# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Stanislav Groysman' _publ_contact_author_email groysman@chem.wayne.edu loop_ _publ_author_name 'Amarnath Bheemaraju' 'Jeffrey Beattie' 'Richard Lord' 'Philip Martin' 'Stanislav Groysman' data_sg3_0m _database_code_depnum_ccdc_archive 'CCDC 887355' #TrackingRef '- combined_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni2L(CS2)2 _chemical_melting_point 'not measured' _chemical_formula_moiety 'C22 H18 N4 Ni2 S4' _chemical_formula_sum 'C11 H9 N2 Ni S2' _chemical_formula_weight 292.03 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 P21/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 7.2464(7) _cell_length_b 10.7305(9) _cell_length_c 14.4456(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.265(5) _cell_angle_gamma 90.00 _cell_volume 1120.14(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 2.073 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6819 _exptl_absorpt_correction_T_max 0.9034 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13679 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1920 _reflns_number_gt 1652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0848P)^2^+9.8229P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1920 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1731 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.79763(11) 0.37157(8) 0.60095(6) 0.0275(3) Uani 1 1 d . . . S1 S 1.0010(3) 0.5496(2) 0.75839(16) 0.0508(6) Uani 1 1 d . . . S2 S 0.8359(3) 0.2827(2) 0.73440(13) 0.0440(6) Uani 1 1 d . . . N1 N 0.6903(7) 0.2719(5) 0.4979(4) 0.0237(12) Uani 1 1 d . . . N2 N 0.7720(7) 0.5043(5) 0.5122(4) 0.0297(13) Uani 1 1 d . . . C1 C 0.6418(9) 0.3359(6) 0.4264(5) 0.0261(14) Uani 1 1 d . . . H1 H 0.5813 0.2986 0.3728 0.031 Uiso 1 1 calc R . . C2 C 0.6823(9) 0.4684(6) 0.4298(5) 0.0266(14) Uani 1 1 d . . . C3 C 0.8173(10) 0.6236(7) 0.5230(7) 0.0401(19) Uani 1 1 d . . . H3 H 0.8804 0.6500 0.5796 0.048 Uiso 1 1 calc R . . C4 C 0.7748(11) 0.7101(8) 0.4540(7) 0.051(2) Uani 1 1 d . . . H4 H 0.8097 0.7947 0.4635 0.061 Uiso 1 1 calc R . . C5 C 0.6832(12) 0.6751(8) 0.3724(7) 0.052(2) Uani 1 1 d . . . H5 H 0.6546 0.7346 0.3247 0.063 Uiso 1 1 calc R . . C6 C 0.6319(11) 0.5500(7) 0.3597(6) 0.0413(19) Uani 1 1 d . . . H6 H 0.5645 0.5228 0.3044 0.050 Uiso 1 1 calc R . . C7 C 0.6538(10) 0.1365(6) 0.4960(5) 0.0309(16) Uani 1 1 d . . . H7A H 0.5769 0.1148 0.4387 0.037 Uiso 1 1 calc R . . H7B H 0.5845 0.1132 0.5499 0.037 Uiso 1 1 calc R . . C8 C 0.8327(9) 0.0651(6) 0.4990(5) 0.0274(15) Uani 1 1 d . . . C9 C 1.0981(10) -0.0045(7) 0.4221(5) 0.0336(16) Uani 1 1 d . . . H9 H 1.1650 -0.0063 0.3680 0.040 Uiso 1 1 calc R . . C10 C 0.9314(10) 0.0594(6) 0.4207(5) 0.0334(16) Uani 1 1 d . . . H10 H 0.8844 0.0997 0.3653 0.040 Uiso 1 1 calc R . . C11 C 0.9019(10) 0.4312(9) 0.7116(5) 0.045(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0238(5) 0.0336(5) 0.0246(5) -0.0065(3) -0.0011(4) 0.0046(3) S1 0.0449(12) 0.0580(14) 0.0500(13) -0.0247(10) 0.0070(10) -0.0084(10) S2 0.0474(12) 0.0480(12) 0.0346(10) -0.0026(8) -0.0115(9) 0.0018(9) N1 0.019(3) 0.028(3) 0.024(3) 0.000(2) 0.005(2) 0.004(2) N2 0.020(3) 0.029(3) 0.041(3) -0.003(2) 0.008(3) 0.002(2) C1 0.019(3) 0.034(4) 0.026(3) -0.001(3) 0.004(3) 0.003(3) C2 0.020(3) 0.027(3) 0.034(4) 0.002(3) 0.009(3) 0.003(3) C3 0.022(3) 0.029(4) 0.071(6) -0.004(4) 0.012(4) 0.002(3) C4 0.031(4) 0.032(4) 0.093(7) 0.000(4) 0.028(5) 0.000(3) C5 0.046(5) 0.044(5) 0.071(6) 0.027(5) 0.031(5) 0.022(4) C6 0.037(4) 0.047(5) 0.042(4) 0.015(4) 0.014(4) 0.013(3) C7 0.033(4) 0.019(3) 0.042(4) -0.005(3) 0.007(3) -0.004(3) C8 0.028(3) 0.020(3) 0.034(4) -0.004(3) 0.005(3) -0.003(3) C9 0.038(4) 0.036(4) 0.029(3) 0.003(3) 0.014(3) 0.008(3) C10 0.040(4) 0.032(4) 0.029(4) 0.006(3) 0.008(3) 0.009(3) C11 0.029(4) 0.082(6) 0.025(4) -0.004(4) 0.004(3) 0.024(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 C11 1.832(8) . ? Ni1 N2 1.916(6) . ? Ni1 N1 1.948(5) . ? Ni1 S2 2.150(2) . ? S1 C11 1.585(10) . ? S2 C11 1.703(10) . ? N1 C1 1.267(8) . ? N1 C7 1.477(8) . ? N2 C3 1.328(9) . ? N2 C2 1.368(9) . ? C1 C2 1.452(9) . ? C1 H1 0.9500 . ? C2 C6 1.367(10) . ? C3 C4 1.380(13) . ? C3 H3 0.9500 . ? C4 C5 1.363(14) . ? C4 H4 0.9500 . ? C5 C6 1.401(13) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.504(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.374(10) 3_756 ? C8 C10 1.384(10) . ? C9 C8 1.374(10) 3_756 ? C9 C10 1.388(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 C11 Ni1 N2 109.7(3) . . ? C11 Ni1 N1 167.0(3) . . ? N2 Ni1 N1 83.3(2) . . ? C11 Ni1 S2 49.9(3) . . ? N2 Ni1 S2 158.31(19) . . ? N1 Ni1 S2 117.36(17) . . ? C11 S2 Ni1 55.3(3) . . ? C1 N1 C7 118.7(6) . . ? C1 N1 Ni1 113.3(5) . . ? C7 N1 Ni1 127.9(4) . . ? C3 N2 C2 118.1(7) . . ? C3 N2 Ni1 128.8(6) . . ? C2 N2 Ni1 112.9(4) . . ? N1 C1 C2 117.4(6) . . ? N1 C1 H1 121.3 . . ? C2 C1 H1 121.3 . . ? C6 C2 N2 123.2(7) . . ? C6 C2 C1 124.1(7) . . ? N2 C2 C1 112.7(6) . . ? N2 C3 C4 121.5(8) . . ? N2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 120.6(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.0(8) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C2 C6 C5 117.6(8) . . ? C2 C6 H6 121.2 . . ? C5 C6 H6 121.2 . . ? N1 C7 C8 110.4(5) . . ? N1 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N1 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C10 118.6(6) 3_756 . ? C9 C8 C7 121.7(6) 3_756 . ? C10 C8 C7 119.7(6) . . ? C8 C9 C10 120.6(7) 3_756 . ? C8 C9 H9 119.7 3_756 . ? C10 C9 H9 119.7 . . ? C8 C10 C9 120.8(7) . . ? C8 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? S1 C11 S2 142.3(5) . . ? S1 C11 Ni1 142.8(6) . . ? S2 C11 Ni1 74.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 S2 C11 -22.1(6) . . . . ? N1 Ni1 S2 C11 177.0(3) . . . . ? C11 Ni1 N1 C1 178.4(11) . . . . ? N2 Ni1 N1 C1 -4.9(5) . . . . ? S2 Ni1 N1 C1 168.1(4) . . . . ? C11 Ni1 N1 C7 1.2(15) . . . . ? N2 Ni1 N1 C7 177.9(5) . . . . ? S2 Ni1 N1 C7 -9.1(6) . . . . ? C11 Ni1 N2 C3 -0.5(7) . . . . ? N1 Ni1 N2 C3 -179.7(6) . . . . ? S2 Ni1 N2 C3 17.3(9) . . . . ? C11 Ni1 N2 C2 -175.5(5) . . . . ? N1 Ni1 N2 C2 5.3(4) . . . . ? S2 Ni1 N2 C2 -157.6(4) . . . . ? C7 N1 C1 C2 -179.0(5) . . . . ? Ni1 N1 C1 C2 3.6(7) . . . . ? C3 N2 C2 C6 -2.3(10) . . . . ? Ni1 N2 C2 C6 173.2(6) . . . . ? C3 N2 C2 C1 179.6(6) . . . . ? Ni1 N2 C2 C1 -4.9(7) . . . . ? N1 C1 C2 C6 -177.3(7) . . . . ? N1 C1 C2 N2 0.8(8) . . . . ? C2 N2 C3 C4 0.5(10) . . . . ? Ni1 N2 C3 C4 -174.3(6) . . . . ? N2 C3 C4 C5 0.4(12) . . . . ? C3 C4 C5 C6 0.4(12) . . . . ? N2 C2 C6 C5 3.1(11) . . . . ? C1 C2 C6 C5 -179.1(6) . . . . ? C4 C5 C6 C2 -2.0(11) . . . . ? C1 N1 C7 C8 112.8(7) . . . . ? Ni1 N1 C7 C8 -70.1(7) . . . . ? N1 C7 C8 C9 105.6(7) . . . 3_756 ? N1 C7 C8 C10 -74.6(8) . . . . ? C9 C8 C10 C9 -1.0(12) 3_756 . . . ? C7 C8 C10 C9 179.1(6) . . . . ? C8 C9 C10 C8 1.0(12) 3_756 . . . ? Ni1 S2 C11 S1 -178.4(9) . . . . ? N2 Ni1 C11 S1 -10.2(8) . . . . ? N1 Ni1 C11 S1 166.3(8) . . . . ? S2 Ni1 C11 S1 178.3(9) . . . . ? N2 Ni1 C11 S2 171.5(2) . . . . ? N1 Ni1 C11 S2 -12.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 3.174 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.160 #=========================================END data_sg14full _database_code_depnum_ccdc_archive 'CCDC 887356' #TrackingRef '- combined_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NiL2(COD) _chemical_melting_point 'not measured' _chemical_formula_moiety 'C21 H24 N2 Ni' _chemical_formula_sum 'C21 H24 N2 Ni' _chemical_formula_weight 363.13 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' 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 25.286(3) _cell_length_b 7.3278(6) _cell_length_c 21.348(2) _cell_angle_alpha 90.00 _cell_angle_beta 120.423(8) _cell_angle_gamma 90.00 _cell_volume 3411.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisms _exptl_crystal_colour violet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6582 _exptl_absorpt_correction_T_max 0.7635 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45269 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 33.73 _reflns_number_total 6713 _reflns_number_gt 5946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0379P)^2^+2.9598P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6713 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.162824(5) 0.885646(16) 0.046016(6) 0.00941(4) Uani 1 1 d . . . N1 N 0.11292(4) 0.66983(11) 0.02544(5) 0.01208(14) Uani 1 1 d . . . N2 N 0.13761(4) 0.86235(11) -0.05588(4) 0.01069(13) Uani 1 1 d . . . C1 C 0.08733(5) 0.61206(13) -0.04196(6) 0.01380(17) Uani 1 1 d . . . H5 H 0.0623 0.5060 -0.0581 0.017 Uiso 1 1 calc R . . C2 C 0.09926(4) 0.71731(13) -0.08947(5) 0.01249(16) Uani 1 1 d . . . C3 C 0.15062(4) 0.97111(14) -0.09773(5) 0.01341(16) Uani 1 1 d . . . H4 H 0.1763 1.0740 -0.0757 0.016 Uiso 1 1 calc R . . C4 C 0.12859(5) 0.94045(15) -0.17025(6) 0.01655(18) Uani 1 1 d . . . H3 H 0.1398 1.0189 -0.1970 0.020 Uiso 1 1 calc R . . C5 C 0.08928(5) 0.79203(16) -0.20447(6) 0.01854(19) Uani 1 1 d . . . H1 H 0.0733 0.7686 -0.2547 0.022 Uiso 1 1 calc R . . C6 C 0.07454(5) 0.68167(15) -0.16368(6) 0.01713(18) Uani 1 1 d . . . H2 H 0.0476 0.5812 -0.1857 0.021 Uiso 1 1 calc R . . C7 C 0.10277(5) 0.55855(13) 0.07520(6) 0.01516(17) Uani 1 1 d . . . H12 H 0.1429 0.5174 0.1157 0.018 Uiso 1 1 calc R . . H6 H 0.0790 0.4487 0.0491 0.018 Uiso 1 1 calc R . . C8 C 0.06898(4) 0.65915(13) 0.10591(5) 0.01178(15) Uani 1 1 d . . . C9 C 0.08124(5) 0.62046(14) 0.17578(6) 0.01490(17) Uani 1 1 d . . . H11 H 0.1114 0.5318 0.2042 0.018 Uiso 1 1 calc R . . C10 C 0.04974(5) 0.71049(15) 0.20442(6) 0.01679(18) Uani 1 1 d . . . H10 H 0.0582 0.6825 0.2521 0.020 Uiso 1 1 calc R . . C11 C 0.00602(5) 0.84092(15) 0.16352(6) 0.01641(18) Uani 1 1 d . . . H9 H -0.0151 0.9037 0.1833 0.020 Uiso 1 1 calc R . . C12 C -0.00679(5) 0.87940(13) 0.09354(6) 0.01414(17) Uani 1 1 d . . . H8 H -0.0369 0.9683 0.0652 0.017 Uiso 1 1 calc R . . C13 C 0.02430(4) 0.78802(13) 0.06484(5) 0.01246(16) Uani 1 1 d . . . H7 H 0.0149 0.8138 0.0167 0.015 Uiso 1 1 calc R . . C14 C 0.16424(4) 1.16401(13) 0.05666(5) 0.01148(15) Uani 1 1 d . . . H24 H 0.1408 1.1704 0.0051 0.014 Uiso 1 1 calc R . . C15 C 0.22892(4) 1.23957(13) 0.09431(5) 0.01401(17) Uani 1 1 d . . . H23 H 0.2406 1.2783 0.1441 0.017 Uiso 1 1 calc R . . H22 H 0.2302 1.3484 0.0676 0.017 Uiso 1 1 calc R . . C16 C 0.27532(5) 1.09750(14) 0.09824(6) 0.01637(18) Uani 1 1 d . . . H21 H 0.2794 1.1097 0.0547 0.020 Uiso 1 1 calc R . . H13 H 0.3159 1.1229 0.1414 0.020 Uiso 1 1 calc R . . C17 C 0.25679(5) 0.90407(14) 0.10268(6) 0.01524(17) Uani 1 1 d . . . H20 H 0.2592 0.8159 0.0716 0.018 Uiso 1 1 calc R . . C18 C 0.23650(5) 0.84552(14) 0.14891(5) 0.01552(17) Uani 1 1 d . . . H14 H 0.2243 0.7217 0.1459 0.019 Uiso 1 1 calc R . . C19 C 0.23270(5) 0.96781(15) 0.20384(5) 0.01791(19) Uani 1 1 d . . . H15 H 0.2637 1.0660 0.2187 0.021 Uiso 1 1 calc R . . H19 H 0.2426 0.8953 0.2476 0.021 Uiso 1 1 calc R . . C20 C 0.16888(5) 1.05418(14) 0.17360(5) 0.01567(17) Uani 1 1 d . . . H17 H 0.1432 0.9730 0.1844 0.019 Uiso 1 1 calc R . . H18 H 0.1731 1.1720 0.1984 0.019 Uiso 1 1 calc R . . C21 C 0.13718(4) 1.08602(13) 0.09286(5) 0.01189(16) Uani 1 1 d . . . H16 H 0.0955 1.0500 0.0645 0.014 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 0.01064(6) 0.00838(6) 0.00973(6) -0.00048(4) 0.00553(4) 0.00014(4) N1 0.0140(3) 0.0093(3) 0.0160(4) 0.0005(3) 0.0098(3) 0.0011(3) N2 0.0102(3) 0.0110(3) 0.0116(3) -0.0008(3) 0.0061(3) 0.0003(2) C1 0.0139(4) 0.0109(4) 0.0179(4) -0.0029(3) 0.0090(4) -0.0017(3) C2 0.0118(4) 0.0120(4) 0.0137(4) -0.0029(3) 0.0065(3) 0.0003(3) C3 0.0135(4) 0.0142(4) 0.0141(4) 0.0013(3) 0.0082(3) 0.0013(3) C4 0.0184(4) 0.0198(4) 0.0138(4) 0.0028(3) 0.0099(4) 0.0048(4) C5 0.0192(5) 0.0228(5) 0.0118(4) -0.0022(4) 0.0065(4) 0.0044(4) C6 0.0161(4) 0.0177(4) 0.0148(4) -0.0050(3) 0.0057(4) 0.0005(3) C7 0.0198(4) 0.0099(4) 0.0216(5) 0.0026(3) 0.0148(4) 0.0018(3) C8 0.0118(4) 0.0101(3) 0.0149(4) 0.0006(3) 0.0079(3) -0.0009(3) C9 0.0147(4) 0.0150(4) 0.0153(4) 0.0033(3) 0.0079(3) 0.0002(3) C10 0.0194(5) 0.0189(4) 0.0140(4) 0.0009(3) 0.0099(4) -0.0016(4) C11 0.0165(4) 0.0184(4) 0.0183(4) -0.0017(4) 0.0116(4) -0.0008(3) C12 0.0118(4) 0.0149(4) 0.0162(4) 0.0004(3) 0.0075(3) 0.0008(3) C13 0.0119(4) 0.0127(4) 0.0129(4) 0.0009(3) 0.0064(3) -0.0002(3) C14 0.0126(4) 0.0091(3) 0.0129(4) -0.0003(3) 0.0066(3) 0.0003(3) C15 0.0141(4) 0.0134(4) 0.0150(4) -0.0019(3) 0.0078(3) -0.0029(3) C16 0.0116(4) 0.0198(4) 0.0177(4) -0.0017(3) 0.0074(4) -0.0019(3) C17 0.0115(4) 0.0166(4) 0.0157(4) -0.0003(3) 0.0055(3) 0.0025(3) C18 0.0156(4) 0.0146(4) 0.0127(4) 0.0026(3) 0.0044(3) 0.0027(3) C19 0.0216(5) 0.0186(4) 0.0105(4) 0.0014(3) 0.0059(4) 0.0012(4) C20 0.0204(5) 0.0161(4) 0.0140(4) -0.0031(3) 0.0112(4) -0.0031(3) C21 0.0128(4) 0.0103(4) 0.0139(4) -0.0017(3) 0.0077(3) 0.0001(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 1.9300(8) . ? Ni1 N2 1.9398(9) . ? Ni1 C14 2.0507(10) . ? Ni1 C17 2.0533(10) . ? Ni1 C21 2.0574(9) . ? Ni1 C18 2.0585(10) . ? N1 C1 1.3136(13) . ? N1 C7 1.4612(13) . ? N2 C3 1.3561(12) . ? N2 C2 1.3711(12) . ? C1 C2 1.4227(14) . ? C1 H5 0.9500 . ? C2 C6 1.4022(14) . ? C3 C4 1.3727(14) . ? C3 H4 0.9500 . ? C4 C5 1.4033(16) . ? C4 H3 0.9500 . ? C5 C6 1.3709(16) . ? C5 H1 0.9500 . ? C6 H2 0.9500 . ? C7 C8 1.5069(14) . ? C7 H12 0.9900 . ? C7 H6 0.9900 . ? C8 C9 1.3903(14) . ? C8 C13 1.3906(13) . ? C9 C10 1.3918(15) . ? C9 H11 0.9500 . ? C10 C11 1.3858(15) . ? C10 H10 0.9500 . ? C11 C12 1.3877(15) . ? C11 H9 0.9500 . ? C12 C13 1.3892(14) . ? C12 H8 0.9500 . ? C13 H7 0.9500 . ? C14 C21 1.3884(13) . ? C14 C15 1.5151(13) . ? C14 H24 0.9500 . ? C15 C16 1.5388(15) . ? C15 H23 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.5108(15) . ? C16 H21 0.9900 . ? C16 H13 0.9900 . ? C17 C18 1.3907(15) . ? C17 H20 0.9500 . ? C18 C19 1.5170(15) . ? C18 H14 0.9500 . ? C19 C20 1.5382(16) . ? C19 H15 0.9900 . ? C19 H19 0.9900 . ? C20 C21 1.5062(14) . ? C20 H17 0.9900 . ? C20 H18 0.9900 . ? C21 H16 0.9500 . ? 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 N2 82.36(4) . . ? N1 Ni1 C14 144.39(4) . . ? N2 Ni1 C14 100.90(4) . . ? N1 Ni1 C17 128.03(4) . . ? N2 Ni1 C17 106.95(4) . . ? C14 Ni1 C17 85.37(4) . . ? N1 Ni1 C21 111.39(4) . . ? N2 Ni1 C21 127.04(4) . . ? C14 Ni1 C21 39.51(4) . . ? C17 Ni1 C21 102.84(4) . . ? N1 Ni1 C18 105.06(4) . . ? N2 Ni1 C18 142.18(4) . . ? C14 Ni1 C18 93.91(4) . . ? C17 Ni1 C18 39.54(4) . . ? C21 Ni1 C18 85.47(4) . . ? C1 N1 C7 116.49(8) . . ? C1 N1 Ni1 114.58(7) . . ? C7 N1 Ni1 128.84(7) . . ? C3 N2 C2 117.02(8) . . ? C3 N2 Ni1 129.45(7) . . ? C2 N2 Ni1 113.48(6) . . ? N1 C1 C2 116.20(9) . . ? N1 C1 H5 121.9 . . ? C2 C1 H5 121.9 . . ? N2 C2 C6 121.86(9) . . ? N2 C2 C1 113.36(8) . . ? C6 C2 C1 124.77(9) . . ? N2 C3 C4 123.48(10) . . ? N2 C3 H4 118.3 . . ? C4 C3 H4 118.3 . . ? C3 C4 C5 119.33(10) . . ? C3 C4 H3 120.3 . . ? C5 C4 H3 120.3 . . ? C6 C5 C4 118.38(9) . . ? C6 C5 H1 120.8 . . ? C4 C5 H1 120.8 . . ? C5 C6 C2 119.91(10) . . ? C5 C6 H2 120.0 . . ? C2 C6 H2 120.0 . . ? N1 C7 C8 112.97(8) . . ? N1 C7 H12 109.0 . . ? C8 C7 H12 109.0 . . ? N1 C7 H6 109.0 . . ? C8 C7 H6 109.0 . . ? H12 C7 H6 107.8 . . ? C9 C8 C13 118.92(9) . . ? C9 C8 C7 119.96(9) . . ? C13 C8 C7 121.10(9) . . ? C8 C9 C10 120.55(9) . . ? C8 C9 H11 119.7 . . ? C10 C9 H11 119.7 . . ? C11 C10 C9 120.10(10) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.70(9) . . ? C10 C11 H9 120.2 . . ? C12 C11 H9 120.2 . . ? C11 C12 C13 120.07(9) . . ? C11 C12 H8 120.0 . . ? C13 C12 H8 120.0 . . ? C12 C13 C8 120.65(9) . . ? C12 C13 H7 119.7 . . ? C8 C13 H7 119.7 . . ? C21 C14 C15 123.98(9) . . ? C21 C14 Ni1 70.51(5) . . ? C15 C14 Ni1 112.08(6) . . ? C21 C14 H24 118.0 . . ? C15 C14 H24 118.0 . . ? Ni1 C14 H24 87.4 . . ? C14 C15 C16 111.72(8) . . ? C14 C15 H23 109.3 . . ? C16 C15 H23 109.3 . . ? C14 C15 H22 109.3 . . ? C16 C15 H22 109.3 . . ? H23 C15 H22 107.9 . . ? C17 C16 C15 112.71(8) . . ? C17 C16 H21 109.0 . . ? C15 C16 H21 109.0 . . ? C17 C16 H13 109.0 . . ? C15 C16 H13 109.0 . . ? H21 C16 H13 107.8 . . ? C18 C17 C16 124.86(9) . . ? C18 C17 Ni1 70.43(6) . . ? C16 C17 Ni1 109.14(7) . . ? C18 C17 H20 117.6 . . ? C16 C17 H20 117.6 . . ? Ni1 C17 H20 90.4 . . ? C17 C18 C19 123.84(10) . . ? C17 C18 Ni1 70.03(6) . . ? C19 C18 Ni1 111.29(7) . . ? C17 C18 H14 118.1 . . ? C19 C18 H14 118.1 . . ? Ni1 C18 H14 88.7 . . ? C18 C19 C20 112.47(8) . . ? C18 C19 H15 109.1 . . ? C20 C19 H15 109.1 . . ? C18 C19 H19 109.1 . . ? C20 C19 H19 109.1 . . ? H15 C19 H19 107.8 . . ? C21 C20 C19 112.41(8) . . ? C21 C20 H17 109.1 . . ? C19 C20 H17 109.1 . . ? C21 C20 H18 109.1 . . ? C19 C20 H18 109.1 . . ? H17 C20 H18 107.9 . . ? C14 C21 C20 125.04(9) . . ? C14 C21 Ni1 69.99(5) . . ? C20 C21 Ni1 109.24(7) . . ? C14 C21 H16 117.5 . . ? C20 C21 H16 117.5 . . ? Ni1 C21 H16 90.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C1 0.08(7) . . . . ? C14 Ni1 N1 C1 98.14(9) . . . . ? C17 Ni1 N1 C1 -105.50(8) . . . . ? C21 Ni1 N1 C1 126.96(7) . . . . ? C18 Ni1 N1 C1 -142.04(7) . . . . ? N2 Ni1 N1 C7 176.44(8) . . . . ? C14 Ni1 N1 C7 -85.49(10) . . . . ? C17 Ni1 N1 C7 70.87(9) . . . . ? C21 Ni1 N1 C7 -56.68(9) . . . . ? C18 Ni1 N1 C7 34.32(9) . . . . ? N1 Ni1 N2 C3 178.10(9) . . . . ? C14 Ni1 N2 C3 34.05(9) . . . . ? C17 Ni1 N2 C3 -54.39(9) . . . . ? C21 Ni1 N2 C3 67.01(10) . . . . ? C18 Ni1 N2 C3 -77.14(10) . . . . ? N1 Ni1 N2 C2 0.80(7) . . . . ? C14 Ni1 N2 C2 -143.25(7) . . . . ? C17 Ni1 N2 C2 128.31(7) . . . . ? C21 Ni1 N2 C2 -110.29(7) . . . . ? C18 Ni1 N2 C2 105.56(8) . . . . ? C7 N1 C1 C2 -177.76(8) . . . . ? Ni1 N1 C1 C2 -0.92(11) . . . . ? C3 N2 C2 C6 0.20(14) . . . . ? Ni1 N2 C2 C6 177.86(8) . . . . ? C3 N2 C2 C1 -179.13(8) . . . . ? Ni1 N2 C2 C1 -1.47(10) . . . . ? N1 C1 C2 N2 1.59(13) . . . . ? N1 C1 C2 C6 -177.72(9) . . . . ? C2 N2 C3 C4 -1.46(14) . . . . ? Ni1 N2 C3 C4 -178.68(8) . . . . ? N2 C3 C4 C5 1.58(16) . . . . ? C3 C4 C5 C6 -0.40(15) . . . . ? C4 C5 C6 C2 -0.78(15) . . . . ? N2 C2 C6 C5 0.90(15) . . . . ? C1 C2 C6 C5 -179.84(10) . . . . ? C1 N1 C7 C8 -118.00(10) . . . . ? Ni1 N1 C7 C8 65.69(11) . . . . ? N1 C7 C8 C9 -147.52(9) . . . . ? N1 C7 C8 C13 34.05(13) . . . . ? C13 C8 C9 C10 -0.61(15) . . . . ? C7 C8 C9 C10 -179.08(9) . . . . ? C8 C9 C10 C11 -0.47(16) . . . . ? C9 C10 C11 C12 0.92(16) . . . . ? C10 C11 C12 C13 -0.28(15) . . . . ? C11 C12 C13 C8 -0.81(15) . . . . ? C9 C8 C13 C12 1.25(14) . . . . ? C7 C8 C13 C12 179.70(9) . . . . ? N1 Ni1 C14 C21 44.86(9) . . . . ? N2 Ni1 C14 C21 136.94(6) . . . . ? C17 Ni1 C14 C21 -116.66(6) . . . . ? C18 Ni1 C14 C21 -78.02(6) . . . . ? N1 Ni1 C14 C15 164.61(6) . . . . ? N2 Ni1 C14 C15 -103.31(7) . . . . ? C17 Ni1 C14 C15 3.09(7) . . . . ? C21 Ni1 C14 C15 119.75(9) . . . . ? C18 Ni1 C14 C15 41.73(7) . . . . ? C21 C14 C15 C16 94.58(11) . . . . ? Ni1 C14 C15 C16 13.83(10) . . . . ? C14 C15 C16 C17 -30.54(12) . . . . ? C15 C16 C17 C18 -46.79(14) . . . . ? C15 C16 C17 Ni1 32.24(11) . . . . ? N1 Ni1 C17 C18 -64.58(7) . . . . ? N2 Ni1 C17 C18 -158.12(6) . . . . ? C14 Ni1 C17 C18 101.88(6) . . . . ? C21 Ni1 C17 C18 66.21(7) . . . . ? N1 Ni1 C17 C16 174.18(6) . . . . ? N2 Ni1 C17 C16 80.63(8) . . . . ? C14 Ni1 C17 C16 -19.37(7) . . . . ? C21 Ni1 C17 C16 -55.04(8) . . . . ? C18 Ni1 C17 C16 -121.24(10) . . . . ? C16 C17 C18 C19 -2.63(16) . . . . ? Ni1 C17 C18 C19 -102.80(10) . . . . ? C16 C17 C18 Ni1 100.16(10) . . . . ? N1 Ni1 C18 C17 132.55(6) . . . . ? N2 Ni1 C18 C17 35.54(9) . . . . ? C14 Ni1 C18 C17 -77.87(6) . . . . ? C21 Ni1 C18 C17 -116.50(6) . . . . ? N1 Ni1 C18 C19 -107.83(7) . . . . ? N2 Ni1 C18 C19 155.16(7) . . . . ? C14 Ni1 C18 C19 41.75(8) . . . . ? C17 Ni1 C18 C19 119.62(10) . . . . ? C21 Ni1 C18 C19 3.12(8) . . . . ? C17 C18 C19 C20 93.58(12) . . . . ? Ni1 C18 C19 C20 13.96(11) . . . . ? C18 C19 C20 C21 -30.84(12) . . . . ? C15 C14 C21 C20 -4.06(15) . . . . ? Ni1 C14 C21 C20 99.96(9) . . . . ? C15 C14 C21 Ni1 -104.02(9) . . . . ? C19 C20 C21 C14 -46.20(13) . . . . ? C19 C20 C21 Ni1 32.38(10) . . . . ? N1 Ni1 C21 C14 -153.83(6) . . . . ? N2 Ni1 C21 C14 -57.13(7) . . . . ? C17 Ni1 C21 C14 66.01(6) . . . . ? C18 Ni1 C21 C14 101.76(6) . . . . ? N1 Ni1 C21 C20 84.84(7) . . . . ? N2 Ni1 C21 C20 -178.46(6) . . . . ? C14 Ni1 C21 C20 -121.33(9) . . . . ? C17 Ni1 C21 C20 -55.33(7) . . . . ? C18 Ni1 C21 C20 -19.57(7) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 33.73 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.579 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.066 #===========================================END data_sg21_0m _database_code_depnum_ccdc_archive 'CCDC 887357' #TrackingRef '- combined_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NiL2(CS2) _chemical_melting_point 'not measured' _chemical_formula_moiety 'C28 H24 N4 Ni2 S4' _chemical_formula_sum 'C28 H24 N4 Ni2 S4' _chemical_formula_weight 662.17 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7358(7) _cell_length_b 9.5434(7) _cell_length_c 17.0075(14) _cell_angle_alpha 98.210(5) _cell_angle_beta 98.742(5) _cell_angle_gamma 96.563(5) _cell_volume 1373.60(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisms _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.701 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6293 _exptl_absorpt_correction_T_max 0.7272 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20969 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.24 _reflns_number_total 5945 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1140P)^2^+10.7716P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5945 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2172 _refine_ls_wR_factor_gt 0.2004 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.29221(10) 0.38902(9) 0.52931(5) 0.0225(2) Uani 1 1 d . . . Ni2 Ni 0.46968(8) 1.10954(8) 0.10967(4) 0.0172(2) Uani 1 1 d . . . S1 S 0.2461(2) 0.16484(18) 0.52752(10) 0.0295(4) Uani 1 1 d . . . S2 S 0.4840(2) 0.2899(2) 0.68651(10) 0.0322(4) Uani 1 1 d . . . S3 S 0.46337(17) 1.33397(16) 0.13708(9) 0.0216(3) Uani 1 1 d . . . S4 S 0.16145(17) 1.20710(17) 0.01099(9) 0.0236(3) Uani 1 1 d . . . N2 N 0.3724(6) 0.5865(6) 0.5660(3) 0.0223(11) Uani 1 1 d . . . C5 C 0.3741(8) 0.2800(7) 0.6048(4) 0.0305(16) Uani 1 1 d . . . N3 N 0.6553(6) 1.0372(6) 0.1600(3) 0.0204(10) Uani 1 1 d . . . N4 N 0.3990(6) 0.9122(5) 0.0687(3) 0.0180(10) Uani 1 1 d . . . C4 C 0.3198(7) 0.6721(7) 0.5132(4) 0.0228(12) Uani 1 1 d . . . C3 C 0.2189(8) 0.5942(7) 0.4405(4) 0.0248(13) Uani 1 1 d . . . H3 H 0.1788 0.6416 0.3980 0.030 Uiso 1 1 calc R . . N1 N 0.1867(6) 0.4598(6) 0.4365(3) 0.0255(11) Uani 1 1 d . . . C11 C 0.0825(8) 0.3690(7) 0.3676(4) 0.0303(15) Uani 1 1 d . . . H11A H -0.0126 0.3298 0.3866 0.036 Uiso 1 1 calc R . . H11B H 0.1357 0.2872 0.3492 0.036 Uiso 1 1 calc R . . C12 C 0.0326(7) 0.4406(7) 0.2960(4) 0.0233(13) Uani 1 1 d . . . C13 C 0.1227(8) 0.4395(8) 0.2358(4) 0.0297(15) Uani 1 1 d . . . H13 H 0.2129 0.3923 0.2387 0.036 Uiso 1 1 calc R . . C14 C 0.0794(9) 0.5085(9) 0.1711(4) 0.0363(17) Uani 1 1 d . . . H14 H 0.1405 0.5086 0.1294 0.044 Uiso 1 1 calc R . . C15 C -0.0528(10) 0.5776(8) 0.1668(4) 0.0396(18) Uani 1 1 d . . . H15 H -0.0809 0.6261 0.1228 0.048 Uiso 1 1 calc R . . C16 C -0.1432(9) 0.5754(8) 0.2269(5) 0.0352(16) Uani 1 1 d . . . H16 H -0.2356 0.6195 0.2233 0.042 Uiso 1 1 calc R . . C17 C -0.0987(7) 0.5090(7) 0.2917(4) 0.0276(14) Uani 1 1 d . . . H17 H -0.1589 0.5103 0.3338 0.033 Uiso 1 1 calc R . . C7 C 0.3585(8) 0.8191(7) 0.5291(4) 0.0255(13) Uani 1 1 d . . . H7 H 0.3202 0.8766 0.4914 0.031 Uiso 1 1 calc R . . C8 C 0.4543(8) 0.8812(8) 0.6014(4) 0.0287(14) Uani 1 1 d . . . H8 H 0.4833 0.9819 0.6138 0.034 Uiso 1 1 calc R . . C9 C 0.5070(8) 0.7934(8) 0.6553(4) 0.0284(14) Uani 1 1 d . . . H9 H 0.5707 0.8334 0.7057 0.034 Uiso 1 1 calc R . . C10 C 0.4657(7) 0.6480(7) 0.6346(4) 0.0257(13) Uani 1 1 d . . . H10 H 0.5054 0.5885 0.6709 0.031 Uiso 1 1 calc R . . C6 C 0.3243(7) 1.2180(7) 0.0726(4) 0.0211(12) Uani 1 1 d . . . C1 C 0.6446(7) 0.9022(6) 0.1455(3) 0.0195(12) Uani 1 1 d . . . H1 H 0.7267 0.8534 0.1662 0.023 Uiso 1 1 calc R . . C2 C 0.4998(6) 0.8244(6) 0.0953(3) 0.0181(11) Uani 1 1 d . . . C21 C 0.2640(7) 0.8527(7) 0.0217(4) 0.0204(12) Uani 1 1 d . . . H21 H 0.1928 0.9129 0.0020 0.024 Uiso 1 1 calc R . . C20 C 0.2244(7) 0.7055(7) 0.0007(4) 0.0236(13) Uani 1 1 d . . . H20 H 0.1271 0.6662 -0.0325 0.028 Uiso 1 1 calc R . . C19 C 0.3275(7) 0.6165(7) 0.0283(4) 0.0230(13) Uani 1 1 d . . . H19 H 0.3026 0.5156 0.0141 0.028 Uiso 1 1 calc R . . C18 C 0.4683(7) 0.6775(7) 0.0774(4) 0.0220(12) Uani 1 1 d . . . H18 H 0.5410 0.6193 0.0980 0.026 Uiso 1 1 calc R . . C22 C 0.7965(7) 1.1256(7) 0.2085(4) 0.0246(13) Uani 1 1 d . . . H22A H 0.7651 1.1834 0.2549 0.030 Uiso 1 1 calc R . . H22B H 0.8384 1.1929 0.1752 0.030 Uiso 1 1 calc R . . C23 C 0.9247(7) 1.0485(7) 0.2398(4) 0.0214(12) Uani 1 1 d . . . C28 C 1.0487(8) 1.0250(8) 0.1984(4) 0.0284(14) Uani 1 1 d . . . H28 H 1.0540 1.0619 0.1497 0.034 Uiso 1 1 calc R . . C27 C 1.1639(7) 0.9480(9) 0.2281(4) 0.0330(16) Uani 1 1 d . . . H27 H 1.2458 0.9300 0.1988 0.040 Uiso 1 1 calc R . . C26 C 1.1602(8) 0.8973(8) 0.3001(4) 0.0311(15) Uani 1 1 d . . . H26 H 1.2406 0.8468 0.3209 0.037 Uiso 1 1 calc R . . C25 C 1.0385(7) 0.9206(8) 0.3415(4) 0.0292(14) Uani 1 1 d . . . H25 H 1.0358 0.8860 0.3911 0.035 Uiso 1 1 calc R . . C24 C 0.9214(7) 0.9934(7) 0.3116(4) 0.0230(13) Uani 1 1 d . . . H24 H 0.8373 1.0065 0.3401 0.028 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 0.0296(4) 0.0180(4) 0.0216(4) 0.0073(3) 0.0039(3) 0.0059(3) Ni2 0.0185(4) 0.0144(4) 0.0188(4) 0.0050(3) -0.0002(3) 0.0040(3) S1 0.0373(9) 0.0229(9) 0.0281(8) 0.0078(6) 0.0007(7) 0.0048(7) S2 0.0363(9) 0.0325(10) 0.0278(8) 0.0075(7) -0.0019(7) 0.0106(7) S3 0.0231(7) 0.0173(7) 0.0235(7) 0.0044(6) -0.0016(6) 0.0048(5) S4 0.0191(7) 0.0252(8) 0.0260(8) 0.0068(6) -0.0013(6) 0.0049(6) N2 0.025(3) 0.023(3) 0.020(2) 0.006(2) 0.004(2) 0.005(2) C5 0.043(4) 0.013(3) 0.048(4) 0.007(3) 0.039(3) 0.013(3) N3 0.022(2) 0.021(3) 0.018(2) 0.0070(19) 0.0006(19) 0.001(2) N4 0.020(2) 0.018(3) 0.018(2) 0.0055(19) 0.0041(19) 0.0044(19) C4 0.028(3) 0.021(3) 0.021(3) 0.007(2) 0.004(2) 0.006(2) C3 0.032(3) 0.022(3) 0.020(3) 0.007(2) 0.001(2) 0.004(3) N1 0.031(3) 0.018(3) 0.027(3) 0.005(2) 0.002(2) 0.004(2) C11 0.036(4) 0.022(3) 0.028(3) 0.003(3) -0.007(3) -0.001(3) C12 0.025(3) 0.019(3) 0.022(3) -0.001(2) 0.000(2) -0.002(2) C13 0.023(3) 0.035(4) 0.028(3) -0.005(3) 0.006(3) 0.001(3) C14 0.037(4) 0.045(5) 0.024(3) 0.001(3) 0.007(3) -0.003(3) C15 0.057(5) 0.029(4) 0.024(3) 0.002(3) -0.011(3) -0.006(3) C16 0.031(4) 0.033(4) 0.038(4) 0.004(3) -0.005(3) 0.008(3) C17 0.023(3) 0.028(4) 0.029(3) -0.007(3) 0.008(3) 0.001(3) C7 0.033(3) 0.018(3) 0.025(3) 0.004(2) 0.006(3) 0.003(2) C8 0.029(3) 0.027(4) 0.027(3) 0.000(3) 0.003(3) -0.002(3) C9 0.027(3) 0.038(4) 0.017(3) 0.000(3) 0.000(2) 0.001(3) C10 0.025(3) 0.031(4) 0.022(3) 0.004(3) 0.003(2) 0.008(3) C6 0.027(3) 0.020(3) 0.025(3) 0.010(2) 0.017(2) 0.010(2) C1 0.021(3) 0.016(3) 0.021(3) 0.005(2) -0.001(2) 0.003(2) C2 0.018(3) 0.022(3) 0.016(3) 0.005(2) 0.002(2) 0.005(2) C21 0.019(3) 0.021(3) 0.021(3) 0.005(2) 0.000(2) 0.003(2) C20 0.018(3) 0.026(3) 0.024(3) 0.002(2) -0.002(2) 0.002(2) C19 0.019(3) 0.021(3) 0.027(3) -0.002(2) 0.006(2) -0.001(2) C18 0.023(3) 0.019(3) 0.025(3) 0.006(2) 0.000(2) 0.006(2) C22 0.027(3) 0.017(3) 0.027(3) 0.006(2) -0.006(3) -0.001(2) C23 0.020(3) 0.021(3) 0.018(3) 0.001(2) -0.004(2) -0.006(2) C28 0.030(3) 0.034(4) 0.019(3) 0.004(3) 0.003(3) -0.003(3) C27 0.016(3) 0.051(5) 0.030(3) 0.000(3) 0.004(3) 0.004(3) C26 0.022(3) 0.033(4) 0.036(4) 0.007(3) -0.004(3) 0.008(3) C25 0.022(3) 0.033(4) 0.030(3) 0.008(3) -0.004(3) 0.003(3) C24 0.020(3) 0.027(3) 0.022(3) 0.009(2) 0.000(2) 0.003(2) _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 C5 1.875(7) . ? Ni1 N2 1.913(5) . ? Ni1 N1 1.950(5) . ? Ni1 S1 2.1262(19) . ? Ni2 C6 1.824(6) . ? Ni2 N4 1.908(5) . ? Ni2 N3 1.960(5) . ? Ni2 S3 2.1347(17) . ? S1 C5 1.745(8) . ? S2 C5 1.548(8) . ? S3 C6 1.686(7) . ? S4 C6 1.617(7) . ? N2 C10 1.332(8) . ? N2 C4 1.363(8) . ? N3 C1 1.266(8) . ? N3 C22 1.472(8) . ? N4 C21 1.335(8) . ? N4 C2 1.356(7) . ? C4 C7 1.382(9) . ? C4 C3 1.454(9) . ? C3 N1 1.271(8) . ? C3 H3 0.9500 . ? N1 C11 1.469(8) . ? C11 C12 1.511(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.381(9) . ? C12 C13 1.384(9) . ? C13 C14 1.387(11) . ? C13 H13 0.9500 . ? C14 C15 1.391(12) . ? C14 H14 0.9500 . ? C15 C16 1.384(11) . ? C15 H15 0.9500 . ? C16 C17 1.376(10) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C7 C8 1.388(9) . ? C7 H7 0.9500 . ? C8 C9 1.391(10) . ? C8 H8 0.9500 . ? C9 C10 1.374(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C1 C2 1.468(8) . ? C1 H1 0.9500 . ? C2 C18 1.378(9) . ? C21 C20 1.388(9) . ? C21 H21 0.9500 . ? C20 C19 1.384(9) . ? C20 H20 0.9500 . ? C19 C18 1.390(8) . ? C19 H19 0.9500 . ? C18 H18 0.9500 . ? C22 C23 1.483(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.400(8) . ? C23 C28 1.400(9) . ? C28 C27 1.389(10) . ? C28 H28 0.9500 . ? C27 C26 1.382(10) . ? C27 H27 0.9500 . ? C26 C25 1.383(10) . ? C26 H26 0.9500 . ? C25 C24 1.376(9) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? 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 C5 Ni1 N2 109.3(3) . . ? C5 Ni1 N1 166.9(3) . . ? N2 Ni1 N1 83.8(2) . . ? C5 Ni1 S1 51.2(2) . . ? N2 Ni1 S1 160.46(16) . . ? N1 Ni1 S1 115.74(17) . . ? C6 Ni2 N4 109.9(3) . . ? C6 Ni2 N3 166.4(3) . . ? N4 Ni2 N3 83.6(2) . . ? C6 Ni2 S3 49.7(2) . . ? N4 Ni2 S3 159.21(16) . . ? N3 Ni2 S3 116.93(16) . . ? C5 S1 Ni1 56.9(2) . . ? C6 S3 Ni2 55.5(2) . . ? C10 N2 C4 118.1(6) . . ? C10 N2 Ni1 129.3(5) . . ? C4 N2 Ni1 112.5(4) . . ? S2 C5 S1 144.8(4) . . ? S2 C5 Ni1 143.3(4) . . ? S1 C5 Ni1 71.8(3) . . ? C1 N3 C22 121.6(5) . . ? C1 N3 Ni2 112.9(4) . . ? C22 N3 Ni2 125.6(4) . . ? C21 N4 C2 118.0(5) . . ? C21 N4 Ni2 128.6(4) . . ? C2 N4 Ni2 113.3(4) . . ? N2 C4 C7 122.2(6) . . ? N2 C4 C3 113.6(6) . . ? C7 C4 C3 124.2(6) . . ? N1 C3 C4 117.0(6) . . ? N1 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C3 N1 C11 122.6(6) . . ? C3 N1 Ni1 113.1(4) . . ? C11 N1 Ni1 124.4(4) . . ? N1 C11 C12 116.1(6) . . ? N1 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C17 C12 C13 120.4(6) . . ? C17 C12 C11 120.6(6) . . ? C13 C12 C11 118.9(6) . . ? C14 C13 C12 119.0(7) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 120.5(7) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.8(7) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C12 120.5(6) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C8 C7 C4 118.7(6) . . ? C8 C7 H7 120.6 . . ? C4 C7 H7 120.6 . . ? C7 C8 C9 118.9(6) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 119.0(6) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C10 C9 123.0(6) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? S4 C6 S3 143.3(4) . . ? S4 C6 Ni2 141.8(4) . . ? S3 C6 Ni2 74.8(3) . . ? N3 C1 C2 117.1(5) . . ? N3 C1 H1 121.4 . . ? C2 C1 H1 121.4 . . ? N4 C2 C18 123.2(5) . . ? N4 C2 C1 113.0(5) . . ? C18 C2 C1 123.8(5) . . ? N4 C21 C20 122.1(6) . . ? N4 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C19 C20 C21 119.6(6) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C20 C19 C18 118.7(6) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C2 C18 C19 118.4(6) . . ? C2 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? N3 C22 C23 116.6(5) . . ? N3 C22 H22A 108.1 . . ? C23 C22 H22A 108.1 . . ? N3 C22 H22B 108.1 . . ? C23 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C24 C23 C28 118.2(6) . . ? C24 C23 C22 119.8(6) . . ? C28 C23 C22 121.9(6) . . ? C27 C28 C23 120.4(6) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? C26 C27 C28 120.4(6) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C26 C25 119.6(6) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C24 C25 C26 120.5(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C24 C23 120.9(6) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 S1 C5 -5.7(5) . . . . ? N1 Ni1 S1 C5 178.2(3) . . . . ? N4 Ni2 S3 C6 -12.6(5) . . . . ? N3 Ni2 S3 C6 177.2(3) . . . . ? C5 Ni1 N2 C10 -3.0(6) . . . . ? N1 Ni1 N2 C10 178.2(6) . . . . ? S1 Ni1 N2 C10 1.7(9) . . . . ? C5 Ni1 N2 C4 178.9(4) . . . . ? N1 Ni1 N2 C4 0.1(4) . . . . ? S1 Ni1 N2 C4 -176.4(4) . . . . ? Ni1 S1 C5 S2 178.3(8) . . . . ? N2 Ni1 C5 S2 -0.3(7) . . . . ? N1 Ni1 C5 S2 174.3(8) . . . . ? S1 Ni1 C5 S2 -178.3(7) . . . . ? N2 Ni1 C5 S1 178.00(19) . . . . ? N1 Ni1 C5 S1 -7.3(12) . . . . ? C6 Ni2 N3 C1 -176.0(9) . . . . ? N4 Ni2 N3 C1 -1.4(4) . . . . ? S3 Ni2 N3 C1 175.0(4) . . . . ? C6 Ni2 N3 C22 2.7(12) . . . . ? N4 Ni2 N3 C22 177.2(5) . . . . ? S3 Ni2 N3 C22 -6.3(5) . . . . ? C6 Ni2 N4 C21 -1.8(6) . . . . ? N3 Ni2 N4 C21 179.6(5) . . . . ? S3 Ni2 N4 C21 8.4(8) . . . . ? C6 Ni2 N4 C2 -178.5(4) . . . . ? N3 Ni2 N4 C2 2.8(4) . . . . ? S3 Ni2 N4 C2 -168.3(3) . . . . ? C10 N2 C4 C7 -0.8(9) . . . . ? Ni1 N2 C4 C7 177.5(5) . . . . ? C10 N2 C4 C3 -179.9(5) . . . . ? Ni1 N2 C4 C3 -1.6(7) . . . . ? N2 C4 C3 N1 3.0(9) . . . . ? C7 C4 C3 N1 -176.1(6) . . . . ? C4 C3 N1 C11 178.1(6) . . . . ? C4 C3 N1 Ni1 -2.9(8) . . . . ? C5 Ni1 N1 C3 -173.4(9) . . . . ? N2 Ni1 N1 C3 1.5(5) . . . . ? S1 Ni1 N1 C3 -179.7(4) . . . . ? C5 Ni1 N1 C11 5.6(14) . . . . ? N2 Ni1 N1 C11 -179.5(6) . . . . ? S1 Ni1 N1 C11 -0.8(6) . . . . ? C3 N1 C11 C12 8.2(10) . . . . ? Ni1 N1 C11 C12 -170.7(5) . . . . ? N1 C11 C12 C17 -88.2(8) . . . . ? N1 C11 C12 C13 90.2(8) . . . . ? C17 C12 C13 C14 0.1(10) . . . . ? C11 C12 C13 C14 -178.3(6) . . . . ? C12 C13 C14 C15 -0.1(11) . . . . ? C13 C14 C15 C16 -1.1(11) . . . . ? C14 C15 C16 C17 2.2(11) . . . . ? C15 C16 C17 C12 -2.1(11) . . . . ? C13 C12 C17 C16 1.0(10) . . . . ? C11 C12 C17 C16 179.3(6) . . . . ? N2 C4 C7 C8 0.0(10) . . . . ? C3 C4 C7 C8 179.1(6) . . . . ? C4 C7 C8 C9 -0.4(10) . . . . ? C7 C8 C9 C10 1.5(10) . . . . ? C4 N2 C10 C9 1.9(9) . . . . ? Ni1 N2 C10 C9 -176.0(5) . . . . ? C8 C9 C10 N2 -2.3(10) . . . . ? Ni2 S3 C6 S4 -177.7(7) . . . . ? N4 Ni2 C6 S4 -7.0(6) . . . . ? N3 Ni2 C6 S4 167.2(7) . . . . ? S3 Ni2 C6 S4 177.7(7) . . . . ? N4 Ni2 C6 S3 175.26(18) . . . . ? N3 Ni2 C6 S3 -10.5(11) . . . . ? C22 N3 C1 C2 -178.9(5) . . . . ? Ni2 N3 C1 C2 -0.2(7) . . . . ? C21 N4 C2 C18 -1.2(9) . . . . ? Ni2 N4 C2 C18 175.9(5) . . . . ? C21 N4 C2 C1 179.3(5) . . . . ? Ni2 N4 C2 C1 -3.6(6) . . . . ? N3 C1 C2 N4 2.5(8) . . . . ? N3 C1 C2 C18 -177.0(6) . . . . ? C2 N4 C21 C20 0.8(9) . . . . ? Ni2 N4 C21 C20 -175.8(4) . . . . ? N4 C21 C20 C19 -0.5(9) . . . . ? C21 C20 C19 C18 0.6(9) . . . . ? N4 C2 C18 C19 1.3(9) . . . . ? C1 C2 C18 C19 -179.3(6) . . . . ? C20 C19 C18 C2 -0.9(9) . . . . ? C1 N3 C22 C23 -0.4(9) . . . . ? Ni2 N3 C22 C23 -179.0(4) . . . . ? N3 C22 C23 C24 -84.1(7) . . . . ? N3 C22 C23 C28 94.1(7) . . . . ? C24 C23 C28 C27 0.5(9) . . . . ? C22 C23 C28 C27 -177.7(6) . . . . ? C23 C28 C27 C26 -1.9(11) . . . . ? C28 C27 C26 C25 1.6(11) . . . . ? C27 C26 C25 C24 0.1(11) . . . . ? C26 C25 C24 C23 -1.6(10) . . . . ? C28 C23 C24 C25 1.3(9) . . . . ? C22 C23 C24 C25 179.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.24 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.680 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.196