# 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_requested_category FM _publ_contact_author_name 'Marc Fourmigue' _publ_contact_author_email marc.fourmigue@univ-rennes1.fr _publ_author_name 'Marc Fourmigue' data_job _database_code_depnum_ccdc_archive 'CCDC 850836' #TrackingRef '- Neutre.cif' _audit_creation_date 2011-05-13T10:07:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H8 Ni0.5 O S4 ' _chemical_formula_sum 'C6 H8 Ni0.5 O S4 ' _chemical_formula_weight 253.72 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6821(6) _cell_length_b 8.1203(7) _cell_length_c 8.7853(6) _cell_angle_alpha 97.483(3) _cell_angle_beta 114.055(3) _cell_angle_gamma 99.403(3) _cell_volume 481.79(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4263 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.46 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 260 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.687 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_number 7481 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.6 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 2157 _reflns_number_gt 1989 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0331P)^2^+0.2016P] 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_number_reflns 2157 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.586 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Fe Fe 0.3463 0.8444 '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' 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 0.5 0.5 0 0.01760(10) Uani 1 2 d S . . S5 S 0.60911(7) 0.12705(6) 0.38724(6) 0.02231(12) Uani 1 1 d . . . S4 S 0.81061(7) 0.04052(6) 0.11924(6) 0.02208(12) Uani 1 1 d . . . S2 S 0.64715(7) 0.31141(6) -0.04538(6) 0.02130(12) Uani 1 1 d . . . S3 S 0.47882(6) 0.40064(6) 0.20631(5) 0.01939(12) Uani 1 1 d . . . O1 O 1.02033(18) 0.31939(16) 0.46057(16) 0.0228(3) Uani 1 1 d . . . C6 C 0.7841(3) 0.2928(3) 0.5745(2) 0.0255(4) Uani 1 1 d . . . H6A H 0.7562 0.4054 0.5566 0.031 Uiso 1 1 calc R . . H6B H 0.7657 0.2706 0.6758 0.031 Uiso 1 1 calc R . . C1 C 0.6752(2) 0.1985(2) 0.1109(2) 0.0187(4) Uani 1 1 d . . . C2 C 0.5960(2) 0.2377(2) 0.2236(2) 0.0181(4) Uani 1 1 d . . . C3 C 1.0617(3) 0.1735(3) 0.2287(3) 0.0254(4) Uani 1 1 d . . . H3A H 1.1493 0.1118 0.2003 0.03 Uiso 1 1 calc R . . H3B H 1.0661 0.2801 0.1857 0.03 Uiso 1 1 calc R . . C5 C 0.9949(3) 0.2999(3) 0.6093(2) 0.0270(4) Uani 1 1 d . . . H5A H 1.083 0.3974 0.7051 0.032 Uiso 1 1 calc R . . H5B H 1.0296 0.1934 0.6421 0.032 Uiso 1 1 calc R . . C4 C 1.1381(3) 0.2191(3) 0.4199(3) 0.0273(4) Uani 1 1 d . . . H4A H 1.132 0.1138 0.4648 0.033 Uiso 1 1 calc R . . H4B H 1.2766 0.2849 0.4728 0.033 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 0.01628(17) 0.02083(18) 0.01633(17) 0.00587(12) 0.00687(13) 0.00542(13) S5 0.0215(2) 0.0239(2) 0.0240(2) 0.01087(19) 0.01079(19) 0.00539(18) S4 0.0202(2) 0.0188(2) 0.0244(2) 0.00091(18) 0.00776(18) 0.00556(18) S2 0.0238(2) 0.0256(3) 0.0185(2) 0.00687(18) 0.01135(19) 0.00920(19) S3 0.0189(2) 0.0230(2) 0.0202(2) 0.00772(18) 0.01051(18) 0.00781(18) O1 0.0229(7) 0.0214(7) 0.0255(7) 0.0055(5) 0.0105(5) 0.0086(5) C6 0.0312(10) 0.0295(10) 0.0191(9) 0.0065(8) 0.0132(8) 0.0090(8) C1 0.0145(8) 0.0180(9) 0.0187(8) 0.0033(7) 0.0036(7) 0.0017(7) C2 0.0155(8) 0.0188(9) 0.0167(8) 0.0043(7) 0.0046(7) 0.0019(7) C3 0.0173(9) 0.0252(10) 0.0330(11) 0.0022(8) 0.0114(8) 0.0058(7) C5 0.0298(10) 0.0273(10) 0.0177(9) 0.0045(8) 0.0053(8) 0.0047(8) C4 0.0183(9) 0.0238(10) 0.0331(11) 0.0005(8) 0.0059(8) 0.0066(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S3 2.1309(4) . ? Ni1 S3 2.1310(4) 2_665 ? Ni1 S2 2.1345(5) 2_665 ? Ni1 S2 2.1345(5) . ? S5 C2 1.7701(18) . ? S5 C6 1.831(2) . ? S4 C1 1.7694(18) . ? S4 C3 1.8297(19) . ? S2 C1 1.7100(18) . ? S3 C2 1.7071(18) . ? O1 C5 1.421(2) . ? O1 C4 1.428(2) . ? C6 C5 1.510(3) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C1 C2 1.387(3) . ? C3 C4 1.505(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? 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 S3 Ni1 S3 180 . 2_665 ? S3 Ni1 S2 88.683(17) . 2_665 ? S3 Ni1 S2 91.317(17) 2_665 2_665 ? S3 Ni1 S2 91.318(17) . . ? S3 Ni1 S2 88.683(17) 2_665 . ? S2 Ni1 S2 179.9990(10) 2_665 . ? C2 S5 C6 99.78(8) . . ? C1 S4 C3 100.64(8) . . ? C1 S2 Ni1 105.13(7) . . ? C2 S3 Ni1 105.18(6) . . ? C5 O1 C4 116.22(15) . . ? C5 C6 S5 112.75(14) . . ? C5 C6 H6A 109 . . ? S5 C6 H6A 109 . . ? C5 C6 H6B 109 . . ? S5 C6 H6B 109 . . ? H6A C6 H6B 107.8 . . ? C2 C1 S2 118.96(14) . . ? C2 C1 S4 124.50(14) . . ? S2 C1 S4 116.53(11) . . ? C1 C2 S3 119.31(13) . . ? C1 C2 S5 123.46(14) . . ? S3 C2 S5 117.23(10) . . ? C4 C3 S4 113.42(14) . . ? C4 C3 H3A 108.9 . . ? S4 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? S4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? O1 C5 C6 109.70(14) . . ? O1 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O1 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O1 C4 C3 108.64(15) . . ? O1 C4 H4A 110 . . ? C3 C4 H4A 110 . . ? O1 C4 H4B 110 . . ? C3 C4 H4B 110 . . ? H4A C4 H4B 108.3 . . ? 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 S3 Ni1 S2 C1 -2.98(6) . . . . ? S3 Ni1 S2 C1 177.02(6) 2_665 . . . ? S2 Ni1 S2 C1 138(5) 2_665 . . . ? S3 Ni1 S3 C2 -153(18) 2_665 . . . ? S2 Ni1 S3 C2 -177.71(6) 2_665 . . . ? S2 Ni1 S3 C2 2.29(6) . . . . ? C2 S5 C6 C5 -82.30(14) . . . . ? Ni1 S2 C1 C2 3.31(16) . . . . ? Ni1 S2 C1 S4 -175.32(8) . . . . ? C3 S4 C1 C2 -99.06(17) . . . . ? C3 S4 C1 S2 79.48(12) . . . . ? S2 C1 C2 S3 -1.7(2) . . . . ? S4 C1 C2 S3 176.85(9) . . . . ? S2 C1 C2 S5 178.28(9) . . . . ? S4 C1 C2 S5 -3.2(2) . . . . ? Ni1 S3 C2 C1 -0.90(16) . . . . ? Ni1 S3 C2 S5 179.15(8) . . . . ? C6 S5 C2 C1 109.26(16) . . . . ? C6 S5 C2 S3 -70.80(12) . . . . ? C1 S4 C3 C4 82.09(15) . . . . ? C4 O1 C5 C6 -138.01(16) . . . . ? S5 C6 C5 O1 54.57(19) . . . . ? C5 O1 C4 C3 147.72(16) . . . . ? S4 C3 C4 O1 -63.03(18) . . . . ? # Attachment '- Ni(DMF)6.cif' data_import1 _database_code_depnum_ccdc_archive 'CCDC 850837' #TrackingRef '- Ni(DMF)6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H42 N6 Ni O6, C12 H16 Ni O2 S8, C12 H12 Ni O2 S8' _chemical_formula_sum 'C42 H70 N6 Ni3 O10 S16' _chemical_formula_weight 1508.23 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' 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' N N 0.0061 0.0033 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9808(2) _cell_length_b 13.5908(2) _cell_length_c 14.3025(3) _cell_angle_alpha 83.5470(10) _cell_angle_beta 81.7430(10) _cell_angle_gamma 79.2450(10) _cell_volume 1690.68(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9043 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 0.933 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.74745 # #-------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37140 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7751 _reflns_number_gt 5754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0333P)^2^+1.4240P] 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 7751 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 0.5000 0.0000 0.5000 0.04187(12) Uani 1 2 d S . . Ni2 Ni 0.5000 0.5000 0.0000 0.05303(15) Uani 1 2 d S . . Ni3 Ni 0.0000 0.0000 0.0000 0.03304(11) Uani 1 2 d S . . S1 S 0.49952(8) -0.14987(6) 0.56691(6) 0.05346(19) Uani 1 1 d . . . S2 S 0.68658(10) -0.29333(6) 0.69458(6) 0.0611(2) Uani 1 1 d . . . S3 S 0.89133(10) -0.11240(7) 0.70047(6) 0.0619(2) Uani 1 1 d . . . S4 S 0.68302(8) 0.01715(5) 0.57540(5) 0.04839(17) Uani 1 1 d . . . S5 S 0.67288(10) 0.59041(7) -0.00322(6) 0.0643(2) Uani 1 1 d . . . S6 S 0.76696(13) 0.71571(6) 0.12698(8) 0.0754(3) Uani 1 1 d . . . S7 S 0.46623(13) 0.66486(9) 0.28070(9) 0.0895(3) Uani 1 1 d . . . S8 S 0.39534(10) 0.54591(8) 0.13648(7) 0.0692(2) Uani 1 1 d . . . O1 O 0.9711(3) -0.26925(18) 0.54467(16) 0.0650(6) Uani 1 1 d . . . O2 O 0.8027(3) 0.53042(18) 0.27935(17) 0.0694(6) Uani 1 1 d . . . N1C N 0.0583(3) 0.13311(18) -0.27575(16) 0.0503(6) Uani 1 1 d . . . N1A N 0.1556(3) -0.26788(17) -0.12440(17) 0.0476(5) Uani 1 1 d . . . N1E N 0.3944(2) 0.02997(19) 0.10626(17) 0.0472(5) Uani 1 1 d . . . C1 C 0.6513(3) -0.1728(2) 0.63333(19) 0.0455(6) Uani 1 1 d . . . C2 C 0.7750(4) -0.3676(3) 0.5984(3) 0.0693(9) Uani 1 1 d . . . H2A H 0.7591 -0.4364 0.6150 0.083 Uiso 1 1 calc R . . H2B H 0.7252 -0.3421 0.5425 0.083 Uiso 1 1 calc R . . C3 C 0.9438(5) -0.3671(3) 0.5747(3) 0.0816(11) Uani 1 1 d . . . H3A H 0.9947 -0.3926 0.6301 0.098 Uiso 1 1 calc R . . H3B H 0.9856 -0.4110 0.5248 0.098 Uiso 1 1 calc R . . C4 C 1.0927(4) -0.2404(3) 0.5821(3) 0.0810(12) Uani 1 1 d . . . H4A H 1.1832 -0.2470 0.5357 0.097 Uiso 1 1 calc R . . H4B H 1.1160 -0.2842 0.6384 0.097 Uiso 1 1 calc R . . C5 C 1.0497(4) -0.1342(3) 0.6068(3) 0.0694(10) Uani 1 1 d . . . H5A H 1.0233 -0.0916 0.5503 0.083 Uiso 1 1 calc R . . H5B H 1.1380 -0.1139 0.6259 0.083 Uiso 1 1 calc R . . C6 C 0.7331(3) -0.0992(2) 0.63643(19) 0.0454(6) Uani 1 1 d . . . C7 C 0.6374(4) 0.6391(2) 0.1057(3) 0.0605(8) Uani 1 1 d . . . C8 C 0.9313(4) 0.6249(3) 0.1521(3) 0.0729(10) Uani 1 1 d . . . H8A H 0.9409 0.5697 0.1129 0.087 Uiso 1 1 calc R . . H8B H 1.0216 0.6557 0.1347 0.087 Uiso 1 1 calc R . . C9 C 0.9260(5) 0.5838(4) 0.2534(3) 0.0931(14) Uani 1 1 d . . . H9A H 1.0213 0.5392 0.2630 0.112 Uiso 1 1 calc R . . H9B H 0.9140 0.6385 0.2935 0.112 Uiso 1 1 calc R . . C10 C 0.7105(6) 0.5536(4) 0.3644(3) 0.0964(15) Uani 1 1 d . . . H10A H 0.7241 0.6186 0.3804 0.116 Uiso 1 1 calc R . . H10B H 0.7422 0.5037 0.4150 0.116 Uiso 1 1 calc R . . C11 C 0.5451(5) 0.5560(4) 0.3570(3) 0.0937(14) Uani 1 1 d . . . C12 C 0.5159(4) 0.6200(2) 0.1671(3) 0.0623(8) Uani 1 1 d . . . O1A O 0.1298(4) -0.1134(3) -0.0749(2) 0.0428(9) Uani 0.682(7) 1 d P A 1 C1A C 0.0784(8) -0.1926(4) -0.0762(4) 0.0408(12) Uani 0.682(7) 1 d P A 1 H1A H -0.0165 -0.1988 -0.0425 0.049 Uiso 0.682(7) 1 calc PR A 1 C2A C 0.0807(11) -0.3578(6) -0.1215(7) 0.067(2) Uani 0.682(7) 1 d P A 1 H2A1 H 0.1462 -0.4073 -0.1586 0.100 Uiso 0.682(7) 1 calc PR A 1 H2A2 H -0.0147 -0.3381 -0.1471 0.100 Uiso 0.682(7) 1 calc PR A 1 H2A3 H 0.0625 -0.3857 -0.0571 0.100 Uiso 0.682(7) 1 calc PR A 1 C3A C 0.2997(13) -0.2691(7) -0.1759(8) 0.070(2) Uani 0.682(7) 1 d P A 1 H3A1 H 0.3317 -0.3316 -0.2043 0.104 Uiso 0.682(7) 1 calc PR A 1 H3A2 H 0.3713 -0.2624 -0.1342 0.104 Uiso 0.682(7) 1 calc PR A 1 H3A3 H 0.2955 -0.2143 -0.2246 0.104 Uiso 0.682(7) 1 calc PR A 1 O1C O -0.0136(4) 0.0950(3) -0.1213(3) 0.0426(9) Uani 0.682(7) 1 d P A 1 C1C C 0.0857(8) 0.0887(4) -0.1905(4) 0.0407(11) Uani 0.682(7) 1 d P A 1 H1C H 0.1822 0.0520 -0.1831 0.049 Uiso 0.682(7) 1 calc PR A 1 C2C C -0.0840(13) 0.1882(7) -0.2955(6) 0.0606(19) Uani 0.682(7) 1 d P A 1 H2C1 H -0.0773 0.2129 -0.3613 0.091 Uiso 0.682(7) 1 calc PR A 1 H2C2 H -0.1123 0.2438 -0.2570 0.091 Uiso 0.682(7) 1 calc PR A 1 H2C3 H -0.1597 0.1455 -0.2819 0.091 Uiso 0.682(7) 1 calc PR A 1 C3C C 0.1910(12) 0.1243(7) -0.3473(6) 0.073(2) Uani 0.682(7) 1 d P A 1 H3C1 H 0.1624 0.1578 -0.4065 0.109 Uiso 0.682(7) 1 calc PR A 1 H3C2 H 0.2298 0.0545 -0.3550 0.109 Uiso 0.682(7) 1 calc PR A 1 H3C3 H 0.2684 0.1546 -0.3278 0.109 Uiso 0.682(7) 1 calc PR A 1 O1E O 0.1974(4) 0.0439(3) 0.0221(2) 0.0415(9) Uani 0.682(7) 1 d P A 1 C1E C 0.2880(6) -0.0061(5) 0.0741(4) 0.0423(13) Uani 0.682(7) 1 d P A 1 H1E H 0.2801 -0.0732 0.0914 0.051 Uiso 0.682(7) 1 calc PR A 1 C2E C 0.4971(7) -0.0345(7) 0.1680(5) 0.076(2) Uani 0.682(7) 1 d P A 1 H2E1 H 0.5677 0.0035 0.1849 0.114 Uiso 0.682(7) 1 calc PR A 1 H2E2 H 0.5525 -0.0906 0.1351 0.114 Uiso 0.682(7) 1 calc PR A 1 H2E3 H 0.4381 -0.0587 0.2244 0.114 Uiso 0.682(7) 1 calc PR A 1 C3E C 0.4113(9) 0.1339(7) 0.0863(6) 0.0662(18) Uani 0.682(7) 1 d P A 1 H3E1 H 0.4951 0.1456 0.1158 0.099 Uiso 0.682(7) 1 calc PR A 1 H3E2 H 0.3191 0.1761 0.1108 0.099 Uiso 0.682(7) 1 calc PR A 1 H3E3 H 0.4309 0.1493 0.0190 0.099 Uiso 0.682(7) 1 calc PR A 1 O1B O 0.0393(8) -0.1424(6) -0.0405(5) 0.045(2) Uani 0.318(7) 1 d P A 2 C1B C 0.1477(15) -0.1764(12) -0.0938(9) 0.047(3) Uani 0.318(7) 1 d P A 2 H1B H 0.2261 -0.1399 -0.1140 0.057 Uiso 0.318(7) 1 calc PR A 2 C2B C 0.051(3) -0.3292(16) -0.1026(16) 0.094(7) Uani 0.318(7) 1 d P A 2 H2B1 H 0.0852 -0.3893 -0.1346 0.140 Uiso 0.318(7) 1 calc PR A 2 H2B2 H -0.0448 -0.2954 -0.1224 0.140 Uiso 0.318(7) 1 calc PR A 2 H2B3 H 0.0376 -0.3464 -0.0353 0.140 Uiso 0.318(7) 1 calc PR A 2 C3B C 0.308(3) -0.3018(14) -0.1921(19) 0.071(5) Uani 0.318(7) 1 d P A 2 H3B1 H 0.3079 -0.3669 -0.2119 0.107 Uiso 0.318(7) 1 calc PR A 2 H3B2 H 0.3946 -0.3050 -0.1586 0.107 Uiso 0.318(7) 1 calc PR A 2 H3B3 H 0.3149 -0.2541 -0.2468 0.107 Uiso 0.318(7) 1 calc PR A 2 O1D O 0.0875(9) 0.0523(6) -0.1335(6) 0.044(2) Uani 0.318(7) 1 d P A 2 C1D C 0.0035(18) 0.1086(9) -0.1815(11) 0.047(3) Uani 0.318(7) 1 d P A 2 H1D H -0.0953 0.1352 -0.1565 0.056 Uiso 0.318(7) 1 calc PR A 2 C2D C -0.075(4) 0.193(2) -0.3295(14) 0.096(8) Uani 0.318(7) 1 d P A 2 H2D1 H -0.0359 0.2096 -0.3944 0.144 Uiso 0.318(7) 1 calc PR A 2 H2D2 H -0.1169 0.2542 -0.3000 0.144 Uiso 0.318(7) 1 calc PR A 2 H2D3 H -0.1526 0.1532 -0.3271 0.144 Uiso 0.318(7) 1 calc PR A 2 C3D C 0.190(4) 0.0923(16) -0.343(3) 0.144(14) Uani 0.318(7) 1 d P A 2 H3D1 H 0.1851 0.1301 -0.4033 0.216 Uiso 0.318(7) 1 calc PR A 2 H3D2 H 0.1872 0.0231 -0.3489 0.216 Uiso 0.318(7) 1 calc PR A 2 H3D3 H 0.2828 0.0972 -0.3190 0.216 Uiso 0.318(7) 1 calc PR A 2 O1F O 0.2138(8) -0.0253(6) 0.0412(5) 0.0425(19) Uani 0.318(7) 1 d P A 2 C1F C 0.2769(14) 0.0435(10) 0.0534(8) 0.038(2) Uani 0.318(7) 1 d P A 2 H1F H 0.2433 0.1075 0.0255 0.046 Uiso 0.318(7) 1 calc PR A 2 C2F C 0.4507(15) -0.0672(12) 0.1530(9) 0.058(3) Uani 0.318(7) 1 d P A 2 H2F1 H 0.5332 -0.0616 0.1869 0.086 Uiso 0.318(7) 1 calc PR A 2 H2F2 H 0.4865 -0.1147 0.1065 0.086 Uiso 0.318(7) 1 calc PR A 2 H2F3 H 0.3697 -0.0896 0.1967 0.086 Uiso 0.318(7) 1 calc PR A 2 C3F C 0.4646(19) 0.1174(15) 0.1154(15) 0.076(5) Uani 0.318(7) 1 d P A 2 H3F1 H 0.5456 0.0974 0.1544 0.114 Uiso 0.318(7) 1 calc PR A 2 H3F2 H 0.3888 0.1686 0.1441 0.114 Uiso 0.318(7) 1 calc PR A 2 H3F3 H 0.5052 0.1434 0.0538 0.114 Uiso 0.318(7) 1 calc PR A 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 0.0301(2) 0.0459(3) 0.0457(3) 0.0005(2) 0.00029(19) -0.00335(19) Ni2 0.0477(3) 0.0574(3) 0.0598(3) 0.0090(3) -0.0219(3) -0.0209(2) Ni3 0.0331(2) 0.0340(2) 0.0336(2) -0.00588(17) -0.00444(17) -0.00785(17) S1 0.0379(4) 0.0525(4) 0.0692(5) 0.0094(3) -0.0098(3) -0.0121(3) S2 0.0644(5) 0.0575(5) 0.0559(5) 0.0158(4) -0.0054(4) -0.0103(4) S3 0.0611(5) 0.0783(6) 0.0501(4) 0.0009(4) -0.0207(4) -0.0150(4) S4 0.0458(4) 0.0496(4) 0.0502(4) -0.0004(3) -0.0068(3) -0.0111(3) S5 0.0655(5) 0.0738(5) 0.0635(5) 0.0092(4) -0.0195(4) -0.0378(4) S6 0.0916(7) 0.0473(4) 0.1000(7) 0.0072(4) -0.0438(6) -0.0288(4) S7 0.0759(7) 0.0932(7) 0.0946(8) -0.0361(6) -0.0211(6) 0.0224(6) S8 0.0474(4) 0.0898(6) 0.0746(6) -0.0053(5) -0.0127(4) -0.0201(4) O1 0.0564(13) 0.0722(15) 0.0604(14) 0.0046(11) -0.0090(11) -0.0011(11) O2 0.0757(16) 0.0697(15) 0.0646(15) -0.0054(12) -0.0143(12) -0.0133(12) N1C 0.0625(16) 0.0530(14) 0.0364(12) 0.0009(10) -0.0059(11) -0.0159(12) N1A 0.0509(14) 0.0402(12) 0.0527(14) -0.0150(10) -0.0104(11) -0.0012(11) N1E 0.0328(11) 0.0650(15) 0.0441(13) -0.0059(11) -0.0061(10) -0.0075(11) C1 0.0380(14) 0.0529(16) 0.0404(14) 0.0028(12) 0.0014(11) -0.0032(12) C2 0.078(2) 0.0501(18) 0.083(3) -0.0065(17) -0.026(2) -0.0076(16) C3 0.084(3) 0.061(2) 0.091(3) -0.013(2) -0.008(2) 0.0113(19) C4 0.0441(19) 0.101(3) 0.089(3) 0.004(2) -0.0108(18) 0.0035(19) C5 0.0432(17) 0.083(2) 0.081(2) 0.0165(19) -0.0137(16) -0.0168(16) C6 0.0408(14) 0.0543(16) 0.0370(14) 0.0008(12) 0.0000(11) -0.0042(12) C7 0.065(2) 0.0463(16) 0.077(2) 0.0078(15) -0.0331(18) -0.0155(14) C8 0.065(2) 0.070(2) 0.093(3) 0.003(2) -0.026(2) -0.0300(18) C9 0.095(3) 0.095(3) 0.102(3) 0.019(3) -0.053(3) -0.037(3) C10 0.104(4) 0.114(4) 0.064(3) -0.017(2) -0.024(2) 0.016(3) C11 0.086(3) 0.117(4) 0.064(2) 0.002(2) 0.001(2) 0.002(3) C12 0.060(2) 0.0564(18) 0.072(2) -0.0077(16) -0.0267(17) 0.0010(15) O1A 0.0440(19) 0.0365(19) 0.0491(17) -0.0121(14) -0.0005(14) -0.0093(14) C1A 0.043(3) 0.036(3) 0.044(3) -0.006(2) -0.002(2) -0.008(2) C2A 0.076(4) 0.052(4) 0.077(5) -0.028(3) 0.011(3) -0.026(3) C3A 0.059(4) 0.066(6) 0.083(5) -0.040(4) 0.003(4) 0.002(4) O1C 0.044(2) 0.0468(18) 0.036(2) 0.0019(14) -0.0016(15) -0.0094(15) C1C 0.038(3) 0.043(3) 0.042(3) -0.002(2) -0.004(2) -0.010(2) C2C 0.062(4) 0.067(4) 0.056(5) 0.003(3) -0.020(4) -0.016(3) C3C 0.077(5) 0.065(6) 0.067(4) -0.017(4) 0.007(3) 0.007(4) O1E 0.0379(17) 0.042(2) 0.0478(17) -0.0024(14) -0.0116(14) -0.0114(14) C1E 0.031(3) 0.045(3) 0.046(3) -0.002(2) 0.004(2) -0.002(2) C2E 0.043(3) 0.119(7) 0.057(4) 0.008(4) -0.015(3) 0.006(3) C3E 0.059(4) 0.086(4) 0.066(4) -0.027(3) -0.009(3) -0.029(4) O1B 0.042(4) 0.042(4) 0.054(4) -0.017(3) -0.008(3) -0.007(3) C1B 0.036(6) 0.054(8) 0.055(7) -0.008(5) -0.009(5) -0.012(6) C2B 0.16(2) 0.064(12) 0.064(10) -0.037(8) -0.022(11) -0.006(11) C3B 0.056(7) 0.058(11) 0.092(12) -0.039(8) 0.019(8) 0.012(8) O1D 0.044(5) 0.048(4) 0.042(4) -0.001(3) -0.006(3) -0.010(3) C1D 0.039(6) 0.047(6) 0.054(9) -0.003(5) -0.001(6) -0.009(5) C2D 0.062(9) 0.156(18) 0.056(13) 0.012(12) -0.008(10) 0.005(9) C3D 0.16(2) 0.036(10) 0.20(3) -0.029(11) 0.083(18) -0.012(11) O1F 0.033(3) 0.049(5) 0.047(4) 0.003(3) -0.010(3) -0.012(3) C1F 0.036(6) 0.040(6) 0.037(5) 0.000(5) -0.002(4) -0.006(5) C2F 0.041(7) 0.093(9) 0.044(6) -0.019(5) -0.015(5) -0.008(6) C3F 0.062(10) 0.084(11) 0.102(14) -0.032(10) -0.009(8) -0.047(9) _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 S4 2.1511(7) . ? Ni1 S4 2.1511(7) 2_656 ? Ni1 S1 2.1515(7) 2_656 ? Ni1 S1 2.1515(7) . ? Ni2 S5 2.1451(8) . ? Ni2 S5 2.1451(8) 2_665 ? Ni2 S8 2.1473(10) 2_665 ? Ni2 S8 2.1473(10) . ? Ni3 O1B 2.035(8) . ? Ni3 O1B 2.035(8) 2 ? Ni3 O1F 2.046(8) . ? Ni3 O1F 2.046(8) 2 ? Ni3 O1C 2.047(4) 2 ? Ni3 O1C 2.047(4) . ? Ni3 O1E 2.048(4) 2 ? Ni3 O1E 2.049(4) . ? Ni3 O1A 2.055(4) . ? Ni3 O1A 2.055(4) 2 ? Ni3 O1D 2.059(9) . ? Ni3 O1D 2.059(9) 2 ? S1 C1 1.733(3) . ? S2 C1 1.764(3) . ? S2 C2 1.800(4) . ? S3 C6 1.770(3) . ? S3 C5 1.814(4) . ? S4 C6 1.732(3) . ? S5 C7 1.725(4) . ? S6 C7 1.776(3) . ? S6 C8 1.790(4) . ? S7 C12 1.767(4) . ? S7 C11 1.830(5) . ? S8 C12 1.739(4) . ? O1 C3 1.406(5) . ? O1 C4 1.417(5) . ? O2 C10 1.401(5) . ? O2 C9 1.418(5) . ? N1C C1C 1.332(7) . ? N1C C1D 1.392(17) . ? N1C C2C 1.405(12) . ? N1C C3C 1.451(11) . ? N1C C3D 1.47(3) . ? N1C C2D 1.56(3) . ? N1A C1A 1.327(7) . ? N1A C1B 1.350(16) . ? N1A C2B 1.35(3) . ? N1A C3A 1.392(12) . ? N1A C2A 1.495(8) . ? N1A C3B 1.59(2) . ? N1E C1E 1.310(7) . ? N1E C1F 1.358(15) . ? N1E C3E 1.441(9) . ? N1E C2F 1.447(16) . ? N1E C2E 1.468(7) . ? N1E C3F 1.472(16) . ? C1 C6 1.356(4) . ? C2 C3 1.506(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.491(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C12 1.345(5) . ? C8 C9 1.491(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.498(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O1A C1A 1.251(7) . ? C1A H1A 0.9300 . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C2A H2A3 0.9600 . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? O1C C1C 1.233(7) . ? C1C H1C 0.9300 . ? C2C H2C1 0.9600 . ? C2C H2C2 0.9600 . ? C2C H2C3 0.9600 . ? C3C H3C1 0.9600 . ? C3C H3C2 0.9600 . ? C3C H3C3 0.9600 . ? O1E C1E 1.238(8) . ? C1E H1E 0.9300 . ? C2E H2E1 0.9600 . ? C2E H2E2 0.9600 . ? C2E H2E3 0.9600 . ? C3E H3E1 0.9600 . ? C3E H3E2 0.9600 . ? C3E H3E3 0.9600 . ? O1B C1B 1.200(17) . ? C1B H1B 0.9300 . ? C2B H2B1 0.9600 . ? C2B H2B2 0.9600 . ? C2B H2B3 0.9600 . ? C3B H3B1 0.9600 . ? C3B H3B2 0.9600 . ? C3B H3B3 0.9600 . ? O1D C1D 1.200(17) . ? C1D H1D 0.9300 . ? C2D H2D1 0.9600 . ? C2D H2D2 0.9600 . ? C2D H2D3 0.9600 . ? C3D H3D1 0.9600 . ? C3D H3D2 0.9600 . ? C3D H3D3 0.9600 . ? O1F C1F 1.221(17) . ? C1F H1F 0.9300 . ? C2F H2F1 0.9600 . ? C2F H2F2 0.9600 . ? C2F H2F3 0.9600 . ? C3F H3F1 0.9600 . ? C3F H3F2 0.9600 . ? C3F H3F3 0.9600 . ? 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 S4 Ni1 S4 180.0 . 2_656 ? S4 Ni1 S1 89.12(3) . 2_656 ? S4 Ni1 S1 90.88(3) 2_656 2_656 ? S4 Ni1 S1 90.88(3) . . ? S4 Ni1 S1 89.12(3) 2_656 . ? S1 Ni1 S1 179.998(1) 2_656 . ? S5 Ni2 S5 180.0 . 2_665 ? S5 Ni2 S8 88.63(4) . 2_665 ? S5 Ni2 S8 91.36(4) 2_665 2_665 ? S5 Ni2 S8 91.36(4) . . ? S5 Ni2 S8 88.64(4) 2_665 . ? S8 Ni2 S8 180.0 2_665 . ? O1B Ni3 O1B 180.0 . 2 ? O1B Ni3 O1F 89.3(3) . . ? O1B Ni3 O1F 90.7(3) 2 . ? O1B Ni3 O1F 90.7(3) . 2 ? O1B Ni3 O1F 89.3(3) 2 2 ? O1F Ni3 O1F 180.0 . 2 ? O1B Ni3 O1C 73.4(2) . 2 ? O1B Ni3 O1C 106.6(2) 2 2 ? O1F Ni3 O1C 68.0(2) . 2 ? O1F Ni3 O1C 112.0(2) 2 2 ? O1B Ni3 O1C 106.6(2) . . ? O1B Ni3 O1C 73.4(2) 2 . ? O1F Ni3 O1C 112.0(2) . . ? O1F Ni3 O1C 68.0(2) 2 . ? O1C Ni3 O1C 180.0 2 . ? O1B Ni3 O1E 68.2(2) . 2 ? O1B Ni3 O1E 111.8(2) 2 2 ? O1F Ni3 O1E 153.45(19) . 2 ? O1F Ni3 O1E 26.55(19) 2 2 ? O1C Ni3 O1E 91.34(13) 2 2 ? O1C Ni3 O1E 88.66(13) . 2 ? O1B Ni3 O1E 111.8(2) . . ? O1B Ni3 O1E 68.2(2) 2 . ? O1F Ni3 O1E 26.55(19) . . ? O1F Ni3 O1E 153.45(19) 2 . ? O1C Ni3 O1E 88.66(13) 2 . ? O1C Ni3 O1E 91.34(13) . . ? O1E Ni3 O1E 180.0 2 . ? O1B Ni3 O1A 28.56(19) . . ? O1B Ni3 O1A 151.44(19) 2 . ? O1F Ni3 O1A 72.7(2) . . ? O1F Ni3 O1A 107.3(2) 2 . ? O1C Ni3 O1A 88.85(13) 2 . ? O1C Ni3 O1A 91.15(13) . . ? O1E Ni3 O1A 91.13(12) 2 . ? O1E Ni3 O1A 88.87(12) . . ? O1B Ni3 O1A 151.45(19) . 2 ? O1B Ni3 O1A 28.56(19) 2 2 ? O1F Ni3 O1A 107.3(2) . 2 ? O1F Ni3 O1A 72.7(2) 2 2 ? O1C Ni3 O1A 91.15(13) 2 2 ? O1C Ni3 O1A 88.85(13) . 2 ? O1E Ni3 O1A 88.87(12) 2 2 ? O1E Ni3 O1A 91.13(12) . 2 ? O1A Ni3 O1A 179.999(1) . 2 ? O1B Ni3 O1D 90.3(3) . . ? O1B Ni3 O1D 89.7(3) 2 . ? O1F Ni3 O1D 90.0(3) . . ? O1F Ni3 O1D 90.0(3) 2 . ? O1C Ni3 O1D 152.21(19) 2 . ? O1C Ni3 O1D 27.79(19) . . ? O1E Ni3 O1D 103.5(2) 2 . ? O1E Ni3 O1D 76.5(2) . . ? O1A Ni3 O1D 67.8(2) . . ? O1A Ni3 O1D 112.2(2) 2 . ? O1B Ni3 O1D 89.7(3) . 2 ? O1B Ni3 O1D 90.3(3) 2 2 ? O1F Ni3 O1D 90.0(3) . 2 ? O1F Ni3 O1D 90.0(3) 2 2 ? O1C Ni3 O1D 27.79(19) 2 2 ? O1C Ni3 O1D 152.21(19) . 2 ? O1E Ni3 O1D 76.5(2) 2 2 ? O1E Ni3 O1D 103.5(2) . 2 ? O1A Ni3 O1D 112.2(2) . 2 ? O1A Ni3 O1D 67.8(2) 2 2 ? O1D Ni3 O1D 180.0(4) . 2 ? C1 S1 Ni1 104.86(10) . . ? C1 S2 C2 100.67(15) . . ? C6 S3 C5 101.31(15) . . ? C6 S4 Ni1 104.84(10) . . ? C7 S5 Ni2 104.52(12) . . ? C7 S6 C8 102.43(16) . . ? C12 S7 C11 101.75(18) . . ? C12 S8 Ni2 104.14(13) . . ? C3 O1 C4 115.6(3) . . ? C10 O2 C9 115.7(4) . . ? C1C N1C C1D 31.2(5) . . ? C1C N1C C2C 123.9(5) . . ? C1D N1C C2C 92.8(7) . . ? C1C N1C C3C 114.3(5) . . ? C1D N1C C3C 145.5(7) . . ? C2C N1C C3C 121.7(5) . . ? C1C N1C C3D 105.9(14) . . ? C1D N1C C3D 135.4(14) . . ? C2C N1C C3D 128.7(15) . . ? C3C N1C C3D 17.0(11) . . ? C1C N1C C2D 141.2(9) . . ? C1D N1C C2D 110.0(10) . . ? C2C N1C C2D 17.6(10) . . ? C3C N1C C2D 104.4(9) . . ? C3D N1C C2D 111.2(17) . . ? C1A N1A C1B 30.4(5) . . ? C1A N1A C2B 96.7(8) . . ? C1B N1A C2B 127.1(10) . . ? C1A N1A C3A 125.0(5) . . ? C1B N1A C3A 94.6(7) . . ? C2B N1A C3A 138.3(8) . . ? C1A N1A C2A 116.5(4) . . ? C1B N1A C2A 146.9(7) . . ? C2B N1A C2A 19.8(8) . . ? C3A N1A C2A 118.5(4) . . ? C1A N1A C3B 143.2(8) . . ? C1B N1A C3B 112.9(10) . . ? C2B N1A C3B 120.1(10) . . ? C3A N1A C3B 18.4(9) . . ? C2A N1A C3B 100.2(8) . . ? C1E N1E C1F 30.4(4) . . ? C1E N1E C3E 122.0(4) . . ? C1F N1E C3E 91.6(6) . . ? C1E N1E C2F 91.4(6) . . ? C1F N1E C2F 121.8(7) . . ? C3E N1E C2F 146.6(6) . . ? C1E N1E C2E 120.3(5) . . ? C1F N1E C2E 150.7(7) . . ? C3E N1E C2E 117.7(4) . . ? C2F N1E C2E 29.0(5) . . ? C1E N1E C3F 148.5(8) . . ? C1F N1E C3F 118.2(9) . . ? C3E N1E C3F 26.6(7) . . ? C2F N1E C3F 120.0(9) . . ? C2E N1E C3F 91.1(8) . . ? C6 C1 S1 119.5(2) . . ? C6 C1 S2 124.3(2) . . ? S1 C1 S2 116.18(17) . . ? C3 C2 S2 113.5(3) . . ? C3 C2 H2A 108.9 . . ? S2 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? S2 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O1 C3 C2 110.6(3) . . ? O1 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O1 C4 C5 110.1(3) . . ? O1 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? O1 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 S3 114.6(3) . . ? C4 C5 H5A 108.6 . . ? S3 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? S3 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C1 C6 S4 119.6(2) . . ? C1 C6 S3 124.3(2) . . ? S4 C6 S3 116.04(17) . . ? C12 C7 S5 120.0(3) . . ? C12 C7 S6 124.3(3) . . ? S5 C7 S6 115.7(2) . . ? C9 C8 S6 113.8(3) . . ? C9 C8 H8A 108.8 . . ? S6 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? S6 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O2 C9 C8 110.5(3) . . ? O2 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O2 C10 C11 111.6(4) . . ? O2 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? O2 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 S7 111.9(4) . . ? C7 C12 S8 119.8(3) . . ? C7 C12 S7 124.8(3) . . ? S8 C12 S7 115.5(2) . . ? C1A O1A Ni3 118.8(5) . . ? O1A C1A N1A 121.7(7) . . ? O1A C1A H1A 119.2 . . ? N1A C1A H1A 119.2 . . ? N1A C2A H2A1 109.5 . . ? N1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? N1A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? N1A C3A H3A1 109.5 . . ? N1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C1C O1C Ni3 123.2(5) . . ? O1C C1C N1C 121.7(7) . . ? O1C C1C H1C 119.2 . . ? N1C C1C H1C 119.2 . . ? N1C C2C H2C1 109.5 . . ? N1C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? N1C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? N1C C3C H3C1 109.5 . . ? N1C C3C H3C2 109.5 . . ? H3C1 C3C H3C2 109.5 . . ? N1C C3C H3C3 109.5 . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? C1E O1E Ni3 123.2(5) . . ? O1E C1E N1E 123.8(7) . . ? O1E C1E H1E 118.1 . . ? N1E C1E H1E 118.1 . . ? N1E C2E H2E1 109.5 . . ? N1E C2E H2E2 109.5 . . ? H2E1 C2E H2E2 109.5 . . ? N1E C2E H2E3 109.5 . . ? H2E1 C2E H2E3 109.5 . . ? H2E2 C2E H2E3 109.5 . . ? N1E C3E H3E1 109.5 . . ? N1E C3E H3E2 109.5 . . ? H3E1 C3E H3E2 109.5 . . ? N1E C3E H3E3 109.5 . . ? H3E1 C3E H3E3 109.5 . . ? H3E2 C3E H3E3 109.5 . . ? C1B O1B Ni3 124.3(11) . . ? O1B C1B N1A 119.8(15) . . ? O1B C1B H1B 120.1 . . ? N1A C1B H1B 120.1 . . ? N1A C2B H2B1 109.5 . . ? N1A C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? N1A C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? N1A C3B H3B1 109.5 . . ? N1A C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? N1A C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C1D O1D Ni3 118.7(12) . . ? O1D C1D N1C 118.2(16) . . ? O1D C1D H1D 120.9 . . ? N1C C1D H1D 120.9 . . ? N1C C2D H2D1 109.5 . . ? N1C C2D H2D2 109.5 . . ? H2D1 C2D H2D2 109.5 . . ? N1C C2D H2D3 109.5 . . ? H2D1 C2D H2D3 109.5 . . ? H2D2 C2D H2D3 109.5 . . ? N1C C3D H3D1 109.5 . . ? N1C C3D H3D2 109.5 . . ? H3D1 C3D H3D2 109.5 . . ? N1C C3D H3D3 109.5 . . ? H3D1 C3D H3D3 109.5 . . ? H3D2 C3D H3D3 109.5 . . ? C1F O1F Ni3 121.9(11) . . ? O1F C1F N1E 122.3(14) . . ? O1F C1F H1F 118.8 . . ? N1E C1F H1F 118.8 . . ? N1E C2F H2F1 109.5 . . ? N1E C2F H2F2 109.5 . . ? H2F1 C2F H2F2 109.5 . . ? N1E C2F H2F3 109.5 . . ? H2F1 C2F H2F3 109.5 . . ? H2F2 C2F H2F3 109.5 . . ? N1E C3F H3F1 109.5 . . ? N1E C3F H3F2 109.5 . . ? H3F1 C3F H3F2 109.5 . . ? N1E C3F H3F3 109.5 . . ? H3F1 C3F H3F3 109.5 . . ? H3F2 C3F H3F3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S4 Ni1 S1 C1 -4.38(10) . . . . ? S4 Ni1 S1 C1 175.62(10) 2_656 . . . ? S1 Ni1 S1 C1 -27(27) 2_656 . . . ? S4 Ni1 S4 C6 -34(34) 2_656 . . . ? S1 Ni1 S4 C6 -175.26(10) 2_656 . . . ? S1 Ni1 S4 C6 4.74(10) . . . . ? S5 Ni2 S5 C7 -164(11) 2_665 . . . ? S8 Ni2 S5 C7 -175.99(11) 2_665 . . . ? S8 Ni2 S5 C7 4.01(11) . . . . ? S5 Ni2 S8 C12 -3.93(12) . . . . ? S5 Ni2 S8 C12 176.07(12) 2_665 . . . ? S8 Ni2 S8 C12 -2(11) 2_665 . . . ? Ni1 S1 C1 C6 3.0(2) . . . . ? Ni1 S1 C1 S2 -177.78(12) . . . . ? C2 S2 C1 C6 -105.3(3) . . . . ? C2 S2 C1 S1 75.5(2) . . . . ? C1 S2 C2 C3 84.1(3) . . . . ? C4 O1 C3 C2 136.7(3) . . . . ? S2 C2 C3 O1 -62.1(4) . . . . ? C3 O1 C4 C5 -139.6(3) . . . . ? O1 C4 C5 S3 64.3(4) . . . . ? C6 S3 C5 C4 -83.0(3) . . . . ? S1 C1 C6 S4 0.9(3) . . . . ? S2 C1 C6 S4 -178.21(15) . . . . ? S1 C1 C6 S3 -179.53(15) . . . . ? S2 C1 C6 S3 1.3(4) . . . . ? Ni1 S4 C6 C1 -4.3(2) . . . . ? Ni1 S4 C6 S3 176.07(12) . . . . ? C5 S3 C6 C1 100.4(3) . . . . ? C5 S3 C6 S4 -80.1(2) . . . . ? Ni2 S5 C7 C12 -3.3(3) . . . . ? Ni2 S5 C7 S6 178.13(14) . . . . ? C8 S6 C7 C12 105.1(3) . . . . ? C8 S6 C7 S5 -76.5(2) . . . . ? C7 S6 C8 C9 -86.0(3) . . . . ? C10 O2 C9 C8 -132.3(4) . . . . ? S6 C8 C9 O2 63.6(4) . . . . ? C9 O2 C10 C11 141.0(4) . . . . ? O2 C10 C11 S7 -70.8(5) . . . . ? C12 S7 C11 C10 85.3(4) . . . . ? S5 C7 C12 S8 0.2(4) . . . . ? S6 C7 C12 S8 178.59(17) . . . . ? S5 C7 C12 S7 179.93(18) . . . . ? S6 C7 C12 S7 -1.6(4) . . . . ? Ni2 S8 C12 C7 3.1(3) . . . . ? Ni2 S8 C12 S7 -176.71(14) . . . . ? C11 S7 C12 C7 -98.5(3) . . . . ? C11 S7 C12 S8 81.3(2) . . . . ? O1B Ni3 O1A C1A 6.5(5) . . . . ? O1B Ni3 O1A C1A -173.5(5) 2 . . . ? O1F Ni3 O1A C1A 129.7(4) . . . . ? O1F Ni3 O1A C1A -50.3(4) 2 . . . ? O1C Ni3 O1A C1A 62.3(3) 2 . . . ? O1C Ni3 O1A C1A -117.7(3) . . . . ? O1E Ni3 O1A C1A -29.0(3) 2 . . . ? O1E Ni3 O1A C1A 151.0(3) . . . . ? O1A Ni3 O1A C1A -159(7) 2 . . . ? O1D Ni3 O1A C1A -133.1(4) . . . . ? O1D Ni3 O1A C1A 46.9(4) 2 . . . ? Ni3 O1A C1A N1A 179.0(3) . . . . ? C1B N1A C1A O1A 4.0(10) . . . . ? C2B N1A C1A O1A -179.3(12) . . . . ? C3A N1A C1A O1A 1.5(9) . . . . ? C2A N1A C1A O1A -179.1(6) . . . . ? C3B N1A C1A O1A -1.5(19) . . . . ? O1B Ni3 O1C C1C -52.8(4) . . . . ? O1B Ni3 O1C C1C 127.2(4) 2 . . . ? O1F Ni3 O1C C1C 43.4(4) . . . . ? O1F Ni3 O1C C1C -136.6(4) 2 . . . ? O1C Ni3 O1C C1C 78(6) 2 . . . ? O1E Ni3 O1C C1C -119.5(4) 2 . . . ? O1E Ni3 O1C C1C 60.5(4) . . . . ? O1A Ni3 O1C C1C -28.4(4) . . . . ? O1A Ni3 O1C C1C 151.6(4) 2 . . . ? O1D Ni3 O1C C1C 3.5(5) . . . . ? O1D Ni3 O1C C1C -176.5(5) 2 . . . ? Ni3 O1C C1C N1C 162.7(3) . . . . ? C1D N1C C1C O1C -5.1(9) . . . . ? C2C N1C C1C O1C -1.6(7) . . . . ? C3C N1C C1C O1C 175.6(5) . . . . ? C3D N1C C1C O1C -168.6(12) . . . . ? C2D N1C C1C O1C -6(2) . . . . ? O1B Ni3 O1E C1E -52.2(4) . . . . ? O1B Ni3 O1E C1E 127.8(4) 2 . . . ? O1F Ni3 O1E C1E -18.5(5) . . . . ? O1F Ni3 O1E C1E 161.5(5) 2 . . . ? O1C Ni3 O1E C1E 19.3(4) 2 . . . ? O1C Ni3 O1E C1E -160.7(4) . . . . ? O1E Ni3 O1E C1E 23(5) 2 . . . ? O1A Ni3 O1E C1E -69.6(4) . . . . ? O1A Ni3 O1E C1E 110.4(4) 2 . . . ? O1D Ni3 O1E C1E -137.0(4) . . . . ? O1D Ni3 O1E C1E 43.0(4) 2 . . . ? Ni3 O1E C1E N1E -163.7(3) . . . . ? C1F N1E C1E O1E -0.9(8) . . . . ? C3E N1E C1E O1E 2.5(7) . . . . ? C2F N1E C1E O1E -177.6(7) . . . . ? C2E N1E C1E O1E 179.8(5) . . . . ? C3F N1E C1E O1E 5.9(17) . . . . ? O1B Ni3 O1B C1B 62.0(15) 2 . . . ? O1F Ni3 O1B C1B -53.6(8) . . . . ? O1F Ni3 O1B C1B 126.4(8) 2 . . . ? O1C Ni3 O1B C1B -120.8(8) 2 . . . ? O1C Ni3 O1B C1B 59.2(8) . . . . ? O1E Ni3 O1B C1B 140.8(8) 2 . . . ? O1E Ni3 O1B C1B -39.2(8) . . . . ? O1A Ni3 O1B C1B -0.5(7) . . . . ? O1A Ni3 O1B C1B 179.5(7) 2 . . . ? O1D Ni3 O1B C1B 36.4(8) . . . . ? O1D Ni3 O1B C1B -143.6(8) 2 . . . ? Ni3 O1B C1B N1A -173.0(6) . . . . ? C1A N1A C1B O1B 5.0(6) . . . . ? C2B N1A C1B O1B 0.9(19) . . . . ? C3A N1A C1B O1B -177.0(10) . . . . ? C2A N1A C1B O1B 0.0(19) . . . . ? C3B N1A C1B O1B -178.6(14) . . . . ? O1B Ni3 O1D C1D 114.6(8) . . . . ? O1B Ni3 O1D C1D -65.4(8) 2 . . . ? O1F Ni3 O1D C1D -156.1(8) . . . . ? O1F Ni3 O1D C1D 23.9(8) 2 . . . ? O1C Ni3 O1D C1D 167.5(7) 2 . . . ? O1C Ni3 O1D C1D -12.5(7) . . . . ? O1E Ni3 O1D C1D 47.1(8) 2 . . . ? O1E Ni3 O1D C1D -132.9(8) . . . . ? O1A Ni3 O1D C1D 132.7(8) . . . . ? O1A Ni3 O1D C1D -47.3(8) 2 . . . ? O1D Ni3 O1D C1D 28(8) 2 . . . ? Ni3 O1D C1D N1C -171.8(6) . . . . ? C1C N1C C1D O1D -8.0(5) . . . . ? C2C N1C C1D O1D 174.9(9) . . . . ? C3C N1C C1D O1D -7.0(17) . . . . ? C3D N1C C1D O1D 15(2) . . . . ? C2D N1C C1D O1D 171.4(15) . . . . ? O1B Ni3 O1F C1F 162.1(8) . . . . ? O1B Ni3 O1F C1F -17.9(8) 2 . . . ? O1F Ni3 O1F C1F 143(5) 2 . . . ? O1C Ni3 O1F C1F -125.5(8) 2 . . . ? O1C Ni3 O1F C1F 54.5(8) . . . . ? O1E Ni3 O1F C1F -166.8(6) 2 . . . ? O1E Ni3 O1F C1F 13.2(6) . . . . ? O1A Ni3 O1F C1F 138.5(8) . . . . ? O1A Ni3 O1F C1F -41.5(8) 2 . . . ? O1D Ni3 O1F C1F 71.9(8) . . . . ? O1D Ni3 O1F C1F -108.1(8) 2 . . . ? Ni3 O1F C1F N1E 160.0(6) . . . . ? C1E N1E C1F O1F -5.1(5) . . . . ? C3E N1E C1F O1F 177.8(9) . . . . ? C2F N1E C1F O1F -1.1(13) . . . . ? C2E N1E C1F O1F -3.8(17) . . . . ? C3F N1E C1F O1F 179.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.604 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.070 # Attachment '- NiCl.cif' data_import2 _database_code_depnum_ccdc_archive 'CCDC 850838' #TrackingRef '- NiCl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Cl N2 Ni2 O4 S8' _chemical_formula_sum 'C18 H30 Cl N2 Ni2 O4 S8' _chemical_formula_weight 747.79 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' Cl Cl 0.1484 0.1585 '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/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.9129(7) _cell_length_b 11.3753(5) _cell_length_c 25.6529(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.211(3) _cell_angle_gamma 90.00 _cell_volume 4018.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3532 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.39 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 1.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.931 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.762696 #-------------------------------------------------------------------# _diffrn_ambient_temperature 150(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 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12097 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.80 _diffrn_reflns_theta_max 27.41 _reflns_number_total 4740 _reflns_number_gt 3530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.017 -0.048 0.500 803.4 299.3 2 0.312 0.000 0.840 138.7 37.1 3 0.688 0.000 0.160 138.7 37.3 4 0.188 0.500 0.160 138.7 37.3 5 0.812 0.500 0.840 138.7 37.1 _platon_squeeze_details ; squeeze of one Et2O and two DMF disordered molecules ; _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^)+(0.0922P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4740 _refine_ls_number_parameters 168 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.077 _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 0.93427(4) 0.5000 0.29034(2) 0.03011(18) Uani 1 2 d S . . Ni2 Ni 0.55523(4) 0.5000 0.13022(2) 0.02684(17) Uani 1 2 d S . . Cl1 Cl 0.62764(7) 0.5000 0.05344(4) 0.0371(3) Uani 1 2 d S . . S1 S 0.66174(6) 0.35338(8) 0.17384(4) 0.0379(2) Uani 1 1 d . . . S2 S 0.84638(6) 0.36347(8) 0.24855(3) 0.0359(2) Uani 1 1 d . . . S3 S 1.02129(6) 0.63403(8) 0.33316(3) 0.0383(2) Uani 1 1 d . . . S4 S 1.19781(7) 0.64895(10) 0.41305(4) 0.0491(3) Uani 1 1 d . . . O2 O 1.3185(3) 0.5000 0.34115(15) 0.0568(10) Uani 1 2 d S . . O3 O 0.45862(16) 0.3680(2) 0.10844(9) 0.0415(6) Uani 1 1 d . . . N1 N 0.3853(2) 0.2309(3) 0.05485(13) 0.0499(8) Uani 1 1 d . . . C1 C 0.7538(2) 0.4402(3) 0.21056(11) 0.0306(7) Uani 1 1 d . . . O1A O 0.5008(2) 0.5000 0.20536(12) 0.0457(9) Uani 0.574(14) 2 d SPD . 1 C2A C 0.5862(3) 0.3157(5) 0.2247(2) 0.0779(18) Uani 0.574(14) 1 d PD . 1 H2A1 H 0.5647 0.2350 0.2190 0.094 Uiso 0.574(14) 1 calc PR . 1 H2A2 H 0.6269 0.3189 0.2587 0.094 Uiso 0.574(14) 1 calc PR . 1 C3A C 0.4969(6) 0.3920(6) 0.2276(4) 0.058(3) Uiso 0.574(14) 1 d PD . 1 H3A1 H 0.4401 0.3510 0.2102 0.070 Uiso 0.574(14) 1 calc PR . 1 H3A2 H 0.4889 0.4018 0.2643 0.070 Uiso 0.574(14) 1 calc PR . 1 O1B O 0.5008(2) 0.5000 0.20536(12) 0.0457(9) Uani 0.426(14) 2 d SPD . 2 C2B C 0.5862(3) 0.3157(5) 0.2247(2) 0.0779(18) Uani 0.426(14) 1 d PD . 2 H2B1 H 0.5344 0.2634 0.2099 0.094 Uiso 0.426(14) 1 calc PR . 2 H2B2 H 0.6255 0.2749 0.2534 0.094 Uiso 0.426(14) 1 calc PR . 2 C3B C 0.5467(7) 0.4157(7) 0.2438(3) 0.040(3) Uiso 0.426(14) 1 d PD . 2 H3B1 H 0.5980 0.4561 0.2666 0.048 Uiso 0.426(14) 1 calc PR . 2 H3B2 H 0.4989 0.3911 0.2656 0.048 Uiso 0.426(14) 1 calc PR . 2 C4 C 1.1128(2) 0.5599(3) 0.37363(12) 0.0391(8) Uani 1 1 d . . . C5 C 1.2788(3) 0.6943(4) 0.36628(17) 0.0566(11) Uani 1 1 d . . . H5A H 1.2411 0.7052 0.3318 0.068 Uiso 1 1 calc R . . H5B H 1.3084 0.7691 0.3774 0.068 Uiso 1 1 calc R . . C6 C 1.3577(4) 0.6044(5) 0.3625(2) 0.0749(14) Uani 1 1 d . . . H6A H 1.4032 0.6351 0.3406 0.090 Uiso 1 1 calc R . . H6B H 1.3928 0.5896 0.3973 0.090 Uiso 1 1 calc R . . C7 C 0.4350(2) 0.3294(3) 0.06506(15) 0.0429(9) Uani 1 1 d . . . H7 H 0.4528 0.3712 0.0368 0.052 Uiso 1 1 calc R . . C8 C 0.3597(5) 0.1612(6) 0.0972(2) 0.109(2) Uani 1 1 d . . . H8A H 0.3444 0.2117 0.1248 0.164 Uiso 1 1 calc R . . H8B H 0.4133 0.1114 0.1105 0.164 Uiso 1 1 calc R . . H8C H 0.3043 0.1136 0.0846 0.164 Uiso 1 1 calc R . . C9 C 0.3670(4) 0.1810(5) 0.0022(2) 0.0868(17) Uani 1 1 d . . . H9A H 0.3926 0.2324 -0.0221 0.130 Uiso 1 1 calc R . . H9B H 0.2983 0.1720 -0.0081 0.130 Uiso 1 1 calc R . . H9C H 0.3979 0.1056 0.0021 0.130 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 0.0255(3) 0.0355(4) 0.0278(3) 0.000 -0.0017(2) 0.000 Ni2 0.0218(3) 0.0343(4) 0.0241(3) 0.000 0.0021(2) 0.000 Cl1 0.0270(5) 0.0588(8) 0.0255(5) 0.000 0.0038(4) 0.000 S1 0.0336(4) 0.0287(5) 0.0465(5) 0.0050(4) -0.0116(4) -0.0058(3) S2 0.0320(4) 0.0311(5) 0.0405(5) 0.0033(4) -0.0089(3) 0.0003(3) S3 0.0350(4) 0.0374(5) 0.0385(5) -0.0031(4) -0.0078(4) 0.0021(4) S4 0.0461(5) 0.0576(7) 0.0398(5) -0.0117(5) -0.0071(4) -0.0038(4) O2 0.064(2) 0.056(3) 0.052(2) 0.000 0.012(2) 0.000 O3 0.0305(11) 0.0522(17) 0.0405(13) 0.0061(12) 0.0004(10) -0.0097(11) N1 0.0474(17) 0.047(2) 0.0511(18) 0.0032(15) -0.0081(14) -0.0152(15) C1 0.0236(14) 0.0381(18) 0.0278(15) -0.0014(13) -0.0037(12) -0.0031(12) O1A 0.0337(17) 0.075(3) 0.0292(16) 0.000 0.0064(14) 0.000 C2A 0.040(2) 0.097(4) 0.089(3) 0.069(3) -0.017(2) -0.031(2) O1B 0.0337(17) 0.075(3) 0.0292(16) 0.000 0.0064(14) 0.000 C2B 0.040(2) 0.097(4) 0.089(3) 0.069(3) -0.017(2) -0.031(2) C4 0.0349(17) 0.051(2) 0.0294(16) -0.0073(14) -0.0019(13) -0.0004(15) C5 0.055(2) 0.048(3) 0.065(3) 0.005(2) 0.002(2) -0.011(2) C6 0.065(3) 0.073(3) 0.093(4) -0.016(3) 0.031(3) -0.012(3) C7 0.0384(18) 0.041(2) 0.047(2) 0.0113(17) -0.0034(16) -0.0090(16) C8 0.111(4) 0.118(5) 0.088(4) 0.032(4) -0.025(3) -0.090(4) C9 0.095(4) 0.082(4) 0.081(3) -0.028(3) 0.006(3) -0.041(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 S3 2.1486(9) . ? Ni1 S3 2.1486(9) 6_565 ? Ni1 S2 2.1638(9) . ? Ni1 S2 2.1638(9) 6_565 ? Ni2 O3 2.039(2) . ? Ni2 O3 2.039(2) 6_565 ? Ni2 O1A 2.170(3) . ? Ni2 Cl1 2.3367(11) . ? Ni2 S1 2.3993(9) 6_565 ? Ni2 S1 2.3993(9) . ? S1 C1 1.777(3) . ? S1 C2A 1.838(4) . ? S2 C1 1.736(3) . ? S3 C4 1.741(3) . ? S4 C4 1.763(3) . ? S4 C5 1.833(4) . ? O2 C6 1.386(5) 6_565 ? O2 C6 1.386(5) . ? O3 C7 1.198(4) . ? N1 C7 1.323(5) . ? N1 C8 1.430(6) . ? N1 C9 1.453(5) . ? C1 C1 1.360(7) 6_565 ? O1A C3A 1.359(7) 6_565 ? O1A C3A 1.359(7) . ? C2A C3A 1.526(8) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C3B C3B 1.918(16) 6_565 ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4 C4 1.362(8) 6_565 ? C5 C6 1.513(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? 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 S3 Ni1 S3 90.40(5) . 6_565 ? S3 Ni1 S2 178.97(4) . . ? S3 Ni1 S2 88.93(3) 6_565 . ? S3 Ni1 S2 88.93(3) . 6_565 ? S3 Ni1 S2 178.97(4) 6_565 6_565 ? S2 Ni1 S2 91.73(5) . 6_565 ? O3 Ni2 O3 94.82(14) . 6_565 ? O3 Ni2 O1A 86.74(9) . . ? O3 Ni2 O1A 86.74(9) 6_565 . ? O3 Ni2 Cl1 96.65(7) . . ? O3 Ni2 Cl1 96.65(7) 6_565 . ? O1A Ni2 Cl1 174.96(9) . . ? O3 Ni2 S1 168.13(8) . 6_565 ? O3 Ni2 S1 87.43(7) 6_565 6_565 ? O1A Ni2 S1 81.74(7) . 6_565 ? Cl1 Ni2 S1 94.66(3) . 6_565 ? O3 Ni2 S1 87.43(7) . . ? O3 Ni2 S1 168.13(8) 6_565 . ? O1A Ni2 S1 81.74(7) . . ? Cl1 Ni2 S1 94.66(3) . . ? S1 Ni2 S1 88.08(4) 6_565 . ? C1 S1 C2A 101.24(19) . . ? C1 S1 Ni2 102.19(11) . . ? C2A S1 Ni2 96.62(15) . . ? C1 S2 Ni1 103.82(11) . . ? C4 S3 Ni1 105.75(12) . . ? C4 S4 C5 102.20(18) . . ? C6 O2 C6 117.9(6) 6_565 . ? C7 O3 Ni2 127.4(2) . . ? C7 N1 C8 120.0(4) . . ? C7 N1 C9 122.2(4) . . ? C8 N1 C9 117.3(4) . . ? C1 C1 S2 120.19(11) 6_565 . ? C1 C1 S1 123.77(11) 6_565 . ? S2 C1 S1 116.0(2) . . ? C3A O1A C3A 129.4(8) 6_565 . ? C3A O1A Ni2 114.4(3) 6_565 . ? C3A O1A Ni2 114.4(3) . . ? C3A C2A S1 117.0(3) . . ? C3A C2A H2A1 108.0 . . ? S1 C2A H2A1 108.0 . . ? C3A C2A H2A2 108.0 . . ? S1 C2A H2A2 108.0 . . ? H2A1 C2A H2A2 107.3 . . ? O1A C3A C2A 114.3(5) . . ? O1A C3A H3A1 108.7 . . ? C2A C3A H3A1 108.7 . . ? O1A C3A H3A2 108.7 . . ? C2A C3A H3A2 108.7 . . ? H3A1 C3A H3A2 107.6 . . ? C3B C3B H3B1 61.7 6_565 . ? C3B C3B H3B2 106.7 6_565 . ? H3B1 C3B H3B2 107.2 . . ? C4 C4 S3 118.98(12) 6_565 . ? C4 C4 S4 125.08(12) 6_565 . ? S3 C4 S4 115.9(2) . . ? C6 C5 S4 111.8(3) . . ? C6 C5 H5A 109.3 . . ? S4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? S4 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? O2 C6 C5 110.9(4) . . ? O2 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.0 . . ? O3 C7 N1 124.1(3) . . ? O3 C7 H7 117.9 . . ? N1 C7 H7 117.9 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ni2 S1 C1 -169.71(12) . . . . ? O3 Ni2 S1 C1 -68.5(4) 6_565 . . . ? O1A Ni2 S1 C1 -82.63(12) . . . . ? Cl1 Ni2 S1 C1 93.82(10) . . . . ? S1 Ni2 S1 C1 -0.70(11) 6_565 . . . ? O3 Ni2 S1 C2A -66.66(19) . . . . ? O3 Ni2 S1 C2A 34.6(4) 6_565 . . . ? O1A Ni2 S1 C2A 20.42(19) . . . . ? Cl1 Ni2 S1 C2A -163.12(18) . . . . ? S1 Ni2 S1 C2A 102.36(18) 6_565 . . . ? S3 Ni1 S2 C1 126(2) . . . . ? S3 Ni1 S2 C1 174.97(11) 6_565 . . . ? S2 Ni1 S2 C1 -4.25(12) 6_565 . . . ? S3 Ni1 S3 C4 3.14(13) 6_565 . . . ? S2 Ni1 S3 C4 52(2) . . . . ? S2 Ni1 S3 C4 -177.63(12) 6_565 . . . ? O3 Ni2 O3 C7 81.5(3) 6_565 . . . ? O1A Ni2 O3 C7 167.9(3) . . . . ? Cl1 Ni2 O3 C7 -15.8(3) . . . . ? S1 Ni2 O3 C7 -178.1(3) 6_565 . . . ? S1 Ni2 O3 C7 -110.2(3) . . . . ? Ni1 S2 C1 C1 3.42(9) . . . 6_565 ? Ni1 S2 C1 S1 -175.78(14) . . . . ? C2A S1 C1 C1 -98.79(18) . . . 6_565 ? Ni2 S1 C1 C1 0.61(10) . . . 6_565 ? C2A S1 C1 S2 80.4(2) . . . . ? Ni2 S1 C1 S2 179.77(14) . . . . ? O3 Ni2 O1A C3A -144.5(5) . . . 6_565 ? O3 Ni2 O1A C3A -49.5(5) 6_565 . . 6_565 ? Cl1 Ni2 O1A C3A 83.0(5) . . . 6_565 ? S1 Ni2 O1A C3A 38.4(5) 6_565 . . 6_565 ? S1 Ni2 O1A C3A 127.7(5) . . . 6_565 ? O3 Ni2 O1A C3A 49.5(5) . . . . ? O3 Ni2 O1A C3A 144.5(5) 6_565 . . . ? Cl1 Ni2 O1A C3A -83.0(5) . . . . ? S1 Ni2 O1A C3A -127.7(5) 6_565 . . . ? S1 Ni2 O1A C3A -38.4(5) . . . . ? C1 S1 C2A C3A 96.5(5) . . . . ? Ni2 S1 C2A C3A -7.3(5) . . . . ? C3A O1A C3A C2A -120.2(6) 6_565 . . . ? Ni2 O1A C3A C2A 43.3(8) . . . . ? S1 C2A C3A O1A -21.3(9) . . . . ? Ni1 S3 C4 C4 -2.53(10) . . . 6_565 ? Ni1 S3 C4 S4 178.84(15) . . . . ? C5 S4 C4 C4 101.54(17) . . . 6_565 ? C5 S4 C4 S3 -79.9(2) . . . . ? C4 S4 C5 C6 -85.6(3) . . . . ? C6 O2 C6 C5 -140.2(4) 6_565 . . . ? S4 C5 C6 O2 65.6(5) . . . . ? Ni2 O3 C7 N1 167.7(3) . . . . ? C8 N1 C7 O3 -2.5(7) . . . . ? C9 N1 C7 O3 -173.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.430 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.100 # Attachment '- TBA.cif' data_import3 _database_code_depnum_ccdc_archive 'CCDC 850839' #TrackingRef '- TBA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 N, C12 H16 Ni O2 S8, C3 H7 N O ' _chemical_formula_sum 'C31 H59 N2 Ni O3 S8' _chemical_formula_weight 822.99 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 monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 22.3070(11) _cell_length_b 12.9869(6) _cell_length_c 17.3369(8) _cell_angle_alpha 90.00 _cell_angle_beta 125.516(2) _cell_angle_gamma 90.00 _cell_volume 4088.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3623 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 26.98 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.938 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.722395 #-------------------------------------------------------------------# _diffrn_ambient_temperature 150(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 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11158 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.44 _reflns_number_total 4634 _reflns_number_gt 3515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0787P)^2^+10.3708P] 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 4634 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1636 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Ni Ni 0.0000 0.0000 0.5000 0.02545(18) Uani 1 2 d S . . S1 S -0.11814(5) 0.00355(7) 0.40451(6) 0.0337(2) Uani 1 1 d . . . S2 S -0.23762(5) 0.15637(9) 0.33527(7) 0.0483(3) Uani 1 1 d . . . S3 S -0.10511(6) 0.32669(8) 0.48501(7) 0.0429(3) Uani 1 1 d . . . S4 S 0.00300(4) 0.15799(7) 0.53915(6) 0.0317(2) Uani 1 1 d . . . N1 N 0.0000 0.1373(3) 0.2500 0.0220(7) Uani 1 2 d S . . O1 O -0.1639(2) 0.3012(3) 0.2688(2) 0.0679(10) Uani 1 1 d . . . C1 C -0.14161(19) 0.1298(3) 0.4084(2) 0.0350(8) Uani 1 1 d . . . C2 C -0.2561(3) 0.1670(4) 0.2214(3) 0.0584(12) Uani 1 1 d . . . H2A H -0.2260 0.1177 0.2160 0.070 Uiso 1 1 calc R . . H2B H -0.3073 0.1502 0.1736 0.070 Uiso 1 1 calc R . . C3 C -0.2400(3) 0.2764(4) 0.2030(4) 0.0796(17) Uani 1 1 d . . . H3A H -0.2532 0.2804 0.1390 0.095 Uiso 1 1 calc R . . H3B H -0.2697 0.3259 0.2088 0.095 Uiso 1 1 calc R . . C4 C -0.1502(4) 0.3999(4) 0.3079(5) 0.091(2) Uani 1 1 d . . . H4A H -0.1937 0.4252 0.3017 0.110 Uiso 1 1 calc R . . H4B H -0.1396 0.4462 0.2734 0.110 Uiso 1 1 calc R . . C5 C -0.0854(3) 0.3991(4) 0.4122(5) 0.0727(16) Uani 1 1 d . . . H5A H -0.0730 0.4695 0.4351 0.087 Uiso 1 1 calc R . . H5B H -0.0429 0.3691 0.4186 0.087 Uiso 1 1 calc R . . C6 C -0.08849(19) 0.1983(3) 0.4680(2) 0.0324(7) Uani 1 1 d . . . C7 C -0.02888(16) 0.2034(3) 0.1628(2) 0.0279(7) Uani 1 1 d . . . H7A H -0.0402 0.1587 0.1111 0.034 Uiso 1 1 calc R . . H7B H 0.0102 0.2494 0.1757 0.034 Uiso 1 1 calc R . . C8 C -0.09666(18) 0.2676(3) 0.1300(3) 0.0335(8) Uani 1 1 d . . . H8A H -0.1387 0.2225 0.1062 0.040 Uiso 1 1 calc R . . H8B H -0.0888 0.3057 0.1833 0.040 Uiso 1 1 calc R . . C9 C -0.1127(2) 0.3417(4) 0.0533(3) 0.0571(12) Uani 1 1 d . . . H9A H -0.1202 0.3032 0.0004 0.068 Uiso 1 1 calc R . . H9B H -0.0705 0.3863 0.0774 0.068 Uiso 1 1 calc R . . C10 C -0.1804(2) 0.4074(4) 0.0185(4) 0.0648(14) Uani 1 1 d . . . H10A H -0.2233 0.3643 -0.0121 0.097 Uiso 1 1 calc R . . H10B H -0.1858 0.4577 -0.0258 0.097 Uiso 1 1 calc R . . H10C H -0.1748 0.4418 0.0714 0.097 Uiso 1 1 calc R . . C11 C -0.06090(15) 0.0706(2) 0.2386(2) 0.0228(6) Uani 1 1 d . . . H11A H -0.0398 0.0287 0.2950 0.027 Uiso 1 1 calc R . . H11B H -0.0973 0.1154 0.2348 0.027 Uiso 1 1 calc R . . C12 C -0.10005(17) -0.0002(2) 0.1527(2) 0.0260(6) Uani 1 1 d . . . H12A H -0.0643 -0.0434 0.1534 0.031 Uiso 1 1 calc R . . H12B H -0.1255 0.0406 0.0951 0.031 Uiso 1 1 calc R . . C13 C -0.15552(17) -0.0676(3) 0.1546(2) 0.0283(7) Uani 1 1 d . . . H13A H -0.1294 -0.1106 0.2108 0.034 Uiso 1 1 calc R . . H13B H -0.1891 -0.0239 0.1581 0.034 Uiso 1 1 calc R . . C14 C -0.19923(19) -0.1356(3) 0.0675(3) 0.0355(8) Uani 1 1 d . . . H14A H -0.2239 -0.0934 0.0116 0.053 Uiso 1 1 calc R . . H14B H -0.2350 -0.1741 0.0696 0.053 Uiso 1 1 calc R . . H14C H -0.1665 -0.1822 0.0661 0.053 Uiso 1 1 calc R . . N1A N 0.0000 0.3742(4) 0.7500 0.0537(13) Uani 1 2 d S . . O1A O -0.0146(6) 0.5364(6) 0.7761(9) 0.117(5) Uani 0.50 1 d P . . C2A C -0.0258(8) 0.2743(9) 0.7412(11) 0.091(5) Uani 0.50 1 d P . . H2A1 H -0.0600 0.2730 0.7578 0.136 Uiso 0.50 1 calc PR . . H2A2 H 0.0149 0.2295 0.7827 0.136 Uiso 0.50 1 calc PR . . H2A3 H -0.0500 0.2515 0.6769 0.136 Uiso 0.50 1 calc PR . . C1A C -0.0291(8) 0.4541(12) 0.7441(15) 0.183(13) Uani 0.50 1 d P . . H1A H -0.0798 0.4484 0.6995 0.220 Uiso 0.50 1 calc PR . . C3A C -0.0753(6) 0.3705(11) 0.7310(9) 0.080(3) Uani 0.50 1 d P . . H3A1 H -0.0868 0.3008 0.7364 0.121 Uiso 0.50 1 calc PR . . H3A2 H -0.1115 0.3955 0.6682 0.121 Uiso 0.50 1 calc PR . . H3A3 H -0.0754 0.4129 0.7763 0.121 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0282(3) 0.0281(3) 0.0216(3) -0.0028(2) 0.0154(2) -0.0007(2) S1 0.0293(4) 0.0360(5) 0.0316(4) -0.0101(4) 0.0154(4) -0.0020(3) S2 0.0319(5) 0.0582(7) 0.0466(6) -0.0071(5) 0.0180(4) 0.0074(4) S3 0.0489(5) 0.0372(5) 0.0481(6) -0.0084(4) 0.0313(5) 0.0064(4) S4 0.0321(4) 0.0310(5) 0.0304(4) -0.0072(4) 0.0172(4) -0.0015(3) N1 0.0184(16) 0.0244(18) 0.0218(17) 0.000 0.0109(14) 0.000 O1 0.100(3) 0.054(2) 0.066(2) 0.0108(17) 0.058(2) 0.0252(19) C1 0.0316(16) 0.042(2) 0.0326(17) -0.0047(16) 0.0192(15) 0.0046(15) C2 0.055(3) 0.076(3) 0.038(2) 0.002(2) 0.023(2) 0.014(2) C3 0.084(4) 0.079(4) 0.059(3) 0.029(3) 0.032(3) 0.041(3) C4 0.144(6) 0.055(3) 0.092(4) 0.027(3) 0.077(5) 0.017(4) C5 0.086(4) 0.041(3) 0.129(5) -0.004(3) 0.084(4) 0.001(2) C6 0.0360(17) 0.0357(19) 0.0292(16) -0.0037(15) 0.0211(15) 0.0050(15) C7 0.0243(14) 0.0277(16) 0.0300(16) 0.0067(13) 0.0148(13) -0.0009(12) C8 0.0265(16) 0.0296(18) 0.0399(19) 0.0078(15) 0.0167(15) 0.0049(13) C9 0.041(2) 0.063(3) 0.066(3) 0.038(2) 0.031(2) 0.019(2) C10 0.049(2) 0.059(3) 0.071(3) 0.032(3) 0.026(2) 0.025(2) C11 0.0197(13) 0.0249(15) 0.0252(14) -0.0008(12) 0.0138(12) -0.0023(11) C12 0.0274(15) 0.0276(17) 0.0242(15) -0.0019(13) 0.0157(13) -0.0036(12) C13 0.0296(15) 0.0259(16) 0.0313(16) -0.0030(14) 0.0188(14) -0.0044(13) C14 0.0347(17) 0.0351(19) 0.0395(19) -0.0120(16) 0.0231(16) -0.0122(15) N1A 0.054(3) 0.049(3) 0.037(3) 0.000 0.014(2) 0.000 O1A 0.084(7) 0.041(4) 0.174(13) 0.007(6) 0.046(6) -0.003(4) C2A 0.137(15) 0.082(7) 0.063(7) -0.017(8) 0.064(12) -0.058(8) C1A 0.077(9) 0.072(9) 0.198(19) -0.060(12) -0.036(12) 0.043(8) C3A 0.077(7) 0.102(9) 0.086(8) 0.021(7) 0.061(7) 0.025(7) _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 S1 2.1492(9) 5_556 ? Ni S1 2.1492(9) . ? Ni S4 2.1500(8) 5_556 ? Ni S4 2.1500(8) . ? S1 C1 1.734(4) . ? S2 C2 1.772(4) . ? S2 C1 1.777(4) . ? S3 C6 1.770(3) . ? S3 C5 1.821(5) . ? S4 C6 1.742(3) . ? N1 C7 1.518(4) 2 ? N1 C7 1.518(4) . ? N1 C11 1.524(3) . ? N1 C11 1.524(3) 2 ? O1 C4 1.398(7) . ? O1 C3 1.426(7) . ? C1 C6 1.356(5) . ? C2 C3 1.544(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.525(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C8 1.519(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.507(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.521(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.520(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.531(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.516(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? N1A C1A 1.198(13) 2_556 ? N1A C1A 1.198(13) . ? N1A C2A 1.390(11) . ? N1A C2A 1.390(11) 2_556 ? N1A C3A 1.513(11) 2_556 ? N1A C3A 1.513(11) . ? O1A C1A 1.160(15) . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C2A H2A3 0.9600 . ? C1A H1A 0.9300 . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? 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 S1 Ni S1 180.00(3) 5_556 . ? S1 Ni S4 91.26(3) 5_556 5_556 ? S1 Ni S4 88.74(3) . 5_556 ? S1 Ni S4 88.74(3) 5_556 . ? S1 Ni S4 91.26(3) . . ? S4 Ni S4 180.0 5_556 . ? C1 S1 Ni 104.66(12) . . ? C2 S2 C1 102.4(2) . . ? C6 S3 C5 102.3(2) . . ? C6 S4 Ni 104.73(12) . . ? C7 N1 C7 111.2(3) 2 . ? C7 N1 C11 106.33(16) 2 . ? C7 N1 C11 111.18(16) . . ? C7 N1 C11 111.18(16) 2 2 ? C7 N1 C11 106.33(16) . 2 ? C11 N1 C11 110.7(3) . 2 ? C4 O1 C3 114.8(5) . . ? C6 C1 S1 120.0(3) . . ? C6 C1 S2 125.0(3) . . ? S1 C1 S2 114.9(2) . . ? C3 C2 S2 111.8(4) . . ? C3 C2 H2A 109.3 . . ? S2 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? S2 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? O1 C3 C2 110.7(4) . . ? O1 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O1 C4 C5 111.0(5) . . ? O1 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? O1 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 S3 112.4(4) . . ? C4 C5 H5A 109.1 . . ? S3 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? S3 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C1 C6 S4 119.2(3) . . ? C1 C6 S3 124.7(3) . . ? S4 C6 S3 116.0(2) . . ? N1 C7 C8 115.9(2) . . ? N1 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C7 110.8(3) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 112.4(4) . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N1 115.6(2) . . ? C12 C11 H11A 108.4 . . ? N1 C11 H11A 108.4 . . ? C12 C11 H11B 108.4 . . ? N1 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? C11 C12 C13 109.7(3) . . ? C11 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C14 C13 C12 111.8(3) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1A N1A C1A 60(2) 2_556 . ? C1A N1A C2A 170.8(15) 2_556 . ? C1A N1A C2A 129.1(12) . . ? C1A N1A C2A 129.1(12) 2_556 2_556 ? C1A N1A C2A 170.8(15) . 2_556 ? C1A N1A C3A 61.9(11) 2_556 2_556 ? C1A N1A C3A 121.7(14) . 2_556 ? C2A N1A C3A 109.3(9) . 2_556 ? C2A N1A C3A 67.1(7) 2_556 2_556 ? C1A N1A C3A 121.7(14) 2_556 . ? C1A N1A C3A 61.9(11) . . ? C2A N1A C3A 67.1(7) . . ? C2A N1A C3A 109.3(9) 2_556 . ? C3A N1A C3A 176.4(11) 2_556 . ? N1A C2A H2A1 109.5 . . ? N1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? N1A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? O1A C1A N1A 140.4(13) . . ? O1A C1A H1A 109.8 . . ? N1A C1A H1A 109.8 . . ? N1A C3A H3A1 109.5 . . ? N1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S4 Ni S1 C1 -176.46(13) 5_556 . . . ? S4 Ni S1 C1 3.54(13) . . . . ? S1 Ni S4 C6 176.68(12) 5_556 . . . ? S1 Ni S4 C6 -3.32(12) . . . . ? Ni S1 C1 C6 -3.2(3) . . . . ? Ni S1 C1 S2 -179.94(16) . . . . ? C2 S2 C1 C6 105.2(4) . . . . ? C2 S2 C1 S1 -78.3(3) . . . . ? C1 S2 C2 C3 -84.9(4) . . . . ? C4 O1 C3 C2 -135.7(5) . . . . ? S2 C2 C3 O1 62.3(5) . . . . ? C3 O1 C4 C5 141.7(5) . . . . ? O1 C4 C5 S3 -66.2(6) . . . . ? C6 S3 C5 C4 82.0(4) . . . . ? S1 C1 C6 S4 0.6(4) . . . . ? S2 C1 C6 S4 177.0(2) . . . . ? S1 C1 C6 S3 -175.6(2) . . . . ? S2 C1 C6 S3 0.8(5) . . . . ? Ni S4 C6 C1 2.4(3) . . . . ? Ni S4 C6 S3 178.85(15) . . . . ? C5 S3 C6 C1 -100.5(4) . . . . ? C5 S3 C6 S4 83.3(3) . . . . ? C7 N1 C7 C8 -66.0(3) 2 . . . ? C11 N1 C7 C8 52.3(4) . . . . ? C11 N1 C7 C8 172.9(3) 2 . . . ? N1 C7 C8 C9 171.0(3) . . . . ? C7 C8 C9 C10 179.9(4) . . . . ? C7 N1 C11 C12 178.0(3) 2 . . . ? C7 N1 C11 C12 56.9(3) . . . . ? C11 N1 C11 C12 -61.1(2) 2 . . . ? N1 C11 C12 C13 175.9(3) . . . . ? C11 C12 C13 C14 176.8(3) . . . . ? C1A N1A C1A O1A -37(3) 2_556 . . . ? C3A N1A C1A O1A -35(5) 2_556 . . . ? C3A N1A C1A O1A 145(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.531 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.131