# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/213 data_global _publ_contact_letter ; Our. Ref: B004846L Title: Structural dependence of \p-\p interactionsd in dithiocarbazato and thiosemicarbazato nickel complexes Author: Liu Ze-hua, Duan Chun-ying, Li ji-hui and You Xiao-zeng ; _publ_contact_author ; Chun-Ying, Duan Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; _journal_name_full 'New Journal Chemistry.' #============================================================== loop_ _publ_author_name _publ_author_address 'Liu Ze-Hua' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; 'Duan Chun-ying' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; 'Li Ji-hui' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; 'Xiao-Zeng, You' ; Coordination Chemistry Institute & State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, P.R. China ; ################################################################### data_nickle_complex_1 _audit_creation_method SHELXL _chemical_name_systematic ; bis(4,5-diazafluorene thiosemicarbazato)nickel trihydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 N10 Ni O3 S2' _chemical_formula_weight 621.35 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 'Trigonal' _symmetry_space_group_name_H-M 'P3(2)12 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-y, -x, -z+1/3' '-x+y, y, -z+2/3' 'x, x-y, -z' _cell_length_a 10.696(4) _cell_length_b 10.696(4) _cell_length_c 19.748(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1956.6(12) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 4.91 _cell_measurement_theta_max 12.70 _exptl_crystal_description 'block ' _exptl_crystal_colour 'black ' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method ? _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 7.42 _diffrn_reflns_number 6084 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 22.51 _reflns_number_total 1723 _reflns_number_gt 1602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.4623P] 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 mixed _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 0.00(2) _refine_ls_number_reflns 1723 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.79919(4) 0.59838(8) 0.8333 0.0355(2) Uani 1 2 d S . . S1 S 0.61335(14) 0.43127(13) 0.88329(7) 0.0528(4) Uani 1 1 d . . . N1 N 0.4086(5) 0.4824(5) 0.9240(3) 0.0651(13) Uani 1 1 d . . . H1A H 0.3735 0.5357 0.9364 0.078 Uiso 1 1 calc R . . H1B H 0.3549 0.3900 0.9242 0.078 Uiso 1 1 calc R . . N2 N 0.6246(4) 0.6851(4) 0.9052(2) 0.0424(10) Uani 1 1 d . . . N3 N 0.7670(4) 0.7284(4) 0.89047(18) 0.0360(9) Uani 1 1 d . . . N4 N 0.9857(5) 1.2424(4) 0.9293(2) 0.0451(10) Uani 1 1 d . . . N5 N 1.2255(4) 1.1597(4) 0.9188(2) 0.0439(10) Uani 1 1 d . . . C1 C 0.5436(5) 0.5420(5) 0.9050(2) 0.0436(12) Uani 1 1 d . . . C2 C 0.8594(5) 0.8613(5) 0.9077(2) 0.0340(10) Uani 1 1 d . . . C3 C 0.8637(6) 1.2474(5) 0.9369(2) 0.0515(13) Uani 1 1 d . . . H3A H 0.8718 1.3376 0.9420 0.062 Uiso 1 1 calc R . . C4 C 0.7272(6) 1.1280(6) 0.9376(2) 0.0520(13) Uani 1 1 d . . . H4A H 0.6471 1.1394 0.9430 0.062 Uiso 1 1 calc R . . C5 C 0.7089(5) 0.9917(6) 0.9303(2) 0.0454(12) Uani 1 1 d . . . H5A H 0.6178 0.9097 0.9308 0.054 Uiso 1 1 calc R . . C6 C 0.8339(5) 0.9829(5) 0.9222(2) 0.0358(10) Uani 1 1 d . . . C7 C 0.9679(5) 1.1095(5) 0.9228(2) 0.0359(11) Uani 1 1 d . . . C8 C 1.0828(5) 1.0730(4) 0.9160(2) 0.0365(11) Uani 1 1 d . . . C9 C 1.0154(5) 0.9206(5) 0.9088(2) 0.0344(11) Uani 1 1 d . . . C10 C 1.1000(5) 0.8567(5) 0.9107(2) 0.0362(11) Uani 1 1 d . . . H10A H 1.0589 0.7568 0.9096 0.043 Uiso 1 1 calc R . . C11 C 1.2475(5) 0.9462(6) 0.9143(3) 0.0482(13) Uani 1 1 d . . . H11A H 1.3088 0.9080 0.9143 0.058 Uiso 1 1 calc R . . C12 C 1.3030(5) 1.0947(5) 0.9180(3) 0.0494(12) Uani 1 1 d . . . H12A H 1.4029 1.1529 0.9199 0.059 Uiso 1 1 calc R . . O1W O 1.1758(5) 1.5532(5) 0.9331(3) 0.1037(17) Uani 1 1 d . . . H1WA H 1.1049 1.4674 0.9317 0.124 Uiso 1 1 d R . . H1WC H 1.1771 1.5995 0.8979 0.124 Uiso 0.50 1 d PR . . H1WB H 1.1795 1.5898 1.0000 0.124 Uiso 1 2 d SR . . O2W O 1.3625(5) 1.7249(10) 0.8333 0.163(5) Uani 1 2 d S . . H2WB H 1.3449 1.7794 0.8085 0.196 Uiso 0.50 1 d PR . . H2WA H 1.3860 1.6760 0.8080 0.196 Uiso 0.50 1 d 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 0.0358(4) 0.0209(4) 0.0447(4) 0.000 0.0038(3) 0.0104(2) S1 0.0449(7) 0.0258(6) 0.0775(9) 0.0048(6) 0.0173(6) 0.0101(5) N1 0.035(3) 0.033(2) 0.110(4) -0.001(2) 0.018(3) 0.003(2) N2 0.032(2) 0.033(2) 0.055(3) -0.0013(19) 0.0077(19) 0.0115(19) N3 0.035(2) 0.025(2) 0.042(2) 0.0036(16) 0.0050(17) 0.0100(18) N4 0.059(3) 0.027(2) 0.045(2) -0.0044(17) -0.005(2) 0.018(2) N5 0.036(2) 0.029(2) 0.049(2) 0.0015(17) -0.0023(17) 0.004(2) C1 0.038(3) 0.032(3) 0.050(3) 0.000(2) 0.006(2) 0.009(2) C2 0.037(3) 0.025(2) 0.034(2) 0.0013(19) 0.0017(19) 0.011(2) C3 0.075(4) 0.043(3) 0.051(3) -0.005(2) 0.000(3) 0.040(3) C4 0.054(3) 0.054(3) 0.060(3) -0.003(3) 0.002(3) 0.036(3) C5 0.045(3) 0.039(3) 0.050(3) -0.004(2) 0.006(2) 0.020(2) C6 0.041(3) 0.033(3) 0.031(2) -0.0027(18) -0.0012(19) 0.017(2) C7 0.047(3) 0.024(3) 0.032(2) -0.0029(18) -0.004(2) 0.015(2) C8 0.046(3) 0.025(2) 0.031(2) -0.0007(18) -0.001(2) 0.013(2) C9 0.036(3) 0.024(2) 0.030(2) -0.0004(18) 0.0027(19) 0.005(2) C10 0.043(3) 0.025(2) 0.039(3) -0.0015(19) -0.003(2) 0.015(2) C11 0.046(3) 0.050(3) 0.050(3) 0.002(2) 0.002(2) 0.025(3) C12 0.033(3) 0.038(3) 0.068(3) 0.002(2) 0.001(2) 0.010(2) O1W 0.080(4) 0.065(3) 0.156(4) -0.010(3) 0.022(3) 0.029(3) O2W 0.225(11) 0.112(7) 0.115(6) 0.000 -0.018(7) 0.056(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 N3 1.951(4) 5_656 ? Ni1 N3 1.951(4) . ? Ni1 S1 2.1369(15) 5_656 ? Ni1 S1 2.1369(15) . ? S1 C1 1.740(5) . ? N1 C1 1.308(6) . ? N2 C1 1.330(6) . ? N2 N3 1.383(5) . ? N3 C2 1.307(6) . ? N4 C3 1.341(7) . ? N4 C7 1.343(6) . ? N5 C12 1.322(7) . ? N5 C8 1.334(6) . ? C2 C9 1.459(6) . ? C2 C6 1.484(6) . ? C3 C4 1.378(8) . ? C4 C5 1.377(8) . ? C5 C6 1.396(7) . ? C6 C7 1.396(7) . ? C7 C8 1.470(7) . ? C8 C9 1.422(6) . ? C9 C10 1.380(6) . ? C10 C11 1.379(7) . ? C11 C12 1.392(7) . ? 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 N3 Ni1 N3 103.7(2) 5_656 . ? N3 Ni1 S1 84.68(10) 5_656 5_656 ? N3 Ni1 S1 170.85(11) . 5_656 ? N3 Ni1 S1 170.85(11) 5_656 . ? N3 Ni1 S1 84.68(11) . . ? S1 Ni1 S1 87.17(7) 5_656 . ? C1 S1 Ni1 94.64(17) . . ? C1 N2 N3 111.1(4) . . ? C2 N3 N2 114.7(4) . . ? C2 N3 Ni1 128.2(3) . . ? N2 N3 Ni1 116.1(3) . . ? C3 N4 C7 115.3(4) . . ? C12 N5 C8 115.8(4) . . ? N1 C1 N2 119.0(5) . . ? N1 C1 S1 119.0(4) . . ? N2 C1 S1 122.0(4) . . ? N3 C2 C9 123.8(4) . . ? N3 C2 C6 129.2(4) . . ? C9 C2 C6 106.7(4) . . ? N4 C3 C4 124.4(4) . . ? C5 C4 C3 120.3(5) . . ? C4 C5 C6 116.7(5) . . ? C7 C6 C5 119.1(4) . . ? C7 C6 C2 107.6(4) . . ? C5 C6 C2 133.1(4) . . ? N4 C7 C6 124.2(4) . . ? N4 C7 C8 126.5(4) . . ? C6 C7 C8 109.3(4) . . ? N5 C8 C9 123.3(4) . . ? N5 C8 C7 129.1(4) . . ? C9 C8 C7 107.6(4) . . ? C10 C9 C8 118.9(4) . . ? C10 C9 C2 132.5(4) . . ? C8 C9 C2 108.3(4) . . ? C11 C10 C9 117.6(4) . . ? C10 C11 C12 118.9(5) . . ? N5 C12 C11 125.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.211 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.058 ################################################# data_nickle_complex_2 _audit_creation_method SHELXL _chemical_name_systematic ; bis(fluorene-9-one thiosemicarbazato)nickel monohydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H22 N6 Ni O S2' _chemical_formula_weight 581.35 _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' 'Ni' 'Ni' 0.3393 1.1124 '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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2943(14) _cell_length_b 14.670(2) _cell_length_c 15.508(2) _cell_angle_alpha 91.439(14) _cell_angle_beta 99.301(12) _cell_angle_gamma 106.954(12) _cell_volume 2632.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 4.77 _cell_measurement_theta_max 12.21 _exptl_crystal_description 'block ' _exptl_crystal_colour 'dark-brown ' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method ? _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.4969 _exptl_absorpt_correction_T_max 0.5793 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 6.16 _diffrn_reflns_number 7281 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6892 _reflns_number_observed 5637 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 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^)+(0.0646P)^2^+3.8471P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6890 _refine_ls_number_parameters 856 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_obs 0.0420 _refine_ls_wR_factor_all 0.1225 _refine_ls_wR_factor_obs 0.1108 _refine_ls_goodness_of_fit_all 1.007 _refine_ls_goodness_of_fit_obs 1.027 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.028 _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 Ni1 Ni 0.69296(4) 0.20286(4) 0.15255(3) 0.0282(2) Uani 1 d . . S1 S 0.51032(9) 0.18267(9) 0.12660(7) 0.0383(3) Uani 1 d . . S2 S 0.69931(11) 0.24080(10) 0.28795(7) 0.0445(3) Uani 1 d . . N1 N 0.4091(4) 0.1940(3) -0.0355(4) 0.0447(11) Uani 1 d . . H1NA H 0.3496(47) 0.1938(35) -0.0079(33) 0.051(15) Uiso 1 d . . H1NB H 0.4046(49) 0.1915(40) -0.0823(37) 0.052(20) Uiso 1 d . . N2 N 0.5849(3) 0.1680(3) -0.0260(2) 0.0322(8) Uani 1 d . . N3 N 0.6718(3) 0.1490(2) 0.0340(2) 0.0286(8) Uani 1 d . . N4 N 0.8696(5) 0.2221(3) 0.4061(3) 0.0463(11) Uani 1 d . . H4NA H 0.8132(44) 0.2088(34) 0.4386(33) 0.044(15) Uiso 1 d . . H4NB H 0.9366(52) 0.2194(40) 0.4248(37) 0.063(19) Uiso 1 d . . N5 N 0.9071(3) 0.2292(3) 0.2657(2) 0.0368(9) Uani 1 d . . N6 N 0.8588(3) 0.2455(2) 0.1813(2) 0.0313(8) Uani 1 d . . C1 C 0.5035(4) 0.1812(3) 0.0133(3) 0.0316(10) Uani 1 d . . C2 C 0.7351(3) 0.1055(3) -0.0007(3) 0.0300(10) Uani 1 d . . C3 C 0.8302(5) 0.0083(4) -0.1831(4) 0.0520(14) Uani 1 d . . H3A H 0.8661(43) -0.0388(36) -0.1879(32) 0.051(15) Uiso 1 d . . C4 C 0.8041(6) 0.0596(5) -0.2515(4) 0.065(2) Uani 1 d . . H4A H 0.8245(53) 0.0449(44) -0.3020(42) 0.083(20) Uiso 1 d . . C5 C 0.7524(5) 0.1303(5) -0.2422(4) 0.060(2) Uani 1 d . . H5A H 0.7446(49) 0.1707(42) -0.2833(39) 0.067(18) Uiso 1 d . . C6 C 0.7221(4) 0.1486(4) -0.1627(3) 0.0443(12) Uani 1 d . . H6A H 0.6877(37) 0.1952(32) -0.1584(28) 0.034(12) Uiso 1 d . . C7 C 0.7457(4) 0.0967(3) -0.0940(3) 0.0347(10) Uani 1 d . . C8 C 0.8034(4) 0.0277(3) -0.1031(3) 0.0368(11) Uani 1 d . . C9 C 0.8304(4) -0.0079(3) -0.0173(3) 0.0358(11) Uani 1 d . . C10 C 0.7972(3) 0.0436(3) 0.0463(3) 0.0308(10) Uani 1 d . . C11 C 0.8104(4) 0.0216(3) 0.1332(3) 0.0369(11) Uani 1 d . . H11A H 0.7757(42) 0.0506(35) 0.1821(33) 0.057(15) Uiso 1 d . . C12 C 0.8574(4) -0.0522(3) 0.1557(3) 0.0430(12) Uani 1 d . . H12A H 0.8703(39) -0.0705(32) 0.2214(32) 0.047(13) Uiso 1 d . . C13 C 0.8906(4) -0.1026(4) 0.0922(4) 0.0492(13) Uani 1 d . . H13A H 0.9178(42) -0.1517(37) 0.1141(32) 0.051(14) Uiso 1 d . . C14 C 0.8765(4) -0.0812(4) 0.0053(4) 0.0454(12) Uani 1 d . . H14A H 0.8993(38) -0.1172(33) -0.0429(31) 0.046(13) Uiso 1 d . . C15 C 0.8368(4) 0.2288(3) 0.3205(3) 0.0355(11) Uani 1 d . . C16 C 0.9310(4) 0.2831(3) 0.1308(3) 0.0331(10) Uani 1 d . . C17 C 1.2051(5) 0.3392(4) 0.0511(5) 0.059(2) Uani 1 d . . H17A H 1.2264(48) 0.3633(40) -0.0020(37) 0.065(17) Uiso 1 d . . C18 C 1.2793(5) 0.3165(4) 0.1170(5) 0.068(2) Uani 1 d . . H18A H 1.3560(53) 0.3216(40) 0.1100(36) 0.071(17) Uiso 1 d . . C19 C 1.2447(5) 0.2843(5) 0.1933(5) 0.067(2) Uani 1 d . . H19A H 1.2878(48) 0.2694(38) 0.2326(36) 0.053(17) Uiso 1 d . . C20 C 1.1328(4) 0.2712(4) 0.2071(4) 0.0527(14) Uani 1 d . . H20A H 1.1105(44) 0.2570(37) 0.2610(35) 0.055(16) Uiso 1 d . . C21 C 1.0561(4) 0.2934(3) 0.1403(3) 0.0397(11) Uani 1 d . . C22 C 1.0920(4) 0.3277(3) 0.0630(3) 0.0444(12) Uani 1 d . . C23 C 0.9972(4) 0.3487(3) 0.0059(3) 0.0425(12) Uani 1 d . . C24 C 0.9001(4) 0.3242(3) 0.0468(3) 0.0352(10) Uani 1 d . . C25 C 0.8043(5) 0.3507(3) 0.0129(3) 0.0402(11) Uani 1 d . . H25A H 0.7452(36) 0.3364(28) 0.0376(26) 0.020(11) Uiso 1 d . . C26 C 0.8025(5) 0.3952(4) -0.0647(3) 0.0518(13) Uani 1 d . . H26A H 0.7364(41) 0.4111(33) -0.0859(30) 0.042(13) Uiso 1 d . . C27 C 0.8951(6) 0.4150(4) -0.1066(4) 0.063(2) Uani 1 d . . H27A H 0.8894(47) 0.4467(40) -0.1584(38) 0.067(17) Uiso 1 d . . C28 C 0.9921(6) 0.3921(4) -0.0721(4) 0.058(2) Uani 1 d . . H28A H 1.0553(45) 0.4102(36) -0.0891(33) 0.048(16) Uiso 1 d . . Ni2 Ni 0.74714(5) 0.88013(4) 0.40790(3) 0.0289(2) Uani 1 d . . S21 S 0.83964(11) 0.97614(8) 0.52011(7) 0.0388(3) Uani 1 d . . S22 S 0.69733(11) 0.99142(8) 0.34145(7) 0.0400(3) Uani 1 d . . N21 N 0.9749(4) 0.9212(4) 0.6474(3) 0.0470(12) Uani 1 d . . H1ND H 1.0069(52) 0.8707(45) 0.6728(40) 0.081(20) Uiso 1 d . . H1NC H 1.0046(41) 0.9638(34) 0.6490(32) 0.020(16) Uiso 1 d . . N22 N 0.8579(3) 0.8008(2) 0.5509(2) 0.0347(9) Uani 1 d . . N23 N 0.7633(3) 0.7795(2) 0.4819(2) 0.0306(8) Uani 1 d . . N24 N 0.5412(4) 0.9517(4) 0.1966(3) 0.0467(11) Uani 1 d . . H4ND H 0.5392(45) 1.0099(42) 0.2061(34) 0.058(17) Uiso 1 d . . H4NC H 0.5074(40) 0.9216(34) 0.1551(32) 0.031(14) Uiso 1 d . . N25 N 0.6127(3) 0.8285(2) 0.2355(2) 0.0351(9) Uani 1 d . . N26 N 0.6986(3) 0.8086(2) 0.2955(2) 0.0296(8) Uani 1 d . . C31 C 0.8938(4) 0.8918(3) 0.5743(3) 0.0323(10) Uani 1 d . . C32 C 0.7056(4) 0.6889(3) 0.4675(3) 0.0322(10) Uani 1 d . . C33 C 0.6866(7) 0.4381(4) 0.4449(4) 0.068(2) Uani 1 d . . H33A H 0.6295(49) 0.3825(43) 0.4108(37) 0.070(17) Uiso 1 d . . C34 C 0.7886(7) 0.4318(5) 0.4921(5) 0.080(2) Uani 1 d . . H34A H 0.8080(53) 0.3721(48) 0.4858(40) 0.086(20) Uiso 1 d . . C35 C 0.8669(6) 0.5104(4) 0.5395(4) 0.068(2) Uani 1 d . . H35A H 0.9355(44) 0.5127(35) 0.5742(33) 0.050(15) Uiso 1 d . . C36 C 0.8464(5) 0.5982(4) 0.5413(4) 0.0500(13) Uani 1 d . . H36A H 0.9012(48) 0.6529(41) 0.5755(35) 0.065(17) Uiso 1 d . . C37 C 0.7448(4) 0.6055(3) 0.4926(3) 0.0387(11) Uani 1 d . . C38 C 0.6635(5) 0.5243(3) 0.4452(3) 0.0470(13) Uani 1 d . . C39 C 0.5647(4) 0.5519(3) 0.4000(3) 0.0448(12) Uani 1 d . . C40 C 0.5895(4) 0.6510(3) 0.4127(3) 0.0360(11) Uani 1 d . . C41 C 0.5070(4) 0.6956(4) 0.3820(3) 0.0466(12) Uani 1 d . . H41A H 0.5210(38) 0.7590(35) 0.3971(29) 0.037(13) Uiso 1 d . . C42 C 0.4010(5) 0.6393(5) 0.3357(4) 0.060(2) Uani 1 d . . H42A H 0.3396(50) 0.6684(40) 0.3131(37) 0.071(17) Uiso 1 d . . C43 C 0.3775(5) 0.5425(5) 0.3213(4) 0.065(2) Uani 1 d . . H43A H 0.2959(59) 0.5054(47) 0.2861(42) 0.097(21) Uiso 1 d . . C44 C 0.4574(5) 0.4976(4) 0.3540(4) 0.065(2) Uani 1 d . . H44A H 0.4374(45) 0.4283(42) 0.3455(34) 0.061(16) Uiso 1 d . . C45 C 0.6099(4) 0.9164(3) 0.2526(3) 0.0337(10) Uani 1 d . . C46 C 0.7303(4) 0.7344(3) 0.2733(3) 0.0296(10) Uani 1 d . . C47 C 0.6939(5) 0.4984(4) 0.1729(4) 0.0514(13) Uani 1 d . . H47A H 0.7420(38) 0.4570(33) 0.1786(29) 0.038(12) Uiso 1 d . . C48 C 0.5851(5) 0.4727(4) 0.1218(4) 0.0589(15) Uani 1 d . . H48A H 0.5607(55) 0.4105(48) 0.0845(43) 0.096(21) Uiso 1 d . . C49 C 0.5189(5) 0.5342(4) 0.1158(4) 0.0547(14) Uani 1 d . . H49A H 0.4410(53) 0.5122(43) 0.0800(39) 0.079(19) Uiso 1 d . . C50 C 0.5592(4) 0.6248(3) 0.1602(3) 0.0415(12) Uani 1 d . . H50A H 0.5149(38) 0.6624(32) 0.1568(28) 0.033(13) Uiso 1 d . . C51 C 0.6676(4) 0.6515(3) 0.2107(3) 0.0317(10) Uani 1 d . . C52 C 0.7352(4) 0.5884(3) 0.2176(3) 0.0374(11) Uani 1 d . . C53 C 0.8444(4) 0.6326(3) 0.2761(3) 0.0368(11) Uani 1 d . . C54 C 0.8419(4) 0.7215(3) 0.3111(3) 0.0323(10) Uani 1 d . . C55 C 0.9399(4) 0.7837(4) 0.3606(3) 0.0359(11) Uani 1 d . . H55A H 0.9387(38) 0.8410(35) 0.3793(29) 0.039(13) Uiso 1 d . . C56 C 1.0399(4) 0.7573(4) 0.3760(3) 0.0450(12) Uani 1 d . . H56A H 1.1046(45) 0.8013(36) 0.4120(33) 0.053(15) Uiso 1 d . . C57 C 1.0424(5) 0.6697(4) 0.3446(3) 0.0512(14) Uani 1 d . . H57A H 1.1127(45) 0.6536(35) 0.3548(32) 0.053(14) Uiso 1 d . . C58 C 0.9443(5) 0.6060(4) 0.2946(3) 0.0487(13) Uani 1 d . . H58A H 0.9451(39) 0.5454(35) 0.2697(30) 0.046(13) Uiso 1 d . . O1W O 0.6669(6) 0.1711(7) 0.5132(4) 0.181(4) Uani 1 d . . H1WA H 0.6728(6) 0.1905(7) 0.5252(4) 0.272 Uiso 1 d R . H1WB H 0.5986(6) 0.0927(7) 0.5289(4) 0.272 Uiso 1 d R . O2W O 0.4101(13) 0.1444(15) 0.3513(11) 0.154(8) Uani 0.47(2) d PU . H2WA H 0.3438(13) 0.0819(15) 0.3723(11) 0.231 Uiso 0.47(2) d PR 1 H2WB H 0.3203(13) 0.1419(15) 0.3190(11) 0.231 Uiso 0.47(2) d PR 1 O2W' O 0.4544(14) 0.1955(16) 0.4080(12) 0.199(8) Uani 0.53(2) d PU 2 H2WD H 0.4596(14) 0.1179(16) 0.4356(12) 0.298 Uiso 0.53(2) d PR 2 H2WC H 0.4837(14) 0.2379(16) 0.4108(12) 0.298 Uiso 0.53(2) d PR 2 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 0.0289(3) 0.0344(3) 0.0224(3) -0.0007(2) 0.0030(2) 0.0120(2) S1 0.0319(6) 0.0573(8) 0.0308(6) 0.0054(5) 0.0077(5) 0.0197(6) S2 0.0504(8) 0.0657(8) 0.0260(6) -0.0032(5) 0.0045(5) 0.0322(7) N1 0.037(3) 0.063(3) 0.039(3) 0.005(2) 0.001(2) 0.025(2) N2 0.029(2) 0.043(2) 0.025(2) 0.001(2) -0.001(2) 0.013(2) N3 0.026(2) 0.034(2) 0.025(2) -0.0009(15) 0.003(2) 0.009(2) N4 0.050(3) 0.060(3) 0.028(2) 0.000(2) -0.002(2) 0.021(2) N5 0.037(2) 0.045(2) 0.024(2) -0.001(2) -0.001(2) 0.011(2) N6 0.035(2) 0.034(2) 0.024(2) -0.001(2) 0.001(2) 0.011(2) C1 0.029(2) 0.031(2) 0.032(2) 0.002(2) 0.002(2) 0.007(2) C2 0.026(2) 0.033(2) 0.028(2) -0.002(2) 0.004(2) 0.006(2) C3 0.053(3) 0.061(4) 0.047(3) -0.007(3) 0.021(3) 0.019(3) C4 0.082(4) 0.079(4) 0.038(3) -0.006(3) 0.030(3) 0.021(4) C5 0.080(4) 0.072(4) 0.037(3) 0.011(3) 0.021(3) 0.028(3) C6 0.051(3) 0.046(3) 0.037(3) 0.002(2) 0.013(2) 0.013(3) C7 0.031(2) 0.040(3) 0.031(2) -0.005(2) 0.007(2) 0.006(2) C8 0.031(2) 0.041(3) 0.036(3) -0.008(2) 0.009(2) 0.005(2) C9 0.025(2) 0.036(3) 0.044(3) -0.007(2) 0.008(2) 0.006(2) C10 0.021(2) 0.034(2) 0.034(3) -0.003(2) 0.003(2) 0.005(2) C11 0.031(2) 0.037(3) 0.037(3) -0.003(2) -0.001(2) 0.005(2) C12 0.035(3) 0.041(3) 0.046(3) 0.001(2) -0.004(2) 0.006(2) C13 0.035(3) 0.037(3) 0.071(4) 0.003(3) 0.000(3) 0.010(2) C14 0.033(3) 0.043(3) 0.058(3) -0.011(3) 0.006(2) 0.011(2) C15 0.044(3) 0.029(2) 0.029(3) -0.004(2) -0.003(2) 0.009(2) C16 0.033(2) 0.029(2) 0.035(2) -0.003(2) 0.004(2) 0.007(2) C17 0.050(4) 0.041(3) 0.088(5) 0.002(3) 0.029(3) 0.007(3) C18 0.033(3) 0.050(4) 0.122(6) -0.001(4) 0.023(4) 0.009(3) C19 0.036(3) 0.056(4) 0.103(6) 0.003(4) -0.004(4) 0.013(3) C20 0.033(3) 0.054(3) 0.065(4) 0.005(3) 0.000(3) 0.010(2) C21 0.033(3) 0.032(3) 0.052(3) -0.003(2) 0.008(2) 0.006(2) C22 0.039(3) 0.034(3) 0.059(3) -0.002(2) 0.017(2) 0.006(2) C23 0.044(3) 0.038(3) 0.044(3) 0.000(2) 0.015(2) 0.004(2) C24 0.036(3) 0.031(2) 0.034(2) 0.001(2) 0.006(2) 0.004(2) C25 0.044(3) 0.036(3) 0.040(3) 0.006(2) 0.012(3) 0.009(2) C26 0.058(4) 0.047(3) 0.049(3) 0.007(3) 0.001(3) 0.018(3) C27 0.082(5) 0.059(4) 0.047(3) 0.018(3) 0.016(3) 0.016(3) C28 0.064(4) 0.056(4) 0.056(4) 0.012(3) 0.029(3) 0.010(3) Ni2 0.0349(3) 0.0258(3) 0.0239(3) -0.0026(2) -0.0012(2) 0.0098(2) S21 0.0521(7) 0.0325(6) 0.0295(6) -0.0066(5) -0.0054(5) 0.0164(5) S22 0.0552(8) 0.0287(6) 0.0329(6) -0.0034(5) -0.0069(5) 0.0161(5) N21 0.055(3) 0.038(3) 0.040(3) -0.004(2) -0.008(2) 0.009(3) N22 0.041(2) 0.032(2) 0.028(2) -0.002(2) -0.002(2) 0.011(2) N23 0.034(2) 0.032(2) 0.025(2) -0.0001(15) 0.003(2) 0.011(2) N24 0.051(3) 0.040(3) 0.046(3) -0.006(2) -0.016(2) 0.021(2) N25 0.038(2) 0.032(2) 0.033(2) -0.002(2) -0.006(2) 0.014(2) N26 0.033(2) 0.025(2) 0.026(2) -0.0012(15) -0.001(2) 0.007(2) C31 0.036(2) 0.039(3) 0.021(2) -0.003(2) 0.002(2) 0.013(2) C32 0.040(3) 0.030(3) 0.026(2) 0.000(2) 0.006(2) 0.009(2) C33 0.106(5) 0.036(3) 0.059(4) -0.005(3) 0.005(4) 0.023(3) C34 0.119(6) 0.044(4) 0.088(5) 0.006(3) 0.011(4) 0.043(4) C35 0.073(4) 0.057(4) 0.078(4) 0.014(3) 0.002(4) 0.035(3) C36 0.052(3) 0.037(3) 0.062(3) 0.014(3) 0.007(3) 0.015(3) C37 0.047(3) 0.031(3) 0.039(3) 0.007(2) 0.014(2) 0.009(2) C38 0.067(3) 0.030(3) 0.040(3) 0.005(2) 0.011(3) 0.008(2) C39 0.050(3) 0.041(3) 0.034(3) -0.001(2) 0.007(2) -0.001(2) C40 0.039(3) 0.034(3) 0.031(2) 0.001(2) 0.009(2) 0.003(2) C41 0.043(3) 0.048(3) 0.047(3) 0.000(3) 0.011(2) 0.010(3) C42 0.035(3) 0.079(5) 0.059(4) 0.006(3) 0.005(3) 0.010(3) C43 0.047(3) 0.068(4) 0.060(4) 0.007(3) -0.002(3) -0.009(3) C44 0.073(4) 0.043(3) 0.056(4) -0.003(3) 0.004(3) -0.011(3) C45 0.037(3) 0.032(3) 0.031(2) 0.000(2) -0.001(2) 0.013(2) C46 0.033(2) 0.027(2) 0.026(2) 0.002(2) 0.003(2) 0.007(2) C47 0.057(3) 0.038(3) 0.061(3) -0.009(3) 0.013(3) 0.016(3) C48 0.066(4) 0.041(3) 0.062(4) -0.021(3) 0.009(3) 0.007(3) C49 0.050(3) 0.049(3) 0.051(3) -0.015(3) -0.002(3) 0.001(3) C50 0.045(3) 0.035(3) 0.039(3) -0.006(2) -0.001(2) 0.009(2) C51 0.039(3) 0.028(2) 0.028(2) 0.000(2) 0.009(2) 0.009(2) C52 0.050(3) 0.031(3) 0.030(2) -0.002(2) 0.009(2) 0.010(2) C53 0.046(3) 0.039(3) 0.030(2) 0.007(2) 0.010(2) 0.018(2) C54 0.039(3) 0.032(2) 0.025(2) 0.003(2) 0.003(2) 0.012(2) C55 0.040(3) 0.040(3) 0.029(2) 0.004(2) 0.006(2) 0.013(2) C56 0.041(3) 0.063(4) 0.030(3) 0.009(2) 0.001(2) 0.017(3) C57 0.045(3) 0.070(4) 0.047(3) 0.017(3) 0.008(3) 0.029(3) C58 0.065(4) 0.047(3) 0.047(3) 0.007(3) 0.015(3) 0.032(3) O1W 0.137(6) 0.361(12) 0.078(4) -0.026(5) -0.001(4) 0.139(7) O2W 0.104(10) 0.222(18) 0.077(11) -0.006(10) 0.010(8) -0.036(10) O2W' 0.106(11) 0.326(21) 0.139(13) -0.096(14) 0.004(10) 0.046(12) _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 N6 1.923(3) . ? Ni1 N3 1.929(3) . ? Ni1 S2 2.1420(12) . ? Ni1 S1 2.1461(12) . ? S1 C1 1.745(4) . ? S2 C15 1.745(5) . ? N1 C1 1.344(6) . ? N2 C1 1.309(5) . ? N2 N3 1.398(5) . ? N3 C2 1.308(5) . ? N4 C15 1.339(6) . ? N5 C15 1.306(6) . ? N5 N6 1.404(5) . ? N6 C16 1.290(5) . ? C2 C7 1.479(6) . ? C2 C10 1.483(6) . ? C3 C4 1.367(8) . ? C3 C8 1.378(7) . ? C4 C5 1.381(9) . ? C5 C6 1.385(7) . ? C6 C7 1.368(7) . ? C7 C8 1.411(6) . ? C8 C9 1.465(6) . ? C9 C14 1.382(7) . ? C9 C10 1.407(6) . ? C10 C11 1.389(6) . ? C11 C12 1.395(7) . ? C12 C13 1.398(7) . ? C13 C14 1.386(8) . ? C16 C21 1.484(6) . ? C16 C24 1.488(6) . ? C17 C18 1.372(9) . ? C17 C22 1.394(7) . ? C18 C19 1.370(10) . ? C19 C20 1.385(8) . ? C20 C21 1.396(7) . ? C21 C22 1.400(7) . ? C22 C23 1.458(7) . ? C23 C28 1.382(7) . ? C23 C24 1.401(6) . ? C24 C25 1.376(7) . ? C25 C26 1.383(7) . ? C26 C27 1.364(8) . ? C27 C28 1.364(9) . ? Ni2 N26 1.924(3) . ? Ni2 N23 1.928(3) . ? Ni2 S22 2.1367(12) . ? Ni2 S21 2.1467(12) . ? S21 C31 1.742(4) . ? S22 C45 1.738(4) . ? N21 C31 1.351(6) . ? N22 C31 1.299(5) . ? N22 N23 1.402(5) . ? N23 C32 1.306(5) . ? N24 C45 1.332(6) . ? N25 C45 1.322(5) . ? N25 N26 1.394(5) . ? N26 C46 1.314(5) . ? C32 C37 1.478(6) . ? C32 C40 1.480(6) . ? C33 C38 1.374(7) . ? C33 C34 1.374(9) . ? C34 C35 1.371(9) . ? C35 C36 1.383(8) . ? C36 C37 1.385(7) . ? C37 C38 1.409(7) . ? C38 C39 1.468(7) . ? C39 C44 1.393(7) . ? C39 C40 1.398(6) . ? C40 C41 1.389(7) . ? C41 C42 1.392(8) . ? C42 C43 1.368(9) . ? C43 C44 1.375(9) . ? C46 C54 1.470(6) . ? C46 C51 1.472(6) . ? C47 C48 1.381(8) . ? C47 C52 1.389(7) . ? C48 C49 1.375(8) . ? C49 C50 1.395(7) . ? C50 C51 1.374(6) . ? C51 C52 1.409(6) . ? C52 C53 1.454(6) . ? C53 C58 1.384(7) . ? C53 C54 1.411(6) . ? C54 C55 1.377(6) . ? C55 C56 1.381(7) . ? C56 C57 1.372(8) . ? C57 C58 1.390(8) . ? O2W O2W' 1.10(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 N6 Ni1 N3 100.30(14) . . ? N6 Ni1 S2 84.97(11) . . ? N3 Ni1 S2 170.88(11) . . ? N6 Ni1 S1 169.27(11) . . ? N3 Ni1 S1 85.68(10) . . ? S2 Ni1 S1 90.32(5) . . ? C1 S1 Ni1 93.43(15) . . ? C15 S2 Ni1 93.76(15) . . ? C1 N2 N3 110.9(3) . . ? C2 N3 N2 114.5(3) . . ? C2 N3 Ni1 129.1(3) . . ? N2 N3 Ni1 116.0(2) . . ? C15 N5 N6 110.7(3) . . ? C16 N6 N5 116.2(3) . . ? C16 N6 Ni1 127.6(3) . . ? N5 N6 Ni1 116.1(3) . . ? N2 C1 N1 118.8(4) . . ? N2 C1 S1 123.5(3) . . ? N1 C1 S1 117.7(4) . . ? N3 C2 C7 127.8(4) . . ? N3 C2 C10 124.7(4) . . ? C7 C2 C10 107.0(3) . . ? C4 C3 C8 118.7(5) . . ? C3 C4 C5 121.7(5) . . ? C4 C5 C6 120.1(6) . . ? C7 C6 C5 119.0(5) . . ? C6 C7 C8 120.4(4) . . ? C6 C7 C2 131.7(4) . . ? C8 C7 C2 107.4(4) . . ? C3 C8 C7 120.0(5) . . ? C3 C8 C9 131.1(5) . . ? C7 C8 C9 108.9(4) . . ? C14 C9 C10 120.9(4) . . ? C14 C9 C8 130.2(4) . . ? C10 C9 C8 108.9(4) . . ? C11 C10 C9 120.5(4) . . ? C11 C10 C2 131.5(4) . . ? C9 C10 C2 107.3(4) . . ? C10 C11 C12 118.4(4) . . ? C11 C12 C13 120.7(5) . . ? C14 C13 C12 120.9(5) . . ? C9 C14 C13 118.7(5) . . ? N5 C15 N4 120.5(4) . . ? N5 C15 S2 122.8(3) . . ? N4 C15 S2 116.7(4) . . ? N6 C16 C21 129.6(4) . . ? N6 C16 C24 124.6(4) . . ? C21 C16 C24 105.8(4) . . ? C18 C17 C22 118.3(6) . . ? C19 C18 C17 121.4(6) . . ? C18 C19 C20 121.9(7) . . ? C19 C20 C21 117.3(6) . . ? C20 C21 C22 120.8(5) . . ? C20 C21 C16 131.6(5) . . ? C22 C21 C16 107.5(4) . . ? C17 C22 C21 120.3(5) . . ? C17 C22 C23 129.9(5) . . ? C21 C22 C23 109.8(4) . . ? C28 C23 C24 119.6(5) . . ? C28 C23 C22 132.0(5) . . ? C24 C23 C22 108.2(4) . . ? C25 C24 C23 119.6(4) . . ? C25 C24 C16 131.5(4) . . ? C23 C24 C16 108.3(4) . . ? C24 C25 C26 119.3(5) . . ? C27 C26 C25 121.0(6) . . ? C28 C27 C26 120.4(6) . . ? C27 C28 C23 120.1(6) . . ? N26 Ni2 N23 99.84(14) . . ? N26 Ni2 S22 85.56(10) . . ? N23 Ni2 S22 166.81(11) . . ? N26 Ni2 S21 165.62(11) . . ? N23 Ni2 S21 85.72(11) . . ? S22 Ni2 S21 91.92(5) . . ? C31 S21 Ni2 94.53(14) . . ? C45 S22 Ni2 94.79(15) . . ? C31 N22 N23 110.6(3) . . ? C32 N23 N22 114.6(3) . . ? C32 N23 Ni2 126.7(3) . . ? N22 N23 Ni2 117.9(3) . . ? C45 N25 N26 110.1(3) . . ? C46 N26 N25 115.9(3) . . ? C46 N26 Ni2 125.2(3) . . ? N25 N26 Ni2 118.4(2) . . ? N22 C31 N21 117.2(4) . . ? N22 C31 S21 124.1(3) . . ? N21 C31 S21 118.6(4) . . ? N23 C32 C37 128.4(4) . . ? N23 C32 C40 124.4(4) . . ? C37 C32 C40 106.9(4) . . ? C38 C33 C34 119.6(6) . . ? C35 C34 C33 120.6(6) . . ? C34 C35 C36 121.4(6) . . ? C35 C36 C37 118.3(6) . . ? C36 C37 C38 120.2(4) . . ? C36 C37 C32 132.2(4) . . ? C38 C37 C32 107.0(4) . . ? C33 C38 C37 119.9(5) . . ? C33 C38 C39 131.1(5) . . ? C37 C38 C39 108.9(4) . . ? C44 C39 C40 119.7(5) . . ? C44 C39 C38 131.6(5) . . ? C40 C39 C38 108.6(4) . . ? C41 C40 C39 120.6(5) . . ? C41 C40 C32 131.3(4) . . ? C39 C40 C32 107.9(4) . . ? C40 C41 C42 118.2(5) . . ? C43 C42 C41 121.3(6) . . ? C42 C43 C44 120.8(6) . . ? C43 C44 C39 119.4(6) . . ? N25 C45 N24 118.7(4) . . ? N25 C45 S22 123.4(3) . . ? N24 C45 S22 117.8(4) . . ? N26 C46 C54 123.0(4) . . ? N26 C46 C51 129.6(4) . . ? C54 C46 C51 107.5(3) . . ? C48 C47 C52 118.3(5) . . ? C49 C48 C47 120.9(5) . . ? C48 C49 C50 121.5(5) . . ? C51 C50 C49 118.1(5) . . ? C50 C51 C52 120.5(4) . . ? C50 C51 C46 132.4(4) . . ? C52 C51 C46 106.6(4) . . ? C47 C52 C51 120.6(4) . . ? C47 C52 C53 129.6(5) . . ? C51 C52 C53 109.7(4) . . ? C58 C53 C54 119.8(4) . . ? C58 C53 C52 131.7(4) . . ? C54 C53 C52 108.2(4) . . ? C55 C54 C53 120.3(4) . . ? C55 C54 C46 131.3(4) . . ? C53 C54 C46 107.7(4) . . ? C54 C55 C56 119.0(5) . . ? C57 C56 C55 121.2(5) . . ? C56 C57 C58 120.6(5) . . ? C53 C58 C57 119.0(5) . . ? _refine_diff_density_max 1.439 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.068 ######################################### data_nickel_complex_3 _audit_creation_method SHELXL _chemical_name_systematic ; bis(fluorene-9-one S-phenyl-dithiocarbazato)nickel ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H30 N4 Ni S4' _chemical_formula_weight 777.65 _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' '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 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9236(11) _cell_length_b 21.696(3) _cell_length_c 18.933(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.772(12) _cell_angle_gamma 90.00 _cell_volume 3600.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 4.60 _cell_measurement_theta_max 12.41 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method ? _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.4305 _exptl_absorpt_correction_T_max 0.4644 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 18.25 _diffrn_reflns_number 7019 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.51 _reflns_number_total 6247 _reflns_number_observed 4304 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 34 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^)+(0.0447P)^2^+3.0244P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6213 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_obs 0.0490 _refine_ls_wR_factor_all 0.1571 _refine_ls_wR_factor_obs 0.1103 _refine_ls_goodness_of_fit_all 1.074 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_restrained_S_all 1.264 _refine_ls_restrained_S_obs 1.083 _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 Ni1 Ni 0.11162(6) 0.24510(2) 0.76095(3) 0.0422(2) Uani 1 d . . S1 S 0.26950(14) 0.16931(5) 0.77975(6) 0.0560(3) Uani 1 d . . S2 S -0.07295(13) 0.18106(4) 0.73111(6) 0.0555(3) Uani 1 d . . S3 S 0.5737(2) 0.17321(6) 0.86864(7) 0.0718(4) Uani 1 d . . S4 S -0.37604(15) 0.21021(6) 0.64872(7) 0.0667(3) Uani 1 d . . N1 N 0.4232(4) 0.27418(14) 0.8173(2) 0.0489(8) Uani 1 d . . N2 N 0.2917(4) 0.29693(14) 0.7726(2) 0.0429(8) Uani 1 d . . N3 N -0.1846(4) 0.29639(14) 0.7112(2) 0.0482(8) Uani 1 d . . N4 N -0.0463(4) 0.30672(13) 0.7585(2) 0.0433(8) Uani 1 d . . C1 C 0.4201(5) 0.2149(2) 0.8211(2) 0.0479(10) Uani 1 d . . C2 C 0.3025(4) 0.3548(2) 0.7530(2) 0.0430(9) Uani 1 d . . C3 C 0.5446(7) 0.5123(2) 0.8387(3) 0.0752(15) Uani 1 d . . H3A H 0.5915(7) 0.5489(2) 0.8563(3) 0.090 Uiso 1 calc R . C4 C 0.4240(6) 0.5140(2) 0.7818(3) 0.0682(14) Uani 1 d . . H4A H 0.3883(6) 0.5514(2) 0.7613(3) 0.082 Uiso 1 calc R . C5 C 0.5967(6) 0.4575(2) 0.8699(3) 0.0700(14) Uani 1 d . . H5A H 0.6783(6) 0.4575(2) 0.9085(3) 0.084 Uiso 1 calc R . C6 C 0.5292(5) 0.4017(2) 0.8447(2) 0.0574(11) Uani 1 d . . H6A H 0.5642(5) 0.3646(2) 0.8663(2) 0.069 Uiso 1 calc R . C7 C 0.4095(5) 0.4029(2) 0.7870(2) 0.0492(10) Uani 1 d . . C8 C 0.3565(5) 0.4593(2) 0.7555(2) 0.0501(10) Uani 1 d . . C9 C 0.2294(5) 0.4480(2) 0.6964(2) 0.0513(11) Uani 1 d . . C10 C 0.1963(5) 0.3843(2) 0.6938(2) 0.0450(9) Uani 1 d . . C11 C 0.0908(5) 0.3597(2) 0.6385(2) 0.0578(11) Uani 1 d . . H11A H 0.0743(5) 0.3174(2) 0.6351(2) 0.069 Uiso 1 calc R . C12 C 0.0096(6) 0.3997(3) 0.5880(3) 0.0734(14) Uani 1 d . . H12A H -0.0627(6) 0.3841(3) 0.5505(3) 0.088 Uiso 1 calc R . C13 C 0.0355(6) 0.4627(3) 0.5931(3) 0.076(2) Uani 1 d . . H13A H -0.0228(6) 0.4890(3) 0.5601(3) 0.091 Uiso 1 calc R . C14 C 0.1461(6) 0.4871(2) 0.6463(3) 0.0680(13) Uani 1 d . . H14A H 0.1646(6) 0.5293(2) 0.6484(3) 0.082 Uiso 1 calc R . C15 C 0.7200(5) 0.2307(2) 0.8921(3) 0.0676(13) Uani 1 d . . H15A H 0.7970(5) 0.2353(2) 0.8655(3) 0.081 Uiso 1 calc R . C16 C 0.7142(5) 0.2713(2) 0.9561(2) 0.0530(11) Uani 1 d . . C17 C 0.6128(6) 0.2644(2) 1.0010(3) 0.0670(13) Uani 1 d . . H17A H 0.5402(6) 0.2331(2) 0.9930(3) 0.080 Uiso 1 calc R . C18 C 0.6180(7) 0.3044(3) 1.0595(3) 0.081(2) Uani 1 d . . H18A H 0.5486(7) 0.2996(3) 1.0901(3) 0.097 Uiso 1 calc R . C19 C 0.7230(8) 0.3501(3) 1.0720(3) 0.088(2) Uani 1 d . . H19A H 0.7241(8) 0.3769(3) 1.1104(3) 0.105 Uiso 1 calc R . C20 C 0.8269(7) 0.3568(3) 1.0282(3) 0.089(2) Uani 1 d . . H20A H 0.9007(7) 0.3875(3) 1.0372(3) 0.106 Uiso 1 calc R . C21 C 0.8215(6) 0.3177(2) 0.9708(3) 0.0718(14) Uani 1 d . . H21A H 0.8923(6) 0.3226(2) 0.9409(3) 0.086 Uiso 1 calc R . C22 C -0.2054(5) 0.2379(2) 0.6986(2) 0.0482(10) Uani 1 d . . C23 C -0.0348(5) 0.3617(2) 0.7880(2) 0.0435(9) Uani 1 d . . C24 C -0.0860(8) 0.5275(2) 0.7883(4) 0.092(2) Uani 1 d . . H24A H -0.0373(8) 0.5600(2) 0.8154(4) 0.111 Uiso 1 calc R . C25 C -0.2002(9) 0.5386(3) 0.7305(4) 0.106(3) Uani 1 d . . H25A H -0.2286(9) 0.5791(3) 0.7188(4) 0.127 Uiso 1 calc R . C26 C -0.2752(7) 0.4910(3) 0.6888(3) 0.088(2) Uani 1 d . . H26A H -0.3528(7) 0.5000(3) 0.6501(3) 0.106 Uiso 1 calc R . C27 C -0.2340(6) 0.4295(2) 0.7050(3) 0.0667(13) Uani 1 d . . H27A H -0.2828(6) 0.3973(2) 0.6776(3) 0.080 Uiso 1 calc R . C28 C -0.1186(5) 0.4187(2) 0.7630(3) 0.0541(11) Uani 1 d . . C29 C -0.0444(6) 0.4668(2) 0.8057(3) 0.0666(14) Uani 1 d . . C30 C 0.0744(6) 0.4419(2) 0.8621(3) 0.0679(14) Uani 1 d . . C31 C 0.0796(5) 0.3779(2) 0.8520(2) 0.0519(11) Uani 1 d . . C32 C 0.1704(5) 0.3414(2) 0.9018(2) 0.0634(12) Uani 1 d . . H32A H 0.1693(5) 0.2988(2) 0.8970(2) 0.076 Uiso 1 calc R . C33 C 0.2643(7) 0.3699(3) 0.9598(3) 0.092(2) Uani 1 d . . H33A H 0.3279(7) 0.3461(3) 0.9937(3) 0.111 Uiso 1 calc R . C34 C 0.2638(9) 0.4328(4) 0.9673(4) 0.120(3) Uani 1 d . . H34A H 0.3292(9) 0.4511(4) 1.0055(4) 0.144 Uiso 1 calc R . C35 C 0.1694(8) 0.4687(3) 0.9199(4) 0.106(2) Uani 1 d . . H35A H 0.1686(8) 0.5111(3) 0.9263(4) 0.127 Uiso 1 calc R . C36 C -0.4898(5) 0.2792(2) 0.6294(2) 0.0617(12) Uani 1 d . . H36A H -0.5601(5) 0.2908(2) 0.6576(2) 0.074 Uiso 1 calc R . C37 C -0.4663(5) 0.3172(2) 0.5660(2) 0.0577(11) Uani 1 d . . C38 C -0.5544(7) 0.3690(3) 0.5501(3) 0.090(2) Uani 1 d . . H38A H -0.6252(7) 0.3792(3) 0.5785(3) 0.108 Uiso 1 calc R . C39 C -0.5396(9) 0.4064(3) 0.4926(4) 0.115(2) Uani 1 d . . H39A H -0.5973(9) 0.4422(3) 0.4839(4) 0.137 Uiso 1 calc R . C40 C -0.4415(8) 0.3910(3) 0.4491(3) 0.094(2) Uani 1 d . . H40A H -0.4338(8) 0.4154(3) 0.4096(3) 0.112 Uiso 1 calc R . C41 C -0.3550(7) 0.3402(3) 0.4636(3) 0.086(2) Uani 1 d . . H41A H -0.2866(7) 0.3298(3) 0.4340(3) 0.103 Uiso 1 calc R . C42 C -0.3663(6) 0.3029(2) 0.5219(3) 0.0706(14) Uani 1 d . . H42A H -0.3053(6) 0.2680(2) 0.5311(3) 0.085 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 0.0539(3) 0.0280(3) 0.0461(3) -0.0010(2) 0.0128(2) -0.0008(2) S1 0.0688(7) 0.0308(5) 0.0662(7) -0.0050(5) 0.0072(6) 0.0055(5) S2 0.0634(7) 0.0304(5) 0.0731(8) -0.0007(5) 0.0136(6) -0.0077(5) S3 0.0817(9) 0.0484(7) 0.0777(9) -0.0060(6) -0.0045(7) 0.0241(6) S4 0.0664(8) 0.0524(7) 0.0759(8) -0.0027(6) -0.0006(6) -0.0152(6) N1 0.054(2) 0.036(2) 0.056(2) -0.002(2) 0.012(2) 0.007(2) N2 0.052(2) 0.032(2) 0.047(2) -0.0005(14) 0.014(2) 0.0034(14) N3 0.050(2) 0.037(2) 0.056(2) -0.001(2) 0.007(2) -0.004(2) N4 0.051(2) 0.031(2) 0.050(2) -0.0045(14) 0.014(2) -0.0046(14) C1 0.058(3) 0.040(2) 0.046(2) -0.002(2) 0.011(2) 0.010(2) C2 0.050(2) 0.034(2) 0.048(2) 0.001(2) 0.017(2) 0.001(2) C3 0.095(4) 0.047(3) 0.084(4) -0.006(3) 0.018(3) -0.020(3) C4 0.088(4) 0.036(2) 0.084(4) 0.007(2) 0.023(3) -0.006(2) C5 0.078(4) 0.055(3) 0.072(3) -0.003(2) 0.002(3) -0.014(3) C6 0.063(3) 0.041(2) 0.066(3) 0.003(2) 0.007(2) -0.004(2) C7 0.057(3) 0.038(2) 0.056(3) 0.000(2) 0.019(2) 0.000(2) C8 0.057(3) 0.036(2) 0.061(3) 0.007(2) 0.020(2) -0.004(2) C9 0.063(3) 0.043(2) 0.053(3) 0.012(2) 0.025(2) 0.006(2) C10 0.052(2) 0.043(2) 0.045(2) 0.007(2) 0.020(2) 0.002(2) C11 0.069(3) 0.060(3) 0.048(2) 0.003(2) 0.018(2) -0.003(2) C12 0.078(4) 0.094(4) 0.047(3) 0.007(3) 0.008(3) -0.002(3) C13 0.090(4) 0.079(4) 0.059(3) 0.029(3) 0.016(3) 0.007(3) C14 0.081(4) 0.060(3) 0.067(3) 0.021(3) 0.024(3) 0.006(3) C15 0.054(3) 0.084(3) 0.066(3) -0.022(3) 0.016(2) 0.004(2) C16 0.052(3) 0.057(3) 0.049(2) 0.009(2) 0.008(2) 0.014(2) C17 0.073(3) 0.071(3) 0.060(3) 0.002(2) 0.018(3) -0.002(3) C18 0.097(4) 0.092(4) 0.057(3) 0.005(3) 0.026(3) 0.017(4) C19 0.121(5) 0.066(4) 0.067(4) -0.010(3) -0.006(4) 0.020(4) C20 0.099(5) 0.065(3) 0.092(4) -0.003(3) -0.006(4) -0.002(3) C21 0.067(3) 0.072(3) 0.078(4) 0.011(3) 0.018(3) 0.004(3) C22 0.056(3) 0.044(2) 0.045(2) -0.001(2) 0.011(2) -0.010(2) C23 0.053(2) 0.031(2) 0.051(2) 0.000(2) 0.022(2) -0.005(2) C24 0.116(5) 0.039(3) 0.136(6) -0.005(3) 0.061(5) 0.004(3) C25 0.144(6) 0.041(3) 0.157(7) 0.023(4) 0.093(6) 0.030(4) C26 0.098(5) 0.067(4) 0.110(5) 0.031(3) 0.047(4) 0.035(3) C27 0.074(3) 0.048(3) 0.085(4) 0.014(2) 0.030(3) 0.012(2) C28 0.065(3) 0.032(2) 0.073(3) 0.004(2) 0.031(3) 0.005(2) C29 0.088(4) 0.033(2) 0.092(4) -0.012(2) 0.050(3) -0.002(2) C30 0.077(4) 0.050(3) 0.084(4) -0.023(3) 0.035(3) -0.013(2) C31 0.061(3) 0.043(2) 0.057(3) -0.012(2) 0.027(2) -0.007(2) C32 0.066(3) 0.071(3) 0.056(3) -0.011(2) 0.020(2) -0.006(3) C33 0.093(4) 0.118(5) 0.061(3) -0.027(3) 0.002(3) -0.008(4) C34 0.138(7) 0.123(6) 0.091(5) -0.058(5) -0.001(5) -0.022(5) C35 0.134(6) 0.070(4) 0.117(5) -0.054(4) 0.027(5) -0.026(4) C36 0.053(3) 0.072(3) 0.064(3) 0.004(2) 0.021(2) 0.003(2) C37 0.053(3) 0.066(3) 0.054(3) -0.010(2) 0.009(2) -0.011(2) C38 0.091(4) 0.090(4) 0.099(4) 0.020(4) 0.045(4) 0.027(3) C39 0.133(6) 0.097(5) 0.120(6) 0.041(4) 0.041(5) 0.035(4) C40 0.097(5) 0.100(5) 0.084(4) 0.029(4) 0.017(4) -0.007(4) C41 0.084(4) 0.118(5) 0.062(3) 0.001(3) 0.028(3) -0.007(4) C42 0.072(3) 0.078(3) 0.065(3) -0.004(3) 0.020(3) 0.004(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 N4 1.936(3) . ? Ni1 N2 1.939(3) . ? Ni1 S2 2.1482(12) . ? Ni1 S1 2.1512(12) . ? S1 C1 1.733(4) . ? S2 C22 1.738(4) . ? S3 C1 1.745(4) . ? S3 C15 1.801(5) . ? S4 C22 1.742(4) . ? S4 C36 1.808(5) . ? N1 C1 1.290(5) . ? N1 N2 1.402(4) . ? N2 C2 1.317(5) . ? N3 C22 1.299(5) . ? N3 N4 1.401(4) . ? N4 C23 1.314(4) . ? C2 C10 1.472(5) . ? C2 C7 1.478(5) . ? C3 C5 1.370(7) . ? C3 C4 1.374(7) . ? C4 C8 1.380(6) . ? C5 C6 1.397(6) . ? C6 C7 1.378(6) . ? C7 C8 1.406(5) . ? C8 C9 1.457(6) . ? C9 C14 1.381(6) . ? C9 C10 1.413(5) . ? C10 C11 1.378(6) . ? C11 C12 1.391(6) . ? C12 C13 1.387(7) . ? C13 C14 1.377(7) . ? C15 C16 1.505(6) . ? C16 C17 1.362(6) . ? C16 C21 1.381(6) . ? C17 C18 1.401(7) . ? C18 C19 1.354(8) . ? C19 C20 1.361(8) . ? C20 C21 1.373(7) . ? C23 C31 1.474(6) . ? C23 C28 1.475(5) . ? C24 C25 1.369(9) . ? C24 C29 1.392(7) . ? C25 C26 1.392(9) . ? C26 C27 1.402(6) . ? C27 C28 1.378(6) . ? C28 C29 1.407(6) . ? C29 C30 1.460(7) . ? C30 C35 1.381(8) . ? C30 C31 1.403(6) . ? C31 C32 1.374(6) . ? C32 C33 1.395(7) . ? C33 C34 1.371(9) . ? C34 C35 1.355(9) . ? C36 C37 1.502(6) . ? C37 C42 1.367(6) . ? C37 C38 1.373(7) . ? C38 C39 1.383(8) . ? C39 C40 1.351(9) . ? C40 C41 1.345(8) . ? C41 C42 1.387(7) . ? 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 N4 Ni1 N2 100.71(13) . . ? N4 Ni1 S2 85.50(10) . . ? N2 Ni1 S2 169.43(10) . . ? N4 Ni1 S1 169.35(10) . . ? N2 Ni1 S1 85.49(10) . . ? S2 Ni1 S1 89.73(5) . . ? C1 S1 Ni1 93.87(13) . . ? C22 S2 Ni1 94.10(14) . . ? C1 S3 C15 103.4(2) . . ? C22 S4 C36 103.0(2) . . ? C1 N1 N2 111.2(3) . . ? C2 N2 N1 114.1(3) . . ? C2 N2 Ni1 128.5(3) . . ? N1 N2 Ni1 116.5(2) . . ? C22 N3 N4 110.6(3) . . ? C23 N4 N3 113.9(3) . . ? C23 N4 Ni1 128.2(3) . . ? N3 N4 Ni1 117.1(2) . . ? N1 C1 S1 124.5(3) . . ? N1 C1 S3 121.5(3) . . ? S1 C1 S3 113.9(2) . . ? N2 C2 C10 124.0(4) . . ? N2 C2 C7 128.7(4) . . ? C10 C2 C7 107.2(3) . . ? C5 C3 C4 120.9(4) . . ? C3 C4 C8 119.1(4) . . ? C3 C5 C6 121.0(5) . . ? C7 C6 C5 118.4(4) . . ? C6 C7 C8 120.1(4) . . ? C6 C7 C2 132.4(4) . . ? C8 C7 C2 107.0(4) . . ? C4 C8 C7 120.4(4) . . ? C4 C8 C9 130.3(4) . . ? C7 C8 C9 109.3(4) . . ? C14 C9 C10 119.6(4) . . ? C14 C9 C8 131.7(4) . . ? C10 C9 C8 108.7(3) . . ? C11 C10 C9 121.0(4) . . ? C11 C10 C2 131.3(4) . . ? C9 C10 C2 107.4(4) . . ? C10 C11 C12 118.3(4) . . ? C11 C12 C13 120.6(5) . . ? C14 C13 C12 121.1(5) . . ? C13 C14 C9 119.1(5) . . ? C16 C15 S3 118.1(4) . . ? C17 C16 C21 118.1(5) . . ? C17 C16 C15 124.4(4) . . ? C21 C16 C15 117.5(4) . . ? C16 C17 C18 119.8(5) . . ? C19 C18 C17 120.8(5) . . ? C18 C19 C20 119.9(5) . . ? C19 C20 C21 119.3(6) . . ? C20 C21 C16 122.0(5) . . ? N3 C22 S2 124.3(3) . . ? N3 C22 S4 121.1(3) . . ? S2 C22 S4 114.5(2) . . ? N4 C23 C31 123.6(4) . . ? N4 C23 C28 129.1(4) . . ? C31 C23 C28 107.2(3) . . ? C25 C24 C29 118.7(6) . . ? C24 C25 C26 122.0(5) . . ? C25 C26 C27 120.1(6) . . ? C28 C27 C26 117.7(5) . . ? C27 C28 C29 122.1(4) . . ? C27 C28 C23 131.1(4) . . ? C29 C28 C23 106.3(4) . . ? C24 C29 C28 119.4(6) . . ? C24 C29 C30 130.4(5) . . ? C28 C29 C30 110.2(4) . . ? C35 C30 C31 119.5(6) . . ? C35 C30 C29 132.8(5) . . ? C31 C30 C29 107.7(4) . . ? C32 C31 C30 120.5(5) . . ? C32 C31 C23 131.0(4) . . ? C30 C31 C23 108.2(4) . . ? C31 C32 C33 118.3(5) . . ? C34 C33 C32 120.6(6) . . ? C35 C34 C33 121.1(6) . . ? C34 C35 C30 119.8(6) . . ? C37 C36 S4 117.3(3) . . ? C42 C37 C38 117.6(5) . . ? C42 C37 C36 124.7(5) . . ? C38 C37 C36 117.7(4) . . ? C37 C38 C39 121.2(6) . . ? C40 C39 C38 120.2(6) . . ? C41 C40 C39 119.4(6) . . ? C40 C41 C42 121.0(6) . . ? C37 C42 C41 120.5(5) . . ? _refine_diff_density_max 0.440 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.058 ############################################## data_nickel_complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(4,5-diazafluorene-9-one S-phenyl-dithiocarbazato)nickel ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H26 N8 Ni S4' _chemical_formula_weight 781.62 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' '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 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.594(3) _cell_length_b 8.500(4) _cell_length_c 38.598(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.79(2) _cell_angle_gamma 90.00 _cell_volume 3451.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.45 _cell_measurement_theta_max 12.45 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method ? _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2362 _exptl_absorpt_correction_T_max 0.2887 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 8.55 _diffrn_reflns_number 6322 _diffrn_reflns_av_R_equivalents 0.1044 _diffrn_reflns_av_sigmaI/netI 0.1818 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5991 _reflns_number_gt 2628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5991 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1588 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.1830 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.41185(9) 0.33650(11) 0.08119(3) 0.0447(3) Uani 1 1 d . . . S1 S 0.4868(2) 0.2437(3) 0.03617(6) 0.0543(6) Uani 1 1 d . . . S2 S 0.2420(2) 0.1948(3) 0.07491(7) 0.0605(6) Uani 1 1 d . . . S3 S 0.7380(2) 0.3045(3) 0.01404(6) 0.0605(6) Uani 1 1 d . . . S4 S 0.0655(2) 0.1681(3) 0.12801(7) 0.0712(7) Uani 1 1 d . . . N1 N 0.6734(6) 0.4032(7) 0.07365(18) 0.0434(16) Uani 1 1 d . . . N2 N 0.5838(6) 0.3968(7) 0.09785(17) 0.0399(15) Uani 1 1 d . . . N3 N 0.8113(6) 0.6998(8) 0.19157(18) 0.0567(19) Uani 1 1 d . . . N4 N 0.5968(7) 0.5247(9) 0.2197(2) 0.067(2) Uani 1 1 d . . . N5 N 0.2244(6) 0.4057(7) 0.12692(18) 0.0497(18) Uani 1 1 d . . . N6 N 0.3229(6) 0.4687(7) 0.11022(17) 0.0475(17) Uani 1 1 d . . . N7 N 0.3819(6) 0.9512(8) 0.1757(2) 0.0583(19) Uani 1 1 d . . . N8 N 0.5500(7) 0.9626(8) 0.1182(2) 0.065(2) Uani 1 1 d . . . C1 C 0.6361(7) 0.3311(9) 0.0459(2) 0.0437(19) Uani 1 1 d . . . C2 C 0.6242(7) 0.4491(8) 0.1287(2) 0.041(2) Uani 1 1 d . . . C3 C 0.8979(8) 0.7623(10) 0.1728(3) 0.064(3) Uani 1 1 d . . . H3A H 0.9554 0.8340 0.1839 0.076 Uiso 1 1 calc R . . C4 C 0.9078(8) 0.7290(10) 0.1390(3) 0.059(2) Uani 1 1 d . . . H4A H 0.9710 0.7773 0.1280 0.071 Uiso 1 1 calc R . . C5 C 0.8258(7) 0.6245(9) 0.1204(2) 0.050(2) Uani 1 1 d . . . H5A H 0.8296 0.6020 0.0970 0.060 Uiso 1 1 calc R . . C6 C 0.7360(7) 0.5549(8) 0.1399(2) 0.045(2) Uani 1 1 d . . . C7 C 0.7325(7) 0.6005(9) 0.1737(2) 0.045(2) Uani 1 1 d . . . C8 C 0.6285(7) 0.5184(9) 0.1877(2) 0.048(2) Uani 1 1 d . . . C9 C 0.5641(7) 0.4248(9) 0.1605(2) 0.0421(19) Uani 1 1 d . . . C10 C 0.4753(7) 0.3186(9) 0.1692(2) 0.051(2) Uani 1 1 d . . . H10A H 0.4378 0.2468 0.1529 0.061 Uiso 1 1 calc R . . C11 C 0.4437(8) 0.3218(11) 0.2025(2) 0.063(2) Uani 1 1 d . . . H11A H 0.3821 0.2537 0.2091 0.075 Uiso 1 1 calc R . . C12 C 0.5045(9) 0.4281(12) 0.2265(3) 0.072(3) Uani 1 1 d . . . H12A H 0.4786 0.4313 0.2487 0.086 Uiso 1 1 calc R . . C13 C 0.8887(7) 0.3725(9) 0.0358(2) 0.053(2) Uani 1 1 d . . . H13A H 0.8945 0.3395 0.0600 0.064 Uiso 1 1 calc R . . H13B H 0.9556 0.3186 0.0254 0.064 Uiso 1 1 calc R . . C14 C 0.9167(7) 0.5490(9) 0.0353(2) 0.045(2) Uani 1 1 d . . . C15 C 1.0313(8) 0.6017(11) 0.0528(2) 0.063(3) Uani 1 1 d . . . H15A H 1.0885 0.5288 0.0636 0.076 Uiso 1 1 calc R . . C16 C 1.0620(9) 0.7592(12) 0.0545(3) 0.076(3) Uani 1 1 d . . . H16A H 1.1399 0.7908 0.0661 0.091 Uiso 1 1 calc R . . C17 C 0.9804(9) 0.8678(11) 0.0396(3) 0.070(3) Uani 1 1 d . . . H17A H 0.9996 0.9743 0.0420 0.084 Uiso 1 1 calc R . . C18 C 0.8671(8) 0.8198(11) 0.0207(2) 0.064(3) Uani 1 1 d . . . H18A H 0.8130 0.8935 0.0090 0.077 Uiso 1 1 calc R . . C19 C 0.8346(8) 0.6587(10) 0.0194(2) 0.054(2) Uani 1 1 d . . . H19A H 0.7571 0.6268 0.0077 0.065 Uiso 1 1 calc R . . C20 C 0.1841(7) 0.2740(9) 0.1103(2) 0.053(2) Uani 1 1 d . . . C21 C 0.3499(7) 0.6188(9) 0.1191(2) 0.045(2) Uani 1 1 d . . . C22 C 0.3017(8) 0.9236(10) 0.2002(2) 0.064(3) Uani 1 1 d . . . H22A H 0.2980 0.9960 0.2181 0.077 Uiso 1 1 calc R . . C23 C 0.2245(8) 0.7887(10) 0.1991(3) 0.064(3) Uani 1 1 d . . . H23A H 0.1698 0.7731 0.2160 0.077 Uiso 1 1 calc R . . C24 C 0.2303(8) 0.6792(9) 0.1728(2) 0.054(2) Uani 1 1 d . . . H24A H 0.1807 0.5886 0.1716 0.064 Uiso 1 1 calc R . . C25 C 0.3111(7) 0.7087(8) 0.1488(2) 0.0416(19) Uani 1 1 d . . . C26 C 0.3858(7) 0.8445(9) 0.1518(2) 0.046(2) Uani 1 1 d . . . C27 C 0.4659(7) 0.8502(9) 0.1231(2) 0.051(2) Uani 1 1 d . . . C28 C 0.4386(6) 0.7188(8) 0.1017(2) 0.0417(19) Uani 1 1 d . . . C29 C 0.4901(7) 0.7077(9) 0.0707(2) 0.053(2) Uani 1 1 d . . . H29A H 0.4688 0.6262 0.0551 0.064 Uiso 1 1 calc R . . C30 C 0.5754(8) 0.8241(10) 0.0641(3) 0.065(3) Uani 1 1 d . . . H30A H 0.6139 0.8215 0.0437 0.078 Uiso 1 1 calc R . . C31 C 0.6032(8) 0.9435(10) 0.0878(3) 0.060(3) Uani 1 1 d . . . H31A H 0.6630 1.0176 0.0827 0.072 Uiso 1 1 calc R . . C32 C 0.0344(9) 0.2860(10) 0.1649(3) 0.074(3) Uani 1 1 d . . . H32A H 0.1144 0.3175 0.1779 0.088 Uiso 1 1 calc R . . H32B H -0.0109 0.3806 0.1567 0.088 Uiso 1 1 calc R . . C33 C -0.0431(8) 0.1970(9) 0.1886(3) 0.059(2) Uani 1 1 d . . . C34 C 0.0086(9) 0.1444(10) 0.2211(3) 0.068(3) Uani 1 1 d . . . H34A H 0.0933 0.1662 0.2287 0.081 Uiso 1 1 calc R . . C35 C -0.0618(11) 0.0610(11) 0.2424(3) 0.082(3) Uani 1 1 d . . . H35A H -0.0269 0.0262 0.2643 0.098 Uiso 1 1 calc R . . C36 C -0.1898(11) 0.0306(12) 0.2295(4) 0.089(4) Uani 1 1 d . . . H36A H -0.2397 -0.0293 0.2428 0.107 Uiso 1 1 calc R . . C37 C -0.2413(10) 0.0862(12) 0.1984(4) 0.084(4) Uani 1 1 d . . . H37A H -0.3273 0.0705 0.1913 0.101 Uiso 1 1 calc R . . C38 C -0.1693(9) 0.1653(10) 0.1772(3) 0.070(3) Uani 1 1 d . . . H38A H -0.2047 0.1979 0.1551 0.084 Uiso 1 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 0.0392(5) 0.0345(5) 0.0605(7) -0.0078(6) 0.0062(5) -0.0060(5) S1 0.0504(13) 0.0500(13) 0.0623(15) -0.0174(11) 0.0058(11) -0.0065(11) S2 0.0542(13) 0.0504(14) 0.0771(18) -0.0134(12) 0.0085(12) -0.0187(11) S3 0.0589(14) 0.0567(14) 0.0689(17) -0.0147(12) 0.0196(12) -0.0042(11) S4 0.0600(15) 0.0530(14) 0.103(2) 0.0024(15) 0.0207(14) -0.0201(13) N1 0.041(4) 0.036(4) 0.054(5) -0.002(3) 0.012(3) -0.005(3) N2 0.038(4) 0.031(3) 0.050(4) -0.005(3) 0.001(3) -0.005(3) N3 0.054(4) 0.058(5) 0.058(5) -0.009(4) 0.006(4) -0.009(4) N4 0.063(5) 0.077(5) 0.064(6) -0.010(4) 0.022(4) -0.015(4) N5 0.042(4) 0.040(4) 0.069(5) 0.004(4) 0.019(3) -0.008(3) N6 0.037(4) 0.038(4) 0.068(5) -0.008(3) 0.009(3) -0.004(3) N7 0.062(5) 0.046(4) 0.070(5) -0.005(4) 0.021(4) -0.004(4) N8 0.061(5) 0.032(4) 0.104(7) 0.001(4) 0.023(4) -0.010(4) C1 0.054(5) 0.031(4) 0.046(5) -0.005(4) 0.006(4) -0.004(4) C2 0.037(4) 0.025(4) 0.060(6) 0.002(4) 0.002(4) 0.003(3) C3 0.055(6) 0.048(5) 0.085(8) -0.020(5) -0.002(5) -0.009(5) C4 0.051(5) 0.051(5) 0.073(7) -0.011(5) -0.003(5) -0.016(4) C5 0.048(5) 0.043(5) 0.060(6) -0.007(4) 0.015(4) -0.003(4) C6 0.039(5) 0.030(4) 0.064(6) -0.006(4) 0.000(4) 0.004(4) C7 0.039(5) 0.038(4) 0.059(6) -0.003(4) 0.006(4) 0.002(4) C8 0.044(5) 0.047(5) 0.052(6) 0.001(4) 0.004(4) 0.005(4) C9 0.038(4) 0.038(4) 0.052(6) -0.002(4) 0.010(4) 0.002(4) C10 0.043(5) 0.037(5) 0.072(7) 0.011(5) 0.006(4) -0.003(4) C11 0.055(5) 0.065(6) 0.071(7) 0.020(6) 0.017(5) -0.012(5) C12 0.065(6) 0.091(8) 0.064(7) 0.003(6) 0.026(5) -0.009(6) C13 0.047(5) 0.046(5) 0.068(6) -0.004(4) 0.016(4) 0.008(4) C14 0.048(5) 0.048(5) 0.042(5) 0.003(4) 0.014(4) 0.006(4) C15 0.049(6) 0.064(6) 0.075(7) 0.011(5) -0.001(5) 0.005(5) C16 0.059(6) 0.078(7) 0.086(8) 0.009(6) -0.007(5) -0.021(6) C17 0.067(6) 0.055(6) 0.090(8) -0.004(6) 0.016(6) -0.009(5) C18 0.061(6) 0.063(6) 0.072(7) 0.016(5) 0.024(5) 0.009(5) C19 0.049(5) 0.052(5) 0.062(6) 0.012(5) 0.006(4) -0.001(5) C20 0.035(4) 0.036(5) 0.089(7) 0.004(5) 0.010(4) -0.005(4) C21 0.032(4) 0.041(5) 0.059(6) -0.004(4) -0.005(4) 0.002(3) C22 0.069(6) 0.055(6) 0.070(7) -0.008(5) 0.019(5) 0.002(5) C23 0.063(6) 0.057(6) 0.076(7) 0.005(5) 0.024(5) 0.004(5) C24 0.056(5) 0.039(5) 0.066(6) -0.004(5) 0.009(4) -0.007(4) C25 0.039(4) 0.033(4) 0.054(5) -0.002(4) 0.011(4) 0.002(3) C26 0.050(5) 0.035(4) 0.053(5) -0.002(4) 0.006(4) -0.001(4) C27 0.042(5) 0.031(5) 0.080(7) 0.003(5) 0.014(4) 0.002(4) C28 0.031(4) 0.036(4) 0.059(6) 0.004(4) 0.010(4) -0.002(3) C29 0.051(5) 0.034(5) 0.076(7) 0.008(4) 0.012(5) 0.012(4) C30 0.068(6) 0.041(5) 0.093(8) 0.028(6) 0.037(5) 0.014(5) C31 0.070(6) 0.044(5) 0.072(7) 0.024(5) 0.034(5) -0.001(5) C32 0.079(7) 0.050(6) 0.096(8) -0.003(5) 0.027(6) -0.010(5) C33 0.054(6) 0.029(5) 0.096(8) 0.003(5) 0.023(5) 0.002(4) C34 0.068(6) 0.045(6) 0.094(8) -0.015(6) 0.026(6) 0.000(5) C35 0.113(9) 0.056(6) 0.085(8) -0.004(6) 0.046(7) -0.003(6) C36 0.087(9) 0.063(7) 0.130(12) -0.026(8) 0.065(8) -0.022(7) C37 0.062(7) 0.067(7) 0.132(12) 0.013(7) 0.043(8) 0.010(6) C38 0.064(6) 0.052(6) 0.098(8) 0.010(6) 0.025(6) 0.012(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 N6 1.912(6) . ? Ni1 N2 1.928(6) . ? Ni1 S1 2.144(2) . ? Ni1 S2 2.155(2) . ? S1 C1 1.747(8) . ? S2 C20 1.702(9) . ? S3 C1 1.746(8) . ? S3 C13 1.808(8) . ? S4 C20 1.748(8) . ? S4 C32 1.804(9) . ? N1 C1 1.256(9) . ? N1 N2 1.409(8) . ? N2 C2 1.295(9) . ? N3 C7 1.322(9) . ? N3 C3 1.344(11) . ? N4 C8 1.320(10) . ? N4 C12 1.326(10) . ? N5 C20 1.334(10) . ? N5 N6 1.397(8) . ? N6 C21 1.343(9) . ? N7 C26 1.296(9) . ? N7 C22 1.364(10) . ? N8 C27 1.334(9) . ? N8 C31 1.372(10) . ? C2 C9 1.462(10) . ? C2 C6 1.509(10) . ? C3 C4 1.352(12) . ? C4 C5 1.382(10) . ? C5 C6 1.410(10) . ? C6 C7 1.368(11) . ? C7 C8 1.460(11) . ? C8 C9 1.426(10) . ? C9 C10 1.374(10) . ? C10 C11 1.366(11) . ? C11 C12 1.397(12) . ? C13 C14 1.530(10) . ? C14 C19 1.369(10) . ? C14 C15 1.392(11) . ? C15 C16 1.377(12) . ? C16 C17 1.347(12) . ? C17 C18 1.390(12) . ? C18 C19 1.412(11) . ? C21 C25 1.474(11) . ? C21 C28 1.484(10) . ? C22 C23 1.406(11) . ? C23 C24 1.385(11) . ? C24 C25 1.357(11) . ? C25 C26 1.397(10) . ? C26 C27 1.475(11) . ? C27 C28 1.398(10) . ? C28 C29 1.376(11) . ? C29 C30 1.384(10) . ? C30 C31 1.374(12) . ? C32 C33 1.503(11) . ? C33 C34 1.384(13) . ? C33 C38 1.383(12) . ? C34 C35 1.370(12) . ? C35 C36 1.413(14) . ? C36 C37 1.345(14) . ? C37 C38 1.361(13) . ? 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 N6 Ni1 N2 99.2(3) . . ? N6 Ni1 S1 161.2(2) . . ? N2 Ni1 S1 86.7(2) . . ? N6 Ni1 S2 86.07(19) . . ? N2 Ni1 S2 158.4(2) . . ? S1 Ni1 S2 95.03(9) . . ? C1 S1 Ni1 94.7(3) . . ? C20 S2 Ni1 93.7(3) . . ? C1 S3 C13 102.6(4) . . ? C20 S4 C32 103.2(4) . . ? C1 N1 N2 112.2(6) . . ? C2 N2 N1 114.9(6) . . ? C2 N2 Ni1 126.4(5) . . ? N1 N2 Ni1 118.2(5) . . ? C7 N3 C3 113.6(8) . . ? C8 N4 C12 115.7(8) . . ? C20 N5 N6 108.3(7) . . ? C21 N6 N5 113.2(6) . . ? C21 N6 Ni1 127.1(5) . . ? N5 N6 Ni1 119.5(5) . . ? C26 N7 C22 116.5(7) . . ? C27 N8 C31 112.7(7) . . ? N1 C1 S3 120.4(6) . . ? N1 C1 S1 125.2(6) . . ? S3 C1 S1 114.4(4) . . ? N2 C2 C9 126.4(7) . . ? N2 C2 C6 129.0(7) . . ? C9 C2 C6 104.5(7) . . ? N3 C3 C4 125.0(8) . . ? C3 C4 C5 121.4(9) . . ? C4 C5 C6 114.5(8) . . ? C7 C6 C5 119.1(7) . . ? C7 C6 C2 109.4(7) . . ? C5 C6 C2 130.9(8) . . ? N3 C7 C6 126.3(8) . . ? N3 C7 C8 124.8(8) . . ? C6 C7 C8 109.0(7) . . ? N4 C8 C9 124.1(8) . . ? N4 C8 C7 127.8(8) . . ? C9 C8 C7 108.1(8) . . ? C10 C9 C8 117.9(8) . . ? C10 C9 C2 132.6(8) . . ? C8 C9 C2 108.8(7) . . ? C11 C10 C9 117.9(8) . . ? C10 C11 C12 119.6(8) . . ? N4 C12 C11 124.2(9) . . ? C14 C13 S3 118.0(6) . . ? C19 C14 C15 118.0(8) . . ? C19 C14 C13 124.0(7) . . ? C15 C14 C13 117.9(7) . . ? C16 C15 C14 121.6(8) . . ? C17 C16 C15 120.6(9) . . ? C16 C17 C18 119.6(9) . . ? C17 C18 C19 119.7(9) . . ? C14 C19 C18 120.4(8) . . ? N5 C20 S2 126.3(6) . . ? N5 C20 S4 116.7(7) . . ? S2 C20 S4 117.0(5) . . ? N6 C21 C25 128.3(7) . . ? N6 C21 C28 123.7(7) . . ? C25 C21 C28 107.7(6) . . ? N7 C22 C23 121.9(8) . . ? C24 C23 C22 119.6(8) . . ? C25 C24 C23 117.6(8) . . ? C24 C25 C26 119.4(8) . . ? C24 C25 C21 133.7(7) . . ? C26 C25 C21 106.7(7) . . ? N7 C26 C25 125.0(7) . . ? N7 C26 C27 125.5(7) . . ? C25 C26 C27 109.5(7) . . ? N8 C27 C28 125.7(8) . . ? N8 C27 C26 125.6(8) . . ? C28 C27 C26 108.7(7) . . ? C29 C28 C27 119.4(7) . . ? C29 C28 C21 133.7(7) . . ? C27 C28 C21 106.8(7) . . ? C28 C29 C30 116.6(8) . . ? C31 C30 C29 119.9(8) . . ? C30 C31 N8 125.4(8) . . ? C33 C32 S4 111.4(6) . . ? C34 C33 C38 119.3(9) . . ? C34 C33 C32 121.9(9) . . ? C38 C33 C32 118.8(10) . . ? C35 C34 C33 121.8(10) . . ? C34 C35 C36 116.8(11) . . ? C37 C36 C35 121.4(11) . . ? C36 C37 C38 121.0(11) . . ? C37 C38 C33 119.6(10) . . ? _refine_diff_density_max 0.750 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.104