# Copyright The Royal Society of Chemistry, 1998. data_koss # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Franc Meyer Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 6221 54-8315' _publ_contact_author_fax '049 6221 54-5707' _publ_contact_author_email MESS@MONDO.ACI.UNI-HEIDELBERG.DE _publ_requested_journal 'JCS Dalton Trans' _publ_requested_coeditor_name ? #================================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; 'Unsymmetrically Substituted Pyrazolates: Nickel(II) Complexes of a Novel Dinucleating Ligand Providing both N- and S-rich Coordination Spheres' ; loop_ _publ_author_name _publ_author_address 'Matthias Konrad' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Franc Meyer' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Katja Heinze' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Laszlo Zsolnai' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #================================================================ _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'compound 4' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H43 Cl5 N4 Ni2 S4' _chemical_formula_weight 786.51 _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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting ORTHOROMBIC _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 15.570(3) _cell_length_b 12.286(3) _cell_length_c 17.346(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3318.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method ? _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.810 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4306 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.01 _reflns_number_total 3429 _reflns_number_observed 2800 _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 0 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^)+(0.0673P)^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_number_reflns 3429 _refine_ls_number_parameters 222 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_obs 0.0516 _refine_ls_wR_factor_all 0.1773 _refine_ls_wR_factor_obs 0.1478 _refine_ls_goodness_of_fit_all 1.771 _refine_ls_goodness_of_fit_obs 1.644 _refine_ls_restrained_S_all 1.775 _refine_ls_restrained_S_obs 1.651 _refine_ls_shift/esd_max 0.066 _refine_ls_shift/esd_mean 0.004 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 0.07334(6) 0.2500 0.23489(5) 0.0207(3) Uani 1 d S . Ni2 Ni 0.14827(5) 0.2500 0.02502(5) 0.0216(3) Uani 1 d S . Cl1 Cl 0.20226(11) 0.2500 0.15596(10) 0.0286(4) Uani 1 d S . Cl2 Cl 0.14524(12) 0.2500 0.35513(10) 0.0323(4) Uani 1 d S . Cl3 Cl 0.28321(11) 0.2500 -0.03573(11) 0.0313(4) Uani 1 d S . S1 S 0.05479(9) 0.04993(11) 0.23416(9) 0.0356(4) Uani 1 d . . S2 S 0.13640(8) 0.04861(11) 0.01394(7) 0.0281(3) Uani 1 d . . N1 N 0.0032(4) 0.2500 0.1400(3) 0.0229(12) Uani 1 d S . N2 N 0.0289(3) 0.2500 0.0661(3) 0.0210(12) Uani 1 d S . N3 N 0.0696(3) 0.2500 -0.0814(3) 0.0217(12) Uani 1 d S . N4 N -0.0576(3) 0.2500 0.2817(3) 0.0240(13) Uani 1 d S . C1 C -0.0831(4) 0.2500 0.1396(4) 0.0159(13) Uani 1 d S . C2 C -0.1143(4) 0.2500 0.0659(4) 0.0159(13) Uani 1 d S . H2 H -0.1712(4) 0.2500 0.0497(4) 0.019 Uiso 1 calc SR . C3 C -0.0386(4) 0.2500 0.0199(4) 0.0203(14) Uani 1 d S . C4 C -0.0233(4) 0.2500 -0.0657(4) 0.026(2) Uani 1 d S . H4A H -0.0494(4) 0.1860 -0.0885(4) 0.047(13) Uiso 0.50 calc PR . H4B H -0.0494(4) 0.3140 -0.0885(4) 0.047(13) Uiso 0.50 calc PR . C5 C 0.0961(3) 0.1513(4) -0.1255(3) 0.0271(11) Uani 1 d . . H5A H 0.1563(3) 0.1574(4) -0.1394(3) 0.042(6) Uiso 1 calc R . H5B H 0.0629(3) 0.1468(4) -0.1727(3) 0.042(6) Uiso 1 calc R . C6 C 0.0826(4) 0.0489(5) -0.0787(3) 0.0321(12) Uani 1 d . . H6A H 0.1029(4) -0.0128(5) -0.1085(3) 0.042(6) Uiso 1 calc R . H6B H 0.0215(4) 0.0391(5) -0.0703(3) 0.042(6) Uiso 1 calc R . C7 C 0.2383(4) -0.0141(5) -0.0095(5) 0.057(2) Uani 0.50 d PD 1 H7A H 0.2327(4) -0.0681(5) -0.0500(5) 0.048(12) Uiso 0.50 calc PR 1 H7B H 0.2813(4) 0.0393(5) -0.0240(5) 0.048(12) Uiso 0.50 calc PR 1 C8 C 0.2592(10) -0.0695(15) 0.0739(10) 0.078(6) Uani 0.50 d PD 1 H8A H 0.2649(64) -0.0135(16) 0.1122(15) 0.073(15) Uiso 0.50 calc PR 1 H8B H 0.3119(36) -0.1100(69) 0.0706(19) 0.073(15) Uiso 0.50 calc PR 1 H8C H 0.2132(33) -0.1176(65) 0.0880(29) 0.073(15) Uiso 0.50 calc PR 1 C70 C 0.2383(4) -0.0141(5) -0.0095(5) 0.057(2) Uani 0.50 d PD 2 H70A H 0.2264(11) -0.0753(15) -0.0432(9) 0.048(12) Uiso 0.50 calc PR 2 H70B H 0.2708(11) 0.0382(15) -0.0396(9) 0.048(12) Uiso 0.50 calc PR 2 C80 C 0.2933(11) -0.0524(15) 0.0501(9) 0.061(5) Uiso 0.50 d PD 2 H80A H 0.3453(32) -0.0803(83) 0.0279(10) 0.073(15) Uiso 0.50 calc PR 2 H80B H 0.2649(30) -0.1092(63) 0.0782(41) 0.073(15) Uiso 0.50 calc PR 2 H80C H 0.3068(57) 0.0065(26) 0.0844(36) 0.073(15) Uiso 0.50 calc PR 2 C9 C -0.1233(5) 0.2500 0.2193(4) 0.031(2) Uani 1 d S . H9A H -0.1594(5) 0.3138 0.2247(4) 0.047(13) Uiso 0.50 calc PR . H9B H -0.1594(5) 0.1862 0.2247(4) 0.047(13) Uiso 0.50 calc PR . C10 C -0.0650(3) 0.1516(5) 0.3293(3) 0.0374(15) Uani 1 d . . H10A H -0.1225(3) 0.1478(5) 0.3506(3) 0.042(6) Uiso 1 calc R . H10B H -0.0250(3) 0.1567(5) 0.3720(3) 0.042(6) Uiso 1 calc R . C11 C -0.0470(4) 0.0490(5) 0.2847(4) 0.048(2) Uani 1 d . . H11A H -0.0927(4) 0.0380(5) 0.2476(4) 0.042(6) Uiso 1 calc R . H11B H -0.0477(4) -0.0121(5) 0.3201(4) 0.042(6) Uiso 1 calc R . C12 C 0.1250(6) -0.0149(6) 0.3044(5) 0.071(3) Uani 0.50 d PD 1 H12A H 0.1257(6) 0.0286(6) 0.3511(5) 0.048(12) Uiso 0.50 calc PR 1 H12B H 0.1017(6) -0.0858(6) 0.3174(5) 0.048(12) Uiso 0.50 calc PR 1 C13 C 0.2080(7) -0.0277(11) 0.2785(8) 0.062(4) Uani 0.60 d PD 1 H13A H 0.2421(14) -0.0604(60) 0.3183(18) 0.073(15) Uiso 0.60 calc PR 1 H13B H 0.2315(19) 0.0422(13) 0.2654(44) 0.073(15) Uiso 0.60 calc PR 1 H13C H 0.2081(8) -0.0736(54) 0.2337(28) 0.073(15) Uiso 0.60 calc PR 1 C120 C 0.1250(6) -0.0149(6) 0.3044(5) 0.071(3) Uani 0.50 d PD 2 H12C H 0.1779(12) 0.0261(15) 0.3091(11) 0.048(12) Uiso 0.50 calc PR 2 H12D H 0.0972(12) -0.0164(15) 0.3544(11) 0.048(12) Uiso 0.50 calc PR 2 C130 C 0.1439(12) -0.1275(15) 0.2786(11) 0.063(5) Uani 0.40 d PD 2 H13D H 0.1821(67) -0.1616(38) 0.3146(41) 0.073(15) Uiso 0.40 calc PR 2 H13E H 0.1704(75) -0.1254(16) 0.2286(35) 0.073(15) Uiso 0.40 calc PR 2 H13F H 0.0914(16) -0.1683(33) 0.2757(71) 0.073(15) Uiso 0.40 calc PR 2 Cl4 Cl -0.0481(2) -0.2500 0.37588(15) 0.0540(6) Uani 1 d S . Cl5 Cl -0.0039(3) -0.0710(3) 0.4754(2) 0.0587(9) Uani 0.50 d P . C14 C -0.0099(8) -0.2126(10) 0.4676(7) 0.049(4) Uani 0.50 d P . H14A H -0.0482(8) -0.2408(10) 0.5070(7) 0.093(32) Uiso 0.50 calc PR . H14B H 0.0465(8) -0.2439(10) 0.4759(7) 0.093(32) Uiso 0.50 calc PR . 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 0.0217(5) 0.0239(5) 0.0166(4) 0.000 -0.0020(3) 0.000 Ni2 0.0171(4) 0.0287(5) 0.0191(5) 0.000 0.0005(3) 0.000 Cl1 0.0199(8) 0.0442(11) 0.0217(8) 0.000 -0.0035(6) 0.000 Cl2 0.0310(10) 0.0435(11) 0.0223(9) 0.000 -0.0085(7) 0.000 Cl3 0.0215(8) 0.0337(10) 0.0388(10) 0.000 0.0113(7) 0.000 S1 0.0358(8) 0.0255(7) 0.0456(9) -0.0026(6) -0.0142(6) 0.0037(6) S2 0.0286(7) 0.0281(7) 0.0274(7) 0.0055(5) -0.0018(5) -0.0032(5) N1 0.029(3) 0.026(3) 0.014(3) 0.000 0.009(2) 0.000 N2 0.013(2) 0.034(3) 0.017(3) 0.000 -0.005(2) 0.000 N3 0.020(3) 0.027(3) 0.018(3) 0.000 -0.003(2) 0.000 N4 0.016(3) 0.037(4) 0.018(3) 0.000 0.008(2) 0.000 C1 0.011(3) 0.017(3) 0.019(3) 0.000 0.006(2) 0.000 C2 0.009(3) 0.015(3) 0.023(3) 0.000 -0.006(2) 0.000 C3 0.019(3) 0.019(3) 0.023(4) 0.000 -0.001(3) 0.000 C4 0.022(3) 0.034(4) 0.022(4) 0.000 -0.006(3) 0.000 C5 0.033(3) 0.026(3) 0.023(2) -0.004(2) 0.005(2) 0.004(2) C6 0.033(3) 0.031(3) 0.032(3) 0.000(2) -0.001(2) -0.006(2) C7 0.039(4) 0.028(3) 0.105(6) -0.006(4) -0.001(4) 0.004(3) C8 0.035(8) 0.072(12) 0.128(17) 0.040(13) -0.005(10) 0.019(8) C70 0.039(4) 0.028(3) 0.105(6) -0.006(4) -0.001(4) 0.004(3) C9 0.029(4) 0.046(5) 0.020(3) 0.000 0.003(3) 0.000 C10 0.026(3) 0.059(4) 0.027(3) 0.015(3) 0.013(2) -0.012(2) C11 0.057(4) 0.037(4) 0.049(4) 0.010(3) -0.011(3) -0.015(3) C12 0.093(6) 0.025(4) 0.095(7) 0.015(4) -0.038(5) -0.001(4) C13 0.028(6) 0.063(8) 0.096(10) 0.017(7) 0.000(6) 0.019(6) C120 0.093(6) 0.025(4) 0.095(7) 0.015(4) -0.038(5) -0.001(4) C130 0.055(11) 0.076(13) 0.060(11) 0.014(11) -0.016(9) -0.005(10) Cl4 0.068(2) 0.0445(13) 0.0498(14) 0.000 0.0076(12) 0.000 Cl5 0.082(3) 0.056(2) 0.038(2) 0.010(2) -0.011(2) -0.014(2) C14 0.044(7) 0.055(9) 0.049(7) 0.020(6) -0.006(6) 0.009(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 Ni1 N1 1.975(6) . ? Ni1 N4 2.195(5) . ? Ni1 Cl2 2.367(2) . ? Ni1 Cl1 2.430(2) . ? Ni1 S1 2.475(2) . ? Ni1 S1 2.475(2) 7_565 ? Ni2 N2 1.991(5) . ? Ni2 N3 2.214(6) . ? Ni2 Cl3 2.350(2) . ? Ni2 Cl1 2.422(2) . ? Ni2 S2 2.4886(14) . ? Ni2 S2 2.4886(15) 7_565 ? S1 C11 1.811(7) . ? S1 C120 1.820(8) . ? S1 C12 1.820(8) . ? S2 C70 1.811(7) . ? S2 C7 1.811(7) . ? S2 C6 1.812(5) . ? N1 N2 1.343(8) . ? N1 C1 1.343(8) . ? N2 C3 1.322(8) . ? N3 C4 1.472(9) . ? N3 C5 1.492(6) 7_565 ? N3 C5 1.492(6) . ? N4 C10 1.469(6) 7_565 ? N4 C10 1.469(6) . ? N4 C9 1.488(9) . ? C1 C2 1.368(9) . ? C1 C9 1.517(9) . ? C2 C3 1.423(9) . ? C2 H2 0.93 . ? C3 C4 1.503(9) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.511(7) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.63(2) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C70 C80 1.42(2) . ? C70 H70A 0.97(2) . ? C70 H70B 0.97(2) . ? C80 H80A 0.96 . ? C80 H80B 0.96 . ? C80 H80C 0.96 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 C11 1.506(9) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 C13 1.377(13) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C120 C130 1.48(2) . ? C120 H12C 0.97(2) . ? C120 H12D 0.97(2) . ? C130 H13D 0.96 . ? C130 H13E 0.96 . ? C130 H13F 0.96 . ? Cl4 C14 1.760(13) . ? Cl4 C14 1.760(13) 7 ? Cl5 C14 1.747(14) . ? Cl5 Cl5 1.945(8) 5_556 ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? 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 Ni1 N4 78.1(2) . . ? N1 Ni1 Cl2 174.7(2) . . ? N4 Ni1 Cl2 96.5(2) . . ? N1 Ni1 Cl1 89.3(2) . . ? N4 Ni1 Cl1 167.4(2) . . ? Cl2 Ni1 Cl1 96.07(7) . . ? N1 Ni1 S1 86.06(4) . . ? N4 Ni1 S1 83.89(4) . . ? Cl2 Ni1 S1 93.42(4) . . ? Cl1 Ni1 S1 95.36(4) . . ? N1 Ni1 S1 86.06(4) . 7_565 ? N4 Ni1 S1 83.89(4) . 7_565 ? Cl2 Ni1 S1 93.42(4) . 7_565 ? Cl1 Ni1 S1 95.36(4) . 7_565 ? S1 Ni1 S1 166.59(8) . 7_565 ? N2 Ni2 N3 77.4(2) . . ? N2 Ni2 Cl3 174.4(2) . . ? N3 Ni2 Cl3 96.9(2) . . ? N2 Ni2 Cl1 89.3(2) . . ? N3 Ni2 Cl1 166.7(2) . . ? Cl3 Ni2 Cl1 96.33(7) . . ? N2 Ni2 S2 87.61(4) . . ? N3 Ni2 S2 83.95(3) . . ? Cl3 Ni2 S2 91.82(4) . . ? Cl1 Ni2 S2 95.64(3) . . ? N2 Ni2 S2 87.61(4) . 7_565 ? N3 Ni2 S2 83.95(3) . 7_565 ? Cl3 Ni2 S2 91.82(4) . 7_565 ? Cl1 Ni2 S2 95.64(3) . 7_565 ? S2 Ni2 S2 167.69(7) . 7_565 ? Ni2 Cl1 Ni1 103.99(7) . . ? C11 S1 C120 101.4(4) . . ? C11 S1 C12 101.4(4) . . ? C11 S1 Ni1 96.1(2) . . ? C120 S1 Ni1 111.2(3) . . ? C12 S1 Ni1 111.2(3) . . ? C70 S2 C6 101.9(3) . . ? C7 S2 C6 101.9(3) . . ? C70 S2 Ni2 112.0(2) . . ? C7 S2 Ni2 112.0(2) . . ? C6 S2 Ni2 95.8(2) . . ? N2 N1 C1 107.0(5) . . ? N2 N1 Ni1 129.1(4) . . ? C1 N1 Ni1 123.9(4) . . ? C3 N2 N1 110.0(5) . . ? C3 N2 Ni2 121.6(5) . . ? N1 N2 Ni2 128.3(4) . . ? C4 N3 C5 111.5(3) . 7_565 ? C4 N3 C5 111.5(3) . . ? C5 N3 C5 108.7(5) 7_565 . ? C4 N3 Ni2 112.9(4) . . ? C5 N3 Ni2 105.9(3) 7_565 . ? C5 N3 Ni2 105.9(3) . . ? C10 N4 C10 110.7(6) 7_565 . ? C10 N4 C9 110.8(4) 7_565 . ? C10 N4 C9 110.8(4) . . ? C10 N4 Ni1 106.3(3) 7_565 . ? C10 N4 Ni1 106.3(3) . . ? C9 N4 Ni1 111.7(4) . . ? N1 C1 C2 111.1(5) . . ? N1 C1 C9 114.0(6) . . ? C2 C1 C9 134.9(6) . . ? C1 C2 C3 103.3(5) . . ? C1 C2 H2 128.3(4) . . ? C3 C2 H2 128.3(4) . . ? N2 C3 C2 108.5(6) . . ? N2 C3 C4 118.2(6) . . ? C2 C3 C4 133.3(6) . . ? N3 C4 C3 109.8(5) . . ? N3 C4 H4A 109.7(2) . . ? C3 C4 H4A 109.7(2) . . ? N3 C4 H4B 109.7(2) . . ? C3 C4 H4B 109.7(2) . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 111.3(4) . . ? N3 C5 H5A 109.4(3) . . ? C6 C5 H5A 109.4(3) . . ? N3 C5 H5B 109.4(3) . . ? C6 C5 H5B 109.4(3) . . ? H5A C5 H5B 108.0 . . ? C5 C6 S2 114.4(4) . . ? C5 C6 H6A 108.7(3) . . ? S2 C6 H6A 108.7(2) . . ? C5 C6 H6B 108.7(3) . . ? S2 C6 H6B 108.7(2) . . ? H6A C6 H6B 107.6 . . ? C8 C7 S2 98.8(7) . . ? C8 C7 H7A 112.0(8) . . ? S2 C7 H7A 112.0(2) . . ? C8 C7 H7B 112.0(7) . . ? S2 C7 H7B 112.0(2) . . ? H7A C7 H7B 109.7 . . ? C7 C8 H8A 109.5(8) . . ? C7 C8 H8B 109.5(7) . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5(7) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C80 C70 S2 120.3(9) . . ? C80 C70 H70A 107.3(15) . . ? S2 C70 H70A 107.2(11) . . ? C80 C70 H70B 107.3(14) . . ? S2 C70 H70B 107.2(11) . . ? H70A C70 H70B 106.9(19) . . ? C70 C80 H80A 109.5(8) . . ? C70 C80 H80B 109.5(8) . . ? H80A C80 H80B 109.5 . . ? C70 C80 H80C 109.5(8) . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N4 C9 C1 112.3(6) . . ? N4 C9 H9A 109.1(2) . . ? C1 C9 H9A 109.1(2) . . ? N4 C9 H9B 109.1(2) . . ? C1 C9 H9B 109.1(2) . . ? H9A C9 H9B 107.9 . . ? N4 C10 C11 112.6(5) . . ? N4 C10 H10A 109.1(3) . . ? C11 C10 H10A 109.1(3) . . ? N4 C10 H10B 109.1(3) . . ? C11 C10 H10B 109.1(4) . . ? H10A C10 H10B 107.8 . . ? C10 C11 S1 114.0(4) . . ? C10 C11 H11A 108.7(4) . . ? S1 C11 H11A 108.7(2) . . ? C10 C11 H11B 108.7(3) . . ? S1 C11 H11B 108.7(2) . . ? H11A C11 H11B 107.6 . . ? C13 C12 S1 113.2(8) . . ? C13 C12 H12A 108.9(7) . . ? S1 C12 H12A 108.9(3) . . ? C13 C12 H12B 108.9(6) . . ? S1 C12 H12B 108.9(3) . . ? H12A C12 H12B 107.7 . . ? C12 C13 H13A 109.5(6) . . ? C12 C13 H13B 109.5(6) . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5(7) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C130 C120 S1 109.0(9) . . ? C130 C120 H12C 109.9(17) . . ? S1 C120 H12C 109.9(12) . . ? C130 C120 H12D 109.9(16) . . ? S1 C120 H12D 109.9(13) . . ? H12C C120 H12D 108.3(19) . . ? C120 C130 H13D 109.5(8) . . ? C120 C130 H13E 109.5(8) . . ? H13D C130 H13E 109.5 . . ? C120 C130 H13F 109.5(8) . . ? H13D C130 H13F 109.5 . . ? H13E C130 H13F 109.5 . . ? C14 Cl4 C14 30.3(8) . 7 ? C14 Cl5 Cl5 158.4(5) . 5_556 ? Cl5 C14 Cl4 110.4(6) . . ? Cl5 C14 H14A 109.6(5) . . ? Cl4 C14 H14A 109.6(4) . . ? Cl5 C14 H14B 109.6(4) . . ? Cl4 C14 H14B 109.6(4) . . ? H14A C14 H14B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni2 Cl1 Ni1 0.0 . . . . ? N3 Ni2 Cl1 Ni1 0.0 . . . . ? Cl3 Ni2 Cl1 Ni1 180.0 . . . . ? S2 Ni2 Cl1 Ni1 -87.53(4) . . . . ? S2 Ni2 Cl1 Ni1 87.53(4) 7_565 . . . ? N1 Ni1 Cl1 Ni2 0.0 . . . . ? N4 Ni1 Cl1 Ni2 0.0 . . . . ? Cl2 Ni1 Cl1 Ni2 180.0 . . . . ? S1 Ni1 Cl1 Ni2 85.97(4) . . . . ? S1 Ni1 Cl1 Ni2 -85.97(4) 7_565 . . . ? N1 Ni1 S1 C11 -85.8(3) . . . . ? N4 Ni1 S1 C11 -7.3(3) . . . . ? Cl2 Ni1 S1 C11 88.9(2) . . . . ? Cl1 Ni1 S1 C11 -174.7(2) . . . . ? S1 Ni1 S1 C11 -31.7(4) 7_565 . . . ? N1 Ni1 S1 C120 169.5(4) . . . . ? N4 Ni1 S1 C120 -112.1(4) . . . . ? Cl2 Ni1 S1 C120 -15.9(4) . . . . ? Cl1 Ni1 S1 C120 80.6(4) . . . . ? S1 Ni1 S1 C120 -136.4(5) 7_565 . . . ? N1 Ni1 S1 C12 169.5(4) . . . . ? N4 Ni1 S1 C12 -112.1(4) . . . . ? Cl2 Ni1 S1 C12 -15.9(4) . . . . ? Cl1 Ni1 S1 C12 80.6(4) . . . . ? S1 Ni1 S1 C12 -136.4(5) 7_565 . . . ? N2 Ni2 S2 C70 -171.0(3) . . . . ? N3 Ni2 S2 C70 111.4(3) . . . . ? Cl3 Ni2 S2 C70 14.7(3) . . . . ? Cl1 Ni2 S2 C70 -81.9(3) . . . . ? S2 Ni2 S2 C70 121.8(4) 7_565 . . . ? N2 Ni2 S2 C7 -171.0(3) . . . . ? N3 Ni2 S2 C7 111.4(3) . . . . ? Cl3 Ni2 S2 C7 14.7(3) . . . . ? Cl1 Ni2 S2 C7 -81.9(3) . . . . ? S2 Ni2 S2 C7 121.8(4) 7_565 . . . ? N2 Ni2 S2 C6 83.7(2) . . . . ? N3 Ni2 S2 C6 6.1(2) . . . . ? Cl3 Ni2 S2 C6 -90.7(2) . . . . ? Cl1 Ni2 S2 C6 172.8(2) . . . . ? S2 Ni2 S2 C6 16.4(4) 7_565 . . . ? N4 Ni1 N1 N2 180.0 . . . . ? Cl2 Ni1 N1 N2 180.000(1) . . . . ? Cl1 Ni1 N1 N2 0.0 . . . . ? S1 Ni1 N1 N2 -95.43(4) . . . . ? S1 Ni1 N1 N2 95.43(4) 7_565 . . . ? N4 Ni1 N1 C1 0.0 . . . . ? Cl2 Ni1 N1 C1 0.000(1) . . . . ? Cl1 Ni1 N1 C1 180.0 . . . . ? S1 Ni1 N1 C1 84.57(4) . . . . ? S1 Ni1 N1 C1 -84.57(4) 7_565 . . . ? C1 N1 N2 C3 0.0 . . . . ? Ni1 N1 N2 C3 180.0 . . . . ? C1 N1 N2 Ni2 180.0 . . . . ? Ni1 N1 N2 Ni2 0.0 . . . . ? N3 Ni2 N2 C3 0.0 . . . . ? Cl3 Ni2 N2 C3 0.0 . . . . ? Cl1 Ni2 N2 C3 180.0 . . . . ? S2 Ni2 N2 C3 -84.33(3) . . . . ? S2 Ni2 N2 C3 84.33(4) 7_565 . . . ? N3 Ni2 N2 N1 180.0 . . . . ? Cl3 Ni2 N2 N1 180.0 . . . . ? Cl1 Ni2 N2 N1 0.0 . . . . ? S2 Ni2 N2 N1 95.67(3) . . . . ? S2 Ni2 N2 N1 -95.67(4) 7_565 . . . ? N2 Ni2 N3 C4 0.0 . . . . ? Cl3 Ni2 N3 C4 180.0 . . . . ? Cl1 Ni2 N3 C4 0.0 . . . . ? S2 Ni2 N3 C4 88.90(4) . . . . ? S2 Ni2 N3 C4 -88.90(4) 7_565 . . . ? N2 Ni2 N3 C5 122.3(3) . . . 7_565 ? Cl3 Ni2 N3 C5 -57.7(3) . . . 7_565 ? Cl1 Ni2 N3 C5 122.3(3) . . . 7_565 ? S2 Ni2 N3 C5 -148.8(3) . . . 7_565 ? S2 Ni2 N3 C5 33.4(3) 7_565 . . 7_565 ? N2 Ni2 N3 C5 -122.3(3) . . . . ? Cl3 Ni2 N3 C5 57.7(3) . . . . ? Cl1 Ni2 N3 C5 -122.3(3) . . . . ? S2 Ni2 N3 C5 -33.4(3) . . . . ? S2 Ni2 N3 C5 148.8(3) 7_565 . . . ? N1 Ni1 N4 C10 -121.0(4) . . . 7_565 ? Cl2 Ni1 N4 C10 59.0(4) . . . 7_565 ? Cl1 Ni1 N4 C10 -121.0(4) . . . 7_565 ? S1 Ni1 N4 C10 151.8(4) . . . 7_565 ? S1 Ni1 N4 C10 -33.8(3) 7_565 . . 7_565 ? N1 Ni1 N4 C10 121.0(4) . . . . ? Cl2 Ni1 N4 C10 -59.0(4) . . . . ? Cl1 Ni1 N4 C10 121.0(4) . . . . ? S1 Ni1 N4 C10 33.8(3) . . . . ? S1 Ni1 N4 C10 -151.8(4) 7_565 . . . ? N1 Ni1 N4 C9 0.0 . . . . ? Cl2 Ni1 N4 C9 180.0 . . . . ? Cl1 Ni1 N4 C9 0.000(1) . . . . ? S1 Ni1 N4 C9 -87.24(4) . . . . ? S1 Ni1 N4 C9 87.24(4) 7_565 . . . ? N2 N1 C1 C2 0.0 . . . . ? Ni1 N1 C1 C2 180.0 . . . . ? N2 N1 C1 C9 180.0 . . . . ? Ni1 N1 C1 C9 0.0 . . . . ? N1 C1 C2 C3 0.0 . . . . ? C9 C1 C2 C3 180.0 . . . . ? N1 N2 C3 C2 0.0 . . . . ? Ni2 N2 C3 C2 180.0 . . . . ? N1 N2 C3 C4 180.0 . . . . ? Ni2 N2 C3 C4 0.0 . . . . ? C1 C2 C3 N2 0.0 . . . . ? C1 C2 C3 C4 180.0 . . . . ? C5 N3 C4 C3 -119.1(4) 7_565 . . . ? C5 N3 C4 C3 119.1(4) . . . . ? Ni2 N3 C4 C3 0.0 . . . . ? N2 C3 C4 N3 0.0 . . . . ? C2 C3 C4 N3 180.0 . . . . ? C4 N3 C5 C6 -64.8(6) . . . . ? C5 N3 C5 C6 171.8(3) 7_565 . . . ? Ni2 N3 C5 C6 58.3(5) . . . . ? N3 C5 C6 S2 -55.9(6) . . . . ? C70 S2 C6 C5 -91.7(4) . . . . ? C7 S2 C6 C5 -91.7(4) . . . . ? Ni2 S2 C6 C5 22.3(4) . . . . ? C70 S2 C7 C8 0.0(1000) . . . . ? C6 S2 C7 C8 -151.3(8) . . . . ? Ni2 S2 C7 C8 107.4(8) . . . . ? C7 S2 C70 C80 0.0(1000) . . . . ? C6 S2 C70 C80 -165.9(10) . . . . ? Ni2 S2 C70 C80 92.8(10) . . . . ? C10 N4 C9 C1 118.3(4) 7_565 . . . ? C10 N4 C9 C1 -118.3(4) . . . . ? Ni1 N4 C9 C1 0.0 . . . . ? N1 C1 C9 N4 0.0 . . . . ? C2 C1 C9 N4 180.0 . . . . ? C10 N4 C10 C11 -172.9(4) 7_565 . . . ? C9 N4 C10 C11 63.7(6) . . . . ? Ni1 N4 C10 C11 -57.9(5) . . . . ? N4 C10 C11 S1 53.4(7) . . . . ? C120 S1 C11 C10 93.4(5) . . . . ? C12 S1 C11 C10 93.4(5) . . . . ? Ni1 S1 C11 C10 -19.7(5) . . . . ? C11 S1 C12 C13 178.0(8) . . . . ? C120 S1 C12 C13 0.0(1000) . . . . ? Ni1 S1 C12 C13 -80.8(8) . . . . ? C11 S1 C120 C130 105.6(10) . . . . ? C12 S1 C120 C130 0.0(1000) . . . . ? Ni1 S1 C120 C130 -153.2(9) . . . . ? Cl5 Cl5 C14 Cl4 162.1(11) 5_556 . . . ? C14 Cl4 C14 Cl5 178.6(5) 7 . . . ? _refine_diff_density_max 0.747 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.163 #=END