data_f _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Cl2 N6 Ni O8' _chemical_formula_weight 656.12 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' 'O' 'O' 0.0106 0.0060 '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system tetragonal _space_group_IT_number 114 _space_group_name_H-M_alt 'P -4 21 c' _space_group_name_Hall 'P -4 2n' _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' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 13.6483(5) _cell_length_b 13.6483(5) _cell_length_c 14.6410(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2727.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 512 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 26.90 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_F_000 1352 _exptl_transmission_factor_min 0.6793 _exptl_transmission_factor_max 0.7458 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.967 _shelx_estimated_absorpt_T_min 0.801 _shelx_estimated_absorpt_T_max 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46739 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.110 _diffrn_reflns_theta_max 29.172 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3693 _reflns_number_gt 3289 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.791 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 1.000 _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. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _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^)+(0.0281P)^2^+1.4319P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1347 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.008(6) _chemical_absolute_configuration ? _refine_ls_number_reflns 3693 _refine_ls_number_parameters 206 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.038 _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 Ni Ni 0.5000 0.0000 0.51035(3) 0.01321(10) Uani 1 2 d S T P . . N1 N 0.60705(16) 0.11129(16) 0.52225(16) 0.0170(4) Uani 1 1 d D . . . . H1A H 0.6559(18) 0.091(2) 0.5627(18) 0.019(8) Uiso 1 1 d D . . . . H1B H 0.639(3) 0.122(3) 0.4662(16) 0.047(12) Uiso 1 1 d D . . . . C2 C 0.5646(2) 0.19863(19) 0.56195(19) 0.0185(5) Uani 1 1 d . . . . . C3 C 0.6137(2) 0.2878(2) 0.5612(2) 0.0279(6) Uani 1 1 d . . . . . H3 H 0.6760 0.2932 0.5328 0.033 Uiso 1 1 calc R U . . . C4 C 0.5713(3) 0.3691(2) 0.6022(3) 0.0378(8) Uani 1 1 d . . . . . H4 H 0.6045 0.4303 0.6015 0.045 Uiso 1 1 calc R U . . . C5 C 0.4807(2) 0.3612(2) 0.6439(2) 0.0349(8) Uani 1 1 d . . . . . H5 H 0.4525 0.4167 0.6729 0.042 Uiso 1 1 calc R U . . . C6 C 0.4308(2) 0.2728(2) 0.6438(2) 0.0243(6) Uani 1 1 d . . . . . H6 H 0.3681 0.2679 0.6717 0.029 Uiso 1 1 calc R U . . . C7 C 0.47315(19) 0.19130(19) 0.60262(18) 0.0170(5) Uani 1 1 d . . . . . N8 N 0.42226(16) 0.09699(17) 0.59938(15) 0.0155(4) Uani 1 1 d D . . . . H8 H 0.420(2) 0.072(2) 0.6595(11) 0.018(8) Uiso 1 1 d D . . . . C9 C 0.32550(19) 0.10438(19) 0.55904(17) 0.0169(5) Uani 1 1 d . . . . . C10 C 0.2411(2) 0.1171(2) 0.6106(2) 0.0240(6) Uani 1 1 d . . . . . H10 H 0.2448 0.1215 0.6753 0.029 Uiso 1 1 calc R U . . . C11 C 0.1508(2) 0.1234(2) 0.5663(2) 0.0291(7) Uani 1 1 d . . . . . H11 H 0.0926 0.1321 0.6010 0.035 Uiso 1 1 calc R U . . . C12 C 0.1456(2) 0.1170(2) 0.4721(2) 0.0297(7) Uani 1 1 d . . . . . H12 H 0.0840 0.1222 0.4423 0.036 Uiso 1 1 calc R U . . . C13 C 0.2297(2) 0.1031(2) 0.4210(2) 0.0246(6) Uani 1 1 d . . . . . H13 H 0.2257 0.0978 0.3564 0.030 Uiso 1 1 calc R U . . . C14 C 0.3198(2) 0.0969(2) 0.46422(17) 0.0190(5) Uani 1 1 d . . . . . N15 N 0.41044(18) 0.07678(18) 0.41653(15) 0.0192(5) Uani 1 1 d D . . . . H15A H 0.402(3) 0.044(2) 0.3612(14) 0.029(9) Uiso 1 1 d D . . . . H15B H 0.440(3) 0.1351(17) 0.398(3) 0.043(11) Uiso 1 1 d D . . . . Cl Cl 0.59828(5) 0.17995(5) 0.27671(4) 0.02344(15) Uani 1 1 d . . . . . O101 O 0.54716(16) 0.09317(17) 0.24787(17) 0.0350(5) Uani 1 1 d . . . . . O102 O 0.6233(2) 0.23707(19) 0.19840(16) 0.0489(7) Uani 1 1 d . . . . . O103 O 0.5346(2) 0.23540(18) 0.33570(18) 0.0497(8) Uani 1 1 d . . . . . O104 O 0.6822(2) 0.1517(3) 0.32668(19) 0.0655(10) 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 Ni 0.0133(2) 0.0121(2) 0.01426(18) 0.000 0.000 0.00156(17) N1 0.0149(11) 0.0159(11) 0.0201(10) -0.0003(9) 0.0008(9) 0.0017(8) C2 0.0193(13) 0.0154(13) 0.0207(13) -0.0015(10) -0.0047(10) 0.0025(10) C3 0.0219(15) 0.0204(14) 0.0413(17) 0.0007(12) -0.0023(13) -0.0037(11) C4 0.0365(19) 0.0151(15) 0.062(2) -0.0048(15) -0.0036(17) -0.0034(13) C5 0.037(2) 0.0157(14) 0.0524(19) -0.0107(13) -0.0047(15) 0.0063(13) C6 0.0252(15) 0.0190(14) 0.0287(15) -0.0040(11) -0.0028(12) 0.0055(11) C7 0.0186(13) 0.0141(12) 0.0185(11) 0.0005(10) -0.0046(9) 0.0025(9) N8 0.0152(11) 0.0145(10) 0.0166(10) 0.0011(8) 0.0003(8) 0.0024(9) C9 0.0144(12) 0.0113(12) 0.0251(13) 0.0025(10) -0.0035(10) 0.0009(10) C10 0.0227(15) 0.0161(14) 0.0331(15) -0.0017(11) 0.0044(12) 0.0027(11) C11 0.0178(14) 0.0198(14) 0.0495(19) -0.0035(14) 0.0063(13) 0.0022(11) C12 0.0171(14) 0.0197(14) 0.052(2) 0.0032(13) -0.0087(13) 0.0018(11) C13 0.0237(15) 0.0194(14) 0.0307(15) 0.0063(12) -0.0087(12) 0.0006(11) C14 0.0185(13) 0.0141(12) 0.0246(13) 0.0038(10) -0.0015(10) 0.0022(11) N15 0.0200(12) 0.0207(12) 0.0167(11) 0.0027(9) -0.0009(9) 0.0012(9) Cl 0.0287(3) 0.0252(3) 0.0165(3) -0.0005(3) 0.0006(3) -0.0109(3) O101 0.0321(12) 0.0341(12) 0.0389(12) -0.0119(11) -0.0023(10) -0.0113(9) O102 0.077(2) 0.0372(14) 0.0324(12) 0.0066(11) 0.0215(13) -0.0115(13) O103 0.082(2) 0.0260(13) 0.0415(14) -0.0085(11) 0.0310(14) -0.0092(13) O104 0.0267(13) 0.128(3) 0.0416(15) 0.0160(17) -0.0135(12) -0.0121(16) _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 Ni N1 2.115(2) . ? Ni N1 2.115(2) 2_655 ? Ni N15 2.116(2) 2_655 ? Ni N15 2.116(2) . ? Ni N8 2.139(2) . ? Ni N8 2.140(2) 2_655 ? N1 C2 1.447(3) . ? N1 H1A 0.935(13) . ? N1 H1B 0.941(13) . ? C2 C7 1.386(4) . ? C2 C3 1.390(4) . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.383(5) . ? C4 H4 0.9500 . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 C7 1.391(4) . ? C6 H6 0.9500 . ? C7 N8 1.463(3) . ? N8 C9 1.450(3) . ? N8 H8 0.944(13) . ? C9 C10 1.388(4) . ? C9 C14 1.394(3) . ? C10 C11 1.395(4) . ? C10 H10 0.9500 . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 N15 1.447(4) . ? N15 H15A 0.933(13) . ? N15 H15B 0.933(13) . ? Cl O104 1.412(3) . ? Cl O102 1.428(2) . ? Cl O101 1.438(2) . ? Cl O103 1.440(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 Ni N1 170.55(13) . 2_655 ? N1 Ni N15 90.58(9) . 2_655 ? N1 Ni N15 95.56(9) 2_655 2_655 ? N1 Ni N15 95.56(9) . . ? N1 Ni N15 90.58(9) 2_655 . ? N15 Ni N15 99.06(13) 2_655 . ? N1 Ni N8 81.26(9) . . ? N1 Ni N8 92.96(9) 2_655 . ? N15 Ni N8 171.21(9) 2_655 . ? N15 Ni N8 78.62(8) . . ? N1 Ni N8 92.96(9) . 2_655 ? N1 Ni N8 81.26(9) 2_655 2_655 ? N15 Ni N8 78.62(8) 2_655 2_655 ? N15 Ni N8 171.21(9) . 2_655 ? N8 Ni N8 104.93(12) . 2_655 ? C2 N1 Ni 110.37(16) . . ? C2 N1 H1A 106(2) . . ? Ni N1 H1A 109(2) . . ? C2 N1 H1B 114(3) . . ? Ni N1 H1B 111(3) . . ? H1A N1 H1B 106(3) . . ? C7 C2 C3 120.0(3) . . ? C7 C2 N1 118.3(2) . . ? C3 C2 N1 121.7(3) . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 119.5(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 120.2(3) . . ? C2 C7 N8 118.5(2) . . ? C6 C7 N8 121.3(2) . . ? C9 N8 C7 112.6(2) . . ? C9 N8 Ni 104.27(16) . . ? C7 N8 Ni 109.18(16) . . ? C9 N8 H8 112(2) . . ? C7 N8 H8 107.7(19) . . ? Ni N8 H8 111(2) . . ? C10 C9 C14 120.3(3) . . ? C10 C9 N8 122.9(2) . . ? C14 C9 N8 116.8(2) . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C9 120.0(3) . . ? C13 C14 N15 123.4(2) . . ? C9 C14 N15 116.6(2) . . ? C14 N15 Ni 105.93(16) . . ? C14 N15 H15A 114(2) . . ? Ni N15 H15A 113(2) . . ? C14 N15 H15B 110(2) . . ? Ni N15 H15B 112(2) . . ? H15A N15 H15B 102(3) . . ? O104 Cl O102 111.78(18) . . ? O104 Cl O101 108.71(19) . . ? O102 Cl O101 109.27(15) . . ? O104 Cl O103 108.78(19) . . ? O102 Cl O103 109.80(16) . . ? O101 Cl O103 108.43(15) . . ? _refine_diff_density_max 0.556 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.055 _shelxl_version_number 2013-4 _shelx_res_file ; TITL f.res in P-42(1)c d=40mm t=5s CELL 0.71073 13.6483 13.6483 14.6410 90.000 90.000 90.000 ZERR 4 0.0005 0.0005 0.0008 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM Y, -X, -Z SYMM -Y, X, -Z SYMM 1/2-X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, 1/2-Z SYMM 1/2-Y, 1/2-X, 1/2+Z SYMM 1/2+Y, 1/2+X, 1/2+Z SFAC C H N O CL NI UNIT 96 104 24 32 8 4 TEMP -123.160 SIZE 0.050 0.120 0.240 acta L.S. 200 BOND BOND $H HTAB FMAP 2 PLAN 20 WGHT 0.028100 1.431900 FVAR 0.32054 NI 6 0.500000 0.000000 0.510352 10.50000 0.01325 0.01212 = 0.01426 0.00000 0.00000 0.00156 dfix 0.95 0.01 N1 H1a N1 H1b N1 3 0.607053 0.111295 0.522251 11.00000 0.01488 0.01587 = 0.02012 -0.00026 0.00080 0.00168 H1A 2 0.655949 0.090628 0.562657 11.00000 0.01904 H1B 2 0.638976 0.122232 0.466219 11.00000 0.04736 C2 1 0.564595 0.198634 0.561948 11.00000 0.01930 0.01538 = 0.02068 -0.00150 -0.00471 0.00247 C3 1 0.613669 0.287844 0.561225 11.00000 0.02188 0.02040 = 0.04132 0.00073 -0.00229 -0.00369 AFIX 43 H3 2 0.676016 0.293156 0.532805 11.00000 -1.20000 AFIX 0 C4 1 0.571274 0.369102 0.602156 11.00000 0.03650 0.01514 = 0.06186 -0.00483 -0.00357 -0.00344 AFIX 43 H4 2 0.604464 0.430280 0.601493 11.00000 -1.20000 AFIX 0 C5 1 0.480711 0.361159 0.643945 11.00000 0.03671 0.01567 = 0.05243 -0.01070 -0.00466 0.00631 AFIX 43 H5 2 0.452548 0.416706 0.672922 11.00000 -1.20000 AFIX 0 C6 1 0.430816 0.272795 0.643833 11.00000 0.02523 0.01896 = 0.02870 -0.00398 -0.00279 0.00551 AFIX 43 H6 2 0.368147 0.267876 0.671696 11.00000 -1.20000 AFIX 0 C7 1 0.473150 0.191304 0.602620 11.00000 0.01857 0.01411 = 0.01847 0.00054 -0.00456 0.00254 dfix 0.95 0.01 N8 H8 N8 3 0.422259 0.096991 0.599383 11.00000 0.01523 0.01452 = 0.01660 0.00109 0.00029 0.00238 H8 2 0.419979 0.071968 0.659472 11.00000 0.01833 C9 1 0.325497 0.104385 0.559041 11.00000 0.01441 0.01126 = 0.02514 0.00254 -0.00346 0.00093 C10 1 0.241091 0.117105 0.610636 11.00000 0.02271 0.01614 = 0.03312 -0.00169 0.00436 0.00266 AFIX 43 H10 2 0.244768 0.121461 0.675304 11.00000 -1.20000 AFIX 0 C11 1 0.150822 0.123409 0.566330 11.00000 0.01780 0.01983 = 0.04952 -0.00354 0.00626 0.00219 AFIX 43 H11 2 0.092634 0.132145 0.600994 11.00000 -1.20000 AFIX 0 C12 1 0.145634 0.116994 0.472093 11.00000 0.01710 0.01967 = 0.05235 0.00321 -0.00872 0.00178 AFIX 43 H12 2 0.083991 0.122172 0.442346 11.00000 -1.20000 AFIX 0 C13 1 0.229744 0.103086 0.421040 11.00000 0.02370 0.01942 = 0.03066 0.00633 -0.00866 0.00057 AFIX 43 H13 2 0.225745 0.097790 0.356449 11.00000 -1.20000 AFIX 0 C14 1 0.319820 0.096891 0.464224 11.00000 0.01851 0.01408 = 0.02455 0.00385 -0.00150 0.00217 dfix 0.95 0.01 n15 H15a N15 H15b N15 3 0.410445 0.076781 0.416526 11.00000 0.02002 0.02071 = 0.01672 0.00266 -0.00091 0.00122 H15A 2 0.402162 0.043792 0.361219 11.00000 0.02917 H15B 2 0.439750 0.135141 0.397717 11.00000 0.04282 mole 2 CL 5 0.598278 0.179946 0.276707 11.00000 0.02870 0.02519 = 0.01645 -0.00049 0.00061 -0.01087 O101 4 0.547155 0.093169 0.247873 11.00000 0.03206 0.03412 = 0.03888 -0.01192 -0.00232 -0.01131 O102 4 0.623287 0.237071 0.198403 11.00000 0.07716 0.03724 = 0.03238 0.00656 0.02152 -0.01149 O103 4 0.534613 0.235404 0.335700 11.00000 0.08151 0.02605 = 0.04147 -0.00849 0.03105 -0.00921 O104 4 0.682170 0.151715 0.326676 11.00000 0.02674 0.12820 = 0.04162 0.01605 -0.01354 -0.01214 HKLF 4 REM f.res in P-42(1)c d=40mm t=5s REM R1 = 0.0292 for 3289 Fo > 4sig(Fo) and 0.0380 for all 3693 data REM 206 parameters refined using 5 restraints END WGHT 0.0280 1.4381 REM Instructions for potential hydrogen bonds EQIV $1 y+1/2, x-1/2, z+1/2 HTAB N1 O102_$1 HTAB N1 Cl HTAB N1 O104 EQIV $2 -y+1/2, -x+1/2, z+1/2 HTAB N8 O101_$2 EQIV $3 -x+1, -y, z HTAB N15 O101_$3 HTAB N15 Cl HTAB N15 O103 REM Highest difference peak 0.556, deepest hole -0.260, 1-sigma level 0.055 Q1 1 0.6849 0.2354 0.2295 11.00000 0.05 0.56 Q2 1 0.6639 0.0889 0.3250 11.00000 0.05 0.40 Q3 1 0.5488 0.1352 0.2106 11.00000 0.05 0.39 Q4 1 0.5945 0.2161 0.3520 11.00000 0.05 0.24 Q5 1 0.5541 0.1421 0.2700 11.00000 0.05 0.22 Q6 1 0.3668 0.1032 0.5844 11.00000 0.05 0.22 Q7 1 0.2808 0.1131 0.5863 11.00000 0.05 0.21 Q8 1 0.5000 0.0000 0.3338 10.50000 0.05 0.21 Q9 1 0.3206 0.0881 0.2986 11.00000 0.05 0.21 Q10 1 0.3112 0.2264 0.7239 11.00000 0.05 0.20 Q11 1 0.3242 0.1165 0.5109 11.00000 0.05 0.20 Q12 1 0.6659 0.1677 0.2050 11.00000 0.05 0.19 Q13 1 0.5059 0.1978 0.5661 11.00000 0.05 0.19 Q14 1 0.5115 0.1932 0.7062 11.00000 0.05 0.19 Q15 1 0.4855 -0.0384 0.5655 11.00000 0.05 0.19 Q16 1 0.4899 0.1419 0.2298 11.00000 0.05 0.19 Q17 1 0.3202 0.0057 0.6758 11.00000 0.05 0.19 Q18 1 0.2303 0.2171 0.7927 11.00000 0.05 0.18 Q19 1 0.5994 0.2285 0.5920 11.00000 0.05 0.18 Q20 1 0.5011 0.0330 0.2731 11.00000 0.05 0.18 ; _shelx_res_checksum 34157 _shelx_hkl_file ; -2 0 0 584.04 23.80 -2 0 0 596.64 24.00 2 0 0 603.64 24.00 2 0 0 613.84 24.00 -3 0 0 0.60 1.70 -3 0 0 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