# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1210 data_global _publ_section_title ; Isolation and crystal structure of a novel dinuclear nickel(II) O-bound sulfinate from the oxidation of 2,2'-bipyridine- 1,2-benzenedithiolatonickel(II) ; loop_ _publ_author_name 'Cocker, T. Matthew' 'Bachman, Robert E.' _publ_author_address ;Department of Chemistry, Box 571227, Georgetown University, Washington, D.C., 20057-1227, USA ; _publ_contact_author_name "Robert E. Bachman" _publ_contact_author_address ;Department of Chemistry, Box 571227, Georgetown University, Washington, D.C., 20057-1227, USA ; _publ_requested_journal 'Chemical Communications' _publ_contact_author_email bachmanr@gusun.georgetown.edu _publ_section_abstract ;Abstract of paper in English ; # --------data for compound 2------------ data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 N4 Ni2 O2.80 S4' _chemical_formula_weight 755.01 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5407(3) _cell_length_b 16.9821(4) _cell_length_c 16.7013(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.9880(10) _cell_angle_gamma 90.00 _cell_volume 3130.39(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour 'RED BROWN' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1546 _exptl_absorpt_coefficient_mu 1.510 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7941 _exptl_absorpt_correction_T_max 0.9421 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25633 _diffrn_reflns_av_R_equivalents 0.2091 _diffrn_reflns_av_sigmaI/netI 0.1678 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5340 _reflns_number_gt 2858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5340 _refine_ls_number_parameters 416 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1523 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1788 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.015 _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 0.02624(10) 0.60996(7) 0.21611(7) 0.0258(4) Uani 1 1 d . . . Ni2 Ni 0.20050(10) 0.77464(7) 0.17608(7) 0.0289(4) Uani 1 1 d . . . S1 S 0.2846(2) 0.66256(14) 0.20506(14) 0.0281(6) Uani 1 1 d . . . S2 S 0.2953(2) 0.79652(15) 0.08452(16) 0.0372(7) Uani 1 1 d D . . S3 S 0.1135(2) 0.88847(15) 0.14783(18) 0.0430(7) Uani 1 1 d . . . S4 S 0.0995(2) 0.74581(14) 0.26207(15) 0.0292(6) Uani 1 1 d . . . O1 O 0.1937(5) 0.5978(3) 0.1910(4) 0.0286(15) Uani 1 1 d . . . O2 O 0.3761(5) 0.6579(4) 0.2875(4) 0.0390(17) Uani 1 1 d . . . O3 O 0.3826(11) 0.8584(7) 0.1010(10) 0.037(4) Uani 0.40 1 d PD . . O4 O 0.1942(10) 0.7960(8) 0.0048(7) 0.027(4) Uani 0.40 1 d PD . . N1 N 0.0938(6) 0.5789(4) 0.3406(5) 0.0270(18) Uani 1 1 d . . . N11 N -0.1235(7) 0.6285(4) 0.2561(4) 0.0244(17) Uani 1 1 d . . . N21 N -0.0151(6) 0.4964(4) 0.1744(4) 0.0284(18) Uani 1 1 d . . . N31 N -0.0649(6) 0.6297(4) 0.0911(4) 0.0263(17) Uani 1 1 d . . . C2 C 0.0164(9) 0.5929(5) 0.3876(6) 0.030(2) Uani 1 1 d . . . C3 C 0.0570(10) 0.5855(6) 0.4749(6) 0.042(3) Uani 1 1 d . . . H3A H 0.0026 0.5940 0.5072 0.050 Uiso 1 1 calc R . . C4 C 0.1751(10) 0.5662(6) 0.5133(6) 0.044(3) Uani 1 1 d . . . H4A H 0.2033 0.5630 0.5727 0.053 Uiso 1 1 calc R . . C5 C 0.2518(9) 0.5516(6) 0.4682(6) 0.042(3) Uani 1 1 d . . . H5A H 0.3336 0.5373 0.4947 0.050 Uiso 1 1 calc R . . C6 C 0.2078(9) 0.5580(6) 0.3812(6) 0.037(2) Uani 1 1 d . . . H6A H 0.2615 0.5469 0.3490 0.044 Uiso 1 1 calc R . . C12 C -0.1057(8) 0.6164(5) 0.3393(5) 0.026(2) Uani 1 1 d . . . C13 C -0.2002(9) 0.6308(5) 0.3733(6) 0.035(2) Uani 1 1 d . . . H13A H -0.1876 0.6215 0.4314 0.042 Uiso 1 1 calc R . . C14 C -0.3111(10) 0.6578(6) 0.3258(6) 0.037(3) Uani 1 1 d . . . H14A H -0.3755 0.6654 0.3498 0.045 Uiso 1 1 calc R . . C15 C -0.3265(8) 0.6737(6) 0.2429(7) 0.036(2) Uani 1 1 d . . . H15A H -0.4003 0.6953 0.2088 0.043 Uiso 1 1 calc R . . C16 C -0.2314(8) 0.6573(5) 0.2098(6) 0.029(2) Uani 1 1 d . . . H16A H -0.2430 0.6669 0.1519 0.035 Uiso 1 1 calc R . . C22 C -0.0811(8) 0.4885(5) 0.0931(5) 0.027(2) Uani 1 1 d . . . C23 C -0.1132(9) 0.4165(6) 0.0566(6) 0.037(2) Uani 1 1 d . . . H23A H -0.1580 0.4130 -0.0009 0.044 Uiso 1 1 calc R . . C24 C -0.0803(8) 0.3492(6) 0.1038(7) 0.038(3) Uani 1 1 d . . . H24A H -0.1053 0.2991 0.0795 0.045 Uiso 1 1 calc R . . C25 C -0.0108(8) 0.3545(6) 0.1862(6) 0.033(2) Uani 1 1 d . . . H25A H 0.0167 0.3088 0.2191 0.040 Uiso 1 1 calc R . . C26 C 0.0171(8) 0.4300(5) 0.2192(6) 0.033(2) Uani 1 1 d . . . H26A H 0.0615 0.4347 0.2767 0.040 Uiso 1 1 calc R . . C32 C -0.1106(8) 0.5648(6) 0.0462(5) 0.029(2) Uani 1 1 d . . . C33 C -0.1789(8) 0.5673(6) -0.0381(6) 0.036(2) Uani 1 1 d . . . H33A H -0.2091 0.5203 -0.0677 0.044 Uiso 1 1 calc R . . C34 C -0.2014(9) 0.6402(6) -0.0777(6) 0.039(3) Uani 1 1 d . . . H34A H -0.2473 0.6439 -0.1349 0.047 Uiso 1 1 calc R . . C35 C -0.1554(9) 0.7078(6) -0.0318(6) 0.042(3) Uani 1 1 d . . . H35A H -0.1705 0.7583 -0.0572 0.050 Uiso 1 1 calc R . . C36 C -0.0873(8) 0.7002(5) 0.0513(6) 0.034(2) Uani 1 1 d . . . H36A H -0.0550 0.7464 0.0817 0.041 Uiso 1 1 calc R . . C41 C 0.3650(7) 0.6449(5) 0.1309(5) 0.025(2) Uani 1 1 d . . . C42 C 0.3737(8) 0.7067(5) 0.0797(5) 0.028(2) Uani 1 1 d . . . C43 C 0.4449(9) 0.6980(6) 0.0254(6) 0.040(3) Uani 1 1 d . . . H43A H 0.4514 0.7399 -0.0107 0.048 Uiso 1 1 calc R . . C44 C 0.5052(9) 0.6285(6) 0.0247(6) 0.042(3) Uani 1 1 d . . . H44A H 0.5539 0.6230 -0.0119 0.050 Uiso 1 1 calc R . . C45 C 0.4967(9) 0.5666(6) 0.0759(6) 0.038(3) Uani 1 1 d . . . H45A H 0.5390 0.5189 0.0740 0.046 Uiso 1 1 calc R . . C46 C 0.4260(8) 0.5736(6) 0.1309(6) 0.037(2) Uani 1 1 d . . . H46A H 0.4196 0.5316 0.1668 0.044 Uiso 1 1 calc R . . C51 C -0.0061(8) 0.8244(5) 0.2525(5) 0.027(2) Uani 1 1 d . . . C52 C 0.0051(8) 0.8887(6) 0.2035(6) 0.033(2) Uani 1 1 d . . . C53 C -0.0731(8) 0.9540(6) 0.1970(6) 0.035(2) Uani 1 1 d . . . H53A H -0.0680 0.9980 0.1630 0.042 Uiso 1 1 calc R . . C54 C -0.1584(8) 0.9522(6) 0.2419(6) 0.038(2) Uani 1 1 d . . . H54A H -0.2119 0.9954 0.2384 0.046 Uiso 1 1 calc R . . C55 C -0.1657(9) 0.8878(6) 0.2915(6) 0.039(3) Uani 1 1 d . . . H55A H -0.2234 0.8879 0.3221 0.047 Uiso 1 1 calc R . . C56 C -0.0905(8) 0.8241(5) 0.2971(6) 0.035(2) Uani 1 1 d . . . H56A H -0.0962 0.7803 0.3310 0.042 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 0.0292(7) 0.0282(7) 0.0201(6) 0.0027(5) 0.0075(5) 0.0014(6) Ni2 0.0303(8) 0.0283(7) 0.0303(7) -0.0019(5) 0.0120(6) -0.0023(5) S1 0.0263(14) 0.0337(13) 0.0245(12) -0.0015(10) 0.0076(11) 0.0000(11) S2 0.0477(17) 0.0359(15) 0.0326(15) 0.0004(11) 0.0188(13) 0.0060(13) S3 0.0462(17) 0.0316(14) 0.0625(19) 0.0087(13) 0.0336(15) 0.0019(13) S4 0.0300(14) 0.0284(13) 0.0303(13) -0.0036(10) 0.0106(11) -0.0005(11) O1 0.022(4) 0.029(3) 0.038(4) 0.001(3) 0.012(3) -0.005(3) O2 0.027(4) 0.054(4) 0.028(4) 0.002(3) -0.004(3) -0.002(3) O3 0.019(9) 0.052(11) 0.046(11) -0.012(9) 0.020(8) -0.002(8) O4 0.017(8) 0.035(9) 0.022(8) 0.005(7) -0.004(7) -0.002(7) N1 0.025(5) 0.029(4) 0.026(4) 0.001(3) 0.007(4) 0.000(3) N11 0.030(5) 0.022(4) 0.023(4) 0.000(3) 0.012(4) -0.006(3) N21 0.035(5) 0.036(5) 0.016(4) 0.008(3) 0.012(4) 0.003(4) N31 0.021(4) 0.030(4) 0.028(4) 0.001(4) 0.006(3) 0.002(3) C2 0.043(6) 0.022(5) 0.024(5) -0.002(4) 0.010(5) -0.001(4) C3 0.063(8) 0.047(7) 0.022(5) 0.003(5) 0.023(6) -0.004(6) C4 0.045(7) 0.061(8) 0.024(6) 0.003(5) 0.004(5) 0.011(6) C5 0.040(7) 0.052(7) 0.026(6) 0.013(5) 0.000(5) 0.010(5) C6 0.037(7) 0.044(6) 0.028(6) 0.005(5) 0.006(5) 0.004(5) C12 0.032(6) 0.026(5) 0.025(5) 0.000(4) 0.014(4) 0.004(4) C13 0.038(7) 0.029(5) 0.036(6) -0.006(5) 0.010(5) -0.001(5) C14 0.049(7) 0.037(6) 0.035(6) -0.015(5) 0.025(5) -0.012(5) C15 0.015(5) 0.040(6) 0.048(7) -0.003(5) 0.000(5) 0.002(4) C16 0.028(6) 0.028(5) 0.030(5) 0.005(4) 0.006(5) 0.013(4) C22 0.027(6) 0.036(5) 0.021(5) -0.005(4) 0.010(4) -0.002(4) C23 0.038(6) 0.045(6) 0.027(5) -0.001(5) 0.010(5) 0.001(5) C24 0.033(6) 0.030(6) 0.053(7) -0.004(5) 0.017(5) -0.008(5) C25 0.034(6) 0.031(5) 0.032(5) 0.005(5) 0.006(5) -0.003(4) C26 0.037(6) 0.033(6) 0.033(6) 0.002(5) 0.013(5) -0.004(5) C32 0.030(6) 0.040(6) 0.017(5) 0.008(4) 0.007(4) 0.003(5) C33 0.037(6) 0.043(6) 0.027(5) -0.001(5) 0.006(5) -0.010(5) C34 0.038(7) 0.061(7) 0.017(5) 0.003(5) 0.006(5) 0.006(5) C35 0.050(7) 0.047(7) 0.027(6) 0.014(5) 0.009(5) 0.015(5) C36 0.041(6) 0.027(5) 0.035(6) 0.014(4) 0.014(5) 0.007(5) C41 0.019(5) 0.035(5) 0.022(5) -0.011(4) 0.007(4) -0.009(4) C42 0.030(6) 0.032(6) 0.020(5) -0.010(4) 0.006(4) -0.004(4) C43 0.051(7) 0.051(7) 0.023(5) 0.000(5) 0.017(5) 0.006(5) C44 0.040(7) 0.048(7) 0.037(6) -0.005(5) 0.012(5) 0.008(5) C45 0.041(7) 0.042(6) 0.033(6) -0.012(5) 0.014(5) 0.011(5) C46 0.040(6) 0.038(6) 0.029(6) -0.004(5) 0.005(5) 0.002(5) C51 0.029(6) 0.031(5) 0.022(5) -0.002(4) 0.008(4) 0.000(4) C52 0.024(6) 0.044(6) 0.032(6) -0.011(5) 0.007(4) -0.003(5) C53 0.038(6) 0.031(5) 0.037(6) 0.008(5) 0.013(5) 0.005(5) C54 0.033(6) 0.039(6) 0.040(6) -0.007(5) 0.008(5) 0.004(5) C55 0.042(7) 0.046(6) 0.031(6) -0.010(5) 0.015(5) -0.002(5) C56 0.041(6) 0.028(6) 0.041(6) -0.002(5) 0.019(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N11 2.051(7) . ? Ni1 N21 2.059(7) . ? Ni1 N1 2.065(7) . ? Ni1 N31 2.073(7) . ? Ni1 O1 2.104(5) . ? Ni1 S4 2.499(3) . ? Ni2 S1 2.127(3) . ? Ni2 S4 2.154(3) . ? Ni2 S2 2.157(3) . ? Ni2 S3 2.166(3) . ? S1 O2 1.473(6) . ? S1 O1 1.490(6) . ? S1 C41 1.777(9) . ? S2 O3 1.427(9) . ? S2 O4 1.492(8) . ? S2 C42 1.788(9) . ? S3 C52 1.763(9) . ? S4 C51 1.782(9) . ? N1 C6 1.339(11) . ? N1 C2 1.371(11) . ? N11 C16 1.351(10) . ? N11 C12 1.360(11) . ? N21 C26 1.346(11) . ? N21 C22 1.356(10) . ? N31 C32 1.351(11) . ? N31 C36 1.357(11) . ? C2 C3 1.400(12) . ? C2 C12 1.461(12) . ? C3 C4 1.366(13) . ? C4 C5 1.343(13) . ? C5 C6 1.397(12) . ? C12 C13 1.390(12) . ? C13 C14 1.374(13) . ? C14 C15 1.370(14) . ? C15 C16 1.394(12) . ? C22 C23 1.367(13) . ? C22 C32 1.500(12) . ? C23 C24 1.378(13) . ? C24 C25 1.379(13) . ? C25 C26 1.396(13) . ? C32 C33 1.399(12) . ? C33 C34 1.391(14) . ? C34 C35 1.396(14) . ? C35 C36 1.386(12) . ? C41 C42 1.376(12) . ? C41 C46 1.400(13) . ? C42 C43 1.398(12) . ? C43 C44 1.371(13) . ? C44 C45 1.377(14) . ? C45 C46 1.400(13) . ? C51 C56 1.387(12) . ? C51 C52 1.394(13) . ? C52 C53 1.414(13) . ? C53 C54 1.402(13) . ? C54 C55 1.388(14) . ? C55 C56 1.373(13) . ? 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 N11 Ni1 N21 96.9(3) . . ? N11 Ni1 N1 79.5(3) . . ? N21 Ni1 N1 94.8(3) . . ? N11 Ni1 N31 94.3(3) . . ? N21 Ni1 N31 79.1(3) . . ? N1 Ni1 N31 170.8(3) . . ? N11 Ni1 O1 172.1(3) . . ? N21 Ni1 O1 88.6(3) . . ? N1 Ni1 O1 94.4(3) . . ? N31 Ni1 O1 92.3(3) . . ? N11 Ni1 S4 90.0(2) . . ? N21 Ni1 S4 173.1(2) . . ? N1 Ni1 S4 86.1(2) . . ? N31 Ni1 S4 100.7(2) . . ? O1 Ni1 S4 84.48(17) . . ? S1 Ni2 S4 86.83(10) . . ? S1 Ni2 S2 91.34(10) . . ? S4 Ni2 S2 175.90(11) . . ? S1 Ni2 S3 179.19(11) . . ? S4 Ni2 S3 92.36(10) . . ? S2 Ni2 S3 89.47(10) . . ? O2 S1 O1 112.8(4) . . ? O2 S1 C41 105.3(4) . . ? O1 S1 C41 104.6(4) . . ? O2 S1 Ni2 114.6(3) . . ? O1 S1 Ni2 111.8(3) . . ? C41 S1 Ni2 106.8(3) . . ? O3 S2 O4 120.0(9) . . ? O3 S2 C42 107.4(7) . . ? O4 S2 C42 103.3(6) . . ? O3 S2 Ni2 117.8(6) . . ? O4 S2 Ni2 101.8(6) . . ? C42 S2 Ni2 104.7(3) . . ? C52 S3 Ni2 104.0(3) . . ? C51 S4 Ni2 105.0(3) . . ? C51 S4 Ni1 120.2(3) . . ? Ni2 S4 Ni1 101.85(10) . . ? S1 O1 Ni1 122.8(4) . . ? C6 N1 C2 117.7(8) . . ? C6 N1 Ni1 127.1(6) . . ? C2 N1 Ni1 114.5(6) . . ? C16 N11 C12 118.6(7) . . ? C16 N11 Ni1 126.4(6) . . ? C12 N11 Ni1 114.8(6) . . ? C26 N21 C22 117.2(8) . . ? C26 N21 Ni1 126.7(6) . . ? C22 N21 Ni1 116.0(6) . . ? C32 N31 C36 117.5(8) . . ? C32 N31 Ni1 115.3(6) . . ? C36 N31 Ni1 127.2(6) . . ? N1 C2 C3 120.3(9) . . ? N1 C2 C12 114.6(8) . . ? C3 C2 C12 125.1(9) . . ? C4 C3 C2 119.6(9) . . ? C5 C4 C3 120.8(9) . . ? C4 C5 C6 118.1(9) . . ? N1 C6 C5 123.5(9) . . ? N11 C12 C13 119.3(8) . . ? N11 C12 C2 116.1(8) . . ? C13 C12 C2 124.6(8) . . ? C14 C13 C12 122.2(9) . . ? C15 C14 C13 118.2(9) . . ? C14 C15 C16 118.6(9) . . ? N11 C16 C15 123.0(9) . . ? N21 C22 C23 122.3(9) . . ? N21 C22 C32 114.4(8) . . ? C23 C22 C32 123.3(8) . . ? C22 C23 C24 119.6(9) . . ? C23 C24 C25 119.9(9) . . ? C24 C25 C26 117.1(9) . . ? N21 C26 C25 123.8(9) . . ? N31 C32 C33 123.2(8) . . ? N31 C32 C22 115.1(7) . . ? C33 C32 C22 121.8(9) . . ? C34 C33 C32 118.5(9) . . ? C33 C34 C35 118.8(9) . . ? C36 C35 C34 119.1(9) . . ? N31 C36 C35 122.9(9) . . ? C42 C41 C46 122.1(8) . . ? C42 C41 S1 116.9(7) . . ? C46 C41 S1 120.8(7) . . ? C41 C42 C43 119.1(9) . . ? C41 C42 S2 119.6(7) . . ? C43 C42 S2 121.4(7) . . ? C44 C43 C42 119.5(10) . . ? C43 C44 C45 121.6(10) . . ? C44 C45 C46 120.1(9) . . ? C41 C46 C45 117.6(9) . . ? C56 C51 C52 121.2(8) . . ? C56 C51 S4 121.2(7) . . ? C52 C51 S4 117.4(7) . . ? C51 C52 C53 119.6(9) . . ? C51 C52 S3 120.7(7) . . ? C53 C52 S3 119.7(8) . . ? C54 C53 C52 118.2(9) . . ? C55 C54 C53 120.8(9) . . ? C56 C55 C54 120.9(9) . . ? C55 C56 C51 119.3(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.308 _refine_diff_density_min -1.149 _refine_diff_density_rms 0.159 #=END # ----data for compound 3--------- data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.50 H20 N4.50 Ni O6.50 S2' _chemical_formula_weight 640.31 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.31350(10) _cell_length_b 12.5526(2) _cell_length_c 12.7451(2) _cell_angle_alpha 96.0170(10) _cell_angle_beta 101.8868(3) _cell_angle_gamma 110.0760(10) _cell_volume 1344.26(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5387 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 657 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.770 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14865 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.1084 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6302 _reflns_number_gt 4041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+2.4213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6302 _refine_ls_number_parameters 376 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1254 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.005 _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 0.83181(7) 0.16391(5) 0.79732(4) 0.01960(15) Uani 1 1 d . . . S1 S 1.00110(16) 0.28935(10) 0.60544(9) 0.0309(3) Uani 1 1 d . . . S2 S 1.20668(13) 0.30038(9) 0.87085(8) 0.0209(2) Uani 1 1 d . . . O1 O 0.9081(4) 0.2076(2) 0.6614(2) 0.0256(7) Uani 1 1 d . . . O2 O 1.0513(4) 0.2640(2) 0.8978(2) 0.0229(7) Uani 1 1 d . . . O3 O 1.1068(5) 0.2453(3) 0.5623(3) 0.0532(11) Uani 1 1 d . . . O4 O 0.9063(5) 0.3255(3) 0.5259(3) 0.0645(14) Uani 1 1 d . . . O5 O 1.2188(4) 0.2137(2) 0.7940(2) 0.0255(7) Uani 1 1 d . . . O6 O 1.3330(4) 0.3426(3) 0.9704(2) 0.0275(7) Uani 1 1 d . . . N1 N 0.7689(4) 0.0996(3) 0.9316(3) 0.0204(8) Uani 1 1 d . . . N11 N 0.8811(4) 0.0155(3) 0.7829(3) 0.0224(8) Uani 1 1 d . . . N21 N 0.6021(4) 0.0860(3) 0.7003(3) 0.0214(8) Uani 1 1 d . . . N31 N 0.7563(4) 0.2998(3) 0.8082(3) 0.0232(8) Uani 1 1 d . . . C2 C 0.7786(5) -0.0046(4) 0.9399(3) 0.0225(9) Uani 1 1 d . . . C3 C 0.7381(6) -0.0591(4) 1.0240(4) 0.0304(11) Uani 1 1 d . . . H3A H 0.7431 -0.1331 1.0274 0.036 Uiso 1 1 calc R . . C4 C 0.6904(6) -0.0066(4) 1.1032(4) 0.0322(11) Uani 1 1 d . . . H4A H 0.6643 -0.0427 1.1622 0.039 Uiso 1 1 calc R . . C5 C 0.6813(6) 0.0992(4) 1.0949(4) 0.0313(11) Uani 1 1 d . . . H5A H 0.6480 0.1373 1.1479 0.038 Uiso 1 1 calc R . . C6 C 0.7214(6) 0.1495(4) 1.0079(3) 0.0280(11) Uani 1 1 d . . . H6A H 0.7147 0.2227 1.0025 0.034 Uiso 1 1 calc R . . C12 C 0.8389(5) -0.0528(4) 0.8549(3) 0.0230(9) Uani 1 1 d . . . C13 C 0.8515(6) -0.1602(4) 0.8489(4) 0.0310(11) Uani 1 1 d . . . H13A H 0.8223 -0.2066 0.9011 0.037 Uiso 1 1 calc R . . C14 C 0.9066(6) -0.1982(4) 0.7665(4) 0.0366(12) Uani 1 1 d . . . H14A H 0.9144 -0.2720 0.7604 0.044 Uiso 1 1 calc R . . C15 C 0.9509(6) -0.1286(4) 0.6924(4) 0.0356(12) Uani 1 1 d . . . H15A H 0.9889 -0.1538 0.6346 0.043 Uiso 1 1 calc R . . C16 C 0.9385(6) -0.0215(4) 0.7043(3) 0.0278(10) Uani 1 1 d . . . H16A H 0.9718 0.0276 0.6550 0.033 Uiso 1 1 calc R . . C22 C 0.5212(5) 0.1560(4) 0.6864(3) 0.0236(10) Uani 1 1 d . . . C23 C 0.3652(6) 0.1161(4) 0.6231(3) 0.0295(11) Uani 1 1 d . . . H23A H 0.3096 0.1668 0.6149 0.035 Uiso 1 1 calc R . . C24 C 0.2935(6) 0.0014(4) 0.5727(4) 0.0327(11) Uani 1 1 d . . . H24A H 0.1875 -0.0279 0.5289 0.039 Uiso 1 1 calc R . . C25 C 0.3766(6) -0.0707(4) 0.5864(3) 0.0300(11) Uani 1 1 d . . . H25A H 0.3290 -0.1499 0.5522 0.036 Uiso 1 1 calc R . . C26 C 0.5296(6) -0.0256(4) 0.6504(3) 0.0272(10) Uani 1 1 d . . . H26A H 0.5866 -0.0753 0.6599 0.033 Uiso 1 1 calc R . . C32 C 0.6086(5) 0.2773(4) 0.7462(3) 0.0236(10) Uani 1 1 d . . . C33 C 0.5452(6) 0.3624(4) 0.7423(4) 0.0313(11) Uani 1 1 d . . . H33A H 0.4411 0.3453 0.6991 0.038 Uiso 1 1 calc R . . C34 C 0.6354(6) 0.4724(4) 0.8022(4) 0.0376(12) Uani 1 1 d . . . H34A H 0.5940 0.5318 0.8003 0.045 Uiso 1 1 calc R . . C35 C 0.7857(6) 0.4950(4) 0.8643(4) 0.0331(11) Uani 1 1 d . . . H35A H 0.8492 0.5700 0.9062 0.040 Uiso 1 1 calc R . . C36 C 0.8425(6) 0.4072(4) 0.8649(3) 0.0286(10) Uani 1 1 d . . . H36A H 0.9469 0.4233 0.9071 0.034 Uiso 1 1 calc R . . C41 C 1.1264(5) 0.4180(4) 0.7034(3) 0.0247(10) Uani 1 1 d . . . C42 C 1.2176(5) 0.4227(3) 0.8081(3) 0.0197(9) Uani 1 1 d . . . C43 C 1.3244(5) 0.5288(4) 0.8695(3) 0.0238(10) Uani 1 1 d . . . H43A H 1.3846 0.5324 0.9406 0.029 Uiso 1 1 calc R . . C44 C 1.3445(6) 0.6293(4) 0.8289(4) 0.0302(11) Uani 1 1 d . . . H44A H 1.4219 0.7006 0.8705 0.036 Uiso 1 1 calc R . . C45 C 1.2526(6) 0.6261(4) 0.7284(4) 0.0349(12) Uani 1 1 d . . . H45A H 1.2637 0.6954 0.7013 0.042 Uiso 1 1 calc R . . C46 C 1.1439(6) 0.5211(4) 0.6668(4) 0.0335(12) Uani 1 1 d . . . H46A H 1.0796 0.5196 0.5978 0.040 Uiso 1 1 calc R . . O1S O 0.5382(13) 0.7221(9) 0.5737(8) 0.085(3) Uiso 0.50 1 d P . . N1S N 0.4733(12) 0.5397(8) 0.5060(8) 0.088(3) Uiso 0.50 1 d PD . . C1S C 0.587(2) 0.6415(14) 0.5539(17) 0.046(6) Uiso 0.25 1 d PD . . C2S C 0.307(3) 0.508(2) 0.4584(19) 0.052(6) Uiso 0.25 1 d P . . C3S C 0.4733(12) 0.5397(8) 0.5060(8) 0.088(3) Uiso 0.25 1 d P . . C1S' C 0.440(3) 0.6346(17) 0.523(2) 0.064(7) Uiso 0.25 1 d PD . . C2S' C 0.649(2) 0.5609(16) 0.5391(13) 0.089(5) Uiso 0.50 1 d P . . 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 0.0192(3) 0.0186(3) 0.0181(3) 0.0039(2) 0.0023(2) 0.0048(2) S1 0.0371(8) 0.0245(6) 0.0175(5) 0.0049(5) -0.0007(5) -0.0007(6) S2 0.0213(6) 0.0187(5) 0.0187(5) 0.0033(4) 0.0015(4) 0.0046(5) O1 0.0291(19) 0.0213(16) 0.0184(15) 0.0038(12) 0.0052(13) -0.0001(15) O2 0.0245(18) 0.0218(16) 0.0181(14) 0.0033(12) 0.0036(13) 0.0046(14) O3 0.049(3) 0.056(3) 0.039(2) -0.0163(18) 0.0233(19) 0.002(2) O4 0.071(3) 0.031(2) 0.050(2) 0.0165(18) -0.031(2) -0.007(2) O5 0.0289(19) 0.0199(16) 0.0262(16) 0.0018(13) 0.0056(14) 0.0088(15) O6 0.0261(19) 0.0254(17) 0.0226(16) 0.0046(13) -0.0044(13) 0.0056(15) N1 0.020(2) 0.0201(18) 0.0191(18) 0.0020(14) 0.0014(15) 0.0074(17) N11 0.017(2) 0.0233(19) 0.0206(18) 0.0006(15) -0.0001(15) 0.0039(17) N21 0.022(2) 0.0204(19) 0.0163(17) 0.0010(14) 0.0023(15) 0.0038(17) N31 0.024(2) 0.0226(19) 0.0199(18) 0.0036(15) 0.0039(15) 0.0062(17) C2 0.022(2) 0.023(2) 0.021(2) 0.0077(18) 0.0029(18) 0.008(2) C3 0.038(3) 0.030(3) 0.029(2) 0.013(2) 0.008(2) 0.017(2) C4 0.040(3) 0.039(3) 0.023(2) 0.016(2) 0.012(2) 0.017(3) C5 0.035(3) 0.034(3) 0.026(2) 0.005(2) 0.011(2) 0.014(2) C6 0.036(3) 0.024(2) 0.024(2) 0.0038(19) 0.006(2) 0.013(2) C12 0.022(2) 0.023(2) 0.022(2) 0.0039(18) 0.0040(18) 0.007(2) C13 0.042(3) 0.025(2) 0.028(2) 0.008(2) 0.009(2) 0.014(2) C14 0.050(4) 0.028(3) 0.038(3) 0.004(2) 0.013(3) 0.020(3) C15 0.041(3) 0.036(3) 0.027(3) 0.001(2) 0.007(2) 0.013(3) C16 0.030(3) 0.028(2) 0.024(2) 0.0048(19) 0.007(2) 0.009(2) C22 0.025(3) 0.027(2) 0.016(2) 0.0037(18) 0.0051(18) 0.006(2) C23 0.024(3) 0.041(3) 0.024(2) 0.005(2) 0.0033(19) 0.014(2) C24 0.021(3) 0.044(3) 0.023(2) 0.003(2) -0.0001(19) 0.003(2) C25 0.026(3) 0.027(2) 0.022(2) 0.0014(19) -0.001(2) -0.003(2) C26 0.027(3) 0.028(2) 0.021(2) 0.0031(19) 0.0024(19) 0.007(2) C32 0.025(3) 0.030(2) 0.019(2) 0.0079(18) 0.0094(18) 0.010(2) C33 0.022(3) 0.034(3) 0.043(3) 0.010(2) 0.010(2) 0.014(2) C34 0.038(3) 0.032(3) 0.055(3) 0.011(2) 0.019(3) 0.023(3) C35 0.039(3) 0.024(2) 0.034(3) 0.001(2) 0.012(2) 0.008(2) C36 0.028(3) 0.027(2) 0.024(2) 0.0021(19) 0.004(2) 0.005(2) C41 0.028(3) 0.024(2) 0.020(2) 0.0063(18) 0.0067(19) 0.006(2) C42 0.018(2) 0.018(2) 0.022(2) 0.0039(17) 0.0069(18) 0.0049(19) C43 0.023(3) 0.025(2) 0.021(2) 0.0013(18) 0.0028(18) 0.008(2) C44 0.031(3) 0.021(2) 0.030(2) -0.0019(19) 0.003(2) 0.004(2) C45 0.047(3) 0.021(2) 0.031(3) 0.009(2) 0.004(2) 0.007(2) C46 0.041(3) 0.028(3) 0.024(2) 0.008(2) -0.001(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.054(3) . ? Ni1 N31 2.059(4) . ? Ni1 O1 2.060(3) . ? Ni1 N11 2.066(4) . ? Ni1 N21 2.069(4) . ? Ni1 N1 2.075(3) . ? S1 O4 1.420(4) . ? S1 O3 1.452(4) . ? S1 O1 1.452(3) . ? S1 C41 1.792(4) . ? S2 O5 1.436(3) . ? S2 O6 1.446(3) . ? S2 O2 1.485(3) . ? S2 C42 1.786(4) . ? N1 C6 1.332(5) . ? N1 C2 1.355(5) . ? N11 C16 1.341(5) . ? N11 C12 1.346(5) . ? N21 C22 1.343(5) . ? N21 C26 1.345(5) . ? N31 C36 1.340(5) . ? N31 C32 1.355(5) . ? C2 C3 1.380(6) . ? C2 C12 1.483(6) . ? C3 C4 1.377(6) . ? C4 C5 1.373(6) . ? C5 C6 1.386(6) . ? C12 C13 1.389(6) . ? C13 C14 1.371(6) . ? C14 C15 1.383(7) . ? C15 C16 1.384(6) . ? C22 C23 1.395(6) . ? C22 C32 1.487(6) . ? C23 C24 1.379(6) . ? C24 C25 1.381(7) . ? C25 C26 1.374(6) . ? C32 C33 1.387(6) . ? C33 C34 1.384(7) . ? C34 C35 1.374(7) . ? C35 C36 1.377(6) . ? C41 C46 1.391(6) . ? C41 C42 1.410(6) . ? C42 C43 1.388(6) . ? C43 C44 1.380(6) . ? C44 C45 1.375(6) . ? C45 C46 1.384(6) . ? O1S C1S' 1.17(3) . ? O1S C1S 1.27(2) . ? N1S C3S 1.267(17) 2_666 ? N1S N1S 1.267(17) 2_666 ? N1S C1S 1.330(10) . ? N1S C1S' 1.338(10) . ? N1S C2S' 1.347(18) 2_666 ? N1S C2S 1.44(3) . ? N1S C2S' 1.52(2) . ? C1S C1S' 1.31(3) . ? C1S C2S' 1.34(3) . ? C2S C2S' 1.08(3) 2_666 ? C2S C1S' 1.64(4) . ? C2S' C2S 1.08(3) 2_666 ? C2S' C3S 1.347(18) 2_666 ? C2S' N1S 1.347(18) 2_666 ? 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 O2 Ni1 N31 91.76(13) . . ? O2 Ni1 O1 90.97(12) . . ? N31 Ni1 O1 90.79(13) . . ? O2 Ni1 N11 94.03(13) . . ? N31 Ni1 N11 173.54(15) . . ? O1 Ni1 N11 91.98(13) . . ? O2 Ni1 N21 170.95(13) . . ? N31 Ni1 N21 79.19(14) . . ? O1 Ni1 N21 89.49(13) . . ? N11 Ni1 N21 94.99(14) . . ? O2 Ni1 N1 88.43(12) . . ? N31 Ni1 N1 98.19(13) . . ? O1 Ni1 N1 171.01(13) . . ? N11 Ni1 N1 79.12(14) . . ? N21 Ni1 N1 92.52(14) . . ? O4 S1 O3 113.2(3) . . ? O4 S1 O1 112.7(2) . . ? O3 S1 O1 111.0(2) . . ? O4 S1 C41 105.3(2) . . ? O3 S1 C41 105.8(2) . . ? O1 S1 C41 108.36(18) . . ? O5 S2 O6 114.49(19) . . ? O5 S2 O2 113.02(18) . . ? O6 S2 O2 109.70(17) . . ? O5 S2 C42 108.00(18) . . ? O6 S2 C42 105.99(19) . . ? O2 S2 C42 104.94(18) . . ? S1 O1 Ni1 151.98(19) . . ? S2 O2 Ni1 128.38(16) . . ? C6 N1 C2 118.4(4) . . ? C6 N1 Ni1 127.0(3) . . ? C2 N1 Ni1 114.6(3) . . ? C16 N11 C12 118.6(4) . . ? C16 N11 Ni1 125.8(3) . . ? C12 N11 Ni1 115.4(3) . . ? C22 N21 C26 118.4(4) . . ? C22 N21 Ni1 115.4(3) . . ? C26 N21 Ni1 126.2(3) . . ? C36 N31 C32 118.7(4) . . ? C36 N31 Ni1 126.0(3) . . ? C32 N31 Ni1 115.1(3) . . ? N1 C2 C3 121.2(4) . . ? N1 C2 C12 115.5(4) . . ? C3 C2 C12 123.3(4) . . ? C4 C3 C2 120.1(4) . . ? C5 C4 C3 118.6(4) . . ? C4 C5 C6 119.0(4) . . ? N1 C6 C5 122.7(4) . . ? N11 C12 C13 121.8(4) . . ? N11 C12 C2 115.1(4) . . ? C13 C12 C2 123.1(4) . . ? C14 C13 C12 119.0(4) . . ? C13 C14 C15 119.7(4) . . ? C14 C15 C16 118.4(4) . . ? N11 C16 C15 122.5(4) . . ? N21 C22 C23 122.0(4) . . ? N21 C22 C32 115.0(4) . . ? C23 C22 C32 123.0(4) . . ? C24 C23 C22 118.5(4) . . ? C23 C24 C25 119.6(4) . . ? C26 C25 C24 118.7(4) . . ? N21 C26 C25 122.7(4) . . ? N31 C32 C33 121.2(4) . . ? N31 C32 C22 115.2(4) . . ? C33 C32 C22 123.6(4) . . ? C34 C33 C32 119.2(4) . . ? C35 C34 C33 119.4(4) . . ? C34 C35 C36 118.9(5) . . ? N31 C36 C35 122.6(5) . . ? C46 C41 C42 118.3(4) . . ? C46 C41 S1 115.4(3) . . ? C42 C41 S1 126.0(3) . . ? C43 C42 C41 119.3(4) . . ? C43 C42 S2 115.9(3) . . ? C41 C42 S2 124.8(3) . . ? C44 C43 C42 121.1(4) . . ? C45 C44 C43 120.0(4) . . ? C44 C45 C46 119.5(4) . . ? C45 C46 C41 121.6(4) . . ? C1S' O1S C1S 65.1(14) . . ? C3S N1S N1S 0.0(10) 2_666 2_666 ? C3S N1S C1S 112.4(16) 2_666 . ? N1S N1S C1S 112.4(16) 2_666 . ? C3S N1S C1S' 171(2) 2_666 . ? N1S N1S C1S' 171(2) 2_666 . ? C1S N1S C1S' 59.0(16) . . ? C3S N1S C2S' 71.2(11) 2_666 2_666 ? N1S N1S C2S' 71.2(11) 2_666 2_666 ? C1S N1S C2S' 175.9(15) . 2_666 ? C1S' N1S C2S' 117.4(18) . 2_666 ? C3S N1S C2S 116.2(15) 2_666 . ? N1S N1S C2S 116.2(15) 2_666 . ? C1S N1S C2S 131.2(16) . . ? C1S' N1S C2S 72.3(17) . . ? C2S' N1S C2S 45.5(11) 2_666 . ? C3S N1S C2S' 56.8(9) 2_666 . ? N1S N1S C2S' 56.8(9) 2_666 . ? C1S N1S C2S' 55.6(12) . . ? C1S' N1S C2S' 114.5(17) . . ? C2S' N1S C2S' 128.1(10) 2_666 . ? C2S N1S C2S' 170.4(14) . . ? O1S C1S C1S' 54.1(13) . . ? O1S C1S N1S 114.6(17) . . ? C1S' C1S N1S 60.8(10) . . ? O1S C1S C2S' 175.5(18) . . ? C1S' C1S C2S' 130.2(15) . . ? N1S C1S C2S' 69.6(12) . . ? C2S' C2S N1S 62.9(16) 2_666 . ? C2S' C2S C1S' 114(2) 2_666 . ? N1S C2S C1S' 51.1(10) . . ? O1S C1S' C1S 60.9(17) . . ? O1S C1S' N1S 121(2) . . ? C1S C1S' N1S 60.2(9) . . ? O1S C1S' C2S 177(2) . . ? C1S C1S' C2S 116.7(13) . . ? N1S C1S' C2S 56.6(13) . . ? C2S C2S' C1S 169(2) 2_666 . ? C2S C2S' C3S 71.6(17) 2_666 2_666 ? C1S C2S' C3S 106.7(15) . 2_666 ? C2S C2S' N1S 71.6(17) 2_666 2_666 ? C1S C2S' N1S 106.7(15) . 2_666 ? C3S C2S' N1S 0.0(9) 2_666 2_666 ? C2S C2S' N1S 123(2) 2_666 . ? C1S C2S' N1S 54.8(8) . . ? C3S C2S' N1S 51.9(10) 2_666 . ? N1S C2S' N1S 51.9(10) 2_666 . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.954 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.107