# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email basu@susqu.edu _publ_contact_author_name 'Swarna Basu' _publ_author_name 'Balwant Chohan' # Attachment '- Dalton-Complex 3.CIF' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 828723' #TrackingRef '- Dalton-Complex 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H20 N2 Ni O2 S2' _chemical_formula_weight 311.10 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 24.571(5) _cell_length_b 24.571(5) _cell_length_c 10.920(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 5710(3) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 1.846 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5451 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2893 _reflns_number_gt 2269 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0487P)^2^+19.0367P] 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 2893 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.808 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 0.532658(13) 0.099214(13) 0.63912(2) 0.02399(10) Uani 1 1 d . . . S14 S 0.52418(3) 0.17031(3) 0.54234(6) 0.03378(16) Uani 1 1 d . . . S1 S 0.43191(3) 0.05385(3) 0.66324(6) 0.03877(17) Uani 1 1 d . . . O16 O 0.50299(10) 0.14954(10) 0.41665(19) 0.0536(5) Uani 1 1 d . . . O15 O 0.49306(11) 0.19998(10) 0.6037(2) 0.0626(6) Uani 1 1 d . . . N10 N 0.62625(9) 0.15115(9) 0.61767(18) 0.0302(4) Uani 1 1 d . . . N5 N 0.53214(10) 0.02648(9) 0.72282(18) 0.0312(4) Uani 1 1 d . . . C12 C 0.64155(13) 0.19640(14) 0.5127(3) 0.0414(6) Uani 1 1 d . . . C4 C 0.46899(14) -0.03077(12) 0.7033(3) 0.0429(6) Uani 1 1 d . . . C3 C 0.41717(14) -0.01838(13) 0.7373(3) 0.0439(7) Uani 1 1 d . . . C7 C 0.57943(15) 0.00993(14) 0.6773(3) 0.0425(6) Uani 1 1 d . . . C6 C 0.54150(17) 0.03991(16) 0.8567(2) 0.0435(7) Uani 1 1 d . . . C8 C 0.64645(15) 0.06334(16) 0.6770(3) 0.0485(7) Uani 1 1 d . . . C9 C 0.65871(13) 0.11517(15) 0.5885(3) 0.0425(6) Uani 1 1 d . . . C11 C 0.65418(14) 0.18830(15) 0.7319(3) 0.0442(7) Uani 1 1 d . . . C13 C 0.60554(14) 0.23043(13) 0.5244(3) 0.0464(7) Uani 1 1 d . . . H6A H 0.5842(17) 0.0755(16) 0.873(3) 0.058(10) Uiso 1 1 d . . . H12A H 0.6274(14) 0.1697(14) 0.438(3) 0.046(8) Uiso 1 1 d . . . H4A H 0.4679(15) -0.0646(16) 0.751(3) 0.056(9) Uiso 1 1 d . . . H4B H 0.4663(13) -0.0424(14) 0.616(3) 0.041(8) Uiso 1 1 d . . . H6C H 0.5127(16) 0.0514(15) 0.883(3) 0.052(9) Uiso 1 1 d . . . H6B H 0.5328(14) 0.0020(15) 0.899(3) 0.050(9) Uiso 1 1 d . . . H8A H 0.6605(14) 0.0807(14) 0.759(3) 0.045(8) Uiso 1 1 d . . . H11A H 0.6991(18) 0.2180(18) 0.714(3) 0.071(11) Uiso 1 1 d . . . H9B H 0.6451(13) 0.0981(13) 0.509(3) 0.039(7) Uiso 1 1 d . . . H11B H 0.6323(16) 0.2066(16) 0.754(3) 0.055(10) Uiso 1 1 d . . . H8B H 0.6704(14) 0.0461(14) 0.651(3) 0.044(8) Uiso 1 1 d . . . H12B H 0.6860(16) 0.2238(16) 0.509(3) 0.058(9) Uiso 1 1 d . . . H9A H 0.7042(16) 0.1466(15) 0.584(3) 0.053(9) Uiso 1 1 d . . . H11C H 0.6521(15) 0.1600(16) 0.797(3) 0.055(9) Uiso 1 1 d . . . H3A H 0.3791(16) -0.0517(15) 0.708(3) 0.053(9) Uiso 1 1 d . . . H7A H 0.5662(13) -0.0063(12) 0.594(3) 0.033(7) Uiso 1 1 d . . . H7B H 0.5737(15) -0.0248(15) 0.726(3) 0.051(8) Uiso 1 1 d . . . H13A H 0.6065(15) 0.2508(16) 0.448(3) 0.054(9) Uiso 1 1 d . . . H3B H 0.4155(15) -0.0131(15) 0.826(3) 0.053(9) Uiso 1 1 d . . . H13B H 0.6155(15) 0.2559(16) 0.598(3) 0.057(9) Uiso 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 0.02334(16) 0.02332(16) 0.02578(16) 0.00109(11) 0.00121(11) 0.01202(12) S14 0.0336(3) 0.0294(3) 0.0410(4) 0.0079(3) 0.0045(3) 0.0177(3) S1 0.0263(3) 0.0373(4) 0.0500(4) 0.0092(3) 0.0060(3) 0.0140(3) O16 0.0536(12) 0.0552(13) 0.0440(11) 0.0101(9) -0.0093(9) 0.0213(11) O15 0.0730(15) 0.0465(12) 0.0859(17) 0.0165(11) 0.0310(13) 0.0431(12) N10 0.0257(10) 0.0340(11) 0.0296(10) -0.0022(8) 0.0010(8) 0.0138(9) N5 0.0374(11) 0.0309(11) 0.0290(10) -0.0004(8) 0.0011(8) 0.0198(9) C12 0.0293(14) 0.0416(15) 0.0429(15) 0.0114(13) 0.0094(11) 0.0100(12) C4 0.0494(17) 0.0257(13) 0.0501(17) 0.0036(12) 0.0029(13) 0.0162(12) C3 0.0376(15) 0.0309(14) 0.0490(17) 0.0055(12) 0.0067(13) 0.0066(12) C7 0.0546(17) 0.0440(16) 0.0453(16) 0.0013(13) 0.0019(13) 0.0368(15) C6 0.0590(19) 0.0497(18) 0.0286(13) 0.0055(12) 0.0018(13) 0.0324(17) C8 0.0463(17) 0.064(2) 0.0544(18) -0.0051(15) -0.0048(14) 0.0417(16) C9 0.0324(14) 0.0550(18) 0.0462(16) -0.0030(14) 0.0051(12) 0.0265(14) C11 0.0348(15) 0.0455(17) 0.0427(16) -0.0115(13) -0.0043(12) 0.0129(14) C13 0.0405(16) 0.0323(14) 0.0577(19) 0.0125(14) 0.0048(14) 0.0116(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 N5 2.002(2) . ? Ni1 N10 2.009(2) . ? Ni1 S14 2.1392(8) . ? Ni1 S1 2.1635(8) . ? S14 O15 1.457(2) . ? S14 O16 1.466(2) . ? S14 C13 1.807(3) . ? S1 C3 1.814(3) . ? N10 C9 1.491(3) . ? N10 C11 1.495(3) . ? N10 C12 1.508(3) . ? N5 C6 1.491(3) . ? N5 C7 1.495(3) . ? N5 C4 1.500(3) . ? C12 C13 1.496(4) . ? C12 H12A 0.99(3) . ? C12 H12B 0.96(3) . ? C4 C3 1.496(4) . ? C4 H4A 0.97(3) . ? C4 H4B 0.99(3) . ? C3 H3A 0.94(3) . ? C3 H3B 0.98(3) . ? C7 C8 1.508(5) . ? C7 H7A 0.98(3) . ? C7 H7B 0.96(3) . ? C6 H6A 0.99(4) . ? C6 H6C 0.93(3) . ? C6 H6B 0.96(3) . ? C8 C9 1.504(4) . ? C8 H8A 0.98(3) . ? C8 H8B 0.93(3) . ? C9 H9B 0.95(3) . ? C9 H9A 0.99(3) . ? C11 H11A 0.99(4) . ? C11 H11B 0.89(3) . ? C11 H11C 0.98(3) . ? C13 H13A 0.97(3) . ? C13 H13B 0.97(3) . ? 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 N5 Ni1 N10 96.58(8) . . ? N5 Ni1 S14 174.25(6) . . ? N10 Ni1 S14 88.38(6) . . ? N5 Ni1 S1 89.40(6) . . ? N10 Ni1 S1 173.13(6) . . ? S14 Ni1 S1 85.83(3) . . ? O15 S14 O16 114.89(15) . . ? O15 S14 C13 106.49(15) . . ? O16 S14 C13 103.78(15) . . ? O15 S14 Ni1 118.11(10) . . ? O16 S14 Ni1 109.92(9) . . ? C13 S14 Ni1 101.62(10) . . ? C3 S1 Ni1 100.11(10) . . ? C9 N10 C11 108.8(2) . . ? C9 N10 C12 105.4(2) . . ? C11 N10 C12 108.4(2) . . ? C9 N10 Ni1 115.46(17) . . ? C11 N10 Ni1 108.71(16) . . ? C12 N10 Ni1 109.94(15) . . ? C6 N5 C7 109.3(2) . . ? C6 N5 C4 108.6(2) . . ? C7 N5 C4 106.1(2) . . ? C6 N5 Ni1 108.60(16) . . ? C7 N5 Ni1 115.61(16) . . ? C4 N5 Ni1 108.32(16) . . ? C13 C12 N10 110.4(2) . . ? C13 C12 H12A 109.3(17) . . ? N10 C12 H12A 105.0(18) . . ? C13 C12 H12B 113(2) . . ? N10 C12 H12B 109(2) . . ? H12A C12 H12B 110(3) . . ? C3 C4 N5 111.1(2) . . ? C3 C4 H4A 112.2(19) . . ? N5 C4 H4A 107.4(19) . . ? C3 C4 H4B 110.9(17) . . ? N5 C4 H4B 107.3(17) . . ? H4A C4 H4B 108(2) . . ? C4 C3 S1 108.34(19) . . ? C4 C3 H3A 108(2) . . ? S1 C3 H3A 109(2) . . ? C4 C3 H3B 111.6(19) . . ? S1 C3 H3B 108.1(19) . . ? H3A C3 H3B 111(3) . . ? N5 C7 C8 115.0(2) . . ? N5 C7 H7A 105.9(15) . . ? C8 C7 H7A 110.3(16) . . ? N5 C7 H7B 105.6(19) . . ? C8 C7 H7B 112.8(19) . . ? H7A C7 H7B 107(2) . . ? N5 C6 H6A 110.2(19) . . ? N5 C6 H6C 109(2) . . ? H6A C6 H6C 108(3) . . ? N5 C6 H6B 108.8(18) . . ? H6A C6 H6B 113(3) . . ? H6C C6 H6B 108(3) . . ? C9 C8 C7 114.1(2) . . ? C9 C8 H8A 109.9(18) . . ? C7 C8 H8A 111.8(18) . . ? C9 C8 H8B 106.5(19) . . ? C7 C8 H8B 105.6(19) . . ? H8A C8 H8B 109(3) . . ? N10 C9 C8 115.1(2) . . ? N10 C9 H9B 106.4(17) . . ? C8 C9 H9B 109.7(17) . . ? N10 C9 H9A 106.1(18) . . ? C8 C9 H9A 111.3(18) . . ? H9B C9 H9A 108(2) . . ? N10 C11 H11A 106(2) . . ? N10 C11 H11B 109(2) . . ? H11A C11 H11B 114(3) . . ? N10 C11 H11C 109.1(19) . . ? H11A C11 H11C 108(3) . . ? H11B C11 H11C 109(3) . . ? C12 C13 S14 105.9(2) . . ? C12 C13 H13A 110.3(19) . . ? S14 C13 H13A 104.3(19) . . ? C12 C13 H13B 114(2) . . ? S14 C13 H13B 104.8(19) . . ? H13A C13 H13B 117(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.270 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.066 # Attachment '- Dalton-Complex 7.CIF' data_bc25 _database_code_depnum_ccdc_archive 'CCDC 828724' #TrackingRef '- Dalton-Complex 7.CIF' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H29 N3 Ni O8 S2' _chemical_formula_weight 466.21 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.453(3) _cell_length_b 14.741(3) _cell_length_c 13.011(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.28(2) _cell_angle_gamma 90.00 _cell_volume 1934.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method ? _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2353 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 21.97 _reflns_number_total 2353 _reflns_number_observed 1596 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 247 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^)+(0.0684P)^2^+3.4511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2106 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_obs 0.0482 _refine_ls_wR_factor_all 0.1464 _refine_ls_wR_factor_obs 0.1191 _refine_ls_goodness_of_fit_all 1.115 _refine_ls_goodness_of_fit_obs 1.189 _refine_ls_restrained_S_all 1.176 _refine_ls_restrained_S_obs 1.189 _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 Ni Ni 0.64586(8) 0.41780(6) 0.16479(7) 0.0266(3) Uani 1 d . . S1 S 0.3630(2) 0.45974(13) 0.2176(2) 0.0388(5) Uani 1 d . . S2 S 0.8027(2) 0.60746(12) 0.1374(2) 0.0382(5) Uani 1 d . . O1 O 0.4642(5) 0.4772(3) 0.1602(4) 0.0427(14) Uani 1 d . . O2 O 0.2383(5) 0.4994(4) 0.1620(5) 0.063(2) Uani 1 d . . O3 O 0.4087(7) 0.4854(4) 0.3276(5) 0.074(2) Uani 1 d . . O4 O 0.6829(4) 0.5521(3) 0.1257(4) 0.0347(12) Uani 1 d . . O5 O 0.7815(6) 0.6786(4) 0.0597(5) 0.061(2) Uani 1 d . . O6 O 0.8573(5) 0.6374(4) 0.2451(4) 0.059(2) Uani 1 d . . O7 O 0.7224(5) 0.4380(4) 0.3240(4) 0.0401(13) Uani 1 d . . O1W O 0.5661(4) 0.3977(3) 0.0012(3) 0.0346(12) Uani 1 d . . N1 N 0.5771(6) 0.2871(4) 0.2047(4) 0.035(2) Uani 1 d . . N2 N 0.8414(5) 0.3741(4) 0.1559(5) 0.0337(15) Uani 1 d . . N3 N 0.7819(6) 0.5269(4) 0.4689(4) 0.038(2) Uani 1 d . . C1 C 0.3460(8) 0.3414(5) 0.2125(7) 0.050(2) Uani 1 d . . H1A H 0.2787(8) 0.3238(5) 0.2476(7) 0.061 Uiso 1 calc R . H1B H 0.3163(8) 0.3224(5) 0.1386(7) 0.061 Uiso 1 calc R . C2 C 0.4745(8) 0.2931(5) 0.2652(7) 0.048(2) Uani 1 d . . H2A H 0.5140(8) 0.3234(5) 0.3323(7) 0.058 Uiso 1 calc R . H2B H 0.4528(8) 0.2318(5) 0.2820(7) 0.058 Uiso 1 calc R . C3 C 0.6888(8) 0.2353(5) 0.2768(6) 0.047(2) Uani 1 d . . H3A H 0.7156(8) 0.2669(5) 0.3445(6) 0.056 Uiso 1 calc R . H3B H 0.6557(8) 0.1762(5) 0.2902(6) 0.056 Uiso 1 calc R . C4 C 0.8090(8) 0.2218(5) 0.2364(7) 0.051(2) Uani 1 d . . H4A H 0.7803(8) 0.2008(5) 0.1632(7) 0.061 Uiso 1 calc R . H4B H 0.8627(8) 0.1742(5) 0.2780(7) 0.061 Uiso 1 calc R . C5 C 0.8949(7) 0.3047(5) 0.2400(6) 0.046(2) Uani 1 d . . H5A H 0.9079(7) 0.3332(5) 0.3092(6) 0.056 Uiso 1 calc R . H5B H 0.9812(7) 0.2853(5) 0.2337(6) 0.056 Uiso 1 calc R . C6 C 0.9423(7) 0.4486(5) 0.1807(7) 0.046(2) Uani 1 d . . H6A H 1.0276(7) 0.4230(5) 0.1800(7) 0.055 Uiso 1 calc R . H6B H 0.9493(7) 0.4694(5) 0.2527(7) 0.055 Uiso 1 calc R . C7 C 0.9174(7) 0.5308(5) 0.1075(7) 0.046(2) Uani 1 d . . H7A H 0.8842(7) 0.5105(5) 0.0344(7) 0.055 Uiso 1 calc R . H7B H 1.0007(7) 0.5620(5) 0.1133(7) 0.055 Uiso 1 calc R . C8 C 0.5235(8) 0.2294(5) 0.1075(6) 0.052(2) Uani 1 d . . H8A H 0.5885(8) 0.2249(5) 0.0677(6) 0.077 Uiso 1 calc R . H8B H 0.4442(8) 0.2566(5) 0.0639(6) 0.077 Uiso 1 calc R . H8C H 0.5035(8) 0.1699(5) 0.1290(6) 0.077 Uiso 1 calc R . C9 C 0.8450(8) 0.3356(5) 0.0512(6) 0.048(2) Uani 1 d . . H9A H 0.8109(8) 0.3793(5) -0.0039(6) 0.072 Uiso 1 calc R . H9B H 0.7916(8) 0.2817(5) 0.0374(6) 0.072 Uiso 1 calc R . H9C H 0.9348(8) 0.3208(5) 0.0523(6) 0.072 Uiso 1 calc R . C10 C 0.7259(7) 0.5130(6) 0.3683(6) 0.042(2) Uani 1 d . . H10 H 0.6861(7) 0.5620(6) 0.3271(6) 0.050 Uiso 1 calc R . C11 C 0.8382(12) 0.4524(6) 0.5392(7) 0.089(4) Uani 1 d . . H11A H 0.8750(12) 0.4751(6) 0.6100(7) 0.133 Uiso 1 calc R . H11B H 0.9068(12) 0.4238(6) 0.5141(7) 0.133 Uiso 1 calc R . H11C H 0.7701(12) 0.4089(6) 0.5400(7) 0.133 Uiso 1 calc R . C12 C 0.7913(10) 0.6164(6) 0.5148(7) 0.065(3) Uani 1 d . . H12A H 0.8355(10) 0.6131(6) 0.5894(7) 0.097 Uiso 1 calc R . H12B H 0.7038(10) 0.6408(6) 0.5057(7) 0.097 Uiso 1 calc R . H12C H 0.8407(10) 0.6551(6) 0.4799(7) 0.097 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 Ni 0.0220(5) 0.0259(5) 0.0279(5) 0.0007(4) -0.0005(4) 0.0012(4) S1 0.0348(11) 0.0396(12) 0.0452(12) 0.0003(9) 0.0164(9) -0.0030(9) S2 0.0293(11) 0.0337(12) 0.0496(13) -0.0035(9) 0.0070(9) -0.0077(8) O1 0.027(3) 0.038(3) 0.066(4) 0.013(3) 0.016(3) 0.002(2) O2 0.027(3) 0.054(4) 0.105(5) 0.000(3) 0.010(3) 0.006(3) O3 0.102(5) 0.070(4) 0.053(4) -0.015(3) 0.025(4) -0.012(4) O4 0.021(3) 0.029(3) 0.052(3) 0.008(2) 0.007(2) -0.002(2) O5 0.066(4) 0.046(4) 0.071(4) 0.012(3) 0.020(3) -0.008(3) O6 0.052(4) 0.064(4) 0.057(4) -0.024(3) 0.009(3) -0.015(3) O7 0.046(3) 0.036(3) 0.033(3) -0.001(3) 0.000(2) 0.006(2) O1W 0.034(3) 0.033(3) 0.030(3) 0.000(2) -0.003(2) 0.000(2) N1 0.039(4) 0.029(3) 0.032(3) 0.000(3) -0.001(3) -0.005(3) N2 0.026(3) 0.030(3) 0.039(4) -0.005(3) -0.003(3) 0.004(3) N3 0.054(4) 0.034(4) 0.021(3) -0.001(3) 0.001(3) 0.002(3) C1 0.046(5) 0.042(5) 0.066(6) 0.007(4) 0.021(4) -0.013(4) C2 0.043(5) 0.039(5) 0.062(6) 0.016(4) 0.013(4) -0.005(4) C3 0.063(6) 0.028(4) 0.038(5) 0.009(4) -0.007(4) 0.001(4) C4 0.047(5) 0.039(5) 0.055(5) 0.008(4) -0.006(4) 0.015(4) C5 0.032(4) 0.047(5) 0.051(5) 0.006(4) -0.005(4) 0.016(4) C6 0.022(4) 0.045(5) 0.064(6) -0.001(4) -0.002(4) 0.003(4) C7 0.025(4) 0.049(5) 0.063(5) -0.015(4) 0.013(4) -0.009(4) C8 0.055(6) 0.030(4) 0.063(6) 0.000(4) 0.004(4) -0.009(4) C9 0.041(5) 0.053(5) 0.049(5) -0.010(4) 0.012(4) 0.010(4) C10 0.035(5) 0.040(5) 0.046(6) 0.008(4) 0.005(4) 0.005(4) C11 0.153(11) 0.054(6) 0.040(5) 0.001(5) -0.008(6) 0.025(7) C12 0.080(7) 0.053(6) 0.052(6) -0.017(5) 0.001(5) 0.002(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 Ni O7 2.036(5) . ? Ni O1 2.078(5) . ? Ni O1W 2.093(4) . ? Ni O4 2.105(5) . ? Ni N1 2.167(6) . ? Ni N2 2.175(6) . ? S1 O3 1.435(6) . ? S1 O2 1.437(6) . ? S1 O1 1.470(5) . ? S1 C1 1.753(8) . ? S2 O5 1.433(6) . ? S2 O6 1.435(5) . ? S2 O4 1.469(5) . ? S2 C7 1.764(8) . ? O7 C10 1.242(9) . ? N1 C2 1.491(9) . ? N1 C3 1.499(9) . ? N1 C8 1.505(9) . ? N2 C9 1.486(9) . ? N2 C5 1.495(9) . ? N2 C6 1.498(9) . ? N3 C10 1.302(9) . ? N3 C12 1.441(10) . ? N3 C11 1.451(10) . ? C1 C2 1.515(11) . ? C3 C4 1.498(11) . ? C4 C5 1.510(11) . ? C6 C7 1.521(11) . ? 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 O7 Ni O1 94.5(2) . . ? O7 Ni O1W 179.6(2) . . ? O1 Ni O1W 85.1(2) . . ? O7 Ni O4 93.5(2) . . ? O1 Ni O4 79.7(2) . . ? O1W Ni O4 86.4(2) . . ? O7 Ni N1 87.3(2) . . ? O1 Ni N1 91.3(2) . . ? O1W Ni N1 92.9(2) . . ? O4 Ni N1 171.1(2) . . ? O7 Ni N2 88.5(2) . . ? O1 Ni N2 171.1(2) . . ? O1W Ni N2 91.8(2) . . ? O4 Ni N2 91.7(2) . . ? N1 Ni N2 97.2(2) . . ? O3 S1 O2 114.4(4) . . ? O3 S1 O1 111.4(4) . . ? O2 S1 O1 110.6(3) . . ? O3 S1 C1 107.7(4) . . ? O2 S1 C1 108.5(4) . . ? O1 S1 C1 103.6(4) . . ? O5 S2 O6 114.3(4) . . ? O5 S2 O4 111.3(3) . . ? O6 S2 O4 112.4(3) . . ? O5 S2 C7 107.5(4) . . ? O6 S2 C7 107.1(4) . . ? O4 S2 C7 103.4(3) . . ? S1 O1 Ni 133.3(3) . . ? S2 O4 Ni 134.7(3) . . ? C10 O7 Ni 123.9(5) . . ? C2 N1 C3 104.5(6) . . ? C2 N1 C8 108.4(6) . . ? C3 N1 C8 107.1(6) . . ? C2 N1 Ni 113.9(4) . . ? C3 N1 Ni 110.5(4) . . ? C8 N1 Ni 112.0(4) . . ? C9 N2 C5 108.4(6) . . ? C9 N2 C6 106.9(6) . . ? C5 N2 C6 103.7(5) . . ? C9 N2 Ni 114.4(4) . . ? C5 N2 Ni 109.8(5) . . ? C6 N2 Ni 112.9(4) . . ? C10 N3 C12 121.6(7) . . ? C10 N3 C11 121.0(7) . . ? C12 N3 C11 117.4(6) . . ? C2 C1 S1 112.4(6) . . ? N1 C2 C1 117.6(7) . . ? C4 C3 N1 115.8(6) . . ? C3 C4 C5 115.4(7) . . ? N2 C5 C4 115.2(6) . . ? N2 C6 C7 117.0(6) . . ? C6 C7 S2 112.7(6) . . ? O7 C10 N3 123.9(7) . . ? _refine_diff_density_max 0.395 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.092 # Attachment '- Complex 9-BC56.CIF' data_bc56 _database_code_depnum_ccdc_archive 'CCDC 828725' #TrackingRef '- Complex 9-BC56.CIF' _audit_update_record ; 2011-06-13 # Formatted by publCIF ; _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H18 N2 Ni S2' _chemical_formula_weight 265.07 _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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 8.7150(3) _cell_length_b 9.2850(3) _cell_length_c 7.7890(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.517(2) _cell_angle_gamma 90.00 _cell_volume 577.93(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method ? _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 1.999 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1965 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1956 _reflns_number_observed 1844 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(2) _refine_ls_number_reflns 1956 _refine_ls_number_parameters 119 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_obs 0.0269 _refine_ls_wR_factor_all 0.0672 _refine_ls_wR_factor_obs 0.0658 _refine_ls_goodness_of_fit_all 1.446 _refine_ls_goodness_of_fit_obs 1.463 _refine_ls_restrained_S_all 1.445 _refine_ls_restrained_S_obs 1.462 _refine_ls_shift/su_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.17204(7) 0.24725(3) 0.84906(7) 0.03292(13) Uani 1 d . . S1 S 0.4026(2) 0.26244(11) 0.8052(2) 0.0554(4) Uani 1 d . . S2 S 0.0202(2) 0.19515(13) 0.5594(2) 0.0514(2) Uani 1 d . . N1 N 0.2984(5) 0.2611(3) 1.1161(5) 0.0385(9) Uani 1 d . . N2 N -0.0310(6) 0.2665(3) 0.8935(5) 0.0384(10) Uani 1 d . . C1 C 0.5436(6) 0.3160(5) 1.0436(7) 0.0653(11) Uani 1 d . . H1A H 0.6159(6) 0.2359(5) 1.1060(7) 0.078 Uiso 1 calc R . H1B H 0.6135(6) 0.3955(5) 1.0378(7) 0.078 Uiso 1 calc R . C2 C 0.4424(5) 0.3605(4) 1.1527(5) 0.0558(9) Uani 1 d . . H2A H 0.5134(5) 0.3602(4) 1.2855(5) 0.067 Uiso 1 calc R . H2B H 0.4011(5) 0.4578(4) 1.1178(5) 0.067 Uiso 1 calc R . C3 C 0.3621(5) 0.1147(4) 1.1916(5) 0.0577(10) Uani 1 d . . H3A H 0.4349(5) 0.0800(4) 1.1351(5) 0.087 Uiso 1 calc R . H3B H 0.2695(5) 0.0498(4) 1.1632(5) 0.087 Uiso 1 calc R . H3C H 0.4229(5) 0.1203(4) 1.3248(5) 0.087 Uiso 1 calc R . C4 C 0.1859(5) 0.3159(4) 1.2021(4) 0.0495(8) Uani 1 d . . H4A H 0.1753(5) 0.4197(4) 1.1894(4) 0.059 Uiso 1 calc R . H4B H 0.2299(5) 0.2918(4) 1.3342(4) 0.059 Uiso 1 calc R . C5 C 0.0167(5) 0.2443(3) 1.0993(5) 0.0439(9) Uani 1 d . . H5A H 0.0238(5) 0.1423(3) 1.1281(5) 0.053 Uiso 1 calc R . H5B H -0.0665(5) 0.2872(3) 1.1371(5) 0.053 Uiso 1 calc R . C6 C -0.1002(5) 0.4143(4) 0.8424(5) 0.0562(10) Uani 1 d . . H6A H -0.0189(5) 0.4835(4) 0.9166(5) 0.084 Uiso 1 calc R . H6B H -0.2000(5) 0.4235(4) 0.8656(5) 0.084 Uiso 1 calc R . H6C H -0.1263(5) 0.4312(4) 0.7122(5) 0.084 Uiso 1 calc R . C7 C -0.1534(4) 0.1579(4) 0.7814(5) 0.0461(8) Uani 1 d . . H7A H -0.2587(4) 0.1726(4) 0.7939(5) 0.055 Uiso 1 calc R . H7B H -0.1128(4) 0.0623(4) 0.8275(5) 0.055 Uiso 1 calc R . C8 C -0.1807(5) 0.1694(5) 0.5797(5) 0.0571(9) Uani 1 d . . H8A H -0.2540(5) 0.2501(5) 0.5225(5) 0.069 Uiso 1 calc R . H8B H -0.2340(5) 0.0824(5) 0.5140(5) 0.069 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 0.0376(2) 0.0323(2) 0.0342(2) 0.00217(13) 0.0199(2) 0.00266(14) S1 0.0549(8) 0.0536(7) 0.0759(10) -0.0065(5) 0.0453(8) -0.0071(5) S2 0.0590(6) 0.0650(6) 0.0333(4) -0.0001(6) 0.0218(4) 0.0052(7) N1 0.033(2) 0.042(2) 0.038(2) 0.0016(10) 0.012(2) -0.0016(10) N2 0.044(2) 0.044(2) 0.033(2) 0.0096(12) 0.022(2) 0.0107(13) C1 0.044(2) 0.061(2) 0.092(3) -0.006(2) 0.029(2) -0.011(2) C2 0.048(2) 0.052(2) 0.065(2) -0.009(2) 0.020(2) -0.013(2) C3 0.050(2) 0.052(2) 0.059(2) 0.015(2) 0.008(2) 0.002(2) C4 0.055(2) 0.059(2) 0.035(2) -0.0069(15) 0.019(2) -0.004(2) C5 0.044(2) 0.059(2) 0.034(2) 0.0032(12) 0.020(2) 0.0026(14) C6 0.068(3) 0.055(2) 0.056(2) 0.011(2) 0.035(2) 0.024(2) C7 0.029(2) 0.061(2) 0.050(2) 0.001(2) 0.017(2) 0.0011(15) C8 0.041(2) 0.079(3) 0.041(2) -0.005(2) 0.006(2) 0.009(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 N1 1.931(4) . ? Ni1 N2 1.942(4) . ? Ni1 S2 2.1664(14) . ? Ni1 S1 2.1726(14) . ? S1 C1 1.840(5) . ? S2 C8 1.835(4) . ? N1 C4 1.481(5) . ? N1 C2 1.491(5) . ? N1 C3 1.498(4) . ? N2 C7 1.474(5) . ? N2 C6 1.488(4) . ? N2 C5 1.501(5) . ? C1 C2 1.506(5) . ? C4 C5 1.521(5) . ? C7 C8 1.497(5) . ? 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 88.3(2) . . ? N1 Ni1 S2 170.30(9) . . ? N2 Ni1 S2 89.12(13) . . ? N1 Ni1 S1 89.95(12) . . ? N2 Ni1 S1 170.93(9) . . ? S2 Ni1 S1 94.01(6) . . ? C1 S1 Ni1 98.42(15) . . ? C8 S2 Ni1 98.45(12) . . ? C4 N1 C2 111.1(3) . . ? C4 N1 C3 110.0(3) . . ? C2 N1 C3 109.6(3) . . ? C4 N1 Ni1 108.3(2) . . ? C2 N1 Ni1 108.8(2) . . ? C3 N1 Ni1 109.0(2) . . ? C7 N2 C6 110.6(4) . . ? C7 N2 C5 111.4(3) . . ? C6 N2 C5 108.8(3) . . ? C7 N2 Ni1 109.1(2) . . ? C6 N2 Ni1 109.8(3) . . ? C5 N2 Ni1 107.1(3) . . ? C2 C1 S1 109.7(3) . . ? N1 C2 C1 111.1(3) . . ? N1 C4 C5 106.8(3) . . ? N2 C5 C4 107.4(3) . . ? N2 C7 C8 110.3(3) . . ? C7 C8 S2 110.0(2) . . ? _refine_diff_density_max 0.203 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.059