Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Verhagen, Johanna A.W.' ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden The Netherlands ; 'Ellis, Dianne D.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Spek, Anthony L.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Bouwman, Elisabeth' ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden The Netherlands ; _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Dr Elisabeth Bouwman' _publ_contact_author_address ; Leiden Institute of Chemistry Leiden University Gorlaeus Laboratories PO Box 9502 Leiden 2300 RA NETHERLANDS ; _publ_contact_author_email BOUWMAN@CHEM.LEIDENUNIV.NL _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' _publ_section_title ; Synthesis, characterisation and crystal structures of new nickel complexes in S~4~ coordination spheres; an unpredicted rearrangement during ligand synthesis ; data_s2323a _database_code_CSD 174229 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 Ni S4' _chemical_formula_sum 'C22 H30 Ni S4' _chemical_formula_weight 481.41 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' 'Ni' 'Ni' 0.3393 1.1124 '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' _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 7.1006(2) _cell_length_b 8.3936(2) _cell_length_c 10.4298(4) _cell_angle_alpha 108.6417(16) _cell_angle_beta 105.6636(17) _cell_angle_gamma 89.9694(19) _cell_volume 564.61(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagons _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 254 _exptl_absorpt_coefficient_mu 1.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7560 _exptl_absorpt_correction_T_max 0.8084 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 6230 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2670 _reflns_number_gt 2283 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DENZO 1.11' _computing_data_reduction 'DENZO 1.11' _computing_structure_solution 'DIRDIF-99 (Beurskens, et al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'PLATON (Spek, 2000)' _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^)+(0.0186P)^2^+0.1845P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 2670 _refine_ls_number_parameters 126 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.5000 0.5000 0.01367(10) Uani 1 2 d S . . S6 S -0.12639(7) 0.26301(5) 0.50178(5) 0.01826(12) Uani 1 1 d . . . S9 S 0.08945(6) 0.35403(5) 0.31656(4) 0.01565(11) Uani 1 1 d . . . C4 C 0.3075(3) 0.1650(2) 0.4732(2) 0.0264(4) Uani 1 1 d . . . H4A H 0.2865 0.2530 0.5549 0.040 Uiso 1 1 calc R . . H4B H 0.4300 0.1960 0.4569 0.040 Uiso 1 1 calc R . . H4C H 0.3163 0.0573 0.4914 0.040 Uiso 1 1 calc R . . C5 C 0.1710(3) 0.0219(2) 0.2114(2) 0.0304(5) Uani 1 1 d . . . H5A H 0.1840 -0.0893 0.2230 0.046 Uiso 1 1 calc R . . H5B H 0.2915 0.0601 0.1969 0.046 Uiso 1 1 calc R . . H5C H 0.0594 0.0142 0.1295 0.046 Uiso 1 1 calc R . . C7 C -0.0597(3) 0.1008(2) 0.36080(18) 0.0186(4) Uani 1 1 d . . . H7A H -0.0535 -0.0066 0.3815 0.022 Uiso 1 1 calc R . . H7B H -0.1634 0.0822 0.2708 0.022 Uiso 1 1 calc R . . C8 C 0.1366(3) 0.1476(2) 0.34338(18) 0.0186(4) Uani 1 1 d . . . C10 C 0.3217(3) 0.4352(2) 0.30735(18) 0.0194(4) Uani 1 1 d . . . H10A H 0.3268 0.5599 0.3359 0.023 Uiso 1 1 calc R . . H10B H 0.4307 0.4063 0.3759 0.023 Uiso 1 1 calc R . . C11 C 0.3532(3) 0.3677(2) 0.16346(18) 0.0168(4) Uani 1 1 d . . . C12 C 0.5325(3) 0.3105(2) 0.15109(19) 0.0246(4) Uani 1 1 d . . . H12 H 0.6309 0.3082 0.2327 0.029 Uiso 1 1 calc R . . C13 C 0.5699(3) 0.2564(3) 0.0212(2) 0.0336(5) Uani 1 1 d . . . H13 H 0.6939 0.2181 0.0143 0.040 Uiso 1 1 calc R . . C14 C 0.4282(3) 0.2581(3) -0.0983(2) 0.0320(5) Uani 1 1 d . . . H14 H 0.4539 0.2205 -0.1875 0.038 Uiso 1 1 calc R . . C15 C 0.2489(3) 0.3146(3) -0.0876(2) 0.0305(5) Uani 1 1 d . . . H15 H 0.1511 0.3167 -0.1696 0.037 Uiso 1 1 calc R . . C16 C 0.2109(3) 0.3683(2) 0.0425(2) 0.0249(4) Uani 1 1 d . . . H16 H 0.0864 0.4059 0.0490 0.030 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 0.01461(18) 0.01249(16) 0.01479(16) 0.00388(12) 0.00640(12) 0.00271(12) S6 0.0217(2) 0.0140(2) 0.0224(2) 0.00525(18) 0.01247(18) 0.00281(18) S9 0.0164(2) 0.0158(2) 0.0154(2) 0.00393(17) 0.00691(17) 0.00211(17) C4 0.0190(10) 0.0248(10) 0.0388(11) 0.0158(9) 0.0075(8) 0.0065(8) C5 0.0408(13) 0.0187(9) 0.0368(12) 0.0032(9) 0.0264(10) 0.0047(9) C7 0.0188(10) 0.0137(8) 0.0209(9) 0.0026(7) 0.0057(7) 0.0031(7) C8 0.0204(10) 0.0138(8) 0.0230(9) 0.0053(7) 0.0092(7) 0.0044(7) C10 0.0173(9) 0.0204(9) 0.0199(9) 0.0035(7) 0.0082(7) -0.0025(7) C11 0.0184(9) 0.0151(8) 0.0181(9) 0.0060(7) 0.0064(7) 0.0009(7) C12 0.0202(10) 0.0316(10) 0.0208(9) 0.0063(8) 0.0069(8) 0.0048(8) C13 0.0287(12) 0.0413(12) 0.0291(11) 0.0031(10) 0.0159(9) 0.0060(10) C14 0.0421(13) 0.0349(11) 0.0181(10) 0.0017(9) 0.0157(9) -0.0050(10) C15 0.0353(12) 0.0359(11) 0.0193(10) 0.0114(9) 0.0034(8) -0.0005(10) C16 0.0226(10) 0.0312(10) 0.0244(10) 0.0134(8) 0.0073(8) 0.0071(8) _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 S9 2.1730(4) 2_566 ? Ni1 S9 2.1730(4) . y Ni1 S6 2.1903(4) . y Ni1 S6 2.1903(4) 2_566 ? S6 C7 1.8264(17) . y S9 C10 1.8226(18) . y S9 C8 1.8581(18) . y C4 C8 1.521(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.523(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.521(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C10 C11 1.504(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.384(3) . ? C11 C16 1.389(2) . ? C12 C13 1.384(3) . ? C12 H12 0.9500 . ? C13 C14 1.378(3) . ? C13 H13 0.9500 . ? C14 C15 1.379(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S9 Ni1 S9 180.0 2_566 . ? S9 Ni1 S6 91.874(16) 2_566 . ? S9 Ni1 S6 88.127(16) . . ? S9 Ni1 S6 88.127(16) 2_566 2_566 ? S9 Ni1 S6 91.873(16) . 2_566 ? S6 Ni1 S6 180.0 . 2_566 ? C7 S6 Ni1 104.05(6) . . ? C10 S9 C8 105.17(9) . . ? C10 S9 Ni1 114.51(6) . . ? C8 S9 Ni1 103.97(6) . . ? C8 C4 H4A 109.5 . . ? C8 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C8 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 H5A 109.5 . . ? C8 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C8 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C8 C7 S6 112.74(12) . . ? C8 C7 H7A 109.0 . . ? S6 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? S6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C4 C8 C7 112.69(15) . . ? C4 C8 C5 111.27(16) . . ? C7 C8 C5 110.64(15) . . ? C4 C8 S9 111.88(12) . . ? C7 C8 S9 99.98(11) . . ? C5 C8 S9 109.87(13) . . ? C11 C10 S9 113.90(12) . . ? C11 C10 H10A 108.8 . . ? S9 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? S9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 118.65(17) . . ? C12 C11 C10 119.34(16) . . ? C16 C11 C10 121.94(16) . . ? C13 C12 C11 120.75(18) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.27(19) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.64(18) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 120.17(18) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.53(18) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? 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 S9 Ni1 S6 C7 -175.92(6) 2_566 . . . ? S9 Ni1 S6 C7 4.08(6) . . . . ? S6 Ni1 S9 C10 -145.45(7) . . . . ? S6 Ni1 S9 C10 34.55(7) 2_566 . . . ? S6 Ni1 S9 C8 -31.25(6) . . . . ? S6 Ni1 S9 C8 148.75(6) 2_566 . . . ? Ni1 S6 C7 C8 32.33(13) . . . . ? S6 C7 C8 C4 63.26(17) . . . . ? S6 C7 C8 C5 -171.46(12) . . . . ? S6 C7 C8 S9 -55.67(13) . . . . ? C10 S9 C8 C4 56.22(15) . . . . ? Ni1 S9 C8 C4 -64.47(13) . . . . ? C10 S9 C8 C7 175.74(11) . . . . ? Ni1 S9 C8 C7 55.04(11) . . . . ? C10 S9 C8 C5 -67.89(14) . . . . ? Ni1 S9 C8 C5 171.42(12) . . . . ? C8 S9 C10 C11 83.69(14) . . . . ? Ni1 S9 C10 C11 -162.82(11) . . . . ? S9 C10 C11 C12 -133.63(16) . . . . ? S9 C10 C11 C16 49.5(2) . . . . ? C16 C11 C12 C13 0.6(3) . . . . ? C10 C11 C12 C13 -176.36(18) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C13 C14 C15 C16 -0.5(3) . . . . ? C14 C15 C16 C11 0.7(3) . . . . ? C12 C11 C16 C15 -0.8(3) . . . . ? C10 C11 C16 C15 176.09(18) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.399 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.076 #===END data_s2399a _database_code_CSD 174230 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 Ni S4' _chemical_formula_sum 'C16 H24 Ni S4' _chemical_formula_weight 403.30 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' 'Ni' 'Ni' 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.2008(2) _cell_length_b 17.3926(2) _cell_length_c 20.6855(2) _cell_angle_alpha 90.00 _cell_angle_beta 129.5047(7) _cell_angle_gamma 90.00 _cell_volume 3664.44(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 114536 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.506 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 65338 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8398 _reflns_number_gt 6460 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0303P)^2^+0.9355P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8398 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _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 0.41106(2) 0.091099(15) 0.248580(15) 0.02055(7) Uani 1 1 d . . . C4 C 0.4740(2) 0.28306(13) 0.22452(13) 0.0318(5) Uani 1 1 d . . . H4A H 0.4881 0.2568 0.2716 0.048 Uiso 1 1 calc R . . H4B H 0.3936 0.3139 0.1943 0.048 Uiso 1 1 calc R . . H4C H 0.5488 0.3167 0.2457 0.048 Uiso 1 1 calc R . . C5 C 0.4299(2) 0.26262(13) 0.08852(14) 0.0342(5) Uani 1 1 d . . . H5A H 0.4979 0.3007 0.1064 0.051 Uiso 1 1 calc R . . H5B H 0.3444 0.2882 0.0565 0.051 Uiso 1 1 calc R . . H5C H 0.4277 0.2238 0.0532 0.051 Uiso 1 1 calc R . . S6 S 0.60666(5) 0.11106(3) 0.28860(3) 0.02855(13) Uani 1 1 d . . . C7 C 0.5812(2) 0.17254(13) 0.20800(13) 0.0286(5) Uani 1 1 d . . . H7A H 0.6597 0.2053 0.2337 0.034 Uiso 1 1 calc R . . H7B H 0.5715 0.1399 0.1651 0.034 Uiso 1 1 calc R . . C8 C 0.4607(2) 0.22375(12) 0.16549(12) 0.0254(5) Uani 1 1 d . . . S9 S 0.33163(5) 0.15157(3) 0.13205(3) 0.02255(12) Uani 1 1 d . . . C10 C 0.18659(19) 0.21133(12) 0.08853(13) 0.0282(5) Uani 1 1 d . . . H10A H 0.1949 0.2367 0.1345 0.034 Uiso 1 1 calc R . . H10B H 0.1797 0.2518 0.0522 0.034 Uiso 1 1 calc R . . C14 C 0.3121(2) 0.12892(13) 0.37054(13) 0.0318(5) Uani 1 1 d . . . H14A H 0.3449 0.1226 0.4281 0.048 Uiso 1 1 calc R . . H14B H 0.2348 0.1625 0.3395 0.048 Uiso 1 1 calc R . . H14C H 0.3808 0.1520 0.3715 0.048 Uiso 1 1 calc R . . C15 C 0.1600(2) 0.01570(13) 0.31877(13) 0.0321(5) Uani 1 1 d . . . H15A H 0.1305 -0.0312 0.2849 0.048 Uiso 1 1 calc R . . H15B H 0.0875 0.0527 0.2912 0.048 Uiso 1 1 calc R . . H15C H 0.1884 0.0031 0.3743 0.048 Uiso 1 1 calc R . . S16 S 0.51671(5) 0.02834(3) 0.36687(3) 0.03164(14) Uani 1 1 d . . . C17 C 0.3900(2) -0.00503(13) 0.37081(13) 0.0288(5) Uani 1 1 d . . . H17A H 0.3577 -0.0558 0.3431 0.035 Uiso 1 1 calc R . . H17B H 0.4285 -0.0115 0.4300 0.035 Uiso 1 1 calc R . . C18 C 0.27463(19) 0.05079(12) 0.32799(12) 0.0239(5) Uani 1 1 d . . . S19 S 0.23074(5) 0.05626(3) 0.22355(3) 0.02103(11) Uani 1 1 d . . . C20 C 0.09807(19) 0.12601(13) 0.16888(12) 0.0261(5) Uani 1 1 d . . . H20A H 0.0375 0.1159 0.1808 0.031 Uiso 1 1 calc R . . H20B H 0.1342 0.1785 0.1887 0.031 Uiso 1 1 calc R . . C21 C 0.06540(19) 0.16167(11) 0.03825(12) 0.0233(4) Uani 1 1 d . . . C22 C 0.02483(19) 0.12032(12) 0.07629(12) 0.0233(4) Uani 1 1 d . . . C23 C -0.0856(2) 0.07399(13) 0.02733(13) 0.0294(5) Uani 1 1 d . . . H23 H -0.1115 0.0444 0.0533 0.035 Uiso 1 1 calc R . . C24 C -0.1587(2) 0.07009(14) -0.05848(14) 0.0346(5) Uani 1 1 d . . . H24 H -0.2345 0.0383 -0.0913 0.041 Uiso 1 1 calc R . . C25 C -0.1209(2) 0.11284(14) -0.09639(14) 0.0349(5) Uani 1 1 d . . . H25 H -0.1714 0.1112 -0.1555 0.042 Uiso 1 1 calc R . . C26 C -0.0097(2) 0.15783(12) -0.04811(13) 0.0292(5) Uani 1 1 d . . . H26 H 0.0161 0.1868 -0.0745 0.035 Uiso 1 1 calc R . . Ni31 Ni 0.03529(2) 0.313665(15) 0.222352(15) 0.02179(7) Uani 1 1 d . . . C34 C 0.2182(2) 0.49733(13) 0.33679(13) 0.0379(6) Uani 1 1 d . . . H34A H 0.1324 0.4818 0.3190 0.057 Uiso 1 1 calc R . . H34B H 0.2060 0.5356 0.2976 0.057 Uiso 1 1 calc R . . H34C H 0.2710 0.5196 0.3931 0.057 Uiso 1 1 calc R . . C35 C 0.4203(2) 0.44908(14) 0.36119(14) 0.0378(6) Uani 1 1 d . . . H35A H 0.4766 0.4724 0.4171 0.057 Uiso 1 1 calc R . . H35B H 0.4058 0.4859 0.3202 0.057 Uiso 1 1 calc R . . H35C H 0.4629 0.4029 0.3613 0.057 Uiso 1 1 calc R . . S36 S 0.14795(6) 0.32343(4) 0.35689(3) 0.03694(15) Uani 1 1 d . . . C37 C 0.3037(2) 0.36362(14) 0.39423(13) 0.0331(5) Uani 1 1 d . . . H37A H 0.3502 0.3845 0.4513 0.040 Uiso 1 1 calc R . . H37B H 0.3585 0.3220 0.3981 0.040 Uiso 1 1 calc R . . C38 C 0.2886(2) 0.42720(12) 0.33788(12) 0.0271(5) Uani 1 1 d . . . S39 S 0.18880(5) 0.37758(3) 0.23447(3) 0.02135(11) Uani 1 1 d . . . C40 C 0.1292(2) 0.45667(11) 0.15975(12) 0.0226(4) Uani 1 1 d . . . H40A H 0.0491 0.4792 0.1467 0.027 Uiso 1 1 calc R . . H40B H 0.1969 0.4974 0.1846 0.027 Uiso 1 1 calc R . . C44 C -0.3182(2) 0.33690(12) 0.06099(14) 0.0289(5) Uani 1 1 d . . . H44A H -0.3322 0.3779 0.0236 0.043 Uiso 1 1 calc R . . H44B H -0.2612 0.3558 0.1188 0.043 Uiso 1 1 calc R . . H44C H -0.4028 0.3211 0.0448 0.043 Uiso 1 1 calc R . . C45 C -0.3386(2) 0.23769(13) -0.03470(13) 0.0331(5) Uani 1 1 d . . . H45A H -0.4214 0.2182 -0.0507 0.050 Uiso 1 1 calc R . . H45B H -0.2920 0.1959 -0.0377 0.050 Uiso 1 1 calc R . . H45C H -0.3568 0.2790 -0.0731 0.050 Uiso 1 1 calc R . . S46 S -0.08983(6) 0.23494(4) 0.22628(4) 0.03549(15) Uani 1 1 d . . . C47 C -0.2169(2) 0.20584(12) 0.11751(13) 0.0294(5) Uani 1 1 d . . . H47A H -0.1858 0.1602 0.1059 0.035 Uiso 1 1 calc R . . H47B H -0.2963 0.1906 0.1097 0.035 Uiso 1 1 calc R . . C48 C -0.2538(2) 0.26874(12) 0.05441(13) 0.0242(5) Uani 1 1 d . . . S49 S -0.09065(5) 0.29471(3) 0.08716(3) 0.02044(11) Uani 1 1 d . . . C50 C -0.12552(19) 0.38057(11) 0.02499(12) 0.0212(4) Uani 1 1 d . . . H50A H -0.2119 0.3752 -0.0316 0.025 Uiso 1 1 calc R . . H50B H -0.1288 0.4263 0.0521 0.025 Uiso 1 1 calc R . . C51 C 0.09879(19) 0.42716(11) 0.08082(12) 0.0198(4) Uani 1 1 d . . . C52 C -0.01974(19) 0.39076(11) 0.01796(12) 0.0193(4) Uani 1 1 d . . . C53 C -0.0400(2) 0.36301(11) -0.05260(12) 0.0230(4) Uani 1 1 d . . . H53 H -0.1197 0.3372 -0.0950 0.028 Uiso 1 1 calc R . . C54 C 0.0545(2) 0.37249(12) -0.06201(13) 0.0260(5) Uani 1 1 d . . . H54 H 0.0392 0.3538 -0.1107 0.031 Uiso 1 1 calc R . . C55 C 0.1709(2) 0.40937(12) 0.00003(13) 0.0261(5) Uani 1 1 d . . . H55 H 0.2356 0.4165 -0.0062 0.031 Uiso 1 1 calc R . . C56 C 0.1933(2) 0.43585(12) 0.07119(12) 0.0238(4) Uani 1 1 d . . . H56 H 0.2743 0.4603 0.1140 0.029 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 0.01882(14) 0.02121(15) 0.02516(14) 0.00173(11) 0.01564(12) 0.00205(11) C4 0.0312(13) 0.0278(13) 0.0383(13) -0.0025(10) 0.0230(12) -0.0033(10) C5 0.0354(13) 0.0355(14) 0.0418(13) 0.0084(11) 0.0293(12) 0.0016(11) S6 0.0198(3) 0.0333(3) 0.0333(3) 0.0062(2) 0.0172(3) 0.0024(2) C7 0.0274(12) 0.0316(13) 0.0363(12) 0.0018(10) 0.0247(11) -0.0009(10) C8 0.0260(12) 0.0247(12) 0.0305(11) 0.0008(9) 0.0203(10) -0.0036(9) S9 0.0225(3) 0.0214(3) 0.0275(3) 0.0013(2) 0.0176(2) 0.0013(2) C10 0.0253(12) 0.0224(12) 0.0347(12) 0.0055(10) 0.0181(11) 0.0057(10) C14 0.0311(13) 0.0379(14) 0.0312(12) -0.0069(10) 0.0221(11) -0.0021(11) C15 0.0275(12) 0.0422(14) 0.0348(12) 0.0024(11) 0.0237(11) -0.0015(11) S16 0.0211(3) 0.0425(4) 0.0329(3) 0.0131(3) 0.0179(3) 0.0075(3) C17 0.0254(12) 0.0342(13) 0.0295(11) 0.0068(10) 0.0188(10) 0.0023(10) C18 0.0254(11) 0.0292(12) 0.0226(10) 0.0015(9) 0.0179(10) 0.0003(10) S19 0.0203(3) 0.0225(3) 0.0237(3) 0.0000(2) 0.0156(2) 0.0011(2) C20 0.0219(11) 0.0300(12) 0.0279(11) 0.0013(9) 0.0165(10) 0.0066(10) C21 0.0214(11) 0.0194(11) 0.0294(11) 0.0007(9) 0.0164(10) 0.0042(9) C22 0.0210(11) 0.0221(11) 0.0283(11) 0.0009(9) 0.0163(10) 0.0061(9) C23 0.0275(12) 0.0291(13) 0.0376(13) 0.0004(10) 0.0236(11) 0.0006(10) C24 0.0278(13) 0.0326(14) 0.0379(13) -0.0098(11) 0.0183(11) -0.0033(11) C25 0.0341(13) 0.0376(14) 0.0266(12) -0.0057(10) 0.0164(11) 0.0035(11) C26 0.0350(13) 0.0274(12) 0.0315(12) 0.0032(10) 0.0241(11) 0.0056(10) Ni31 0.02421(15) 0.02201(15) 0.02433(14) 0.00430(11) 0.01786(13) 0.00253(12) C34 0.0405(14) 0.0335(14) 0.0287(12) -0.0070(10) 0.0170(11) 0.0047(11) C35 0.0283(13) 0.0399(15) 0.0313(12) 0.0010(11) 0.0124(11) -0.0044(11) S36 0.0370(3) 0.0531(4) 0.0265(3) 0.0035(3) 0.0229(3) -0.0027(3) C37 0.0311(13) 0.0383(14) 0.0252(11) 0.0022(10) 0.0157(11) 0.0021(11) C38 0.0249(12) 0.0277(12) 0.0206(10) -0.0018(9) 0.0108(10) 0.0002(10) S39 0.0231(3) 0.0200(3) 0.0232(3) 0.0015(2) 0.0158(2) 0.0015(2) C40 0.0248(11) 0.0174(11) 0.0250(10) 0.0030(9) 0.0155(10) -0.0001(9) C44 0.0263(12) 0.0280(12) 0.0402(13) 0.0026(10) 0.0248(11) 0.0023(10) C45 0.0276(13) 0.0342(14) 0.0373(13) -0.0065(11) 0.0206(11) -0.0099(10) S46 0.0378(3) 0.0405(4) 0.0355(3) 0.0080(3) 0.0268(3) -0.0052(3) C47 0.0301(12) 0.0250(12) 0.0403(13) 0.0014(10) 0.0257(11) -0.0037(10) C48 0.0228(11) 0.0210(11) 0.0353(12) -0.0015(9) 0.0216(10) -0.0036(9) S49 0.0217(3) 0.0187(3) 0.0263(3) 0.0020(2) 0.0178(2) 0.0006(2) C50 0.0208(11) 0.0196(11) 0.0233(10) 0.0044(9) 0.0141(9) 0.0006(9) C51 0.0228(11) 0.0156(10) 0.0231(10) 0.0045(8) 0.0155(9) 0.0011(9) C52 0.0197(11) 0.0161(10) 0.0229(10) 0.0061(8) 0.0139(9) 0.0034(8) C53 0.0232(11) 0.0210(11) 0.0210(10) 0.0028(9) 0.0123(10) 0.0000(9) C54 0.0349(13) 0.0244(11) 0.0262(11) 0.0068(9) 0.0230(11) 0.0059(10) C55 0.0295(12) 0.0247(12) 0.0358(12) 0.0103(10) 0.0261(11) 0.0061(10) C56 0.0217(11) 0.0200(11) 0.0296(11) 0.0054(9) 0.0163(10) -0.0004(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 S19 2.1756(5) . ? Ni1 S6 2.1802(6) . ? Ni1 S16 2.1869(6) . ? Ni1 S9 2.1909(5) . ? C4 C8 1.521(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.528(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? S6 C7 1.823(2) . ? C7 C8 1.522(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 S9 1.860(2) . ? S9 C10 1.834(2) . ? C10 C21 1.507(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C14 C18 1.521(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C18 1.527(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? S16 C17 1.821(2) . ? C17 C18 1.527(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 S19 1.8492(18) . ? S19 C20 1.816(2) . ? C20 C22 1.502(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.388(3) . ? C21 C22 1.400(3) . ? C22 C23 1.387(3) . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 C26 1.378(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? Ni31 S36 2.1725(6) . ? Ni31 S39 2.1814(5) . ? Ni31 S49 2.1858(5) . ? Ni31 S46 2.1864(6) . ? C34 C38 1.525(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C38 1.528(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? S36 C37 1.814(2) . ? C37 C38 1.525(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 S39 1.863(2) . ? S39 C40 1.8310(19) . ? C40 C51 1.502(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C44 C48 1.514(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48 1.522(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? S46 C47 1.825(2) . ? C47 C48 1.526(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 S49 1.8566(19) . ? S49 C50 1.8283(19) . ? C50 C52 1.504(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C56 1.392(3) . ? C51 C52 1.397(3) . ? C52 C53 1.392(3) . ? C53 C54 1.389(3) . ? C53 H53 0.9500 . ? C54 C55 1.383(3) . ? C54 H54 0.9500 . ? C55 C56 1.383(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S19 Ni1 S6 170.72(2) . . ? S19 Ni1 S16 87.11(2) . . ? S6 Ni1 S16 84.05(2) . . ? S19 Ni1 S9 100.75(2) . . ? S6 Ni1 S9 87.92(2) . . ? S16 Ni1 S9 171.45(2) . . ? C8 C4 H4A 109.5 . . ? C8 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C8 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 H5A 109.5 . . ? C8 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C8 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 S6 Ni1 105.15(7) . . ? C8 C7 S6 112.86(13) . . ? C8 C7 H7A 109.0 . . ? S6 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? S6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C4 C8 C7 112.88(17) . . ? C4 C8 C5 110.79(18) . . ? C7 C8 C5 110.39(16) . . ? C4 C8 S9 111.52(14) . . ? C7 C8 S9 101.15(14) . . ? C5 C8 S9 109.73(15) . . ? C10 S9 C8 102.91(10) . . ? C10 S9 Ni1 115.57(7) . . ? C8 S9 Ni1 103.35(7) . . ? C21 C10 S9 109.42(14) . . ? C21 C10 H10A 109.8 . . ? S9 C10 H10A 109.8 . . ? C21 C10 H10B 109.8 . . ? S9 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? C18 C14 H14A 109.5 . . ? C18 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C18 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 H15A 109.5 . . ? C18 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C18 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 S16 Ni1 105.02(7) . . ? C18 C17 S16 112.16(14) . . ? C18 C17 H17A 109.2 . . ? S16 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? S16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C14 C18 C15 111.16(16) . . ? C14 C18 C17 113.29(17) . . ? C15 C18 C17 111.21(17) . . ? C14 C18 S19 112.03(14) . . ? C15 C18 S19 109.00(14) . . ? C17 C18 S19 99.56(13) . . ? C20 S19 C18 102.90(9) . . ? C20 S19 Ni1 115.97(7) . . ? C18 S19 Ni1 104.72(7) . . ? C22 C20 S19 109.48(13) . . ? C22 C20 H20A 109.8 . . ? S19 C20 H20A 109.8 . . ? C22 C20 H20B 109.8 . . ? S19 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? C26 C21 C22 118.91(19) . . ? C26 C21 C10 119.44(18) . . ? C22 C21 C10 121.64(18) . . ? C23 C22 C21 119.27(18) . . ? C23 C22 C20 119.61(18) . . ? C21 C22 C20 121.12(19) . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 119.5(2) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 121.3(2) . . ? C25 C26 H26 119.3 . . ? C21 C26 H26 119.3 . . ? S36 Ni31 S39 89.09(2) . . ? S36 Ni31 S49 173.93(2) . . ? S39 Ni31 S49 96.820(19) . . ? S36 Ni31 S46 85.35(2) . . ? S39 Ni31 S46 169.53(2) . . ? S49 Ni31 S46 88.59(2) . . ? C38 C34 H34A 109.5 . . ? C38 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C38 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C38 C35 H35A 109.5 . . ? C38 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C38 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 S36 Ni31 104.03(7) . . ? C38 C37 S36 113.09(15) . . ? C38 C37 H37A 109.0 . . ? S36 C37 H37A 109.0 . . ? C38 C37 H37B 109.0 . . ? S36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 C34 111.94(18) . . ? C37 C38 C35 111.72(18) . . ? C34 C38 C35 111.46(19) . . ? C37 C38 S39 101.24(14) . . ? C34 C38 S39 112.00(14) . . ? C35 C38 S39 108.00(14) . . ? C40 S39 C38 103.39(9) . . ? C40 S39 Ni31 114.64(7) . . ? C38 S39 Ni31 107.12(7) . . ? C51 C40 S39 109.58(13) . . ? C51 C40 H40A 109.8 . . ? S39 C40 H40A 109.8 . . ? C51 C40 H40B 109.8 . . ? S39 C40 H40B 109.8 . . ? H40A C40 H40B 108.2 . . ? C48 C44 H44A 109.5 . . ? C48 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C48 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48 C45 H45A 109.5 . . ? C48 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C48 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 S46 Ni31 104.55(7) . . ? C48 C47 S46 113.51(15) . . ? C48 C47 H47A 108.9 . . ? S46 C47 H47A 108.9 . . ? C48 C47 H47B 108.9 . . ? S46 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C44 C48 C45 111.38(18) . . ? C44 C48 C47 112.14(16) . . ? C45 C48 C47 111.73(17) . . ? C44 C48 S49 111.34(14) . . ? C45 C48 S49 108.43(13) . . ? C47 C48 S49 101.35(14) . . ? C50 S49 C48 103.15(9) . . ? C50 S49 Ni31 115.03(7) . . ? C48 S49 Ni31 105.38(7) . . ? C52 C50 S49 109.30(13) . . ? C52 C50 H50A 109.8 . . ? S49 C50 H50A 109.8 . . ? C52 C50 H50B 109.8 . . ? S49 C50 H50B 109.8 . . ? H50A C50 H50B 108.3 . . ? C56 C51 C52 119.44(17) . . ? C56 C51 C40 118.34(18) . . ? C52 C51 C40 122.22(16) . . ? C53 C52 C51 119.19(17) . . ? C53 C52 C50 119.30(17) . . ? C51 C52 C50 121.51(17) . . ? C54 C53 C52 120.98(19) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C55 C54 C53 119.49(18) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 120.09(18) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.80(19) . . ? C55 C56 H56 119.6 . . ? C51 C56 H56 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S16 Ni1 S6 C7 -176.80(8) . . . . ? S9 Ni1 S6 C7 6.15(8) . . . . ? Ni1 S6 C7 C8 29.04(16) . . . . ? S6 C7 C8 C4 65.8(2) . . . . ? S6 C7 C8 C5 -169.57(15) . . . . ? S6 C7 C8 S9 -53.44(16) . . . . ? C4 C8 S9 C10 54.93(16) . . . . ? C7 C8 S9 C10 175.16(13) . . . . ? C5 C8 S9 C10 -68.22(16) . . . . ? C4 C8 S9 Ni1 -65.70(15) . . . . ? C7 C8 S9 Ni1 54.53(12) . . . . ? C5 C8 S9 Ni1 171.15(13) . . . . ? S19 Ni1 S9 C10 39.69(8) . . . . ? S6 Ni1 S9 C10 -143.67(8) . . . . ? S19 Ni1 S9 C8 151.29(7) . . . . ? S6 Ni1 S9 C8 -32.08(7) . . . . ? C8 S9 C10 C21 165.20(14) . . . . ? Ni1 S9 C10 C21 -82.95(14) . . . . ? S19 Ni1 S16 C17 -3.94(8) . . . . ? S6 Ni1 S16 C17 178.91(8) . . . . ? Ni1 S16 C17 C18 -32.42(16) . . . . ? S16 C17 C18 C14 -63.62(19) . . . . ? S16 C17 C18 C15 170.31(14) . . . . ? S16 C17 C18 S19 55.50(16) . . . . ? C14 C18 S19 C20 -57.12(16) . . . . ? C15 C18 S19 C20 66.33(16) . . . . ? C17 C18 S19 C20 -177.17(13) . . . . ? C14 C18 S19 Ni1 64.51(15) . . . . ? C15 C18 S19 Ni1 -172.03(13) . . . . ? C17 C18 S19 Ni1 -55.53(13) . . . . ? S16 Ni1 S19 C20 144.19(7) . . . . ? S9 Ni1 S19 C20 -39.21(7) . . . . ? S16 Ni1 S19 C18 31.58(7) . . . . ? S9 Ni1 S19 C18 -151.83(7) . . . . ? C18 S19 C20 C22 -163.45(14) . . . . ? Ni1 S19 C20 C22 82.89(15) . . . . ? S9 C10 C21 C26 -97.62(19) . . . . ? S9 C10 C21 C22 83.7(2) . . . . ? C26 C21 C22 C23 2.9(3) . . . . ? C10 C21 C22 C23 -178.41(18) . . . . ? C26 C21 C22 C20 -176.44(18) . . . . ? C10 C21 C22 C20 2.3(3) . . . . ? S19 C20 C22 C23 93.60(19) . . . . ? S19 C20 C22 C21 -87.1(2) . . . . ? C21 C22 C23 C24 -2.3(3) . . . . ? C20 C22 C23 C24 177.05(19) . . . . ? C22 C23 C24 C25 0.3(3) . . . . ? C23 C24 C25 C26 1.0(3) . . . . ? C24 C25 C26 C21 -0.4(3) . . . . ? C22 C21 C26 C25 -1.6(3) . . . . ? C10 C21 C26 C25 179.69(19) . . . . ? S39 Ni31 S36 C37 -8.40(8) . . . . ? S46 Ni31 S36 C37 162.72(8) . . . . ? Ni31 S36 C37 C38 41.57(17) . . . . ? S36 C37 C38 C34 65.1(2) . . . . ? S36 C37 C38 C35 -169.10(15) . . . . ? S36 C37 C38 S39 -54.36(16) . . . . ? C37 C38 S39 C40 165.05(13) . . . . ? C34 C38 S39 C40 45.63(18) . . . . ? C35 C38 S39 C40 -77.48(16) . . . . ? C37 C38 S39 Ni31 43.60(14) . . . . ? C34 C38 S39 Ni31 -75.82(16) . . . . ? C35 C38 S39 Ni31 161.08(13) . . . . ? S36 Ni31 S39 C40 -131.78(7) . . . . ? S49 Ni31 S39 C40 49.61(7) . . . . ? S46 Ni31 S39 C40 170.34(14) . . . . ? S36 Ni31 S39 C38 -17.72(7) . . . . ? S49 Ni31 S39 C38 163.68(7) . . . . ? S46 Ni31 S39 C38 -75.60(15) . . . . ? C38 S39 C40 C51 155.43(14) . . . . ? Ni31 S39 C40 C51 -88.33(14) . . . . ? S36 Ni31 S46 C47 179.60(8) . . . . ? S39 Ni31 S46 C47 -122.23(14) . . . . ? S49 Ni31 S46 C47 -0.86(8) . . . . ? Ni31 S46 C47 C48 -33.17(15) . . . . ? S46 C47 C48 C44 -65.7(2) . . . . ? S46 C47 C48 C45 168.47(14) . . . . ? S46 C47 C48 S49 53.18(15) . . . . ? C44 C48 S49 C50 -51.58(16) . . . . ? C45 C48 S49 C50 71.29(16) . . . . ? C47 C48 S49 C50 -170.99(13) . . . . ? C44 C48 S49 Ni31 69.40(14) . . . . ? C45 C48 S49 Ni31 -167.72(13) . . . . ? C47 C48 S49 Ni31 -50.01(13) . . . . ? S39 Ni31 S49 C50 -49.37(7) . . . . ? S46 Ni31 S49 C50 139.61(7) . . . . ? S39 Ni31 S49 C48 -162.26(7) . . . . ? S46 Ni31 S49 C48 26.73(7) . . . . ? C48 S49 C50 C52 -157.91(13) . . . . ? Ni31 S49 C50 C52 87.91(14) . . . . ? S39 C40 C51 C56 -96.96(18) . . . . ? S39 C40 C51 C52 82.2(2) . . . . ? C56 C51 C52 C53 0.8(3) . . . . ? C40 C51 C52 C53 -178.32(18) . . . . ? C56 C51 C52 C50 -179.44(18) . . . . ? C40 C51 C52 C50 1.4(3) . . . . ? S49 C50 C52 C53 96.07(18) . . . . ? S49 C50 C52 C51 -83.6(2) . . . . ? C51 C52 C53 C54 -1.4(3) . . . . ? C50 C52 C53 C54 178.90(18) . . . . ? C52 C53 C54 C55 0.6(3) . . . . ? C53 C54 C55 C56 0.6(3) . . . . ? C54 C55 C56 C51 -1.2(3) . . . . ? C52 C51 C56 C55 0.4(3) . . . . ? C40 C51 C56 C55 179.62(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.346 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.068 #===END