Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Ponomarova, Vira V.' ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; 'Komarchuk, Vasiliy V.' ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; 'Boldog, Ishtvan' ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; 'Chernega, Alexander N.' ; Institute of Organic Chemistry Murmanskaya Str. 4 253660 Kiev Ukraine ; 'Sieler, Joachim' ; Institut fur Anorganische Chemie Universitaet Leipzig Linnestrasse 3 D-04103 Leipzig Bundesrepublik Deutschland ; 'Domasevitch, Konstantin V.' ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr Konstantin V Domasevitch' _publ_contact_author_address ; Inorganic Chemistry Department Kiev University Volodimirska Street 64 Kiev 01033 UKRAINE ; _publ_contact_author_phone ? _publ_contact_author_fax ? _publ_contact_author_email 'dk@anorgchemie.univ.kiev.ua' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Mixed-Anion Complexes with a Bipyrazolyl Ligand: A New Entry to a Realm of Three-Dimensional Five-Connected Coordination Topologies ; _publ_section_acknowledgements ; The work was in part supported by grant from Deutsche Forschungsgemeinschaft (JS and KVD) ; #============================================================================== data_c1024 _database_code_CSD 175727 _audit_creation_method SHELXL _chemical_name_systematic ; Tetrakis(3,3',5,5'-tetramethyl-4,4'-bipyrazolyl) Sulfato Diperchlorato Dicobalt(II), trihydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H62 Cl2 Co2 N15 O16 S' _chemical_formula_weight 1229.87 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/mnc loop_ _symmetry_equiv_pos_as_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' '-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 13.7588(9) _cell_length_b 13.7588(9) _cell_length_c 16.7261(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3166.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method ? _exptl_crystal_F_000 1278 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD Siemens' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19462 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.88 _reflns_number_total 2070 _reflns_number_observed 1443 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 390 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+2.0818P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1680 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_obs 0.0440 _refine_ls_wR_factor_all 0.2066 _refine_ls_wR_factor_obs 0.1196 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.745 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.0000 0.0000 0.19607(3) 0.0242(2) Uani 1 d S . S1 S 0.0368(2) 0.0335(2) 0.0000 0.0221(5) Uani 0.25 d SP . O1 O 0.0000 0.0000 0.3244(2) 0.0523(9) Uani 1 d S . O2 O 0.0000 0.0000 0.0710(2) 0.0470(8) Uani 1 d S . O3 O 0.0213(6) 0.1385(4) 0.0000 0.0546(15) Uani 0.50 d SP . N1 N 0.08956(13) -0.12800(12) 0.19421(10) 0.0304(4) Uani 1 d . . N2 N 0.05750(13) -0.20421(12) 0.15005(11) 0.0346(4) Uani 1 d . . H2A H 0.01122(13) -0.19954(12) 0.11222(11) 0.042 Uiso 1 d R . C1 C 0.15816(15) -0.16460(15) 0.24189(13) 0.0331(4) Uani 1 d . . C2 C 0.16806(14) -0.26531(14) 0.22923(13) 0.0320(4) Uani 1 d . . C3 C 0.1027(2) -0.2873(2) 0.16917(15) 0.0379(5) Uani 1 d . . C4 C 0.0801(3) -0.3813(2) 0.1292(3) 0.0717(10) Uani 1 d . . H4A H 0.0304(3) -0.3717(2) 0.0896(3) 0.086 Uiso 1 d R . H4B H 0.1377(3) -0.4060(2) 0.1039(3) 0.086 Uiso 1 d R . H4C H 0.0578(3) -0.4270(2) 0.1684(3) 0.086 Uiso 1 d R . C5 C 0.2166(2) -0.1039(2) 0.2979(2) 0.0580(8) Uani 1 d . . H5A H 0.1943(2) -0.0378(2) 0.2954(2) 0.070 Uiso 1 d R . H5B H 0.2098(2) -0.1277(2) 0.3515(2) 0.070 Uiso 1 d R . H5C H 0.2836(2) -0.1067(2) 0.2823(2) 0.070 Uiso 1 d R . Cl1 Cl 0.3368(3) -0.2029(3) 0.5000 0.0514(9) Uani 0.25 d SP . O4 O 0.2377(14) -0.2315(17) 0.5000 0.094(6) Uani 0.25 d SP . O5 O 0.3746(8) -0.2299(14) 0.5741(7) 0.102(4) Uani 0.25 d P . O6 O 0.3456(22) -0.1089(15) 0.5000 0.121(8) Uani 0.25 d SP . Cl1A Cl 0.1840(6) 0.0267(6) 0.5000 0.091(2) Uani 0.25 d SP . O4A O 0.2724(15) -0.0149(18) 0.5000 0.101(5) Uani 0.25 d SP . O5A O 0.1569(11) 0.0698(10) 0.4302(5) 0.095(4) Uani 0.25 d P . O6A O 0.1178(25) -0.0505(31) 0.5000 0.224(27) Uani 0.25 d SP . O7 O 0.1958(7) -0.0685(6) 0.0000 0.035(2) Uani 0.25 d SP . 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 Co1 0.0247(2) 0.0247(2) 0.0232(3) 0.000 0.000 0.000 S1 0.025(2) 0.021(2) 0.0198(9) 0.000 0.000 -0.0005(8) O1 0.0640(15) 0.0640(15) 0.0290(15) 0.000 0.000 0.000 O2 0.0590(13) 0.0590(13) 0.0229(14) 0.000 0.000 0.000 O3 0.112(5) 0.026(2) 0.025(2) 0.000 0.000 0.008(3) N1 0.0304(8) 0.0264(8) 0.0345(8) -0.0002(6) -0.0090(6) 0.0003(6) N2 0.0336(9) 0.0280(8) 0.0422(9) -0.0031(7) -0.0132(7) 0.0016(7) C1 0.0321(10) 0.0302(10) 0.0370(10) 0.0025(8) -0.0094(8) 0.0025(7) C2 0.0283(9) 0.0281(9) 0.0395(10) 0.0039(8) -0.0053(8) 0.0011(7) C3 0.0334(10) 0.0289(10) 0.0513(12) -0.0019(9) -0.0105(9) 0.0018(8) C4 0.083(2) 0.0348(13) 0.097(2) -0.0174(14) -0.043(2) 0.0101(13) C5 0.065(2) 0.0409(13) 0.068(2) -0.0086(11) -0.0409(14) 0.0085(12) Cl1 0.041(2) 0.086(3) 0.0275(13) 0.000 0.000 0.001(2) O4 0.090(11) 0.132(15) 0.060(8) 0.000 0.000 -0.044(11) O5 0.064(6) 0.168(13) 0.074(7) 0.024(7) -0.023(5) -0.015(7) O6 0.163(21) 0.075(11) 0.125(16) 0.000 0.000 -0.031(13) Cl1A 0.100(4) 0.134(5) 0.040(2) 0.000 0.000 0.011(4) O4A 0.077(11) 0.132(16) 0.093(11) 0.000 0.000 0.001(11) O5A 0.128(10) 0.118(9) 0.039(4) -0.025(5) -0.035(5) 0.013(8) O6A 0.105(19) 0.131(24) 0.437(88) 0.000 0.000 -0.031(17) O7 0.030(4) 0.034(4) 0.041(4) 0.000 0.000 0.005(3) _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 Co1 O2 2.092(3) . ? Co1 O1 2.146(4) . ? Co1 N1 2.150(2) 4 ? Co1 N1 2.150(2) 3 ? Co1 N1 2.150(2) . ? Co1 N1 2.150(2) 2 ? S1 S1 0.968(4) 3 ? S1 S1 0.968(4) 11 ? S1 S1 1.369(5) 9 ? S1 O2 1.371(3) . ? S1 O2 1.371(3) 9 ? S1 O3 1.461(6) . ? S1 O3 1.589(7) 11 ? O2 S1 1.371(3) 9 ? O2 S1 1.371(3) 11 ? O2 S1 1.371(3) 3 ? O3 O7 1.021(10) 3 ? O3 S1 1.589(7) 3 ? N1 C1 1.334(3) . ? N1 N2 1.356(2) . ? N2 C3 1.341(3) . ? C1 C2 1.408(3) . ? C1 C5 1.490(3) . ? C2 C3 1.382(3) . ? C2 C2 1.471(4) 7_545 ? C3 C4 1.488(4) . ? Cl1 O6 1.30(2) . ? Cl1 O5 1.394(11) 10_556 ? Cl1 O5 1.394(11) . ? Cl1 O4 1.42(2) . ? Cl1 O7 1.908(10) 7_545 ? O5 O7 1.79(2) 7_545 ? O6 O4A 1.64(4) . ? Cl1A O4A 1.34(2) . ? Cl1A O5A 1.362(12) 10_556 ? Cl1A O5A 1.362(12) . ? Cl1A O6A 1.40(4) . ? O7 O3 1.021(10) 11 ? O7 O5 1.79(2) 16_655 ? O7 O5 1.79(2) 7_545 ? O7 Cl1 1.908(10) 7_545 ? 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 Co1 O1 180.0 . . ? O2 Co1 N1 89.17(5) . 4 ? O1 Co1 N1 90.83(5) . 4 ? O2 Co1 N1 89.17(5) . 3 ? O1 Co1 N1 90.83(5) . 3 ? N1 Co1 N1 178.35(9) 4 3 ? O2 Co1 N1 89.17(5) . . ? O1 Co1 N1 90.83(5) . . ? N1 Co1 N1 89.988(1) 4 . ? N1 Co1 N1 89.988(1) 3 . ? O2 Co1 N1 89.17(5) . 2 ? O1 Co1 N1 90.83(5) . 2 ? N1 Co1 N1 89.988(1) 4 2 ? N1 Co1 N1 89.988(1) 3 2 ? N1 Co1 N1 178.35(9) . 2 ? S1 S1 S1 90.0 3 11 ? S1 S1 S1 45.0 3 9 ? S1 S1 S1 45.0 11 9 ? S1 S1 O2 69.32(7) 3 . ? S1 S1 O2 69.32(7) 11 . ? S1 S1 O2 60.04(11) 9 . ? S1 S1 O2 69.32(8) 3 9 ? S1 S1 O2 69.32(8) 11 9 ? S1 S1 O2 60.04(11) 9 9 ? O2 S1 O2 120.1(2) . 9 ? S1 S1 O3 78.9(5) 3 . ? S1 S1 O3 168.9(5) 11 . ? S1 S1 O3 123.9(5) 9 . ? O2 S1 O3 106.2(2) . . ? O2 S1 O3 106.2(2) 9 . ? S1 S1 O3 154.4(4) 3 11 ? S1 S1 O3 64.4(4) 11 11 ? S1 S1 O3 109.4(4) 9 11 ? O2 S1 O3 99.6(2) . 11 ? O2 S1 O3 99.6(2) 9 11 ? O3 S1 O3 126.7(2) . 11 ? S1 O2 S1 41.36(15) 9 11 ? S1 O2 S1 41.36(15) 9 3 ? S1 O2 S1 59.9(2) 11 3 ? S1 O2 S1 59.9(2) 9 . ? S1 O2 S1 41.36(15) 11 . ? S1 O2 S1 41.36(15) 3 . ? S1 O2 Co1 150.04(11) 9 . ? S1 O2 Co1 150.04(11) 11 . ? S1 O2 Co1 150.04(11) 3 . ? S1 O2 Co1 150.04(11) . . ? O7 O3 S1 132.2(8) 3 . ? O7 O3 S1 168.9(8) 3 3 ? S1 O3 S1 36.7(2) . 3 ? C1 N1 N2 105.3(2) . . ? C1 N1 Co1 134.91(14) . . ? N2 N1 Co1 117.06(12) . . ? C3 N2 N1 112.3(2) . . ? N1 C1 C2 110.5(2) . . ? N1 C1 C5 123.1(2) . . ? C2 C1 C5 126.4(2) . . ? C3 C2 C1 105.2(2) . . ? C3 C2 C2 127.8(2) . 7_545 ? C1 C2 C2 127.0(2) . 7_545 ? N2 C3 C2 106.7(2) . . ? N2 C3 C4 122.5(2) . . ? C2 C3 C4 130.8(2) . . ? O6 Cl1 O5 103.3(10) . 10_556 ? O6 Cl1 O5 103.3(10) . . ? O5 Cl1 O5 125.5(13) 10_556 . ? O6 Cl1 O4 111.5(17) . . ? O5 Cl1 O4 106.5(7) 10_556 . ? O5 Cl1 O4 106.5(7) . . ? O6 Cl1 O7 131.6(14) . 7_545 ? O5 Cl1 O7 63.3(7) 10_556 7_545 ? O5 Cl1 O7 63.3(7) . 7_545 ? O4 Cl1 O7 117.0(11) . 7_545 ? Cl1 O5 O7 72.5(7) . 7_545 ? Cl1 O6 O4A 136.7(22) . . ? O4A Cl1A O5A 115.7(7) . 10_556 ? O4A Cl1A O5A 115.7(7) . . ? O5A Cl1A O5A 118.1(11) 10_556 . ? O4A Cl1A O6A 105.4(20) . . ? O5A Cl1A O6A 98.7(11) 10_556 . ? O5A Cl1A O6A 98.7(11) . . ? Cl1A O4A O6 153.1(19) . . ? O3 O7 O5 136.1(5) 11 16_655 ? O3 O7 O5 136.1(5) 11 7_545 ? O5 O7 O5 87.8(9) 16_655 7_545 ? O3 O7 Cl1 176.3(8) 11 7_545 ? O5 O7 Cl1 44.2(4) 16_655 7_545 ? O5 O7 Cl1 44.2(4) 7_545 7_545 ? _refine_diff_density_max 0.667 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.050 #============================================================================== data_c1026 _database_code_CSD 175728 _audit_creation_method SHELXL _chemical_name_systematic ; Tetrakis(3,3',5,5'-Tetramethyl-4,4'-bipyrazolyl) Sulfato Dinitrato Dinickel(II), trihydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H62 N18 Ni2 O13 S' _chemical_formula_weight 1152.56 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/mnc loop_ _symmetry_equiv_pos_as_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' '-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 13.6542(13) _cell_length_b 13.6542(13) _cell_length_c 16.477(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3071.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method ? _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD Siemens' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8138 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.09 _reflns_number_total 1129 _reflns_number_observed 1021 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 108 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+14.8433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0169(66) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1021 _refine_ls_number_parameters 108 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_obs 0.0801 _refine_ls_wR_factor_all 0.3476 _refine_ls_wR_factor_obs 0.1836 _refine_ls_goodness_of_fit_all 1.370 _refine_ls_goodness_of_fit_obs 1.370 _refine_ls_restrained_S_all 3.410 _refine_ls_restrained_S_obs 1.368 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.30168(9) 0.0362(6) Uani 1 d S . O1 O 0.0000 0.0000 0.1732(6) 0.075(3) Uani 1 d S . S1 S 0.0291(7) 0.0475(6) 0.5000 0.029(2) Uani 0.25 d SP . O2 O 0.0000 0.0000 0.4281(5) 0.044(2) Uani 1 d S . O3 O 0.1445(11) 0.0320(18) 0.5000 0.076(7) Uani 0.50 d SP . N1 N 0.0869(4) 0.1267(4) 0.3040(3) 0.0381(13) Uani 1 d . . N2 N 0.0551(4) 0.2035(4) 0.3494(3) 0.0390(13) Uani 1 d . . H2A H 0.0091(4) 0.1983(4) 0.3874(3) 0.047 Uiso 1 d R . C1 C 0.1011(5) 0.2873(5) 0.3314(4) 0.043(2) Uani 1 d . . C2 C 0.1666(5) 0.2655(5) 0.2702(4) 0.040(2) Uani 1 d . . C3 C 0.1561(5) 0.1650(5) 0.2556(4) 0.0435(15) Uani 1 d . . C4 C 0.2145(8) 0.1047(7) 0.1986(7) 0.077(3) Uani 1 d . . H4A H 0.1929(8) 0.0384(7) 0.2000(7) 0.093 Uiso 1 d R . H4B H 0.2059(8) 0.1304(7) 0.1457(7) 0.093 Uiso 1 d R . H4C H 0.2820(8) 0.1077(7) 0.2129(7) 0.093 Uiso 1 d R . C5 C 0.0786(8) 0.3813(6) 0.3736(7) 0.077(3) Uani 1 d . . H5A H 0.0295(8) 0.3705(6) 0.4134(7) 0.092 Uiso 1 d R . H5B H 0.1362(8) 0.4062(6) 0.3986(7) 0.092 Uiso 1 d R . H5C H 0.0553(8) 0.4274(6) 0.3350(7) 0.092 Uiso 1 d R . O4 O -0.2034(15) -0.0705(12) 0.5000 0.011(4) Uiso 0.25 d SP . N3 N 0.3194(38) 0.4568(35) 0.5000 0.098(16) Uiso 0.25 d SPD . N3A N 0.2061(28) 0.5930(28) 0.5000 0.131(23) Uiso 0.25 d SPD . O8 O 0.3389(29) 0.4208(29) 0.5661(18) 0.115(11) Uiso 0.25 d PD . O6 O 0.1192(25) 0.5836(33) 0.5000 0.102(13) Uiso 0.25 d SPD . O7 O 0.2420(42) 0.6734(29) 0.5000 0.180(30) Uiso 0.25 d SPD . O5 O 0.2575(26) 0.5219(29) 0.5000 0.177(15) Uiso 0.50 d SPD . 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 Ni1 0.0409(8) 0.0409(8) 0.0267(8) 0.000 0.000 0.000 O1 0.096(6) 0.096(6) 0.032(5) 0.000 0.000 0.000 S1 0.035(6) 0.029(6) 0.023(3) 0.000 0.000 0.003(4) O2 0.052(3) 0.052(3) 0.027(4) 0.000 0.000 0.000 O3 0.030(7) 0.176(21) 0.021(6) 0.000 0.000 0.019(10) N1 0.042(3) 0.034(3) 0.039(3) -0.002(3) 0.013(3) 0.000(2) N2 0.038(3) 0.037(3) 0.042(3) 0.001(2) 0.014(2) 0.005(2) C1 0.039(3) 0.041(4) 0.048(4) 0.001(3) 0.009(3) 0.002(3) C2 0.038(4) 0.034(3) 0.048(4) 0.006(3) 0.010(3) 0.005(3) C3 0.041(4) 0.043(4) 0.047(3) -0.001(3) 0.020(3) 0.004(3) C4 0.095(7) 0.052(5) 0.085(6) -0.003(5) 0.058(6) 0.000(4) C5 0.091(7) 0.045(4) 0.094(7) -0.014(5) 0.037(6) -0.001(4) _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 Ni1 O2 2.084(8) . ? Ni1 N1 2.098(5) . ? Ni1 N1 2.098(5) 4 ? Ni1 N1 2.098(5) 2 ? Ni1 N1 2.098(5) 3 ? Ni1 O1 2.118(10) . ? S1 S1 1.075(11) 11_556 ? S1 S1 1.075(11) 3 ? S1 O2 1.407(8) . ? S1 O2 1.407(8) 9_556 ? S1 S1 1.52(2) 9_556 ? S1 O3 1.57(2) 3 ? S1 O3 1.59(2) . ? O2 S1 1.407(8) 11_556 ? O2 S1 1.407(8) 3 ? O2 S1 1.407(8) 9_556 ? O3 O4 0.96(2) 9_556 ? O3 S1 1.57(2) 11_556 ? N1 C3 1.343(8) . ? N1 N2 1.360(7) . ? N2 C1 1.338(9) . ? C1 C2 1.380(10) . ? C1 C5 1.492(11) . ? C2 C3 1.401(10) . ? C2 C2 1.470(13) 8 ? C3 C4 1.481(11) . ? O4 O3 0.96(2) 9_556 ? N3 O8 1.22(2) 10_556 ? N3 O8 1.22(2) . ? N3 O5 1.23(2) . ? N3A O6 1.19(2) . ? N3A O5 1.20(2) . ? N3A O7 1.20(2) . ? 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 Ni1 N1 88.9(2) . . ? O2 Ni1 N1 88.9(2) . 4 ? N1 Ni1 N1 89.981(6) . 4 ? O2 Ni1 N1 88.9(2) . 2 ? N1 Ni1 N1 177.9(3) . 2 ? N1 Ni1 N1 89.981(6) 4 2 ? O2 Ni1 N1 88.9(2) . 3 ? N1 Ni1 N1 89.981(6) . 3 ? N1 Ni1 N1 177.9(3) 4 3 ? N1 Ni1 N1 89.981(6) 2 3 ? O2 Ni1 O1 180.0 . . ? N1 Ni1 O1 91.1(2) . . ? N1 Ni1 O1 91.1(2) 4 . ? N1 Ni1 O1 91.1(2) 2 . ? N1 Ni1 O1 91.1(2) 3 . ? S1 S1 S1 90.0 11_556 3 ? S1 S1 O2 67.5(2) 11_556 . ? S1 S1 O2 67.5(2) 3 . ? S1 S1 O2 67.5(2) 11_556 9_556 ? S1 S1 O2 67.5(2) 3 9_556 ? O2 S1 O2 114.6(6) . 9_556 ? S1 S1 S1 45.000(3) 11_556 9_556 ? S1 S1 S1 45.000(1) 3 9_556 ? O2 S1 S1 57.3(3) . 9_556 ? O2 S1 S1 57.3(3) 9_556 9_556 ? S1 S1 O3 161.3(13) 11_556 3 ? S1 S1 O3 71.3(12) 3 3 ? O2 S1 O3 103.9(6) . 3 ? O2 S1 O3 103.9(6) 9_556 3 ? S1 S1 O3 116.3(12) 9_556 3 ? S1 S1 O3 68.8(13) 11_556 . ? S1 S1 O3 158.8(13) 3 . ? O2 S1 O3 102.6(7) . . ? O2 S1 O3 102.6(7) 9_556 . ? S1 S1 O3 113.8(13) 9_556 . ? O3 S1 O3 129.8(7) 3 . ? S1 O2 S1 44.9(4) . 11_556 ? S1 O2 S1 44.9(4) . 3 ? S1 O2 S1 65.4(6) 11_556 3 ? S1 O2 S1 65.4(6) . 9_556 ? S1 O2 S1 44.9(4) 11_556 9_556 ? S1 O2 S1 44.9(4) 3 9_556 ? S1 O2 Ni1 147.3(3) . . ? S1 O2 Ni1 147.3(3) 11_556 . ? S1 O2 Ni1 147.3(3) 3 . ? S1 O2 Ni1 147.3(3) 9_556 . ? O4 O3 S1 179.1(23) 9_556 11_556 ? O4 O3 S1 139.2(25) 9_556 . ? S1 O3 S1 39.8(7) 11_556 . ? C3 N1 N2 104.5(5) . . ? C3 N1 Ni1 135.1(5) . . ? N2 N1 Ni1 117.7(4) . . ? C1 N2 N1 112.8(5) . . ? N2 C1 C2 106.4(6) . . ? N2 C1 C5 122.3(6) . . ? C2 C1 C5 131.3(7) . . ? C1 C2 C3 105.7(6) . . ? C1 C2 C2 127.1(6) . 8 ? C3 C2 C2 127.2(6) . 8 ? N1 C3 C2 110.6(6) . . ? N1 C3 C4 122.6(7) . . ? C2 C3 C4 126.7(6) . . ? O8 N3 O8 125.6(51) 10_556 . ? O8 N3 O5 116.2(27) 10_556 . ? O8 N3 O5 116.2(27) . . ? O6 N3A O5 119.7(21) . . ? O6 N3A O7 120.2(21) . . ? O5 N3A O7 120.1(21) . . ? N3A O5 N3 172.3(44) . . ? _refine_diff_density_max 0.690 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.076 #============================================================================== data_c998 _database_code_CSD 175729 _audit_creation_method SHELXL _chemical_name_systematic ; Tetrakis(3,3',5,5'-Tetramethyl-4,4'-Bipyrazolyl) Sulfato Bis(thiocyanato) Dicobalt(II), Bis(Methanol) Bis(Chloroform) Solvate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H66 Cl6 Co2 N18 O6 S3' _chemical_formula_weight 1393.91 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.699(2) _cell_length_b 21.594(3) _cell_length_c 22.220(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6573.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method ? _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD Siemens' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41390 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.01 _reflns_number_total 14262 _reflns_number_observed 8693 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2509 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.41(2) _refine_ls_number_reflns 11753 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_obs 0.0550 _refine_ls_wR_factor_all 0.2292 _refine_ls_wR_factor_obs 0.1373 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.549 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max 0.006 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.77433(4) 0.84719(2) 0.13498(2) 0.02540(15) Uani 1 d . . Co2 Co 1.26815(4) 1.15405(2) 0.13188(2) 0.0268(2) Uani 1 d . . S1 S 0.71255(7) 0.76461(4) 0.26177(4) 0.0270(2) Uani 1 d . . S2 S 0.8669(2) 0.95614(10) -0.04411(8) 0.0809(6) Uani 1 d . . S3 S 1.2616(3) 1.0297(2) -0.04669(12) 0.1358(13) Uani 1 d . . O1 O 0.7499(2) 0.70572(13) 0.28595(13) 0.0320(6) Uani 1 d . . O2 O 0.7644(2) 0.77638(14) 0.20408(12) 0.0327(7) Uani 1 d . . O3 O 0.7322(3) 0.81519(14) 0.30388(13) 0.0413(8) Uani 1 d . . O4 O 0.6075(2) 0.7581(2) 0.24993(14) 0.0417(7) Uani 1 d . . N1 N 0.6518(3) 0.8012(2) 0.0903(2) 0.0303(8) Uani 1 d . . N2 N 0.5730(3) 0.7883(2) 0.1259(2) 0.0360(9) Uani 1 d . . H2A H 0.5743(3) 0.7890(2) 0.1645(2) 0.043 Uiso 1 calc R . N3 N 0.3776(3) 0.7209(2) -0.0960(2) 0.0305(8) Uani 1 d . . N4 N 0.3370(3) 0.7774(2) -0.0850(2) 0.0335(8) Uani 1 d . . H4D H 0.2885(3) 0.7924(2) -0.1048(2) 0.040 Uiso 1 calc R . N5 N 0.8881(3) 0.8917(2) 0.1870(2) 0.0305(8) Uani 1 d . . N6 N 0.9658(3) 0.8577(2) 0.2048(2) 0.0347(8) Uani 1 d . . H6A H 0.9646(3) 0.8182(2) 0.2093(2) 0.042 Uiso 1 calc R . N7 N 1.1637(3) 1.0929(2) 0.1768(2) 0.0307(8) Uani 1 d . . N8 N 1.1836(3) 1.0796(2) 0.2351(2) 0.0330(8) Uani 1 d . . H8A H 1.2225(3) 1.1010(2) 0.2572(2) 0.040 Uiso 1 calc R . N9 N 1.1485(3) 1.2081(2) 0.0959(2) 0.0332(8) Uani 1 d . . N10 N 1.0693(3) 1.2152(2) 0.1313(2) 0.0360(8) Uani 1 d . . H10D H 1.0703(3) 1.2118(2) 0.1698(2) 0.043 Uiso 1 calc R . N11 N 0.8441(3) 1.2224(2) -0.0841(2) 0.0361(8) Uani 1 d . . H11A H 0.8014(3) 1.2046(2) -0.1066(2) 0.043 Uiso 1 calc R . N12 N 0.8740(3) 1.2818(2) -0.0918(2) 0.0344(8) Uani 1 d . . N13 N 1.4577(3) 1.1396(2) 0.2011(2) 0.0375(9) Uani 1 d . . H13A H 1.4540(3) 1.1789(2) 0.2073(2) 0.045 Uiso 1 calc R . N14 N 1.3857(3) 1.1061(2) 0.1774(2) 0.0329(8) Uani 1 d . . N15 N 1.6694(3) 0.9077(2) 0.1765(2) 0.0287(8) Uani 1 d . . N16 N 1.6722(3) 0.9174(2) 0.2369(2) 0.0328(8) Uani 1 d . . H16A H 1.7058(3) 0.8951(2) 0.2614(2) 0.039 Uiso 1 calc R . N17 N 0.8015(3) 0.9049(2) 0.0633(2) 0.0367(9) Uani 1 d . . N18 N 1.2757(4) 1.0981(2) 0.0582(2) 0.0423(9) Uani 1 d . . C1 C 0.6200(4) 0.7946(2) 0.0334(2) 0.0346(10) Uani 1 d . . C2 C 0.5200(4) 0.7782(2) 0.0332(2) 0.0338(10) Uani 1 d . . C3 C 0.4932(4) 0.7745(2) 0.0932(2) 0.0374(11) Uani 1 d . . C4 C 0.3976(5) 0.7570(5) 0.1218(3) 0.072(2) Uani 1 d . . H4A H 0.4037(5) 0.7591(5) 0.1648(3) 0.087 Uiso 1 calc R . H4B H 0.3805(5) 0.7156(5) 0.1102(3) 0.087 Uiso 1 calc R . H4C H 0.3477(5) 0.7852(5) 0.1087(3) 0.087 Uiso 1 calc R . C5 C 0.6845(4) 0.8039(3) -0.0192(2) 0.0489(13) Uani 1 d . . H5A H 0.7488(4) 0.8148(3) -0.0056(2) 0.059 Uiso 1 calc R . H5B H 0.6589(4) 0.8365(3) -0.0439(2) 0.059 Uiso 1 calc R . H5C H 0.6876(4) 0.7663(3) -0.0422(2) 0.059 Uiso 1 calc R . C6 C 0.3819(4) 0.8067(2) -0.0394(2) 0.0386(11) Uani 1 d . . C7 C 0.4554(3) 0.7677(2) -0.0192(2) 0.0319(9) Uani 1 d . . C8 C 0.4494(3) 0.7155(2) -0.0561(2) 0.0332(10) Uani 1 d . . C9 C 0.5154(4) 0.6600(3) -0.0557(2) 0.0442(11) Uani 1 d . . H9A H 0.4943(4) 0.6311(3) -0.0858(2) 0.053 Uiso 1 calc R . H9B H 0.5132(4) 0.6406(3) -0.0169(2) 0.053 Uiso 1 calc R . H9C H 0.5811(4) 0.6728(3) -0.0642(2) 0.053 Uiso 1 calc R . C10 C 0.3503(6) 0.8695(3) -0.0175(3) 0.058(2) Uani 1 d . . H10A H 0.2967(6) 0.8839(3) -0.0415(3) 0.070 Uiso 1 calc R . H10B H 0.4038(6) 0.8980(3) -0.0208(3) 0.070 Uiso 1 calc R . H10C H 0.3303(6) 0.8666(3) 0.0238(3) 0.070 Uiso 1 calc R . C11 C 1.0454(4) 0.8929(2) 0.2148(2) 0.0373(10) Uani 1 d . . C12 C 1.0189(3) 0.9527(2) 0.2036(2) 0.0315(9) Uani 1 d . . C13 C 0.9197(4) 0.9503(2) 0.1869(2) 0.0330(10) Uani 1 d . . C14 C 0.8537(4) 1.0037(2) 0.1728(2) 0.0409(11) Uani 1 d . . H14A H 0.7899(4) 0.9884(2) 0.1628(2) 0.049 Uiso 1 calc R . H14B H 0.8796(4) 1.0265(2) 0.1394(2) 0.049 Uiso 1 calc R . H14C H 0.8493(4) 1.0303(2) 0.2073(2) 0.049 Uiso 1 calc R . C15 C 1.1399(4) 0.8646(3) 0.2330(4) 0.060(2) Uani 1 d . . H15A H 1.1319(4) 0.8206(3) 0.2369(4) 0.071 Uiso 1 calc R . H15B H 1.1603(4) 0.8817(3) 0.2708(4) 0.071 Uiso 1 calc R . H15C H 1.1883(4) 0.8732(3) 0.2029(4) 0.071 Uiso 1 calc R . C16 C 1.1356(4) 1.0295(2) 0.2543(2) 0.0372(10) Uani 1 d . . C17 C 1.0808(4) 1.0081(2) 0.2056(2) 0.0342(10) Uani 1 d . . C18 C 1.1025(4) 1.0497(2) 0.1584(2) 0.0344(10) Uani 1 d . . C19 C 1.0623(5) 1.0486(3) 0.0962(2) 0.0501(13) Uani 1 d . . H19A H 1.0895(5) 1.0823(3) 0.0734(2) 0.060 Uiso 1 calc R . H19B H 0.9926(5) 1.0529(3) 0.0977(2) 0.060 Uiso 1 calc R . H19C H 1.0789(5) 1.0101(3) 0.0772(2) 0.060 Uiso 1 calc R . C20 C 1.1480(5) 1.0060(3) 0.3169(2) 0.0553(15) Uani 1 d . . H20A H 1.1920(5) 1.0326(3) 0.3384(2) 0.066 Uiso 1 calc R . H20B H 1.1742(5) 0.9648(3) 0.3158(2) 0.066 Uiso 1 calc R . H20C H 1.0858(5) 1.0055(3) 0.3368(2) 0.066 Uiso 1 calc R . C21 C 1.1164(4) 1.2164(2) 0.0402(2) 0.0340(10) Uani 1 d . . C22 C 1.0154(4) 1.2285(2) 0.0397(2) 0.0374(10) Uani 1 d . . C23 C 0.9883(4) 1.2282(3) 0.0991(2) 0.0421(11) Uani 1 d . . C24 C 0.8926(5) 1.2371(4) 0.1291(3) 0.071(2) Uani 1 d . . H24A H 0.9007(5) 1.2339(4) 0.1719(3) 0.085 Uiso 1 calc R . H24B H 0.8478(5) 1.2059(4) 0.1155(3) 0.085 Uiso 1 calc R . H24C H 0.8675(5) 1.2774(4) 0.1192(3) 0.085 Uiso 1 calc R . C25 C 1.1813(4) 1.2144(3) -0.0126(2) 0.0509(13) Uani 1 d . . H25A H 1.2467(4) 1.2053(3) 0.0001(2) 0.061 Uiso 1 calc R . H25B H 1.1802(4) 1.2538(3) -0.0326(2) 0.061 Uiso 1 calc R . H25C H 1.1593(4) 1.1828(3) -0.0398(2) 0.061 Uiso 1 calc R . C26 C 0.8886(4) 1.1942(2) -0.0372(2) 0.0383(11) Uani 1 d . . C27 C 0.9521(4) 1.2382(3) -0.0130(2) 0.0379(10) Uani 1 d . . C28 C 0.9414(4) 1.2912(2) -0.0493(2) 0.0377(11) Uani 1 d . . C29 C 0.9965(5) 1.3501(3) -0.0427(3) 0.0558(14) Uani 1 d . . H29A H 0.9755(5) 1.3789(3) -0.0730(3) 0.067 Uiso 1 calc R . H29B H 1.0650(5) 1.3421(3) -0.0474(3) 0.067 Uiso 1 calc R . H29C H 0.9845(5) 1.3673(3) -0.0035(3) 0.067 Uiso 1 calc R . C30 C 0.8689(6) 1.1294(3) -0.0197(3) 0.065(2) Uani 1 d . . H30A H 0.8206(6) 1.1121(3) -0.0461(3) 0.078 Uiso 1 calc R . H30B H 0.8453(6) 1.1282(3) 0.0209(3) 0.078 Uiso 1 calc R . H30C H 0.9280(6) 1.1056(3) -0.0226(3) 0.078 Uiso 1 calc R . C31 C 1.5369(4) 1.1051(3) 0.2143(2) 0.0454(12) Uani 1 d . . C32 C 1.5130(4) 1.0444(2) 0.1979(2) 0.0366(10) Uani 1 d . . C33 C 1.4169(4) 1.0477(2) 0.1753(2) 0.0335(10) Uani 1 d . . C34 C 1.3564(4) 0.9954(2) 0.1524(3) 0.0485(13) Uani 1 d . . H34A H 1.2939(4) 1.0108(2) 0.1398(3) 0.058 Uiso 1 calc R . H34B H 1.3476(4) 0.9654(2) 0.1837(3) 0.058 Uiso 1 calc R . H34C H 1.3887(4) 0.9764(2) 0.1188(3) 0.058 Uiso 1 calc R . C35 C 1.6262(5) 1.1310(4) 0.2416(5) 0.077(2) Uani 1 d . . H35A H 1.6185(5) 1.1748(4) 0.2471(5) 0.093 Uiso 1 calc R . H35B H 1.6808(5) 1.1232(4) 0.2156(5) 0.093 Uiso 1 calc R . H35C H 1.6374(5) 1.1117(4) 0.2799(5) 0.093 Uiso 1 calc R . C36 C 1.6171(4) 0.9654(2) 0.2542(2) 0.0398(11) Uani 1 d . . C37 C 1.5764(3) 0.9898(2) 0.2024(2) 0.0335(10) Uani 1 d . . C38 C 1.6104(3) 0.9516(2) 0.1550(2) 0.0327(10) Uani 1 d . . C39 C 1.5877(4) 0.9574(3) 0.0901(2) 0.0459(12) Uani 1 d . . H39A H 1.6207(4) 0.9253(3) 0.0683(2) 0.055 Uiso 1 calc R . H39B H 1.6092(4) 0.9971(3) 0.0759(2) 0.055 Uiso 1 calc R . H39C H 1.5185(4) 0.9536(3) 0.0842(2) 0.055 Uiso 1 calc R . C40 C 1.6060(6) 0.9827(4) 0.3188(3) 0.064(2) Uani 1 d . . H40A H 1.6452(6) 0.9557(4) 0.3431(3) 0.077 Uiso 1 calc R . H40B H 1.5388(6) 0.9788(4) 0.3303(3) 0.077 Uiso 1 calc R . H40C H 1.6269(6) 1.0247(4) 0.3245(3) 0.077 Uiso 1 calc R . C41 C 1.2719(6) 1.0706(3) 0.0151(3) 0.0595(14) Uani 1 d . . C42 C 0.8291(4) 0.9261(2) 0.0186(2) 0.0416(10) Uani 1 d . . C43 C 0.6355(7) 1.0097(4) -0.1046(3) 0.079(2) Uani 1 d . . H43A H 0.6943(7) 1.0017(4) -0.0807(3) 0.095 Uiso 1 calc R . C44 C 0.4319(18) 0.8393(10) 0.3234(9) 0.157(6) Uani 1 d . . H44A H 0.5013(18) 0.8309(10) 0.3304(9) 0.188 Uiso 1 calc R . Cl1 Cl 0.6441(2) 1.08301(13) -0.1370(2) 0.1118(8) Uani 1 d . . Cl2 Cl 0.6300(3) 0.9556(2) -0.16494(15) 0.1227(9) Uani 1 d . . Cl3 Cl 0.5335(2) 1.0029(2) -0.05863(10) 0.1190(10) Uani 1 d . . Cl4 Cl 0.4061(6) 0.8919(2) 0.3684(3) 0.176(2) Uani 1 d . . Cl5 Cl 0.3788(5) 0.7707(2) 0.3263(2) 0.164(2) Uani 1 d . . Cl6 Cl 0.4255(3) 0.8669(2) 0.2434(2) 0.1462(13) Uani 1 d . . O5 O 0.9543(3) 0.7249(2) 0.2336(2) 0.0443(8) Uani 1 d . . C45 C 1.0056(5) 0.6795(4) 0.2014(4) 0.069(2) Uani 1 d . . H45A H 1.0646(5) 0.6693(4) 0.2224(4) 0.083 Uiso 1 d R . H45B H 1.0213(5) 0.6950(4) 0.1621(4) 0.083 Uiso 1 d R . H45C H 0.9658(5) 0.6431(4) 0.1976(4) 0.083 Uiso 1 d R . O6 O 0.6955(3) 0.6449(2) 0.1604(2) 0.0618(10) Uani 1 d . . C46 C 0.6173(8) 0.6113(6) 0.1336(6) 0.106(3) Uani 1 d . . H46A H 0.6421(8) 0.5736(6) 0.1164(6) 0.127 Uiso 1 d R . H46B H 0.5877(8) 0.6359(6) 0.1027(6) 0.127 Uiso 1 d R . H46C H 0.5695(8) 0.6015(6) 0.1638(6) 0.127 Uiso 1 d R . 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 Co1 0.0273(3) 0.0263(3) 0.0227(2) -0.0011(2) 0.0006(2) 0.0001(2) Co2 0.0282(3) 0.0271(3) 0.0249(3) 0.0013(2) 0.0005(2) 0.0007(2) S1 0.0327(5) 0.0257(4) 0.0226(4) 0.0013(3) 0.0012(4) -0.0005(4) S2 0.0846(12) 0.1021(13) 0.0559(9) 0.0426(9) 0.0147(8) 0.0015(10) S3 0.204(3) 0.128(2) 0.0756(13) -0.0645(14) -0.014(2) 0.042(2) O1 0.038(2) 0.0268(14) 0.0316(13) 0.0059(11) 0.0004(12) 0.0022(12) O2 0.038(2) 0.0339(15) 0.0262(13) 0.0064(11) 0.0058(12) 0.0005(13) O3 0.067(2) 0.0312(15) 0.0259(13) -0.0003(12) -0.0019(15) -0.006(2) O4 0.032(2) 0.052(2) 0.041(2) 0.0142(14) -0.0023(13) -0.0008(14) N1 0.030(2) 0.033(2) 0.028(2) -0.0041(14) -0.0032(15) -0.0007(15) N2 0.034(2) 0.047(2) 0.027(2) -0.001(2) -0.003(2) -0.008(2) N3 0.033(2) 0.028(2) 0.031(2) -0.0016(14) -0.006(2) -0.0057(15) N4 0.027(2) 0.037(2) 0.036(2) -0.003(2) -0.008(2) -0.001(2) N5 0.031(2) 0.028(2) 0.033(2) -0.0020(14) 0.002(2) 0.001(2) N6 0.036(2) 0.025(2) 0.043(2) 0.008(2) -0.004(2) -0.002(2) N7 0.034(2) 0.035(2) 0.023(2) 0.0029(14) -0.003(2) -0.007(2) N8 0.039(2) 0.034(2) 0.026(2) -0.0016(15) -0.003(2) -0.008(2) N9 0.033(2) 0.041(2) 0.026(2) 0.0031(15) -0.005(2) 0.004(2) N10 0.032(2) 0.047(2) 0.029(2) 0.002(2) -0.004(2) 0.005(2) N11 0.044(2) 0.032(2) 0.032(2) 0.001(2) -0.010(2) 0.001(2) N12 0.033(2) 0.037(2) 0.034(2) 0.003(2) -0.004(2) -0.001(2) N13 0.032(2) 0.036(2) 0.044(2) -0.006(2) -0.002(2) 0.009(2) N14 0.031(2) 0.031(2) 0.037(2) -0.001(2) -0.004(2) 0.006(2) N15 0.030(2) 0.035(2) 0.022(2) -0.0057(14) -0.0042(15) 0.003(2) N16 0.040(2) 0.033(2) 0.025(2) -0.0039(14) 0.000(2) 0.007(2) N17 0.041(2) 0.037(2) 0.032(2) 0.007(2) -0.001(2) 0.004(2) N18 0.049(2) 0.043(2) 0.035(2) -0.004(2) 0.004(2) 0.003(2) C1 0.038(2) 0.038(2) 0.028(2) -0.007(2) -0.007(2) -0.001(2) C2 0.032(2) 0.039(2) 0.031(2) -0.001(2) -0.006(2) -0.003(2) C3 0.032(2) 0.046(3) 0.034(2) -0.002(2) -0.003(2) -0.012(2) C4 0.042(3) 0.124(6) 0.051(3) 0.000(4) 0.001(3) -0.030(4) C5 0.040(3) 0.080(4) 0.027(2) -0.011(2) 0.000(2) -0.006(2) C6 0.046(3) 0.037(3) 0.032(2) 0.000(2) -0.004(2) -0.003(2) C7 0.035(2) 0.035(2) 0.026(2) -0.001(2) -0.005(2) -0.003(2) C8 0.034(2) 0.035(2) 0.030(2) -0.003(2) -0.005(2) 0.001(2) C9 0.042(3) 0.044(3) 0.046(2) -0.008(2) -0.014(2) 0.005(2) C10 0.071(4) 0.043(3) 0.061(3) -0.018(2) -0.025(3) 0.010(3) C11 0.039(3) 0.031(2) 0.043(2) 0.006(2) -0.004(2) -0.007(2) C12 0.032(2) 0.036(2) 0.026(2) 0.005(2) 0.000(2) -0.005(2) C13 0.037(2) 0.026(2) 0.036(2) 0.002(2) -0.002(2) -0.002(2) C14 0.041(3) 0.029(2) 0.052(3) -0.001(2) -0.002(2) -0.003(2) C15 0.040(3) 0.051(3) 0.088(4) 0.011(3) -0.017(3) -0.005(2) C16 0.039(2) 0.040(2) 0.033(2) 0.001(2) -0.004(2) -0.005(2) C17 0.037(2) 0.029(2) 0.037(2) 0.003(2) -0.003(2) -0.003(2) C18 0.036(2) 0.033(2) 0.034(2) 0.001(2) -0.002(2) -0.004(2) C19 0.050(3) 0.064(3) 0.036(2) 0.003(2) -0.007(2) -0.019(3) C20 0.075(4) 0.061(3) 0.030(2) 0.012(2) -0.010(2) -0.025(3) C21 0.037(2) 0.035(2) 0.031(2) 0.004(2) -0.006(2) 0.001(2) C22 0.034(2) 0.042(3) 0.037(2) 0.006(2) -0.007(2) 0.007(2) C23 0.040(3) 0.052(3) 0.034(2) 0.002(2) -0.006(2) 0.005(2) C24 0.040(3) 0.120(6) 0.053(3) -0.008(4) 0.004(3) 0.026(3) C25 0.045(3) 0.076(4) 0.032(2) 0.013(2) 0.002(2) 0.010(3) C26 0.041(3) 0.037(2) 0.037(2) 0.005(2) -0.015(2) 0.003(2) C27 0.036(2) 0.047(3) 0.031(2) 0.001(2) -0.004(2) -0.001(2) C28 0.036(2) 0.041(3) 0.036(2) -0.002(2) -0.011(2) 0.003(2) C29 0.059(3) 0.055(3) 0.054(3) 0.008(3) -0.022(3) -0.016(3) C30 0.081(4) 0.054(3) 0.061(4) 0.016(3) -0.025(3) -0.007(3) C31 0.040(3) 0.049(3) 0.047(3) -0.011(2) -0.011(2) 0.012(2) C32 0.039(2) 0.031(2) 0.040(2) -0.008(2) -0.003(2) 0.008(2) C33 0.035(2) 0.030(2) 0.035(2) 0.000(2) -0.004(2) 0.007(2) C34 0.041(3) 0.031(2) 0.074(4) -0.002(2) -0.007(2) 0.001(2) C35 0.050(3) 0.061(4) 0.121(6) -0.037(4) -0.038(4) 0.018(3) C36 0.046(3) 0.039(2) 0.034(2) -0.006(2) -0.002(2) 0.015(2) C37 0.036(2) 0.034(2) 0.031(2) -0.007(2) -0.002(2) 0.008(2) C38 0.032(2) 0.031(2) 0.035(2) -0.004(2) -0.004(2) 0.004(2) C39 0.050(3) 0.056(3) 0.032(2) -0.002(2) -0.008(2) 0.016(2) C40 0.077(4) 0.080(4) 0.034(3) -0.016(3) -0.002(3) 0.033(4) C41 0.081(4) 0.052(3) 0.046(3) -0.009(3) 0.004(3) 0.014(3) C42 0.047(3) 0.040(2) 0.038(2) 0.004(2) 0.002(2) 0.003(2) C43 0.085(5) 0.095(5) 0.057(4) 0.008(3) -0.022(3) -0.022(4) C44 0.180(15) 0.146(13) 0.144(12) -0.028(10) -0.057(11) 0.039(12) Cl1 0.113(2) 0.095(2) 0.127(2) 0.0291(15) -0.003(2) -0.0161(14) Cl2 0.125(2) 0.131(2) 0.112(2) -0.037(2) -0.005(2) -0.027(2) Cl3 0.126(2) 0.171(3) 0.0605(11) 0.0119(13) 0.0087(11) -0.044(2) Cl4 0.251(6) 0.118(2) 0.159(3) -0.019(2) 0.063(4) -0.010(3) Cl5 0.233(5) 0.123(3) 0.135(3) 0.001(2) 0.050(3) -0.028(3) Cl6 0.140(3) 0.166(3) 0.133(3) 0.045(2) 0.011(2) 0.004(2) O5 0.047(2) 0.045(2) 0.041(2) 0.0014(15) 0.0008(14) -0.0002(15) C45 0.064(4) 0.061(4) 0.083(4) -0.016(3) 0.000(3) 0.015(3) O6 0.065(2) 0.060(2) 0.061(2) -0.006(2) 0.005(2) -0.006(2) C46 0.087(6) 0.112(7) 0.119(7) -0.023(6) -0.001(6) -0.021(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 Co1 N17 2.056(4) . ? Co1 N15 2.150(4) 1_455 ? Co1 N5 2.165(4) . ? Co1 O2 2.171(3) . ? Co1 N1 2.189(4) . ? Co1 N3 2.217(4) 4_565 ? Co2 N18 2.038(4) . ? Co2 O1 2.154(3) 3_755 ? Co2 N9 2.164(4) . ? Co2 N14 2.165(4) . ? Co2 N7 2.188(4) . ? Co2 N12 2.194(4) 4_575 ? S1 O3 1.463(3) . ? S1 O4 1.469(3) . ? S1 O1 1.472(3) . ? S1 O2 1.487(3) . ? S2 C42 1.621(5) . ? S3 C41 1.640(6) . ? O1 Co2 2.154(3) 3_745 ? N1 C1 1.344(6) . ? N1 N2 1.366(6) . ? N2 C3 1.345(6) . ? N3 C8 1.329(6) . ? N3 N4 1.362(6) . ? N3 Co1 2.217(4) 4_465 ? N4 C6 1.345(6) . ? N5 C13 1.337(6) . ? N5 N6 1.353(6) . ? N6 C11 1.347(7) . ? N7 C18 1.319(6) . ? N7 N8 1.353(5) . ? N8 C16 1.337(7) . ? N9 C21 1.326(6) . ? N9 N10 1.348(6) . ? N10 C23 1.349(7) . ? N11 C26 1.351(6) . ? N11 N12 1.358(6) . ? N12 C28 1.336(6) . ? N12 Co2 2.194(4) 4_475 ? N13 N14 1.332(6) . ? N13 C31 1.349(7) . ? N14 C33 1.332(6) . ? N15 C38 1.335(6) . ? N15 N16 1.359(5) . ? N15 Co1 2.150(4) 1_655 ? N16 C36 1.338(6) . ? N17 C42 1.158(6) . ? N18 C41 1.126(7) . ? C1 C2 1.415(7) . ? C1 C5 1.479(7) . ? C2 C3 1.386(7) . ? C2 C7 1.480(6) . ? C3 C4 1.503(8) . ? C6 C7 1.387(7) . ? C6 C10 1.503(8) . ? C7 C8 1.397(7) . ? C8 C9 1.502(7) . ? C11 C12 1.364(7) . ? C11 C15 1.487(8) . ? C12 C13 1.410(7) . ? C12 C17 1.467(7) . ? C13 C14 1.498(7) . ? C16 C17 1.395(7) . ? C16 C20 1.490(7) . ? C17 C18 1.413(7) . ? C18 C19 1.490(7) . ? C21 C22 1.409(8) . ? C21 C25 1.473(8) . ? C22 C23 1.371(8) . ? C22 C27 1.473(7) . ? C23 C24 1.482(9) . ? C26 C27 1.397(8) . ? C26 C30 1.478(9) . ? C27 C28 1.407(8) . ? C28 C29 1.485(8) . ? C31 C32 1.401(8) . ? C31 C35 1.474(9) . ? C32 C33 1.410(7) . ? C32 C37 1.466(7) . ? C33 C34 1.491(8) . ? C36 C37 1.385(7) . ? C36 C40 1.490(7) . ? C37 C38 1.418(7) . ? C38 C39 1.479(7) . ? C43 Cl3 1.736(10) . ? C43 Cl1 1.743(9) . ? C43 Cl2 1.780(9) . ? C44 Cl4 1.55(2) . ? C44 Cl5 1.65(3) . ? C44 Cl6 1.88(2) . ? O5 C45 1.403(8) . ? O6 C46 1.424(12) . ? 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 N17 Co1 N15 94.9(2) . 1_455 ? N17 Co1 N5 90.8(2) . . ? N15 Co1 N5 88.96(14) 1_455 . ? N17 Co1 O2 170.35(14) . . ? N15 Co1 O2 94.77(13) 1_455 . ? N5 Co1 O2 88.86(13) . . ? N17 Co1 N1 93.6(2) . . ? N15 Co1 N1 87.61(14) 1_455 . ? N5 Co1 N1 174.63(14) . . ? O2 Co1 N1 87.32(13) . . ? N17 Co1 N3 89.08(15) . 4_565 ? N15 Co1 N3 175.76(15) 1_455 4_565 ? N5 Co1 N3 92.52(15) . 4_565 ? O2 Co1 N3 81.30(13) . 4_565 ? N1 Co1 N3 90.62(14) . 4_565 ? N18 Co2 O1 173.80(15) . 3_755 ? N18 Co2 N9 93.5(2) . . ? O1 Co2 N9 86.96(13) 3_755 . ? N18 Co2 N14 93.1(2) . . ? O1 Co2 N14 86.41(13) 3_755 . ? N9 Co2 N14 173.36(15) . . ? N18 Co2 N7 92.4(2) . . ? O1 Co2 N7 81.41(13) 3_755 . ? N9 Co2 N7 89.9(2) . . ? N14 Co2 N7 89.10(15) . . ? N18 Co2 N12 90.8(2) . 4_575 ? O1 Co2 N12 95.36(13) 3_755 4_575 ? N9 Co2 N12 90.6(2) . 4_575 ? N14 Co2 N12 90.0(2) . 4_575 ? N7 Co2 N12 176.69(15) . 4_575 ? O3 S1 O4 111.5(2) . . ? O3 S1 O1 110.3(2) . . ? O4 S1 O1 108.8(2) . . ? O3 S1 O2 109.6(2) . . ? O4 S1 O2 109.3(2) . . ? O1 S1 O2 107.2(2) . . ? S1 O1 Co2 135.8(2) . 3_745 ? S1 O2 Co1 139.4(2) . . ? C1 N1 N2 105.4(4) . . ? C1 N1 Co1 136.3(3) . . ? N2 N1 Co1 115.8(3) . . ? C3 N2 N1 112.1(4) . . ? C8 N3 N4 105.1(3) . . ? C8 N3 Co1 132.3(3) . 4_465 ? N4 N3 Co1 113.8(3) . 4_465 ? C6 N4 N3 111.8(4) . . ? C13 N5 N6 105.0(4) . . ? C13 N5 Co1 130.7(3) . . ? N6 N5 Co1 118.8(3) . . ? C11 N6 N5 112.3(4) . . ? C18 N7 N8 105.9(4) . . ? C18 N7 Co2 134.5(3) . . ? N8 N7 Co2 115.7(3) . . ? C16 N8 N7 112.2(4) . . ? C21 N9 N10 105.2(4) . . ? C21 N9 Co2 132.0(3) . . ? N10 N9 Co2 117.1(3) . . ? N9 N10 C23 112.2(4) . . ? C26 N11 N12 112.7(4) . . ? C28 N12 N11 105.3(4) . . ? C28 N12 Co2 130.4(3) . 4_475 ? N11 N12 Co2 116.6(3) . 4_475 ? N14 N13 C31 112.4(4) . . ? C33 N14 N13 106.9(4) . . ? C33 N14 Co2 132.5(3) . . ? N13 N14 Co2 118.4(3) . . ? C38 N15 N16 105.2(3) . . ? C38 N15 Co1 133.1(3) . 1_655 ? N16 N15 Co1 119.9(3) . 1_655 ? C36 N16 N15 112.8(4) . . ? C42 N17 Co1 164.5(4) . . ? C41 N18 Co2 172.8(5) . . ? N1 C1 C2 110.1(4) . . ? N1 C1 C5 122.3(4) . . ? C2 C1 C5 127.6(4) . . ? C3 C2 C1 105.5(4) . . ? C3 C2 C7 126.2(4) . . ? C1 C2 C7 128.3(4) . . ? N2 C3 C2 106.9(4) . . ? N2 C3 C4 122.4(4) . . ? C2 C3 C4 130.6(5) . . ? N4 C6 C7 106.8(4) . . ? N4 C6 C10 122.5(5) . . ? C7 C6 C10 130.7(5) . . ? C6 C7 C8 105.0(4) . . ? C6 C7 C2 126.5(4) . . ? C8 C7 C2 128.4(4) . . ? N3 C8 C7 111.3(4) . . ? N3 C8 C9 121.3(4) . . ? C7 C8 C9 127.3(4) . . ? N6 C11 C12 106.8(4) . . ? N6 C11 C15 121.1(4) . . ? C12 C11 C15 132.1(5) . . ? C11 C12 C13 105.6(4) . . ? C11 C12 C17 127.8(4) . . ? C13 C12 C17 126.5(4) . . ? N5 C13 C12 110.3(4) . . ? N5 C13 C14 122.2(4) . . ? C12 C13 C14 127.5(4) . . ? N8 C16 C17 106.6(4) . . ? N8 C16 C20 121.2(4) . . ? C17 C16 C20 132.2(5) . . ? C16 C17 C18 104.6(4) . . ? C16 C17 C12 127.2(4) . . ? C18 C17 C12 128.1(4) . . ? N7 C18 C17 110.7(4) . . ? N7 C18 C19 122.3(4) . . ? C17 C18 C19 127.0(5) . . ? N9 C21 C22 110.9(4) . . ? N9 C21 C25 122.7(5) . . ? C22 C21 C25 126.4(4) . . ? C23 C22 C21 105.0(4) . . ? C23 C22 C27 127.4(5) . . ? C21 C22 C27 127.6(4) . . ? N10 C23 C22 106.7(5) . . ? N10 C23 C24 121.1(5) . . ? C22 C23 C24 132.1(5) . . ? N11 C26 C27 105.7(4) . . ? N11 C26 C30 123.2(5) . . ? C27 C26 C30 131.1(5) . . ? C26 C27 C28 105.6(4) . . ? C26 C27 C22 125.1(5) . . ? C28 C27 C22 129.3(5) . . ? N12 C28 C27 110.6(4) . . ? N12 C28 C29 123.4(5) . . ? C27 C28 C29 125.9(4) . . ? N13 C31 C32 105.8(5) . . ? N13 C31 C35 123.2(5) . . ? C32 C31 C35 131.0(5) . . ? C31 C32 C33 105.3(4) . . ? C31 C32 C37 126.6(5) . . ? C33 C32 C37 128.1(5) . . ? N14 C33 C32 109.6(4) . . ? N14 C33 C34 123.3(4) . . ? C32 C33 C34 127.1(4) . . ? N16 C36 C37 106.4(4) . . ? N16 C36 C40 121.9(5) . . ? C37 C36 C40 131.6(5) . . ? C36 C37 C38 105.3(4) . . ? C36 C37 C32 127.0(4) . . ? C38 C37 C32 127.7(4) . . ? N15 C38 C37 110.2(4) . . ? N15 C38 C39 122.5(4) . . ? C37 C38 C39 127.3(4) . . ? N18 C41 S3 177.5(7) . . ? N17 C42 S2 179.5(5) . . ? Cl3 C43 Cl1 112.0(6) . . ? Cl3 C43 Cl2 110.7(5) . . ? Cl1 C43 Cl2 106.7(4) . . ? Cl4 C44 Cl5 122.1(18) . . ? Cl4 C44 Cl6 111.6(12) . . ? Cl5 C44 Cl6 107.5(9) . . ? _refine_diff_density_max 0.674 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.062 #============================================================================== data_c1066 _database_code_CSD 175730 _audit_creation_method SHELXL _chemical_name_systematic ; Tetrakis(3,3',5,5'-Tetramethyl-4,4'-bipyrazolyl) Sulfato Bis(thiocyanato) Dinickel(II), Bis(methanol) Bis(chloroform) Solvate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H66 Cl6 N18 Ni2 O6 S3' _chemical_formula_weight 1393.47 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.6250(14) _cell_length_b 21.376(2) _cell_length_c 22.072(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6428.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour light-green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method ? _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD Siemens' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59185 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.28 _reflns_number_total 15614 _reflns_number_observed 12729 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1356 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+8.5034P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.490(13) _refine_ls_number_reflns 14258 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_obs 0.0496 _refine_ls_wR_factor_all 0.1762 _refine_ls_wR_factor_obs 0.1149 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.585 _refine_ls_restrained_S_obs 1.056 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.77421(3) 0.84666(2) 0.13415(2) 0.01631(9) Uani 1 d . . Ni2 Ni 1.26884(3) 1.15378(2) 0.13122(2) 0.01797(9) Uani 1 d . . S1 S 0.71297(5) 0.76505(3) 0.26233(3) 0.01769(14) Uani 1 d . . S2 S 0.86615(12) 0.95452(8) -0.04581(6) 0.0687(4) Uani 1 d . . S3 S 1.2620(3) 1.03248(13) -0.04981(10) 0.1384(12) Uani 1 d . . O1 O 0.7491(2) 0.70507(10) 0.28632(10) 0.0232(5) Uani 1 d . . O2 O 0.7630(2) 0.77585(11) 0.20358(10) 0.0233(5) Uani 1 d . . O3 O 0.7364(2) 0.81581(11) 0.30436(10) 0.0316(5) Uani 1 d . . O4 O 0.6071(2) 0.76051(13) 0.25149(11) 0.0302(5) Uani 1 d . . N1 N 0.6530(2) 0.80195(14) 0.09048(12) 0.0211(6) Uani 1 d . . N2 N 0.5739(2) 0.79033(15) 0.12607(13) 0.0242(6) Uani 1 d . . H2A H 0.5754(2) 0.79167(15) 0.16500(13) 0.029 Uiso 1 calc R . N3 N 0.3740(2) 0.72034(14) -0.09554(13) 0.0222(6) Uani 1 d . . N4 N 0.3344(2) 0.77776(14) -0.08417(13) 0.0239(6) Uani 1 d . . H4D H 0.2856(2) 0.79309(14) -0.10392(13) 0.029 Uiso 1 calc R . N5 N 0.8876(2) 0.89067(13) 0.18398(13) 0.0208(5) Uani 1 d . . N6 N 0.9651(2) 0.85588(14) 0.20273(14) 0.0244(6) Uani 1 d . . H6A H 0.9632(2) 0.81598(14) 0.20756(14) 0.029 Uiso 1 calc R . N7 N 1.1681(2) 1.09269(14) 0.17423(12) 0.0216(6) Uani 1 d . . N8 N 1.1869(2) 1.07873(14) 0.23318(13) 0.0237(6) Uani 1 d . . H8A H 1.2262(2) 1.10011(14) 0.25559(13) 0.028 Uiso 1 calc R . N9 N 1.1498(2) 1.20550(15) 0.09552(13) 0.0232(6) Uani 1 d . . N10 N 1.0709(2) 1.2132(2) 0.13137(15) 0.0288(6) Uani 1 d . . H10D H 1.0726(2) 1.2099(2) 0.17019(15) 0.035 Uiso 1 calc R . N11 N 0.8419(2) 1.22286(15) -0.08357(14) 0.0280(6) Uani 1 d . . H11A H 0.7984(2) 1.20509(15) -0.10596(14) 0.034 Uiso 1 calc R . N12 N 0.8717(2) 1.28203(15) -0.09127(14) 0.0252(6) Uani 1 d . . N13 N 1.4569(2) 1.14055(15) 0.19877(14) 0.0267(6) Uani 1 d . . H13A H 1.4531(2) 1.18016(15) 0.20514(14) 0.032 Uiso 1 calc R . N14 N 1.3846(2) 1.10646(15) 0.17429(14) 0.0246(6) Uani 1 d . . N15 N 1.6728(2) 0.90749(13) 0.17445(12) 0.0206(6) Uani 1 d . . N16 N 1.6760(2) 0.91716(13) 0.23525(13) 0.0234(6) Uani 1 d . . H16A H 1.7102(2) 0.89499(13) 0.25999(13) 0.028 Uiso 1 calc R . N17 N 0.8010(2) 0.90336(14) 0.06266(13) 0.0260(6) Uani 1 d . . N18 N 1.2763(3) 1.09867(15) 0.05735(14) 0.0311(6) Uani 1 d . . C1 C 0.6202(3) 0.7952(2) 0.03360(15) 0.0238(7) Uani 1 d . . C2 C 0.5200(3) 0.7793(2) 0.03326(15) 0.0245(7) Uani 1 d . . C3 C 0.4924(3) 0.7764(2) 0.0937(2) 0.0286(8) Uani 1 d . . C4 C 0.3979(3) 0.7606(3) 0.1227(2) 0.0537(13) Uani 1 d . . H4A H 0.4046(3) 0.7633(3) 0.1660(2) 0.064 Uiso 1 calc R . H4B H 0.3791(3) 0.7189(3) 0.1117(2) 0.064 Uiso 1 calc R . H4C H 0.3484(3) 0.7895(3) 0.1095(2) 0.064 Uiso 1 calc R . C5 C 0.6854(3) 0.8028(2) -0.0204(2) 0.0373(9) Uani 1 d . . H5A H 0.7503(3) 0.8138(2) -0.0073(2) 0.045 Uiso 1 calc R . H5B H 0.6599(3) 0.8353(2) -0.0460(2) 0.045 Uiso 1 calc R . H5C H 0.6877(3) 0.7642(2) -0.0426(2) 0.045 Uiso 1 calc R . C6 C 0.3799(3) 0.8076(2) -0.0388(2) 0.0284(7) Uani 1 d . . C7 C 0.4543(2) 0.7686(2) -0.01890(15) 0.0234(7) Uani 1 d . . C8 C 0.4480(2) 0.7152(2) -0.0557(2) 0.0223(7) Uani 1 d . . C9 C 0.5147(3) 0.6595(2) -0.0548(2) 0.0337(8) Uani 1 d . . H9A H 0.4934(3) 0.6298(2) -0.0847(2) 0.040 Uiso 1 calc R . H9B H 0.5128(3) 0.6404(2) -0.0155(2) 0.040 Uiso 1 calc R . H9C H 0.5805(3) 0.6725(2) -0.0637(2) 0.040 Uiso 1 calc R . C10 C 0.3470(4) 0.8704(2) -0.0169(2) 0.0464(11) Uani 1 d . . H10A H 0.2928(4) 0.8846(2) -0.0411(2) 0.056 Uiso 1 calc R . H10B H 0.4002(4) 0.8997(2) -0.0202(2) 0.056 Uiso 1 calc R . H10C H 0.3268(4) 0.8673(2) 0.0247(2) 0.056 Uiso 1 calc R . C11 C 1.0451(3) 0.8909(2) 0.2128(2) 0.0277(7) Uani 1 d . . C12 C 1.0197(3) 0.9518(2) 0.20128(15) 0.0234(7) Uani 1 d . . C13 C 0.9200(3) 0.9497(2) 0.1838(2) 0.0236(7) Uani 1 d . . C14 C 0.8545(3) 1.0040(2) 0.1691(2) 0.0307(8) Uani 1 d . . H14A H 0.7903(3) 0.9889(2) 0.1587(2) 0.037 Uiso 1 calc R . H14B H 0.8814(3) 1.0269(2) 0.1356(2) 0.037 Uiso 1 calc R . H14C H 0.8498(3) 1.0310(2) 0.2038(2) 0.037 Uiso 1 calc R . C15 C 1.1400(3) 0.8617(2) 0.2312(3) 0.0526(13) Uani 1 d . . H15A H 1.1313(3) 0.8173(2) 0.2354(3) 0.063 Uiso 1 calc R . H15B H 1.1610(3) 0.8790(2) 0.2691(3) 0.063 Uiso 1 calc R . H15C H 1.1887(3) 0.8698(2) 0.2007(3) 0.063 Uiso 1 calc R . C16 C 1.1382(3) 1.0284(2) 0.2527(2) 0.0272(7) Uani 1 d . . C17 C 1.0831(3) 1.0072(2) 0.2034(2) 0.0244(7) Uani 1 d . . C18 C 1.1048(3) 1.0491(2) 0.1559(2) 0.0236(7) Uani 1 d . . C19 C 1.0651(4) 1.0477(2) 0.0928(2) 0.0413(10) Uani 1 d . . H19A H 1.0923(4) 1.0818(2) 0.0700(2) 0.050 Uiso 1 calc R . H19B H 0.9949(4) 1.0516(2) 0.0939(2) 0.050 Uiso 1 calc R . H19C H 1.0825(4) 1.0088(2) 0.0738(2) 0.050 Uiso 1 calc R . C20 C 1.1484(4) 1.0046(2) 0.3151(2) 0.0427(10) Uani 1 d . . H20A H 1.1928(4) 1.0309(2) 0.3373(2) 0.051 Uiso 1 calc R . H20B H 1.1735(4) 0.9627(2) 0.3141(2) 0.051 Uiso 1 calc R . H20C H 1.0854(4) 1.0048(2) 0.3346(2) 0.051 Uiso 1 calc R . C21 C 1.1178(3) 1.2150(2) 0.0392(2) 0.0249(7) Uani 1 d . . C22 C 1.0155(3) 1.2281(2) 0.0398(2) 0.0287(8) Uani 1 d . . C23 C 0.9895(3) 1.2266(2) 0.1001(2) 0.0331(8) Uani 1 d . . C24 C 0.8932(4) 1.2375(4) 0.1297(2) 0.066(2) Uani 1 d . . H24A H 0.9000(4) 1.2329(4) 0.1727(2) 0.079 Uiso 1 calc R . H24B H 0.8463(4) 1.2077(4) 0.1148(2) 0.079 Uiso 1 calc R . H24C H 0.8709(4) 1.2791(4) 0.1206(2) 0.079 Uiso 1 calc R . C25 C 1.1819(3) 1.2130(3) -0.0149(2) 0.0444(11) Uani 1 d . . H25A H 1.2478(3) 1.2031(3) -0.0028(2) 0.053 Uiso 1 calc R . H25B H 1.1812(3) 1.2531(3) -0.0346(2) 0.053 Uiso 1 calc R . H25C H 1.1584(3) 1.1816(3) -0.0425(2) 0.053 Uiso 1 calc R . C26 C 0.8873(3) 1.1941(2) -0.0370(2) 0.0324(8) Uani 1 d . . C27 C 0.9509(3) 1.2376(2) -0.0129(2) 0.0287(7) Uani 1 d . . C28 C 0.9401(3) 1.2919(2) -0.0484(2) 0.0294(8) Uani 1 d . . C29 C 0.9960(4) 1.3509(3) -0.0422(2) 0.0481(11) Uani 1 d . . H29A H 0.9740(4) 1.3803(3) -0.0721(2) 0.058 Uiso 1 calc R . H29B H 1.0647(4) 1.3427(3) -0.0480(2) 0.058 Uiso 1 calc R . H29C H 0.9858(4) 1.3680(3) -0.0025(2) 0.058 Uiso 1 calc R . C30 C 0.8671(5) 1.1280(2) -0.0206(3) 0.0556(14) Uani 1 d . . H30A H 0.8177(5) 1.1113(2) -0.0471(3) 0.067 Uiso 1 calc R . H30B H 0.8442(5) 1.1260(2) 0.0205(3) 0.067 Uiso 1 calc R . H30C H 0.9262(5) 1.1039(2) -0.0245(3) 0.067 Uiso 1 calc R . C31 C 1.5367(3) 1.1056(2) 0.2123(2) 0.0342(9) Uani 1 d . . C32 C 1.5139(3) 1.0445(2) 0.1956(2) 0.0271(7) Uani 1 d . . C33 C 1.4173(3) 1.0476(2) 0.1727(2) 0.0244(7) Uani 1 d . . C34 C 1.3575(3) 0.9944(2) 0.1494(2) 0.0366(9) Uani 1 d . . H34A H 1.2944(3) 1.0096(2) 0.1366(2) 0.044 Uiso 1 calc R . H34B H 1.3490(3) 0.9639(2) 0.1809(2) 0.044 Uiso 1 calc R . H34C H 1.3904(3) 0.9755(2) 0.1156(2) 0.044 Uiso 1 calc R . C35 C 1.6274(4) 1.1333(3) 0.2386(3) 0.0598(15) Uani 1 d . . H35A H 1.6180(4) 1.1773(3) 0.2447(3) 0.072 Uiso 1 calc R . H35B H 1.6813(4) 1.1267(3) 0.2114(3) 0.072 Uiso 1 calc R . H35C H 1.6414(4) 1.1136(3) 0.2768(3) 0.072 Uiso 1 calc R . C36 C 1.6192(3) 0.9656(2) 0.2521(2) 0.0291(8) Uani 1 d . . C37 C 1.5780(3) 0.9898(2) 0.2004(2) 0.0264(7) Uani 1 d . . C38 C 1.6122(3) 0.9516(2) 0.15285(15) 0.0229(7) Uani 1 d . . C39 C 1.5891(3) 0.9579(2) 0.0870(2) 0.0352(9) Uani 1 d . . H39A H 1.6223(3) 0.9256(2) 0.0648(2) 0.042 Uiso 1 calc R . H39B H 1.6106(3) 0.9981(2) 0.0728(2) 0.042 Uiso 1 calc R . H39C H 1.5196(3) 0.9540(2) 0.0811(2) 0.042 Uiso 1 calc R . C40 C 1.6076(4) 0.9825(3) 0.3177(2) 0.0548(14) Uani 1 d . . H40A H 1.6479(4) 0.9555(3) 0.3420(2) 0.066 Uiso 1 calc R . H40B H 1.5401(4) 0.9777(3) 0.3294(2) 0.066 Uiso 1 calc R . H40C H 1.6273(4) 1.0252(3) 0.3238(2) 0.066 Uiso 1 calc R . C41 C 1.2731(5) 1.0718(2) 0.0136(2) 0.0507(11) Uani 1 d . . C42 C 0.8284(3) 0.9248(2) 0.0179(2) 0.0311(7) Uani 1 d . . C43 C 0.6351(5) 1.0082(4) -0.1068(3) 0.072(2) Uani 1 d . . H43A H 0.6937 0.9988 -0.0830 0.087 Uiso 1 d . . C44 C 0.4245(15) 0.8421(8) 0.3261(8) 0.153(5) Uani 1 d . . H44A H 0.5005 0.8276 0.3287 0.183 Uiso 1 d . . Cl1 Cl 0.6440(4) 1.0836(2) -0.1363(2) 0.069(2) Uani 0.55(2) d P . Cl2 Cl 0.6360(10) 0.9513(5) -0.1647(6) 0.139(5) Uani 0.55(2) d P . Cl3 Cl 0.5305(6) 1.0031(3) -0.0606(2) 0.084(2) Uani 0.55(2) d P . Cl1A Cl 0.6160(17) 1.0863(10) -0.1217(15) 0.209(8) Uani 0.45(2) d P . Cl2A Cl 0.6305(7) 0.9645(7) -0.1718(4) 0.104(4) Uani 0.45(2) d P . Cl3A Cl 0.5421(12) 0.9730(19) -0.0649(7) 0.193(10) Uani 0.45(2) d P . Cl4 Cl 0.4088(6) 0.8942(2) 0.3709(3) 0.206(3) Uani 1 d . . Cl5 Cl 0.3760(5) 0.7731(2) 0.3260(2) 0.189(2) Uani 1 d . . Cl6 Cl 0.4274(4) 0.8725(3) 0.2450(2) 0.171(2) Uani 1 d . . O5 O 0.9530(2) 0.72300(13) 0.23287(13) 0.0350(6) Uani 1 d . . C45 C 1.0043(4) 0.6763(3) 0.2003(3) 0.0617(14) Uani 1 d . . H45A H 1.0635(4) 0.6662(3) 0.2216(3) 0.074 Uiso 1 d R . H45B H 1.0202(4) 0.6915(3) 0.1606(3) 0.074 Uiso 1 d R . H45C H 0.9643(4) 0.6396(3) 0.1968(3) 0.074 Uiso 1 d R . O6 O 0.6937(3) 0.6448(2) 0.1602(2) 0.0541(8) Uani 1 d . . C46 C 0.6138(6) 0.6105(4) 0.1347(5) 0.089(2) Uani 1 d . . H46A H 0.6381(6) 0.5724(4) 0.1172(5) 0.107 Uiso 1 d R . H46B H 0.5822(6) 0.6350(4) 0.1040(5) 0.107 Uiso 1 d R . H46C H 0.5675(6) 0.6007(4) 0.1661(5) 0.107 Uiso 1 d R . 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 Ni1 0.0172(2) 0.0174(2) 0.0143(2) -0.00135(15) 0.00042(14) 0.00023(15) Ni2 0.0178(2) 0.0191(2) 0.0170(2) 0.0013(2) 0.00017(15) 0.0007(2) S1 0.0212(3) 0.0172(3) 0.0146(3) 0.0018(2) 0.0004(3) -0.0004(3) S2 0.0740(9) 0.0885(10) 0.0435(6) 0.0403(7) 0.0159(6) 0.0026(8) S3 0.228(3) 0.123(2) 0.0643(10) -0.0647(12) -0.021(2) 0.058(2) O1 0.0280(12) 0.0208(11) 0.0208(10) 0.0032(8) 0.0003(9) 0.0049(9) O2 0.0253(11) 0.0241(11) 0.0205(10) 0.0028(8) 0.0068(9) -0.0003(9) O3 0.054(2) 0.0202(11) 0.0204(10) -0.0001(9) -0.0014(11) -0.0033(11) O4 0.0203(11) 0.0384(13) 0.0318(13) 0.0117(10) 0.0002(9) -0.0007(10) N1 0.0188(13) 0.0251(14) 0.0196(12) -0.0026(10) -0.0011(10) -0.0038(11) N2 0.0214(13) 0.035(2) 0.0160(12) -0.0023(11) -0.0024(11) -0.0059(11) N3 0.0232(14) 0.0244(15) 0.0191(13) -0.0013(10) -0.0055(11) -0.0019(11) N4 0.0224(13) 0.0229(14) 0.0264(14) -0.0017(11) -0.0073(11) 0.0006(11) N5 0.0210(13) 0.0187(13) 0.0227(13) 0.0000(10) -0.0020(11) -0.0018(11) N6 0.0248(13) 0.0169(14) 0.0316(14) 0.0057(11) -0.0046(11) -0.0005(11) N7 0.0245(13) 0.0232(14) 0.0171(12) 0.0008(10) -0.0027(11) -0.0037(11) N8 0.0263(14) 0.0269(14) 0.0179(12) 0.0030(11) -0.0023(11) -0.0085(11) N9 0.0223(14) 0.029(2) 0.0181(12) 0.0057(11) -0.0001(11) 0.0011(11) N10 0.0234(13) 0.040(2) 0.0227(13) 0.0030(13) -0.0028(12) 0.0070(12) N11 0.032(2) 0.026(2) 0.0259(14) 0.0016(12) -0.0101(13) 0.0002(13) N12 0.0233(14) 0.0252(15) 0.0270(14) 0.0049(11) -0.0028(11) -0.0023(11) N13 0.0231(14) 0.024(2) 0.0331(15) -0.0072(12) -0.0050(11) 0.0060(12) N14 0.0211(13) 0.0244(14) 0.0283(14) -0.0018(11) -0.0025(11) 0.0031(12) N15 0.0219(13) 0.0219(14) 0.0179(12) -0.0047(10) -0.0025(11) 0.0039(11) N16 0.0295(14) 0.0229(13) 0.0178(12) -0.0022(11) -0.0038(11) 0.0065(11) N17 0.0279(15) 0.0285(14) 0.0216(13) 0.0025(11) -0.0002(11) 0.0019(12) N18 0.034(2) 0.034(2) 0.0252(14) -0.0036(12) 0.0007(13) 0.0028(14) C1 0.026(2) 0.029(2) 0.0168(14) -0.0060(12) -0.0026(12) 0.0003(13) C2 0.025(2) 0.031(2) 0.0177(14) -0.0014(13) -0.0045(12) -0.0041(14) C3 0.020(2) 0.040(2) 0.026(2) -0.0001(15) -0.0034(13) -0.0104(15) C4 0.030(2) 0.096(4) 0.035(2) 0.001(2) 0.001(2) -0.023(2) C5 0.030(2) 0.065(3) 0.0163(15) -0.008(2) 0.0032(13) -0.009(2) C6 0.031(2) 0.027(2) 0.027(2) 0.0001(14) -0.0049(15) -0.0044(15) C7 0.023(2) 0.027(2) 0.0203(14) -0.0047(13) -0.0038(12) -0.0070(14) C8 0.0215(15) 0.027(2) 0.0185(14) -0.0008(12) -0.0041(12) -0.0013(13) C9 0.027(2) 0.036(2) 0.038(2) -0.005(2) -0.0125(14) 0.005(2) C10 0.052(3) 0.030(2) 0.057(3) -0.019(2) -0.019(2) 0.007(2) C11 0.026(2) 0.025(2) 0.032(2) 0.0061(14) -0.0018(15) -0.0036(14) C12 0.023(2) 0.027(2) 0.0201(14) 0.0025(13) -0.0011(12) -0.0059(13) C13 0.027(2) 0.020(2) 0.024(2) 0.0017(12) -0.0032(13) -0.0015(13) C14 0.033(2) 0.017(2) 0.042(2) -0.0012(14) -0.004(2) -0.0016(14) C15 0.032(2) 0.038(2) 0.088(4) 0.015(2) -0.024(2) -0.005(2) C16 0.028(2) 0.033(2) 0.021(2) 0.0035(13) -0.0030(13) -0.0056(14) C17 0.027(2) 0.024(2) 0.023(2) 0.0013(13) -0.0035(13) -0.0040(13) C18 0.026(2) 0.022(2) 0.023(2) -0.0011(12) -0.0019(13) -0.0027(14) C19 0.044(2) 0.052(3) 0.027(2) 0.009(2) -0.012(2) -0.022(2) C20 0.056(3) 0.044(2) 0.029(2) 0.012(2) -0.005(2) -0.019(2) C21 0.025(2) 0.030(2) 0.0206(15) 0.0028(13) -0.0039(13) 0.0033(13) C22 0.027(2) 0.032(2) 0.027(2) 0.0031(14) -0.0060(13) 0.0054(15) C23 0.029(2) 0.043(2) 0.028(2) 0.000(2) -0.0060(14) 0.007(2) C24 0.033(2) 0.127(5) 0.038(2) -0.003(3) 0.001(2) 0.032(3) C25 0.037(2) 0.070(3) 0.027(2) 0.009(2) -0.001(2) 0.007(2) C26 0.038(2) 0.031(2) 0.029(2) 0.0066(15) -0.011(2) 0.003(2) C27 0.028(2) 0.036(2) 0.022(2) -0.0012(14) -0.0060(13) 0.003(2) C28 0.028(2) 0.031(2) 0.028(2) 0.0036(14) -0.0067(14) -0.0024(15) C29 0.047(2) 0.046(2) 0.051(2) 0.005(2) -0.024(2) -0.016(2) C30 0.072(3) 0.039(2) 0.056(3) 0.017(2) -0.031(3) -0.006(2) C31 0.029(2) 0.035(2) 0.039(2) -0.013(2) -0.013(2) 0.010(2) C32 0.028(2) 0.024(2) 0.029(2) -0.0069(13) -0.0067(13) 0.0092(14) C33 0.025(2) 0.023(2) 0.025(2) -0.0023(13) -0.0006(13) 0.0070(13) C34 0.029(2) 0.024(2) 0.056(2) -0.007(2) -0.008(2) 0.0066(14) C35 0.035(2) 0.049(3) 0.095(4) -0.027(3) -0.026(3) 0.009(2) C36 0.033(2) 0.030(2) 0.024(2) -0.0090(13) -0.0059(14) 0.0138(15) C37 0.025(2) 0.029(2) 0.025(2) -0.0057(14) -0.0037(13) 0.0097(14) C38 0.022(2) 0.025(2) 0.021(2) -0.0059(12) -0.0049(12) 0.0066(13) C39 0.038(2) 0.044(2) 0.023(2) -0.0010(15) -0.0090(15) 0.019(2) C40 0.072(3) 0.069(3) 0.023(2) -0.016(2) -0.006(2) 0.038(3) C41 0.075(3) 0.046(2) 0.032(2) -0.007(2) 0.006(2) 0.020(2) C42 0.033(2) 0.033(2) 0.028(2) 0.0061(14) 0.0000(15) 0.0009(15) C43 0.070(4) 0.087(5) 0.060(3) 0.009(3) -0.019(3) -0.020(3) C44 0.190(14) 0.133(10) 0.134(10) -0.030(8) -0.022(10) 0.025(10) Cl1 0.064(2) 0.056(2) 0.087(3) 0.0272(14) 0.003(2) -0.0115(14) Cl2 0.146(8) 0.088(4) 0.183(10) -0.032(4) -0.024(6) -0.050(4) Cl3 0.102(3) 0.111(4) 0.037(2) 0.007(2) 0.013(2) -0.047(2) Cl1A 0.128(9) 0.212(15) 0.288(21) 0.025(12) 0.018(11) -0.042(8) Cl2A 0.083(4) 0.166(9) 0.065(3) -0.041(4) -0.009(2) 0.000(5) Cl3A 0.123(7) 0.357(27) 0.099(6) 0.106(11) -0.039(5) -0.104(12) Cl4 0.308(7) 0.135(3) 0.175(4) -0.018(3) 0.070(5) -0.014(4) Cl5 0.271(6) 0.143(3) 0.154(3) -0.008(2) 0.061(4) -0.044(4) Cl6 0.158(3) 0.198(4) 0.157(3) 0.053(3) 0.012(3) -0.006(3) O5 0.0331(13) 0.0343(14) 0.0377(14) -0.0001(11) 0.0028(11) 0.0018(11) C45 0.057(3) 0.053(3) 0.075(4) -0.017(3) 0.003(3) 0.014(2) O6 0.054(2) 0.050(2) 0.058(2) -0.003(2) 0.0028(15) -0.011(2) C46 0.067(4) 0.089(5) 0.113(6) -0.035(5) 0.003(4) -0.018(4) _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 Ni1 N17 2.023(3) . ? Ni1 N15 2.095(3) 1_455 ? Ni1 N5 2.117(3) . ? Ni1 N1 2.138(3) . ? Ni1 N3 2.151(3) 4_565 ? Ni1 O2 2.159(2) . ? Ni2 N18 2.014(3) . ? Ni2 N14 2.101(3) . ? Ni2 N9 2.115(3) . ? Ni2 N7 2.119(3) . ? Ni2 O1 2.139(2) 3_755 ? Ni2 N12 2.151(3) 4_575 ? S1 O3 1.463(2) . ? S1 O4 1.465(2) . ? S1 O1 1.472(2) . ? S1 O2 1.483(2) . ? S2 C42 1.627(4) . ? S3 C41 1.639(5) . ? O1 Ni2 2.139(2) 3_745 ? N1 C1 1.341(4) . ? N1 N2 1.357(4) . ? N2 C3 1.353(4) . ? N3 C8 1.343(4) . ? N3 N4 1.364(4) . ? N3 Ni1 2.151(3) 4_465 ? N4 C6 1.339(5) . ? N5 C13 1.337(5) . ? N5 N6 1.357(4) . ? N6 C11 1.341(5) . ? N7 C18 1.333(5) . ? N7 N8 1.359(4) . ? N8 C16 1.336(5) . ? N9 C21 1.333(4) . ? N9 N10 1.345(4) . ? N10 C23 1.337(5) . ? N11 N12 1.339(5) . ? N11 C26 1.347(5) . ? N12 C28 1.345(5) . ? N12 Ni2 2.151(3) 4_475 ? N13 N14 1.340(4) . ? N13 C31 1.352(5) . ? N14 C33 1.336(5) . ? N15 C38 1.342(5) . ? N15 N16 1.358(4) . ? N15 Ni1 2.095(3) 1_655 ? N16 C36 1.346(5) . ? N17 C42 1.151(5) . ? N18 C41 1.125(5) . ? C1 C2 1.407(5) . ? C1 C5 1.495(5) . ? C2 C3 1.388(5) . ? C2 C7 1.476(5) . ? C3 C4 1.478(6) . ? C6 C7 1.383(5) . ? C6 C10 1.497(6) . ? C7 C8 1.404(5) . ? C8 C9 1.497(5) . ? C11 C12 1.372(5) . ? C11 C15 1.493(6) . ? C12 C13 1.413(5) . ? C12 C17 1.467(5) . ? C13 C14 1.500(5) . ? C16 C17 1.398(5) . ? C16 C20 1.476(5) . ? C17 C18 1.409(5) . ? C18 C19 1.495(5) . ? C21 C22 1.422(5) . ? C21 C25 1.481(6) . ? C22 C23 1.378(6) . ? C22 C27 1.472(5) . ? C23 C24 1.484(6) . ? C26 C27 1.377(6) . ? C26 C30 1.486(6) . ? C27 C28 1.409(6) . ? C28 C29 1.479(6) . ? C31 C32 1.393(6) . ? C31 C35 1.488(6) . ? C32 C33 1.410(5) . ? C32 C37 1.464(5) . ? C33 C34 1.490(6) . ? C36 C37 1.372(5) . ? C36 C40 1.502(5) . ? C37 C38 1.408(5) . ? C38 C39 1.492(5) . ? C43 Cl2A 1.712(11) . ? C43 Cl1A 1.72(2) . ? C43 Cl3A 1.740(14) . ? C43 Cl1 1.743(8) . ? C43 Cl3 1.756(10) . ? C43 Cl2 1.764(13) . ? C44 Cl4 1.50(2) . ? C44 Cl5 1.62(2) . ? C44 Cl6 1.90(2) . ? Cl1 Cl1A 0.50(3) . ? Cl3 Cl3A 0.67(4) . ? O5 C45 1.415(6) . ? O6 C46 1.428(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 N17 Ni1 N15 94.49(12) . 1_455 ? N17 Ni1 N5 90.42(12) . . ? N15 Ni1 N5 89.11(11) 1_455 . ? N17 Ni1 N1 93.18(12) . . ? N15 Ni1 N1 87.69(11) 1_455 . ? N5 Ni1 N1 175.36(11) . . ? N17 Ni1 N3 88.61(11) . 4_565 ? N15 Ni1 N3 176.58(12) 1_455 4_565 ? N5 Ni1 N3 92.32(11) . 4_565 ? N1 Ni1 N3 90.69(11) . 4_565 ? N17 Ni1 O2 170.51(10) . . ? N15 Ni1 O2 95.00(10) 1_455 . ? N5 Ni1 O2 89.67(10) . . ? N1 Ni1 O2 87.25(10) . . ? N3 Ni1 O2 81.90(10) 4_565 . ? N18 Ni2 N14 92.67(13) . . ? N18 Ni2 N9 92.47(13) . . ? N14 Ni2 N9 174.76(12) . . ? N18 Ni2 N7 92.01(12) . . ? N14 Ni2 N7 89.24(12) . . ? N9 Ni2 N7 89.55(12) . . ? N18 Ni2 O1 173.99(11) . 3_755 ? N14 Ni2 O1 86.99(10) . 3_755 ? N9 Ni2 O1 87.80(10) . 3_755 ? N7 Ni2 O1 81.99(10) . 3_755 ? N18 Ni2 N12 90.47(13) . 4_575 ? N14 Ni2 N12 90.21(12) . 4_575 ? N9 Ni2 N12 90.78(12) . 4_575 ? N7 Ni2 N12 177.48(12) . 4_575 ? O1 Ni2 N12 95.53(10) 3_755 4_575 ? O3 S1 O4 111.6(2) . . ? O3 S1 O1 110.19(14) . . ? O4 S1 O1 109.27(14) . . ? O3 S1 O2 109.79(14) . . ? O4 S1 O2 108.68(14) . . ? O1 S1 O2 107.25(12) . . ? S1 O1 Ni2 135.60(14) . 3_745 ? S1 O2 Ni1 139.65(14) . . ? C1 N1 N2 104.9(3) . . ? C1 N1 Ni1 136.7(2) . . ? N2 N1 Ni1 115.7(2) . . ? C3 N2 N1 112.7(3) . . ? C8 N3 N4 104.5(3) . . ? C8 N3 Ni1 132.8(2) . 4_465 ? N4 N3 Ni1 114.9(2) . 4_465 ? C6 N4 N3 112.5(3) . . ? C13 N5 N6 105.1(3) . . ? C13 N5 Ni1 131.2(2) . . ? N6 N5 Ni1 118.9(2) . . ? C11 N6 N5 112.2(3) . . ? C18 N7 N8 105.0(3) . . ? C18 N7 Ni2 135.6(2) . . ? N8 N7 Ni2 116.2(2) . . ? C16 N8 N7 113.1(3) . . ? C21 N9 N10 105.6(3) . . ? C21 N9 Ni2 132.7(2) . . ? N10 N9 Ni2 117.3(2) . . ? C23 N10 N9 112.7(3) . . ? N12 N11 C26 112.8(3) . . ? N11 N12 C28 105.6(3) . . ? N11 N12 Ni2 117.2(2) . 4_475 ? C28 N12 Ni2 129.8(3) . 4_475 ? N14 N13 C31 112.4(3) . . ? C33 N14 N13 106.1(3) . . ? C33 N14 Ni2 133.8(2) . . ? N13 N14 Ni2 118.2(2) . . ? C38 N15 N16 105.3(3) . . ? C38 N15 Ni1 133.8(2) . 1_655 ? N16 N15 Ni1 119.5(2) . 1_655 ? C36 N16 N15 111.8(3) . . ? C42 N17 Ni1 165.1(3) . . ? C41 N18 Ni2 172.7(4) . . ? N1 C1 C2 110.8(3) . . ? N1 C1 C5 122.5(3) . . ? C2 C1 C5 126.7(3) . . ? C3 C2 C1 105.6(3) . . ? C3 C2 C7 125.4(3) . . ? C1 C2 C7 129.1(3) . . ? N2 C3 C2 106.0(3) . . ? N2 C3 C4 122.5(3) . . ? C2 C3 C4 131.5(3) . . ? N4 C6 C7 106.8(3) . . ? N4 C6 C10 122.1(4) . . ? C7 C6 C10 131.1(3) . . ? C6 C7 C8 105.2(3) . . ? C6 C7 C2 126.8(3) . . ? C8 C7 C2 127.8(3) . . ? N3 C8 C7 110.9(3) . . ? N3 C8 C9 121.9(3) . . ? C7 C8 C9 127.1(3) . . ? N6 C11 C12 107.1(3) . . ? N6 C11 C15 121.0(3) . . ? C12 C11 C15 131.8(4) . . ? C11 C12 C13 105.2(3) . . ? C11 C12 C17 127.7(3) . . ? C13 C12 C17 127.0(3) . . ? N5 C13 C12 110.3(3) . . ? N5 C13 C14 122.3(3) . . ? C12 C13 C14 127.3(3) . . ? N8 C16 C17 106.0(3) . . ? N8 C16 C20 122.2(3) . . ? C17 C16 C20 131.8(3) . . ? C16 C17 C18 105.1(3) . . ? C16 C17 C12 127.1(3) . . ? C18 C17 C12 127.8(3) . . ? N7 C18 C17 110.7(3) . . ? N7 C18 C19 122.1(3) . . ? C17 C18 C19 127.2(3) . . ? N9 C21 C22 110.0(3) . . ? N9 C21 C25 123.7(3) . . ? C22 C21 C25 126.3(3) . . ? C23 C22 C21 104.8(3) . . ? C23 C22 C27 127.8(4) . . ? C21 C22 C27 127.3(3) . . ? N10 C23 C22 106.9(3) . . ? N10 C23 C24 122.7(4) . . ? C22 C23 C24 130.4(4) . . ? N11 C26 C27 106.0(3) . . ? N11 C26 C30 122.3(4) . . ? C27 C26 C30 131.6(4) . . ? C26 C27 C28 106.0(3) . . ? C26 C27 C22 126.1(4) . . ? C28 C27 C22 128.0(4) . . ? N12 C28 C27 109.5(3) . . ? N12 C28 C29 123.8(4) . . ? C27 C28 C29 126.7(3) . . ? N13 C31 C32 106.2(3) . . ? N13 C31 C35 122.3(4) . . ? C32 C31 C35 131.4(4) . . ? C31 C32 C33 105.1(3) . . ? C31 C32 C37 126.6(3) . . ? C33 C32 C37 128.3(3) . . ? N14 C33 C32 110.2(3) . . ? N14 C33 C34 123.0(3) . . ? C32 C33 C34 126.8(3) . . ? N16 C36 C37 107.2(3) . . ? N16 C36 C40 120.8(3) . . ? C37 C36 C40 132.0(3) . . ? C36 C37 C38 105.5(3) . . ? C36 C37 C32 127.2(3) . . ? C38 C37 C32 127.3(3) . . ? N15 C38 C37 110.3(3) . . ? N15 C38 C39 122.6(3) . . ? C37 C38 C39 127.2(3) . . ? N18 C41 S3 176.9(6) . . ? N17 C42 S2 179.3(4) . . ? Cl2A C43 Cl1A 111.3(11) . . ? Cl2A C43 Cl3A 100.5(10) . . ? Cl1A C43 Cl3A 114.3(11) . . ? Cl2A C43 Cl1 101.2(6) . . ? Cl1A C43 Cl1 16.7(10) . . ? Cl3A C43 Cl1 130.5(13) . . ? Cl2A C43 Cl3 115.0(5) . . ? Cl1A C43 Cl3 92.8(11) . . ? Cl3A C43 Cl3 22.1(14) . . ? Cl1 C43 Cl3 109.3(5) . . ? Cl2A C43 Cl2 10.8(8) . . ? Cl1A C43 Cl2 122.2(12) . . ? Cl3A C43 Cl2 95.3(12) . . ? Cl1 C43 Cl2 111.6(6) . . ? Cl3 C43 Cl2 112.5(5) . . ? Cl4 C44 Cl5 128.1(14) . . ? Cl4 C44 Cl6 111.6(10) . . ? Cl5 C44 Cl6 108.5(8) . . ? Cl1A Cl1 C43 79.2(27) . . ? Cl3A Cl3 C43 77.6(15) . . ? Cl1 Cl1A C43 84.1(29) . . ? Cl3 Cl3A C43 80.3(17) . . ? _refine_diff_density_max 0.628 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.062 #==============================================================================