# Copyright The Royal Society of Chemistry, 1998. data_korr # 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 5' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H51 B0 Cl3 N6 Ni2 S2' _chemical_formula_weight 723.61 _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' 'B' 'B' 0.0013 0.0007 '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 MONOCLINIC _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.712(9) _cell_length_b 10.960(2) _cell_length_c 14.176(2) _cell_angle_alpha 90.00 _cell_angle_beta 89.460(10) _cell_angle_gamma 90.00 _cell_volume 6635.8(21) _cell_formula_units_Z 8 _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 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method ? _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 1.528 _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 6271 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6185 _reflns_number_observed 4440 _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^)+(0.0510P)^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 6185 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_obs 0.0457 _refine_ls_wR_factor_all 0.1099 _refine_ls_wR_factor_obs 0.0963 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.028 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.016 _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 0.374172(13) 0.13136(5) 0.32097(4) 0.01892(14) Uani 1 d . . Ni2 Ni 0.414539(13) 0.40417(5) 0.43585(4) 0.01877(14) Uani 1 d . . Cl1 Cl 0.36028(3) 0.11766(11) 0.16623(7) 0.0296(3) Uani 1 d . . Cl2 Cl 0.44624(3) 0.56171(10) 0.37525(7) 0.0290(3) Uani 1 d . . Cl3 Cl 0.41287(2) 0.28500(9) 0.29219(7) 0.0222(2) Uani 1 d . . S1 S 0.37045(3) 0.54157(10) 0.38907(7) 0.0247(3) Uani 1 d . . S2 S 0.45662(3) 0.28962(10) 0.51118(8) 0.0240(2) Uani 1 d . . N1 N 0.36880(8) 0.1950(3) 0.4487(2) 0.0190(8) Uani 1 d . . N2 N 0.38427(8) 0.2870(3) 0.4916(2) 0.0185(7) Uani 1 d . . N3 N 0.40786(8) 0.4805(3) 0.5755(2) 0.0209(8) Uani 1 d . . N4 N 0.33331(9) 0.0232(3) 0.3739(3) 0.0262(9) Uani 1 d . . N5 N 0.40128(9) -0.0234(3) 0.3472(2) 0.0231(8) Uani 1 d . . N6 N 0.26092(9) 0.1711(4) 0.2693(3) 0.0349(10) Uani 1 d . . C1 C 0.34650(10) 0.1552(4) 0.5088(3) 0.0208(9) Uani 1 d . . C2 C 0.34793(10) 0.2220(4) 0.5919(3) 0.0241(10) Uani 1 d . . H2 H 0.33537(10) 0.2136(4) 0.6454(3) 0.044(15) Uiso 1 calc R . C3 C 0.37216(10) 0.3039(4) 0.5774(3) 0.0195(9) Uani 1 d . . C4 C 0.38719(10) 0.4013(4) 0.6357(3) 0.0220(9) Uani 1 d . . H4A H 0.39951(10) 0.3639(4) 0.6850(3) 0.019(6) Uiso 1 calc R . H4B H 0.37110(10) 0.4509(4) 0.6655(3) 0.019(6) Uiso 1 calc R . C5 C 0.39317(11) 0.6025(4) 0.5636(3) 0.0260(10) Uani 1 d . . H5A H 0.40769(11) 0.6561(4) 0.5307(3) 0.025(4) Uiso 1 calc R . H5B H 0.38888(11) 0.6376(4) 0.6252(3) 0.025(4) Uiso 1 calc R . C6 C 0.36301(11) 0.5950(4) 0.5087(3) 0.0290(11) Uani 1 d . . H6A H 0.35326(11) 0.6749(4) 0.5067(3) 0.025(4) Uiso 1 calc R . H6B H 0.34866(11) 0.5395(4) 0.5404(3) 0.025(4) Uiso 1 calc R . C7 C 0.43954(10) 0.4949(4) 0.6164(3) 0.0245(10) Uani 1 d . . H7A H 0.43755(10) 0.5286(4) 0.6794(3) 0.025(4) Uiso 1 calc R . H7B H 0.45148(10) 0.5522(4) 0.5783(3) 0.025(4) Uiso 1 calc R . C8 C 0.45720(11) 0.3751(4) 0.6213(3) 0.0265(10) Uani 1 d . . H8A H 0.44807(11) 0.3253(4) 0.6710(3) 0.025(4) Uiso 1 calc R . H8B H 0.47877(11) 0.3916(4) 0.6379(3) 0.025(4) Uiso 1 calc R . C9 C 0.32696(11) 0.0496(4) 0.4759(3) 0.0279(10) Uani 1 d . . H9A H 0.33171(11) -0.0221(4) 0.5133(3) 0.019(6) Uiso 1 calc R . H9B H 0.30495(11) 0.0686(4) 0.4848(3) 0.019(6) Uiso 1 calc R . C10 C 0.34667(11) -0.1011(4) 0.3616(3) 0.0292(11) Uani 1 d . . H10A H 0.34714(11) -0.1220(4) 0.2951(3) 0.021(4) Uiso 1 calc R . H10B H 0.33355(11) -0.1601(4) 0.3942(3) 0.021(4) Uiso 1 calc R . C11 C 0.37937(11) -0.1060(4) 0.4004(3) 0.0283(10) Uani 1 d . . H11A H 0.38709(11) -0.1891(4) 0.3968(3) 0.021(4) Uiso 1 calc R . H11B H 0.37888(11) -0.0822(4) 0.4663(3) 0.021(4) Uiso 1 calc R . C12 C 0.33572(11) 0.4531(4) 0.3674(3) 0.0322(11) Uani 1 d . . H12A H 0.33896(11) 0.4045(4) 0.3110(3) 0.036(7) Uiso 1 calc R . H12B H 0.33232(11) 0.3976(4) 0.4198(3) 0.036(7) Uiso 1 calc R . C13 C 0.30676(13) 0.5312(5) 0.3551(4) 0.055(2) Uani 1 d . . H13A H 0.2892(2) 0.4799(6) 0.3404(27) 0.074(9) Uiso 1 calc R . H13B H 0.3102(3) 0.5882(24) 0.3047(18) 0.074(9) Uiso 1 calc R . H13C H 0.3025(5) 0.5748(27) 0.4125(10) 0.074(9) Uiso 1 calc R . C14 C 0.49382(11) 0.3291(5) 0.4577(3) 0.0334(11) Uani 1 d . . H14A H 0.49365(11) 0.4140(5) 0.4385(3) 0.036(7) Uiso 1 calc R . H14B H 0.51045(11) 0.3181(5) 0.5031(3) 0.036(7) Uiso 1 calc R . C15 C 0.49957(12) 0.2494(6) 0.3738(4) 0.057(2) Uani 1 d . . H15A H 0.5201(4) 0.2654(26) 0.3486(17) 0.074(9) Uiso 1 calc R . H15B H 0.4842(6) 0.2664(25) 0.3266(11) 0.074(9) Uiso 1 calc R . H15C H 0.4981(9) 0.1654(6) 0.3924(6) 0.074(9) Uiso 1 calc R . C16 C 0.30374(10) 0.0339(4) 0.3198(3) 0.0275(10) Uani 1 d . . H16A H 0.28768(10) -0.0152(4) 0.3502(3) 0.021(4) Uiso 1 calc R . H16B H 0.30712(10) 0.0017(4) 0.2568(3) 0.021(4) Uiso 1 calc R . C17 C 0.29226(11) 0.1650(4) 0.3126(3) 0.0302(11) Uani 1 d . . H17A H 0.29134(11) 0.2009(4) 0.3751(3) 0.021(4) Uiso 1 calc R . H17B H 0.30697(11) 0.2121(4) 0.2748(3) 0.021(4) Uiso 1 calc R . C18 C 0.26050(13) 0.2469(6) 0.1848(4) 0.051(2) Uani 1 d . . H18A H 0.27021(13) 0.3248(6) 0.1983(4) 0.054(6) Uiso 1 calc R . H18B H 0.23897(13) 0.2621(6) 0.1670(4) 0.054(6) Uiso 1 calc R . C19 C 0.27756(14) 0.1870(7) 0.1037(4) 0.067(2) Uani 1 d . . H19A H 0.2766(7) 0.2389(16) 0.0492(8) 0.065(5) Uiso 1 calc R . H19B H 0.2679(5) 0.1101(16) 0.0898(17) 0.065(5) Uiso 1 calc R . H19C H 0.2990(2) 0.1739(31) 0.1204(10) 0.065(5) Uiso 1 calc R . C20 C 0.23727(13) 0.2132(5) 0.3380(4) 0.0475(14) Uani 1 d . . H20A H 0.21789(13) 0.2292(5) 0.3050(4) 0.054(6) Uiso 1 calc R . H20B H 0.24427(13) 0.2896(5) 0.3652(4) 0.054(6) Uiso 1 calc R . C21 C 0.23085(13) 0.1245(6) 0.4158(4) 0.059(2) Uani 1 d . . H21A H 0.2140(6) 0.1545(16) 0.4547(15) 0.065(5) Uiso 1 calc R . H21B H 0.2493(3) 0.1150(25) 0.4532(15) 0.065(5) Uiso 1 calc R . H21C H 0.2251(8) 0.0471(11) 0.3895(4) 0.065(5) Uiso 1 calc R . C22 C 0.41232(12) -0.0872(4) 0.2602(3) 0.0327(11) Uani 1 d . . H22A H 0.39435(12) -0.1047(4) 0.2212(3) 0.054(6) Uiso 1 calc R . H22B H 0.42154(12) -0.1645(4) 0.2782(3) 0.054(6) Uiso 1 calc R . C23 C 0.43589(12) -0.0170(5) 0.2023(4) 0.0412(13) Uani 1 d . . H23A H 0.4407(6) -0.0616(16) 0.1457(12) 0.065(5) Uiso 1 calc R . H23B H 0.4546(3) -0.0059(28) 0.2381(10) 0.065(5) Uiso 1 calc R . H23C H 0.4274(3) 0.0612(14) 0.1861(21) 0.065(5) Uiso 1 calc R . C24 C 0.42796(11) 0.0121(4) 0.4082(3) 0.0291(11) Uani 1 d . . H24A H 0.41960(11) 0.0535(4) 0.4634(3) 0.054(6) Uiso 1 calc R . H24B H 0.44081(11) 0.0704(4) 0.3739(3) 0.054(6) Uiso 1 calc R . C25 C 0.44894(12) -0.0912(5) 0.4413(4) 0.0454(14) Uani 1 d . . H25A H 0.4658(5) -0.0583(6) 0.4778(21) 0.065(5) Uiso 1 calc R . H25B H 0.4574(7) -0.1336(21) 0.3875(4) 0.065(5) Uiso 1 calc R . H25C H 0.4369(2) -0.1468(17) 0.4794(21) 0.065(5) Uiso 1 calc 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 0.0243(3) 0.0155(3) 0.0170(3) 0.0006(2) -0.0043(2) -0.0019(2) Ni2 0.0254(3) 0.0170(3) 0.0140(3) -0.0004(2) -0.0016(2) -0.0037(2) Cl1 0.0361(6) 0.0328(6) 0.0201(5) 0.0003(5) -0.0090(5) -0.0062(5) Cl2 0.0377(6) 0.0266(6) 0.0225(5) 0.0011(5) -0.0012(5) -0.0119(5) Cl3 0.0305(6) 0.0203(5) 0.0157(5) 0.0000(4) -0.0009(4) -0.0062(4) S1 0.0336(6) 0.0206(6) 0.0200(5) 0.0005(4) -0.0053(5) -0.0013(5) S2 0.0266(6) 0.0224(6) 0.0230(5) -0.0025(5) -0.0022(4) -0.0009(5) N1 0.024(2) 0.015(2) 0.018(2) 0.0008(14) -0.0028(15) -0.002(2) N2 0.025(2) 0.014(2) 0.016(2) 0.0003(14) -0.0030(14) -0.002(2) N3 0.027(2) 0.019(2) 0.017(2) 0.0006(15) -0.0040(15) -0.001(2) N4 0.028(2) 0.023(2) 0.027(2) 0.002(2) -0.006(2) -0.004(2) N5 0.033(2) 0.015(2) 0.022(2) 0.0014(15) -0.005(2) -0.002(2) N6 0.027(2) 0.042(3) 0.036(2) 0.000(2) -0.007(2) 0.006(2) C1 0.023(2) 0.022(2) 0.017(2) 0.008(2) -0.003(2) 0.000(2) C2 0.024(2) 0.027(2) 0.021(2) 0.006(2) 0.000(2) 0.000(2) C3 0.025(2) 0.018(2) 0.015(2) 0.004(2) -0.003(2) 0.001(2) C4 0.029(2) 0.021(2) 0.016(2) -0.001(2) 0.003(2) 0.001(2) C5 0.036(3) 0.018(2) 0.023(2) -0.006(2) -0.004(2) 0.003(2) C6 0.042(3) 0.021(2) 0.025(2) -0.002(2) -0.002(2) 0.005(2) C7 0.030(2) 0.029(2) 0.014(2) -0.005(2) -0.004(2) -0.005(2) C8 0.029(2) 0.032(3) 0.018(2) -0.003(2) -0.004(2) 0.000(2) C9 0.028(3) 0.027(2) 0.028(2) 0.010(2) -0.002(2) -0.009(2) C10 0.034(3) 0.016(2) 0.038(3) 0.005(2) -0.006(2) -0.008(2) C11 0.034(3) 0.019(2) 0.032(3) 0.006(2) -0.005(2) 0.001(2) C12 0.037(3) 0.025(2) 0.034(3) -0.003(2) -0.009(2) 0.000(2) C13 0.041(3) 0.048(4) 0.076(4) -0.001(3) -0.025(3) -0.001(3) C14 0.026(3) 0.041(3) 0.033(3) -0.003(2) -0.003(2) 0.000(2) C15 0.031(3) 0.099(5) 0.040(3) -0.025(3) 0.003(2) -0.004(3) C16 0.026(2) 0.026(2) 0.031(2) 0.003(2) -0.008(2) -0.005(2) C17 0.031(3) 0.030(3) 0.030(2) 0.002(2) -0.007(2) -0.008(2) C18 0.042(3) 0.058(4) 0.054(4) 0.008(3) -0.020(3) 0.006(3) C19 0.040(3) 0.117(6) 0.044(4) 0.006(4) -0.009(3) 0.016(4) C20 0.039(3) 0.055(4) 0.048(3) -0.007(3) -0.011(3) 0.004(3) C21 0.040(3) 0.082(5) 0.054(4) -0.007(4) 0.006(3) -0.001(3) C22 0.051(3) 0.019(2) 0.028(2) -0.007(2) -0.007(2) 0.007(2) C23 0.047(3) 0.038(3) 0.038(3) -0.008(2) 0.007(2) 0.004(3) C24 0.034(3) 0.021(2) 0.033(3) -0.004(2) -0.009(2) 0.000(2) C25 0.044(3) 0.036(3) 0.056(4) 0.001(3) -0.023(3) 0.009(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 Ni1 N1 1.952(3) . ? Ni1 N5 2.089(4) . ? Ni1 N4 2.234(4) . ? Ni1 Cl1 2.2828(12) . ? Ni1 Cl3 2.3921(12) . ? Ni2 N2 1.981(3) . ? Ni2 N3 2.166(3) . ? Ni2 Cl2 2.3518(12) . ? Ni2 Cl3 2.4210(11) . ? Ni2 S2 2.4462(13) . ? Ni2 S1 2.5054(13) . ? S1 C12 1.801(5) . ? S1 C6 1.819(4) . ? S2 C14 1.806(5) . ? S2 C8 1.821(4) . ? N1 C1 1.345(5) . ? N1 N2 1.353(4) . ? N2 C3 1.331(5) . ? N3 C7 1.486(5) . ? N3 C5 1.488(5) . ? N3 C4 1.499(5) . ? N4 C10 1.486(6) . ? N4 C16 1.489(5) . ? N4 C9 1.496(5) . ? N5 C24 1.490(5) . ? N5 C22 1.490(5) . ? N5 C11 1.501(5) . ? N6 C18 1.459(7) . ? N6 C20 1.471(7) . ? N6 C17 1.479(6) . ? C1 C2 1.389(6) . ? C1 C9 1.504(6) . ? C2 C3 1.384(6) . ? C2 H2 0.93 . ? C3 C4 1.498(6) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.513(6) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.516(6) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 C11 1.507(6) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 C13 1.515(7) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C14 C15 1.494(7) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 C17 1.522(6) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 C19 1.505(8) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 C21 1.494(8) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 C23 1.504(7) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 C25 1.520(6) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? 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 N5 100.71(14) . . ? N1 Ni1 N4 78.07(14) . . ? N5 Ni1 N4 86.67(14) . . ? N1 Ni1 Cl1 152.32(11) . . ? N5 Ni1 Cl1 105.48(10) . . ? N4 Ni1 Cl1 94.51(10) . . ? N1 Ni1 Cl3 88.95(10) . . ? N5 Ni1 Cl3 102.63(10) . . ? N4 Ni1 Cl3 165.32(10) . . ? Cl1 Ni1 Cl3 93.89(4) . . ? N2 Ni2 N3 78.84(13) . . ? N2 Ni2 Cl2 173.14(10) . . ? N3 Ni2 Cl2 96.93(10) . . ? N2 Ni2 Cl3 87.78(10) . . ? N3 Ni2 Cl3 166.59(10) . . ? Cl2 Ni2 Cl3 96.33(4) . . ? N2 Ni2 S2 88.43(10) . . ? N3 Ni2 S2 83.70(9) . . ? Cl2 Ni2 S2 96.51(5) . . ? Cl3 Ni2 S2 96.77(4) . . ? N2 Ni2 S1 90.34(10) . . ? N3 Ni2 S1 85.23(9) . . ? Cl2 Ni2 S1 83.90(4) . . ? Cl3 Ni2 S1 94.21(4) . . ? S2 Ni2 S1 168.89(4) . . ? Ni1 Cl3 Ni2 105.19(4) . . ? C12 S1 C6 101.3(2) . . ? C12 S1 Ni2 110.1(2) . . ? C6 S1 Ni2 94.12(15) . . ? C14 S2 C8 102.6(2) . . ? C14 S2 Ni2 109.9(2) . . ? C8 S2 Ni2 97.25(15) . . ? C1 N1 N2 107.6(3) . . ? C1 N1 Ni1 123.3(3) . . ? N2 N1 Ni1 129.0(3) . . ? C3 N2 N1 109.1(3) . . ? C3 N2 Ni2 121.4(3) . . ? N1 N2 Ni2 128.6(3) . . ? C7 N3 C5 109.6(3) . . ? C7 N3 C4 111.9(3) . . ? C5 N3 C4 109.8(3) . . ? C7 N3 Ni2 106.5(2) . . ? C5 N3 Ni2 107.2(2) . . ? C4 N3 Ni2 111.6(2) . . ? C10 N4 C16 109.8(3) . . ? C10 N4 C9 110.9(3) . . ? C16 N4 C9 109.6(3) . . ? C10 N4 Ni1 98.6(3) . . ? C16 N4 Ni1 116.7(3) . . ? C9 N4 Ni1 110.8(2) . . ? C24 N5 C22 111.4(4) . . ? C24 N5 C11 110.0(3) . . ? C22 N5 C11 108.9(3) . . ? C24 N5 Ni1 108.6(3) . . ? C22 N5 Ni1 113.9(3) . . ? C11 N5 Ni1 103.6(3) . . ? C18 N6 C20 110.5(4) . . ? C18 N6 C17 112.6(4) . . ? C20 N6 C17 111.0(4) . . ? N1 C1 C2 109.3(4) . . ? N1 C1 C9 116.4(4) . . ? C2 C1 C9 134.3(4) . . ? C3 C2 C1 104.8(4) . . ? C3 C2 H2 127.6(2) . . ? C1 C2 H2 127.6(2) . . ? N2 C3 C2 109.2(4) . . ? N2 C3 C4 116.0(4) . . ? C2 C3 C4 134.7(4) . . ? C3 C4 N3 110.6(3) . . ? C3 C4 H4A 109.5(2) . . ? N3 C4 H4A 109.5(2) . . ? C3 C4 H4B 109.5(2) . . ? N3 C4 H4B 109.5(2) . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 111.8(3) . . ? N3 C5 H5A 109.3(2) . . ? C6 C5 H5A 109.3(2) . . ? N3 C5 H5B 109.3(2) . . ? C6 C5 H5B 109.3(2) . . ? H5A C5 H5B 107.9 . . ? C5 C6 S1 110.8(3) . . ? C5 C6 H6A 109.5(2) . . ? S1 C6 H6A 109.49(15) . . ? C5 C6 H6B 109.5(3) . . ? S1 C6 H6B 109.5(2) . . ? H6A C6 H6B 108.1 . . ? N3 C7 C8 112.5(3) . . ? N3 C7 H7A 109.1(2) . . ? C8 C7 H7A 109.1(2) . . ? N3 C7 H7B 109.1(2) . . ? C8 C7 H7B 109.1(2) . . ? H7A C7 H7B 107.8 . . ? C7 C8 S2 113.3(3) . . ? C7 C8 H8A 108.9(2) . . ? S2 C8 H8A 108.92(15) . . ? C7 C8 H8B 108.9(2) . . ? S2 C8 H8B 108.92(15) . . ? H8A C8 H8B 107.7 . . ? N4 C9 C1 110.6(3) . . ? N4 C9 H9A 109.5(2) . . ? C1 C9 H9A 109.5(2) . . ? N4 C9 H9B 109.5(2) . . ? C1 C9 H9B 109.5(2) . . ? H9A C9 H9B 108.1 . . ? N4 C10 C11 110.3(4) . . ? N4 C10 H10A 109.6(2) . . ? C11 C10 H10A 109.6(3) . . ? N4 C10 H10B 109.6(2) . . ? C11 C10 H10B 109.6(2) . . ? H10A C10 H10B 108.1 . . ? C10 C11 N5 111.7(4) . . ? C10 C11 H11A 109.3(2) . . ? N5 C11 H11A 109.3(2) . . ? C10 C11 H11B 109.3(3) . . ? N5 C11 H11B 109.3(2) . . ? H11A C11 H11B 107.9 . . ? C13 C12 S1 113.0(4) . . ? C13 C12 H12A 109.0(3) . . ? S1 C12 H12A 109.0(2) . . ? C13 C12 H12B 109.0(3) . . ? S1 C12 H12B 109.0(2) . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5(3) . . ? C12 C13 H13B 109.5(3) . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5(3) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 S2 109.4(4) . . ? C15 C14 H14A 109.8(3) . . ? S2 C14 H14A 109.8(2) . . ? C15 C14 H14B 109.8(3) . . ? S2 C14 H14B 109.8(2) . . ? H14A C14 H14B 108.3 . . ? C14 C15 H15A 109.5(3) . . ? C14 C15 H15B 109.5(3) . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5(3) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 112.6(4) . . ? N4 C16 H16A 109.1(2) . . ? C17 C16 H16A 109.1(2) . . ? N4 C16 H16B 109.1(2) . . ? C17 C16 H16B 109.1(3) . . ? H16A C16 H16B 107.8 . . ? N6 C17 C16 111.3(4) . . ? N6 C17 H17A 109.4(2) . . ? C16 C17 H17A 109.4(2) . . ? N6 C17 H17B 109.4(2) . . ? C16 C17 H17B 109.4(3) . . ? H17A C17 H17B 108.0 . . ? N6 C18 C19 111.7(5) . . ? N6 C18 H18A 109.3(3) . . ? C19 C18 H18A 109.3(4) . . ? N6 C18 H18B 109.3(3) . . ? C19 C18 H18B 109.3(3) . . ? H18A C18 H18B 107.9 . . ? C18 C19 H19A 109.5(3) . . ? C18 C19 H19B 109.5(4) . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5(3) . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 C21 113.8(5) . . ? N6 C20 H20A 108.8(3) . . ? C21 C20 H20A 108.8(3) . . ? N6 C20 H20B 108.8(3) . . ? C21 C20 H20B 108.8(3) . . ? H20A C20 H20B 107.7 . . ? C20 C21 H21A 109.5(3) . . ? C20 C21 H21B 109.5(3) . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5(3) . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 C23 114.6(4) . . ? N5 C22 H22A 108.6(2) . . ? C23 C22 H22A 108.6(3) . . ? N5 C22 H22B 108.6(2) . . ? C23 C22 H22B 108.6(3) . . ? H22A C22 H22B 107.6 . . ? C22 C23 H23A 109.5(3) . . ? C22 C23 H23B 109.5(3) . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5(3) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C25 116.2(4) . . ? N5 C24 H24A 108.2(2) . . ? C25 C24 H24A 108.2(3) . . ? N5 C24 H24B 108.2(2) . . ? C25 C24 H24B 108.2(3) . . ? H24A C24 H24B 107.4 . . ? C24 C25 H25A 109.5(3) . . ? C24 C25 H25B 109.5(3) . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5(3) . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 Cl3 Ni2 -2.18(10) . . . . ? N5 Ni1 Cl3 Ni2 -102.92(10) . . . . ? N4 Ni1 Cl3 Ni2 25.4(4) . . . . ? Cl1 Ni1 Cl3 Ni2 150.26(5) . . . . ? N2 Ni2 Cl3 Ni1 4.41(10) . . . . ? N3 Ni2 Cl3 Ni1 1.3(4) . . . . ? Cl2 Ni2 Cl3 Ni1 -170.09(5) . . . . ? S2 Ni2 Cl3 Ni1 92.56(5) . . . . ? S1 Ni2 Cl3 Ni1 -85.77(5) . . . . ? N2 Ni2 S1 C12 -29.3(2) . . . . ? N3 Ni2 S1 C12 -108.1(2) . . . . ? Cl2 Ni2 S1 C12 154.4(2) . . . . ? Cl3 Ni2 S1 C12 58.5(2) . . . . ? S2 Ni2 S1 C12 -112.9(3) . . . . ? N2 Ni2 S1 C6 74.2(2) . . . . ? N3 Ni2 S1 C6 -4.5(2) . . . . ? Cl2 Ni2 S1 C6 -102.0(2) . . . . ? Cl3 Ni2 S1 C6 162.0(2) . . . . ? S2 Ni2 S1 C6 -9.3(3) . . . . ? N2 Ni2 S2 C14 163.2(2) . . . . ? N3 Ni2 S2 C14 -117.8(2) . . . . ? Cl2 Ni2 S2 C14 -21.5(2) . . . . ? Cl3 Ni2 S2 C14 75.7(2) . . . . ? S1 Ni2 S2 C14 -113.0(3) . . . . ? N2 Ni2 S2 C8 -90.5(2) . . . . ? N3 Ni2 S2 C8 -11.6(2) . . . . ? Cl2 Ni2 S2 C8 84.7(2) . . . . ? Cl3 Ni2 S2 C8 -178.1(2) . . . . ? S1 Ni2 S2 C8 -6.8(3) . . . . ? N5 Ni1 N1 C1 -83.9(3) . . . . ? N4 Ni1 N1 C1 0.3(3) . . . . ? Cl1 Ni1 N1 C1 77.1(4) . . . . ? Cl3 Ni1 N1 C1 173.4(3) . . . . ? N5 Ni1 N1 N2 100.1(3) . . . . ? N4 Ni1 N1 N2 -175.6(3) . . . . ? Cl1 Ni1 N1 N2 -98.9(4) . . . . ? Cl3 Ni1 N1 N2 -2.5(3) . . . . ? C1 N1 N2 C3 0.6(4) . . . . ? Ni1 N1 N2 C3 177.1(3) . . . . ? C1 N1 N2 Ni2 -168.3(3) . . . . ? Ni1 N1 N2 Ni2 8.2(5) . . . . ? N3 Ni2 N2 C3 3.9(3) . . . . ? Cl2 Ni2 N2 C3 -48.4(10) . . . . ? Cl3 Ni2 N2 C3 -175.3(3) . . . . ? S2 Ni2 N2 C3 87.8(3) . . . . ? S1 Ni2 N2 C3 -81.1(3) . . . . ? N3 Ni2 N2 N1 171.7(3) . . . . ? Cl2 Ni2 N2 N1 119.3(8) . . . . ? Cl3 Ni2 N2 N1 -7.6(3) . . . . ? S2 Ni2 N2 N1 -104.4(3) . . . . ? S1 Ni2 N2 N1 86.6(3) . . . . ? N2 Ni2 N3 C7 126.7(3) . . . . ? Cl2 Ni2 N3 C7 -58.8(3) . . . . ? Cl3 Ni2 N3 C7 129.8(4) . . . . ? S2 Ni2 N3 C7 37.0(2) . . . . ? S1 Ni2 N3 C7 -142.0(3) . . . . ? N2 Ni2 N3 C5 -116.0(3) . . . . ? Cl2 Ni2 N3 C5 58.5(3) . . . . ? Cl3 Ni2 N3 C5 -112.9(4) . . . . ? S2 Ni2 N3 C5 154.3(3) . . . . ? S1 Ni2 N3 C5 -24.7(2) . . . . ? N2 Ni2 N3 C4 4.2(3) . . . . ? Cl2 Ni2 N3 C4 178.8(2) . . . . ? Cl3 Ni2 N3 C4 7.4(6) . . . . ? S2 Ni2 N3 C4 -85.4(3) . . . . ? S1 Ni2 N3 C4 95.5(3) . . . . ? N1 Ni1 N4 C10 -121.7(3) . . . . ? N5 Ni1 N4 C10 -20.1(3) . . . . ? Cl1 Ni1 N4 C10 85.2(2) . . . . ? Cl3 Ni1 N4 C10 -150.0(3) . . . . ? N1 Ni1 N4 C16 121.0(3) . . . . ? N5 Ni1 N4 C16 -137.3(3) . . . . ? Cl1 Ni1 N4 C16 -32.1(3) . . . . ? Cl3 Ni1 N4 C16 92.7(5) . . . . ? N1 Ni1 N4 C9 -5.4(3) . . . . ? N5 Ni1 N4 C9 96.3(3) . . . . ? Cl1 Ni1 N4 C9 -158.4(3) . . . . ? Cl3 Ni1 N4 C9 -33.7(6) . . . . ? N1 Ni1 N5 C24 -49.2(3) . . . . ? N4 Ni1 N5 C24 -126.4(3) . . . . ? Cl1 Ni1 N5 C24 139.8(3) . . . . ? Cl3 Ni1 N5 C24 42.1(3) . . . . ? N1 Ni1 N5 C22 -174.1(3) . . . . ? N4 Ni1 N5 C22 108.7(3) . . . . ? Cl1 Ni1 N5 C22 15.0(3) . . . . ? Cl3 Ni1 N5 C22 -82.8(3) . . . . ? N1 Ni1 N5 C11 67.7(3) . . . . ? N4 Ni1 N5 C11 -9.5(3) . . . . ? Cl1 Ni1 N5 C11 -103.2(2) . . . . ? Cl3 Ni1 N5 C11 159.1(2) . . . . ? N2 N1 C1 C2 -0.6(4) . . . . ? Ni1 N1 C1 C2 -177.3(3) . . . . ? N2 N1 C1 C9 -178.3(3) . . . . ? Ni1 N1 C1 C9 5.0(5) . . . . ? N1 C1 C2 C3 0.3(5) . . . . ? C9 C1 C2 C3 177.4(5) . . . . ? N1 N2 C3 C2 -0.4(5) . . . . ? Ni2 N2 C3 C2 169.4(3) . . . . ? N1 N2 C3 C4 178.7(3) . . . . ? Ni2 N2 C3 C4 -11.4(5) . . . . ? C1 C2 C3 N2 0.1(5) . . . . ? C1 C2 C3 C4 -178.8(4) . . . . ? N2 C3 C4 N3 14.1(5) . . . . ? C2 C3 C4 N3 -167.1(4) . . . . ? C7 N3 C4 C3 -129.8(4) . . . . ? C5 N3 C4 C3 108.2(4) . . . . ? Ni2 N3 C4 C3 -10.5(4) . . . . ? C7 N3 C5 C6 171.3(3) . . . . ? C4 N3 C5 C6 -65.3(4) . . . . ? Ni2 N3 C5 C6 56.1(4) . . . . ? N3 C5 C6 S1 -63.7(4) . . . . ? C12 S1 C6 C5 145.4(3) . . . . ? Ni2 S1 C6 C5 33.9(3) . . . . ? C5 N3 C7 C8 -174.2(3) . . . . ? C4 N3 C7 C8 63.7(4) . . . . ? Ni2 N3 C7 C8 -58.5(4) . . . . ? N3 C7 C8 S2 48.8(4) . . . . ? C14 S2 C8 C7 97.9(4) . . . . ? Ni2 S2 C8 C7 -14.5(3) . . . . ? C10 N4 C9 C1 117.4(4) . . . . ? C16 N4 C9 C1 -121.2(4) . . . . ? Ni1 N4 C9 C1 9.0(4) . . . . ? N1 C1 C9 N4 -9.3(5) . . . . ? C2 C1 C9 N4 173.8(4) . . . . ? C16 N4 C10 C11 169.3(4) . . . . ? C9 N4 C10 C11 -69.3(4) . . . . ? Ni1 N4 C10 C11 46.9(4) . . . . ? N4 C10 C11 N5 -63.8(5) . . . . ? C24 N5 C11 C10 155.3(4) . . . . ? C22 N5 C11 C10 -82.3(5) . . . . ? Ni1 N5 C11 C10 39.3(4) . . . . ? C6 S1 C12 C13 71.5(4) . . . . ? Ni2 S1 C12 C13 170.2(3) . . . . ? C8 S2 C14 C15 170.3(4) . . . . ? Ni2 S2 C14 C15 -87.1(4) . . . . ? C10 N4 C16 C17 -168.3(4) . . . . ? C9 N4 C16 C17 69.6(5) . . . . ? Ni1 N4 C16 C17 -57.4(4) . . . . ? C18 N6 C17 C16 -122.3(5) . . . . ? C20 N6 C17 C16 113.1(5) . . . . ? N4 C16 C17 N6 -172.7(4) . . . . ? C20 N6 C18 C19 -164.1(5) . . . . ? C17 N6 C18 C19 71.0(6) . . . . ? C18 N6 C20 C21 166.3(5) . . . . ? C17 N6 C20 C21 -68.0(6) . . . . ? C24 N5 C22 C23 -55.4(5) . . . . ? C11 N5 C22 C23 -177.0(4) . . . . ? Ni1 N5 C22 C23 67.9(5) . . . . ? C22 N5 C24 C25 -58.4(5) . . . . ? C11 N5 C24 C25 62.5(5) . . . . ? Ni1 N5 C24 C25 175.3(4) . . . . ? _refine_diff_density_max 0.536 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.091 #=END