# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2015 ####################################################################### # # 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_l0612a _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H71 Ir N2 O6 P2 S2, C H2 Cl2, 0.5(C4 H10 O)' _chemical_formula_sum 'C60 H78 Cl2 Ir N2 O6.50 P2 S2' _chemical_formula_weight 1320.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6106(3) _cell_length_b 17.2668(6) _cell_length_c 18.6161(4) _cell_angle_alpha 113.198(2) _cell_angle_beta 95.475(2) _cell_angle_gamma 105.211(1) _cell_volume 3226.02(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 44333 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 27.58 loop_ _diffrn_orient_matrix_type _diffrn_orient_matrix_UB_11 _diffrn_orient_matrix_UB_12 _diffrn_orient_matrix_UB_13 _diffrn_orient_matrix_UB_21 _diffrn_orient_matrix_UB_22 _diffrn_orient_matrix_UB_23 _diffrn_orient_matrix_UB_31 _diffrn_orient_matrix_UB_32 _diffrn_orient_matrix_UB_33 'Nonius RMAT' -0.0783263 -0.0396267 -0.0406932 -0.0358757 0.0492829 0.0198926 0.0315352 0.0214509 -0.0393877 'Nonius RMAT' -0.0770101 -0.0453545 -0.0391812 -0.0422987 0.0458352 0.0155502 0.0263970 0.0173589 -0.0427326 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_F_000 1354 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_absorpt_coefficient_mu 2.314 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details TWINABS-2012/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 50934 _diffrn_reflns_av_unetI/netI 0.0166 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.865 _diffrn_reflns_theta_max 27.718 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 14853 _reflns_number_gt 14073 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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. ; _computing_data_collection Apex2 _computing_cell_refinement Peakref _computing_data_reduction 'Eval15, Twinabs' _computing_structure_solution SHELXT _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+2.4464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 14853 _refine_ls_number_parameters 718 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ir1 Ir 0.12552(2) 0.08584(2) 0.20654(2) 0.01508(4) Uani 1 1 d . . . . . H1 H 0.1509 0.0535 0.2677 0.050 Uiso 1 1 d . . . . . S1 S 0.08333(5) -0.10601(4) 0.06978(3) 0.01699(11) Uani 1 1 d . . . . . S2 S 0.35204(5) 0.23616(4) 0.32704(4) 0.01908(12) Uani 1 1 d . . . . . P1 P -0.05752(6) -0.01999(4) 0.16260(4) 0.01648(12) Uani 1 1 d . . . . . P2 P 0.10650(6) 0.19615(4) 0.31396(4) 0.01829(12) Uani 1 1 d . . . . . O1 O -0.14114(16) 0.13353(12) 0.23099(10) 0.0187(3) Uani 1 1 d . . . . . O2 O 0.17257(16) -0.01308(12) 0.11051(11) 0.0195(3) Uani 1 1 d . . . . . O3 O 0.07965(17) -0.14709(12) -0.01561(11) 0.0225(4) Uani 1 1 d . . . . . O4 O 0.31177(16) 0.17660(12) 0.23806(11) 0.0190(3) Uani 1 1 d . . . . . O5 O 0.4072(2) 0.19457(13) 0.36754(13) 0.0316(5) Uani 1 1 d . . . . . O6 O 0.10258(18) 0.13574(13) 0.11338(11) 0.0245(4) Uani 1 1 d . . . . . H1O H 0.0501 0.1459 0.0880 0.050 Uiso 1 1 d . . . . . H2O H 0.1414 0.1138 0.0783 0.050 Uiso 1 1 d . . . . . N1 N -0.04567(19) -0.10745(14) 0.08635(13) 0.0204(4) Uani 1 1 d . . . . . N2 N 0.2464(2) 0.26691(16) 0.36116(13) 0.0243(5) Uani 1 1 d . . . . . C1 C -0.1846(2) -0.00028(17) 0.11547(14) 0.0173(5) Uani 1 1 d . . . . . C2 C -0.2057(2) 0.08005(17) 0.15270(15) 0.0180(5) Uani 1 1 d . . . . . C3 C -0.2826(2) 0.11008(17) 0.11602(15) 0.0200(5) Uani 1 1 d . . . . . C4 C -0.3479(2) 0.05123(18) 0.03794(16) 0.0228(5) Uani 1 1 d . . . . . H4 H -0.4010 0.0687 0.0099 0.027 Uiso 1 1 calc R U . . . C5 C -0.3361(2) -0.03289(19) 0.00063(16) 0.0234(5) Uani 1 1 d . . . . . H5 H -0.3848 -0.0732 -0.0515 0.028 Uiso 1 1 calc R U . . . C6 C -0.2548(2) -0.05900(17) 0.03799(15) 0.0199(5) Uani 1 1 d . . . . . H6 H -0.2468 -0.1162 0.0113 0.024 Uiso 1 1 calc R U . . . C7 C 0.0262(2) 0.26501(17) 0.29387(15) 0.0207(5) Uani 1 1 d . . . . . C8 C -0.0920(2) 0.22257(17) 0.24721(15) 0.0195(5) Uani 1 1 d . . . . . C9 C -0.1591(2) 0.26187(18) 0.21574(17) 0.0235(5) Uani 1 1 d . . . . . C10 C -0.1031(3) 0.3524(2) 0.2375(2) 0.0335(7) Uani 1 1 d . . . . . H10 H -0.1453 0.3831 0.2182 0.040 Uiso 1 1 calc R U . . . C11 C 0.0138(3) 0.3985(2) 0.2871(2) 0.0384(7) Uani 1 1 d . . . . . H11 H 0.0493 0.4604 0.3019 0.046 Uiso 1 1 calc R U . . . C12 C 0.0790(3) 0.35552(19) 0.31505(19) 0.0300(6) Uani 1 1 d . . . . . H12 H 0.1590 0.3875 0.3484 0.036 Uiso 1 1 calc R U . . . C13 C -0.2871(2) 0.20434(19) 0.16367(17) 0.0236(5) Uani 1 1 d . . . . . C14 C -0.3755(3) 0.2007(2) 0.22040(18) 0.0307(6) Uani 1 1 d . . . . . H14A H -0.3497 0.1741 0.2542 0.046 Uiso 1 1 calc R U . . . H14B H -0.4588 0.1645 0.1885 0.046 Uiso 1 1 calc R U . . . H14C H -0.3737 0.2613 0.2544 0.046 Uiso 1 1 calc R U . . . C15 C -0.3292(3) 0.2420(2) 0.1080(2) 0.0327(6) Uani 1 1 d . . . . . H15A H -0.3302 0.3023 0.1401 0.049 Uiso 1 1 calc R U . . . H15B H -0.4117 0.2037 0.0758 0.049 Uiso 1 1 calc R U . . . H15C H -0.2726 0.2441 0.0725 0.049 Uiso 1 1 calc R U . . . C16 C 0.1328(3) -0.17221(18) 0.11210(16) 0.0219(5) Uani 1 1 d . . . . . C17 C 0.2487(3) -0.1422(2) 0.16401(18) 0.0283(6) Uani 1 1 d . . . . . C18 C 0.2644(3) -0.1908(2) 0.20694(19) 0.0337(7) Uani 1 1 d . . . . . H18 H 0.3406 -0.1708 0.2434 0.040 Uiso 1 1 calc R U . . . C19 C 0.1750(3) -0.2662(2) 0.19912(19) 0.0340(7) Uani 1 1 d . . . . . C20 C 0.0677(3) -0.2990(2) 0.1412(2) 0.0336(7) Uani 1 1 d . . . . . H20 H 0.0082 -0.3536 0.1320 0.040 Uiso 1 1 calc R U . . . C21 C 0.0445(3) -0.25448(19) 0.09610(17) 0.0273(6) Uani 1 1 d . . . . . C22 C 0.3616(3) -0.0673(2) 0.1721(2) 0.0407(8) Uani 1 1 d . . . . . H22 H 0.3361 -0.0353 0.1422 0.049 Uiso 1 1 calc R U . . . C23 C 0.4194(4) -0.0003(3) 0.2583(3) 0.0546(11) Uani 1 1 d . . . . . H23A H 0.3600 0.0272 0.2820 0.082 Uiso 1 1 calc R U . . . H23B H 0.4915 0.0459 0.2602 0.082 Uiso 1 1 calc R U . . . H23C H 0.4443 -0.0306 0.2888 0.082 Uiso 1 1 calc R U . . . C24 C 0.4564(3) -0.1074(3) 0.1337(2) 0.0506(10) Uani 1 1 d . . . . . H24A H 0.4887 -0.1339 0.1655 0.076 Uiso 1 1 calc R U . . . H24B H 0.5236 -0.0604 0.1321 0.076 Uiso 1 1 calc R U . . . H24C H 0.4174 -0.1536 0.0790 0.076 Uiso 1 1 calc R U . . . C25 C 0.1974(4) -0.3105(2) 0.2530(2) 0.0436(8) Uani 1 1 d . . . . . H25 H 0.2882 -0.2916 0.2719 0.052 Uiso 1 1 calc R U . . . C26 C 0.1535(8) -0.4086(3) 0.2115(3) 0.100(2) Uani 1 1 d . . . . . H26A H 0.1988 -0.4320 0.2405 0.149 Uiso 1 1 calc R U . . . H26B H 0.1666 -0.4280 0.1568 0.149 Uiso 1 1 calc R U . . . H26C H 0.0660 -0.4310 0.2096 0.149 Uiso 1 1 calc R U . . . C27 C 0.1477(6) -0.2771(4) 0.3258(3) 0.0792(17) Uani 1 1 d . . . . . H27A H 0.0580 -0.3000 0.3108 0.119 Uiso 1 1 calc R U . . . H27B H 0.1756 -0.2117 0.3505 0.119 Uiso 1 1 calc R U . . . H27C H 0.1768 -0.2974 0.3641 0.119 Uiso 1 1 calc R U . . . C28 C -0.0723(3) -0.3010(2) 0.0298(2) 0.0366(7) Uani 1 1 d . . . . . H28 H -0.0755 -0.2618 0.0024 0.044 Uiso 1 1 calc R U . . . C29 C -0.0642(5) -0.3888(2) -0.0322(3) 0.0601(13) Uani 1 1 d . . . . . H29A H 0.0065 -0.3760 -0.0556 0.090 Uiso 1 1 calc R U . . . H29B H -0.1392 -0.4196 -0.0747 0.090 Uiso 1 1 calc R U . . . H29C H -0.0548 -0.4268 -0.0060 0.090 Uiso 1 1 calc R U . . . C30 C -0.1880(4) -0.3152(3) 0.0626(3) 0.0551(11) Uani 1 1 d . . . . . H30A H -0.1877 -0.3540 0.0893 0.083 Uiso 1 1 calc R U . . . H30B H -0.2603 -0.3431 0.0183 0.083 Uiso 1 1 calc R U . . . H30C H -0.1900 -0.2575 0.1011 0.083 Uiso 1 1 calc R U . . . C31 C -0.1184(2) -0.06190(17) 0.23135(15) 0.0210(5) Uani 1 1 d . . . . . C32 C -0.0590(3) -0.1101(2) 0.25703(18) 0.0313(6) Uani 1 1 d . . . . . H32 H 0.0143 -0.1172 0.2410 0.038 Uiso 1 1 calc R U . . . C33 C -0.1067(3) -0.1475(2) 0.3059(2) 0.0382(7) Uani 1 1 d . . . . . H33 H -0.0672 -0.1817 0.3220 0.046 Uiso 1 1 calc R U . . . C34 C -0.2117(3) -0.1352(2) 0.3314(2) 0.0382(7) Uani 1 1 d . . . . . H34 H -0.2443 -0.1612 0.3646 0.046 Uiso 1 1 calc R U . . . C35 C -0.2686(3) -0.0852(3) 0.3085(2) 0.0417(8) Uani 1 1 d . . . . . H35 H -0.3393 -0.0756 0.3271 0.050 Uiso 1 1 calc R U . . . C36 C -0.2226(3) -0.0488(2) 0.25828(19) 0.0320(6) Uani 1 1 d . . . . . H36 H -0.2626 -0.0148 0.2423 0.038 Uiso 1 1 calc R U . . . C37 C 0.4661(2) 0.33631(17) 0.33999(16) 0.0207(5) Uani 1 1 d . . . . . C38 C 0.4552(3) 0.37147(17) 0.28364(16) 0.0236(5) Uani 1 1 d . . . . . C39 C 0.5519(3) 0.44405(19) 0.29174(19) 0.0318(6) Uani 1 1 d . . . . . H39 H 0.5474 0.4665 0.2529 0.038 Uiso 1 1 calc R U . . . C40 C 0.6554(3) 0.4852(2) 0.3546(2) 0.0359(7) Uani 1 1 d . . . . . C41 C 0.6586(3) 0.4525(2) 0.41126(19) 0.0344(7) Uani 1 1 d . . . . . H41 H 0.7273 0.4814 0.4554 0.041 Uiso 1 1 calc R U . . . C42 C 0.5664(2) 0.37940(18) 0.40718(16) 0.0252(5) Uani 1 1 d . . . . . C43 C 0.3433(3) 0.33770(18) 0.21558(16) 0.0242(5) Uani 1 1 d . . . . . H43 H 0.2750 0.2959 0.2247 0.029 Uiso 1 1 calc R U . . . C44 C 0.3694(3) 0.2862(2) 0.13407(18) 0.0319(6) Uani 1 1 d . . . . . H44A H 0.4394 0.3250 0.1253 0.048 Uiso 1 1 calc R U . . . H44B H 0.2972 0.2670 0.0915 0.048 Uiso 1 1 calc R U . . . H44C H 0.3882 0.2339 0.1333 0.048 Uiso 1 1 calc R U . . . C45 C 0.3010(3) 0.4144(2) 0.21436(19) 0.0344(7) Uani 1 1 d . . . . . H45A H 0.3581 0.4487 0.1937 0.052 Uiso 1 1 calc R U . . . H45B H 0.2989 0.4535 0.2689 0.052 Uiso 1 1 calc R U . . . H45C H 0.2189 0.3900 0.1797 0.052 Uiso 1 1 calc R U . . . C46 C 0.7555(4) 0.5675(3) 0.3625(2) 0.0548(11) Uani 1 1 d . . . . . H46 H 0.7646 0.5603 0.3076 0.066 Uiso 1 1 calc R U . . . C47 C 0.7171(5) 0.6503(3) 0.4031(4) 0.0761(16) Uani 1 1 d . . . . . H47A H 0.6354 0.6402 0.3743 0.114 Uiso 1 1 calc R U . . . H47B H 0.7760 0.7020 0.4021 0.114 Uiso 1 1 calc R U . . . H47C H 0.7156 0.6615 0.4588 0.114 Uiso 1 1 calc R U . . . C48 C 0.8797(5) 0.5837(4) 0.4114(4) 0.091(2) Uani 1 1 d . . . . . H48A H 0.8759 0.6017 0.4679 0.136 Uiso 1 1 calc R U . . . H48B H 0.9423 0.6310 0.4067 0.136 Uiso 1 1 calc R U . . . H48C H 0.9008 0.5287 0.3912 0.136 Uiso 1 1 calc R U . . . C49 C 0.5827(3) 0.3540(2) 0.47649(17) 0.0300(6) Uani 1 1 d . . . . . H49 H 0.5018 0.3133 0.4741 0.036 Uiso 1 1 calc R U . . . C50 C 0.6217(4) 0.4358(3) 0.5585(2) 0.0562(12) Uani 1 1 d . . . . . H50A H 0.6160 0.4160 0.6011 0.084 Uiso 1 1 calc R U . . . H50B H 0.5675 0.4713 0.5607 0.084 Uiso 1 1 calc R U . . . H50C H 0.7063 0.4722 0.5660 0.084 Uiso 1 1 calc R U . . . C51 C 0.6740(3) 0.3030(3) 0.4672(2) 0.0489(9) Uani 1 1 d . . . . . H51A H 0.7534 0.3405 0.4669 0.073 Uiso 1 1 calc R U . . . H51B H 0.6437 0.2485 0.4166 0.073 Uiso 1 1 calc R U . . . H51C H 0.6832 0.2872 0.5120 0.073 Uiso 1 1 calc R U . . . C52 C 0.0386(2) 0.16645(18) 0.38744(15) 0.0223(5) Uani 1 1 d . . . . . C53 C -0.0620(3) 0.1884(2) 0.41299(17) 0.0305(6) Uani 1 1 d . . . . . H53 H -0.0986 0.2203 0.3918 0.037 Uiso 1 1 calc R U . . . C54 C -0.1093(3) 0.1634(3) 0.4697(2) 0.0392(7) Uani 1 1 d . . . . . H54 H -0.1785 0.1779 0.4869 0.047 Uiso 1 1 calc R U . . . C55 C -0.0557(3) 0.1178(2) 0.50077(19) 0.0383(7) Uani 1 1 d . . . . . H55 H -0.0885 0.1006 0.5391 0.046 Uiso 1 1 calc R U . . . C56 C 0.0453(3) 0.0968(2) 0.47657(19) 0.0356(7) Uani 1 1 d . . . . . H56 H 0.0825 0.0658 0.4987 0.043 Uiso 1 1 calc R U . . . C57 C 0.0924(3) 0.1209(2) 0.41977(17) 0.0292(6) Uani 1 1 d . . . . . H57 H 0.1617 0.1063 0.4030 0.035 Uiso 1 1 calc R U . . . Cl1 Cl 0.49519(16) 0.18475(13) 0.58208(10) 0.1023(6) Uani 1 1 d . . . . . Cl2 Cl 0.33453(13) 0.01156(10) 0.46612(11) 0.0864(4) Uani 1 1 d . . . . . C58 C 0.4576(4) 0.1048(3) 0.4827(3) 0.0651(12) Uani 1 1 d . . . . . H58A H 0.5295 0.0861 0.4693 0.078 Uiso 1 1 calc R U . . . H58B H 0.4361 0.1312 0.4469 0.078 Uiso 1 1 calc R U . . . O7 O 0.4078(10) 0.6001(6) 0.0568(7) 0.105(3) Uani 0.5 1 d . U P . . C59 C 0.4991(10) 0.6630(7) 0.1305(7) 0.074(3) Uani 0.5 1 d . U P . . H59A H 0.5716 0.6896 0.1136 0.089 Uiso 0.5 1 calc R U P . . H59B H 0.4658 0.7116 0.1575 0.089 Uiso 0.5 1 calc R U P . . C60 C 0.5447(11) 0.6413(7) 0.1912(7) 0.082(3) Uani 0.5 1 d . U P . . H60A H 0.6042 0.6951 0.2348 0.123 Uiso 0.5 1 calc R U P . . H60B H 0.5845 0.5965 0.1685 0.123 Uiso 0.5 1 calc R U P . . H60C H 0.4767 0.6175 0.2122 0.123 Uiso 0.5 1 calc R U P . . C61 C 0.3579(15) 0.6123(9) -0.0049(8) 0.098(4) Uani 0.5 1 d . U P . . H61A H 0.4290 0.6365 -0.0242 0.118 Uiso 0.5 1 calc R U P . . H61B H 0.3271 0.6626 0.0211 0.118 Uiso 0.5 1 calc R U P . . C62 C 0.2702(13) 0.5559(7) -0.0732(9) 0.100(4) Uani 0.5 1 d . U P . . H62A H 0.2543 0.5889 -0.1034 0.150 Uiso 0.5 1 calc R U P . . H62B H 0.1946 0.5307 -0.0592 0.150 Uiso 0.5 1 calc R U P . . H62C H 0.2986 0.5076 -0.1062 0.150 Uiso 0.5 1 calc R U 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 Ir1 0.01243(5) 0.01845(5) 0.01321(5) 0.00682(4) 0.00036(3) 0.00429(4) S1 0.0162(3) 0.0197(3) 0.0152(3) 0.0076(2) 0.0016(2) 0.0067(2) S2 0.0155(3) 0.0194(3) 0.0180(3) 0.0071(2) -0.0020(2) 0.0028(2) P1 0.0137(3) 0.0195(3) 0.0153(3) 0.0076(2) 0.0016(2) 0.0046(2) P2 0.0157(3) 0.0212(3) 0.0138(3) 0.0055(2) 0.0012(2) 0.0038(2) O1 0.0189(8) 0.0198(8) 0.0155(8) 0.0070(7) 0.0018(7) 0.0050(7) O2 0.0173(8) 0.0197(8) 0.0201(9) 0.0077(7) 0.0037(7) 0.0059(7) O3 0.0239(9) 0.0272(9) 0.0147(8) 0.0078(7) 0.0026(7) 0.0086(7) O4 0.0149(8) 0.0197(8) 0.0182(8) 0.0057(7) 0.0016(7) 0.0038(7) O5 0.0313(11) 0.0244(10) 0.0306(11) 0.0114(8) -0.0116(9) 0.0035(8) O6 0.0233(9) 0.0334(10) 0.0212(9) 0.0164(8) 0.0027(7) 0.0099(8) N1 0.0159(10) 0.0211(10) 0.0219(10) 0.0070(9) 0.0031(8) 0.0063(8) N2 0.0185(11) 0.0273(11) 0.0170(10) 0.0042(9) 0.0022(8) 0.0009(9) C1 0.0126(10) 0.0230(12) 0.0161(11) 0.0091(9) 0.0024(9) 0.0047(9) C2 0.0128(10) 0.0235(12) 0.0163(11) 0.0082(9) 0.0027(9) 0.0044(9) C3 0.0155(11) 0.0259(12) 0.0215(12) 0.0120(10) 0.0062(9) 0.0080(10) C4 0.0160(11) 0.0315(14) 0.0227(13) 0.0142(11) 0.0023(10) 0.0075(10) C5 0.0158(11) 0.0310(14) 0.0170(12) 0.0081(10) -0.0007(9) 0.0032(10) C6 0.0152(11) 0.0229(12) 0.0184(12) 0.0066(10) 0.0029(9) 0.0052(9) C7 0.0195(12) 0.0217(12) 0.0187(12) 0.0064(10) 0.0051(9) 0.0067(10) C8 0.0205(12) 0.0194(12) 0.0179(11) 0.0073(9) 0.0061(9) 0.0063(9) C9 0.0209(12) 0.0246(13) 0.0249(13) 0.0093(11) 0.0056(10) 0.0096(10) C10 0.0310(15) 0.0267(14) 0.0456(18) 0.0175(13) 0.0051(13) 0.0124(12) C11 0.0362(17) 0.0216(14) 0.052(2) 0.0130(14) 0.0056(15) 0.0063(12) C12 0.0254(14) 0.0232(13) 0.0335(15) 0.0070(12) 0.0025(12) 0.0053(11) C13 0.0201(12) 0.0293(13) 0.0258(13) 0.0137(11) 0.0051(10) 0.0123(10) C14 0.0247(14) 0.0365(15) 0.0317(15) 0.0114(12) 0.0105(12) 0.0154(12) C15 0.0318(15) 0.0337(15) 0.0380(16) 0.0193(13) 0.0030(13) 0.0154(13) C16 0.0251(13) 0.0258(13) 0.0202(12) 0.0122(10) 0.0053(10) 0.0130(11) C17 0.0261(14) 0.0313(14) 0.0324(15) 0.0173(12) 0.0024(12) 0.0127(12) C18 0.0318(16) 0.0375(16) 0.0335(16) 0.0185(13) -0.0036(12) 0.0131(13) C19 0.0447(18) 0.0353(16) 0.0298(15) 0.0186(13) 0.0050(13) 0.0196(14) C20 0.0383(17) 0.0282(14) 0.0373(16) 0.0192(13) 0.0034(13) 0.0094(13) C21 0.0286(14) 0.0266(13) 0.0269(14) 0.0125(11) 0.0019(11) 0.0094(11) C22 0.0228(14) 0.0477(19) 0.061(2) 0.0370(18) -0.0036(14) 0.0101(13) C23 0.0345(19) 0.0351(19) 0.075(3) 0.0094(19) 0.0043(18) 0.0070(15) C24 0.0315(18) 0.080(3) 0.045(2) 0.036(2) 0.0087(15) 0.0128(18) C25 0.055(2) 0.047(2) 0.0436(19) 0.0315(17) 0.0064(16) 0.0231(17) C26 0.191(7) 0.050(3) 0.070(4) 0.038(3) 0.008(4) 0.049(4) C27 0.130(5) 0.103(4) 0.060(3) 0.061(3) 0.045(3) 0.076(4) C28 0.0396(17) 0.0219(14) 0.0379(17) 0.0131(13) -0.0109(14) 0.0009(12) C29 0.081(3) 0.0279(17) 0.049(2) 0.0037(16) -0.021(2) 0.0160(19) C30 0.0351(19) 0.052(2) 0.072(3) 0.037(2) -0.0072(18) -0.0049(17) C31 0.0195(12) 0.0229(12) 0.0177(11) 0.0092(10) 0.0022(9) 0.0024(10) C32 0.0347(16) 0.0418(17) 0.0284(15) 0.0211(13) 0.0115(12) 0.0191(13) C33 0.049(2) 0.0466(19) 0.0349(17) 0.0286(15) 0.0138(15) 0.0222(16) C34 0.0403(18) 0.0486(19) 0.0341(16) 0.0291(15) 0.0126(14) 0.0084(15) C35 0.0322(16) 0.064(2) 0.048(2) 0.0397(19) 0.0214(15) 0.0181(16) C36 0.0253(14) 0.0467(17) 0.0378(16) 0.0292(15) 0.0119(12) 0.0146(13) C37 0.0160(11) 0.0193(12) 0.0218(12) 0.0049(10) 0.0039(9) 0.0046(9) C38 0.0234(13) 0.0200(12) 0.0233(13) 0.0055(10) 0.0053(10) 0.0068(10) C39 0.0342(16) 0.0246(14) 0.0306(15) 0.0101(12) 0.0089(12) 0.0027(12) C40 0.0305(15) 0.0252(14) 0.0349(16) 0.0051(12) 0.0070(13) -0.0047(12) C41 0.0232(14) 0.0321(15) 0.0297(15) 0.0046(12) -0.0004(12) -0.0029(12) C42 0.0196(12) 0.0245(13) 0.0221(13) 0.0029(10) 0.0023(10) 0.0050(10) C43 0.0249(13) 0.0239(12) 0.0231(13) 0.0098(10) 0.0035(10) 0.0080(10) C44 0.0364(16) 0.0312(15) 0.0232(14) 0.0083(12) 0.0047(12) 0.0100(13) C45 0.0440(18) 0.0318(15) 0.0322(16) 0.0158(13) 0.0059(13) 0.0178(14) C46 0.054(2) 0.0393(19) 0.042(2) 0.0121(16) 0.0050(17) -0.0194(17) C47 0.085(4) 0.033(2) 0.090(4) 0.027(2) 0.005(3) -0.008(2) C48 0.051(3) 0.062(3) 0.119(5) 0.019(3) 0.025(3) -0.015(2) C49 0.0250(14) 0.0319(15) 0.0205(13) 0.0052(11) -0.0025(11) 0.0024(11) C50 0.073(3) 0.041(2) 0.0225(16) -0.0002(15) 0.0011(17) -0.0069(19) C51 0.0374(19) 0.069(3) 0.048(2) 0.0306(19) 0.0018(16) 0.0241(18) C52 0.0198(12) 0.0261(13) 0.0136(11) 0.0052(10) 0.0015(9) 0.0024(10) C53 0.0292(15) 0.0423(17) 0.0222(13) 0.0137(12) 0.0092(11) 0.0148(13) C54 0.0343(17) 0.057(2) 0.0297(16) 0.0199(15) 0.0171(13) 0.0162(15) C55 0.0421(18) 0.0463(19) 0.0258(15) 0.0192(14) 0.0133(13) 0.0061(15) C56 0.0441(18) 0.0391(17) 0.0266(15) 0.0179(13) 0.0093(13) 0.0122(14) C57 0.0316(15) 0.0338(15) 0.0235(13) 0.0137(12) 0.0078(11) 0.0103(12) Cl1 0.0868(11) 0.1222(14) 0.0742(9) 0.0384(9) 0.0202(8) 0.0035(10) Cl2 0.0607(7) 0.0822(9) 0.1299(13) 0.0675(10) 0.0137(8) 0.0141(7) C58 0.057(3) 0.081(3) 0.072(3) 0.052(3) 0.009(2) 0.019(2) O7 0.117(6) 0.076(5) 0.131(7) 0.056(5) 0.040(5) 0.021(4) C59 0.072(6) 0.056(5) 0.097(7) 0.046(5) 0.020(5) 0.004(4) C60 0.082(7) 0.052(5) 0.093(8) 0.036(5) 0.001(6) -0.009(5) C61 0.137(9) 0.080(6) 0.098(7) 0.075(6) 0.009(6) 0.016(5) C62 0.126(10) 0.062(6) 0.143(10) 0.089(7) 0.016(8) 0.016(6) _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 Ir1 O2 2.1639(18) . ? Ir1 O4 2.1752(17) . ? Ir1 P1 2.2311(6) . ? Ir1 P2 2.2315(6) . ? Ir1 O6 2.2427(18) . ? Ir1 H1 1.4894 . ? S1 O3 1.4541(18) . ? S1 O2 1.4974(18) . ? S1 N1 1.554(2) . ? S1 C16 1.796(3) . ? S2 O5 1.439(2) . ? S2 O4 1.5093(18) . ? S2 N2 1.554(2) . ? S2 C37 1.792(3) . ? P1 N1 1.665(2) . ? P1 C31 1.815(3) . ? P1 C1 1.821(2) . ? P2 N2 1.656(2) . ? P2 C7 1.814(3) . ? P2 C52 1.817(3) . ? O1 C2 1.381(3) . ? O1 C8 1.386(3) . ? O6 H1O 0.8318 . ? O6 H2O 0.8509 . ? C1 C2 1.384(3) . ? C1 C6 1.401(3) . ? C2 C3 1.392(3) . ? C3 C4 1.394(4) . ? C3 C13 1.535(4) . ? C4 C5 1.392(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.384(4) . ? C7 C12 1.393(4) . ? C8 C9 1.384(4) . ? C9 C10 1.396(4) . ? C9 C13 1.525(4) . ? C10 C11 1.394(5) . ? C10 H10 0.9500 . ? C11 C12 1.386(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.528(4) . ? C13 C14 1.548(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.415(4) . ? C16 C17 1.416(4) . ? C17 C18 1.398(4) . ? C17 C22 1.527(4) . ? C18 C19 1.381(5) . ? C18 H18 0.9500 . ? C19 C20 1.389(5) . ? C19 C25 1.523(4) . ? C20 C21 1.393(4) . ? C20 H20 0.9500 . ? C21 C28 1.529(4) . ? C22 C23 1.514(6) . ? C22 C24 1.537(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.471(6) . ? C25 C27 1.487(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.528(6) . ? C28 C29 1.535(5) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.392(4) . ? C31 C32 1.395(4) . ? C32 C33 1.388(4) . ? C32 H32 0.9500 . ? C33 C34 1.387(5) . ? C33 H33 0.9500 . ? C34 C35 1.377(5) . ? C34 H34 0.9500 . ? C35 C36 1.393(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.415(4) . ? C37 C42 1.417(4) . ? C38 C39 1.391(4) . ? C38 C43 1.529(4) . ? C39 C40 1.396(5) . ? C39 H39 0.9500 . ? C40 C41 1.379(5) . ? C40 C46 1.526(4) . ? C41 C42 1.395(4) . ? C41 H41 0.9500 . ? C42 C49 1.528(4) . ? C43 C44 1.533(4) . ? C43 C45 1.537(4) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C48 1.525(8) . ? C46 C47 1.536(7) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51 1.528(5) . ? C49 C50 1.538(4) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C57 1.388(4) . ? C52 C53 1.390(4) . ? C53 C54 1.396(4) . ? C53 H53 0.9500 . ? C54 C55 1.374(5) . ? C54 H54 0.9500 . ? C55 C56 1.380(5) . ? C55 H55 0.9500 . ? C56 C57 1.389(4) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? Cl1 C58 1.743(6) . ? Cl2 C58 1.745(5) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? O7 C61 1.351(15) . ? O7 C59 1.460(15) . ? C59 C60 1.421(15) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.364(17) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? 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 O2 Ir1 O4 89.55(7) . . ? O2 Ir1 P1 83.16(5) . . ? O4 Ir1 P1 172.69(5) . . ? O2 Ir1 P2 171.53(5) . . ? O4 Ir1 P2 82.71(5) . . ? P1 Ir1 P2 104.54(2) . . ? O2 Ir1 O6 81.40(7) . . ? O4 Ir1 O6 82.68(7) . . ? P1 Ir1 O6 96.66(5) . . ? P2 Ir1 O6 100.93(5) . . ? O2 Ir1 H1 96.1 . . ? O4 Ir1 H1 93.5 . . ? P1 Ir1 H1 86.8 . . ? P2 Ir1 H1 81.0 . . ? O6 Ir1 H1 175.5 . . ? O3 S1 O2 111.56(11) . . ? O3 S1 N1 111.91(12) . . ? O2 S1 N1 110.91(11) . . ? O3 S1 C16 107.31(12) . . ? O2 S1 C16 108.40(12) . . ? N1 S1 C16 106.48(13) . . ? O5 S2 O4 110.30(12) . . ? O5 S2 N2 114.76(14) . . ? O4 S2 N2 111.31(11) . . ? O5 S2 C37 108.28(12) . . ? O4 S2 C37 106.79(11) . . ? N2 S2 C37 104.92(12) . . ? N1 P1 C31 105.95(12) . . ? N1 P1 C1 101.20(11) . . ? C31 P1 C1 104.80(12) . . ? N1 P1 Ir1 106.69(8) . . ? C31 P1 Ir1 118.42(9) . . ? C1 P1 Ir1 117.87(8) . . ? N2 P2 C7 103.35(12) . . ? N2 P2 C52 106.61(12) . . ? C7 P2 C52 105.64(12) . . ? N2 P2 Ir1 106.86(8) . . ? C7 P2 Ir1 115.96(9) . . ? C52 P2 Ir1 117.21(9) . . ? C2 O1 C8 113.19(19) . . ? S1 O2 Ir1 117.95(10) . . ? S2 O4 Ir1 111.27(10) . . ? Ir1 O6 H1O 141.0 . . ? Ir1 O6 H2O 107.7 . . ? H1O O6 H2O 102.8 . . ? S1 N1 P1 118.55(13) . . ? S2 N2 P2 115.39(14) . . ? C2 C1 C6 117.3(2) . . ? C2 C1 P1 119.65(18) . . ? C6 C1 P1 122.62(19) . . ? O1 C2 C1 115.7(2) . . ? O1 C2 C3 119.5(2) . . ? C1 C2 C3 124.7(2) . . ? C2 C3 C4 116.3(2) . . ? C2 C3 C13 118.0(2) . . ? C4 C3 C13 125.7(2) . . ? C5 C4 C3 120.6(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 121.4(2) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 119.5(2) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C8 C7 C12 117.8(3) . . ? C8 C7 P2 117.36(19) . . ? C12 C7 P2 124.5(2) . . ? C9 C8 C7 124.9(2) . . ? C9 C8 O1 120.1(2) . . ? C7 C8 O1 114.9(2) . . ? C8 C9 C10 115.7(3) . . ? C8 C9 C13 117.9(2) . . ? C10 C9 C13 126.3(3) . . ? C11 C10 C9 121.1(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C7 119.3(3) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? C9 C13 C15 111.7(2) . . ? C9 C13 C3 107.1(2) . . ? C15 C13 C3 111.4(2) . . ? C9 C13 C14 107.6(2) . . ? C15 C13 C14 110.2(2) . . ? C3 C13 C14 108.7(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 120.9(2) . . ? C21 C16 S1 115.8(2) . . ? C17 C16 S1 123.1(2) . . ? C18 C17 C16 116.8(3) . . ? C18 C17 C22 116.7(3) . . ? C16 C17 C22 126.3(3) . . ? C19 C18 C17 123.4(3) . . ? C19 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C18 C19 C20 117.9(3) . . ? C18 C19 C25 119.5(3) . . ? C20 C19 C25 122.6(3) . . ? C19 C20 C21 122.1(3) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 118.1(3) . . ? C20 C21 C28 117.0(3) . . ? C16 C21 C28 124.8(3) . . ? C23 C22 C17 112.8(3) . . ? C23 C22 C24 109.6(3) . . ? C17 C22 C24 109.5(3) . . ? C23 C22 H22 108.3 . . ? C17 C22 H22 108.3 . . ? C24 C22 H22 108.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 111.6(4) . . ? C26 C25 C19 113.8(3) . . ? C27 C25 C19 111.1(3) . . ? C26 C25 H25 106.6 . . ? C27 C25 H25 106.6 . . ? C19 C25 H25 106.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C21 112.4(3) . . ? C30 C28 C29 112.3(3) . . ? C21 C28 C29 108.8(3) . . ? C30 C28 H28 107.7 . . ? C21 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 119.1(3) . . ? C36 C31 P1 122.4(2) . . ? C32 C31 P1 118.5(2) . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 120.0(3) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.2(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 120.3(3) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C42 120.9(2) . . ? C38 C37 S2 120.0(2) . . ? C42 C37 S2 119.1(2) . . ? C39 C38 C37 117.8(3) . . ? C39 C38 C43 117.0(3) . . ? C37 C38 C43 125.1(2) . . ? C38 C39 C40 122.7(3) . . ? C38 C39 H39 118.7 . . ? C40 C39 H39 118.7 . . ? C41 C40 C39 117.5(3) . . ? C41 C40 C46 122.2(3) . . ? C39 C40 C46 120.1(3) . . ? C40 C41 C42 123.5(3) . . ? C40 C41 H41 118.3 . . ? C42 C41 H41 118.3 . . ? C41 C42 C37 117.3(3) . . ? C41 C42 C49 116.6(3) . . ? C37 C42 C49 126.2(3) . . ? C38 C43 C44 111.2(2) . . ? C38 C43 C45 111.6(2) . . ? C44 C43 C45 109.8(2) . . ? C38 C43 H43 108.0 . . ? C44 C43 H43 108.0 . . ? C45 C43 H43 108.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C48 C46 C40 113.7(4) . . ? C48 C46 C47 108.0(4) . . ? C40 C46 C47 109.2(4) . . ? C48 C46 H46 108.6 . . ? C40 C46 H46 108.6 . . ? C47 C46 H46 108.6 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C42 110.6(3) . . ? C51 C49 C50 110.9(3) . . ? C42 C49 C50 112.0(3) . . ? C51 C49 H49 107.7 . . ? C42 C49 H49 107.7 . . ? C50 C49 H49 107.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C57 C52 C53 119.4(3) . . ? C57 C52 P2 117.5(2) . . ? C53 C52 P2 123.1(2) . . ? C52 C53 C54 120.0(3) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0(3) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 120.5(3) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C55 C56 C57 119.9(3) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C52 C57 C56 120.3(3) . . ? C52 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? Cl1 C58 Cl2 111.4(3) . . ? Cl1 C58 H58A 109.4 . . ? Cl2 C58 H58A 109.4 . . ? Cl1 C58 H58B 109.4 . . ? Cl2 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C61 O7 C59 130.6(9) . . ? C60 C59 O7 125.1(9) . . ? C60 C59 H59A 106.0 . . ? O7 C59 H59A 106.0 . . ? C60 C59 H59B 106.0 . . ? O7 C59 H59B 106.0 . . ? H59A C59 H59B 106.3 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O7 C61 C62 132.1(10) . . ? O7 C61 H61A 104.2 . . ? C62 C61 H61A 104.2 . . ? O7 C61 H61B 104.2 . . ? C62 C61 H61B 104.2 . . ? H61A C61 H61B 105.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O2 Ir1 143.47(11) . . . . ? N1 S1 O2 Ir1 17.98(16) . . . . ? C16 S1 O2 Ir1 -98.58(13) . . . . ? O5 S2 O4 Ir1 89.18(13) . . . . ? N2 S2 O4 Ir1 -39.41(15) . . . . ? C37 S2 O4 Ir1 -153.38(11) . . . . ? O3 S1 N1 P1 -142.80(14) . . . . ? O2 S1 N1 P1 -17.51(19) . . . . ? C16 S1 N1 P1 100.23(16) . . . . ? C31 P1 N1 S1 -117.94(16) . . . . ? C1 P1 N1 S1 132.95(15) . . . . ? Ir1 P1 N1 S1 9.11(17) . . . . ? O5 S2 N2 P2 -96.24(17) . . . . ? O4 S2 N2 P2 29.92(19) . . . . ? C37 S2 N2 P2 145.06(15) . . . . ? C7 P2 N2 S2 -129.18(16) . . . . ? C52 P2 N2 S2 119.73(16) . . . . ? Ir1 P2 N2 S2 -6.36(17) . . . . ? N1 P1 C1 C2 -164.3(2) . . . . ? C31 P1 C1 C2 85.7(2) . . . . ? Ir1 P1 C1 C2 -48.5(2) . . . . ? N1 P1 C1 C6 8.1(2) . . . . ? C31 P1 C1 C6 -101.9(2) . . . . ? Ir1 P1 C1 C6 124.0(2) . . . . ? C8 O1 C2 C1 136.3(2) . . . . ? C8 O1 C2 C3 -41.7(3) . . . . ? C6 C1 C2 O1 175.6(2) . . . . ? P1 C1 C2 O1 -11.6(3) . . . . ? C6 C1 C2 C3 -6.5(4) . . . . ? P1 C1 C2 C3 166.3(2) . . . . ? O1 C2 C3 C4 -177.8(2) . . . . ? C1 C2 C3 C4 4.3(4) . . . . ? O1 C2 C3 C13 3.0(3) . . . . ? C1 C2 C3 C13 -174.9(2) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C13 C3 C4 C5 179.9(2) . . . . ? C3 C4 C5 C6 -3.4(4) . . . . ? C4 C5 C6 C1 1.2(4) . . . . ? C2 C1 C6 C5 3.5(4) . . . . ? P1 C1 C6 C5 -169.1(2) . . . . ? N2 P2 C7 C8 173.8(2) . . . . ? C52 P2 C7 C8 -74.4(2) . . . . ? Ir1 P2 C7 C8 57.2(2) . . . . ? N2 P2 C7 C12 0.6(3) . . . . ? C52 P2 C7 C12 112.4(3) . . . . ? Ir1 P2 C7 C12 -115.9(2) . . . . ? C12 C7 C8 C9 4.2(4) . . . . ? P2 C7 C8 C9 -169.4(2) . . . . ? C12 C7 C8 O1 -177.4(2) . . . . ? P2 C7 C8 O1 8.9(3) . . . . ? C2 O1 C8 C9 40.3(3) . . . . ? C2 O1 C8 C7 -138.2(2) . . . . ? C7 C8 C9 C10 -3.6(4) . . . . ? O1 C8 C9 C10 178.2(2) . . . . ? C7 C8 C9 C13 178.4(2) . . . . ? O1 C8 C9 C13 0.2(4) . . . . ? C8 C9 C10 C11 0.7(5) . . . . ? C13 C9 C10 C11 178.5(3) . . . . ? C9 C10 C11 C12 1.3(5) . . . . ? C10 C11 C12 C7 -0.7(5) . . . . ? C8 C7 C12 C11 -1.9(4) . . . . ? P2 C7 C12 C11 171.2(3) . . . . ? C8 C9 C13 C15 -157.6(3) . . . . ? C10 C9 C13 C15 24.6(4) . . . . ? C8 C9 C13 C3 -35.4(3) . . . . ? C10 C9 C13 C3 146.8(3) . . . . ? C8 C9 C13 C14 81.4(3) . . . . ? C10 C9 C13 C14 -96.4(3) . . . . ? C2 C3 C13 C9 33.9(3) . . . . ? C4 C3 C13 C9 -145.2(3) . . . . ? C2 C3 C13 C15 156.3(2) . . . . ? C4 C3 C13 C15 -22.8(4) . . . . ? C2 C3 C13 C14 -82.1(3) . . . . ? C4 C3 C13 C14 98.8(3) . . . . ? O3 S1 C16 C21 -75.1(2) . . . . ? O2 S1 C16 C21 164.3(2) . . . . ? N1 S1 C16 C21 44.9(2) . . . . ? O3 S1 C16 C17 110.2(2) . . . . ? O2 S1 C16 C17 -10.5(3) . . . . ? N1 S1 C16 C17 -129.8(2) . . . . ? C21 C16 C17 C18 -9.0(4) . . . . ? S1 C16 C17 C18 165.5(2) . . . . ? C21 C16 C17 C22 165.2(3) . . . . ? S1 C16 C17 C22 -20.3(4) . . . . ? C16 C17 C18 C19 1.9(5) . . . . ? C22 C17 C18 C19 -172.8(3) . . . . ? C17 C18 C19 C20 5.0(5) . . . . ? C17 C18 C19 C25 -175.5(3) . . . . ? C18 C19 C20 C21 -5.2(5) . . . . ? C25 C19 C20 C21 175.4(3) . . . . ? C19 C20 C21 C16 -1.6(5) . . . . ? C19 C20 C21 C28 175.4(3) . . . . ? C17 C16 C21 C20 8.9(4) . . . . ? S1 C16 C21 C20 -166.0(2) . . . . ? C17 C16 C21 C28 -167.9(3) . . . . ? S1 C16 C21 C28 17.2(4) . . . . ? C18 C17 C22 C23 -55.7(4) . . . . ? C16 C17 C22 C23 130.2(3) . . . . ? C18 C17 C22 C24 66.6(4) . . . . ? C16 C17 C22 C24 -107.5(3) . . . . ? C18 C19 C25 C26 -139.5(5) . . . . ? C20 C19 C25 C26 39.9(6) . . . . ? C18 C19 C25 C27 93.5(5) . . . . ? C20 C19 C25 C27 -87.1(5) . . . . ? C20 C21 C28 C30 62.5(4) . . . . ? C16 C21 C28 C30 -120.8(3) . . . . ? C20 C21 C28 C29 -62.5(4) . . . . ? C16 C21 C28 C29 114.3(4) . . . . ? N1 P1 C31 C36 -126.2(2) . . . . ? C1 P1 C31 C36 -19.7(3) . . . . ? Ir1 P1 C31 C36 114.1(2) . . . . ? N1 P1 C31 C32 52.8(2) . . . . ? C1 P1 C31 C32 159.4(2) . . . . ? Ir1 P1 C31 C32 -66.8(2) . . . . ? C36 C31 C32 C33 2.8(5) . . . . ? P1 C31 C32 C33 -176.3(3) . . . . ? C31 C32 C33 C34 -1.8(5) . . . . ? C32 C33 C34 C35 -0.4(6) . . . . ? C33 C34 C35 C36 1.5(6) . . . . ? C32 C31 C36 C35 -1.6(5) . . . . ? P1 C31 C36 C35 177.5(3) . . . . ? C34 C35 C36 C31 -0.5(6) . . . . ? O5 S2 C37 C38 155.2(2) . . . . ? O4 S2 C37 C38 36.4(2) . . . . ? N2 S2 C37 C38 -81.9(2) . . . . ? O5 S2 C37 C42 -25.0(2) . . . . ? O4 S2 C37 C42 -143.8(2) . . . . ? N2 S2 C37 C42 97.9(2) . . . . ? C42 C37 C38 C39 6.5(4) . . . . ? S2 C37 C38 C39 -173.7(2) . . . . ? C42 C37 C38 C43 -171.6(2) . . . . ? S2 C37 C38 C43 8.2(4) . . . . ? C37 C38 C39 C40 -2.9(4) . . . . ? C43 C38 C39 C40 175.4(3) . . . . ? C38 C39 C40 C41 -1.4(5) . . . . ? C38 C39 C40 C46 -176.9(3) . . . . ? C39 C40 C41 C42 2.2(5) . . . . ? C46 C40 C41 C42 177.6(3) . . . . ? C40 C41 C42 C37 1.3(5) . . . . ? C40 C41 C42 C49 -178.1(3) . . . . ? C38 C37 C42 C41 -5.8(4) . . . . ? S2 C37 C42 C41 174.4(2) . . . . ? C38 C37 C42 C49 173.5(3) . . . . ? S2 C37 C42 C49 -6.2(4) . . . . ? C39 C38 C43 C44 74.6(3) . . . . ? C37 C38 C43 C44 -107.3(3) . . . . ? C39 C38 C43 C45 -48.4(3) . . . . ? C37 C38 C43 C45 129.7(3) . . . . ? C41 C40 C46 C48 26.8(6) . . . . ? C39 C40 C46 C48 -158.0(4) . . . . ? C41 C40 C46 C47 -93.9(5) . . . . ? C39 C40 C46 C47 81.3(5) . . . . ? C41 C42 C49 C51 -78.3(3) . . . . ? C37 C42 C49 C51 102.4(3) . . . . ? C41 C42 C49 C50 46.0(4) . . . . ? C37 C42 C49 C50 -133.3(3) . . . . ? N2 P2 C52 C57 -64.0(2) . . . . ? C7 P2 C52 C57 -173.5(2) . . . . ? Ir1 P2 C52 C57 55.6(2) . . . . ? N2 P2 C52 C53 115.0(2) . . . . ? C7 P2 C52 C53 5.5(3) . . . . ? Ir1 P2 C52 C53 -125.4(2) . . . . ? C57 C52 C53 C54 -1.0(4) . . . . ? P2 C52 C53 C54 -180.0(2) . . . . ? C52 C53 C54 C55 0.5(5) . . . . ? C53 C54 C55 C56 0.4(5) . . . . ? C54 C55 C56 C57 -0.7(5) . . . . ? C53 C52 C57 C56 0.6(4) . . . . ? P2 C52 C57 C56 179.6(2) . . . . ? C55 C56 C57 C52 0.2(5) . . . . ? C61 O7 C59 C60 -179.8(15) . . . . ? C59 O7 C61 C62 -177.7(16) . . . . ? _refine_diff_density_max 3.458 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.106 _shelxl_version_number 2013-4 _shelx_res_file ; TITL l0612a CELL 0.71073 11.61063 17.26685 18.61611 113.198 95.475 105.211 ZERR 2 0.00025 0.00062 0.00042 0.002 0.002 0.001 LATT 1 SFAC C H Cl Ir N O P S UNIT 120 156 4 2 4 13 4 4 MERG 0 TEMP -123 L.S. 5 FMAP 2 PLAN -20 ACTA BOND $H CONF ISOR 0.01 O7 > C62 WGHT 0.053400 2.446400 BASF 0.12458 FVAR 0.25339 IR1 4 0.125517 0.085842 0.206541 11.00000 0.01243 0.01845 = 0.01321 0.00682 0.00036 0.00429 AFIX 1 H1 2 0.150900 0.053500 0.267700 11.00000 0.05000 AFIX 0 S1 8 0.083333 -0.106006 0.069775 11.00000 0.01617 0.01969 = 0.01523 0.00760 0.00161 0.00674 S2 8 0.352038 0.236162 0.327042 11.00000 0.01552 0.01944 = 0.01800 0.00705 -0.00196 0.00283 P1 7 -0.057520 -0.019990 0.162602 11.00000 0.01371 0.01948 = 0.01533 0.00760 0.00158 0.00458 P2 7 0.106505 0.196146 0.313961 11.00000 0.01566 0.02123 = 0.01384 0.00548 0.00117 0.00377 O1 6 -0.141141 0.133530 0.230991 11.00000 0.01887 0.01977 = 0.01551 0.00695 0.00184 0.00504 O2 6 0.172568 -0.013076 0.110506 11.00000 0.01727 0.01975 = 0.02008 0.00765 0.00371 0.00589 O3 6 0.079653 -0.147092 -0.015607 11.00000 0.02388 0.02723 = 0.01469 0.00780 0.00257 0.00864 O4 6 0.311769 0.176600 0.238064 11.00000 0.01489 0.01971 = 0.01821 0.00568 0.00163 0.00375 O5 6 0.407157 0.194569 0.367539 11.00000 0.03132 0.02441 = 0.03064 0.01136 -0.01164 0.00350 O6 6 0.102581 0.135735 0.113384 11.00000 0.02332 0.03344 = 0.02116 0.01638 0.00272 0.00988 AFIX 1 H1O 2 0.050100 0.145900 0.088000 11.00000 0.05000 H2O 2 0.141400 0.113800 0.078300 11.00000 0.05000 AFIX 0 N1 5 -0.045674 -0.107452 0.086351 11.00000 0.01589 0.02106 = 0.02188 0.00700 0.00306 0.00629 N2 5 0.246391 0.266911 0.361155 11.00000 0.01851 0.02727 = 0.01701 0.00415 0.00222 0.00091 C1 1 -0.184626 -0.000279 0.115474 11.00000 0.01256 0.02297 = 0.01609 0.00906 0.00236 0.00473 C2 1 -0.205664 0.080049 0.152699 11.00000 0.01284 0.02348 = 0.01628 0.00823 0.00275 0.00442 C3 1 -0.282585 0.110085 0.116020 11.00000 0.01554 0.02588 = 0.02146 0.01198 0.00616 0.00798 C4 1 -0.347950 0.051235 0.037938 11.00000 0.01596 0.03151 = 0.02275 0.01425 0.00226 0.00754 AFIX 43 H4 2 -0.401040 0.068673 0.009918 11.00000 -1.20000 AFIX 0 C5 1 -0.336142 -0.032890 0.000627 11.00000 0.01585 0.03098 = 0.01702 0.00812 -0.00072 0.00320 AFIX 43 H5 2 -0.384799 -0.073238 -0.051502 11.00000 -1.20000 AFIX 0 C6 1 -0.254821 -0.058996 0.037989 11.00000 0.01522 0.02293 = 0.01836 0.00660 0.00287 0.00519 AFIX 43 H6 2 -0.246783 -0.116219 0.011261 11.00000 -1.20000 AFIX 0 C7 1 0.026172 0.265009 0.293867 11.00000 0.01953 0.02174 = 0.01867 0.00642 0.00515 0.00667 C8 1 -0.091970 0.222569 0.247213 11.00000 0.02052 0.01944 = 0.01787 0.00731 0.00606 0.00632 C9 1 -0.159147 0.261866 0.215739 11.00000 0.02087 0.02459 = 0.02486 0.00930 0.00564 0.00955 C10 1 -0.103070 0.352427 0.237474 11.00000 0.03100 0.02671 = 0.04564 0.01754 0.00508 0.01240 AFIX 43 H10 2 -0.145266 0.383098 0.218150 11.00000 -1.20000 AFIX 0 C11 1 0.013808 0.398549 0.287059 11.00000 0.03615 0.02158 = 0.05154 0.01295 0.00562 0.00633 AFIX 43 H11 2 0.049330 0.460430 0.301904 11.00000 -1.20000 AFIX 0 C12 1 0.079028 0.355521 0.315049 11.00000 0.02541 0.02319 = 0.03346 0.00704 0.00248 0.00529 AFIX 43 H12 2 0.158986 0.387461 0.348351 11.00000 -1.20000 AFIX 0 C13 1 -0.287144 0.204336 0.163674 11.00000 0.02006 0.02928 = 0.02577 0.01371 0.00507 0.01230 C14 1 -0.375451 0.200721 0.220404 11.00000 0.02466 0.03652 = 0.03172 0.01144 0.01046 0.01536 AFIX 137 H14A 2 -0.349717 0.174068 0.254169 11.00000 -1.50000 H14B 2 -0.458812 0.164510 0.188526 11.00000 -1.50000 H14C 2 -0.373740 0.261295 0.254438 11.00000 -1.50000 AFIX 0 C15 1 -0.329176 0.241988 0.107992 11.00000 0.03181 0.03375 = 0.03801 0.01927 0.00300 0.01544 AFIX 137 H15A 2 -0.330219 0.302341 0.140060 11.00000 -1.50000 H15B 2 -0.411691 0.203693 0.075763 11.00000 -1.50000 H15C 2 -0.272566 0.244071 0.072450 11.00000 -1.50000 AFIX 0 C16 1 0.132803 -0.172212 0.112099 11.00000 0.02507 0.02577 = 0.02022 0.01224 0.00530 0.01296 C17 1 0.248708 -0.142234 0.164014 11.00000 0.02607 0.03125 = 0.03240 0.01735 0.00242 0.01269 C18 1 0.264420 -0.190770 0.206943 11.00000 0.03179 0.03754 = 0.03350 0.01851 -0.00358 0.01310 AFIX 43 H18 2 0.340572 -0.170830 0.243395 11.00000 -1.20000 AFIX 0 C19 1 0.175000 -0.266202 0.199124 11.00000 0.04474 0.03533 = 0.02979 0.01862 0.00497 0.01961 C20 1 0.067664 -0.299016 0.141166 11.00000 0.03832 0.02816 = 0.03733 0.01924 0.00343 0.00937 AFIX 43 H20 2 0.008157 -0.353558 0.131963 11.00000 -1.20000 AFIX 0 C21 1 0.044504 -0.254482 0.096103 11.00000 0.02861 0.02656 = 0.02690 0.01254 0.00188 0.00942 C22 1 0.361568 -0.067347 0.172072 11.00000 0.02284 0.04770 = 0.06096 0.03696 -0.00359 0.01009 AFIX 13 H22 2 0.336103 -0.035307 0.142185 11.00000 -1.20000 AFIX 0 C23 1 0.419443 -0.000311 0.258342 11.00000 0.03450 0.03509 = 0.07491 0.00941 0.00427 0.00698 AFIX 137 H23A 2 0.360010 0.027196 0.281956 11.00000 -1.50000 H23B 2 0.491454 0.045908 0.260152 11.00000 -1.50000 H23C 2 0.444329 -0.030645 0.288763 11.00000 -1.50000 AFIX 0 C24 1 0.456409 -0.107444 0.133684 11.00000 0.03149 0.08048 = 0.04511 0.03611 0.00865 0.01280 AFIX 137 H24A 2 0.488669 -0.133919 0.165481 11.00000 -1.50000 H24B 2 0.523644 -0.060397 0.132118 11.00000 -1.50000 H24C 2 0.417375 -0.153577 0.078981 11.00000 -1.50000 AFIX 0 C25 1 0.197436 -0.310504 0.253022 11.00000 0.05549 0.04666 = 0.04357 0.03149 0.00635 0.02312 AFIX 13 H25 2 0.288234 -0.291624 0.271930 11.00000 -1.20000 AFIX 0 C26 1 0.153534 -0.408557 0.211529 11.00000 0.19113 0.05026 = 0.06997 0.03766 0.00847 0.04851 AFIX 137 H26A 2 0.198804 -0.431955 0.240543 11.00000 -1.50000 H26B 2 0.166579 -0.428002 0.156798 11.00000 -1.50000 H26C 2 0.065978 -0.431025 0.209606 11.00000 -1.50000 AFIX 0 C27 1 0.147700 -0.277080 0.325790 11.00000 0.12965 0.10310 = 0.06027 0.06090 0.04512 0.07604 AFIX 137 H27A 2 0.058003 -0.300023 0.310761 11.00000 -1.50000 H27B 2 0.175559 -0.211738 0.350465 11.00000 -1.50000 H27C 2 0.176751 -0.297442 0.364116 11.00000 -1.50000 AFIX 0 C28 1 -0.072335 -0.301012 0.029810 11.00000 0.03957 0.02189 = 0.03795 0.01311 -0.01085 0.00085 AFIX 13 H28 2 -0.075509 -0.261816 0.002446 11.00000 -1.20000 AFIX 0 C29 1 -0.064236 -0.388763 -0.032238 11.00000 0.08126 0.02791 = 0.04858 0.00368 -0.02150 0.01595 AFIX 137 H29A 2 0.006480 -0.375988 -0.055590 11.00000 -1.50000 H29B 2 -0.139229 -0.419562 -0.074705 11.00000 -1.50000 H29C 2 -0.054789 -0.426773 -0.006038 11.00000 -1.50000 AFIX 0 C30 1 -0.187961 -0.315183 0.062561 11.00000 0.03512 0.05173 = 0.07178 0.03669 -0.00725 -0.00487 AFIX 137 H30A 2 -0.187673 -0.354021 0.089266 11.00000 -1.50000 H30B 2 -0.260335 -0.343102 0.018271 11.00000 -1.50000 H30C 2 -0.190024 -0.257515 0.101148 11.00000 -1.50000 AFIX 0 C31 1 -0.118367 -0.061897 0.231352 11.00000 0.01945 0.02290 = 0.01772 0.00920 0.00218 0.00236 C32 1 -0.058994 -0.110051 0.257035 11.00000 0.03466 0.04179 = 0.02843 0.02107 0.01154 0.01909 AFIX 43 H32 2 0.014268 -0.117215 0.241002 11.00000 -1.20000 AFIX 0 C33 1 -0.106660 -0.147517 0.305942 11.00000 0.04925 0.04656 = 0.03489 0.02858 0.01378 0.02217 AFIX 43 H33 2 -0.067246 -0.181709 0.322025 11.00000 -1.20000 AFIX 0 C34 1 -0.211662 -0.135187 0.331403 11.00000 0.04034 0.04857 = 0.03405 0.02910 0.01265 0.00844 AFIX 43 H34 2 -0.244339 -0.161199 0.364629 11.00000 -1.20000 AFIX 0 C35 1 -0.268563 -0.085238 0.308521 11.00000 0.03217 0.06422 = 0.04840 0.03975 0.02137 0.01810 AFIX 43 H35 2 -0.339344 -0.075642 0.327064 11.00000 -1.20000 AFIX 0 C36 1 -0.222627 -0.048755 0.258276 11.00000 0.02527 0.04670 = 0.03779 0.02916 0.01193 0.01459 AFIX 43 H36 2 -0.262598 -0.014758 0.242304 11.00000 -1.20000 AFIX 0 C37 1 0.466129 0.336306 0.339992 11.00000 0.01598 0.01934 = 0.02182 0.00488 0.00386 0.00460 C38 1 0.455156 0.371467 0.283637 11.00000 0.02338 0.02002 = 0.02333 0.00553 0.00527 0.00680 C39 1 0.551938 0.444054 0.291735 11.00000 0.03418 0.02461 = 0.03056 0.01015 0.00892 0.00274 AFIX 43 H39 2 0.547393 0.466549 0.252854 11.00000 -1.20000 AFIX 0 C40 1 0.655427 0.485170 0.354646 11.00000 0.03046 0.02521 = 0.03488 0.00512 0.00702 -0.00474 C41 1 0.658615 0.452531 0.411259 11.00000 0.02324 0.03206 = 0.02969 0.00457 -0.00043 -0.00287 AFIX 43 H41 2 0.727266 0.481364 0.455379 11.00000 -1.20000 AFIX 0 C42 1 0.566364 0.379404 0.407184 11.00000 0.01956 0.02452 = 0.02214 0.00294 0.00228 0.00500 C43 1 0.343316 0.337701 0.215585 11.00000 0.02488 0.02387 = 0.02311 0.00981 0.00351 0.00805 AFIX 13 H43 2 0.274983 0.295899 0.224655 11.00000 -1.20000 AFIX 0 C44 1 0.369403 0.286229 0.134067 11.00000 0.03643 0.03124 = 0.02317 0.00833 0.00468 0.00997 AFIX 137 H44A 2 0.439399 0.324957 0.125300 11.00000 -1.50000 H44B 2 0.297235 0.266980 0.091490 11.00000 -1.50000 H44C 2 0.388249 0.233851 0.133310 11.00000 -1.50000 AFIX 0 C45 1 0.300966 0.414445 0.214358 11.00000 0.04400 0.03175 = 0.03220 0.01580 0.00585 0.01778 AFIX 137 H45A 2 0.358130 0.448740 0.193721 11.00000 -1.50000 H45B 2 0.298892 0.453531 0.268903 11.00000 -1.50000 H45C 2 0.218872 0.390004 0.179670 11.00000 -1.50000 AFIX 0 C46 1 0.755484 0.567525 0.362495 11.00000 0.05363 0.03930 = 0.04212 0.01208 0.00498 -0.01939 AFIX 13 H46 2 0.764577 0.560330 0.307555 11.00000 -1.20000 AFIX 0 C47 1 0.717147 0.650292 0.403095 11.00000 0.08533 0.03266 = 0.08976 0.02699 0.00530 -0.00814 AFIX 137 H47A 2 0.635431 0.640153 0.374273 11.00000 -1.50000 H47B 2 0.775988 0.702049 0.402125 11.00000 -1.50000 H47C 2 0.715560 0.661486 0.458792 11.00000 -1.50000 AFIX 0 C48 1 0.879710 0.583680 0.411447 11.00000 0.05131 0.06162 = 0.11884 0.01867 0.02540 -0.01502 AFIX 137 H48A 2 0.875927 0.601699 0.467866 11.00000 -1.50000 H48B 2 0.942260 0.631020 0.406736 11.00000 -1.50000 H48C 2 0.900759 0.528702 0.391191 11.00000 -1.50000 AFIX 0 C49 1 0.582722 0.354008 0.476492 11.00000 0.02502 0.03189 = 0.02049 0.00515 -0.00255 0.00241 AFIX 13 H49 2 0.501778 0.313295 0.474093 11.00000 -1.20000 AFIX 0 C50 1 0.621689 0.435797 0.558514 11.00000 0.07286 0.04054 = 0.02250 -0.00018 0.00113 -0.00690 AFIX 137 H50A 2 0.616045 0.415994 0.601070 11.00000 -1.50000 H50B 2 0.567545 0.471312 0.560705 11.00000 -1.50000 H50C 2 0.706309 0.472207 0.566039 11.00000 -1.50000 AFIX 0 C51 1 0.673958 0.302969 0.467161 11.00000 0.03737 0.06939 = 0.04767 0.03058 0.00181 0.02407 AFIX 137 H51A 2 0.753427 0.340493 0.466930 11.00000 -1.50000 H51B 2 0.643740 0.248508 0.416574 11.00000 -1.50000 H51C 2 0.683241 0.287163 0.511994 11.00000 -1.50000 AFIX 0 C52 1 0.038623 0.166454 0.387444 11.00000 0.01980 0.02612 = 0.01361 0.00515 0.00154 0.00237 C53 1 -0.062026 0.188351 0.412988 11.00000 0.02915 0.04235 = 0.02224 0.01367 0.00916 0.01479 AFIX 43 H53 2 -0.098639 0.220306 0.391836 11.00000 -1.20000 AFIX 0 C54 1 -0.109319 0.163390 0.469725 11.00000 0.03432 0.05749 = 0.02967 0.01988 0.01707 0.01624 AFIX 43 H54 2 -0.178528 0.177938 0.486883 11.00000 -1.20000 AFIX 0 C55 1 -0.055748 0.117760 0.500769 11.00000 0.04208 0.04629 = 0.02580 0.01920 0.01325 0.00609 AFIX 43 H55 2 -0.088463 0.100558 0.539140 11.00000 -1.20000 AFIX 0 C56 1 0.045280 0.096754 0.476571 11.00000 0.04406 0.03915 = 0.02659 0.01790 0.00930 0.01219 AFIX 43 H56 2 0.082511 0.065825 0.498711 11.00000 -1.20000 AFIX 0 C57 1 0.092383 0.120942 0.419775 11.00000 0.03161 0.03382 = 0.02347 0.01370 0.00780 0.01032 AFIX 43 H57 2 0.161710 0.106272 0.402976 11.00000 -1.20000 AFIX 0 CL1 3 0.495186 0.184748 0.582080 11.00000 0.08682 0.12218 = 0.07425 0.03840 0.02015 0.00353 CL2 3 0.334535 0.011564 0.466124 11.00000 0.06075 0.08220 = 0.12991 0.06748 0.01375 0.01412 C58 1 0.457554 0.104771 0.482665 11.00000 0.05683 0.08091 = 0.07225 0.05151 0.00889 0.01884 AFIX 23 H58A 2 0.529486 0.086149 0.469334 11.00000 -1.20000 H58B 2 0.436127 0.131177 0.446902 11.00000 -1.20000 AFIX 0 O7 6 0.407788 0.600082 0.056777 10.50000 0.11662 0.07576 = 0.13145 0.05613 0.04037 0.02145 C59 1 0.499064 0.663010 0.130530 10.50000 0.07231 0.05550 = 0.09727 0.04568 0.01963 0.00442 AFIX 23 H59A 2 0.571555 0.689634 0.113633 10.50000 -1.20000 H59B 2 0.465783 0.711583 0.157495 10.50000 -1.20000 AFIX 0 C60 1 0.544664 0.641345 0.191208 10.50000 0.08188 0.05174 = 0.09252 0.03626 0.00064 -0.00894 AFIX 33 H60A 2 0.604215 0.695114 0.234750 10.50000 -1.50000 H60B 2 0.584514 0.596478 0.168497 10.50000 -1.50000 H60C 2 0.476714 0.617501 0.212225 10.50000 -1.50000 AFIX 0 C61 1 0.357863 0.612331 -0.004859 10.50000 0.13658 0.08003 = 0.09816 0.07451 0.00943 0.01602 AFIX 23 H61A 2 0.429040 0.636507 -0.024159 10.50000 -1.20000 H61B 2 0.327069 0.662604 0.021078 10.50000 -1.20000 AFIX 0 C62 1 0.270154 0.555915 -0.073214 10.50000 0.12624 0.06194 = 0.14326 0.08877 0.01598 0.01579 AFIX 33 H62A 2 0.254271 0.588884 -0.103371 10.50000 -1.50000 H62B 2 0.194593 0.530683 -0.059189 10.50000 -1.50000 H62C 2 0.298588 0.507647 -0.106187 10.50000 -1.50000 AFIX 0 HKLF 5 REM l0612a REM R1 = 0.0273 for 14073 Fo > 4sig(Fo) and 0.0293 for all 14853 data REM 718 parameters refined using 30 restraints END WGHT 0.0534 2.4456 REM Highest difference peak 3.458, deepest hole -1.141, 1-sigma level 0.106 Q1 1 0.0825 0.1170 0.1966 11.00000 0.05 3.46 Q2 1 0.1631 0.0468 0.2132 11.00000 0.05 3.11 Q3 1 0.1666 0.1447 0.2371 11.00000 0.05 1.17 Q4 1 0.0606 0.2283 0.2996 11.00000 0.05 1.05 Q5 1 0.7789 0.5688 0.2768 11.00000 0.05 1.05 Q6 1 0.4354 0.6345 0.0220 11.00000 0.05 1.02 Q7 1 0.1201 -0.1434 0.0828 11.00000 0.05 0.87 Q8 1 0.5213 0.6345 0.0968 11.00000 0.05 0.84 Q9 1 0.2228 0.5351 -0.1001 11.00000 0.05 0.82 Q10 1 0.2628 0.5990 -0.0122 11.00000 0.05 0.81 Q11 1 0.2734 -0.3595 0.2377 11.00000 0.05 0.78 Q12 1 0.3782 0.5843 -0.0352 11.00000 0.05 0.78 Q13 1 0.4271 0.1488 0.5386 11.00000 0.05 0.71 Q14 1 0.5177 0.6828 0.1647 11.00000 0.05 0.65 Q15 1 -0.1082 0.0058 0.1472 11.00000 0.05 0.64 Q16 1 0.2996 0.2612 0.3186 11.00000 0.05 0.62 Q17 1 0.4975 0.6822 0.1125 11.00000 0.05 0.56 Q18 1 0.3757 0.2026 0.3363 11.00000 0.05 0.56 Q19 1 0.5065 0.6111 0.1681 11.00000 0.05 0.53 Q20 1 0.1375 -0.0560 0.0916 11.00000 0.05 0.49 ; _shelx_res_checksum 25091 _database_code_depnum_ccdc_archive 'CCDC 1020151'