# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2091 data_complex1 _publ_section_title ; Crystal and molecular structure of complex 1 ; _publ_section_abstract ; We present the crystal and molecular structure of complex 1. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All Diagrams and calculations were performed using Crystan (MacScience, Japan). ; loop_ _publ_author_name _publ_author_address 'T. Kawamoto' ; Osaka University ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Reddish brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _chemical_formula_moiety 'C42 H52 O2 N2 S2 Ni1' _chemical_formula_weight 739.71 _cell_length_a 12.724(7) _cell_length_b 21.161(10) _cell_length_c 15.295(11) _cell_angle_alpha 90.0 _cell_angle_beta 108.70(5) _cell_angle_gamma 90.0 _cell_volume 3901(4) _cell_measurement_reflns_used '21' _cell_measurement_theta_min '3.3' _cell_measurement_theta_max '12.3' _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_meas ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.637 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science MXC3' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 2896 _reflns_number_total 1905 _reflns_number_observed 1482 _reflns_observed_criterion 'refl_observed_if_I_>_1.50_sigma(I)' _diffrn_reflns_av_R_equivalents 0.191 _diffrn_reflns_theta_max 21.95 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.068 _refine_ls_wR_factor_obs 0.065 _refine_ls_hydrogen_treatment 'refU' _refine_ls_number_reflns 1482 _refine_ls_number_parameters 238 _refine_ls_goodness_of_fit_obs 3.370 _refine_ls_weighting_scheme 'w = 1/(\s^2^(Fo) + 0.001Fo^2^)' _refine_ls_shift/esd_max 0.0408 _refine_ls_shift/esd_mean 0.0067 _refine_diff_density_min -0.73 _refine_diff_density_max 0.76 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _diffrn_orient_matrix_type 'standard' _diffrn_orient_matrix_UB_11 -0.06973 _diffrn_orient_matrix_UB_12 -0.02391 _diffrn_orient_matrix_UB_13 -0.00593 _diffrn_orient_matrix_UB_21 0.04118 _diffrn_orient_matrix_UB_22 -0.04076 _diffrn_orient_matrix_UB_23 0.00446 _diffrn_orient_matrix_UB_31 0.01805 _diffrn_orient_matrix_UB_32 0.00056 _diffrn_orient_matrix_UB_33 0.06863 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X+0.5,-Y+0.5,-Z +X+0.5,+Y+0.5,+Z -X,+Y,-Z+0.5 +X,-Y,+Z+0.5 +X+0.5,-Y+0.5,+Z+0.5 -X+0.5,+Y+0.5,-Z+0.5 _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_cell_setting 'Monoclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ni1 0.0000 -0.3417(2) 0.2500 0.040(1) 0.500 Uij S1 -0.1167(6) -0.2692(3) 0.2575(5) 0.058(4) 1.000 Uij O1 0.3256(14) -0.5265(8) 0.5677(12) 0.07(1) 1.000 Uij N1 -0.1023(16) -0.4028(9) 0.2703(12) 0.04(1) 1.000 Uij C1 -0.235(2) -0.319(1) 0.224(2) 0.04(2) 1.000 Uij C2 -0.215(2) -0.384(1) 0.230(2) 0.04(2) 1.000 Uij C3 -0.305(2) -0.425(1) 0.204(2) 0.06(2) 1.000 Uij C4 -0.413(3) -0.401(2) 0.173(2) 0.07(2) 1.000 Uij C5 -0.430(2) -0.337(2) 0.171(2) 0.07(2) 1.000 Uij C6 -0.341(3) -0.295(2) 0.197(2) 0.06(2) 1.000 Uij C7 -0.080(2) -0.453(1) 0.319(2) 0.04(1) 1.000 Uij C8 0.0284(19) -0.4708(10) 0.3789(15) 0.04(1) 1.000 Uij C9 0.102(2) -0.427(1) 0.434(2) 0.04(2) 1.000 Uij C10 0.201(2) -0.443(1) 0.499(2) 0.04(2) 1.000 Uij C11 0.229(2) -0.508(1) 0.504(2) 0.05(2) 1.000 Uij C12 0.162(2) -0.554(1) 0.447(2) 0.04(2) 1.000 Uij C13 0.060(2) -0.534(1) 0.388(2) 0.04(1) 1.000 Uij C14 0.272(2) -0.392(1) 0.564(2) 0.05(2) 1.000 Uij C15 0.277(3) -0.404(1) 0.663(2) 0.08(2) 1.000 Uij C16 0.225(3) -0.327(1) 0.537(2) 0.09(2) 1.000 Uij C17 0.390(3) -0.390(2) 0.558(2) 0.10(3) 1.000 Uij C18 0.199(2) -0.623(1) 0.450(2) 0.05(2) 1.000 Uij C19 0.115(3) -0.663(2) 0.377(2) 0.09(2) 1.000 Uij C20 0.210(3) -0.654(2) 0.543(2) 0.08(2) 1.000 Uij C21 0.309(3) -0.629(1) 0.428(2) 0.09(2) 1.000 Uij H1 0.37118 -0.49482 0.60677 0.065 1.000 Uiso H3 -0.29243 -0.46949 0.20584 0.04(7) 1.000 Uiso H4 -0.47390 -0.43022 0.15476 0.05(7) 1.000 Uiso H5 -0.50470 -0.32025 0.15033 0.05(7) 1.000 Uiso H6 -0.35438 -0.25038 0.19563 0.1(1) 1.000 Uiso H7 -0.14006 -0.48113 0.31580 0.04(7) 1.000 Uiso H9 0.08150 -0.38301 0.42693 0.02(5) 1.000 Uiso H13 0.00954 -0.56520 0.35263 0.07(8) 1.000 Uiso H15A 0.32062 -0.37259 0.70309 0.03(6) 1.000 Uiso H15B 0.20272 -0.40349 0.66668 0.065 1.000 Uiso H15C 0.30842 -0.44519 0.68178 0.1(1) 1.000 Uiso H16A 0.26863 -0.29501 0.57749 0.05(7) 1.000 Uiso H16B 0.22003 -0.31701 0.47489 0.085 1.000 Uiso H16C 0.15113 -0.32621 0.54219 0.085 1.000 Uiso H17A 0.43366 -0.35828 0.59811 0.090 1.000 Uiso H17B 0.42386 -0.43048 0.57531 0.090 1.000 Uiso H17C 0.38626 -0.38078 0.49561 0.090 1.000 Uiso H19A 0.13770 -0.70595 0.37908 0.06(8) 1.000 Uiso H19B 0.04470 -0.66035 0.38728 0.080 1.000 Uiso H19C 0.10810 -0.64536 0.31748 0.07(9) 1.000 Uiso H20A 0.23283 -0.69776 0.54455 0.1(1) 1.000 Uiso H20B 0.26483 -0.63156 0.59055 0.1(1) 1.000 Uiso H20C 0.14033 -0.65226 0.55375 0.080 1.000 Uiso H21A 0.33132 -0.67194 0.43003 0.06(8) 1.000 Uiso H21B 0.30122 -0.61124 0.36853 0.1(1) 1.000 Uiso H21C 0.36402 -0.60504 0.47423 0.090 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.043(3) 0.030(3) 0.040(3) 0.000 0.012(2) 0.000 S1 0.067(6) 0.039(5) 0.061(5) 0.015(4) 0.019(4) 0.004(4) O1 0.05(1) 0.06(1) 0.07(1) 0.01(1) -0.02(1) -0.01(1) N1 0.04(1) 0.03(1) 0.03(1) 0.01(1) 0.01(1) 0.00(1) C1 0.04(2) 0.06(2) 0.03(1) 0.01(1) 0.02(1) 0.01(1) C2 0.04(2) 0.04(2) 0.03(1) 0.01(1) 0.01(1) 0.01(1) C3 0.05(2) 0.07(2) 0.04(2) 0.00(2) 0.01(2) 0.01(2) C4 0.04(2) 0.11(3) 0.05(2) 0.00(2) 0.02(2) 0.01(2) C5 0.04(2) 0.11(3) 0.06(2) 0.03(2) 0.02(2) 0.02(2) C6 0.06(2) 0.07(2) 0.05(2) 0.03(2) 0.03(2) 0.01(2) C7 0.04(2) 0.03(1) 0.04(2) 0.00(1) 0.01(1) 0.01(1) C8 0.03(2) 0.03(1) 0.04(1) 0.00(1) 0.01(1) 0.01(1) C9 0.06(2) 0.02(1) 0.04(2) 0.00(1) 0.01(1) 0.01(1) C10 0.05(2) 0.05(2) 0.03(1) 0.00(1) 0.02(1) 0.01(1) C11 0.04(2) 0.06(2) 0.04(2) 0.01(1) 0.01(1) 0.00(1) C12 0.05(2) 0.03(1) 0.04(2) 0.00(1) 0.02(1) 0.00(1) C13 0.04(2) 0.04(2) 0.03(1) -0.01(1) 0.01(1) 0.00(1) C14 0.06(2) 0.05(2) 0.04(2) -0.02(1) 0.00(1) 0.00(1) C15 0.11(3) 0.06(2) 0.04(2) -0.03(2) 0.02(2) -0.01(2) C16 0.14(3) 0.05(2) 0.05(2) -0.03(2) 0.00(2) -0.01(2) C17 0.09(3) 0.12(3) 0.08(3) -0.05(2) 0.03(2) -0.03(2) C18 0.06(2) 0.04(2) 0.05(2) 0.01(1) 0.02(1) 0.00(1) C19 0.11(3) 0.06(2) 0.08(2) 0.03(2) 0.02(2) 0.00(2) C20 0.12(3) 0.05(2) 0.07(2) 0.03(2) 0.04(2) 0.02(2) C21 0.10(3) 0.06(2) 0.09(3) 0.04(2) 0.04(2) 0.01(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.163(8) . . yes Ni1 N1 1.928(19) . . yes S1 C1 1.76(3) . . yes O1 C11 1.37(3) . . yes N1 C2 1.43(4) . . yes N1 C7 1.28(3) . . yes C1 C2 1.40(4) . . yes C1 C6 1.38(5) . . yes C2 C3 1.39(4) . . yes C3 C4 1.38(5) . . yes C4 C5 1.39(6) . . yes C5 C6 1.39(5) . . yes C7 C8 1.43(4) . . yes C8 C9 1.39(4) . . yes C8 C13 1.39(4) . . yes C9 C10 1.37(4) . . yes C10 C11 1.40(4) . . yes C10 C14 1.55(4) . . yes C11 C12 1.40(4) . . yes C12 C13 1.38(4) . . yes C12 C18 1.54(4) . . yes C14 C15 1.52(4) . . yes C14 C16 1.51(4) . . yes C14 C17 1.53(5) . . yes C18 C19 1.52(5) . . yes C18 C20 1.53(5) . . yes C18 C21 1.53(5) . . yes O1 H1 0.960(18) . . yes C3 H3 0.96(3) . . yes C4 H4 0.96(4) . . yes C5 H5 0.96(4) . . yes C6 H6 0.96(4) . . yes C7 H7 0.96(3) . . yes C9 H9 0.96(3) . . yes C13 H13 0.96(3) . . yes C15 H15A 0.96(4) . . yes C15 H15B 0.96(4) . . yes C15 H15C 0.96(4) . . yes C16 H16A 0.96(3) . . yes C16 H16B 0.96(3) . . yes C16 H16C 0.96(4) . . yes C17 H17A 0.96(4) . . yes C17 H17B 0.96(4) . . yes C17 H17C 0.96(4) . . yes C19 H19A 0.96(4) . . yes C19 H19B 0.96(4) . . yes C19 H19C 0.96(4) . . yes C20 H20A 0.96(4) . . yes C20 H20B 0.96(4) . . yes C20 H20C 0.96(4) . . yes C21 H21A 0.96(4) . . yes C21 H21B 0.96(4) . . yes C21 H21C 0.96(4) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni1 S1 89.7(4) . . 5_555 yes S1 Ni1 N1 87.5(6) . . . yes S1 Ni1 N1 173.6(6) . . 5_555 yes N1 Ni1 N1 95.8(9) . . 5_555 yes Ni1 S1 C1 95.8(9) . . . yes Ni1 N1 C2 112.4(15) . . . yes Ni1 N1 C7 127.9(17) . . . yes C2 N1 C7 119.5(20) . . . yes S1 C1 C2 116.7(19) . . . yes S1 C1 C6 122.6(22) . . . yes C2 C1 C6 120.7(25) . . . yes N1 C2 C1 116.0(22) . . . yes N1 C2 C3 124.8(22) . . . yes C1 C2 C3 119.0(24) . . . yes C2 C3 C4 120.3(28) . . . yes C3 C4 C5 119.9(29) . . . yes C4 C5 C6 120.5(29) . . . yes C1 C6 C5 119.5(30) . . . yes N1 C7 C8 125.5(22) . . . yes C7 C8 C9 122.1(21) . . . yes C7 C8 C13 120.2(21) . . . yes C9 C8 C13 117.5(21) . . . yes C8 C9 C10 123.3(21) . . . yes C9 C10 C11 116.3(22) . . . yes C9 C10 C14 119.7(21) . . . yes C11 C10 C14 124.0(21) . . . yes O1 C11 C10 118.5(22) . . . yes O1 C11 C12 118.1(22) . . . yes C10 C11 C12 123.5(23) . . . yes C11 C12 C13 116.7(22) . . . yes C11 C12 C18 121.8(22) . . . yes C13 C12 C18 121.5(22) . . . yes C8 C13 C12 122.4(22) . . . yes C10 C14 C15 110.6(22) . . . yes C10 C14 C16 111.4(22) . . . yes C10 C14 C17 111.1(22) . . . yes C15 C14 C16 108.0(23) . . . yes C15 C14 C17 110.0(24) . . . yes C16 C14 C17 105.6(24) . . . yes C12 C18 C19 111.2(23) . . . yes C12 C18 C20 112.0(22) . . . yes C12 C18 C21 110.7(22) . . . yes C19 C18 C20 106.1(23) . . . yes C19 C18 C21 106.2(24) . . . yes C20 C18 C21 110.4(24) . . . yes C11 O1 H1 117.9(19) . . . yes C2 C3 H3 119.3(26) . . . yes C4 C3 H3 120.4(29) . . . yes C3 C4 H4 119.4(35) . . . yes C5 C4 H4 120.7(31) . . . yes C4 C5 H5 120.0(33) . . . yes C6 C5 H5 119.4(37) . . . yes C1 C6 H6 120.4(30) . . . yes C5 C6 H6 120.1(31) . . . yes N1 C7 H7 117.1(23) . . . yes C8 C7 H7 117.5(22) . . . yes C8 C9 H9 118.0(24) . . . yes C10 C9 H9 118.7(23) . . . yes C8 C13 H13 118.9(23) . . . yes C12 C13 H13 118.7(23) . . . yes C14 C15 H15A 110.4(27) . . . yes C14 C15 H15B 109.4(26) . . . yes C14 C15 H15C 109.2(26) . . . yes H15A C15 H15B 109.3(30) . . . yes H15A C15 H15C 109.5(30) . . . yes H15B C15 H15C 109.0(31) . . . yes C14 C16 H16A 111.4(27) . . . yes C14 C16 H16B 110.9(26) . . . yes C14 C16 H16C 107.6(26) . . . yes H16A C16 H16B 108.9(29) . . . yes H16A C16 H16C 109.0(30) . . . yes H16B C16 H16C 109.0(31) . . . yes C14 C17 H17A 111.3(29) . . . yes C14 C17 H17B 108.8(29) . . . yes C14 C17 H17C 109.6(29) . . . yes H17A C17 H17B 109.0(33) . . . yes H17A C17 H17C 109.0(34) . . . yes H17B C17 H17C 109.1(33) . . . yes C18 C19 H19A 111.7(28) . . . yes C18 C19 H19B 109.5(28) . . . yes C18 C19 H19C 108.6(28) . . . yes H19A C19 H19B 109.1(32) . . . yes H19A C19 H19C 109.0(31) . . . yes H19B C19 H19C 109.0(32) . . . yes C18 C20 H20A 112.0(28) . . . yes C18 C20 H20B 108.7(29) . . . yes C18 C20 H20C 109.2(29) . . . yes H20A C20 H20B 108.9(32) . . . yes H20A C20 H20C 108.9(33) . . . yes H20B C20 H20C 109.1(32) . . . yes C18 C21 H21A 110.4(28) . . . yes C18 C21 H21B 111.0(29) . . . yes C18 C21 H21C 108.0(28) . . . yes H21A C21 H21B 109.2(32) . . . yes H21A C21 H21C 109.3(33) . . . yes H21B C21 H21C 109.0(31) . . . yes #=========END data_complex2 _publ_section_title ; Crystal and molecular structure of complex 2 ; _publ_section_abstract ; We present the crystal and molecular structure of complex 2. ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All Diagrams and calculations were performed using Crystan (MacScience, Japan). ; loop_ _publ_author_name _publ_author_address 'T. Kawamoto' ; Osaka University ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Reddish brown' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _chemical_formula_moiety 'C28 H24 N2 S2 Ni1 ' _chemical_formula_weight 511.30 _cell_length_a 12.163(5) _cell_length_b 14.804(5) _cell_length_c 7.028(6) _cell_angle_alpha 90.06(5) _cell_angle_beta 106.80(5) _cell_angle_gamma 86.29(3) _cell_volume 1209(1) _cell_measurement_reflns_used '21' _cell_measurement_theta_min '9.4' _cell_measurement_theta_max '12.5' _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_meas ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.9894 _cell_measurement_temperature '298' _diffrn_measurement_device 'Mac Science MXC3' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type 'empirical \y scans' _exptl_absorpt_correction_T_min .557 _exptl_absorpt_correction_T_max .998 _diffrn_reflns_number 6205 _reflns_number_total 4654 _reflns_number_observed 3826 _reflns_observed_criterion 'refl_observed_if_I_>_2.00_sigma(I)' _diffrn_reflns_av_R_equivalents 0.146 _diffrn_reflns_theta_max 26.47 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.085 _refine_ls_wR_factor_obs 0.098 _refine_ls_hydrogen_treatment 'refU' _refine_ls_number_reflns 3826 _refine_ls_number_parameters 309 _refine_ls_goodness_of_fit_obs 2.134 _refine_ls_weighting_scheme 'w = 1/(\s^2^(Fo) + 0.002Fo^2^)' _refine_ls_shift/esd_max 0.1523 _refine_ls_shift/esd_mean 0.0162 _refine_diff_density_min -1.56 _refine_diff_density_max 1.48 _refine_ls_extinction_method 'None' _atom_type_scat_source 'International Tables (1974)' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'Crystan' _computing_molecular_graphics 'Crystan' _computing_publication_material 'Crystan' _computing_structure_refinement 'Crystan' _computing_structure_solution 'Crystan' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ni1 0.00002(7) 0.25010(6) 0.71618(11) 0.0401(4) 1.000 Uij S1 0.13069(15) 0.21063(13) 0.56933(23) 0.0548(9) 1.000 Uij S2 -0.13111(15) 0.28944(13) 0.43872(22) 0.0539(9) 1.000 Uij N1 0.0954(4) 0.1845(3) 0.9479(7) 0.042(3) 1.000 Uij N2 -0.0949(4) 0.3162(3) 0.8502(7) 0.037(2) 1.000 Uij C1 0.2441(5) 0.1912(4) 0.7900(9) 0.045(3) 1.000 Uij C2 0.2158(5) 0.1845(4) 0.9706(9) 0.042(3) 1.000 Uij C3 0.3004(5) 0.1746(4) 1.1496(9) 0.049(3) 1.000 Uij C4 0.4148(6) 0.1682(5) 1.1543(11) 0.060(4) 1.000 Uij C5 0.4440(6) 0.1707(5) 0.9752(12) 0.065(4) 1.000 Uij C6 0.3598(6) 0.1839(5) 0.7959(10) 0.058(4) 1.000 Uij C7 0.0620(5) 0.1304(4) 1.0618(8) 0.042(3) 1.000 Uij C8 -0.0545(6) 0.1069(4) 1.0436(10) 0.050(3) 1.000 Uij C9 -0.1411(6) 0.1075(4) 0.8657(11) 0.057(4) 1.000 Uij C10 -0.2488(6) 0.0761(5) 0.8544(13) 0.067(4) 1.000 Uij C11 -0.2660(8) 0.0451(6) 1.0305(16) 0.084(5) 1.000 Uij C12 -0.1819(8) 0.0424(6) 1.2089(14) 0.082(6) 1.000 Uij C13 -0.0756(7) 0.0727(5) 1.2171(11) 0.065(4) 1.000 Uij C14 -0.0625(5) 0.3686(4) 0.9990(9) 0.043(3) 1.000 Uij C15 0.0547(6) 0.3932(4) 1.0998(9) 0.048(3) 1.000 Uij C16 0.0765(7) 0.4263(5) 1.2899(11) 0.060(4) 1.000 Uij C17 0.1821(8) 0.4570(6) 1.3888(12) 0.074(5) 1.000 Uij C18 0.2654(7) 0.4549(5) 1.2923(14) 0.073(5) 1.000 Uij C19 0.2484(6) 0.4246(5) 1.1017(13) 0.065(4) 1.000 Uij C20 0.1402(6) 0.3929(4) 1.0054(10) 0.055(4) 1.000 Uij C21 -0.2441(5) 0.3093(4) 0.5465(9) 0.044(3) 1.000 Uij C22 -0.2158(5) 0.3162(4) 0.7528(9) 0.041(3) 1.000 Uij C23 -0.3004(6) 0.3251(4) 0.8494(9) 0.050(3) 1.000 Uij C24 -0.4148(6) 0.3308(5) 0.7373(11) 0.058(4) 1.000 Uij C25 -0.4438(6) 0.3270(5) 0.5316(12) 0.062(4) 1.000 Uij C26 -0.3598(6) 0.3158(5) 0.4357(10) 0.054(4) 1.000 Uij C27 -0.3399(9) 0.0748(8) 0.6620(16) 0.107(7) 1.000 Uij C28 0.3394(8) 0.4245(7) 1.0030(17) 0.099(6) 1.000 Uij H3 0.27940 0.17147 1.27092 0.03(1) 1.000 Uiso H4 0.47358 0.16378 1.27967 0.07(2) 1.000 Uiso H5 0.52351 0.16252 0.97876 0.07(2) 1.000 Uiso H6 0.38122 0.18691 0.67486 0.08(3) 1.000 Uiso H7 0.12087 0.10382 1.17333 0.045 1.000 Uiso H9 -0.12567 0.12857 0.74742 0.060(8) 1.000 Uiso H11 -0.33966 0.02443 1.02694 0.08(1) 1.000 Uiso H12 -0.19656 0.01869 1.32569 0.08(1) 1.000 Uiso H13 -0.01627 0.07299 1.34172 0.07(3) 1.000 Uiso H14 -0.12299 0.39515 1.04781 0.02(1) 1.000 Uiso H16 0.01586 0.42867 1.35250 0.05(2) 1.000 Uiso H17 0.19662 0.48035 1.52070 0.07(2) 1.000 Uiso H18 0.33955 0.47468 1.36265 0.06(6) 1.000 Uiso H20 0.12562 0.37035 0.87298 0.01(1) 1.000 Uiso H23 -0.27890 0.32691 0.99189 0.05(2) 1.000 Uiso H24 -0.47403 0.33906 0.80237 0.05(2) 1.000 Uiso H25 -0.52319 0.33172 0.45429 0.08(2) 1.000 Uiso H26 -0.38075 0.31210 0.29350 0.07(2) 1.000 Uiso H27A -0.41427 0.05434 0.65450 0.100 1.000 Uiso H27B -0.35257 0.13554 0.60830 0.100 1.000 Uiso H27C -0.30877 0.03654 0.57720 0.100 1.000 Uiso H28A 0.41269 0.44637 1.07137 0.090 1.000 Uiso H28B 0.35239 0.36227 0.97167 0.090 1.000 Uiso H28C 0.30929 0.45907 0.88147 0.090 1.000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.0313(4) 0.0480(5) 0.0360(4) 0.0015(3) 0.0055(3) 0.0139(3) S1 0.045(1) 0.077(1) 0.038(1) 0.006(1) 0.013(1) 0.011(1) S2 0.043(1) 0.078(1) 0.034(1) 0.006(1) 0.006(1) 0.016(1) N1 0.029(3) 0.055(3) 0.039(3) -0.002(2) 0.007(2) 0.014(2) N2 0.030(3) 0.040(3) 0.037(3) -0.001(2) 0.004(2) 0.015(2) C1 0.037(3) 0.050(4) 0.044(3) -0.003(3) 0.011(3) 0.007(3) C2 0.028(3) 0.041(3) 0.051(4) -0.003(2) 0.003(3) 0.012(3) C3 0.038(3) 0.054(4) 0.049(4) -0.005(3) 0.006(3) 0.011(3) C4 0.034(4) 0.070(5) 0.065(5) -0.009(3) -0.004(3) 0.017(3) C5 0.028(4) 0.069(5) 0.090(6) 0.001(3) 0.012(4) 0.013(4) C6 0.039(4) 0.069(5) 0.062(4) -0.003(3) 0.018(3) 0.012(3) C7 0.042(3) 0.042(3) 0.038(3) -0.003(3) 0.009(3) 0.009(2) C8 0.044(4) 0.031(3) 0.070(4) 0.000(3) 0.018(3) 0.004(3) C9 0.045(4) 0.040(4) 0.077(5) -0.003(3) 0.008(3) 0.016(3) C10 0.042(4) 0.046(4) 0.101(6) 0.001(3) 0.000(4) 0.014(4) C11 0.057(5) 0.062(5) 0.130(8) -0.001(4) 0.046(6) 0.018(5) C12 0.076(6) 0.078(6) 0.092(6) -0.023(5) 0.047(5) 0.004(5) C13 0.068(5) 0.059(4) 0.066(5) -0.015(4) 0.033(4) 0.005(3) C14 0.041(3) 0.042(3) 0.043(3) 0.004(3) 0.011(3) 0.015(3) C15 0.043(4) 0.039(3) 0.052(4) -0.001(3) 0.001(3) 0.014(3) C16 0.064(5) 0.051(4) 0.055(4) -0.011(3) 0.000(4) 0.014(3) C17 0.080(6) 0.065(5) 0.062(5) -0.023(4) -0.006(4) 0.019(4) C18 0.055(5) 0.045(4) 0.100(7) -0.007(3) -0.022(5) 0.022(4) C19 0.046(4) 0.037(4) 0.099(6) -0.002(3) 0.009(4) 0.013(4) C20 0.051(4) 0.040(4) 0.067(5) -0.004(3) 0.009(3) 0.006(3) C21 0.035(3) 0.044(3) 0.047(3) -0.002(3) 0.003(3) 0.012(3) C22 0.034(3) 0.033(3) 0.048(3) -0.001(2) 0.005(3) 0.013(2) C23 0.045(4) 0.052(4) 0.050(4) -0.004(3) 0.014(3) 0.011(3) C24 0.035(4) 0.058(4) 0.075(5) -0.004(3) 0.017(3) 0.010(3) C25 0.039(4) 0.060(5) 0.075(5) -0.004(3) -0.001(4) 0.009(4) C26 0.035(4) 0.066(4) 0.050(4) 0.000(3) -0.004(3) 0.016(3) C27 0.066(6) 0.112(8) 0.124(8) -0.028(6) -0.007(6) 0.032(6) C28 0.058(6) 0.080(6) 0.149(9) -0.010(5) 0.030(6) 0.009(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.182(2) . . yes Ni1 S2 2.184(2) . . yes Ni1 N1 1.925(5) . . yes Ni1 N2 1.912(5) . . yes S1 C1 1.762(7) . . yes S2 C21 1.761(7) . . yes N1 C2 1.427(8) . . yes N1 C7 1.296(8) . . yes N2 C14 1.286(8) . . yes N2 C22 1.431(8) . . yes C1 C2 1.413(9) . . yes C1 C6 1.393(10) . . yes C2 C3 1.377(9) . . yes C3 C4 1.379(10) . . yes C4 C5 1.405(11) . . yes C5 C6 1.380(11) . . yes C7 C8 1.450(9) . . yes C8 C9 1.382(10) . . yes C8 C13 1.417(10) . . yes C9 C10 1.399(11) . . yes C10 C11 1.396(14) . . yes C10 C27 1.481(14) . . yes C11 C12 1.368(14) . . yes C12 C13 1.381(13) . . yes C14 C15 1.466(9) . . yes C15 C16 1.380(10) . . yes C15 C20 1.387(10) . . yes C16 C17 1.379(12) . . yes C17 C18 1.371(13) . . yes C18 C19 1.374(13) . . yes C19 C20 1.405(11) . . yes C19 C28 1.466(13) . . yes C21 C22 1.395(9) . . yes C21 C26 1.395(9) . . yes C22 C23 1.387(9) . . yes C23 C24 1.384(10) . . yes C24 C25 1.387(11) . . yes C25 C26 1.378(10) . . yes C3 H3 0.960(7) . . yes C4 H4 0.960(8) . . yes C5 H5 0.960(7) . . yes C6 H6 0.960(7) . . yes C7 H7 0.960(6) . . yes C9 H9 0.960(8) . . yes C11 H11 0.959(9) . . yes C12 H12 0.960(10) . . yes C13 H13 0.960(8) . . yes C14 H14 0.960(7) . . yes C16 H16 0.960(8) . . yes C17 H17 0.960(8) . . yes C18 H18 0.960(9) . . yes C20 H20 0.960(7) . . yes C23 H23 0.960(7) . . yes C24 H24 0.960(7) . . yes C25 H25 0.960(8) . . yes C26 H26 0.960(7) . . yes C27 H27A 0.960(11) . . yes C27 H27B 0.961(12) . . yes C27 H27C 0.960(11) . . yes C28 H28A 0.959(10) . . yes C28 H28B 0.960(10) . . yes C28 H28C 0.960(11) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni1 S2 93.9(1) . . . yes S1 Ni1 N1 87.5(2) . . . yes S1 Ni1 N2 164.0(2) . . . yes S2 Ni1 N1 164.2(2) . . . yes S2 Ni1 N2 87.0(2) . . . yes N1 Ni1 N2 96.0(2) . . . yes Ni1 S1 C1 95.7(3) . . . yes Ni1 S2 C21 95.6(3) . . . yes Ni1 N1 C2 114.1(4) . . . yes Ni1 N1 C7 127.0(5) . . . yes C2 N1 C7 117.8(5) . . . yes Ni1 N2 C14 127.5(5) . . . yes Ni1 N2 C22 114.4(4) . . . yes C14 N2 C22 117.4(5) . . . yes S1 C1 C2 118.0(5) . . . yes S1 C1 C6 123.5(5) . . . yes C2 C1 C6 118.5(6) . . . yes N1 C2 C1 114.4(6) . . . yes N1 C2 C3 124.5(6) . . . yes C1 C2 C3 121.0(6) . . . yes C2 C3 C4 120.0(6) . . . yes C3 C4 C5 119.5(7) . . . yes C4 C5 C6 120.7(7) . . . yes C1 C6 C5 120.1(7) . . . yes N1 C7 C8 127.6(6) . . . yes C7 C8 C9 124.0(6) . . . yes C7 C8 C13 116.8(6) . . . yes C9 C8 C13 118.9(7) . . . yes C8 C9 C10 121.4(7) . . . yes C9 C10 C11 117.4(8) . . . yes C9 C10 C27 120.9(8) . . . yes C11 C10 C27 121.7(8) . . . yes C10 C11 C12 122.9(9) . . . yes C11 C12 C13 119.0(9) . . . yes C8 C13 C12 120.4(8) . . . yes N2 C14 C15 127.8(6) . . . yes C14 C15 C16 118.0(7) . . . yes C14 C15 C20 122.6(6) . . . yes C16 C15 C20 119.1(7) . . . yes C15 C16 C17 121.4(8) . . . yes C16 C17 C18 118.1(8) . . . yes C17 C18 C19 123.4(8) . . . yes C18 C19 C20 117.2(8) . . . yes C18 C19 C28 121.6(8) . . . yes C20 C19 C28 121.2(8) . . . yes C15 C20 C19 120.8(7) . . . yes S2 C21 C22 118.0(5) . . . yes S2 C21 C26 123.0(5) . . . yes C22 C21 C26 119.0(6) . . . yes N2 C22 C21 114.4(6) . . . yes N2 C22 C23 124.4(6) . . . yes C21 C22 C23 121.2(6) . . . yes C22 C23 C24 119.0(6) . . . yes C23 C24 C25 120.2(7) . . . yes C24 C25 C26 120.9(7) . . . yes C21 C26 C25 119.6(7) . . . yes C2 C3 H3 119.7(7) . . . yes C4 C3 H3 120.2(7) . . . yes C3 C4 H4 119.8(7) . . . yes C5 C4 H4 120.7(7) . . . yes C4 C5 H5 119.1(8) . . . yes C6 C5 H5 120.2(8) . . . yes C1 C6 H6 120.1(7) . . . yes C5 C6 H6 119.7(7) . . . yes N1 C7 H7 116.3(6) . . . yes C8 C7 H7 116.0(6) . . . yes C8 C9 H9 118.8(7) . . . yes C10 C9 H9 119.8(8) . . . yes C10 C11 H11 118.9(10) . . . yes C12 C11 H11 118.3(10) . . . yes C11 C12 H12 120.1(10) . . . yes C13 C12 H12 120.8(9) . . . yes C8 C13 H13 119.4(8) . . . yes C12 C13 H13 120.2(8) . . . yes N2 C14 H14 115.4(6) . . . yes C15 C14 H14 116.8(6) . . . yes C15 C16 H16 118.8(8) . . . yes C17 C16 H16 119.9(8) . . . yes C16 C17 H17 121.0(9) . . . yes C18 C17 H17 120.9(9) . . . yes C17 C18 H18 118.0(9) . . . yes C19 C18 H18 118.6(9) . . . yes C15 C20 H20 119.6(7) . . . yes C19 C20 H20 119.5(8) . . . yes C22 C23 H23 119.8(7) . . . yes C24 C23 H23 121.3(7) . . . yes C23 C24 H24 119.6(8) . . . yes C25 C24 H24 120.1(7) . . . yes C24 C25 H25 120.0(7) . . . yes C26 C25 H25 119.2(8) . . . yes C21 C26 H26 120.1(7) . . . yes C25 C26 H26 120.3(7) . . . yes C10 C27 H27A 121.0(10) . . . yes C10 C27 H27B 107.2(10) . . . yes C10 C27 H27C 106.1(9) . . . yes H27A C27 H27B 106.6(10) . . . yes H27A C27 H27C 106.6(11) . . . yes H27B C27 H27C 109.0(11) . . . yes C19 C28 H28A 119.9(10) . . . yes C19 C28 H28B 105.0(9) . . . yes C19 C28 H28C 107.5(9) . . . yes H28A C28 H28B 107.6(10) . . . yes H28A C28 H28C 107.6(10) . . . yes H28B C28 H28C 109.0(11) . . . yes #===================================================