d . . . H41A H 0.5810 0.4743 0.5258 0.121 Uiso 1 1 calc R . . H41B H 0.5712 0.4452 0.6164 0.121 Uiso 1 1 calc R . . H41C H 0.4848 0.4465 0.5266 0.121 Uiso 1 1 calc R . . C413 C 0.5920(5) 0.38342(19) 0.5045(7) 0.069(2) Uani 1 1 d . . . H41D H 0.5160 0.3808 0.4948 0.103 Uiso 1 1 calc R . . H41E H 0.6103 0.3780 0.5763 0.103 Uiso 1 1 calc R . . H41F H 0.6287 0.3666 0.4588 0.103 Uiso 1 1 calc R . . C451 C 1.0066(4) 0.41472(15) 0.3370(4) 0.0323(11) Uani 1 1 d . . . H451 H 0.9653 0.4118 0.2718 0.039 Uiso 1 1 calc R . . C452 C 1.0850(5) 0.4465(2) 0.3212(6) 0.0635(19) Uani 1 1 d . . . H45A H 1.0458 0.4688 0.3086 0.095 Uiso 1 1 calc R . . H45B H 1.1299 0.4413 0.2619 0.095 Uiso 1 1 calc R . . H45C H 1.1285 0.4493 0.3830 0.095 Uiso 1 1 calc R . . C453 C 1.0664(7) 0.3790(2) 0.3568(6) 0.078(2) Uani 1 1 d . . . H45D H 1.1156 0.3746 0.3004 0.117 Uiso 1 1 calc R . . H45E H 1.0162 0.3590 0.3608 0.117 Uiso 1 1 calc R . . H45F H 1.1054 0.3808 0.4219 0.117 Uiso 1 1 calc R . . C511 C 0.4712(4) 0.41680(15) 0.1801(4) 0.0357(12) Uani 1 1 d . . . H511 H 0.5263 0.4131 0.2341 0.043 Uiso 1 1 calc R . . C512 C 0.3854(5) 0.4418(2) 0.2259(6) 0.067(2) Uani 1 1 d . . . H51A H 0.3539 0.4301 0.2861 0.101 Uiso 1 1 calc R . . H51B H 0.3310 0.4463 0.1739 0.101 Uiso 1 1 calc R . . H51C H 0.4172 0.4648 0.2468 0.101 Uiso 1 1 calc R . . C513 C 0.4251(6) 0.3789(2) 0.1509(6) 0.068(2) Uani 1 1 d . . . H51D H 0.3910 0.3682 0.2113 0.102 Uiso 1 1 calc R . . H51E H 0.4820 0.3630 0.1278 0.102 Uiso 1 1 calc R . . H51F H 0.3734 0.3817 0.0953 0.102 Uiso 1 1 calc R . . C551 C 0.8066(4) 0.44854(19) -0.0269(4) 0.0459(15) Uani 1 1 d . . . H551 H 0.8387 0.4413 0.0404 0.055 Uiso 1 1 calc R . . C552 C 0.8399(6) 0.4204(2) -0.1101(6) 0.069(2) Uani 1 1 d . . . H55A H 0.9165 0.4206 -0.1171 0.103 Uiso 1 1 calc R . . H55B H 0.8074 0.4267 -0.1763 0.103 Uiso 1 1 calc R . . H55C H 0.8168 0.3963 -0.0891 0.103 Uiso 1 1 calc R . . C553 C 0.8475(6) 0.4874(2) -0.0551(8) 0.088(3) Uani 1 1 d . . . H55D H 0.9240 0.4869 -0.0623 0.132 Uiso 1 1 calc R . . H55E H 0.8283 0.5044 -0.0003 0.132 Uiso 1 1 calc R . . H55F H 0.8155 0.4952 -0.1202 0.132 Uiso 1 1 calc R . . N1 N 0.7680(3) 0.17227(9) 0.1974(3) 0.0190(7) Uani 1 1 d . . . N2 N 0.6184(3) 0.16471(9) 0.2766(3) 0.0186(7) Uani 1 1 d . . . N3 N 0.7754(3) 0.41300(9) 0.3084(3) 0.0205(7) Uani 1 1 d . . . N4 N 0.6994(3) 0.41970(9) 0.1585(3) 0.0201(7) Uani 1 1 d . . . Ni1 Ni 0.69641(5) 0.239369(15) 0.30279(5) 0.02339(15) Uani 1 1 d . . . Ni2 Ni 0.71702(5) 0.488985(15) 0.26897(5) 0.02720(16) Uani 1 1 d . . . H1 H 0.643(6) 0.231(2) 0.386(6) 0.08(2) Uiso 1 1 d . . . H2 H 0.597(7) 0.482(2) 0.262(7) 0.11(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0165(19) 0.020(2) 0.0153(19) 0.0030(15) 0.0025(15) -0.0001(16) C2 0.026(2) 0.017(2) 0.026(2) -0.0021(17) 0.0037(18) 0.0011(17) C3 0.027(2) 0.016(2) 0.027(2) -0.0008(17) 0.0012(18) -0.0022(17) C4 0.037(3) 0.024(2) 0.025(2) 0.0033(18) -0.003(2) -0.005(2) C5 0.029(2) 0.018(2) 0.044(3) 0.003(2) 0.012(2) 0.0022(18) C6 0.048(3) 0.016(2) 0.028(2) -0.0054(18) 0.007(2) -0.006(2) C7 0.031(2) 0.023(2) 0.035(3) 0.0010(19) -0.004(2) -0.0051(19) C8 0.031(2) 0.020(2) 0.030(2) -0.0017(18) 0.015(2) -0.0028(18) C10 0.018(2) 0.018(2) 0.024(2) -0.0035(16) 0.0059(17) 0.0016(16) C11 0.019(2) 0.025(2) 0.032(2) -0.0034(19) 0.0020(18) 0.0016(18) C12 0.019(2) 0.038(3) 0.040(3) -0.005(2) 0.000(2) -0.002(2) C13 0.027(2) 0.031(3) 0.047(3) -0.006(2) 0.014(2) -0.007(2) C14 0.031(2) 0.029(2) 0.026(2) -0.0006(19) 0.012(2) -0.002(2) C15 0.022(2) 0.022(2) 0.026(2) -0.0076(18) 0.0076(18) 0.0016(17) C20 0.0168(19) 0.0158(19) 0.022(2) 0.0013(16) 0.0039(16) -0.0018(15) C21 0.021(2) 0.022(2) 0.025(2) 0.0039(17) -0.0010(17) 0.0000(17) C22 0.035(3) 0.034(3) 0.024(2) 0.008(2) 0.006(2) 0.004(2) C23 0.022(2) 0.045(3) 0.033(3) 0.006(2) 0.011(2) 0.004(2) C24 0.019(2) 0.040(3) 0.032(3) 0.006(2) -0.0026(19) 0.005(2) C25 0.019(2) 0.028(2) 0.023(2) 0.0029(18) -0.0003(17) -0.0002(17) C30 0.018(2) 0.019(2) 0.022(2) 0.0010(16) -0.0019(16) -0.0017(16) C31 0.030(2) 0.019(2) 0.029(2) -0.0023(18) -0.0033(19) 0.0023(18) C32 0.029(2) 0.018(2) 0.034(3) 0.0000(18) -0.003(2) 0.0008(18) C33 0.034(3) 0.049(4) 0.075(5) -0.008(3) 0.004(3) -0.013(3) C34 0.057(4) 0.021(3) 0.068(4) 0.012(3) -0.015(3) -0.016(2) C35 0.042(3) 0.019(2) 0.072(4) -0.013(3) -0.022(3) 0.006(2) C36 0.041(3) 0.032(3) 0.054(3) -0.018(2) -0.014(3) 0.001(2) C37 0.034(3) 0.027(3) 0.060(4) -0.009(2) -0.021(3) -0.003(2) C40 0.023(2) 0.017(2) 0.024(2) 0.0023(17) -0.0017(17) 0.0027(16) C41 0.031(2) 0.025(2) 0.026(2) 0.0039(18) -0.0021(19) 0.0034(19) C42 0.034(3) 0.042(3) 0.027(3) 0.001(2) 0.005(2) 0.005(2) C43 0.039(3) 0.038(3) 0.024(2) -0.005(2) -0.006(2) 0.001(2) C44 0.026(2) 0.029(2) 0.034(3) -0.002(2) -0.006(2) -0.0017(19) C45 0.027(2) 0.020(2) 0.028(2) 0.0018(18) -0.0042(19) 0.0018(18) C50 0.024(2) 0.017(2) 0.029(2) 0.0010(17) -0.0075(18) 0.0004(17) C51 0.028(2) 0.022(2) 0.031(2) 0.0025(19) -0.0064(19) -0.0033(18) C52 0.027(2) 0.031(3) 0.045(3) 0.001(2) -0.009(2) 0.001(2) C53 0.042(3) 0.027(2) 0.035(3) 0.005(2) -0.015(2) -0.001(2) C54 0.045(3) 0.037(3) 0.024(2) 0.006(2) -0.006(2) 0.000(2) C55 0.034(3) 0.031(3) 0.024(2) 0.0008(19) -0.003(2) -0.001(2) C111 0.026(2) 0.038(3) 0.033(3) 0.002(2) -0.007(2) -0.003(2) C112 0.097(5) 0.043(4) 0.039(3) -0.005(3) -0.020(3) 0.010(3) C113 0.144(8) 0.035(3) 0.046(4) 0.004(3) -0.009(4) 0.017(4) C151 0.031(2) 0.031(2) 0.020(2) -0.0016(18) 0.0044(18) -0.0024(19) C152 0.046(4) 0.148(8) 0.043(4) -0.044(4) -0.001(3) -0.002(4) C153 0.045(3) 0.059(4) 0.063(4) -0.014(3) -0.024(3) 0.007(3) C211 0.026(2) 0.038(3) 0.023(2) 0.005(2) -0.0013(19) 0.008(2) C212 0.058(4) 0.045(3) 0.055(4) -0.008(3) -0.028(3) 0.018(3) C213 0.045(3) 0.043(3) 0.057(4) 0.016(3) -0.011(3) 0.010(3) C251 0.027(2) 0.048(3) 0.021(2) 0.005(2) -0.0018(19) 0.006(2) C252 0.064(4) 0.038(3) 0.034(3) 0.011(2) -0.005(3) -0.006(3) C253 0.087(5) 0.034(3) 0.041(3) -0.003(3) -0.026(3) 0.006(3) C411 0.024(2) 0.052(3) 0.029(3) 0.005(2) 0.002(2) 0.004(2) C412 0.031(3) 0.067(5) 0.145(8) -0.019(5) 0.022(4) 0.011(3) C413 0.034(3) 0.055(4) 0.117(7) 0.000(4) 0.002(4) -0.010(3) C451 0.023(2) 0.045(3) 0.029(3) -0.004(2) -0.0037(19) 0.002(2) C452 0.045(4) 0.079(5) 0.066(5) -0.009(4) 0.023(3) -0.012(3) C453 0.085(6) 0.074(5) 0.076(5) 0.000(4) 0.027(4) 0.048(4) C511 0.024(2) 0.043(3) 0.040(3) 0.008(2) -0.003(2) -0.007(2) C512 0.040(4) 0.100(6) 0.062(4) 0.018(4) 0.022(3) 0.007(4) C513 0.072(5) 0.063(4) 0.068(5) 0.026(4) -0.019(4) -0.043(4) C551 0.030(3) 0.081(4) 0.027(3) 0.013(3) 0.001(2) 0.003(3) C552 0.055(4) 0.090(6) 0.061(4) 0.021(4) 0.019(3) 0.032(4) C553 0.048(4) 0.095(6) 0.121(8) -0.001(6) 0.017(5) -0.033(4) N1 0.0204(17) 0.0153(17) 0.0213(18) -0.0001(14) 0.0050(14) -0.0001(14) N2 0.0196(17) 0.0154(17) 0.0208(18) -0.0001(14) 0.0015(14) -0.0004(14) N3 0.0210(18) 0.0167(17) 0.0238(19) 0.0026(14) -0.0036(15) 0.0014(14) N4 0.0227(18) 0.0152(17) 0.0224(18) 0.0016(14) -0.0014(15) 0.0001(14) Ni1 0.0288(3) 0.0154(3) 0.0261(3) -0.0027(2) 0.0101(2) -0.0030(2) Ni2 0.0287(3) 0.0150(3) 0.0378(4) -0.0009(2) -0.0125(3) -0.0001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.373(5) . ? C1 N2 1.366(5) . ? C1 Ni1 1.849(4) . ? C2 C3 1.333(6) . ? C2 N1 1.387(5) . ? C3 N2 1.396(5) . ? C4 C5 1.398(7) . ? C4 C8 1.407(7) . ? C4 Ni1 2.156(5) . ? C5 C6 1.406(7) . ? C5 Ni1 2.102(5) . ? C6 C7 1.402(7) . ? C6 Ni1 2.068(4) . ? C7 C8 1.398(7) . ? C7 Ni1 2.160(5) . ? C8 Ni1 2.165(4) . ? C10 C11 1.401(6) . ? C10 C15 1.391(6) . ? C10 N1 1.442(5) . ? C11 C12 1.395(6) . ? C11 C111 1.525(7) . ? C12 C13 1.373(7) . ? C13 C14 1.374(7) . ? C14 C15 1.392(6) . ? C15 C151 1.521(6) . ? C20 C21 1.393(6) . ? C20 C25 1.396(6) . ? C20 N2 1.438(5) . ? C21 C22 1.394(6) . ? C21 C211 1.520(6) . ? C22 C23 1.378(7) . ? C23 C24 1.384(7) . ? C24 C25 1.397(6) . ? C25 C251 1.513(6) . ? C30 N3 1.362(5) . ? C30 N4 1.366(5) . ? C30 Ni2 1.838(4) . ? C31 C32 1.333(6) . ? C31 N4 1.387(5) . ? C32 N3 1.391(6) . ? C33 C34 1.407(9) . ? C33 C37 1.411(9) . ? C33 Ni2 2.125(6) . ? C34 C35 1.410(9) . ? C34 Ni2 2.121(5) . ? C35 C36 1.406(8) . ? C35 Ni2 2.070(5) . ? C36 C37 1.386(8) . ? C36 Ni2 2.148(5) . ? C37 Ni2 2.146(5) . ? C40 C41 1.409(6) . ? C40 C45 1.384(6) . ? C40 N3 1.444(5) . ? C41 C42 1.389(7) . ? C41 C411 1.513(7) . ? C42 C43 1.380(7) . ? C43 C44 1.379(7) . ? C44 C45 1.392(6) . ? C45 C451 1.519(7) . ? C50 C51 1.388(6) . ? C50 C55 1.390(7) . ? C50 N4 1.447(5) . ? C51 C52 1.401(7) . ? C51 C511 1.512(7) . ? C52 C53 1.374(7) . ? C53 C54 1.373(7) . ? C54 C55 1.400(7) . ? C55 C551 1.506(7) . ? C111 C112 1.518(7) . ? C111 C113 1.521(8) . ? C151 C152 1.505(7) . ? C151 C153 1.514(7) . ? C211 C212 1.517(7) . ? C211 C213 1.523(7) . ? C251 C252 1.518(7) . ? C251 C253 1.530(8) . ? C411 C412 1.517(8) . ? C411 C413 1.512(8) . ? C451 C452 1.523(8) . ? C451 C453 1.514(8) . ? C511 C512 1.520(8) . ? C511 C513 1.536(8) . ? C551 C552 1.528(9) . ? C551 C553 1.542(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 129.3(3) . . ? N2 C1 N1 102.8(3) . . ? N2 C1 Ni1 127.8(3) . . ? C3 C2 N1 107.1(4) . . ? C2 C3 N2 106.7(4) . . ? C5 C4 C8 108.4(4) . . ? C5 C4 Ni1 68.7(3) . . ? C8 C4 Ni1 71.3(3) . . ? C4 C5 C6 107.5(4) . . ? C4 C5 Ni1 73.0(3) . . ? C6 C5 Ni1 69.0(3) . . ? C5 C6 Ni1 71.6(3) . . ? C7 C6 C5 108.3(4) . . ? C7 C6 Ni1 74.3(3) . . ? C6 C7 Ni1 67.1(3) . . ? C8 C7 C6 107.8(4) . . ? C8 C7 Ni1 71.3(3) . . ? C4 C8 Ni1 70.7(3) . . ? C7 C8 C4 107.8(4) . . ? C7 C8 Ni1 71.0(3) . . ? C11 C10 N1 117.6(4) . . ? C15 C10 C11 123.3(4) . . ? C15 C10 N1 119.1(4) . . ? C10 C11 C111 121.7(4) . . ? C12 C11 C10 116.6(4) . . ? C12 C11 C111 121.6(4) . . ? C13 C12 C11 121.1(5) . . ? C12 C13 C14 120.8(4) . . ? C13 C14 C15 120.9(4) . . ? C10 C15 C14 117.1(4) . . ? C10 C15 C151 121.6(4) . . ? C14 C15 C151 121.4(4) . . ? C21 C20 C25 123.3(4) . . ? C21 C20 N2 118.5(4) . . ? C25 C20 N2 118.2(4) . . ? C20 C21 C22 117.4(4) . . ? C20 C21 C211 122.4(4) . . ? C22 C21 C211 120.2(4) . . ? C23 C22 C21 121.2(4) . . ? C22 C23 C24 119.9(4) . . ? C23 C24 C25 121.6(4) . . ? C20 C25 C24 116.7(4) . . ? C20 C25 C251 123.1(4) . . ? C24 C25 C251 120.2(4) . . ? N3 C30 N4 103.3(3) . . ? N3 C30 Ni2 128.8(3) . . ? N4 C30 Ni2 127.9(3) . . ? C32 C31 N4 106.9(4) . . ? C31 C32 N3 106.8(4) . . ? C34 C33 C37 108.5(6) . . ? C34 C33 Ni2 70.5(3) . . ? C37 C33 Ni2 71.5(3) . . ? C33 C34 C35 106.7(6) . . ? C33 C34 Ni2 70.8(3) . . ? C35 C34 Ni2 68.4(3) . . ? C34 C35 Ni2 72.3(3) . . ? C36 C35 C34 108.4(5) . . ? C36 C35 Ni2 73.5(3) . . ? C35 C36 Ni2 67.6(3) . . ? C37 C36 C35 108.2(6) . . ? C37 C36 Ni2 71.1(3) . . ? C33 C37 Ni2 69.9(3) . . ? C36 C37 C33 107.9(5) . . ? C36 C37 Ni2 71.2(3) . . ? C41 C40 N3 117.8(4) . . ? C45 C40 C41 123.4(4) . . ? C45 C40 N3 118.8(4) . . ? C40 C41 C411 122.3(4) . . ? C42 C41 C40 116.4(4) . . ? C42 C41 C411 121.4(4) . . ? C43 C42 C41 121.5(5) . . ? C44 C43 C42 120.3(5) . . ? C43 C44 C45 120.8(4) . . ? C40 C45 C44 117.5(4) . . ? C40 C45 C451 123.0(4) . . ? C44 C45 C451 119.5(4) . . ? C51 C50 C55 123.7(4) . . ? C51 C50 N4 117.3(4) . . ? C55 C50 N4 119.0(4) . . ? C50 C51 C52 117.1(4) . . ? C50 C51 C511 122.5(4) . . ? C52 C51 C511 120.4(4) . . ? C53 C52 C51 120.8(5) . . ? C54 C53 C52 120.4(5) . . ? C53 C54 C55 121.5(5) . . ? C50 C55 C54 116.5(5) . . ? C50 C55 C551 122.9(4) . . ? C54 C55 C551 120.6(4) . . ? C112 C111 C11 113.0(4) . . ? C112 C111 C113 109.3(5) . . ? C113 C111 C11 108.8(4) . . ? C152 C151 C15 111.9(4) . . ? C152 C151 C153 110.9(5) . . ? C153 C151 C15 112.5(4) . . ? C21 C211 C213 110.7(4) . . ? C212 C211 C21 111.9(4) . . ? C212 C211 C213 110.8(5) . . ? C25 C251 C252 112.0(4) . . ? C25 C251 C253 109.9(4) . . ? C252 C251 C253 110.6(4) . . ? C41 C411 C412 113.3(5) . . ? C413 C411 C41 110.1(4) . . ? C413 C411 C412 110.2(5) . . ? C45 C451 C452 112.0(4) . . ? C453 C451 C45 110.7(5) . . ? C453 C451 C452 110.6(5) . . ? C51 C511 C512 112.6(5) . . ? C51 C511 C513 109.2(5) . . ? C512 C511 C513 111.3(5) . . ? C55 C551 C552 110.0(5) . . ? C55 C551 C553 110.8(5) . . ? C552 C551 C553 111.0(6) . . ? C1 N1 C2 111.7(3) . . ? C1 N1 C10 123.2(3) . . ? C2 N1 C10 125.1(3) . . ? C1 N2 C3 111.7(3) . . ? C1 N2 C20 124.9(3) . . ? C3 N2 C20 123.4(3) . . ? C30 N3 C32 111.5(4) . . ? C30 N3 C40 123.3(3) . . ? C32 N3 C40 125.2(4) . . ? C30 N4 C31 111.4(4) . . ? C30 N4 C50 124.7(4) . . ? C31 N4 C50 123.2(4) . . ? C1 Ni1 C4 122.82(18) . . ? C1 Ni1 C5 151.03(19) . . ? C1 Ni1 C6 169.52(19) . . ? C1 Ni1 C7 135.22(18) . . ? C1 Ni1 C8 115.92(17) . . ? C4 Ni1 C7 63.36(18) . . ? C4 Ni1 C8 38.00(18) . . ? C5 Ni1 C4 38.30(18) . . ? C5 Ni1 C7 64.55(19) . . ? C5 Ni1 C8 64.41(17) . . ? C6 Ni1 C4 64.67(19) . . ? C6 Ni1 C5 39.4(2) . . ? C6 Ni1 C7 38.64(19) . . ? C6 Ni1 C8 64.59(18) . . ? C7 Ni1 C8 37.73(18) . . ? C30 Ni2 C33 116.4(2) . . ? C30 Ni2 C34 142.9(2) . . ? C30 Ni2 C35 177.8(2) . . ? C30 Ni2 C36 139.9(2) . . ? C30 Ni2 C37 115.25(19) . . ? C33 Ni2 C36 63.9(2) . . ? C33 Ni2 C37 38.6(2) . . ? C34 Ni2 C33 38.7(2) . . ? C34 Ni2 C36 64.7(3) . . ? C34 Ni2 C37 64.8(2) . . ? C35 Ni2 C33 65.2(2) . . ? C35 Ni2 C34 39.3(2) . . ? C35 Ni2 C36 38.9(2) . . ? C35 Ni2 C37 64.9(2) . . ? C37 Ni2 C36 37.7(2) . . ? _database_code_depnum_ccdc_archive 'CCDC 995939' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_date 2014-03-18 _audit_creation_method ; Olex2 1.2 (compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781) ; _shelxl_version_number 2013-4 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H29 N2 Ni' _chemical_formula_sum 'C26 H29 N2 Ni' _chemical_formula_weight 428.22 _chemical_melting_point ? _chemical_oxdiff_formula 'C26 H41 N2 Ni' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P 2ac 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 22.89090(10) _cell_length_b 11.10740(10) _cell_length_c 9.03710(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2297.76(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 31289 _cell_measurement_temperature 123.1(4) _cell_measurement_theta_max 66.9240 _cell_measurement_theta_min 5.2430 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.299 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 908 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_unetI/netI 0.0112 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 49162 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 67.034 _diffrn_reflns_theta_min 3.862 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 123.1(4) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1773 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1169996000 _diffrn_orient_matrix_UB_12 0.0926894000 _diffrn_orient_matrix_UB_13 0.0192892000 _diffrn_orient_matrix_UB_21 0.0591175000 _diffrn_orient_matrix_UB_22 0.0897542000 _diffrn_orient_matrix_UB_23 -0.0456906000 _diffrn_orient_matrix_UB_31 -0.1088984000 _diffrn_orient_matrix_UB_32 -0.0509322000 _diffrn_orient_matrix_UB_33 -0.0455121000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2072 _reflns_number_total 2165 _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)' _computing_data_collection 'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'SIR97 (Burla et al., 2007)' _refine_diff_density_max 0.212 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.095 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 167 _refine_ls_number_reflns 2165 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0298 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.0664P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.0798 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Others Fixed U12: C1(0) C2(0) C3(0) C6(0) C7(0) C10(0) C12(0) C13(0) C16(0) C18(0) N1(0) N2(0) Ni1(0) Fixed U23: C1(0) C2(0) C3(0) C6(0) C7(0) C10(0) C12(0) C13(0) C16(0) C18(0) N1(0) N2(0) Ni1(0) Fixed Uiso: H2(0.028) H3(0.029) H4(0.038) H5(0.033) H6(0.03) H9(0.031) H11A(0.05) H11B(0.05) H11C(0.05) H15(0.026) H17A(0.045) H17B(0.045) H17C(0.045) Fixed X: H2(0.3765) H3(0.2763) H4(0.4627) H5(0.3591) H6(0.2957) H9(0.5741) H11A(0.435) H11B(0.4877) H11C(0.4379) H15(0.1751) H17A(0.307) H17B(0.2455) H17C(0.2662) Fixed Y: C1(0.25) C2(0.25) H2(0.25) C3(0.25) H3(0.25) H4(0.1366) H5(0.4325) C6(0.25) H6(0.25) C7(0.25) H9(0.43) C10(0.25) H11A(0.4757) H11B(0.5421) H11C(0.4867) C12(0.25) C13(0.25) H15(0.0698) C16(0.25) H17A(0.0187) H17B(- 0.0428) H17C(0.0175) C18(0.25) N1(0.25) N2(0.25) Ni1(0.25) H18B(0.25) H12A(0.25) Fixed Z: H2(0.872) H3(0.777) H4(0.1096) H5(0.1336) H6(0.1551) H9(0.7046) H11A(0.5838) H11B(0.6588) H11C(0.7566) H15(0.3061) H17A(0.4436) H17B(0.435) H17C(0.5828) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.37127(8) 0.2500 0.5207(2) 0.0175(4) Uani 1 2 d S T P . . C2 C 0.36524(9) 0.2500 0.7731(2) 0.0236(4) Uani 1 2 d S T P . . H2 H 0.3765 0.2500 0.8720 0.028 Uiso 1 2 calc R U P . . C3 C 0.31039(8) 0.2500 0.7211(2) 0.0238(4) Uani 1 2 d S T P . . H3 H 0.2763 0.2500 0.7770 0.029 Uiso 1 2 calc R U P . . C4 C 0.42999(6) 0.18593(15) 0.11759(15) 0.0315(3) Uani 1 1 d . . . . . H4 H 0.4627 0.1366 0.1096 0.038 Uiso 1 1 calc R U . . . C5 C 0.37173(7) 0.35293(13) 0.13180(15) 0.0275(3) Uani 1 1 d . . . . . H5 H 0.3591 0.4325 0.1336 0.033 Uiso 1 1 calc R U . . . C6 C 0.33601(9) 0.2500 0.1427(2) 0.0248(4) Uani 1 2 d S T P . . H6 H 0.2957 0.2500 0.1551 0.030 Uiso 1 2 calc R U P . . C7 C 0.46467(8) 0.2500 0.66424(19) 0.0182(4) Uani 1 2 d S T P . . C8 C 0.49348(6) 0.35971(12) 0.67573(14) 0.0224(3) Uani 1 1 d . . . . . C9 C 0.55382(6) 0.35763(13) 0.69796(16) 0.0259(3) Uani 1 1 d . . . . . H9 H 0.5741 0.4300 0.7046 0.031 Uiso 1 1 calc R U . . . C10 C 0.58418(9) 0.2500 0.7103(2) 0.0252(4) Uani 1 2 d S T P . . C11 C 0.46054(7) 0.47662(14) 0.66805(19) 0.0336(4) Uani 1 1 d . . . . . H11A H 0.4350 0.4757 0.5838 0.050 Uiso 1 1 calc R U . . . H11B H 0.4877 0.5421 0.6588 0.050 Uiso 1 1 calc R U . . . H11C H 0.4379 0.4867 0.7566 0.050 Uiso 1 1 calc R U . . . C12 C 0.64940(9) 0.2500 0.7370(3) 0.0369(6) Uani 1 2 d DS T P . . C13 C 0.26418(7) 0.2500 0.47191(19) 0.0172(4) Uani 1 2 d S T P . . C14 C 0.24064(5) 0.14017(11) 0.42831(14) 0.0193(3) Uani 1 1 d . . . . . C15 C 0.19176(6) 0.14224(12) 0.33601(14) 0.0214(3) Uani 1 1 d . . . . . H15 H 0.1751 0.0698 0.3061 0.026 Uiso 1 1 calc R U . . . C16 C 0.16731(8) 0.2500 0.2876(2) 0.0222(4) Uani 1 2 d S T P . . C17 C 0.26723(6) 0.02275(13) 0.47683(17) 0.0298(3) Uani 1 1 d . . . . . H17A H 0.3070 0.0187 0.4436 0.045 Uiso 1 1 calc R U . . . H17B H 0.2455 -0.0428 0.4350 0.045 Uiso 1 1 calc R U . . . H17C H 0.2662 0.0175 0.5828 0.045 Uiso 1 1 calc R U . . . C18 C 0.11544(11) 0.2500 0.1846(3) 0.0335(5) Uani 1 2 d S T P . . N1 N 0.40185(6) 0.2500 0.65116(17) 0.0183(3) Uani 1 2 d S T P . . N2 N 0.31437(6) 0.2500 0.56773(16) 0.0179(3) Uani 1 2 d S T P . . Ni1 Ni 0.39915(2) 0.2500 0.32554(3) 0.02147(13) Uani 1 2 d S T P . . H18A H 0.1154(8) 0.1775(18) 0.124(2) 0.045(5) Uiso 1 1 d . . . . . H18B H 0.0812(14) 0.2500 0.241(4) 0.052(8) Uiso 1 2 d S . P . . H12B H 0.6629(12) 0.1776(19) 0.786(2) 0.096(9) Uiso 1 1 d D . . . . H12A H 0.6690(17) 0.2500 0.639(2) 0.096(13) Uiso 1 2 d DS . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0152(8) 0.0207(9) 0.0167(9) 0.000 -0.0023(7) 0.000 C2 0.0210(9) 0.0380(11) 0.0118(8) 0.000 0.0003(7) 0.000 C3 0.0200(9) 0.0360(11) 0.0154(9) 0.000 0.0036(7) 0.000 C4 0.0274(7) 0.0523(9) 0.0147(6) -0.0043(6) -0.0012(5) 0.0143(7) C5 0.0391(8) 0.0274(7) 0.0160(6) 0.0000(6) -0.0052(6) 0.0020(6) C6 0.0194(9) 0.0425(12) 0.0124(8) 0.000 -0.0018(7) 0.000 C7 0.0147(9) 0.0272(10) 0.0127(8) 0.000 -0.0023(7) 0.000 C8 0.0203(7) 0.0246(7) 0.0224(7) -0.0023(5) -0.0026(5) 0.0010(5) C9 0.0206(7) 0.0259(7) 0.0313(7) -0.0033(6) -0.0047(6) -0.0040(6) C10 0.0167(9) 0.0323(10) 0.0264(10) 0.000 -0.0052(8) 0.000 C11 0.0260(7) 0.0247(8) 0.0501(10) -0.0050(7) -0.0050(6) 0.0031(6) C12 0.0177(10) 0.0395(13) 0.0536(15) 0.000 -0.0113(10) 0.000 C13 0.0115(8) 0.0263(9) 0.0139(8) 0.000 0.0001(7) 0.000 C14 0.0168(6) 0.0217(7) 0.0194(6) 0.0009(5) 0.0014(5) 0.0012(5) C15 0.0189(6) 0.0216(7) 0.0237(7) -0.0029(5) -0.0021(5) -0.0024(5) C16 0.0168(9) 0.0259(9) 0.0239(9) 0.000 -0.0026(8) 0.000 C17 0.0281(7) 0.0230(7) 0.0383(8) 0.0031(6) -0.0070(6) 0.0024(6) C18 0.0289(12) 0.0292(12) 0.0424(14) 0.000 -0.0176(10) 0.000 N1 0.0147(8) 0.0269(8) 0.0131(7) 0.000 -0.0012(6) 0.000 N2 0.0140(7) 0.0258(8) 0.0138(7) 0.000 -0.0017(6) 0.000 Ni1 0.01615(19) 0.0361(2) 0.01212(19) 0.000 -0.00017(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.371(2) . ? C1 N2 1.370(2) . ? C1 Ni1 1.8760(18) . ? C2 C3 1.341(3) . ? C2 N1 1.385(2) . ? C3 N2 1.389(2) . ? C4 C4 1.423(3) 8_565 ? C4 C5 1.408(2) 8_565 ? C4 Ni1 2.1299(14) . ? C5 C4 1.408(2) 8_565 ? C5 C6 1.4092(19) . ? C5 Ni1 2.1833(14) . ? C6 C5 1.4092(19) 8_565 ? C6 Ni1 2.1952(19) . ? C7 C8 1.3895(16) . ? C7 C8 1.3895(16) 8_565 ? C7 N1 1.443(2) . ? C8 C9 1.3960(19) . ? C8 C11 1.5033(19) . ? C9 C10 1.3872(17) . ? C10 C9 1.3872(17) 8_565 ? C10 C12 1.512(3) . ? C13 C14 1.3906(15) . ? C13 C14 1.3906(15) 8_565 ? C13 N2 1.439(2) . ? C14 C15 1.3959(18) . ? C14 C17 1.5046(18) . ? C15 C16 1.3918(16) . ? C16 C15 1.3918(17) 8_565 ? C16 C18 1.509(3) . ? Ni1 C4 2.1299(14) 8_565 ? Ni1 C5 2.1833(14) 8_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 129.41(13) . . ? N2 C1 N1 102.64(15) . . ? N2 C1 Ni1 127.95(13) . . ? C3 C2 N1 106.71(16) . . ? C2 C3 N2 106.76(16) . . ? C4 C4 Ni1 70.48(5) 8_565 . ? C5 C4 C4 107.86(9) 8_565 8_565 ? C5 C4 Ni1 73.02(8) 8_565 . ? C4 C5 C6 107.90(13) 8_565 . ? C4 C5 Ni1 68.91(8) 8_565 . ? C6 C5 Ni1 71.69(9) . . ? C5 C6 C5 108.46(17) . 8_565 ? C5 C6 Ni1 70.77(9) 8_565 . ? C5 C6 Ni1 70.77(9) . . ? C8 C7 C8 122.56(17) 8_565 . ? C8 C7 N1 118.63(8) . . ? C8 C7 N1 118.63(8) 8_565 . ? C7 C8 C9 117.77(13) . . ? C7 C8 C11 121.06(12) . . ? C9 C8 C11 121.16(12) . . ? C10 C9 C8 121.43(13) . . ? C9 C10 C9 119.03(17) 8_565 . ? C9 C10 C12 120.48(9) . . ? C9 C10 C12 120.48(9) 8_565 . ? C14 C13 C14 122.64(16) 8_565 . ? C14 C13 N2 118.68(8) 8_565 . ? C14 C13 N2 118.68(8) . . ? C13 C14 C15 117.74(12) . . ? C13 C14 C17 121.41(12) . . ? C15 C14 C17 120.84(12) . . ? C16 C15 C14 121.62(13) . . ? C15 C16 C15 118.64(17) 8_565 . ? C15 C16 C18 120.68(9) . . ? C15 C16 C18 120.68(9) 8_565 . ? C1 N1 C2 112.06(15) . . ? C1 N1 C7 125.40(15) . . ? C2 N1 C7 122.54(15) . . ? C1 N2 C3 111.82(15) . . ? C1 N2 C13 124.94(15) . . ? C3 N2 C13 123.24(15) . . ? C1 Ni1 C4 160.47(5) . 8_565 ? C1 Ni1 C4 160.47(5) . . ? C1 Ni1 C5 131.02(6) . . ? C1 Ni1 C5 131.02(6) . 8_565 ? C1 Ni1 C6 118.93(7) . . ? C4 Ni1 C4 39.04(9) . 8_565 ? C4 Ni1 C5 38.07(6) 8_565 . ? C4 Ni1 C5 64.07(6) . . ? C4 Ni1 C5 64.07(6) 8_565 8_565 ? C4 Ni1 C5 38.07(6) . 8_565 ? C4 Ni1 C6 63.52(6) 8_565 . ? C4 Ni1 C6 63.52(6) . . ? C5 Ni1 C5 63.16(8) 8_565 . ? C5 Ni1 C6 37.55(5) . . ? C5 Ni1 C6 37.55(5) 8_565 . ? _shelx_res_file ; TITL oPnma in Pnma CELL 1.54178 22.8909 11.1074 9.0371 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0001 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, 1/2 - Z SYMM - X, 1/2 + Y, - Z SFAC C H N NI UNIT 104 116 8 4 MERG 2 DFIX 1.568 0.01 H12A H12B SADI C12 H12A C12 H12B FMAP 2 PLAN 25 ACTA L.S. 20 WGHT 0.040100 1.066400 FVAR 0.12611 C1 1 0.371271 0.250000 0.520743 10.50000 0.01522 0.02067 = 0.01673 0.00000 -0.00226 0.00000 C2 1 0.365242 0.250000 0.773138 10.50000 0.02104 0.03796 = 0.01179 0.00000 0.00030 0.00000 AFIX 43 H2 2 0.376521 0.250000 0.872002 10.50000 -1.20000 AFIX 0 C3 1 0.310387 0.250000 0.721121 10.50000 0.01995 0.03601 = 0.01545 0.00000 0.00357 0.00000 AFIX 43 H3 2 0.276258 0.250000 0.776952 10.50000 -1.20000 AFIX 0 C4 1 0.429992 0.185932 0.117594 11.00000 0.02744 0.05227 = 0.01468 -0.00432 -0.00120 0.01429 AFIX 43 H4 2 0.462680 0.136635 0.109625 11.00000 -1.20000 AFIX 0 C5 1 0.371734 0.352934 0.131795 11.00000 0.03914 0.02740 = 0.01597 0.00001 -0.00517 0.00196 AFIX 43 H5 2 0.359063 0.432471 0.133643 11.00000 -1.20000 AFIX 0 C6 1 0.336008 0.250000 0.142721 10.50000 0.01945 0.04246 = 0.01243 0.00000 -0.00179 0.00000 AFIX 43 H6 2 0.295673 0.250000 0.155055 10.50000 -1.20000 AFIX 0 C7 1 0.464672 0.250000 0.664237 10.50000 0.01466 0.02721 = 0.01272 0.00000 -0.00234 0.00000 C8 1 0.493484 0.359712 0.675733 11.00000 0.02030 0.02457 = 0.02240 -0.00231 -0.00264 0.00103 C9 1 0.553825 0.357630 0.697956 11.00000 0.02055 0.02591 = 0.03131 -0.00334 -0.00474 -0.00405 AFIX 43 H9 2 0.574113 0.429966 0.704647 11.00000 -1.20000 AFIX 0 C10 1 0.584181 0.250000 0.710276 10.50000 0.01675 0.03230 = 0.02645 0.00000 -0.00519 0.00000 C11 1 0.460536 0.476619 0.668051 11.00000 0.02603 0.02466 = 0.05014 -0.00502 -0.00502 0.00313 AFIX 137 H11A 2 0.434981 0.475719 0.583830 11.00000 -1.50000 H11B 2 0.487684 0.542064 0.658805 11.00000 -1.50000 H11C 2 0.437902 0.486731 0.756613 11.00000 -1.50000 AFIX 0 C12 1 0.649398 0.250000 0.736983 10.50000 0.01769 0.03953 = 0.05360 0.00000 -0.01126 0.00000 C13 1 0.264178 0.250000 0.471913 10.50000 0.01148 0.02635 = 0.01388 0.00000 0.00014 0.00000 C14 1 0.240644 0.140169 0.428311 11.00000 0.01682 0.02174 = 0.01942 0.00092 0.00140 0.00117 C15 1 0.191761 0.142236 0.336008 11.00000 0.01885 0.02158 = 0.02372 -0.00289 -0.00212 -0.00236 AFIX 43 H15 2 0.175122 0.069830 0.306107 11.00000 -1.20000 AFIX 0 C16 1 0.167311 0.250000 0.287623 10.50000 0.01679 0.02589 = 0.02388 0.00000 -0.00257 0.00000 C17 1 0.267234 0.022745 0.476831 11.00000 0.02812 0.02300 = 0.03830 0.00309 -0.00702 0.00240 AFIX 137 H17A 2 0.307018 0.018681 0.443597 11.00000 -1.50000 H17B 2 0.245477 -0.042849 0.435026 11.00000 -1.50000 H17C 2 0.266172 0.017482 0.582829 11.00000 -1.50000 AFIX 0 C18 1 0.115445 0.250000 0.184604 10.50000 0.02886 0.02920 = 0.04243 0.00000 -0.01757 0.00000 N1 3 0.401845 0.250000 0.651160 10.50000 0.01475 0.02694 = 0.01308 0.00000 -0.00118 0.00000 N2 3 0.314371 0.250000 0.567734 10.50000 0.01402 0.02575 = 0.01385 0.00000 -0.00165 0.00000 NI1 4 0.399153 0.250000 0.325541 10.50000 0.01615 0.03614 = 0.01212 0.00000 -0.00017 0.00000 H18A 2 0.115399 0.177494 0.123583 11.00000 0.04474 H18B 2 0.081228 0.250000 0.241189 10.50000 0.05162 H12B 2 0.662894 0.177552 0.786084 11.00000 0.09643 H12A 2 0.668976 0.250000 0.639333 10.50000 0.09601 HKLF 4 REM oPnma in Pnma REM R1 = 0.0298 for 2072 Fo > 4sig(Fo) and 0.0309 for all 2165 data REM 167 parameters refined using 2 restraints END WGHT 0.0401 1.0663 REM Highest difference peak 0.212, deepest hole -0.423, 1-sigma level 0.095 Q1 1 0.2182 0.1381 0.3974 11.00000 0.05 0.21 Q2 1 0.3095 0.0207 0.5370 11.00000 0.05 0.21 Q3 1 0.6693 0.1658 0.7060 11.00000 0.05 0.21 Q4 1 0.2502 0.0850 0.4556 11.00000 0.05 0.20 Q5 1 0.4789 0.4160 0.6771 11.00000 0.05 0.20 Q6 1 0.4173 0.4804 0.6241 11.00000 0.05 0.19 Q7 1 0.4501 0.4871 0.5153 11.00000 0.05 0.19 Q8 1 0.1795 0.0245 0.2995 11.00000 0.05 0.18 Q9 1 0.2394 -0.0475 0.5078 11.00000 0.05 0.18 Q10 1 0.4095 0.4764 0.9595 11.00000 0.05 0.18 Q11 1 0.3900 0.5047 -0.0530 11.00000 0.05 0.18 Q12 1 0.1584 0.0435 0.3798 11.00000 0.05 0.17 Q13 1 0.5780 0.4729 0.6588 11.00000 0.05 0.17 Q14 1 0.3812 0.5182 -0.0007 11.00000 0.05 0.17 Q15 1 0.3800 0.4775 0.1094 11.00000 0.05 0.17 Q16 1 0.3388 0.5184 0.0160 11.00000 0.05 0.16 Q17 1 0.3123 -0.0234 0.3737 11.00000 0.05 0.16 Q18 1 0.1497 0.0297 0.1356 11.00000 0.05 0.16 Q19 1 0.3717 0.0240 0.3675 11.00000 0.05 0.16 Q20 1 0.5220 0.3601 0.6726 11.00000 0.05 0.16 Q21 1 0.2366 0.0049 0.6197 11.00000 0.05 0.16 Q22 1 0.2713 -0.0417 0.3764 11.00000 0.05 0.15 Q23 1 0.3209 0.0248 0.6748 11.00000 0.05 0.15 Q24 1 0.3604 -0.0454 0.4239 11.00000 0.05 0.15 Q25 1 0.4146 0.5572 -0.0072 11.00000 0.05 0.15 ; _shelx_res_checksum 93627 _olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)' _database_code_depnum_ccdc_archive 'CCDC 995940' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_date 2014-03-28 _audit_creation_method ; Olex2 1.2 (compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781) ; _shelxl_version_number 2013-4 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H51 N2 Ni' _chemical_formula_sum 'C37 H51 N2 Ni' _chemical_formula_weight 582.50 _chemical_melting_point ? _chemical_oxdiff_formula 'C37 H51 N2 Ni' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.23970(10) _cell_length_b 18.6957(2) _cell_length_c 21.5074(2) _cell_angle_alpha 90 _cell_angle_beta 93.7790(10) _cell_angle_gamma 90 _cell_volume 3707.17(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11315 _cell_measurement_temperature 123.1(2) _cell_measurement_theta_max 66.9840 _cell_measurement_theta_min 4.7340 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1260 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_unetI/netI 0.0270 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19260 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 67.006 _diffrn_reflns_theta_min 4.120 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 123.1(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1773 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1557828000 _diffrn_orient_matrix_UB_12 0.0256590000 _diffrn_orient_matrix_UB_13 0.0087068000 _diffrn_orient_matrix_UB_21 -0.0600185000 _diffrn_orient_matrix_UB_22 -0.0706028000 _diffrn_orient_matrix_UB_23 -0.0282376000 _diffrn_orient_matrix_UB_31 0.0069263000 _diffrn_orient_matrix_UB_32 -0.0339176000 _diffrn_orient_matrix_UB_33 0.0654056000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5815 _reflns_number_total 6556 _reflns_odcompleteness_completeness 99.05 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'SIR97 (Burla et al., 2007)' _refine_diff_density_max 0.567 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.054 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 410 _refine_ls_number_reflns 6556 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0384 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.9398P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.1121 _refine_special_details ; A disordered iso-propyl moiety was refined over split positions. A badly disordered toluene solvate molecule could not be refined successfully. The electron density was removed with SQUEEZE implemented in PLATON (78 electrons in a total solvent accessible void of 506.5 Ang^3). ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.013 0.000 0.000 251 39 ' ' 2 -0.053 0.500 0.500 251 39 ' ' _platon_squeeze_details ; ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C23-C25 \\sim C23-C24 \\sim C23A-C24A \\sim C23A-C25A with sigma of 0.02 3. Others Fixed Sof: C23(0.67) H23(0.67) C24(0.67) H24A(0.67) H24B(0.67) H24C(0.67) C25(0.67) H25A(0.67) H25B(0.67) H25C(0.67) C23A(0.33) H23A(0.33) C24A(0.33) H24D(0.33) H24E(0.33) H24F(0.33) C25A(0.33) H25D(0.33) H25E(0.33) H25F(0.33) 4.a Ternary CH refined with riding coordinates: C23(H23), C23A(H23A) 4.b Ternary CH refined with riding coordinates and stretchable bonds: C20(H20), C32(H32), C35(H35) 4.c Me refined with riding coordinates: C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C24A(H24D,H24E,H24F), C25A(H25D, H25E,H25F) 4.d Aromatic/amide H refined with riding coordinates and stretchable bonds: C2(H2), C3(H3), C16(H16), C17(H17), C18(H18), C28(H28), C29(H29), C30(H30) 4.e Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B, H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C33(H33A, H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.38449(11) 0.17228(6) 0.65430(5) 0.0188(2) Uani 1 1 d . . . . . C2 C 0.63320(11) 0.17411(6) 0.66421(5) 0.0261(3) Uani 1 1 d . . . . . H2 H 0.7305(15) 0.18084(12) 0.6820(3) 0.031 Uiso 1 1 calc GR . . . . C3 C 0.59371(11) 0.15172(7) 0.60635(5) 0.0281(3) Uani 1 1 d . . . . . H3 H 0.6516(10) 0.1404(2) 0.5776(5) 0.034 Uiso 1 1 calc GR . . . . C4 C 0.00964(11) 0.17031(7) 0.72951(5) 0.0247(2) Uani 1 1 d . . . . . C5 C 0.02354(11) 0.24565(6) 0.72017(5) 0.0250(2) Uani 1 1 d . . . . . C6 C 0.00897(11) 0.25971(6) 0.65517(5) 0.0253(2) Uani 1 1 d . . . . . C7 C -0.00930(11) 0.19269(6) 0.62397(5) 0.0247(3) Uani 1 1 d . . . . . C8 C -0.01151(11) 0.13734(6) 0.66993(5) 0.0241(2) Uani 1 1 d . . . . . C9 C 0.00626(14) 0.13441(8) 0.79189(6) 0.0388(3) Uani 1 1 d . . . . . H9A H -0.0845 0.1444 0.8094 0.058 Uiso 1 1 calc GR . . . . H9B H 0.0844 0.1522 0.8192 0.058 Uiso 1 1 calc GR . . . . H9C H 0.0167 0.0837 0.7869 0.058 Uiso 1 1 calc GR . . . . C10 C 0.04215(14) 0.29974(7) 0.77196(6) 0.0367(3) Uani 1 1 d . . . . . H10A H 0.0559 0.3464 0.7546 0.055 Uiso 1 1 calc GR . . . . H10B H 0.1253 0.2874 0.7990 0.055 Uiso 1 1 calc GR . . . . H10C H -0.0428 0.3000 0.7954 0.055 Uiso 1 1 calc GR . . . . C11 C 0.00053(15) 0.33178(8) 0.62453(7) 0.0399(3) Uani 1 1 d . . . . . H11A H -0.0993 0.3445 0.6154 0.060 Uiso 1 1 calc GR . . . . H11B H 0.0495 0.3302 0.5865 0.060 Uiso 1 1 calc GR . . . . H11C H 0.0460 0.3668 0.6520 0.060 Uiso 1 1 calc GR . . . . C12 C -0.03250(13) 0.18344(8) 0.55473(5) 0.0354(3) Uani 1 1 d . . . . . H12A H -0.1279 0.1998 0.5412 0.053 Uiso 1 1 calc GR . . . . H12B H -0.0230 0.1338 0.5443 0.053 Uiso 1 1 calc GR . . . . H12C H 0.0385 0.2108 0.5344 0.053 Uiso 1 1 calc GR . . . . C13 C -0.04220(13) 0.05975(7) 0.65767(7) 0.0378(3) Uani 1 1 d . . . . . H13A H 0.0108 0.0313 0.6885 0.057 Uiso 1 1 calc GR . . . . H13B H -0.0129 0.0473 0.6171 0.057 Uiso 1 1 calc GR . . . . H13C H -0.1442 0.0510 0.6596 0.057 Uiso 1 1 calc GR . . . . C14 C 0.49369(11) 0.20966(6) 0.75601(5) 0.0213(2) Uani 1 1 d . . . . . C15 C 0.48994(12) 0.28273(7) 0.76699(5) 0.0277(3) Uani 1 1 d . . . . . C16 C 0.46958(15) 0.30462(8) 0.82779(6) 0.0425(3) Uani 1 1 d . . . . . H16 H 0.46691(16) 0.3557(10) 0.83739(19) 0.051 Uiso 1 1 calc GR . . . . C17 C 0.45327(16) 0.25579(10) 0.87426(6) 0.0506(4) Uani 1 1 d . . . . . H17 H 0.4364(4) 0.2720(3) 0.9154(8) 0.061 Uiso 1 1 calc GR . . . . C18 C 0.46090(16) 0.18401(10) 0.86239(6) 0.0475(4) Uani 1 1 d . . . . . H18 H 0.4524(2) 0.1549(7) 0.8916(6) 0.057 Uiso 1 1 calc GR . . . . C19 C 0.48252(13) 0.15822(7) 0.80272(6) 0.0325(3) Uani 1 1 d . . . . . C20 C 0.50950(14) 0.33715(7) 0.71588(7) 0.0366(3) Uani 1 1 d . . . . . H20 H 0.51068(14) 0.3121(4) 0.6777(7) 0.044 Uiso 1 1 calc GR . . . . C21 C 0.38447(19) 0.39037(10) 0.71024(11) 0.0690(5) Uani 1 1 d . . . . . H21A H 0.2950 0.3651 0.7014 0.103 Uiso 1 1 calc GR . . . . H21B H 0.3995 0.4234 0.6771 0.103 Uiso 1 1 calc GR . . . . H21C H 0.3801 0.4161 0.7487 0.103 Uiso 1 1 calc GR . . . . C22 C 0.65357(18) 0.37575(12) 0.72655(10) 0.0712(6) Uani 1 1 d . . . . . H22A H 0.6551 0.4017 0.7651 0.107 Uiso 1 1 calc GR . . . . H22B H 0.6656 0.4085 0.6929 0.107 Uiso 1 1 calc GR . . . . H22C H 0.7311 0.3415 0.7283 0.107 Uiso 1 1 calc GR . . . . C26 C 0.36008(11) 0.12979(6) 0.54450(5) 0.0213(2) Uani 1 1 d . . . . . C27 C 0.34897(12) 0.17930(6) 0.49582(5) 0.0252(3) Uani 1 1 d . . . . . C28 C 0.27145(12) 0.15874(7) 0.44068(5) 0.0282(3) Uani 1 1 d . . . . . H28 H 0.26264(18) 0.1914(5) 0.4059(5) 0.034 Uiso 1 1 calc GR . . . . C29 C 0.20735(13) 0.09199(7) 0.43564(5) 0.0298(3) Uani 1 1 d . . . . . H29 H 0.1516(8) 0.0782(2) 0.3961(6) 0.036 Uiso 1 1 calc GR . . . . C30 C 0.21946(12) 0.04408(6) 0.48473(5) 0.0275(3) Uani 1 1 d . . . . . H30 H 0.1697(7) -0.0055(7) 0.47999(8) 0.033 Uiso 1 1 calc GR . . . . C31 C 0.29735(11) 0.06126(6) 0.54048(5) 0.0223(2) Uani 1 1 d . . . . . C32 C 0.41747(14) 0.25321(7) 0.50104(6) 0.0332(3) Uani 1 1 d . . . . . H32 H 0.4551(6) 0.25942(12) 0.5417(7) 0.040 Uiso 1 1 calc GR . . . . C33 C 0.3071(2) 0.31222(9) 0.48618(15) 0.0881(8) Uani 1 1 d . . . . . H33A H 0.2657 0.3063 0.4444 0.132 Uiso 1 1 calc GR . . . . H33B H 0.3543 0.3579 0.4900 0.132 Uiso 1 1 calc GR . . . . H33C H 0.2319 0.3097 0.5148 0.132 Uiso 1 1 calc GR . . . . C34 C 0.54148(19) 0.25998(10) 0.45808(8) 0.0582(4) Uani 1 1 d . . . . . H34A H 0.6123 0.2235 0.4681 0.087 Uiso 1 1 calc GR . . . . H34B H 0.5859 0.3062 0.4635 0.087 Uiso 1 1 calc GR . . . . H34C H 0.5044 0.2546 0.4156 0.087 Uiso 1 1 calc GR . . . . C35 C 0.31486(12) 0.00784(6) 0.59391(5) 0.0267(3) Uani 1 1 d . . . . . H35 H 0.2888(4) 0.0324(3) 0.6326(5) 0.032 Uiso 1 1 calc GR . . . . C36 C 0.47110(14) -0.01888(8) 0.60418(6) 0.0380(3) Uani 1 1 d . . . . . H36A H 0.4993 -0.0421 0.5671 0.057 Uiso 1 1 calc GR . . . . H36B H 0.4776 -0.0522 0.6382 0.057 Uiso 1 1 calc GR . . . . H36C H 0.5344 0.0209 0.6137 0.057 Uiso 1 1 calc GR . . . . C37 C 0.21833(14) -0.05804(7) 0.58484(7) 0.0378(3) Uani 1 1 d . . . . . H37A H 0.1194 -0.0433 0.5767 0.057 Uiso 1 1 calc GR . . . . H37B H 0.2264 -0.0868 0.6219 0.057 Uiso 1 1 calc GR . . . . H37C H 0.2484 -0.0855 0.5502 0.057 Uiso 1 1 calc GR . . . . N1 N 0.50545(9) 0.18560(5) 0.69320(4) 0.0205(2) Uani 1 1 d . . . . . N2 N 0.44255(9) 0.14993(5) 0.60093(4) 0.0215(2) Uani 1 1 d . . . . . Ni1 Ni 0.19583(2) 0.19037(2) 0.67821(2) 0.02139(5) Uani 1 1 d . . . . . C23 C 0.5053(2) 0.07874(11) 0.79132(11) 0.0372(5) Uani 0.67 1 d . . P A 1 H23 H 0.5483 0.0742 0.7511 0.045 Uiso 0.67 1 calc R . P A 1 C24 C 0.3580(2) 0.04021(12) 0.78548(12) 0.0464(6) Uani 0.67 1 d . . P A 1 H24A H 0.3731 -0.0099 0.7784 0.070 Uiso 0.67 1 calc R . P A 1 H24B H 0.2995 0.0599 0.7511 0.070 Uiso 0.67 1 calc R . P A 1 H24C H 0.3096 0.0465 0.8232 0.070 Uiso 0.67 1 calc R . P A 1 C25 C 0.6086(3) 0.04328(15) 0.83979(16) 0.0725(8) Uani 0.67 1 d . . P A 1 H25A H 0.6178 -0.0065 0.8300 0.109 Uiso 0.67 1 calc R . P A 1 H25B H 0.5713 0.0482 0.8802 0.109 Uiso 0.67 1 calc R . P A 1 H25C H 0.7020 0.0658 0.8398 0.109 Uiso 0.67 1 calc R . P A 1 C23A C 0.4707(4) 0.0788(3) 0.7845(2) 0.0483(13) Uani 0.33 1 d . . P A 2 H23A H 0.4338 0.0741 0.7409 0.058 Uiso 0.33 1 calc R . P A 2 C24A C 0.3767(6) 0.0350(3) 0.8270(4) 0.086(2) Uani 0.33 1 d . . P A 2 H24D H 0.2773 0.0497 0.8205 0.129 Uiso 0.33 1 calc R . P A 2 H24E H 0.4095 0.0428 0.8698 0.129 Uiso 0.33 1 calc R . P A 2 H24F H 0.3847 -0.0149 0.8173 0.129 Uiso 0.33 1 calc R . P A 2 C25A C 0.6257(5) 0.0500(3) 0.7929(3) 0.0624(15) Uani 0.33 1 d . . P A 2 H25D H 0.6855 0.0740 0.7646 0.094 Uiso 0.33 1 calc R . P A 2 H25E H 0.6255 -0.0004 0.7845 0.094 Uiso 0.33 1 calc R . P A 2 H25F H 0.6635 0.0583 0.8349 0.094 Uiso 0.33 1 calc R . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0175(4) 0.0178(5) 0.0211(4) -0.0016(4) 0.0000(4) -0.0001(4) C2 0.0140(5) 0.0325(6) 0.0320(5) -0.0064(5) 0.0025(4) 0.0000(4) C3 0.0150(5) 0.0377(6) 0.0322(5) -0.0094(5) 0.0065(4) -0.0006(4) C4 0.0148(4) 0.0332(6) 0.0264(5) -0.0012(5) 0.0031(4) 0.0021(4) C5 0.0163(4) 0.0329(6) 0.0261(5) -0.0068(4) 0.0029(4) 0.0033(4) C6 0.0170(5) 0.0292(5) 0.0297(5) -0.0016(5) 0.0018(4) 0.0054(4) C7 0.0133(4) 0.0369(6) 0.0237(5) -0.0048(4) -0.0002(4) 0.0032(4) C8 0.0126(4) 0.0299(6) 0.0299(5) -0.0055(4) 0.0017(4) 0.0006(4) C9 0.0321(6) 0.0540(8) 0.0310(6) 0.0070(6) 0.0079(5) 0.0011(6) C10 0.0319(6) 0.0420(7) 0.0362(6) -0.0160(5) 0.0039(5) 0.0040(5) C11 0.0361(6) 0.0376(7) 0.0464(7) 0.0076(6) 0.0042(6) 0.0087(6) C12 0.0252(6) 0.0568(8) 0.0238(5) -0.0067(5) -0.0020(4) 0.0015(5) C13 0.0246(6) 0.0338(6) 0.0546(7) -0.0092(6) -0.0001(5) -0.0026(5) C14 0.0150(4) 0.0272(5) 0.0212(4) -0.0044(4) -0.0022(4) -0.0001(4) C15 0.0216(5) 0.0292(6) 0.0319(5) -0.0091(5) -0.0015(4) -0.0003(4) C16 0.0368(7) 0.0506(8) 0.0398(6) -0.0254(6) 0.0006(5) -0.0009(6) C17 0.0418(7) 0.0841(11) 0.0257(6) -0.0201(6) -0.0001(5) -0.0025(7) C18 0.0396(7) 0.0766(11) 0.0259(6) 0.0108(6) -0.0001(5) -0.0040(7) C19 0.0270(5) 0.0382(6) 0.0320(6) 0.0059(5) -0.0010(5) -0.0016(5) C20 0.0363(6) 0.0229(6) 0.0508(7) -0.0013(5) 0.0034(5) 0.0005(5) C21 0.0461(8) 0.0490(9) 0.1126(14) 0.0286(9) 0.0108(9) 0.0114(7) C22 0.0415(8) 0.0778(12) 0.0944(12) 0.0241(10) 0.0043(8) -0.0177(8) C26 0.0168(4) 0.0272(5) 0.0202(4) -0.0060(4) 0.0033(4) 0.0002(4) C27 0.0217(5) 0.0276(5) 0.0268(5) -0.0044(4) 0.0059(4) 0.0008(4) C28 0.0282(5) 0.0321(6) 0.0244(5) 0.0003(5) 0.0027(4) 0.0049(5) C29 0.0281(5) 0.0343(6) 0.0264(5) -0.0084(5) -0.0032(4) 0.0028(5) C30 0.0244(5) 0.0277(5) 0.0303(5) -0.0085(5) 0.0009(4) -0.0002(4) C31 0.0179(4) 0.0247(5) 0.0247(5) -0.0047(4) 0.0044(4) 0.0010(4) C32 0.0364(6) 0.0288(6) 0.0347(6) -0.0023(5) 0.0050(5) -0.0068(5) C33 0.0550(10) 0.0304(8) 0.179(2) -0.0108(11) 0.0088(13) -0.0009(7) C34 0.0621(9) 0.0508(9) 0.0643(9) 0.0000(7) 0.0232(7) -0.0209(7) C35 0.0276(5) 0.0265(5) 0.0267(5) -0.0027(4) 0.0055(4) -0.0009(5) C36 0.0327(6) 0.0362(7) 0.0449(7) 0.0086(6) 0.0010(5) 0.0043(5) C37 0.0371(6) 0.0298(6) 0.0469(7) 0.0011(5) 0.0074(5) -0.0043(5) N1 0.0152(4) 0.0239(4) 0.0223(4) -0.0059(3) 0.0000(3) -0.0003(3) N2 0.0146(4) 0.0267(4) 0.0234(4) -0.0067(4) 0.0025(3) -0.0014(3) Ni1 0.01371(8) 0.02830(10) 0.02221(9) -0.00491(7) 0.00155(7) 0.00174(7) C23 0.0310(9) 0.0296(9) 0.0509(11) 0.0125(9) 0.0025(8) -0.0001(8) C24 0.0388(10) 0.0356(10) 0.0636(13) 0.0093(10) -0.0058(10) -0.0019(9) C25 0.0370(11) 0.0535(14) 0.124(2) 0.0364(14) -0.0185(13) 0.0001(11) C23A 0.0261(19) 0.044(2) 0.071(3) 0.027(2) -0.0227(18) 0.0010(17) C24A 0.058(3) 0.054(3) 0.148(5) 0.043(3) 0.022(3) -0.008(3) C25A 0.042(2) 0.055(3) 0.090(4) 0.005(3) 0.002(3) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3741(13) . ? C1 N2 1.3642(13) . ? C1 Ni1 1.8803(10) . ? C2 C3 1.3404(16) . ? C2 N1 1.3875(14) . ? C3 N2 1.3943(13) . ? C4 C5 1.4298(17) . ? C4 C8 1.4239(15) . ? C4 C9 1.5022(17) . ? C4 Ni1 2.1373(11) . ? C5 C6 1.4201(15) . ? C5 C10 1.5059(17) . ? C5 Ni1 2.1463(11) . ? C6 C7 1.4260(16) . ? C6 C11 1.4996(18) . ? C6 Ni1 2.1895(11) . ? C7 C8 1.4321(16) . ? C7 C12 1.5005(16) . ? C7 Ni1 2.1595(10) . ? C8 C13 1.4981(18) . ? C8 Ni1 2.1540(10) . ? C14 C15 1.3872(17) . ? C14 C19 1.3995(17) . ? C14 N1 1.4346(13) . ? C15 C16 1.3948(18) . ? C15 C20 1.5172(18) . ? C16 C17 1.369(2) . ? C17 C18 1.369(3) . ? C18 C19 1.3978(19) . ? C19 C23 1.523(3) . ? C19 C23A 1.538(5) . ? C20 C21 1.523(2) . ? C20 C22 1.518(2) . ? C26 C27 1.3960(16) . ? C26 C31 1.4065(15) . ? C26 N2 1.4400(13) . ? C27 C28 1.3984(16) . ? C27 C32 1.5209(17) . ? C28 C29 1.3826(18) . ? C29 C30 1.3835(17) . ? C30 C31 1.3946(15) . ? C31 C35 1.5231(16) . ? C32 C33 1.522(2) . ? C32 C34 1.524(2) . ? C35 C36 1.5298(17) . ? C35 C37 1.5255(17) . ? C23 C24 1.537(3) . ? C23 C25 1.519(3) . ? C23A C24A 1.539(7) . ? C23A C25A 1.530(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 122.17(7) . . ? N2 C1 N1 102.63(8) . . ? N2 C1 Ni1 135.09(7) . . ? C3 C2 N1 106.14(9) . . ? C2 C3 N2 107.16(9) . . ? C5 C4 C9 124.97(11) . . ? C5 C4 Ni1 70.84(6) . . ? C8 C4 C5 107.95(10) . . ? C8 C4 C9 126.91(11) . . ? C8 C4 Ni1 71.26(6) . . ? C9 C4 Ni1 127.18(8) . . ? C4 C5 C10 124.36(10) . . ? C4 C5 Ni1 70.16(6) . . ? C6 C5 C4 108.49(10) . . ? C6 C5 C10 127.06(11) . . ? C6 C5 Ni1 72.54(6) . . ? C10 C5 Ni1 125.64(8) . . ? C5 C6 C7 107.53(10) . . ? C5 C6 C11 126.70(11) . . ? C5 C6 Ni1 69.24(6) . . ? C7 C6 C11 125.56(11) . . ? C7 C6 Ni1 69.72(6) . . ? C11 C6 Ni1 130.45(8) . . ? C6 C7 C8 108.47(9) . . ? C6 C7 C12 124.96(11) . . ? C6 C7 Ni1 72.00(6) . . ? C8 C7 C12 126.45(11) . . ? C8 C7 Ni1 70.40(6) . . ? C12 C7 Ni1 126.63(8) . . ? C4 C8 C7 107.52(10) . . ? C4 C8 C13 126.21(11) . . ? C4 C8 Ni1 69.99(6) . . ? C7 C8 C13 126.11(10) . . ? C7 C8 Ni1 70.82(6) . . ? C13 C8 Ni1 128.11(8) . . ? C15 C14 C19 123.42(10) . . ? C15 C14 N1 118.25(10) . . ? C19 C14 N1 118.30(10) . . ? C14 C15 C16 117.06(11) . . ? C14 C15 C20 122.11(10) . . ? C16 C15 C20 120.82(12) . . ? C17 C16 C15 121.12(14) . . ? C18 C17 C16 120.54(13) . . ? C17 C18 C19 121.45(14) . . ? C14 C19 C23 122.52(13) . . ? C14 C19 C23A 119.2(2) . . ? C18 C19 C14 116.34(13) . . ? C18 C19 C23 120.94(14) . . ? C18 C19 C23A 123.7(2) . . ? C15 C20 C21 111.70(12) . . ? C15 C20 C22 110.75(12) . . ? C22 C20 C21 110.75(13) . . ? C27 C26 C31 123.25(9) . . ? C27 C26 N2 117.86(10) . . ? C31 C26 N2 118.88(9) . . ? C26 C27 C28 117.52(10) . . ? C26 C27 C32 122.51(10) . . ? C28 C27 C32 119.98(10) . . ? C29 C28 C27 120.49(11) . . ? C28 C29 C30 120.79(10) . . ? C29 C30 C31 121.21(11) . . ? C26 C31 C35 121.88(9) . . ? C30 C31 C26 116.73(10) . . ? C30 C31 C35 121.38(10) . . ? C27 C32 C33 111.93(12) . . ? C27 C32 C34 110.89(11) . . ? C33 C32 C34 109.42(15) . . ? C31 C35 C36 112.04(9) . . ? C31 C35 C37 113.63(10) . . ? C37 C35 C36 107.04(10) . . ? C1 N1 C2 112.34(9) . . ? C1 N1 C14 121.41(8) . . ? C2 N1 C14 126.24(9) . . ? C1 N2 C3 111.69(8) . . ? C1 N2 C26 125.01(8) . . ? C3 N2 C26 123.25(9) . . ? C1 Ni1 C4 154.41(5) . . ? C1 Ni1 C5 158.17(4) . . ? C1 Ni1 C6 140.90(4) . . ? C1 Ni1 C7 130.72(4) . . ? C1 Ni1 C8 136.90(4) . . ? C4 Ni1 C5 39.00(4) . . ? C4 Ni1 C6 64.61(4) . . ? C4 Ni1 C7 64.83(4) . . ? C4 Ni1 C8 38.75(4) . . ? C5 Ni1 C6 38.22(4) . . ? C5 Ni1 C7 64.44(4) . . ? C5 Ni1 C8 64.92(4) . . ? C7 Ni1 C6 38.27(4) . . ? C8 Ni1 C6 64.53(4) . . ? C8 Ni1 C7 38.78(4) . . ? C19 C23 C24 109.85(16) . . ? C25 C23 C19 113.74(19) . . ? C25 C23 C24 111.36(19) . . ? C19 C23A C24A 113.3(4) . . ? C25A C23A C19 105.1(3) . . ? C25A C23A C24A 107.6(4) . . ? _shelx_res_file ; TITL mP21n in P2(1)/n CELL 1.54178 9.2397 18.6957 21.5074 90.000 93.779 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N NI UNIT 148 204 8 4 MERG 2 SADI C23 C25 C23 C24 C23A C24A C23A C25A FMAP 2 PLAN 25 ACTA L.S. 20 DAMP 1000.00 15.00 WGHT 0.065200 0.939800 FVAR 1.25356 C1 1 0.384489 0.172277 0.654297 11.00000 0.01748 0.01778 = 0.02106 -0.00158 -0.00003 -0.00012 C2 1 0.633201 0.174107 0.664210 11.00000 0.01396 0.03246 = 0.03199 -0.00643 0.00248 0.00000 AFIX 44 H2 2 0.730470 0.180844 0.682030 11.00000 -1.20000 AFIX 0 C3 1 0.593711 0.151723 0.606354 11.00000 0.01499 0.03770 = 0.03222 -0.00936 0.00646 -0.00065 AFIX 44 H3 2 0.651619 0.140420 0.577551 11.00000 -1.20000 AFIX 0 C4 1 0.009640 0.170311 0.729515 11.00000 0.01479 0.03323 = 0.02639 -0.00123 0.00311 0.00210 C5 1 0.023536 0.245654 0.720166 11.00000 0.01629 0.03289 = 0.02611 -0.00677 0.00287 0.00327 C6 1 0.008973 0.259709 0.655169 11.00000 0.01703 0.02916 = 0.02966 -0.00165 0.00180 0.00545 C7 1 -0.009303 0.192694 0.623973 11.00000 0.01335 0.03689 = 0.02370 -0.00482 -0.00021 0.00316 C8 1 -0.011514 0.137343 0.669930 11.00000 0.01264 0.02992 = 0.02986 -0.00547 0.00170 0.00060 C9 1 0.006263 0.134405 0.791886 11.00000 0.03214 0.05402 = 0.03095 0.00699 0.00791 0.00109 AFIX 137 H9A 2 -0.084493 0.144410 0.809395 11.00000 -1.50000 H9B 2 0.084402 0.152180 0.819231 11.00000 -1.50000 H9C 2 0.016721 0.083680 0.786890 11.00000 -1.50000 AFIX 0 C10 1 0.042153 0.299742 0.771959 11.00000 0.03192 0.04204 = 0.03623 -0.01603 0.00394 0.00401 AFIX 137 H10A 2 0.055865 0.346363 0.754585 11.00000 -1.50000 H10B 2 0.125272 0.287368 0.798952 11.00000 -1.50000 H10C 2 -0.042810 0.299977 0.795357 11.00000 -1.50000 AFIX 0 C11 1 0.000531 0.331776 0.624528 11.00000 0.03611 0.03756 = 0.04635 0.00758 0.00421 0.00874 AFIX 137 H11A 2 -0.099288 0.344457 0.615386 11.00000 -1.50000 H11B 2 0.049491 0.330241 0.586543 11.00000 -1.50000 H11C 2 0.045985 0.366763 0.652039 11.00000 -1.50000 AFIX 0 C12 1 -0.032498 0.183440 0.554734 11.00000 0.02517 0.05683 = 0.02382 -0.00669 -0.00204 0.00152 AFIX 137 H12A 2 -0.127886 0.199794 0.541158 11.00000 -1.50000 H12B 2 -0.022989 0.133800 0.544338 11.00000 -1.50000 H12C 2 0.038543 0.210806 0.534405 11.00000 -1.50000 AFIX 0 C13 1 -0.042200 0.059753 0.657668 11.00000 0.02464 0.03375 = 0.05457 -0.00916 -0.00010 -0.00265 AFIX 137 H13A 2 0.010828 0.031269 0.688539 11.00000 -1.50000 H13B 2 -0.012913 0.047314 0.617051 11.00000 -1.50000 H13C 2 -0.144180 0.050956 0.659557 11.00000 -1.50000 AFIX 0 C14 1 0.493687 0.209662 0.756008 11.00000 0.01499 0.02720 = 0.02116 -0.00438 -0.00219 -0.00012 C15 1 0.489941 0.282732 0.766986 11.00000 0.02160 0.02925 = 0.03188 -0.00907 -0.00150 -0.00026 C16 1 0.469577 0.304617 0.827794 11.00000 0.03683 0.05056 = 0.03978 -0.02544 0.00055 -0.00087 AFIX 44 H16 2 0.466907 0.355659 0.837393 11.00000 -1.20000 AFIX 0 C17 1 0.453267 0.255790 0.874256 11.00000 0.04176 0.08410 = 0.02574 -0.02007 -0.00006 -0.00248 AFIX 44 H17 2 0.436385 0.271988 0.915379 11.00000 -1.20000 AFIX 0 C18 1 0.460899 0.184015 0.862395 11.00000 0.03962 0.07659 = 0.02589 0.01077 -0.00008 -0.00398 AFIX 44 H18 2 0.452416 0.154877 0.891568 11.00000 -1.20000 AFIX 0 C19 1 0.482524 0.158216 0.802717 11.00000 0.02701 0.03819 = 0.03204 0.00594 -0.00098 -0.00158 C20 1 0.509496 0.337150 0.715883 11.00000 0.03627 0.02287 = 0.05076 -0.00132 0.00337 0.00048 AFIX 14 H20 2 0.510682 0.312107 0.677671 11.00000 -1.20000 AFIX 0 C21 1 0.384465 0.390370 0.710244 11.00000 0.04607 0.04900 = 0.11255 0.02862 0.01076 0.01139 AFIX 137 H21A 2 0.294998 0.365131 0.701375 11.00000 -1.50000 H21B 2 0.399478 0.423401 0.677106 11.00000 -1.50000 H21C 2 0.380132 0.416114 0.748697 11.00000 -1.50000 AFIX 0 C22 1 0.653568 0.375748 0.726548 11.00000 0.04154 0.07779 = 0.09440 0.02406 0.00434 -0.01765 AFIX 137 H22A 2 0.655117 0.401655 0.765124 11.00000 -1.50000 H22B 2 0.665587 0.408522 0.692914 11.00000 -1.50000 H22C 2 0.731098 0.341474 0.728347 11.00000 -1.50000 AFIX 0 C26 1 0.360080 0.129790 0.544496 11.00000 0.01679 0.02723 = 0.02018 -0.00603 0.00334 0.00018 C27 1 0.348971 0.179299 0.495825 11.00000 0.02168 0.02764 = 0.02677 -0.00440 0.00589 0.00083 C28 1 0.271453 0.158742 0.440677 11.00000 0.02821 0.03209 = 0.02440 0.00027 0.00273 0.00493 AFIX 44 H28 2 0.262644 0.191371 0.405896 11.00000 -1.20000 AFIX 0 C29 1 0.207346 0.091992 0.435644 11.00000 0.02805 0.03434 = 0.02635 -0.00845 -0.00322 0.00280 AFIX 44 H29 2 0.151587 0.078186 0.396071 11.00000 -1.20000 AFIX 0 C30 1 0.219461 0.044080 0.484733 11.00000 0.02437 0.02772 = 0.03030 -0.00846 0.00088 -0.00020 AFIX 44 H30 2 0.169699 -0.005526 0.479990 11.00000 -1.20000 AFIX 0 C31 1 0.297353 0.061260 0.540478 11.00000 0.01788 0.02475 = 0.02467 -0.00472 0.00439 0.00103 C32 1 0.417466 0.253212 0.501043 11.00000 0.03642 0.02877 = 0.03468 -0.00229 0.00501 -0.00681 AFIX 14 H32 2 0.455078 0.259424 0.541723 11.00000 -1.20000 AFIX 0 C33 1 0.307148 0.312219 0.486177 11.00000 0.05497 0.03039 = 0.17898 -0.01079 0.00883 -0.00093 AFIX 137 H33A 2 0.265655 0.306267 0.444392 11.00000 -1.50000 H33B 2 0.354310 0.357912 0.489951 11.00000 -1.50000 H33C 2 0.231876 0.309705 0.514810 11.00000 -1.50000 AFIX 0 C34 1 0.541476 0.259980 0.458084 11.00000 0.06210 0.05075 = 0.06428 -0.00003 0.02316 -0.02090 AFIX 137 H34A 2 0.612263 0.223467 0.468098 11.00000 -1.50000 H34B 2 0.585857 0.306183 0.463504 11.00000 -1.50000 H34C 2 0.504432 0.254554 0.415587 11.00000 -1.50000 AFIX 0 C35 1 0.314857 0.007835 0.593911 11.00000 0.02758 0.02648 = 0.02666 -0.00274 0.00549 -0.00088 AFIX 14 H35 2 0.288775 0.032442 0.632611 11.00000 -1.20000 AFIX 0 C36 1 0.471102 -0.018880 0.604182 11.00000 0.03271 0.03622 = 0.04494 0.00863 0.00105 0.00427 AFIX 137 H36A 2 0.499350 -0.042113 0.567063 11.00000 -1.50000 H36B 2 0.477637 -0.052210 0.638206 11.00000 -1.50000 H36C 2 0.534366 0.020918 0.613722 11.00000 -1.50000 AFIX 0 C37 1 0.218331 -0.058036 0.584839 11.00000 0.03714 0.02982 = 0.04695 0.00106 0.00736 -0.00432 AFIX 137 H37A 2 0.119366 -0.043293 0.576712 11.00000 -1.50000 H37B 2 0.226444 -0.086816 0.621871 11.00000 -1.50000 H37C 2 0.248441 -0.085452 0.550226 11.00000 -1.50000 AFIX 0 N1 3 0.505454 0.185599 0.693205 11.00000 0.01521 0.02394 = 0.02234 -0.00585 0.00004 -0.00026 N2 3 0.442550 0.149928 0.600929 11.00000 0.01460 0.02666 = 0.02336 -0.00671 0.00250 -0.00138 NI1 4 0.195830 0.190369 0.678205 11.00000 0.01371 0.02830 = 0.02221 -0.00491 0.00155 0.00174 PART 1 C23 1 0.505280 0.078736 0.791319 10.67000 0.03099 0.02955 = 0.05093 0.01253 0.00251 -0.00007 AFIX 13 H23 2 0.548300 0.074177 0.751059 10.67000 -1.20000 AFIX 0 C24 1 0.358048 0.040210 0.785485 10.67000 0.03878 0.03562 = 0.06356 0.00929 -0.00584 -0.00195 AFIX 33 H24A 2 0.373087 -0.009866 0.778429 10.67000 -1.50000 H24B 2 0.299517 0.059949 0.751141 10.67000 -1.50000 H24C 2 0.309584 0.046485 0.823241 10.67000 -1.50000 AFIX 0 C25 1 0.608579 0.043276 0.839794 10.67000 0.03702 0.05345 = 0.12391 0.03642 -0.01852 0.00013 AFIX 33 H25A 2 0.617753 -0.006545 0.829987 10.67000 -1.50000 H25B 2 0.571323 0.048162 0.880203 10.67000 -1.50000 H25C 2 0.701960 0.065795 0.839834 10.67000 -1.50000 AFIX 0 PART 2 C23A 1 0.470716 0.078811 0.784470 10.33000 0.02613 0.04380 = 0.07144 0.02722 -0.02267 0.00105 AFIX 13 H23A 2 0.433767 0.074072 0.740899 10.33000 -1.20000 AFIX 0 C24A 1 0.376730 0.034972 0.827010 10.33000 0.05841 0.05391 = 0.14759 0.04281 0.02174 -0.00823 AFIX 33 H24D 2 0.277331 0.049681 0.820545 10.33000 -1.50000 H24E 2 0.409501 0.042810 0.869754 10.33000 -1.50000 H24F 2 0.384719 -0.014925 0.817271 10.33000 -1.50000 AFIX 0 C25A 1 0.625726 0.049979 0.792887 10.33000 0.04195 0.05531 = 0.08982 0.00512 0.00234 0.00851 AFIX 33 H25D 2 0.685477 0.073972 0.764557 10.33000 -1.50000 H25E 2 0.625501 -0.000449 0.784468 10.33000 -1.50000 H25F 2 0.663470 0.058322 0.834919 10.33000 -1.50000 AFIX 0 HKLF 4 REM mP21n in P2(1)/n REM R1 = 0.0384 for 5815 Fo > 4sig(Fo) and 0.0427 for all 6556 data REM 410 parameters refined using 6 restraints END WGHT 0.0652 0.9405 REM Highest difference peak 0.567, deepest hole -0.427, 1-sigma level 0.054 Q1 1 0.3144 0.3013 0.5327 11.00000 0.05 0.57 Q2 1 0.4573 0.2824 0.4372 11.00000 0.05 0.44 Q3 1 0.3163 0.0953 0.5455 11.00000 0.05 0.27 Q4 1 0.4503 0.5141 0.5571 11.00000 0.05 0.24 Q5 1 0.4485 0.5028 0.4438 11.00000 0.05 0.23 Q6 1 0.3121 0.1754 0.6638 11.00000 0.05 0.23 Q7 1 0.1962 0.2302 0.6445 11.00000 0.05 0.22 Q8 1 0.3730 0.5224 0.5029 11.00000 0.05 0.22 Q9 1 0.4976 0.3120 0.7393 11.00000 0.05 0.21 Q10 1 0.3116 0.0361 0.5641 11.00000 0.05 0.21 Q11 1 0.3248 0.1616 0.4647 11.00000 0.05 0.21 Q12 1 0.4768 0.2978 0.7991 11.00000 0.05 0.19 Q13 1 0.5733 0.1824 0.6817 11.00000 0.05 0.19 Q14 1 0.2550 0.1242 0.4350 11.00000 0.05 0.18 Q15 1 0.3933 0.1382 0.5723 11.00000 0.05 0.18 Q16 1 0.1978 0.3157 0.4966 11.00000 0.05 0.18 Q17 1 0.3084 0.1802 0.4853 11.00000 0.05 0.18 Q18 1 0.3803 0.1425 0.5189 11.00000 0.05 0.17 Q19 1 0.3788 0.2167 0.4997 11.00000 0.05 0.17 Q20 1 -0.0127 0.1860 0.5929 11.00000 0.05 0.17 Q21 1 0.5171 0.1418 0.6047 11.00000 0.05 0.17 Q22 1 -0.0474 0.3225 0.5792 11.00000 0.05 0.17 Q23 1 0.3327 0.1577 0.5223 11.00000 0.05 0.17 Q24 1 0.0036 0.2619 0.6870 11.00000 0.05 0.17 Q25 1 0.2603 0.0469 0.9893 11.00000 0.05 0.16 ; _shelx_res_checksum 39278 _olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)' _database_code_depnum_ccdc_archive 'CCDC 995941' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mccc _audit_creation_date 2013-08-21 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H49 N2 Ni O, F6 P' _chemical_formula_sum 'C36 H49 F6 N2 Ni O P' _chemical_formula_weight 729.45 _chemical_absolute_configuration unk _chemical_melting_point ? _chemical_oxdiff_formula 'C32 H41 N2 Ni P F6' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_H-M_alt 'C 1 c 1' _space_group_name_Hall 'C -2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x, -y, z+1/2' 3 'x+1/2, y+1/2, z' 4 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.7889(2) _cell_length_b 16.8666(3) _cell_length_c 16.4852(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.4860(10) _cell_angle_gamma 90.00 _cell_volume 3545.05(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13554 _cell_measurement_temperature 122.96(18) _cell_measurement_theta_max 73.1390 _cell_measurement_theta_min 4.2980 _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light pink' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1536 _exptl_crystal_size_max 0.1974 _exptl_crystal_size_mid 0.0705 _exptl_crystal_size_min 0.0462 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 20803 _diffrn_reflns_theta_full 66.97 _diffrn_reflns_theta_max 73.66 _diffrn_reflns_theta_min 4.35 _diffrn_ambient_temperature 122.96(18) _diffrn_detector_area_resol_mean 10.3546 _diffrn_measured_fraction_theta_full 0.9985 _diffrn_measured_fraction_theta_max 0.9840 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 22.00 111.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 37.0000 -60.0000 178 #__ type_ start__ end____ width___ exp.time_ 2 omega 27.00 117.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 37.0000 -150.0000 180 #__ type_ start__ end____ width___ exp.time_ 3 omega 32.00 74.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -45.0000 -30.0000 84 #__ type_ start__ end____ width___ exp.time_ 4 omega 36.00 64.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 0.0000 56 #__ type_ start__ end____ width___ exp.time_ 5 omega 38.00 109.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 0.0000 142 #__ type_ start__ end____ width___ exp.time_ 6 omega 31.00 68.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 -150.0000 74 #__ type_ start__ end____ width___ exp.time_ 7 omega 76.00 158.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 77.0000 120.0000 164 #__ type_ start__ end____ width___ exp.time_ 8 omega 29.00 69.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 30.0000 80 #__ type_ start__ end____ width___ exp.time_ 9 omega 35.00 86.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 -120.0000 102 #__ type_ start__ end____ width___ exp.time_ 10 omega 26.00 82.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -94.0000 -180.0000 112 #__ type_ start__ end____ width___ exp.time_ 11 omega -98.00 -2.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 125.0000 -60.0000 192 #__ type_ start__ end____ width___ exp.time_ 12 omega -33.00 71.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 -57.0000 150.0000 208 #__ type_ start__ end____ width___ exp.time_ 13 omega 15.00 117.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 37.0000 90.0000 204 #__ type_ start__ end____ width___ exp.time_ 14 omega 79.00 158.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 45.0000 90.0000 158 #__ type_ start__ end____ width___ exp.time_ 15 omega 76.00 158.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 30.0000 -150.0000 164 #__ type_ start__ end____ width___ exp.time_ 16 omega 77.00 158.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 61.0000 -90.0000 162 #__ type_ start__ end____ width___ exp.time_ 17 omega 29.00 69.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -30.0000 -180.0000 80 #__ type_ start__ end____ width___ exp.time_ 18 omega 32.00 121.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -125.0000 -180.0000 178 #__ type_ start__ end____ width___ exp.time_ 19 omega 46.00 158.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 15.0000 30.0000 224 #__ type_ start__ end____ width___ exp.time_ 20 omega -120.00 -8.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - -41.2064 -77.0000 150.0000 224 #__ type_ start__ end____ width___ exp.time_ 21 omega 8.00 120.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 77.0000 90.0000 224 #__ type_ start__ end____ width___ exp.time_ 22 omega 12.00 115.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 41.2064 57.0000 -30.0000 206 #__ type_ start__ end____ width___ exp.time_ 23 omega -162.00 -49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 -50.7416 226 #__ type_ start__ end____ width___ exp.time_ 24 omega -162.00 -49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - -83.0000 -77.0000 30.0000 226 #__ type_ start__ end____ width___ exp.time_ 25 omega 73.00 158.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 77.0000 -150.0000 170 #__ type_ start__ end____ width___ exp.time_ 26 omega 32.00 76.50 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 106.9800 -45.0000 150.0000 89 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0229755000 _diffrn_orient_matrix_UB_12 0.0203420000 _diffrn_orient_matrix_UB_13 0.0879466000 _diffrn_orient_matrix_UB_21 -0.1068947000 _diffrn_orient_matrix_UB_22 0.0351564000 _diffrn_orient_matrix_UB_23 -0.0312645000 _diffrn_orient_matrix_UB_31 -0.0516670000 _diffrn_orient_matrix_UB_32 -0.0817579000 _diffrn_orient_matrix_UB_33 0.0083566000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6549 _reflns_number_total 6714 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2\s(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.229 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(13) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 424 _refine_ls_number_reflns 6714 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0258 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.6977P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.0671 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C15(H15), C18(H18), C27(H27), C30(H30) 2.b Secondary CH2 refined with riding coordinates: C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B) 2.c Me refined with riding coordinates: C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B, H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A, H32B,H32C) 2.d Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C23(H23), C24(H24), C25(H25) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn C1 C 0.58064(13) 0.28108(11) 0.07626(10) 0.0204(3) Uani 1 1 d . . . C2 C 0.48162(14) 0.35090(12) -0.01884(11) 0.0254(4) Uani 1 1 d . . . H2 H 0.4256 0.3657 -0.0551 0.031 Uiso 1 1 calc . . R C3 C 0.57246(14) 0.39025(12) -0.00416(11) 0.0265(4) Uani 1 1 d . . . H3 H 0.5911 0.4377 -0.0279 0.032 Uiso 1 1 calc . . R C4 C 0.63652(16) 0.16009(16) 0.28256(13) 0.0398(5) Uani 1 1 d . . . H4 H 0.7003 0.1513 0.3123 0.048 Uiso 1 1 calc . . R C5 C 0.57948(17) 0.23029(14) 0.28127(12) 0.0357(4) Uani 1 1 d . . . H5 H 0.5946 0.2753 0.3127 0.043 Uiso 1 1 calc . . R C6 C 0.49363(15) 0.21958(13) 0.22243(13) 0.0329(4) Uani 1 1 d . . . H6 H 0.4463 0.2587 0.2042 0.039 Uiso 1 1 calc . . R C7 C 0.49158(16) 0.13900(14) 0.19565(12) 0.0346(5) Uani 1 1 d . . . H7 H 0.4397 0.1152 0.1612 0.042 Uiso 1 1 calc . . R C8 C 0.58100(18) 0.10329(13) 0.23054(13) 0.0372(5) Uani 1 1 d . . . H8 H 0.6018 0.0513 0.2219 0.045 Uiso 1 1 calc . . R C9 C 0.40716(13) 0.22339(11) 0.02416(11) 0.0228(3) Uani 1 1 d . . . C10 C 0.31090(13) 0.23918(12) 0.05633(11) 0.0258(4) Uani 1 1 d . . . C11 C 0.23478(15) 0.17932(13) 0.04780(13) 0.0338(4) Uani 1 1 d . . . H11 H 0.1695 0.1877 0.0675 0.041 Uiso 1 1 calc . . R C12 C 0.25471(16) 0.10832(14) 0.01082(13) 0.0379(5) Uani 1 1 d . . . H12 H 0.2032 0.0693 0.0064 0.045 Uiso 1 1 calc . . R C13 C 0.35129(15) 0.09448(12) -0.01996(12) 0.0315(4) Uani 1 1 d . . . H13 H 0.3642 0.0458 -0.0436 0.038 Uiso 1 1 calc . . R C14 C 0.42882(14) 0.15249(12) -0.01582(11) 0.0247(4) Uani 1 1 d . . . C15 C 0.28523(14) 0.31616(12) 0.09737(13) 0.0298(4) Uani 1 1 d . . . H15 H 0.3513 0.3435 0.1131 0.036 Uiso 1 1 calc . . R C16 C 0.22699(16) 0.30382(14) 0.17413(14) 0.0367(5) Uani 1 1 d . . . H16A H 0.2126 0.3544 0.1976 0.055 Uiso 1 1 calc . . R H16B H 0.2697 0.2729 0.2127 0.055 Uiso 1 1 calc . . R H16C H 0.1622 0.2765 0.1602 0.055 Uiso 1 1 calc . . R C17 C 0.21934(17) 0.36980(16) 0.03819(16) 0.0466(6) Uani 1 1 d . . . H17A H 0.2035 0.4183 0.0652 0.070 Uiso 1 1 calc . . R H17B H 0.1552 0.3432 0.0204 0.070 Uiso 1 1 calc . . R H17C H 0.2580 0.3814 -0.0080 0.070 Uiso 1 1 calc . . R C18 C 0.53050(14) 0.13913(12) -0.05580(12) 0.0285(4) Uani 1 1 d . . . H18 H 0.5868 0.1652 -0.0219 0.034 Uiso 1 1 calc . . R C19 C 0.55984(18) 0.05177(14) -0.06256(16) 0.0419(5) Uani 1 1 d . . . H19A H 0.6244 0.0473 -0.0882 0.063 Uiso 1 1 calc . . R H19B H 0.5053 0.0243 -0.0945 0.063 Uiso 1 1 calc . . R H19C H 0.5683 0.0288 -0.0092 0.063 Uiso 1 1 calc . . R C20 C 0.52507(18) 0.17849(16) -0.14015(13) 0.0410(5) Uani 1 1 d . . . H20A H 0.5898 0.1696 -0.1646 0.061 Uiso 1 1 calc . . R H20B H 0.5139 0.2344 -0.1345 0.061 Uiso 1 1 calc . . R H20C H 0.4682 0.1560 -0.1740 0.061 Uiso 1 1 calc . . R C21 C 0.74026(13) 0.36830(10) 0.07806(11) 0.0211(3) Uani 1 1 d . . . C22 C 0.76104(13) 0.40906(11) 0.15143(11) 0.0233(4) Uani 1 1 d . . . C23 C 0.86481(14) 0.43285(12) 0.17160(12) 0.0289(4) Uani 1 1 d . . . H23 H 0.8817 0.4595 0.2203 0.035 Uiso 1 1 calc . . R C24 C 0.94216(14) 0.41727(13) 0.12016(14) 0.0332(4) Uani 1 1 d . . . H24 H 1.0107 0.4332 0.1347 0.040 Uiso 1 1 calc . . R C25 C 0.91919(14) 0.37834(12) 0.04750(13) 0.0311(4) Uani 1 1 d . . . H25 H 0.9723 0.3691 0.0133 0.037 Uiso 1 1 calc . . R C26 C 0.81718(14) 0.35234(11) 0.02426(12) 0.0252(4) Uani 1 1 d . . . C27 C 0.67617(14) 0.43150(12) 0.20600(11) 0.0264(4) Uani 1 1 d . . . H27 H 0.6153 0.3973 0.1926 0.032 Uiso 1 1 calc . . R C28 C 0.71050(16) 0.42072(13) 0.29616(12) 0.0338(4) Uani 1 1 d . . . H28A H 0.6541 0.4355 0.3282 0.051 Uiso 1 1 calc . . R H28B H 0.7703 0.4537 0.3105 0.051 Uiso 1 1 calc . . R H28C H 0.7287 0.3662 0.3065 0.051 Uiso 1 1 calc . . R C29 C 0.64329(17) 0.51718(13) 0.18863(13) 0.0372(5) Uani 1 1 d . . . H29A H 0.5892 0.5318 0.2230 0.056 Uiso 1 1 calc . . R H29B H 0.6173 0.5222 0.1326 0.056 Uiso 1 1 calc . . R H29C H 0.7027 0.5515 0.1993 0.056 Uiso 1 1 calc . . R C30 C 0.79418(16) 0.31154(12) -0.05697(12) 0.0308(4) Uani 1 1 d . . . H30 H 0.7285 0.2819 -0.0551 0.037 Uiso 1 1 calc . . R C31 C 0.7797(2) 0.37266(15) -0.12602(14) 0.0454(5) Uani 1 1 d . . . H31A H 0.7655 0.3457 -0.1770 0.068 Uiso 1 1 calc . . R H31B H 0.8426 0.4035 -0.1277 0.068 Uiso 1 1 calc . . R H31C H 0.7220 0.4070 -0.1165 0.068 Uiso 1 1 calc . . R C32 C 0.8798(2) 0.25339(16) -0.07728(14) 0.0420(5) Uani 1 1 d . . . H32A H 0.8613 0.2296 -0.1293 0.063 Uiso 1 1 calc . . R H32B H 0.8869 0.2129 -0.0363 0.063 Uiso 1 1 calc . . R H32C H 0.9451 0.2812 -0.0790 0.063 Uiso 1 1 calc . . R C33 C 0.78277(15) 0.11351(13) 0.08143(13) 0.0333(4) Uani 1 1 d . . . H33A H 0.7665 0.1224 0.0237 0.040 Uiso 1 1 calc . . R H33B H 0.7400 0.0700 0.0985 0.040 Uiso 1 1 calc . . R C34 C 0.89865(16) 0.09445(14) 0.09889(13) 0.0360(4) Uani 1 1 d . . . H34A H 0.9313 0.0834 0.0489 0.043 Uiso 1 1 calc . . R H34B H 0.9083 0.0491 0.1349 0.043 Uiso 1 1 calc . . R C35 C 0.94455(14) 0.16924(14) 0.13967(13) 0.0346(4) Uani 1 1 d . . . H35A H 1.0041 0.1568 0.1776 0.041 Uiso 1 1 calc . . R H35B H 0.9662 0.2068 0.0997 0.041 Uiso 1 1 calc . . R C36 C 0.85411(14) 0.20103(12) 0.18333(12) 0.0292(4) Uani 1 1 d . . . H36A H 0.8487 0.1739 0.2347 0.035 Uiso 1 1 calc . . R H36B H 0.8619 0.2575 0.1934 0.035 Uiso 1 1 calc . . R N1 N 0.48714(11) 0.28455(9) 0.02998(9) 0.0210(3) Uani 1 1 d . . . N2 N 0.63326(11) 0.34662(9) 0.05329(9) 0.0208(3) Uani 1 1 d . . . F1 F 0.44719(11) 0.54886(8) 0.30785(9) 0.0478(3) Uani 1 1 d . . . F2 F 0.45174(13) 0.45410(11) 0.40218(9) 0.0615(4) Uani 1 1 d . . . F3 F 0.31137(12) 0.53566(10) 0.38406(11) 0.0622(5) Uani 1 1 d . . . F4 F 0.29471(12) 0.40761(9) 0.34766(10) 0.0508(3) Uani 1 1 d . . . F5 F 0.29274(12) 0.50185(10) 0.25193(10) 0.0554(4) Uani 1 1 d . . . F6 F 0.43075(11) 0.42025(9) 0.26967(9) 0.0488(3) Uani 1 1 d . . . P1 P 0.37196(4) 0.47700(3) 0.32741(3) 0.03002(11) Uani 1 1 d . . . Ni1 Ni 0.62305(2) 0.207784(17) 0.160228(17) 0.02205(7) Uani 1 1 d . . . O1 O 0.76277(9) 0.18487(8) 0.12716(8) 0.0266(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0171(7) 0.0222(9) 0.0224(8) -0.0016(6) 0.0036(6) -0.0016(6) C2 0.0194(8) 0.0276(10) 0.0285(9) 0.0078(7) -0.0028(7) -0.0006(7) C3 0.0231(8) 0.0244(9) 0.0316(9) 0.0078(7) 0.0005(7) -0.0010(7) C4 0.0295(10) 0.0608(15) 0.0293(10) 0.0188(10) 0.0038(8) -0.0005(10) C5 0.0415(11) 0.0416(12) 0.0255(9) -0.0015(8) 0.0127(8) -0.0066(9) C6 0.0253(9) 0.0408(12) 0.0340(10) 0.0102(9) 0.0115(8) 0.0058(8) C7 0.0306(10) 0.0414(12) 0.0322(10) 0.0086(9) 0.0051(8) -0.0133(9) C8 0.0437(11) 0.0300(11) 0.0394(11) 0.0126(9) 0.0138(9) 0.0016(9) C9 0.0182(8) 0.0254(9) 0.0248(8) 0.0040(7) 0.0014(6) -0.0039(7) C10 0.0183(8) 0.0327(10) 0.0265(9) 0.0018(8) 0.0019(6) -0.0043(7) C11 0.0216(9) 0.0426(12) 0.0383(11) -0.0049(9) 0.0079(8) -0.0110(8) C12 0.0320(10) 0.0434(12) 0.0390(11) -0.0080(10) 0.0080(8) -0.0198(9) C13 0.0341(10) 0.0300(10) 0.0306(10) -0.0062(8) 0.0036(8) -0.0095(8) C14 0.0224(8) 0.0288(10) 0.0226(8) 0.0008(7) -0.0009(6) -0.0047(7) C15 0.0179(8) 0.0322(10) 0.0396(10) 0.0005(8) 0.0046(7) -0.0006(7) C16 0.0293(10) 0.0422(12) 0.0393(11) -0.0070(9) 0.0080(8) -0.0035(8) C17 0.0308(11) 0.0503(14) 0.0599(15) 0.0160(12) 0.0114(10) 0.0111(10) C18 0.0247(9) 0.0311(10) 0.0297(9) -0.0058(8) 0.0023(7) -0.0026(7) C19 0.0369(11) 0.0353(12) 0.0546(14) -0.0077(10) 0.0109(10) 0.0008(9) C20 0.0399(11) 0.0533(14) 0.0311(10) -0.0004(10) 0.0118(9) -0.0026(10) C21 0.0157(7) 0.0200(8) 0.0279(8) 0.0017(7) 0.0021(6) -0.0025(6) C22 0.0194(8) 0.0203(9) 0.0301(9) 0.0005(7) 0.0010(6) -0.0001(6) C23 0.0249(9) 0.0248(9) 0.0359(10) -0.0031(8) -0.0050(7) -0.0016(7) C24 0.0162(8) 0.0316(10) 0.0515(12) -0.0023(9) 0.0005(8) -0.0051(7) C25 0.0199(8) 0.0302(10) 0.0442(11) -0.0007(8) 0.0091(7) -0.0020(7) C26 0.0218(8) 0.0216(9) 0.0328(9) 0.0015(7) 0.0053(7) 0.0001(6) C27 0.0244(8) 0.0282(10) 0.0268(9) -0.0024(7) 0.0029(7) 0.0015(7) C28 0.0380(11) 0.0340(11) 0.0291(10) -0.0033(8) 0.0006(8) 0.0006(9) C29 0.0374(11) 0.0375(12) 0.0378(11) 0.0035(9) 0.0112(8) 0.0133(9) C30 0.0318(9) 0.0304(10) 0.0311(9) -0.0022(8) 0.0084(7) -0.0027(8) C31 0.0640(15) 0.0391(13) 0.0338(11) 0.0022(10) 0.0080(10) 0.0052(11) C32 0.0523(13) 0.0379(12) 0.0374(12) -0.0015(9) 0.0142(10) 0.0080(9) C33 0.0302(10) 0.0331(11) 0.0367(10) -0.0081(8) 0.0040(8) 0.0055(8) C34 0.0311(10) 0.0413(12) 0.0361(10) -0.0004(9) 0.0056(8) 0.0119(9) C35 0.0199(9) 0.0405(12) 0.0433(11) 0.0092(9) 0.0026(8) 0.0046(8) C36 0.0200(8) 0.0290(10) 0.0380(10) 0.0003(8) -0.0009(7) -0.0003(7) N1 0.0145(6) 0.0236(8) 0.0248(7) 0.0020(6) 0.0002(5) -0.0024(5) N2 0.0166(6) 0.0224(7) 0.0232(7) 0.0010(6) 0.0005(5) -0.0027(5) F1 0.0519(8) 0.0383(7) 0.0554(8) -0.0037(6) 0.0171(6) -0.0121(6) F2 0.0624(10) 0.0759(12) 0.0437(8) 0.0141(8) -0.0129(7) -0.0074(8) F3 0.0519(8) 0.0601(10) 0.0785(11) -0.0370(8) 0.0300(8) -0.0125(7) F4 0.0514(8) 0.0439(8) 0.0589(8) 0.0005(7) 0.0149(6) -0.0131(6) F5 0.0521(8) 0.0555(9) 0.0560(9) 0.0065(7) -0.0128(7) 0.0049(7) F6 0.0435(7) 0.0450(8) 0.0595(8) -0.0189(7) 0.0147(6) 0.0019(6) P1 0.0317(2) 0.0288(3) 0.0302(2) -0.0024(2) 0.00646(18) -0.00050(19) Ni1 0.01834(13) 0.02364(15) 0.02435(14) 0.00374(13) 0.00288(10) 0.00083(12) O1 0.0199(6) 0.0282(7) 0.0315(7) 0.0015(6) 0.0010(5) 0.0031(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.368(2) . ? C1 N2 1.363(2) . ? C1 Ni1 1.9029(18) . ? C2 C3 1.343(3) . ? C2 N1 1.377(2) . ? C3 N2 1.389(2) . ? C4 C5 1.390(3) . ? C4 C8 1.436(4) . ? C4 Ni1 2.165(2) . ? C5 C6 1.419(3) . ? C5 Ni1 2.1471(19) . ? C6 C7 1.429(3) . ? C6 Ni1 2.0239(19) . ? C7 C8 1.378(3) . ? C7 Ni1 2.1604(19) . ? C8 Ni1 2.199(2) . ? C9 C10 1.404(3) . ? C9 C14 1.403(3) . ? C9 N1 1.451(2) . ? C10 C11 1.402(3) . ? C10 C15 1.512(3) . ? C11 C12 1.377(3) . ? C12 C13 1.391(3) . ? C13 C14 1.391(3) . ? C14 C18 1.520(3) . ? C15 C16 1.532(3) . ? C15 C17 1.533(3) . ? C18 C19 1.527(3) . ? C18 C20 1.538(3) . ? C21 C22 1.398(3) . ? C21 C26 1.401(2) . ? C21 N2 1.444(2) . ? C22 C23 1.401(2) . ? C22 C27 1.511(2) . ? C23 C24 1.378(3) . ? C24 C25 1.377(3) . ? C25 C26 1.401(3) . ? C26 C30 1.514(3) . ? C27 C28 1.527(3) . ? C27 C29 1.526(3) . ? C30 C31 1.536(3) . ? C30 C32 1.527(3) . ? C33 C34 1.522(3) . ? C33 O1 1.453(2) . ? C34 C35 1.525(3) . ? C35 C36 1.508(3) . ? C36 O1 1.459(2) . ? F1 P1 1.5959(14) . ? F2 P1 1.5850(15) . ? F3 P1 1.6014(15) . ? F4 P1 1.5840(14) . ? F5 P1 1.5980(14) . ? F6 P1 1.5811(13) . ? Ni1 O1 1.9473(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Ni1 128.34(13) . . ? N2 C1 N1 103.85(15) . . ? N2 C1 Ni1 127.59(12) . . ? C3 C2 N1 106.99(15) . . ? C2 C3 N2 106.94(16) . . ? C5 C4 C8 108.95(19) . . ? C5 C4 Ni1 70.48(12) . . ? C8 C4 Ni1 72.07(12) . . ? C4 C5 C6 106.2(2) . . ? C4 C5 Ni1 71.92(12) . . ? C6 C5 Ni1 65.50(11) . . ? C5 C6 C7 109.09(19) . . ? C5 C6 Ni1 74.87(11) . . ? C7 C6 Ni1 75.28(12) . . ? C6 C7 Ni1 64.96(11) . . ? C8 C7 C6 106.99(19) . . ? C8 C7 Ni1 73.11(12) . . ? C4 C8 Ni1 69.53(12) . . ? C7 C8 C4 108.2(2) . . ? C7 C8 Ni1 70.05(12) . . ? C10 C9 C14 123.39(16) . . ? C10 C9 N1 118.35(16) . . ? C14 C9 N1 118.23(15) . . ? C9 C10 C15 124.03(16) . . ? C11 C10 C9 116.62(18) . . ? C11 C10 C15 119.34(17) . . ? C12 C11 C10 121.32(18) . . ? C11 C12 C13 120.53(18) . . ? C14 C13 C12 120.92(19) . . ? C9 C14 C18 122.47(16) . . ? C13 C14 C9 117.16(17) . . ? C13 C14 C18 120.35(18) . . ? C10 C15 C16 112.93(17) . . ? C10 C15 C17 110.47(18) . . ? C16 C15 C17 109.10(17) . . ? C14 C18 C19 113.46(17) . . ? C14 C18 C20 110.39(16) . . ? C19 C18 C20 110.16(18) . . ? C22 C21 C26 123.12(16) . . ? C22 C21 N2 118.74(15) . . ? C26 C21 N2 117.97(15) . . ? C21 C22 C23 117.29(16) . . ? C21 C22 C27 122.76(15) . . ? C23 C22 C27 119.87(17) . . ? C24 C23 C22 120.77(18) . . ? C23 C24 C25 120.77(17) . . ? C24 C25 C26 121.18(17) . . ? C21 C26 C30 123.35(16) . . ? C25 C26 C21 116.85(17) . . ? C25 C26 C30 119.77(16) . . ? C22 C27 C28 112.60(15) . . ? C22 C27 C29 109.01(16) . . ? C29 C27 C28 110.45(17) . . ? C26 C30 C31 110.75(18) . . ? C26 C30 C32 113.13(17) . . ? C32 C30 C31 108.39(18) . . ? O1 C33 C34 106.56(16) . . ? C33 C34 C35 104.14(16) . . ? C36 C35 C34 102.79(15) . . ? O1 C36 C35 103.69(16) . . ? C1 N1 C2 111.30(14) . . ? C1 N1 C9 125.97(15) . . ? C2 N1 C9 122.39(14) . . ? C1 N2 C3 110.91(14) . . ? C1 N2 C21 127.18(15) . . ? C3 N2 C21 121.75(15) . . ? F1 P1 F3 88.60(8) . . ? F1 P1 F5 89.94(9) . . ? F2 P1 F1 88.89(9) . . ? F2 P1 F3 90.49(10) . . ? F2 P1 F5 178.80(10) . . ? F4 P1 F1 178.22(9) . . ? F4 P1 F2 91.73(9) . . ? F4 P1 F3 89.73(9) . . ? F4 P1 F5 89.42(9) . . ? F5 P1 F3 89.19(10) . . ? F6 P1 F1 90.89(8) . . ? F6 P1 F2 90.76(9) . . ? F6 P1 F3 178.65(10) . . ? F6 P1 F4 90.77(8) . . ? F6 P1 F5 89.56(9) . . ? C1 Ni1 C4 156.37(9) . . ? C1 Ni1 C5 118.77(8) . . ? C1 Ni1 C6 96.13(8) . . ? C1 Ni1 C7 111.22(8) . . ? C1 Ni1 C8 146.77(8) . . ? C1 Ni1 O1 98.10(6) . . ? C4 Ni1 C8 38.41(9) . . ? C5 Ni1 C4 37.60(9) . . ? C5 Ni1 C7 65.15(8) . . ? C5 Ni1 C8 63.89(9) . . ? C6 Ni1 C4 64.74(8) . . ? C6 Ni1 C5 39.63(9) . . ? C6 Ni1 C7 39.76(9) . . ? C6 Ni1 C8 64.43(8) . . ? C7 Ni1 C4 63.62(8) . . ? C7 Ni1 C8 36.83(8) . . ? O1 Ni1 C4 100.32(7) . . ? O1 Ni1 C5 127.29(7) . . ? O1 Ni1 C6 165.03(7) . . ? O1 Ni1 C7 136.03(8) . . ? O1 Ni1 C8 104.84(7) . . ? C33 O1 C36 108.63(14) . . ? C33 O1 Ni1 120.80(11) . . ? C36 O1 Ni1 119.47(11) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -2 -10 3 0.0354 -1.9956 -10.0090 2.9962 0.1058 -0.2322 0.9465 2 10 -4 0.0295 1.9948 10.0106 -3.9958 -0.1936 0.2636 -0.9549 6 4 5 0.0705 6.0016 3.9947 4.9912 0.3823 -0.6571 -0.5950 -6 0 -7 0.1065 -6.0038 0.0100 -6.9881 -0.4764 0.8606 0.2510 4 -5 -8 0.0346 3.9928 -4.9872 -8.0059 -0.8973 -0.3518 0.1345 -4 5 8 0.0116 -3.9928 4.9872 8.0059 0.8973 0.3518 -0.1345 -6 -7 4 0.0484 -5.9939 -7.0108 4.0036 0.3472 0.2691 0.9163 5 -6 -6 0.0167 4.9943 -5.9906 -6.0088 -0.7651 -0.5566 0.1815 -8 0 4 0.0521 -7.9942 -0.0090 4.0107 0.5362 0.7288 0.4473 _database_code_depnum_ccdc_archive 'CCDC 999501'