Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Berthold Kersting' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Leipzig Johannisallee 29 Leipzig 04103 GERMANY ; _publ_contact_author_email B.KERSTING@UNI-LEIPZIG.DE _publ_section_title ; Preparation and Characterization of Mononuclear Co, Ni and Zn Complexes of Dinucleating Macrocyclic Hexaazadithiophenolate Ligands and their Open-Chein Derivatives ; loop_ _publ_author_name 'Berthold Kersting' 'Thorsten Fritz' 'Steffen Kass' 'Gunther Steinfeld' data_4 _database_code_depnum_ccdc_archive 'CCDC 601289' _chemical_formula_structural ; [Ni(L4)] ; _chemical_formula_sum 'C18 H23 N3 Ni S2' _chemical_formula_weight 404.22 _chemical_melting_point ? _chemical_compound_source ; Crystals were taken from the mother liquor. ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.799(2) _cell_length_b 13.289(3) _cell_length_c 12.474(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.68(3) _cell_angle_gamma 90.00 _cell_volume 1778.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 180 _cell_measurement_theta_min 8 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.510 _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.331 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS, SHELDRICK, 1996)' _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11219 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.1199 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.33 _reflns_number_total 4239 _reflns_number_gt 2125 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA _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^)+(0.0373P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4239 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.625 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.117 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.19173(5) 0.21236(4) 0.26382(4) 0.02139(16) Uani 1 1 d . . . S1 S 0.33123(11) 0.20625(10) 0.13867(9) 0.0335(3) Uani 1 1 d . . . S2 S 0.08636(11) 0.33046(8) 0.35892(9) 0.0242(3) Uani 1 1 d . . . N1 N 0.3305(3) 0.1959(3) 0.3957(3) 0.0241(8) Uani 1 1 d . . . H1 H 0.3099 0.2398 0.4468 0.029 Uiso 1 1 calc R . . N2 N 0.1331(3) 0.0762(3) 0.3130(3) 0.0238(9) Uani 1 1 d . . . H2 H 0.1669 0.0266 0.2753 0.029 Uiso 1 1 calc R . . N3 N 0.0397(3) 0.1945(3) 0.1420(3) 0.0232(8) Uani 1 1 d . . . H3 H 0.0736 0.1797 0.0804 0.028 Uiso 1 1 calc R . . C1 C 0.4643(4) 0.1413(3) 0.1936(3) 0.0231(10) Uani 1 1 d . . . C2 C 0.5265(4) 0.0780(3) 0.1258(4) 0.0295(11) Uani 1 1 d . . . H2A H 0.4982 0.0748 0.0526 0.035 Uiso 1 1 calc R . . C3 C 0.6278(4) 0.0214(4) 0.1659(4) 0.0338(12) Uani 1 1 d . . . H3A H 0.6662 -0.0204 0.1198 0.041 Uiso 1 1 calc R . . C4 C 0.6730(4) 0.0260(4) 0.2738(4) 0.0347(12) Uani 1 1 d . . . H4 H 0.7404 -0.0136 0.3010 0.042 Uiso 1 1 calc R . . C5 C 0.6170(4) 0.0903(3) 0.3412(4) 0.0303(11) Uani 1 1 d . . . H5 H 0.6487 0.0945 0.4136 0.036 Uiso 1 1 calc R . . C6 C 0.5148(4) 0.1485(3) 0.3031(3) 0.0243(10) Uani 1 1 d . . . C7 C 0.4598(4) 0.2203(3) 0.3790(3) 0.0249(10) Uani 1 1 d . . . H7A H 0.5110 0.2193 0.4482 0.030 Uiso 1 1 calc R . . H7B H 0.4622 0.2880 0.3502 0.030 Uiso 1 1 calc R . . C8 C 0.3169(4) 0.0939(3) 0.4418(4) 0.0270(11) Uani 1 1 d . . . H8A H 0.3491 0.0935 0.5177 0.032 Uiso 1 1 calc R . . H8B H 0.3636 0.0453 0.4046 0.032 Uiso 1 1 calc R . . C9 C 0.1793(4) 0.0665(3) 0.4281(3) 0.0248(10) Uani 1 1 d . . . H9A H 0.1681 -0.0020 0.4522 0.030 Uiso 1 1 calc R . . H9B H 0.1336 0.1113 0.4706 0.030 Uiso 1 1 calc R . . C10 C -0.0035(4) 0.0759(3) 0.2860(3) 0.0272(11) Uani 1 1 d . . . H10A H -0.0413 0.1243 0.3306 0.033 Uiso 1 1 calc R . . H10B H -0.0368 0.0098 0.2990 0.033 Uiso 1 1 calc R . . C11 C -0.0323(4) 0.1037(3) 0.1673(4) 0.0278(11) Uani 1 1 d . . . H11A H -0.0111 0.0478 0.1229 0.033 Uiso 1 1 calc R . . H11B H -0.1209 0.1169 0.1509 0.033 Uiso 1 1 calc R . . C12 C -0.0375(4) 0.2857(3) 0.1176(3) 0.0255(10) Uani 1 1 d . . . H12A H -0.0887 0.2756 0.0493 0.031 Uiso 1 1 calc R . . H12B H 0.0175 0.3420 0.1087 0.031 Uiso 1 1 calc R . . C13 C -0.1216(4) 0.3137(3) 0.2015(3) 0.0208(10) Uani 1 1 d . . . C14 C -0.2485(4) 0.3217(3) 0.1698(4) 0.0298(11) Uani 1 1 d . . . H14 H -0.2801 0.3009 0.1008 0.036 Uiso 1 1 calc R . . C15 C -0.3293(4) 0.3597(3) 0.2376(4) 0.0328(12) Uani 1 1 d . . . H15 H -0.4137 0.3671 0.2139 0.039 Uiso 1 1 calc R . . C16 C -0.2822(4) 0.3866(3) 0.3419(4) 0.0316(12) Uani 1 1 d . . . H16 H -0.3354 0.4122 0.3887 0.038 Uiso 1 1 calc R . . C17 C -0.1577(4) 0.3756(3) 0.3763(4) 0.0268(11) Uani 1 1 d . . . H17 H -0.1283 0.3931 0.4469 0.032 Uiso 1 1 calc R . . C18 C -0.0723(4) 0.3385(3) 0.3076(3) 0.0196(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0229(3) 0.0215(3) 0.0200(3) 0.0010(3) 0.0035(2) 0.0010(3) S1 0.0269(7) 0.0544(8) 0.0199(6) 0.0083(6) 0.0054(5) 0.0106(6) S2 0.0260(7) 0.0221(6) 0.0241(6) -0.0033(5) 0.0014(5) 0.0028(5) N1 0.026(2) 0.025(2) 0.0210(19) -0.0029(16) 0.0028(16) -0.0005(16) N2 0.025(2) 0.027(2) 0.019(2) -0.0035(16) 0.0052(16) -0.0012(16) N3 0.024(2) 0.022(2) 0.0243(19) -0.0037(16) 0.0042(16) 0.0050(16) C1 0.022(3) 0.022(2) 0.026(2) 0.0011(19) 0.0040(19) -0.0020(19) C2 0.029(3) 0.029(3) 0.031(3) -0.005(2) 0.007(2) -0.003(2) C3 0.031(3) 0.028(3) 0.044(3) -0.007(2) 0.015(2) -0.004(2) C4 0.022(3) 0.036(3) 0.046(3) 0.003(3) 0.002(2) 0.006(2) C5 0.025(3) 0.032(3) 0.033(3) 0.005(2) 0.000(2) 0.004(2) C6 0.024(3) 0.025(3) 0.025(2) 0.0013(19) 0.006(2) -0.0020(19) C7 0.021(2) 0.030(3) 0.023(2) -0.004(2) -0.0003(18) -0.003(2) C8 0.029(3) 0.028(3) 0.023(2) 0.000(2) 0.000(2) 0.002(2) C9 0.030(3) 0.023(3) 0.022(2) 0.0023(19) 0.008(2) 0.0014(19) C10 0.029(3) 0.021(3) 0.031(3) 0.000(2) 0.005(2) -0.001(2) C11 0.029(3) 0.022(3) 0.031(3) -0.003(2) -0.005(2) -0.002(2) C12 0.032(3) 0.023(2) 0.022(2) 0.006(2) 0.0035(19) 0.001(2) C13 0.021(2) 0.018(2) 0.023(2) 0.0028(18) 0.0022(18) 0.0035(17) C14 0.032(3) 0.025(3) 0.032(3) 0.006(2) 0.002(2) 0.004(2) C15 0.025(3) 0.034(3) 0.039(3) 0.013(2) 0.001(2) 0.002(2) C16 0.028(3) 0.034(3) 0.034(3) 0.005(2) 0.011(2) 0.006(2) C17 0.031(3) 0.027(3) 0.023(2) 0.007(2) 0.004(2) 0.004(2) C18 0.021(2) 0.012(2) 0.026(2) 0.0020(18) 0.0041(19) -0.0011(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N2 2.036(3) . ? Ni N1 2.104(4) . ? Ni N3 2.117(4) . ? Ni S1 2.2936(13) . ? Ni S2 2.3407(13) . ? S1 C1 1.747(4) . ? S2 C18 1.762(4) . ? N1 C7 1.472(5) . ? N1 C8 1.486(5) . ? N2 C9 1.469(5) . ? N2 C10 1.475(5) . ? N3 C12 1.483(5) . ? N3 C11 1.490(5) . ? C1 C6 1.414(6) . ? C1 C2 1.416(6) . ? C2 C3 1.373(6) . ? C3 C4 1.379(6) . ? C4 C5 1.387(6) . ? C5 C6 1.386(6) . ? C6 C7 1.513(6) . ? C8 C9 1.521(6) . ? C10 C11 1.523(6) . ? C12 C13 1.510(5) . ? C13 C14 1.385(6) . ? C13 C18 1.406(6) . ? C14 C15 1.379(6) . ? C15 C16 1.387(6) . ? C16 C17 1.370(6) . ? C17 C18 1.419(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni N1 83.68(14) . . ? N2 Ni N3 82.79(13) . . ? N1 Ni N3 166.44(13) . . ? N2 Ni S1 115.19(10) . . ? N1 Ni S1 93.68(10) . . ? N3 Ni S1 91.32(10) . . ? N2 Ni S2 104.89(10) . . ? N1 Ni S2 91.00(10) . . ? N3 Ni S2 93.28(10) . . ? S1 Ni S2 139.92(5) . . ? C1 S1 Ni 109.03(15) . . ? C18 S2 Ni 111.46(14) . . ? C7 N1 C8 113.2(3) . . ? C7 N1 Ni 117.9(3) . . ? C8 N1 Ni 107.7(3) . . ? C9 N2 C10 116.1(3) . . ? C9 N2 Ni 106.9(3) . . ? C10 N2 Ni 105.7(3) . . ? C12 N3 C11 114.2(3) . . ? C12 N3 Ni 115.2(3) . . ? C11 N3 Ni 108.6(3) . . ? C6 C1 C2 117.4(4) . . ? C6 C1 S1 123.5(3) . . ? C2 C1 S1 119.0(3) . . ? C3 C2 C1 121.5(4) . . ? C2 C3 C4 120.5(4) . . ? C3 C4 C5 119.3(5) . . ? C6 C5 C4 121.5(4) . . ? C5 C6 C1 119.7(4) . . ? C5 C6 C7 119.5(4) . . ? C1 C6 C7 120.8(4) . . ? N1 C7 C6 113.4(3) . . ? N1 C8 C9 108.3(3) . . ? N2 C9 C8 107.8(3) . . ? N2 C10 C11 107.9(3) . . ? N3 C11 C10 110.5(4) . . ? N3 C12 C13 115.4(3) . . ? C14 C13 C18 120.3(4) . . ? C14 C13 C12 118.4(4) . . ? C18 C13 C12 121.1(4) . . ? C15 C14 C13 121.8(4) . . ? C14 C15 C16 118.7(4) . . ? C17 C16 C15 120.4(4) . . ? C16 C17 C18 122.0(4) . . ? C13 C18 C17 116.6(4) . . ? C13 C18 S2 125.0(3) . . ? C17 C18 S2 118.3(3) . . ? #===END # Attachment 'CCDC_601290n.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 601290' _chemical_formula_structural ; [Ni(L5)] ; _chemical_formula_sum 'C21 H29 N3 Ni S2' _chemical_formula_weight 446.30 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown from acetonitrile. ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.320(4) _cell_length_b 7.583(2) _cell_length_c 15.183(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.70(3) _cell_angle_gamma 90.00 _cell_volume 2094.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 138 _cell_measurement_theta_min 10 _cell_measurement_theta_max 24 _exptl_crystal_description red _exptl_crystal_colour block _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.415 _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS, Sheldrick, 1996)' _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12760 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.1223 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4931 _reflns_number_gt 2489 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA _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^)+(0.0392P)^2^+1.2582P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4931 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.644 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.108 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.25153(3) 0.21330(8) 0.16465(4) 0.02372(16) Uani 1 1 d . . . S1 S 0.33430(7) 0.39164(16) 0.10417(8) 0.0317(3) Uani 1 1 d . . . S2 S 0.20486(7) 0.33539(18) 0.28432(8) 0.0399(4) Uani 1 1 d . . . N1 N 0.3335(2) 0.0592(5) 0.2493(2) 0.0253(9) Uani 1 1 d . . . N2 N 0.2440(2) -0.0189(5) 0.0883(2) 0.0262(9) Uani 1 1 d . . . N3 N 0.15121(19) 0.2892(5) 0.0696(2) 0.0244(8) Uani 1 1 d . . . C1 C 0.4188(2) 0.2798(6) 0.1116(3) 0.0252(10) Uani 1 1 d . . . C2 C 0.4619(2) 0.2964(6) 0.0420(3) 0.0314(11) Uani 1 1 d . . . H2 H 0.4444 0.3635 -0.0072 0.038 Uiso 1 1 calc R . . C3 C 0.5297(3) 0.2161(7) 0.0440(3) 0.0349(12) Uani 1 1 d . . . H3 H 0.5575 0.2309 -0.0030 0.042 Uiso 1 1 calc R . . C4 C 0.5564(3) 0.1133(7) 0.1164(3) 0.0352(12) Uani 1 1 d . . . H4 H 0.6020 0.0584 0.1183 0.042 Uiso 1 1 calc R . . C5 C 0.5141(2) 0.0936(6) 0.1857(3) 0.0313(11) Uani 1 1 d . . . H5 H 0.5317 0.0235 0.2338 0.038 Uiso 1 1 calc R . . C6 C 0.4456(2) 0.1762(6) 0.1855(3) 0.0259(10) Uani 1 1 d . . . C7 C 0.4047(2) 0.1548(6) 0.2651(3) 0.0296(11) Uani 1 1 d . . . H7A H 0.4362 0.0926 0.3106 0.035 Uiso 1 1 calc R . . H7B H 0.3954 0.2710 0.2880 0.035 Uiso 1 1 calc R . . C8 C 0.3085(3) 0.0233(6) 0.3378(3) 0.0345(12) Uani 1 1 d . . . H8A H 0.2591 -0.0213 0.3298 0.052 Uiso 1 1 calc R . . H8B H 0.3099 0.1305 0.3716 0.052 Uiso 1 1 calc R . . H8C H 0.3403 -0.0624 0.3689 0.052 Uiso 1 1 calc R . . C10 C 0.2673(3) -0.1604(6) 0.1522(3) 0.0343(12) Uani 1 1 d . . . H10A H 0.2720 -0.2705 0.1208 0.041 Uiso 1 1 calc R . . H10B H 0.2306 -0.1762 0.1927 0.041 Uiso 1 1 calc R . . C11 C 0.2882(3) -0.0257(6) 0.0129(3) 0.0340(12) Uani 1 1 d . . . H11A H 0.3389 -0.0052 0.0339 0.051 Uiso 1 1 calc R . . H11B H 0.2713 0.0634 -0.0296 0.051 Uiso 1 1 calc R . . H11C H 0.2830 -0.1397 -0.0146 0.051 Uiso 1 1 calc R . . C9 C 0.3398(2) -0.1129(6) 0.2036(3) 0.0301(11) Uani 1 1 d . . . H9A H 0.3543 -0.2040 0.2470 0.036 Uiso 1 1 calc R . . H9B H 0.3773 -0.1050 0.1635 0.036 Uiso 1 1 calc R . . C12 C 0.1644(2) -0.0344(6) 0.0563(3) 0.0295(11) Uani 1 1 d . . . H12A H 0.1370 -0.0565 0.1061 0.035 Uiso 1 1 calc R . . H12B H 0.1565 -0.1328 0.0156 0.035 Uiso 1 1 calc R . . C13 C 0.1375(3) 0.1342(6) 0.0100(3) 0.0295(11) Uani 1 1 d . . . H13A H 0.1624 0.1510 -0.0423 0.035 Uiso 1 1 calc R . . H13B H 0.0852 0.1245 -0.0090 0.035 Uiso 1 1 calc R . . C14 C 0.1614(2) 0.4465(6) 0.0153(3) 0.0302(11) Uani 1 1 d . . . H14A H 0.1990 0.4238 -0.0223 0.045 Uiso 1 1 calc R . . H14B H 0.1757 0.5447 0.0534 0.045 Uiso 1 1 calc R . . H14C H 0.1161 0.4736 -0.0206 0.045 Uiso 1 1 calc R . . C15 C 0.0860(2) 0.3132(6) 0.1187(3) 0.0291(11) Uani 1 1 d . . . H15A H 0.0822 0.2127 0.1575 0.035 Uiso 1 1 calc R . . H15B H 0.0420 0.3157 0.0765 0.035 Uiso 1 1 calc R . . C16 C 0.0892(2) 0.4807(6) 0.1739(3) 0.0275(11) Uani 1 1 d . . . C17 C 0.1404(3) 0.4992(6) 0.2494(3) 0.0293(11) Uani 1 1 d . . . C18 C 0.1372(3) 0.6538(6) 0.2995(3) 0.0340(12) Uani 1 1 d . . . H18 H 0.1706 0.6686 0.3500 0.041 Uiso 1 1 calc R . . C19 C 0.0866(3) 0.7842(7) 0.2763(3) 0.0365(12) Uani 1 1 d . . . H19 H 0.0864 0.8858 0.3106 0.044 Uiso 1 1 calc R . . C20 C 0.0362(3) 0.7647(7) 0.2026(3) 0.0373(12) Uani 1 1 d . . . H20 H 0.0013 0.8517 0.1870 0.045 Uiso 1 1 calc R . . C21 C 0.0380(3) 0.6142(6) 0.1519(3) 0.0318(11) Uani 1 1 d . . . H21 H 0.0042 0.6015 0.1016 0.038 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 Ni 0.0268(3) 0.0206(3) 0.0241(3) -0.0007(3) 0.0045(2) 0.0014(3) S1 0.0291(7) 0.0220(6) 0.0447(7) 0.0079(6) 0.0066(6) 0.0011(5) S2 0.0458(8) 0.0490(9) 0.0248(7) -0.0034(6) 0.0039(6) 0.0214(6) N1 0.029(2) 0.021(2) 0.027(2) 0.0002(16) 0.0069(17) 0.0000(17) N2 0.029(2) 0.019(2) 0.031(2) -0.0006(16) 0.0066(17) 0.0021(16) N3 0.027(2) 0.0212(19) 0.0252(19) -0.0020(17) 0.0038(16) -0.0024(17) C1 0.030(3) 0.017(2) 0.028(2) -0.002(2) 0.005(2) -0.004(2) C2 0.032(3) 0.031(3) 0.031(3) 0.005(2) 0.000(2) -0.007(2) C3 0.032(3) 0.037(3) 0.037(3) -0.004(2) 0.011(2) -0.004(2) C4 0.029(3) 0.035(3) 0.043(3) -0.006(2) 0.007(2) 0.000(2) C5 0.029(3) 0.026(3) 0.038(3) 0.000(2) -0.002(2) 0.003(2) C6 0.030(3) 0.019(3) 0.028(2) -0.0019(19) 0.002(2) -0.0010(19) C7 0.030(3) 0.030(3) 0.029(3) -0.003(2) 0.001(2) 0.000(2) C8 0.043(3) 0.033(3) 0.028(3) 0.006(2) 0.007(2) 0.007(2) C10 0.040(3) 0.022(3) 0.040(3) 0.002(2) 0.002(2) -0.001(2) C11 0.038(3) 0.034(3) 0.032(3) -0.003(2) 0.012(2) -0.001(2) C9 0.037(3) 0.021(3) 0.032(3) -0.001(2) 0.003(2) 0.002(2) C12 0.028(3) 0.027(3) 0.033(3) -0.005(2) 0.003(2) -0.003(2) C13 0.031(3) 0.033(3) 0.025(2) -0.002(2) 0.002(2) -0.001(2) C14 0.030(3) 0.031(3) 0.030(3) 0.001(2) 0.006(2) -0.001(2) C15 0.021(2) 0.033(3) 0.035(3) 0.001(2) 0.009(2) -0.003(2) C16 0.027(3) 0.025(3) 0.033(3) -0.001(2) 0.010(2) -0.002(2) C17 0.030(3) 0.032(3) 0.029(3) 0.000(2) 0.012(2) -0.001(2) C18 0.039(3) 0.035(3) 0.029(3) -0.003(2) 0.008(2) 0.005(2) C19 0.045(3) 0.030(3) 0.037(3) -0.004(2) 0.013(2) 0.004(3) C20 0.035(3) 0.037(3) 0.042(3) 0.000(2) 0.014(2) 0.011(2) C21 0.030(3) 0.034(3) 0.032(3) 0.003(2) 0.005(2) 0.003(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 Ni N2 2.104(4) . ? Ni N1 2.196(4) . ? Ni N3 2.274(4) . ? Ni S2 2.2916(13) . ? Ni S1 2.3013(14) . ? S1 C1 1.757(5) . ? S2 C17 1.753(5) . ? N1 C7 1.486(5) . ? N1 C9 1.489(5) . ? N1 C8 1.494(5) . ? N2 C10 1.476(5) . ? N2 C11 1.477(5) . ? N2 C12 1.487(6) . ? N3 C14 1.475(5) . ? N3 C13 1.487(5) . ? N3 C15 1.492(5) . ? C1 C2 1.397(6) . ? C1 C6 1.410(6) . ? C2 C3 1.381(6) . ? C3 C4 1.389(6) . ? C4 C5 1.385(6) . ? C5 C6 1.402(6) . ? C6 C7 1.503(6) . ? C10 C9 1.504(6) . ? C12 C13 1.514(6) . ? C15 C16 1.519(6) . ? C16 C21 1.393(6) . ? C16 C17 1.402(6) . ? C17 C18 1.403(6) . ? C18 C19 1.373(6) . ? C19 C20 1.374(7) . ? C20 C21 1.379(6) . ? 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 N2 Ni N1 82.72(14) . . ? N2 Ni N3 82.31(14) . . ? N1 Ni N3 162.33(13) . . ? N2 Ni S2 140.23(11) . . ? N1 Ni S2 92.51(10) . . ? N3 Ni S2 92.99(9) . . ? N2 Ni S1 106.00(11) . . ? N1 Ni S1 96.25(10) . . ? N3 Ni S1 96.86(9) . . ? S2 Ni S1 113.77(6) . . ? C1 S1 Ni 107.89(15) . . ? C17 S2 Ni 110.30(15) . . ? C7 N1 C9 112.8(3) . . ? C7 N1 C8 107.4(3) . . ? C9 N1 C8 108.0(3) . . ? C7 N1 Ni 111.2(3) . . ? C9 N1 Ni 106.2(3) . . ? C8 N1 Ni 111.3(3) . . ? C10 N2 C11 110.0(4) . . ? C10 N2 C12 110.7(3) . . ? C11 N2 C12 110.4(4) . . ? C10 N2 Ni 104.5(3) . . ? C11 N2 Ni 116.7(3) . . ? C12 N2 Ni 104.1(3) . . ? C14 N3 C13 108.8(3) . . ? C14 N3 C15 110.0(3) . . ? C13 N3 C15 108.2(3) . . ? C14 N3 Ni 114.5(3) . . ? C13 N3 Ni 104.6(3) . . ? C15 N3 Ni 110.4(3) . . ? C2 C1 C6 118.5(4) . . ? C2 C1 S1 118.7(3) . . ? C6 C1 S1 122.9(3) . . ? C3 C2 C1 122.1(4) . . ? C2 C3 C4 119.8(4) . . ? C5 C4 C3 119.0(5) . . ? C4 C5 C6 122.0(4) . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C7 118.7(4) . . ? C1 C6 C7 122.6(4) . . ? N1 C7 C6 115.7(4) . . ? N2 C10 C9 109.7(4) . . ? N1 C9 C10 109.9(4) . . ? N2 C12 C13 109.8(4) . . ? N3 C13 C12 111.2(3) . . ? N3 C15 C16 113.3(3) . . ? C21 C16 C17 119.4(4) . . ? C21 C16 C15 119.6(4) . . ? C17 C16 C15 120.9(4) . . ? C16 C17 C18 117.4(4) . . ? C16 C17 S2 122.7(4) . . ? C18 C17 S2 119.8(4) . . ? C19 C18 C17 122.2(5) . . ? C18 C19 C20 120.1(5) . . ? C19 C20 C21 119.1(5) . . ? C20 C21 C16 121.8(5) . . ? #===END # Attachment 'CCDC_601291n.CIF' data_6 _database_code_depnum_ccdc_archive 'CCDC 601291' _chemical_formula_structural ; [Co(L5)] ; _chemical_formula_sum 'C21 H29 Co N3 S2' _chemical_formula_weight 446.52 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown from acetonitrile. ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.334(4) _cell_length_b 7.601(2) _cell_length_c 15.163(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.46(3) _cell_angle_gamma 90.00 _cell_volume 2099.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 155 _cell_measurement_theta_min 8 _cell_measurement_theta_max 22.5 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.413 _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS, Sheldrick, 1996)' _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12807 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 28.35 _reflns_number_total 4993 _reflns_number_gt 3026 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA _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^)+(0.0356P)^2^+1.2593P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4993 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.700 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.094 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.25491(2) 0.22276(6) 0.16542(3) 0.02233(13) Uani 1 1 d . . . S1 S 0.33848(5) 0.40104(12) 0.11102(6) 0.0300(2) Uani 1 1 d . . . S2 S 0.20142(5) 0.32543(13) 0.28540(6) 0.0361(3) Uani 1 1 d . . . N1 N 0.33568(15) 0.0555(3) 0.25152(17) 0.0238(6) Uani 1 1 d . . . N2 N 0.24195(14) -0.0164(3) 0.09208(18) 0.0231(6) Uani 1 1 d . . . N3 N 0.14930(14) 0.2909(4) 0.06801(18) 0.0240(6) Uani 1 1 d . . . C1 C 0.42110(17) 0.2817(4) 0.1148(2) 0.0244(7) Uani 1 1 d . . . C2 C 0.46315(19) 0.3015(5) 0.0446(2) 0.0289(8) Uani 1 1 d . . . H2 H 0.4460 0.3741 -0.0026 0.035 Uiso 1 1 calc R . . C3 C 0.52991(19) 0.2162(5) 0.0429(2) 0.0331(8) Uani 1 1 d . . . H3 H 0.5569 0.2318 -0.0049 0.040 Uiso 1 1 calc R . . C4 C 0.5560(2) 0.1078(5) 0.1127(2) 0.0342(9) Uani 1 1 d . . . H4 H 0.6006 0.0498 0.1124 0.041 Uiso 1 1 calc R . . C5 C 0.51481(19) 0.0871(5) 0.1828(2) 0.0300(8) Uani 1 1 d . . . H5 H 0.5326 0.0141 0.2295 0.036 Uiso 1 1 calc R . . C6 C 0.44742(18) 0.1711(4) 0.1864(2) 0.0250(8) Uani 1 1 d . . . C7 C 0.40798(18) 0.1453(5) 0.2673(2) 0.0274(8) Uani 1 1 d . . . H7A H 0.4394 0.0774 0.3105 0.033 Uiso 1 1 calc R . . H7B H 0.4007 0.2596 0.2934 0.033 Uiso 1 1 calc R . . C8 C 0.3108(2) 0.0218(5) 0.3401(2) 0.0328(9) Uani 1 1 d . . . H8A H 0.2615 -0.0228 0.3326 0.049 Uiso 1 1 calc R . . H8B H 0.3123 0.1295 0.3733 0.049 Uiso 1 1 calc R . . H8C H 0.3427 -0.0630 0.3716 0.049 Uiso 1 1 calc R . . C10 C 0.26545(19) -0.1585(5) 0.1558(2) 0.0314(8) Uani 1 1 d . . . H10A H 0.2684 -0.2688 0.1242 0.038 Uiso 1 1 calc R . . H10B H 0.2297 -0.1718 0.1979 0.038 Uiso 1 1 calc R . . C11 C 0.28634(19) -0.0225(5) 0.0162(2) 0.0334(9) Uani 1 1 d . . . H11A H 0.3370 -0.0021 0.0371 0.050 Uiso 1 1 calc R . . H11B H 0.2695 0.0667 -0.0261 0.050 Uiso 1 1 calc R . . H11C H 0.2812 -0.1360 -0.0116 0.050 Uiso 1 1 calc R . . C9 C 0.33985(19) -0.1144(4) 0.2049(2) 0.0298(8) Uani 1 1 d . . . H9A H 0.3548 -0.2064 0.2474 0.036 Uiso 1 1 calc R . . H9B H 0.3762 -0.1070 0.1632 0.036 Uiso 1 1 calc R . . C12 C 0.16269(18) -0.0321(4) 0.0602(2) 0.0284(8) Uani 1 1 d . . . H12A H 0.1350 -0.0503 0.1103 0.034 Uiso 1 1 calc R . . H12B H 0.1548 -0.1329 0.0210 0.034 Uiso 1 1 calc R . . C13 C 0.13599(19) 0.1324(4) 0.0111(2) 0.0268(8) Uani 1 1 d . . . H13A H 0.1612 0.1454 -0.0414 0.032 Uiso 1 1 calc R . . H13B H 0.0839 0.1218 -0.0079 0.032 Uiso 1 1 calc R . . C14 C 0.15933(19) 0.4461(5) 0.0125(2) 0.0297(8) Uani 1 1 d . . . H14A H 0.1970 0.4225 -0.0250 0.045 Uiso 1 1 calc R . . H14B H 0.1733 0.5452 0.0499 0.045 Uiso 1 1 calc R . . H14C H 0.1141 0.4717 -0.0236 0.045 Uiso 1 1 calc R . . C15 C 0.08515(18) 0.3177(5) 0.1180(2) 0.0288(8) Uani 1 1 d . . . H15A H 0.0807 0.2164 0.1560 0.035 Uiso 1 1 calc R . . H15B H 0.0412 0.3227 0.0761 0.035 Uiso 1 1 calc R . . C16 C 0.08868(18) 0.4805(4) 0.1741(2) 0.0245(7) Uani 1 1 d . . . C17 C 0.13916(18) 0.4941(4) 0.2506(2) 0.0253(8) Uani 1 1 d . . . C18 C 0.13733(19) 0.6457(5) 0.3020(2) 0.0309(8) Uani 1 1 d . . . H18 H 0.1707 0.6569 0.3526 0.037 Uiso 1 1 calc R . . C19 C 0.0878(2) 0.7798(5) 0.2805(2) 0.0362(9) Uani 1 1 d . . . H19 H 0.0880 0.8791 0.3163 0.043 Uiso 1 1 calc R . . C20 C 0.03786(19) 0.7660(5) 0.2052(2) 0.0329(9) Uani 1 1 d . . . H20 H 0.0039 0.8551 0.1902 0.039 Uiso 1 1 calc R . . C21 C 0.03927(19) 0.6179(5) 0.1529(2) 0.0311(8) Uani 1 1 d . . . H21 H 0.0062 0.6092 0.1019 0.037 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 Co 0.0251(2) 0.0230(2) 0.0192(2) -0.0010(2) 0.00405(17) 0.0005(2) S1 0.0263(5) 0.0261(5) 0.0379(5) 0.0080(4) 0.0046(4) 0.0021(4) S2 0.0429(6) 0.0477(6) 0.0177(4) -0.0007(4) 0.0036(4) 0.0191(5) N1 0.0287(16) 0.0245(15) 0.0183(14) 0.0019(12) 0.0030(12) 0.0018(12) N2 0.0249(15) 0.0222(15) 0.0229(15) -0.0018(12) 0.0052(12) -0.0003(12) N3 0.0238(14) 0.0262(15) 0.0224(14) 0.0016(13) 0.0040(11) -0.0013(12) C1 0.0250(17) 0.0198(17) 0.0280(18) -0.0027(15) 0.0009(14) -0.0043(14) C2 0.031(2) 0.029(2) 0.0263(19) 0.0013(15) 0.0018(15) -0.0067(16) C3 0.031(2) 0.039(2) 0.031(2) -0.0034(18) 0.0114(16) -0.0039(17) C4 0.028(2) 0.036(2) 0.039(2) -0.0026(18) 0.0058(17) 0.0008(17) C5 0.030(2) 0.0284(19) 0.031(2) 0.0013(16) 0.0023(16) 0.0007(15) C6 0.0254(18) 0.0272(19) 0.0219(18) -0.0019(15) 0.0005(14) -0.0024(14) C7 0.030(2) 0.0303(19) 0.0208(18) 0.0007(15) -0.0021(15) 0.0036(15) C8 0.041(2) 0.037(2) 0.0208(18) 0.0081(16) 0.0067(16) 0.0064(17) C10 0.039(2) 0.0209(17) 0.033(2) 0.0024(16) 0.0010(17) 0.0011(16) C11 0.039(2) 0.037(2) 0.026(2) -0.0061(17) 0.0093(16) -0.0003(17) C9 0.036(2) 0.0246(19) 0.0283(19) 0.0013(16) 0.0022(16) 0.0055(16) C12 0.0282(19) 0.0280(19) 0.029(2) -0.0058(16) 0.0036(15) -0.0037(15) C13 0.0290(19) 0.032(2) 0.0193(17) -0.0057(15) 0.0009(14) -0.0028(15) C14 0.0287(19) 0.034(2) 0.0257(19) 0.0044(16) 0.0015(15) -0.0007(16) C15 0.0245(18) 0.036(2) 0.0263(19) 0.0025(16) 0.0055(15) -0.0015(15) C16 0.0226(17) 0.0271(19) 0.0250(18) -0.0019(15) 0.0076(14) -0.0030(14) C17 0.0244(18) 0.030(2) 0.0225(18) 0.0007(15) 0.0090(14) 0.0042(15) C18 0.033(2) 0.037(2) 0.0223(19) -0.0049(16) 0.0037(15) 0.0040(17) C19 0.046(2) 0.033(2) 0.032(2) -0.0047(17) 0.0144(18) 0.0053(18) C20 0.033(2) 0.034(2) 0.033(2) 0.0022(17) 0.0132(16) 0.0103(17) C21 0.0271(19) 0.038(2) 0.028(2) 0.0029(17) 0.0055(15) 0.0034(16) _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 Co N2 2.130(3) . ? Co N1 2.253(3) . ? Co S1 2.2692(11) . ? Co S2 2.2982(11) . ? Co N3 2.357(3) . ? S1 C1 1.761(3) . ? S2 C17 1.758(3) . ? N1 C9 1.478(4) . ? N1 C7 1.486(4) . ? N1 C8 1.489(4) . ? N2 C10 1.480(4) . ? N2 C11 1.483(4) . ? N2 C12 1.484(4) . ? N3 C14 1.472(4) . ? N3 C15 1.483(4) . ? N3 C13 1.486(4) . ? C1 C2 1.392(5) . ? C1 C6 1.414(5) . ? C2 C3 1.388(5) . ? C3 C4 1.384(5) . ? C4 C5 1.380(5) . ? C5 C6 1.398(5) . ? C6 C7 1.506(5) . ? C10 C9 1.516(5) . ? C12 C13 1.508(5) . ? C15 C16 1.500(5) . ? C16 C21 1.396(5) . ? C16 C17 1.403(5) . ? C17 C18 1.394(5) . ? C18 C19 1.380(5) . ? C19 C20 1.384(5) . ? C20 C21 1.379(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co N1 81.28(10) . . ? N2 Co S1 111.10(8) . . ? N1 Co S1 96.94(8) . . ? N2 Co S2 132.11(8) . . ? N1 Co S2 92.52(8) . . ? S1 Co S2 116.79(5) . . ? N2 Co N3 79.92(10) . . ? N1 Co N3 157.97(10) . . ? S1 Co N3 100.46(7) . . ? S2 Co N3 91.59(7) . . ? C1 S1 Co 107.10(12) . . ? C17 S2 Co 109.29(12) . . ? C9 N1 C7 112.6(3) . . ? C9 N1 C8 108.6(3) . . ? C7 N1 C8 106.9(3) . . ? C9 N1 Co 106.36(19) . . ? C7 N1 Co 110.5(2) . . ? C8 N1 Co 111.8(2) . . ? C10 N2 C11 109.8(3) . . ? C10 N2 C12 110.9(3) . . ? C11 N2 C12 110.3(3) . . ? C10 N2 Co 105.9(2) . . ? C11 N2 Co 113.1(2) . . ? C12 N2 Co 106.64(19) . . ? C14 N3 C15 109.9(3) . . ? C14 N3 C13 109.9(3) . . ? C15 N3 C13 108.7(3) . . ? C14 N3 Co 112.82(19) . . ? C15 N3 Co 110.6(2) . . ? C13 N3 Co 104.78(19) . . ? C2 C1 C6 118.8(3) . . ? C2 C1 S1 117.9(3) . . ? C6 C1 S1 123.3(3) . . ? C3 C2 C1 122.0(3) . . ? C4 C3 C2 119.6(3) . . ? C5 C4 C3 119.0(3) . . ? C4 C5 C6 122.8(3) . . ? C5 C6 C1 117.9(3) . . ? C5 C6 C7 118.7(3) . . ? C1 C6 C7 123.3(3) . . ? N1 C7 C6 115.5(3) . . ? N2 C10 C9 109.8(3) . . ? N1 C9 C10 109.6(3) . . ? N2 C12 C13 110.2(3) . . ? N3 C13 C12 111.3(3) . . ? N3 C15 C16 114.7(3) . . ? C21 C16 C17 119.1(3) . . ? C21 C16 C15 120.1(3) . . ? C17 C16 C15 120.8(3) . . ? C18 C17 C16 117.9(3) . . ? C18 C17 S2 119.4(3) . . ? C16 C17 S2 122.7(3) . . ? C19 C18 C17 122.4(3) . . ? C18 C19 C20 119.7(4) . . ? C21 C20 C19 118.8(3) . . ? C20 C21 C16 122.1(3) . . ? #===END # Attachment 'CCDC_601292n.CIF' data_7_ClO4 _database_code_depnum_ccdc_archive 'CCDC 601292' _chemical_formula_structural ; [NiH2(L2)](ClO4)2MeOH ; _chemical_formula_sum 'C39 H70 Cl2 N6 Ni O9 S2' _chemical_formula_weight 960.74 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown from methanol. ; #CRYSTAL DATA _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 14.073(3) _cell_length_b 17.070(3) _cell_length_c 19.323(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.04(3) _cell_angle_gamma 90.00 _cell_volume 4635.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 8 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.377 _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS, Sheldrick, 1996)' _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28635 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10921 _reflns_number_gt 6237 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA _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^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10921 _refine_ls_number_parameters 560 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.922 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.082 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.36937(3) 0.12139(2) 0.15326(2) 0.02750(11) Uani 1 1 d . . . S1 S 0.40849(5) 0.19088(5) 0.25330(4) 0.03242(19) Uani 1 1 d . . . S2 S 0.33411(6) -0.00257(4) 0.19151(4) 0.03162(19) Uani 1 1 d . . . N1 N 0.51369(18) 0.08956(14) 0.13280(14) 0.0316(6) Uani 1 1 d . . . N2 N 0.3812(2) 0.19299(16) 0.06712(14) 0.0389(7) Uani 1 1 d . . . N3 N 0.21634(19) 0.15571(16) 0.14006(15) 0.0368(7) Uani 1 1 d . . . N4 N 0.38000(17) 0.00366(14) 0.35398(14) 0.0311(6) Uani 1 1 d . . . H4 H 0.3917 0.0279 0.3134 0.037 Uiso 1 1 calc R . . N5 N 0.37259(19) 0.19073(15) 0.45758(14) 0.0349(6) Uani 1 1 d . . . N6 N 0.43415(17) 0.31563(14) 0.37323(13) 0.0271(6) Uani 1 1 d . . . H6 H 0.3960 0.2758 0.3571 0.033 Uiso 1 1 calc R . . C1 C 0.5284(2) 0.22213(17) 0.25184(15) 0.0272(7) Uani 1 1 d . . . C2 C 0.5547(2) 0.29422(17) 0.28235(15) 0.0270(7) Uani 1 1 d . . . C3 C 0.6482(2) 0.31919(18) 0.28274(16) 0.0310(7) Uani 1 1 d . . . H3 H 0.6644 0.3663 0.3045 0.037 Uiso 1 1 calc R . . C4 C 0.7190(2) 0.27686(18) 0.25195(16) 0.0298(7) Uani 1 1 d . . . C5 C 0.6924(2) 0.20535(18) 0.22271(16) 0.0309(7) Uani 1 1 d . . . H5 H 0.7383 0.1753 0.2022 0.037 Uiso 1 1 calc R . . C6 C 0.5993(2) 0.17673(17) 0.22295(16) 0.0288(7) Uani 1 1 d . . . C7 C 0.5802(2) 0.09540(17) 0.19570(17) 0.0317(7) Uani 1 1 d . . . H7A H 0.6405 0.0720 0.1849 0.038 Uiso 1 1 calc R . . H7B H 0.5544 0.0645 0.2324 0.038 Uiso 1 1 calc R . . C8 C 0.5187(2) 0.00764(19) 0.1073(2) 0.0423(9) Uani 1 1 d . . . H8A H 0.4724 0.0002 0.0696 0.064 Uiso 1 1 calc R . . H8B H 0.5060 -0.0278 0.1442 0.064 Uiso 1 1 calc R . . H8C H 0.5812 -0.0024 0.0916 0.064 Uiso 1 1 calc R . . C9 C 0.5437(3) 0.1429(2) 0.07700(18) 0.0416(8) Uani 1 1 d . . . H9A H 0.5938 0.1185 0.0520 0.050 Uiso 1 1 calc R . . H9B H 0.5683 0.1913 0.0972 0.050 Uiso 1 1 calc R . . C10 C 0.4590(3) 0.1601(2) 0.02781(18) 0.0449(9) Uani 1 1 d . . . H10A H 0.4770 0.1973 -0.0072 0.054 Uiso 1 1 calc R . . H10B H 0.4378 0.1123 0.0046 0.054 Uiso 1 1 calc R . . C11 C 0.3996(3) 0.2762(2) 0.0821(2) 0.0575(11) Uani 1 1 d . . . H11A H 0.4626 0.2821 0.1031 0.086 Uiso 1 1 calc R . . H11B H 0.3540 0.2952 0.1133 0.086 Uiso 1 1 calc R . . H11C H 0.3943 0.3057 0.0398 0.086 Uiso 1 1 calc R . . C12 C 0.2866(3) 0.1802(2) 0.0287(2) 0.0545(10) Uani 1 1 d . . . H12A H 0.2822 0.2133 -0.0122 0.065 Uiso 1 1 calc R . . H12B H 0.2816 0.1261 0.0136 0.065 Uiso 1 1 calc R . . C13 C 0.2078(3) 0.1987(2) 0.0734(2) 0.0544(11) Uani 1 1 d . . . H13A H 0.1478 0.1852 0.0493 0.065 Uiso 1 1 calc R . . H13B H 0.2074 0.2545 0.0826 0.065 Uiso 1 1 calc R . . C14 C 0.1843(2) 0.2089(2) 0.1955(2) 0.0490(10) Uani 1 1 d . . . H14A H 0.2238 0.2548 0.1978 0.074 Uiso 1 1 calc R . . H14B H 0.1890 0.1822 0.2393 0.074 Uiso 1 1 calc R . . H14C H 0.1194 0.2241 0.1851 0.074 Uiso 1 1 calc R . . C15 C 0.1526(2) 0.08554(19) 0.13536(18) 0.0365(8) Uani 1 1 d . . . H15A H 0.1763 0.0489 0.1019 0.044 Uiso 1 1 calc R . . H15B H 0.0892 0.1017 0.1190 0.044 Uiso 1 1 calc R . . C16 C 0.1472(2) 0.04521(17) 0.20430(16) 0.0298(7) Uani 1 1 d . . . C17 C 0.2268(2) 0.00700(17) 0.23443(17) 0.0298(7) Uani 1 1 d . . . C18 C 0.2201(2) -0.02510(17) 0.30082(16) 0.0291(7) Uani 1 1 d . . . C19 C 0.1361(2) -0.02049(18) 0.33467(17) 0.0338(7) Uani 1 1 d . . . H19 H 0.1337 -0.0423 0.3786 0.041 Uiso 1 1 calc R . . C20 C 0.0549(2) 0.01585(17) 0.30506(17) 0.0321(7) Uani 1 1 d . . . C21 C 0.0634(2) 0.04820(18) 0.23955(18) 0.0346(7) Uani 1 1 d . . . H21 H 0.0107 0.0730 0.2183 0.042 Uiso 1 1 calc R . . C22 C 0.3070(2) -0.05948(18) 0.33702(17) 0.0326(7) Uani 1 1 d . . . H22A H 0.3341 -0.0987 0.3076 0.039 Uiso 1 1 calc R . . H22B H 0.2896 -0.0849 0.3794 0.039 Uiso 1 1 calc R . . C23 C 0.4708(2) -0.0328(2) 0.3797(2) 0.0462(9) Uani 1 1 d . . . H23A H 0.5176 0.0073 0.3889 0.069 Uiso 1 1 calc R . . H23B H 0.4927 -0.0681 0.3453 0.069 Uiso 1 1 calc R . . H23C H 0.4609 -0.0612 0.4216 0.069 Uiso 1 1 calc R . . C24 C 0.3406(2) 0.06449(18) 0.40018(18) 0.0347(7) Uani 1 1 d . . . H24A H 0.3082 0.0386 0.4369 0.042 Uiso 1 1 calc R . . H24B H 0.2940 0.0955 0.3736 0.042 Uiso 1 1 calc R . . C25 C 0.4158(2) 0.11836(17) 0.43212(17) 0.0328(7) Uani 1 1 d . . . H25A H 0.4499 0.0918 0.4703 0.039 Uiso 1 1 calc R . . H25B H 0.4612 0.1314 0.3979 0.039 Uiso 1 1 calc R . . C26 C 0.3055(3) 0.1743(2) 0.5110(2) 0.0589(11) Uani 1 1 d . . . H26A H 0.3370 0.1450 0.5479 0.088 Uiso 1 1 calc R . . H26B H 0.2530 0.1444 0.4913 0.088 Uiso 1 1 calc R . . H26C H 0.2824 0.2228 0.5290 0.088 Uiso 1 1 calc R . . C27 C 0.4468(2) 0.24463(19) 0.48520(17) 0.0353(8) Uani 1 1 d . . . H27A H 0.4910 0.2160 0.5160 0.042 Uiso 1 1 calc R . . H27B H 0.4176 0.2852 0.5121 0.042 Uiso 1 1 calc R . . C28 C 0.5010(2) 0.28255(18) 0.42813(16) 0.0333(7) Uani 1 1 d . . . H28A H 0.5411 0.3240 0.4477 0.040 Uiso 1 1 calc R . . H28B H 0.5416 0.2439 0.4078 0.040 Uiso 1 1 calc R . . C29 C 0.3712(3) 0.3770(2) 0.40164(19) 0.0429(9) Uani 1 1 d . . . H29A H 0.3332 0.3542 0.4362 0.064 Uiso 1 1 calc R . . H29B H 0.3304 0.3981 0.3648 0.064 Uiso 1 1 calc R . . H29C H 0.4097 0.4182 0.4221 0.064 Uiso 1 1 calc R . . C30 C 0.4837(2) 0.34823(17) 0.31247(16) 0.0299(7) Uani 1 1 d . . . H30A H 0.4360 0.3618 0.2764 0.036 Uiso 1 1 calc R . . H30B H 0.5160 0.3962 0.3269 0.036 Uiso 1 1 calc R . . C31 C 0.8211(2) 0.30829(19) 0.25432(18) 0.0348(7) Uani 1 1 d . . . C32 C 0.8856(2) 0.2608(2) 0.2090(2) 0.0495(10) Uani 1 1 d . . . H32A H 0.8894 0.2078 0.2256 0.074 Uiso 1 1 calc R . . H32B H 0.9480 0.2836 0.2110 0.074 Uiso 1 1 calc R . . H32C H 0.8599 0.2612 0.1620 0.074 Uiso 1 1 calc R . . C33 C 0.8217(3) 0.3932(2) 0.2294(2) 0.0476(9) Uani 1 1 d . . . H33A H 0.7967 0.3957 0.1822 0.071 Uiso 1 1 calc R . . H33B H 0.8858 0.4128 0.2321 0.071 Uiso 1 1 calc R . . H33C H 0.7831 0.4246 0.2581 0.071 Uiso 1 1 calc R . . C34 C 0.8610(3) 0.3059(2) 0.3298(2) 0.0510(10) Uani 1 1 d . . . H34A H 0.8279 0.3433 0.3567 0.077 Uiso 1 1 calc R . . H34B H 0.9275 0.3184 0.3315 0.077 Uiso 1 1 calc R . . H34C H 0.8524 0.2543 0.3484 0.077 Uiso 1 1 calc R . . C35 C -0.0336(2) 0.0241(2) 0.34651(19) 0.0390(8) Uani 1 1 d . . . C36 C -0.1217(3) 0.0455(2) 0.3003(2) 0.0568(11) Uani 1 1 d . . . H36A H -0.1775 0.0417 0.3267 0.085 Uiso 1 1 calc R . . H36B H -0.1274 0.0101 0.2618 0.085 Uiso 1 1 calc R . . H36C H -0.1155 0.0981 0.2836 0.085 Uiso 1 1 calc R . . C37 C -0.0571(3) -0.0524(2) 0.3831(2) 0.0627(12) Uani 1 1 d . . . H37A H -0.0053 -0.0663 0.4151 0.094 Uiso 1 1 calc R . . H37B H -0.0669 -0.0933 0.3494 0.094 Uiso 1 1 calc R . . H37C H -0.1139 -0.0456 0.4079 0.094 Uiso 1 1 calc R . . C38 C -0.0144(3) 0.0888(3) 0.4000(3) 0.0792(16) Uani 1 1 d . . . H38A H 0.0406 0.0754 0.4292 0.119 Uiso 1 1 calc R . . H38B H -0.0685 0.0944 0.4279 0.119 Uiso 1 1 calc R . . H38C H -0.0031 0.1373 0.3767 0.119 Uiso 1 1 calc R . . Cl1 Cl 0.82480(7) 0.02238(5) 0.07054(5) 0.0475(2) Uani 1 1 d . . . O1 O 0.7550(2) 0.0273(2) 0.01429(18) 0.0817(10) Uani 1 1 d . . . O2 O 0.7818(3) -0.0050(2) 0.13003(19) 0.1028(13) Uani 1 1 d . . . O3 O 0.8640(4) 0.0950(2) 0.0819(2) 0.156(2) Uani 1 1 d . . . O4 O 0.8928(3) -0.0314(3) 0.0514(3) 0.1380(18) Uani 1 1 d . . . Cl2 Cl 0.79780(6) 0.60046(5) 0.04638(5) 0.0473(2) Uani 1 1 d D . . O5 O 0.8623(2) 0.6303(2) -0.00025(16) 0.0783(10) Uani 1 1 d D A 1 O6A O 0.7145(4) 0.5807(5) 0.0037(4) 0.076(3) Uani 0.568(12) 1 d PD A 1 O7A O 0.7769(11) 0.6528(6) 0.0935(6) 0.173(8) Uani 0.568(12) 1 d PD A 1 O8A O 0.8293(6) 0.5307(4) 0.0709(7) 0.129(5) Uani 0.568(12) 1 d PD A 1 O6B O 0.7428(15) 0.5424(11) 0.0226(11) 0.274(16) Uani 0.432(12) 1 d PD A 2 O7B O 0.7446(9) 0.6616(6) 0.0709(7) 0.108(6) Uani 0.432(12) 1 d PD A 2 O8B O 0.8488(8) 0.5782(15) 0.1088(6) 0.182(11) Uani 0.432(12) 1 d PD A 2 C39 C 0.1708(12) 0.2856(9) 0.3461(8) 0.360(13) Uani 1 1 d . B 2 O9 O 0.1368(4) 0.3124(6) 0.3998(5) 0.297(6) Uani 1 1 d . B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0336(2) 0.0253(2) 0.0234(2) -0.00197(16) -0.00059(16) -0.00098(17) S1 0.0294(4) 0.0412(5) 0.0268(4) -0.0100(3) 0.0025(3) -0.0032(3) S2 0.0333(4) 0.0270(4) 0.0346(5) 0.0000(3) 0.0026(3) 0.0004(3) N1 0.0377(15) 0.0275(14) 0.0302(15) -0.0070(11) 0.0072(12) -0.0014(11) N2 0.0495(17) 0.0406(17) 0.0270(15) 0.0038(12) 0.0058(13) 0.0024(13) N3 0.0386(15) 0.0329(15) 0.0380(17) 0.0077(12) -0.0077(13) -0.0012(12) N4 0.0286(13) 0.0332(14) 0.0314(15) 0.0006(11) -0.0002(11) -0.0010(11) N5 0.0394(15) 0.0363(16) 0.0291(15) -0.0032(12) 0.0015(12) 0.0014(12) N6 0.0311(13) 0.0257(13) 0.0244(14) -0.0028(10) 0.0008(11) 0.0029(11) C1 0.0271(15) 0.0315(16) 0.0228(16) -0.0029(12) -0.0002(12) 0.0003(13) C2 0.0290(16) 0.0283(16) 0.0237(16) -0.0004(12) 0.0023(13) 0.0022(13) C3 0.0352(17) 0.0285(17) 0.0291(17) -0.0008(13) 0.0016(14) -0.0016(13) C4 0.0301(16) 0.0315(17) 0.0279(17) 0.0006(13) 0.0010(13) -0.0019(13) C5 0.0312(16) 0.0315(17) 0.0303(18) 0.0001(13) 0.0037(13) 0.0056(13) C6 0.0314(16) 0.0286(16) 0.0263(17) -0.0034(12) 0.0000(13) 0.0043(13) C7 0.0319(16) 0.0276(16) 0.0359(19) -0.0012(13) 0.0029(14) 0.0035(13) C8 0.042(2) 0.0354(19) 0.050(2) -0.0178(16) 0.0083(17) -0.0006(15) C9 0.046(2) 0.048(2) 0.0312(19) -0.0021(15) 0.0094(16) -0.0030(16) C10 0.055(2) 0.052(2) 0.0278(19) 0.0004(16) 0.0115(17) -0.0032(18) C11 0.088(3) 0.033(2) 0.051(3) 0.0089(17) 0.006(2) -0.004(2) C12 0.065(3) 0.065(3) 0.032(2) 0.0063(18) -0.0121(19) 0.010(2) C13 0.051(2) 0.059(3) 0.052(3) 0.023(2) -0.010(2) -0.0008(19) C14 0.040(2) 0.035(2) 0.072(3) -0.0100(18) -0.0044(19) 0.0077(16) C15 0.0338(17) 0.0410(19) 0.0340(19) 0.0011(15) -0.0061(15) -0.0026(15) C16 0.0309(16) 0.0288(16) 0.0290(17) -0.0016(13) -0.0045(13) -0.0046(13) C17 0.0307(16) 0.0241(16) 0.0341(18) -0.0035(13) -0.0021(14) -0.0035(13) C18 0.0317(16) 0.0251(15) 0.0301(17) -0.0025(13) -0.0031(14) -0.0031(13) C19 0.0372(18) 0.0321(17) 0.0320(19) 0.0000(13) 0.0024(15) -0.0039(14) C20 0.0312(17) 0.0280(17) 0.0369(19) -0.0041(14) -0.0013(14) -0.0031(13) C21 0.0323(17) 0.0334(18) 0.038(2) -0.0027(14) -0.0041(15) 0.0022(14) C22 0.0354(17) 0.0290(17) 0.0330(18) 0.0014(13) -0.0023(14) -0.0015(14) C23 0.0299(18) 0.049(2) 0.059(3) -0.0018(18) -0.0063(17) 0.0076(16) C24 0.0329(17) 0.0352(18) 0.0359(19) -0.0029(14) 0.0005(14) 0.0017(14) C25 0.0356(17) 0.0312(17) 0.0309(18) 0.0009(14) -0.0057(14) 0.0026(14) C26 0.062(3) 0.065(3) 0.051(3) -0.014(2) 0.024(2) -0.013(2) C27 0.046(2) 0.0325(18) 0.0270(18) 0.0007(13) -0.0053(15) 0.0002(15) C28 0.0361(18) 0.0343(18) 0.0285(18) 0.0000(14) -0.0067(14) 0.0021(14) C29 0.051(2) 0.041(2) 0.038(2) -0.0004(16) 0.0132(17) 0.0176(17) C30 0.0358(17) 0.0266(16) 0.0275(17) 0.0001(13) 0.0033(14) 0.0018(13) C31 0.0312(17) 0.0348(18) 0.039(2) 0.0001(14) 0.0067(15) -0.0027(14) C32 0.0340(19) 0.050(2) 0.065(3) 0.0023(19) 0.0121(18) -0.0010(17) C33 0.044(2) 0.039(2) 0.061(3) 0.0023(17) 0.0152(18) -0.0036(16) C34 0.040(2) 0.066(3) 0.046(2) 0.0059(19) -0.0064(18) -0.0085(18) C35 0.0347(18) 0.040(2) 0.043(2) -0.0048(16) 0.0035(16) 0.0001(15) C36 0.035(2) 0.069(3) 0.067(3) 0.010(2) 0.0085(19) 0.0058(19) C37 0.053(2) 0.067(3) 0.070(3) 0.020(2) 0.023(2) 0.005(2) C38 0.054(3) 0.098(4) 0.088(4) -0.053(3) 0.020(3) -0.007(2) Cl1 0.0577(6) 0.0459(5) 0.0400(5) 0.0073(4) 0.0129(4) 0.0021(4) O1 0.081(2) 0.096(3) 0.067(2) 0.0189(18) -0.0017(18) 0.0034(18) O2 0.105(3) 0.139(3) 0.067(2) 0.050(2) 0.036(2) 0.013(2) O3 0.267(6) 0.087(3) 0.109(4) 0.007(3) -0.025(4) -0.090(4) O4 0.108(3) 0.178(4) 0.130(4) -0.019(3) 0.023(3) 0.081(3) Cl2 0.0429(5) 0.0478(5) 0.0518(6) 0.0060(4) 0.0077(4) 0.0054(4) O5 0.0594(18) 0.117(3) 0.060(2) 0.0049(18) 0.0160(16) -0.0264(18) O6A 0.025(3) 0.124(7) 0.077(5) 0.002(5) -0.017(3) -0.004(3) O7A 0.321(19) 0.113(9) 0.097(8) -0.085(7) 0.106(10) -0.110(10) O8A 0.097(6) 0.049(4) 0.233(13) 0.061(6) -0.064(7) 0.000(4) O6B 0.36(3) 0.179(16) 0.31(3) -0.201(17) 0.29(2) -0.216(18) O7B 0.133(9) 0.086(8) 0.114(10) 0.046(7) 0.072(7) 0.087(8) O8B 0.083(8) 0.38(3) 0.086(9) 0.131(13) 0.044(7) 0.123(13) C39 0.44(2) 0.356(18) 0.299(17) -0.280(16) 0.208(16) -0.257(17) O9 0.094(4) 0.464(14) 0.333(12) 0.261(11) 0.006(6) -0.047(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N2 2.079(3) . ? Ni N1 2.159(3) . ? Ni N3 2.233(3) . ? Ni S2 2.3041(9) . ? Ni S1 2.3096(10) . ? S1 C1 1.772(3) . ? S2 C17 1.768(3) . ? N1 C8 1.486(4) . ? N1 C9 1.489(4) . ? N1 C7 1.498(4) . ? N2 C11 1.470(4) . ? N2 C10 1.476(4) . ? N2 C12 1.506(5) . ? N3 C13 1.481(4) . ? N3 C14 1.493(4) . ? N3 C15 1.496(4) . ? N4 C23 1.484(4) . ? N4 C24 1.495(4) . ? N4 C22 1.513(4) . ? N5 C26 1.463(4) . ? N5 C27 1.470(4) . ? N5 C25 1.473(4) . ? N6 C28 1.491(4) . ? N6 C29 1.495(4) . ? N6 C30 1.504(4) . ? C1 C6 1.402(4) . ? C1 C2 1.406(4) . ? C2 C3 1.383(4) . ? C2 C30 1.500(4) . ? C3 C4 1.390(4) . ? C4 C5 1.388(4) . ? C4 C31 1.531(4) . ? C5 C6 1.399(4) . ? C6 C7 1.504(4) . ? C9 C10 1.513(5) . ? C12 C13 1.476(5) . ? C15 C16 1.505(4) . ? C16 C21 1.394(4) . ? C16 C17 1.397(4) . ? C17 C18 1.403(4) . ? C18 C19 1.383(4) . ? C18 C22 1.496(4) . ? C19 C20 1.396(4) . ? C20 C21 1.392(5) . ? C20 C35 1.523(5) . ? C24 C25 1.509(4) . ? C27 C28 1.519(4) . ? C31 C32 1.527(5) . ? C31 C33 1.528(5) . ? C31 C34 1.535(5) . ? C35 C38 1.528(5) . ? C35 C37 1.529(5) . ? C35 C36 1.533(5) . ? Cl1 O3 1.369(4) . ? Cl1 O4 1.390(4) . ? Cl1 O2 1.407(3) . ? Cl1 O1 1.429(3) . ? Cl2 O7A 1.319(7) . ? Cl2 O6B 1.324(10) . ? Cl2 O8A 1.348(6) . ? Cl2 O7B 1.383(7) . ? Cl2 O5 1.408(3) . ? Cl2 O8B 1.422(9) . ? Cl2 O6A 1.438(5) . ? C39 O9 1.252(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 N2 Ni N1 83.41(11) . . ? N2 Ni N3 82.65(11) . . ? N1 Ni N3 162.91(10) . . ? N2 Ni S2 145.54(8) . . ? N1 Ni S2 92.77(7) . . ? N3 Ni S2 93.14(7) . . ? N2 Ni S1 110.03(8) . . ? N1 Ni S1 95.61(8) . . ? N3 Ni S1 98.42(8) . . ? S2 Ni S1 104.42(4) . . ? C1 S1 Ni 109.04(10) . . ? C17 S2 Ni 105.62(10) . . ? C8 N1 C9 108.4(3) . . ? C8 N1 C7 107.0(2) . . ? C9 N1 C7 111.0(2) . . ? C8 N1 Ni 111.08(19) . . ? C9 N1 Ni 106.5(2) . . ? C7 N1 Ni 112.85(19) . . ? C11 N2 C10 109.9(3) . . ? C11 N2 C12 112.3(3) . . ? C10 N2 C12 110.6(3) . . ? C11 N2 Ni 115.5(2) . . ? C10 N2 Ni 106.4(2) . . ? C12 N2 Ni 101.8(2) . . ? C13 N3 C14 108.0(3) . . ? C13 N3 C15 108.8(3) . . ? C14 N3 C15 109.1(3) . . ? C13 N3 Ni 105.2(2) . . ? C14 N3 Ni 113.8(2) . . ? C15 N3 Ni 111.61(19) . . ? C23 N4 C24 115.5(3) . . ? C23 N4 C22 109.7(2) . . ? C24 N4 C22 110.8(2) . . ? C26 N5 C27 109.6(3) . . ? C26 N5 C25 111.6(3) . . ? C27 N5 C25 110.4(2) . . ? C28 N6 C29 111.6(2) . . ? C28 N6 C30 113.3(2) . . ? C29 N6 C30 109.6(2) . . ? C6 C1 C2 118.3(3) . . ? C6 C1 S1 122.6(2) . . ? C2 C1 S1 119.1(2) . . ? C3 C2 C1 120.1(3) . . ? C3 C2 C30 117.5(3) . . ? C1 C2 C30 122.3(3) . . ? C2 C3 C4 122.8(3) . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C31 123.5(3) . . ? C3 C4 C31 119.8(3) . . ? C4 C5 C6 122.6(3) . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C7 118.1(3) . . ? C1 C6 C7 122.2(3) . . ? N1 C7 C6 116.0(2) . . ? N1 C9 C10 109.3(3) . . ? N2 C10 C9 109.4(3) . . ? C13 C12 N2 110.6(3) . . ? C12 C13 N3 112.0(3) . . ? N3 C15 C16 111.7(3) . . ? C21 C16 C17 119.6(3) . . ? C21 C16 C15 120.0(3) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 118.2(3) . . ? C16 C17 S2 122.3(2) . . ? C18 C17 S2 119.6(2) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 C22 119.9(3) . . ? C17 C18 C22 119.2(3) . . ? C18 C19 C20 122.2(3) . . ? C21 C20 C19 116.1(3) . . ? C21 C20 C35 123.6(3) . . ? C19 C20 C35 120.0(3) . . ? C20 C21 C16 123.1(3) . . ? C18 C22 N4 110.5(2) . . ? N4 C24 C25 113.2(3) . . ? N5 C25 C24 110.8(3) . . ? N5 C27 C28 112.2(3) . . ? N6 C28 C27 110.9(3) . . ? C2 C30 N6 114.9(2) . . ? C32 C31 C33 108.0(3) . . ? C32 C31 C4 112.5(3) . . ? C33 C31 C4 110.1(3) . . ? C32 C31 C34 109.4(3) . . ? C33 C31 C34 108.5(3) . . ? C4 C31 C34 108.3(3) . . ? C20 C35 C38 107.6(3) . . ? C20 C35 C37 111.5(3) . . ? C38 C35 C37 109.8(4) . . ? C20 C35 C36 112.0(3) . . ? C38 C35 C36 109.3(3) . . ? C37 C35 C36 106.6(3) . . ? O3 Cl1 O4 111.3(4) . . ? O3 Cl1 O2 111.0(3) . . ? O4 Cl1 O2 109.2(3) . . ? O3 Cl1 O1 108.9(3) . . ? O4 Cl1 O1 107.0(3) . . ? O2 Cl1 O1 109.4(2) . . ? O7A Cl2 O6B 126.8(8) . . ? O7A Cl2 O8A 115.9(7) . . ? O6B Cl2 O8A 68.6(12) . . ? O7A Cl2 O7B 26.9(8) . . ? O6B Cl2 O7B 111.5(8) . . ? O8A Cl2 O7B 136.1(7) . . ? O7A Cl2 O5 111.8(5) . . ? O6B Cl2 O5 115.7(6) . . ? O8A Cl2 O5 109.5(5) . . ? O7B Cl2 O5 108.9(5) . . ? O7A Cl2 O8B 73.5(8) . . ? O6B Cl2 O8B 110.7(8) . . ? O8A Cl2 O8B 47.5(8) . . ? O7B Cl2 O8B 99.7(7) . . ? O5 Cl2 O8B 109.0(6) . . ? O7A Cl2 O6A 110.5(7) . . ? O6B Cl2 O6A 35.0(12) . . ? O8A Cl2 O6A 103.7(4) . . ? O7B Cl2 O6A 86.2(7) . . ? O5 Cl2 O6A 104.6(3) . . ? O8B Cl2 O6A 141.6(9) . . ? #===END # Attachment 'CCDC_601293n.CIF' data_7_BPH4 _database_code_depnum_ccdc_archive 'CCDC 601293' _chemical_formula_structural ; [(L2)NiH2](BPh4)2MeCN ; _chemical_formula_sum 'C88 H109 B2 N7 Ni S2' _chemical_formula_weight 1409.27 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from acetonitrile. ; #CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.177(4) _cell_length_b 17.826(4) _cell_length_c 48.531(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15725(6) _cell_formula_units_Z 8 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 230 _cell_measurement_theta_min 8 _cell_measurement_theta_max 22 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.191 _exptl_crystal_F_000 6048 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS, Sheldrick, 1996)' _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46215 _diffrn_reflns_av_R_equivalents 0.1689 _diffrn_reflns_av_sigmaI/netI 0.4246 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.37 _reflns_number_total 18528 _reflns_number_gt 4108 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA _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^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18528 _refine_ls_number_parameters 901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2973 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.2099 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 0.741 _refine_ls_restrained_S_all 0.741 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.328 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.092 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.84711(4) 0.89030(4) 0.818979(16) 0.0353(2) Uani 1 1 d . . . S1 S 0.94130(9) 0.85449(9) 0.84762(3) 0.0409(4) Uani 1 1 d . . . S2 S 0.77198(9) 0.94955(10) 0.85051(4) 0.0447(5) Uani 1 1 d . . . N1 N 0.7874(2) 0.7862(3) 0.82088(11) 0.0407(14) Uani 1 1 d . . . N2 N 0.8789(3) 0.8490(3) 0.77967(10) 0.0402(14) Uani 1 1 d . . . N3 N 0.8802(3) 0.9948(3) 0.80135(10) 0.0362(13) Uani 1 1 d . . . N4 N 0.8530(3) 0.9100(3) 0.90981(10) 0.0374(13) Uani 1 1 d . . . H4 H 0.8568 0.8952 0.8919 0.045 Uiso 1 1 calc R . . N5 N 1.0549(3) 0.8759(3) 0.91917(11) 0.0469(15) Uani 1 1 d . . . N6 N 1.1031(3) 0.8077(3) 0.87053(10) 0.0405(14) Uani 1 1 d . . . H6 H 1.0685 0.8442 0.8724 0.049 Uiso 1 1 calc R . . C1 C 0.9449(3) 0.7543(3) 0.84740(12) 0.0351(15) Uani 1 1 d . . . C2 C 1.0131(3) 0.7184(3) 0.84788(13) 0.0366(16) Uani 1 1 d . . . C3 C 1.0178(3) 0.6412(4) 0.85182(13) 0.0415(17) Uani 1 1 d . . . H3 H 1.0642 0.6194 0.8531 0.050 Uiso 1 1 calc R . . C4 C 0.9565(3) 0.5954(3) 0.85386(12) 0.0382(17) Uani 1 1 d . . . C5 C 0.8876(3) 0.6320(3) 0.85077(13) 0.0429(17) Uani 1 1 d . . . H5 H 0.8451 0.6030 0.8508 0.051 Uiso 1 1 calc R . . C6 C 0.8809(3) 0.7095(3) 0.84774(13) 0.0359(16) Uani 1 1 d . . . C7 C 0.8039(3) 0.7428(3) 0.84655(13) 0.0411(17) Uani 1 1 d . . . H7A H 0.7685 0.7024 0.8482 0.049 Uiso 1 1 calc R . . H7B H 0.7974 0.7757 0.8623 0.049 Uiso 1 1 calc R . . C8 C 0.7070(3) 0.8032(4) 0.82133(15) 0.056(2) Uani 1 1 d . . . H8A H 0.6802 0.7589 0.8264 0.084 Uiso 1 1 calc R . . H8B H 0.6916 0.8194 0.8034 0.084 Uiso 1 1 calc R . . H8C H 0.6975 0.8422 0.8345 0.084 Uiso 1 1 calc R . . C9 C 0.8044(4) 0.7430(4) 0.79531(13) 0.0489(19) Uani 1 1 d . . . H9A H 0.7633 0.7107 0.7907 0.059 Uiso 1 1 calc R . . H9B H 0.8474 0.7119 0.7982 0.059 Uiso 1 1 calc R . . C10 C 0.8185(4) 0.7975(4) 0.77216(13) 0.0486(19) Uani 1 1 d . . . H10A H 0.8315 0.7701 0.7556 0.058 Uiso 1 1 calc R . . H10B H 0.7742 0.8260 0.7684 0.058 Uiso 1 1 calc R . . C11 C 0.9505(4) 0.8073(4) 0.77793(14) 0.058(2) Uani 1 1 d . . . H11A H 0.9420 0.7549 0.7813 0.088 Uiso 1 1 calc R . . H11B H 0.9840 0.8266 0.7915 0.088 Uiso 1 1 calc R . . H11C H 0.9712 0.8136 0.7599 0.088 Uiso 1 1 calc R . . C12 C 0.8820(4) 0.9144(4) 0.76017(13) 0.056(2) Uani 1 1 d . . . H12A H 0.8560 0.9021 0.7433 0.067 Uiso 1 1 calc R . . H12B H 0.9328 0.9252 0.7555 0.067 Uiso 1 1 calc R . . C13 C 0.8470(4) 0.9831(4) 0.77356(11) 0.0467(18) Uani 1 1 d . . . H13A H 0.8553 1.0270 0.7622 0.056 Uiso 1 1 calc R . . H13B H 0.7943 0.9757 0.7753 0.056 Uiso 1 1 calc R . . C14 C 0.9605(3) 1.0071(4) 0.79987(14) 0.055(2) Uani 1 1 d . . . H14A H 0.9844 0.9612 0.7946 0.083 Uiso 1 1 calc R . . H14B H 0.9783 1.0229 0.8176 0.083 Uiso 1 1 calc R . . H14C H 0.9710 1.0452 0.7864 0.083 Uiso 1 1 calc R . . C15 C 0.8455(4) 1.0648(3) 0.81252(12) 0.0460(18) Uani 1 1 d . . . H15A H 0.8642 1.1079 0.8025 0.055 Uiso 1 1 calc R . . H15B H 0.7927 1.0625 0.8097 0.055 Uiso 1 1 calc R . . C16 C 0.8610(4) 1.0745(4) 0.84263(14) 0.0426(18) Uani 1 1 d . . . C17 C 0.8277(3) 1.0250(3) 0.86136(14) 0.0401(17) Uani 1 1 d . . . C18 C 0.8406(3) 1.0367(3) 0.88956(13) 0.0366(16) Uani 1 1 d . . . C19 C 0.8853(3) 1.0959(3) 0.89804(14) 0.0460(18) Uani 1 1 d . . . H19 H 0.8932 1.1024 0.9168 0.055 Uiso 1 1 calc R . . C20 C 0.9189(4) 1.1460(4) 0.87983(14) 0.0416(17) Uani 1 1 d . . . C21 C 0.9053(3) 1.1335(4) 0.85219(14) 0.0455(18) Uani 1 1 d . . . H21 H 0.9264 1.1657 0.8393 0.055 Uiso 1 1 calc R . . C22 C 0.8092(3) 0.9833(3) 0.91020(13) 0.0421(17) Uani 1 1 d . . . H22A H 0.7581 0.9732 0.9059 0.051 Uiso 1 1 calc R . . H22B H 0.8114 1.0054 0.9284 0.051 Uiso 1 1 calc R . . C23 C 0.8128(4) 0.8500(4) 0.92502(15) 0.063(2) Uani 1 1 d . . . H23A H 0.8458 0.8093 0.9289 0.094 Uiso 1 1 calc R . . H23B H 0.7726 0.8322 0.9140 0.094 Uiso 1 1 calc R . . H23C H 0.7941 0.8699 0.9420 0.094 Uiso 1 1 calc R . . C24 C 0.9293(3) 0.9232(3) 0.92039(14) 0.0466(18) Uani 1 1 d . . . H24A H 0.9258 0.9464 0.9384 0.056 Uiso 1 1 calc R . . H24B H 0.9536 0.9585 0.9082 0.056 Uiso 1 1 calc R . . C25 C 0.9763(3) 0.8543(4) 0.92272(13) 0.0467(18) Uani 1 1 d . . . H25A H 0.9693 0.8312 0.9406 0.056 Uiso 1 1 calc R . . H25B H 0.9624 0.8183 0.9087 0.056 Uiso 1 1 calc R . . C26 C 1.0762(4) 0.9341(4) 0.94055(13) 0.057(2) Uani 1 1 d . . . H26A H 1.0707 0.9131 0.9587 0.086 Uiso 1 1 calc R . . H26B H 1.0450 0.9772 0.9387 0.086 Uiso 1 1 calc R . . H26C H 1.1265 0.9487 0.9378 0.086 Uiso 1 1 calc R . . C27 C 1.1038(4) 0.8121(4) 0.92153(14) 0.054(2) Uani 1 1 d . . . H27A H 1.0904 0.7831 0.9377 0.065 Uiso 1 1 calc R . . H27B H 1.1538 0.8299 0.9240 0.065 Uiso 1 1 calc R . . C28 C 1.1007(4) 0.7617(4) 0.89619(13) 0.0477(19) Uani 1 1 d . . . H28A H 1.1420 0.7272 0.8964 0.057 Uiso 1 1 calc R . . H28B H 1.0557 0.7324 0.8965 0.057 Uiso 1 1 calc R . . C29 C 1.1754(3) 0.8463(4) 0.86653(14) 0.060(2) Uani 1 1 d . . . H29A H 1.1917 0.8670 0.8838 0.090 Uiso 1 1 calc R . . H29B H 1.1699 0.8859 0.8533 0.090 Uiso 1 1 calc R . . H29C H 1.2111 0.8109 0.8600 0.090 Uiso 1 1 calc R . . C30 C 1.0827(3) 0.7627(3) 0.84531(12) 0.0409(17) Uani 1 1 d . . . H30A H 1.0779 0.7967 0.8298 0.049 Uiso 1 1 calc R . . H30B H 1.1227 0.7284 0.8412 0.049 Uiso 1 1 calc R . . C31 C 0.9615(4) 0.5107(3) 0.85993(14) 0.0403(17) Uani 1 1 d . . . C32 C 0.9297(3) 0.4665(4) 0.83548(13) 0.052(2) Uani 1 1 d . . . H32A H 0.9330 0.4137 0.8392 0.079 Uiso 1 1 calc R . . H32B H 0.9572 0.4779 0.8191 0.079 Uiso 1 1 calc R . . H32C H 0.8791 0.4801 0.8328 0.079 Uiso 1 1 calc R . . C33 C 1.0418(4) 0.4858(4) 0.86384(16) 0.069(2) Uani 1 1 d . . . H33A H 1.0632 0.5127 0.8790 0.104 Uiso 1 1 calc R . . H33B H 1.0692 0.4961 0.8473 0.104 Uiso 1 1 calc R . . H33C H 1.0433 0.4329 0.8676 0.104 Uiso 1 1 calc R . . C34 C 0.9181(4) 0.4936(4) 0.88584(13) 0.063(2) Uani 1 1 d . . . H34A H 0.9274 0.4429 0.8915 0.095 Uiso 1 1 calc R . . H34B H 0.8665 0.4998 0.8822 0.095 Uiso 1 1 calc R . . H34C H 0.9327 0.5274 0.9002 0.095 Uiso 1 1 calc R . . C35 C 0.9653(4) 1.2106(4) 0.89011(14) 0.053(2) Uani 1 1 d . . . C36 C 1.0181(5) 1.2403(5) 0.86906(16) 0.115(4) Uani 1 1 d . . . H36A H 1.0518 1.2013 0.8638 0.173 Uiso 1 1 calc R . . H36B H 1.0451 1.2816 0.8767 0.173 Uiso 1 1 calc R . . H36C H 0.9914 1.2570 0.8531 0.173 Uiso 1 1 calc R . . C37 C 1.0074(5) 1.1904(4) 0.91681(17) 0.099(3) Uani 1 1 d . . . H37A H 1.0195 1.1379 0.9166 0.148 Uiso 1 1 calc R . . H37B H 0.9770 1.2012 0.9325 0.148 Uiso 1 1 calc R . . H37C H 1.0518 1.2194 0.9178 0.148 Uiso 1 1 calc R . . C38 C 0.9121(5) 1.2756(4) 0.8977(2) 0.114(4) Uani 1 1 d . . . H38A H 0.9395 1.3160 0.9058 0.171 Uiso 1 1 calc R . . H38B H 0.8761 1.2579 0.9106 0.171 Uiso 1 1 calc R . . H38C H 0.8878 1.2932 0.8814 0.171 Uiso 1 1 calc R . . B1 B 0.7142(4) 0.7260(4) 0.99549(16) 0.039(2) Uani 1 1 d . . . C101 C 0.6339(3) 0.6855(4) 0.99260(12) 0.0409(17) Uani 1 1 d . . . C102 C 0.5683(4) 0.7191(4) 1.00196(14) 0.0489(19) Uani 1 1 d . . . H102 H 0.5711 0.7667 1.0097 0.059 Uiso 1 1 calc R . . C103 C 0.5002(4) 0.6852(4) 1.00022(14) 0.054(2) Uani 1 1 d . . . H103 H 0.4585 0.7108 1.0062 0.065 Uiso 1 1 calc R . . C104 C 0.4935(4) 0.6146(5) 0.98985(14) 0.057(2) Uani 1 1 d . . . H104 H 0.4476 0.5918 0.9886 0.068 Uiso 1 1 calc R . . C105 C 0.5553(4) 0.5774(4) 0.98126(13) 0.0495(19) Uani 1 1 d . . . H105 H 0.5515 0.5287 0.9745 0.059 Uiso 1 1 calc R . . C106 C 0.6237(4) 0.6122(4) 0.98266(13) 0.0439(17) Uani 1 1 d . . . H106 H 0.6647 0.5857 0.9767 0.053 Uiso 1 1 calc R . . C201 C 0.7467(3) 0.7085(4) 1.02599(14) 0.0434(18) Uani 1 1 d . . . C202 C 0.7668(4) 0.6349(4) 1.03283(14) 0.053(2) Uani 1 1 d . . . H202 H 0.7609 0.5979 1.0195 0.063 Uiso 1 1 calc R . . C203 C 0.7949(4) 0.6139(5) 1.05826(18) 0.070(2) Uani 1 1 d . . . H203 H 0.8054 0.5640 1.0622 0.084 Uiso 1 1 calc R . . C204 C 0.8068(4) 0.6696(6) 1.07748(18) 0.078(3) Uani 1 1 d . . . H204 H 0.8289 0.6579 1.0942 0.093 Uiso 1 1 calc R . . C205 C 0.7864(4) 0.7415(5) 1.07210(17) 0.069(2) Uani 1 1 d . . . H205 H 0.7931 0.7779 1.0856 0.083 Uiso 1 1 calc R . . C206 C 0.7557(4) 0.7617(4) 1.04702(15) 0.053(2) Uani 1 1 d . . . H206 H 0.7410 0.8110 1.0441 0.064 Uiso 1 1 calc R . . C301 C 0.7733(4) 0.6930(3) 0.97258(14) 0.0415(17) Uani 1 1 d . . . C302 C 0.7528(4) 0.6787(3) 0.94588(15) 0.0501(19) Uani 1 1 d . . . H302 H 0.7034 0.6831 0.9411 0.060 Uiso 1 1 calc R . . C303 C 0.8035(5) 0.6576(4) 0.92561(16) 0.062(2) Uani 1 1 d . . . H303 H 0.7876 0.6475 0.9078 0.074 Uiso 1 1 calc R . . C304 C 0.8775(5) 0.6517(4) 0.9322(2) 0.071(3) Uani 1 1 d . . . H304 H 0.9115 0.6378 0.9189 0.085 Uiso 1 1 calc R . . C305 C 0.9001(4) 0.6664(4) 0.95833(19) 0.070(3) Uani 1 1 d . . . H305 H 0.9497 0.6632 0.9628 0.084 Uiso 1 1 calc R . . C306 C 0.8496(4) 0.6861(4) 0.97806(15) 0.056(2) Uani 1 1 d . . . H306 H 0.8662 0.6953 0.9959 0.067 Uiso 1 1 calc R . . C401 C 0.7103(4) 0.8158(4) 0.98847(13) 0.0423(18) Uani 1 1 d . . . C402 C 0.7654(4) 0.8666(4) 0.99669(14) 0.053(2) Uani 1 1 d . . . H402 H 0.8047 0.8486 1.0070 0.064 Uiso 1 1 calc R . . C403 C 0.7639(5) 0.9423(4) 0.99013(16) 0.064(2) Uani 1 1 d . . . H403 H 0.8003 0.9741 0.9969 0.077 Uiso 1 1 calc R . . C404 C 0.7090(5) 0.9706(4) 0.97370(16) 0.066(2) Uani 1 1 d . . . H404 H 0.7078 1.0213 0.9693 0.079 Uiso 1 1 calc R . . C405 C 0.6558(4) 0.9228(4) 0.96387(16) 0.062(2) Uani 1 1 d . . . H405 H 0.6194 0.9410 0.9522 0.074 Uiso 1 1 calc R . . C406 C 0.6561(4) 0.8466(4) 0.97132(14) 0.0536(19) Uani 1 1 d . . . H406 H 0.6190 0.8156 0.9646 0.064 Uiso 1 1 calc R . . B2 B 1.2112(4) 1.1097(5) 0.80096(16) 0.043(2) Uani 1 1 d . . . C501 C 1.1635(4) 1.1884(4) 0.80034(13) 0.0422(17) Uani 1 1 d . . . C502 C 1.0889(4) 1.1916(4) 0.79290(14) 0.052(2) Uani 1 1 d . . . H502 H 1.0662 1.1488 0.7860 0.063 Uiso 1 1 calc R . . C503 C 1.0482(4) 1.2572(5) 0.79556(15) 0.067(2) Uani 1 1 d . . . H503 H 0.9986 1.2570 0.7908 0.081 Uiso 1 1 calc R . . C504 C 1.0802(5) 1.3230(5) 0.80512(16) 0.070(3) Uani 1 1 d . . . H504 H 1.0531 1.3672 0.8063 0.085 Uiso 1 1 calc R . . C505 C 1.1514(5) 1.3211(4) 0.81269(15) 0.072(2) Uani 1 1 d . . . H505 H 1.1735 1.3641 0.8197 0.086 Uiso 1 1 calc R . . C506 C 1.1924(4) 1.2555(4) 0.81014(14) 0.060(2) Uani 1 1 d . . . H506 H 1.2416 1.2567 0.8153 0.072 Uiso 1 1 calc R . . C601 C 1.2968(3) 1.1220(4) 0.79047(13) 0.0413(17) Uani 1 1 d . . . C602 C 1.3509(4) 1.0674(4) 0.79520(13) 0.0460(18) Uani 1 1 d . . . H602 H 1.3384 1.0253 0.8055 0.055 Uiso 1 1 calc R . . C603 C 1.4225(4) 1.0731(5) 0.78516(15) 0.058(2) Uani 1 1 d . . . H603 H 1.4567 1.0360 0.7892 0.070 Uiso 1 1 calc R . . C604 C 1.4427(4) 1.1336(5) 0.76924(16) 0.061(2) Uani 1 1 d . . . H604 H 1.4904 1.1380 0.7625 0.073 Uiso 1 1 calc R . . C605 C 1.3914(4) 1.1869(4) 0.76360(16) 0.065(2) Uani 1 1 d . . . H605 H 1.4044 1.2280 0.7528 0.078 Uiso 1 1 calc R . . C606 C 1.3191(4) 1.1812(4) 0.77372(15) 0.057(2) Uani 1 1 d . . . H606 H 1.2852 1.2182 0.7691 0.068 Uiso 1 1 calc R . . C701 C 1.2069(4) 1.0833(3) 0.83275(14) 0.0405(17) Uani 1 1 d . . . C702 C 1.1407(4) 1.0578(4) 0.84358(16) 0.065(2) Uani 1 1 d . . . H702 H 1.1007 1.0522 0.8318 0.078 Uiso 1 1 calc R . . C703 C 1.1318(5) 1.0405(4) 0.87121(18) 0.073(3) Uani 1 1 d . . . H703 H 1.0869 1.0227 0.8777 0.088 Uiso 1 1 calc R . . C704 C 1.1898(6) 1.0497(5) 0.88882(17) 0.076(3) Uani 1 1 d . . . H704 H 1.1838 1.0394 0.9075 0.092 Uiso 1 1 calc R . . C705 C 1.2557(5) 1.0736(4) 0.87954(17) 0.073(3) Uani 1 1 d . . . H705 H 1.2953 1.0793 0.8915 0.088 Uiso 1 1 calc R . . C706 C 1.2630(4) 1.0894(4) 0.85197(15) 0.056(2) Uani 1 1 d . . . H706 H 1.3088 1.1053 0.8458 0.067 Uiso 1 1 calc R . . C801 C 1.1780(3) 1.0460(4) 0.78024(14) 0.0444(18) Uani 1 1 d . . . C802 C 1.1746(4) 0.9702(4) 0.78596(16) 0.061(2) Uani 1 1 d . . . H802 H 1.1901 0.9537 0.8032 0.074 Uiso 1 1 calc R . . C803 C 1.1493(5) 0.9179(5) 0.7673(2) 0.086(3) Uani 1 1 d . . . H803 H 1.1487 0.8675 0.7722 0.103 Uiso 1 1 calc R . . C804 C 1.1252(5) 0.9378(7) 0.7420(2) 0.100(4) Uani 1 1 d . . . H804 H 1.1062 0.9027 0.7297 0.120 Uiso 1 1 calc R . . C805 C 1.1304(5) 1.0141(6) 0.73514(19) 0.091(3) Uani 1 1 d . . . H805 H 1.1162 1.0301 0.7177 0.110 Uiso 1 1 calc R . . C806 C 1.1558(4) 1.0644(4) 0.75366(16) 0.064(2) Uani 1 1 d . . . H806 H 1.1585 1.1145 0.7483 0.077 Uiso 1 1 calc R . . N7 N 0.9129(6) 0.3998(6) 1.0710(2) 0.134(4) Uani 1 1 d . . . C39 C 0.9201(6) 0.4328(7) 1.0517(3) 0.102(4) Uani 1 1 d . . . C40 C 0.9323(6) 0.4748(7) 1.0277(2) 0.164(6) Uani 1 1 d . . . H40A H 0.9660 0.4485 1.0159 0.246 Uiso 1 1 calc R . . H40B H 0.9526 0.5227 1.0325 0.246 Uiso 1 1 calc R . . H40C H 0.8865 0.4820 1.0182 0.246 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 Ni 0.0316(4) 0.0379(5) 0.0363(4) 0.0002(4) -0.0008(4) 0.0008(4) S1 0.0382(10) 0.0381(10) 0.0464(11) 0.0018(9) -0.0073(9) -0.0004(8) S2 0.0345(10) 0.0479(11) 0.0516(11) -0.0055(10) 0.0041(9) 0.0004(9) N1 0.028(3) 0.048(3) 0.046(4) 0.005(3) -0.004(3) 0.004(3) N2 0.042(3) 0.042(3) 0.037(3) 0.001(3) -0.002(3) 0.001(3) N3 0.040(3) 0.036(3) 0.033(3) -0.001(3) -0.005(3) 0.001(3) N4 0.039(3) 0.035(3) 0.038(3) 0.000(2) 0.005(3) -0.001(3) N5 0.037(3) 0.057(4) 0.047(4) 0.005(3) -0.003(3) 0.005(3) N6 0.036(3) 0.038(3) 0.047(4) -0.003(3) -0.001(3) 0.002(3) C1 0.036(4) 0.031(4) 0.038(4) -0.001(3) -0.005(3) -0.004(3) C2 0.028(4) 0.036(4) 0.045(4) 0.001(3) 0.001(3) -0.001(3) C3 0.030(4) 0.040(4) 0.055(5) -0.009(4) 0.001(3) 0.003(3) C4 0.036(4) 0.035(4) 0.044(4) 0.000(3) 0.002(3) -0.001(3) C5 0.033(4) 0.039(4) 0.056(5) 0.005(4) -0.003(4) -0.005(3) C6 0.032(4) 0.037(4) 0.038(4) 0.001(3) 0.001(3) 0.002(3) C7 0.030(4) 0.039(4) 0.055(5) 0.003(4) -0.002(4) -0.002(3) C8 0.028(4) 0.056(5) 0.084(6) 0.007(4) -0.004(4) 0.005(3) C9 0.056(5) 0.051(5) 0.040(4) -0.009(4) -0.004(4) 0.002(4) C10 0.056(5) 0.050(5) 0.040(4) -0.002(4) -0.005(4) -0.004(4) C11 0.053(5) 0.067(5) 0.055(5) -0.013(4) 0.003(4) 0.010(4) C12 0.073(5) 0.053(5) 0.040(4) -0.001(4) -0.001(4) -0.008(4) C13 0.066(5) 0.053(4) 0.021(4) 0.000(3) -0.004(4) 0.001(4) C14 0.044(5) 0.061(5) 0.062(5) -0.001(4) 0.000(4) -0.012(4) C15 0.064(5) 0.031(4) 0.043(4) 0.002(3) -0.008(4) 0.005(4) C16 0.047(5) 0.035(4) 0.045(4) 0.000(3) -0.003(4) 0.006(4) C17 0.033(4) 0.033(4) 0.054(5) 0.003(4) -0.001(3) 0.005(3) C18 0.040(4) 0.029(4) 0.041(4) 0.000(3) 0.005(4) 0.005(3) C19 0.056(5) 0.038(4) 0.044(4) 0.000(4) -0.002(4) 0.001(4) C20 0.057(5) 0.028(4) 0.039(4) 0.000(4) 0.002(4) -0.001(4) C21 0.055(5) 0.037(4) 0.044(5) 0.003(4) 0.003(4) -0.002(4) C22 0.036(4) 0.036(4) 0.054(5) 0.005(4) 0.013(4) 0.007(3) C23 0.057(5) 0.051(5) 0.081(6) 0.021(4) 0.026(4) -0.007(4) C24 0.041(4) 0.040(4) 0.059(5) -0.001(4) -0.010(4) 0.002(4) C25 0.045(4) 0.050(5) 0.045(4) 0.011(4) -0.003(4) 0.000(4) C26 0.062(5) 0.060(5) 0.048(5) -0.012(4) -0.010(4) -0.006(4) C27 0.047(5) 0.068(5) 0.048(5) 0.002(4) -0.014(4) 0.018(4) C28 0.050(5) 0.048(5) 0.045(5) 0.002(4) -0.008(4) 0.014(4) C29 0.049(5) 0.073(5) 0.057(5) -0.004(4) 0.004(4) -0.023(4) C30 0.041(4) 0.045(4) 0.037(4) -0.004(3) -0.001(3) -0.002(3) C31 0.044(4) 0.029(4) 0.048(5) 0.002(3) 0.002(4) 0.003(3) C32 0.058(5) 0.050(5) 0.049(5) -0.004(4) 0.005(4) -0.001(4) C33 0.062(5) 0.037(5) 0.109(7) 0.006(4) -0.013(5) 0.012(4) C34 0.095(6) 0.042(5) 0.053(5) 0.006(4) 0.007(5) 0.005(4) C35 0.070(5) 0.039(5) 0.049(5) -0.003(4) 0.004(4) -0.015(4) C36 0.158(9) 0.118(8) 0.070(6) -0.028(6) 0.041(6) -0.094(7) C37 0.115(8) 0.085(7) 0.097(7) 0.017(6) -0.044(6) -0.046(6) C38 0.138(9) 0.053(6) 0.150(10) -0.039(6) 0.004(8) -0.005(6) B1 0.040(5) 0.036(5) 0.040(5) -0.005(4) 0.006(4) -0.009(4) C101 0.044(5) 0.041(4) 0.037(4) 0.005(3) 0.003(3) 0.003(4) C102 0.047(5) 0.041(4) 0.059(5) -0.006(4) 0.007(4) 0.001(4) C103 0.041(5) 0.067(6) 0.054(5) 0.003(4) 0.011(4) 0.002(4) C104 0.038(5) 0.066(6) 0.067(5) -0.002(5) -0.001(4) -0.007(5) C105 0.052(5) 0.049(5) 0.047(5) -0.007(4) 0.000(4) -0.011(4) C106 0.046(4) 0.035(4) 0.051(4) 0.000(4) 0.002(3) 0.003(4) C201 0.033(4) 0.046(5) 0.052(5) -0.005(4) 0.010(4) -0.003(4) C202 0.056(5) 0.057(5) 0.044(5) 0.004(4) -0.002(4) 0.006(4) C203 0.054(5) 0.084(7) 0.071(6) 0.010(6) 0.008(5) 0.005(5) C204 0.042(5) 0.129(9) 0.062(6) 0.006(7) -0.008(5) 0.001(6) C205 0.054(5) 0.096(7) 0.057(6) -0.012(5) 0.006(5) -0.025(5) C206 0.044(5) 0.062(5) 0.053(5) 0.001(4) 0.009(4) -0.010(4) C301 0.048(5) 0.033(4) 0.044(5) 0.001(3) -0.003(4) -0.009(3) C302 0.051(5) 0.040(5) 0.060(5) 0.009(4) 0.008(4) -0.006(4) C303 0.084(6) 0.040(5) 0.061(6) -0.003(4) 0.019(5) -0.013(5) C304 0.061(6) 0.050(5) 0.101(8) -0.015(5) 0.039(6) -0.007(5) C305 0.056(6) 0.070(6) 0.085(7) -0.024(5) 0.018(5) -0.007(4) C306 0.049(5) 0.048(5) 0.069(5) -0.015(4) 0.013(5) -0.010(4) C401 0.045(5) 0.041(4) 0.041(4) -0.006(4) 0.019(4) -0.007(4) C402 0.062(5) 0.039(5) 0.060(5) -0.001(4) 0.006(4) -0.007(4) C403 0.078(6) 0.038(5) 0.076(6) 0.000(4) 0.015(5) -0.011(5) C404 0.091(7) 0.032(5) 0.074(6) 0.010(4) 0.027(5) 0.005(5) C405 0.061(5) 0.053(5) 0.071(6) 0.009(4) 0.015(5) 0.007(5) C406 0.064(5) 0.034(4) 0.062(5) 0.001(4) 0.009(5) -0.002(4) B2 0.035(5) 0.049(5) 0.044(5) 0.004(5) 0.004(4) 0.002(4) C501 0.048(5) 0.043(4) 0.036(4) 0.003(3) -0.001(4) -0.001(4) C502 0.045(5) 0.065(6) 0.047(5) 0.004(4) 0.004(4) 0.008(4) C503 0.053(5) 0.090(7) 0.059(6) 0.020(5) 0.012(5) 0.021(6) C504 0.079(7) 0.077(7) 0.055(6) 0.017(5) 0.024(5) 0.031(6) C505 0.090(7) 0.057(6) 0.068(6) -0.008(4) 0.012(6) 0.011(6) C506 0.054(5) 0.059(5) 0.068(6) -0.006(4) 0.003(4) -0.006(5) C601 0.041(4) 0.039(4) 0.044(4) 0.000(4) -0.008(3) -0.002(4) C602 0.045(4) 0.050(5) 0.043(4) 0.001(3) -0.001(4) 0.001(4) C603 0.044(5) 0.081(6) 0.050(5) -0.015(5) -0.010(4) 0.009(5) C604 0.038(5) 0.077(6) 0.068(6) -0.014(5) 0.007(4) -0.007(5) C605 0.048(5) 0.060(6) 0.086(6) 0.007(5) 0.018(5) -0.015(5) C606 0.053(5) 0.047(5) 0.070(6) 0.003(4) -0.006(4) -0.006(4) C701 0.033(4) 0.042(4) 0.046(4) 0.000(3) -0.002(4) -0.003(3) C702 0.052(5) 0.080(6) 0.063(6) 0.014(5) -0.005(5) 0.003(4) C703 0.070(6) 0.081(7) 0.068(6) 0.011(5) 0.028(5) -0.003(5) C704 0.104(8) 0.078(7) 0.047(5) 0.014(5) 0.006(6) 0.002(6) C705 0.077(7) 0.093(7) 0.049(6) 0.007(5) 0.003(5) -0.005(5) C706 0.050(5) 0.069(6) 0.049(5) 0.003(4) 0.004(4) -0.003(4) C801 0.035(4) 0.054(5) 0.044(5) -0.004(4) -0.008(3) 0.001(4) C802 0.061(5) 0.052(5) 0.071(6) -0.012(5) -0.007(4) 0.003(4) C803 0.071(6) 0.054(6) 0.132(9) -0.033(6) 0.010(7) -0.012(5) C804 0.060(6) 0.133(10) 0.107(9) -0.081(9) -0.002(6) -0.010(7) C805 0.069(7) 0.131(9) 0.075(7) -0.048(7) -0.008(5) -0.001(7) C806 0.061(5) 0.073(6) 0.058(5) -0.016(5) -0.011(5) -0.007(5) N7 0.135(8) 0.131(9) 0.136(9) -0.001(7) 0.047(8) -0.007(7) C39 0.095(8) 0.112(10) 0.099(10) 0.001(8) 0.027(8) 0.014(7) C40 0.171(12) 0.220(14) 0.101(9) 0.069(10) 0.034(9) 0.057(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N2 2.125(5) . ? Ni N3 2.137(5) . ? Ni N1 2.152(5) . ? Ni S1 2.2960(18) . ? Ni S2 2.3070(19) . ? S1 C1 1.787(6) . ? S2 C17 1.764(6) . ? N1 C8 1.492(6) . ? N1 C9 1.493(7) . ? N1 C7 1.497(7) . ? N2 C10 1.478(7) . ? N2 C11 1.501(7) . ? N2 C12 1.502(7) . ? N3 C14 1.478(7) . ? N3 C13 1.493(7) . ? N3 C15 1.499(7) . ? N4 C23 1.491(7) . ? N4 C24 1.497(7) . ? N4 C22 1.529(7) . ? N5 C27 1.448(7) . ? N5 C25 1.490(7) . ? N5 C26 1.517(7) . ? N6 C28 1.491(7) . ? N6 C29 1.497(7) . ? N6 C30 1.510(7) . ? C1 C2 1.395(7) . ? C1 C6 1.412(8) . ? C2 C3 1.392(8) . ? C2 C30 1.497(7) . ? C3 C4 1.386(8) . ? C4 C5 1.420(8) . ? C4 C31 1.540(8) . ? C5 C6 1.395(8) . ? C6 C7 1.520(7) . ? C9 C10 1.506(8) . ? C12 C13 1.526(8) . ? C15 C16 1.498(8) . ? C16 C21 1.403(8) . ? C16 C17 1.404(8) . ? C17 C18 1.404(8) . ? C18 C19 1.395(8) . ? C18 C22 1.495(8) . ? C19 C20 1.397(8) . ? C20 C21 1.382(8) . ? C20 C35 1.511(8) . ? C24 C25 1.500(8) . ? C27 C28 1.525(8) . ? C31 C34 1.516(8) . ? C31 C33 1.538(8) . ? C31 C32 1.538(8) . ? C35 C36 1.499(9) . ? C35 C37 1.548(9) . ? C35 C38 1.554(9) . ? B1 C201 1.623(10) . ? B1 C101 1.635(9) . ? B1 C401 1.639(9) . ? B1 C301 1.654(9) . ? C101 C106 1.404(8) . ? C101 C102 1.410(8) . ? C102 C103 1.381(8) . ? C103 C104 1.361(9) . ? C104 C105 1.368(8) . ? C105 C106 1.392(8) . ? C201 C202 1.402(9) . ? C201 C206 1.403(9) . ? C202 C203 1.388(9) . ? C203 C204 1.379(10) . ? C204 C205 1.359(10) . ? C205 C206 1.387(9) . ? C301 C302 1.372(8) . ? C301 C306 1.417(8) . ? C302 C303 1.399(9) . ? C303 C304 1.388(10) . ? C304 C305 1.357(10) . ? C305 C306 1.372(9) . ? C401 C406 1.403(8) . ? C401 C402 1.408(8) . ? C402 C403 1.386(9) . ? C403 C404 1.374(9) . ? C404 C405 1.373(9) . ? C405 C406 1.405(8) . ? B2 C701 1.615(9) . ? B2 C801 1.632(10) . ? B2 C501 1.649(9) . ? B2 C601 1.652(9) . ? C501 C506 1.390(8) . ? C501 C502 1.405(8) . ? C502 C503 1.390(9) . ? C503 C504 1.389(10) . ? C504 C505 1.347(10) . ? C505 C506 1.390(9) . ? C601 C606 1.392(8) . ? C601 C602 1.404(8) . ? C602 C603 1.392(8) . ? C603 C604 1.376(9) . ? C604 C605 1.358(9) . ? C605 C606 1.406(9) . ? C701 C706 1.386(8) . ? C701 C702 1.389(8) . ? C702 C703 1.386(9) . ? C703 C704 1.368(10) . ? C704 C705 1.349(10) . ? C705 C706 1.374(9) . ? C801 C802 1.380(9) . ? C801 C806 1.391(9) . ? C802 C803 1.381(10) . ? C803 C804 1.351(12) . ? C804 C805 1.402(12) . ? C805 C806 1.352(10) . ? N7 C39 1.116(12) . ? C39 C40 1.400(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 N2 Ni N3 82.28(19) . . ? N2 Ni N1 83.0(2) . . ? N3 Ni N1 155.7(2) . . ? N2 Ni S1 104.16(15) . . ? N3 Ni S1 105.95(14) . . ? N1 Ni S1 96.35(14) . . ? N2 Ni S2 156.21(15) . . ? N3 Ni S2 91.90(14) . . ? N1 Ni S2 93.87(15) . . ? S1 Ni S2 99.62(7) . . ? C1 S1 Ni 107.6(2) . . ? C17 S2 Ni 101.9(2) . . ? C8 N1 C9 108.6(5) . . ? C8 N1 C7 106.8(5) . . ? C9 N1 C7 112.6(5) . . ? C8 N1 Ni 108.7(4) . . ? C9 N1 Ni 107.7(4) . . ? C7 N1 Ni 112.3(4) . . ? C10 N2 C11 108.7(5) . . ? C10 N2 C12 110.8(5) . . ? C11 N2 C12 108.5(5) . . ? C10 N2 Ni 103.6(4) . . ? C11 N2 Ni 117.2(4) . . ? C12 N2 Ni 107.9(4) . . ? C14 N3 C13 112.1(5) . . ? C14 N3 C15 108.1(5) . . ? C13 N3 C15 105.8(4) . . ? C14 N3 Ni 115.3(4) . . ? C13 N3 Ni 97.2(3) . . ? C15 N3 Ni 117.5(4) . . ? C23 N4 C24 113.3(5) . . ? C23 N4 C22 110.6(5) . . ? C24 N4 C22 110.1(5) . . ? C27 N5 C25 112.1(5) . . ? C27 N5 C26 109.0(5) . . ? C25 N5 C26 110.0(5) . . ? C28 N6 C29 112.8(5) . . ? C28 N6 C30 112.2(5) . . ? C29 N6 C30 110.8(5) . . ? C2 C1 C6 118.2(5) . . ? C2 C1 S1 119.4(5) . . ? C6 C1 S1 122.3(5) . . ? C3 C2 C1 120.7(6) . . ? C3 C2 C30 118.7(6) . . ? C1 C2 C30 120.5(6) . . ? C4 C3 C2 122.9(6) . . ? C3 C4 C5 115.5(6) . . ? C3 C4 C31 122.9(6) . . ? C5 C4 C31 121.5(6) . . ? C6 C5 C4 123.0(6) . . ? C5 C6 C1 119.2(6) . . ? C5 C6 C7 118.2(6) . . ? C1 C6 C7 122.5(5) . . ? N1 C7 C6 114.7(5) . . ? N1 C9 C10 108.9(5) . . ? N2 C10 C9 110.1(5) . . ? N2 C12 C13 109.8(5) . . ? N3 C13 C12 109.2(5) . . ? C16 C15 N3 111.7(5) . . ? C21 C16 C17 120.3(6) . . ? C21 C16 C15 121.1(6) . . ? C17 C16 C15 118.5(6) . . ? C18 C17 C16 117.8(6) . . ? C18 C17 S2 120.0(5) . . ? C16 C17 S2 122.3(5) . . ? C19 C18 C17 119.8(6) . . ? C19 C18 C22 120.4(6) . . ? C17 C18 C22 119.7(6) . . ? C18 C19 C20 123.5(6) . . ? C21 C20 C19 115.6(6) . . ? C21 C20 C35 122.9(6) . . ? C19 C20 C35 121.5(6) . . ? C20 C21 C16 123.0(6) . . ? C18 C22 N4 109.7(5) . . ? N4 C24 C25 115.2(5) . . ? N5 C25 C24 109.1(5) . . ? N5 C27 C28 112.1(5) . . ? N6 C28 C27 110.4(5) . . ? C2 C30 N6 114.8(5) . . ? C34 C31 C33 109.5(6) . . ? C34 C31 C32 109.9(5) . . ? C33 C31 C32 107.7(5) . . ? C34 C31 C4 108.9(5) . . ? C33 C31 C4 111.3(5) . . ? C32 C31 C4 109.5(5) . . ? C36 C35 C20 113.7(6) . . ? C36 C35 C37 109.6(7) . . ? C20 C35 C37 112.0(6) . . ? C36 C35 C38 107.3(7) . . ? C20 C35 C38 107.4(6) . . ? C37 C35 C38 106.5(6) . . ? C201 B1 C101 108.6(5) . . ? C201 B1 C401 113.1(6) . . ? C101 B1 C401 112.0(6) . . ? C201 B1 C301 108.0(5) . . ? C101 B1 C301 111.5(5) . . ? C401 B1 C301 103.6(5) . . ? C106 C101 C102 113.2(6) . . ? C106 C101 B1 123.9(6) . . ? C102 C101 B1 122.7(6) . . ? C103 C102 C101 123.6(7) . . ? C104 C103 C102 120.4(7) . . ? C103 C104 C105 119.2(7) . . ? C104 C105 C106 120.1(7) . . ? C105 C106 C101 123.4(6) . . ? C202 C201 C206 115.5(7) . . ? C202 C201 B1 119.3(6) . . ? C206 C201 B1 125.2(6) . . ? C203 C202 C201 124.0(7) . . ? C204 C203 C202 117.7(8) . . ? C205 C204 C203 120.4(9) . . ? C204 C205 C206 121.6(8) . . ? C205 C206 C201 120.6(7) . . ? C302 C301 C306 115.3(7) . . ? C302 C301 B1 121.6(6) . . ? C306 C301 B1 122.7(6) . . ? C301 C302 C303 122.3(7) . . ? C304 C303 C302 119.7(8) . . ? C305 C304 C303 119.7(8) . . ? C304 C305 C306 119.9(8) . . ? C305 C306 C301 123.1(7) . . ? C406 C401 C402 114.6(6) . . ? C406 C401 B1 122.4(6) . . ? C402 C401 B1 122.6(6) . . ? C403 C402 C401 123.2(7) . . ? C404 C403 C402 120.3(8) . . ? C405 C404 C403 119.0(7) . . ? C404 C405 C406 120.5(8) . . ? C401 C406 C405 122.2(7) . . ? C701 B2 C801 111.6(6) . . ? C701 B2 C501 103.9(5) . . ? C801 B2 C501 112.8(6) . . ? C701 B2 C601 112.2(6) . . ? C801 B2 C601 104.5(5) . . ? C501 B2 C601 112.1(6) . . ? C506 C501 C502 114.6(7) . . ? C506 C501 B2 121.9(6) . . ? C502 C501 B2 123.1(6) . . ? C503 C502 C501 121.7(7) . . ? C504 C503 C502 121.2(8) . . ? C505 C504 C503 118.1(8) . . ? C504 C505 C506 120.8(8) . . ? C501 C506 C505 123.5(7) . . ? C606 C601 C602 114.7(6) . . ? C606 C601 B2 123.7(6) . . ? C602 C601 B2 121.2(6) . . ? C603 C602 C601 123.1(7) . . ? C604 C603 C602 120.2(7) . . ? C605 C604 C603 118.5(7) . . ? C604 C605 C606 121.4(7) . . ? C601 C606 C605 122.1(7) . . ? C706 C701 C702 114.1(6) . . ? C706 C701 B2 125.8(6) . . ? C702 C701 B2 119.9(6) . . ? C703 C702 C701 122.7(7) . . ? C704 C703 C702 119.1(8) . . ? C705 C704 C703 121.0(8) . . ? C704 C705 C706 118.4(8) . . ? C705 C706 C701 124.7(7) . . ? C802 C801 C806 113.9(7) . . ? C802 C801 B2 125.0(7) . . ? C806 C801 B2 121.0(7) . . ? C801 C802 C803 123.0(8) . . ? C804 C803 C802 121.8(9) . . ? C803 C804 C805 116.6(9) . . ? C806 C805 C804 120.7(10) . . ? C805 C806 C801 124.0(8) . . ? N7 C39 C40 177.6(16) . . ? #===END # Attachment 'CCDC_601294n.CIF' data_8 _database_code_depnum_ccdc_archive 'CCDC 601294' _chemical_formula_structural ; [ZnH2(L2)(ClO4)2MeOH ; _chemical_formula_sum 'C39 H70 Cl2 N6 O9 S2 Zn' _chemical_formula_weight 967.40 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown from methanol. ; #CRYSTAL DATA _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 14.270(3) _cell_length_b 16.937(3) _cell_length_c 19.708(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.15(3) _cell_angle_gamma 90.00 _cell_volume 4750.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 88 _cell_measurement_theta_min 6 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS, Sheldrick, 1996)' _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29408 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.31 _reflns_number_total 11276 _reflns_number_gt 7641 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA _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^)+(0.0962P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11276 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.563 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.079 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' 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 Zn Zn 0.36417(3) 0.12085(2) 0.160769(17) 0.03112(11) Uani 1 1 d . . . S1 S 0.40690(5) 0.18940(5) 0.25941(4) 0.03398(18) Uani 1 1 d . . . S2 S 0.32207(6) -0.00742(4) 0.18696(4) 0.03428(18) Uani 1 1 d . . . N1 N 0.51060(19) 0.08431(15) 0.13669(13) 0.0356(6) Uani 1 1 d . . . N2 N 0.3708(2) 0.18135(16) 0.06809(14) 0.0405(6) Uani 1 1 d . . . N3 N 0.20452(19) 0.15706(16) 0.13937(14) 0.0381(6) Uani 1 1 d . . . N4 N 0.38128(17) 0.00095(15) 0.34977(13) 0.0320(5) Uani 1 1 d . . . H4 H 0.3908 0.0270 0.3105 0.038 Uiso 1 1 calc R . . N5 N 0.38633(19) 0.18519(15) 0.45790(13) 0.0359(6) Uani 1 1 d . . . N6 N 0.43870(17) 0.31604(14) 0.37536(12) 0.0287(5) Uani 1 1 d . . . H6 H 0.3971 0.2779 0.3607 0.034 Uiso 1 1 calc R . . C1 C 0.5242(2) 0.22192(17) 0.25304(14) 0.0304(6) Uani 1 1 d . . . C2 C 0.5509(2) 0.29531(17) 0.28243(15) 0.0306(6) Uani 1 1 d . . . C3 C 0.6429(2) 0.32156(18) 0.28150(16) 0.0334(7) Uani 1 1 d . . . H3 H 0.6592 0.3695 0.3022 0.040 Uiso 1 1 calc R . . C4 C 0.7121(2) 0.27876(18) 0.25065(16) 0.0336(7) Uani 1 1 d . . . C5 C 0.6852(2) 0.20700(18) 0.22234(16) 0.0352(7) Uani 1 1 d . . . H5 H 0.7295 0.1774 0.2012 0.042 Uiso 1 1 calc R . . C6 C 0.5938(2) 0.17684(18) 0.22412(15) 0.0327(6) Uani 1 1 d . . . C7 C 0.5768(2) 0.09354(18) 0.19895(17) 0.0364(7) Uani 1 1 d . . . H7A H 0.6368 0.0707 0.1894 0.044 Uiso 1 1 calc R . . H7B H 0.5525 0.0630 0.2354 0.044 Uiso 1 1 calc R . . C8 C 0.5149(3) 0.0005(2) 0.1158(2) 0.0494(9) Uani 1 1 d . . . H8A H 0.4695 -0.0088 0.0783 0.074 Uiso 1 1 calc R . . H8B H 0.5013 -0.0327 0.1533 0.074 Uiso 1 1 calc R . . H8C H 0.5767 -0.0112 0.1023 0.074 Uiso 1 1 calc R . . C9 C 0.5348(3) 0.1355(2) 0.08029(18) 0.0470(9) Uani 1 1 d . . . H9A H 0.5847 0.1115 0.0564 0.056 Uiso 1 1 calc R . . H9B H 0.5568 0.1862 0.0979 0.056 Uiso 1 1 calc R . . C10 C 0.4476(3) 0.1469(3) 0.03145(19) 0.0570(10) Uani 1 1 d . . . H10A H 0.4624 0.1816 -0.0054 0.068 Uiso 1 1 calc R . . H10B H 0.4278 0.0964 0.0120 0.068 Uiso 1 1 calc R . . C11 C 0.3880(3) 0.2670(2) 0.0788(2) 0.0562(10) Uani 1 1 d . . . H11A H 0.4501 0.2748 0.0997 0.084 Uiso 1 1 calc R . . H11B H 0.3428 0.2878 0.1078 0.084 Uiso 1 1 calc R . . H11C H 0.3821 0.2937 0.0358 0.084 Uiso 1 1 calc R . . C12 C 0.2788(3) 0.1665(2) 0.02937(18) 0.0533(10) Uani 1 1 d . . . H12A H 0.2723 0.1106 0.0194 0.064 Uiso 1 1 calc R . . H12B H 0.2764 0.1950 -0.0134 0.064 Uiso 1 1 calc R . . C13 C 0.1997(3) 0.1931(2) 0.0702(2) 0.0517(10) Uani 1 1 d . . . H13A H 0.2017 0.2502 0.0746 0.062 Uiso 1 1 calc R . . H13B H 0.1403 0.1791 0.0461 0.062 Uiso 1 1 calc R . . C14 C 0.1742(3) 0.2144(2) 0.1896(2) 0.0508(9) Uani 1 1 d . . . H14A H 0.2150 0.2596 0.1907 0.076 Uiso 1 1 calc R . . H14B H 0.1771 0.1903 0.2338 0.076 Uiso 1 1 calc R . . H14C H 0.1109 0.2308 0.1771 0.076 Uiso 1 1 calc R . . C15 C 0.1420(2) 0.0861(2) 0.13745(17) 0.0381(7) Uani 1 1 d . . . H15A H 0.1631 0.0487 0.1045 0.046 Uiso 1 1 calc R . . H15B H 0.0785 0.1020 0.1225 0.046 Uiso 1 1 calc R . . C16 C 0.1412(2) 0.04641(18) 0.20565(16) 0.0335(7) Uani 1 1 d . . . C17 C 0.2217(2) 0.00706(17) 0.23327(16) 0.0314(6) Uani 1 1 d . . . C18 C 0.2200(2) -0.02448(17) 0.29905(16) 0.0320(6) Uani 1 1 d . . . C19 C 0.1397(2) -0.01875(19) 0.33502(16) 0.0355(7) Uani 1 1 d . . . H19 H 0.1406 -0.0397 0.3787 0.043 Uiso 1 1 calc R . . C20 C 0.0583(2) 0.01762(18) 0.30707(17) 0.0353(7) Uani 1 1 d . . . C21 C 0.0618(2) 0.05053(19) 0.24297(17) 0.0373(7) Uani 1 1 d . . . H21 H 0.0089 0.0766 0.2239 0.045 Uiso 1 1 calc R . . C22 C 0.3068(2) -0.06103(17) 0.33281(17) 0.0342(7) Uani 1 1 d . . . H22A H 0.3312 -0.1002 0.3028 0.041 Uiso 1 1 calc R . . H22B H 0.2914 -0.0875 0.3742 0.041 Uiso 1 1 calc R . . C23 C 0.4714(2) -0.0389(2) 0.37236(19) 0.0432(8) Uani 1 1 d . . . H23A H 0.5193 0.0002 0.3819 0.065 Uiso 1 1 calc R . . H23B H 0.4897 -0.0734 0.3370 0.065 Uiso 1 1 calc R . . H23C H 0.4631 -0.0690 0.4127 0.065 Uiso 1 1 calc R . . C24 C 0.3475(2) 0.06047(18) 0.39862(16) 0.0345(7) Uani 1 1 d . . . H24A H 0.3181 0.0330 0.4347 0.041 Uiso 1 1 calc R . . H24B H 0.3001 0.0935 0.3750 0.041 Uiso 1 1 calc R . . C25 C 0.4259(2) 0.11285(18) 0.43003(17) 0.0354(7) Uani 1 1 d . . . H25A H 0.4614 0.0843 0.4660 0.042 Uiso 1 1 calc R . . H25B H 0.4685 0.1267 0.3957 0.042 Uiso 1 1 calc R . . C26 C 0.3265(3) 0.1669(2) 0.51274(19) 0.0548(10) Uani 1 1 d . . . H26A H 0.3619 0.1378 0.5477 0.082 Uiso 1 1 calc R . . H26B H 0.2740 0.1357 0.4952 0.082 Uiso 1 1 calc R . . H26C H 0.3040 0.2151 0.5315 0.082 Uiso 1 1 calc R . . C27 C 0.4612(2) 0.23915(19) 0.48250(15) 0.0390(7) Uani 1 1 d . . . H27A H 0.5078 0.2100 0.5107 0.047 Uiso 1 1 calc R . . H27B H 0.4350 0.2794 0.5106 0.047 Uiso 1 1 calc R . . C28 C 0.5090(2) 0.27886(19) 0.42491(16) 0.0353(7) Uani 1 1 d . . . H28A H 0.5522 0.3189 0.4436 0.042 Uiso 1 1 calc R . . H28B H 0.5450 0.2400 0.4017 0.042 Uiso 1 1 calc R . . C29 C 0.3846(3) 0.3795(2) 0.40732(19) 0.0502(9) Uani 1 1 d . . . H29A H 0.3474 0.3568 0.4411 0.075 Uiso 1 1 calc R . . H29B H 0.3441 0.4052 0.3731 0.075 Uiso 1 1 calc R . . H29C H 0.4274 0.4174 0.4284 0.075 Uiso 1 1 calc R . . C30 C 0.4816(2) 0.34911(17) 0.31343(15) 0.0325(6) Uani 1 1 d . . . H30A H 0.4314 0.3612 0.2792 0.039 Uiso 1 1 calc R . . H30B H 0.5130 0.3983 0.3260 0.039 Uiso 1 1 calc R . . C31 C 0.8124(2) 0.31053(19) 0.25262(17) 0.0383(7) Uani 1 1 d . . . C32 C 0.8746(3) 0.2619(2) 0.2083(2) 0.0525(9) Uani 1 1 d . . . H32A H 0.8785 0.2086 0.2249 0.079 Uiso 1 1 calc R . . H32B H 0.9364 0.2846 0.2101 0.079 Uiso 1 1 calc R . . H32C H 0.8480 0.2620 0.1622 0.079 Uiso 1 1 calc R . . C33 C 0.8130(3) 0.3961(2) 0.2282(2) 0.0542(10) Uani 1 1 d . . . H33A H 0.7883 0.3986 0.1816 0.081 Uiso 1 1 calc R . . H33B H 0.8763 0.4158 0.2318 0.081 Uiso 1 1 calc R . . H33C H 0.7748 0.4276 0.2558 0.081 Uiso 1 1 calc R . . C34 C 0.8540(3) 0.3073(3) 0.3268(2) 0.0593(11) Uani 1 1 d . . . H34A H 0.8215 0.3442 0.3537 0.089 Uiso 1 1 calc R . . H34B H 0.9195 0.3207 0.3286 0.089 Uiso 1 1 calc R . . H34C H 0.8468 0.2550 0.3445 0.089 Uiso 1 1 calc R . . C35 C -0.0275(2) 0.0244(2) 0.34990(18) 0.0429(8) Uani 1 1 d . . . C36 C -0.1159(3) 0.0503(3) 0.3060(2) 0.0653(12) Uani 1 1 d . . . H36A H -0.1698 0.0464 0.3323 0.098 Uiso 1 1 calc R . . H36B H -0.1244 0.0166 0.2669 0.098 Uiso 1 1 calc R . . H36C H -0.1085 0.1039 0.2916 0.098 Uiso 1 1 calc R . . C37 C -0.0489(3) -0.0550(2) 0.3817(2) 0.0589(10) Uani 1 1 d . . . H37A H 0.0021 -0.0697 0.4137 0.088 Uiso 1 1 calc R . . H37B H -0.0566 -0.0944 0.3467 0.088 Uiso 1 1 calc R . . H37C H -0.1057 -0.0510 0.4048 0.088 Uiso 1 1 calc R . . C38 C -0.0054(3) 0.0845(3) 0.4066(3) 0.0815(16) Uani 1 1 d . . . H38A H 0.0496 0.0682 0.4338 0.122 Uiso 1 1 calc R . . H38B H -0.0576 0.0880 0.4346 0.122 Uiso 1 1 calc R . . H38C H 0.0056 0.1353 0.3869 0.122 Uiso 1 1 calc R . . Cl1 Cl 0.82525(7) 0.02862(5) 0.07486(5) 0.0478(2) Uani 1 1 d . . . O1 O 0.7549(3) 0.0347(3) 0.0216(2) 0.1032(13) Uani 1 1 d . . . O2 O 0.7862(3) 0.0060(3) 0.1341(2) 0.1259(17) Uani 1 1 d . . . O3 O 0.8710(5) 0.1011(3) 0.0824(2) 0.144(2) Uani 1 1 d . . . O4 O 0.8876(3) -0.0291(3) 0.0541(3) 0.1356(18) Uani 1 1 d . . . Cl2 Cl 0.79191(6) 0.59665(5) 0.04342(5) 0.0449(2) Uani 1 1 d . . . O5 O 0.8543(2) 0.6188(2) -0.00623(16) 0.0764(10) Uani 1 1 d . . . O6 O 0.7132(3) 0.5579(3) 0.0085(2) 0.1160(16) Uani 1 1 d . . . O7 O 0.7551(4) 0.6637(2) 0.0717(2) 0.1206(16) Uani 1 1 d . . . O8 O 0.8323(3) 0.5484(4) 0.0911(3) 0.172(3) Uani 1 1 d . . . C39 C 0.2086(11) 0.2949(7) 0.3366(5) 0.231(7) Uani 1 1 d . . . O9 O 0.1452(6) 0.2803(6) 0.4068(8) 0.388(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0393(2) 0.02623(18) 0.02746(19) -0.00259(13) -0.00024(14) -0.00264(14) S1 0.0324(4) 0.0388(4) 0.0308(4) -0.0101(3) 0.0029(3) -0.0039(3) S2 0.0377(4) 0.0258(4) 0.0395(4) -0.0021(3) 0.0036(3) -0.0010(3) N1 0.0425(15) 0.0308(13) 0.0342(15) -0.0089(11) 0.0081(11) -0.0031(11) N2 0.0508(17) 0.0379(15) 0.0320(15) 0.0012(11) -0.0017(12) -0.0052(12) N3 0.0396(15) 0.0329(14) 0.0405(16) 0.0055(11) -0.0063(12) -0.0013(11) N4 0.0306(13) 0.0312(13) 0.0338(14) 0.0000(10) 0.0003(10) 0.0012(10) N5 0.0411(15) 0.0338(14) 0.0326(14) -0.0024(11) 0.0010(11) 0.0021(11) N6 0.0317(13) 0.0260(12) 0.0280(13) -0.0018(9) -0.0010(10) 0.0025(10) C1 0.0335(15) 0.0294(15) 0.0280(15) -0.0011(11) 0.0001(12) -0.0007(12) C2 0.0351(16) 0.0273(14) 0.0294(15) -0.0008(11) 0.0030(12) 0.0010(12) C3 0.0383(16) 0.0277(15) 0.0340(17) -0.0029(12) 0.0023(13) -0.0033(12) C4 0.0330(16) 0.0345(16) 0.0337(16) 0.0031(12) 0.0042(12) -0.0022(12) C5 0.0355(16) 0.0359(16) 0.0348(17) -0.0012(13) 0.0065(13) 0.0039(13) C6 0.0359(16) 0.0294(15) 0.0327(16) -0.0015(12) 0.0018(13) 0.0024(12) C7 0.0379(17) 0.0277(15) 0.0438(19) -0.0035(13) 0.0051(14) 0.0039(13) C8 0.050(2) 0.0386(19) 0.061(2) -0.0195(17) 0.0157(18) -0.0018(16) C9 0.054(2) 0.052(2) 0.0367(19) -0.0015(15) 0.0140(16) -0.0034(17) C10 0.071(3) 0.067(3) 0.034(2) -0.0019(18) 0.0101(18) -0.008(2) C11 0.070(3) 0.040(2) 0.057(2) 0.0115(17) -0.006(2) -0.0130(18) C12 0.065(2) 0.056(2) 0.0359(19) 0.0100(17) -0.0162(18) -0.0136(19) C13 0.050(2) 0.046(2) 0.056(2) 0.0209(17) -0.0150(18) -0.0021(17) C14 0.050(2) 0.0365(19) 0.065(3) -0.0060(17) 0.0001(18) 0.0079(16) C15 0.0374(17) 0.0378(17) 0.0377(18) 0.0024(13) -0.0077(14) -0.0031(14) C16 0.0344(16) 0.0304(15) 0.0348(17) -0.0026(12) -0.0044(13) -0.0056(12) C17 0.0335(15) 0.0249(14) 0.0350(16) -0.0057(12) -0.0026(12) -0.0030(12) C18 0.0349(16) 0.0251(14) 0.0347(16) -0.0007(12) -0.0048(13) -0.0023(12) C19 0.0375(17) 0.0328(16) 0.0357(17) -0.0016(12) -0.0004(13) -0.0054(13) C20 0.0335(16) 0.0312(16) 0.0408(18) -0.0041(13) 0.0006(13) -0.0011(13) C21 0.0326(16) 0.0330(16) 0.0453(19) -0.0024(14) -0.0046(13) 0.0018(13) C22 0.0346(16) 0.0274(15) 0.0401(18) 0.0020(12) -0.0020(13) -0.0010(12) C23 0.0312(17) 0.0415(18) 0.057(2) -0.0047(15) 0.0006(15) 0.0074(14) C24 0.0339(16) 0.0331(16) 0.0364(17) -0.0032(13) 0.0012(13) 0.0037(12) C25 0.0362(17) 0.0320(16) 0.0367(17) -0.0016(12) -0.0058(13) 0.0035(13) C26 0.067(3) 0.055(2) 0.045(2) -0.0042(17) 0.0192(18) 0.0019(19) C27 0.052(2) 0.0332(16) 0.0299(16) -0.0011(12) -0.0096(14) 0.0020(14) C28 0.0355(16) 0.0346(16) 0.0342(17) 0.0014(13) -0.0090(13) 0.0024(13) C29 0.067(3) 0.045(2) 0.040(2) 0.0035(15) 0.0145(17) 0.0270(18) C30 0.0376(16) 0.0275(14) 0.0327(16) -0.0003(12) 0.0035(12) 0.0012(12) C31 0.0343(17) 0.0373(17) 0.0442(19) 0.0034(14) 0.0083(14) -0.0048(13) C32 0.0389(19) 0.048(2) 0.073(3) 0.0023(18) 0.0170(18) 0.0020(16) C33 0.046(2) 0.044(2) 0.075(3) 0.0066(18) 0.0221(19) -0.0049(16) C34 0.047(2) 0.071(3) 0.059(3) 0.003(2) -0.0081(19) -0.0153(19) C35 0.0374(18) 0.0432(19) 0.048(2) -0.0034(15) 0.0055(15) 0.0011(14) C36 0.039(2) 0.080(3) 0.078(3) 0.018(2) 0.011(2) 0.011(2) C37 0.053(2) 0.061(3) 0.065(3) 0.013(2) 0.0177(19) 0.0027(19) C38 0.058(3) 0.095(4) 0.094(4) -0.049(3) 0.028(3) -0.018(3) Cl1 0.0560(5) 0.0449(5) 0.0434(5) 0.0062(4) 0.0100(4) 0.0017(4) O1 0.104(3) 0.103(3) 0.098(3) 0.015(2) -0.025(2) 0.009(2) O2 0.136(4) 0.159(4) 0.088(3) 0.054(3) 0.048(3) 0.019(3) O3 0.226(6) 0.086(3) 0.118(4) -0.008(3) 0.007(4) -0.075(4) O4 0.106(3) 0.132(4) 0.171(5) -0.041(3) 0.018(3) 0.051(3) Cl2 0.0399(4) 0.0448(5) 0.0507(5) 0.0035(4) 0.0079(4) 0.0021(3) O5 0.065(2) 0.106(3) 0.060(2) 0.0003(17) 0.0171(15) -0.0299(18) O6 0.076(3) 0.149(4) 0.127(4) -0.051(3) 0.033(2) -0.048(3) O7 0.192(5) 0.071(3) 0.106(3) -0.015(2) 0.055(3) 0.025(3) O8 0.097(3) 0.243(7) 0.179(5) 0.151(5) 0.038(3) 0.076(4) C39 0.356(17) 0.205(11) 0.123(7) -0.125(8) -0.042(8) 0.125(11) O9 0.169(7) 0.265(11) 0.70(2) 0.313(14) -0.140(11) -0.105(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn N2 2.103(3) . ? Zn N1 2.262(3) . ? Zn S1 2.3083(9) . ? Zn S2 2.3221(9) . ? Zn N3 2.368(3) . ? S1 C1 1.776(3) . ? S2 C17 1.770(3) . ? N1 C9 1.470(4) . ? N1 C8 1.481(4) . ? N1 C7 1.502(4) . ? N2 C10 1.475(5) . ? N2 C11 1.483(4) . ? N2 C12 1.491(4) . ? N3 C14 1.474(5) . ? N3 C13 1.490(4) . ? N3 C15 1.495(4) . ? N4 C23 1.491(4) . ? N4 C24 1.498(4) . ? N4 C22 1.513(4) . ? N5 C26 1.459(4) . ? N5 C27 1.462(4) . ? N5 C25 1.472(4) . ? N6 C28 1.488(4) . ? N6 C29 1.490(4) . ? N6 C30 1.512(4) . ? C1 C6 1.406(4) . ? C1 C2 1.412(4) . ? C2 C3 1.387(4) . ? C2 C30 1.507(4) . ? C3 C4 1.398(4) . ? C4 C5 1.380(4) . ? C4 C31 1.528(4) . ? C5 C6 1.403(4) . ? C6 C7 1.509(4) . ? C9 C10 1.530(6) . ? C12 C13 1.503(6) . ? C15 C16 1.504(4) . ? C16 C21 1.397(5) . ? C16 C17 1.403(4) . ? C17 C18 1.404(4) . ? C18 C19 1.393(4) . ? C18 C22 1.497(4) . ? C19 C20 1.393(4) . ? C20 C21 1.385(5) . ? C20 C35 1.541(5) . ? C24 C25 1.524(4) . ? C27 C28 1.522(4) . ? C31 C33 1.527(5) . ? C31 C32 1.530(5) . ? C31 C34 1.539(5) . ? C35 C37 1.524(5) . ? C35 C38 1.528(5) . ? C35 C36 1.540(5) . ? Cl1 O2 1.384(4) . ? Cl1 O3 1.393(4) . ? Cl1 O1 1.402(4) . ? Cl1 O4 1.403(4) . ? Cl2 O8 1.344(4) . ? Cl2 O7 1.385(4) . ? Cl2 O5 1.421(3) . ? Cl2 O6 1.432(4) . ? C39 O9 1.724(16) . ? 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 N2 Zn N1 81.41(11) . . ? N2 Zn S1 117.43(8) . . ? N1 Zn S1 97.04(7) . . ? N2 Zn S2 132.67(8) . . ? N1 Zn S2 92.78(7) . . ? S1 Zn S2 109.89(3) . . ? N2 Zn N3 79.77(11) . . ? N1 Zn N3 157.67(10) . . ? S1 Zn N3 102.23(8) . . ? S2 Zn N3 91.20(7) . . ? C1 S1 Zn 106.83(10) . . ? C17 S2 Zn 102.53(10) . . ? C9 N1 C8 109.8(3) . . ? C9 N1 C7 112.8(3) . . ? C8 N1 C7 106.9(3) . . ? C9 N1 Zn 105.6(2) . . ? C8 N1 Zn 112.2(2) . . ? C7 N1 Zn 109.64(18) . . ? C10 N2 C11 109.6(3) . . ? C10 N2 C12 109.9(3) . . ? C11 N2 C12 111.6(3) . . ? C10 N2 Zn 108.3(2) . . ? C11 N2 Zn 111.7(2) . . ? C12 N2 Zn 105.6(2) . . ? C14 N3 C13 110.4(3) . . ? C14 N3 C15 110.1(3) . . ? C13 N3 C15 108.6(3) . . ? C14 N3 Zn 112.1(2) . . ? C13 N3 Zn 104.4(2) . . ? C15 N3 Zn 111.17(19) . . ? C23 N4 C24 115.1(2) . . ? C23 N4 C22 109.2(2) . . ? C24 N4 C22 110.8(2) . . ? C26 N5 C27 109.9(3) . . ? C26 N5 C25 111.1(3) . . ? C27 N5 C25 110.7(3) . . ? C28 N6 C29 111.9(2) . . ? C28 N6 C30 113.2(2) . . ? C29 N6 C30 109.1(2) . . ? C6 C1 C2 117.8(3) . . ? C6 C1 S1 123.9(2) . . ? C2 C1 S1 118.2(2) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 C30 117.5(3) . . ? C1 C2 C30 122.2(3) . . ? C2 C3 C4 122.5(3) . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C31 123.6(3) . . ? C3 C4 C31 119.7(3) . . ? C4 C5 C6 122.8(3) . . ? C5 C6 C1 119.8(3) . . ? C5 C6 C7 117.4(3) . . ? C1 C6 C7 122.6(3) . . ? N1 C7 C6 116.3(3) . . ? N1 C9 C10 109.0(3) . . ? N2 C10 C9 109.9(3) . . ? N2 C12 C13 110.1(3) . . ? N3 C13 C12 112.3(3) . . ? N3 C15 C16 112.3(2) . . ? C21 C16 C17 119.5(3) . . ? C21 C16 C15 120.4(3) . . ? C17 C16 C15 120.1(3) . . ? C16 C17 C18 118.1(3) . . ? C16 C17 S2 122.4(2) . . ? C18 C17 S2 119.5(2) . . ? C19 C18 C17 120.9(3) . . ? C19 C18 C22 119.1(3) . . ? C17 C18 C22 119.9(3) . . ? C20 C19 C18 121.5(3) . . ? C21 C20 C19 117.0(3) . . ? C21 C20 C35 123.5(3) . . ? C19 C20 C35 119.3(3) . . ? C20 C21 C16 123.0(3) . . ? C18 C22 N4 110.9(2) . . ? N4 C24 C25 113.1(3) . . ? N5 C25 C24 110.2(3) . . ? N5 C27 C28 112.6(2) . . ? N6 C28 C27 111.1(3) . . ? C2 C30 N6 114.8(2) . . ? C4 C31 C33 110.6(3) . . ? C4 C31 C32 112.2(3) . . ? C33 C31 C32 108.3(3) . . ? C4 C31 C34 107.9(3) . . ? C33 C31 C34 108.8(3) . . ? C32 C31 C34 108.9(3) . . ? C37 C35 C38 109.0(4) . . ? C37 C35 C36 107.6(3) . . ? C38 C35 C36 109.7(4) . . ? C37 C35 C20 110.5(3) . . ? C38 C35 C20 108.7(3) . . ? C36 C35 C20 111.4(3) . . ? O2 Cl1 O3 111.6(3) . . ? O2 Cl1 O1 110.0(3) . . ? O3 Cl1 O1 108.6(3) . . ? O2 Cl1 O4 110.8(3) . . ? O3 Cl1 O4 110.1(4) . . ? O1 Cl1 O4 105.5(3) . . ? O8 Cl2 O7 111.9(4) . . ? O8 Cl2 O5 112.6(2) . . ? O7 Cl2 O5 109.6(3) . . ? O8 Cl2 O6 109.8(4) . . ? O7 Cl2 O6 105.2(3) . . ? O5 Cl2 O6 107.4(2) . . ? #===END # Attachment 'CCDC_601295n.CIF' data_9 _database_code_depnum_ccdc_archive 'CCDC 601295' _chemical_formula_structural ; [NiH2(L3)](BPh4)2 ; _chemical_formula_sum 'C98 H130 B2 N6 Ni S2' _chemical_formula_weight 1536.53 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown from acetonitrile. ; #CRYSTAL DATA _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 14.095(3) _cell_length_b 15.097(3) _cell_length_c 23.640(5) _cell_angle_alpha 89.52(3) _cell_angle_beta 75.64(3) _cell_angle_gamma 65.07(3) _cell_volume 4392.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 76 _cell_measurement_theta_min 10 _cell_measurement_theta_max 22 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS, Sheldrick, 1996)' _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40508 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.1488 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.34 _reflns_number_total 20741 _reflns_number_gt 8857 _reflns_threshold_expression >2sigma(I) #REFINEMENT DATA _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^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20741 _refine_ls_number_parameters 1038 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1378 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.541 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.051 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.88668(3) 0.61131(2) 0.270391(16) 0.02852(10) Uani 1 1 d . . . S1 S 0.72871(6) 0.71863(5) 0.24972(3) 0.03117(17) Uani 1 1 d . . . S2 S 0.99235(6) 0.69283(5) 0.23099(3) 0.03223(18) Uani 1 1 d . . . N1 N 0.95748(17) 0.50803(15) 0.19352(10) 0.0303(5) Uani 1 1 d . . . N2 N 0.84466(17) 0.49786(16) 0.31052(10) 0.0324(6) Uani 1 1 d . . . N3 N 0.86287(17) 0.66099(15) 0.35886(9) 0.0282(5) Uani 1 1 d . . . N4 N 0.89783(18) 0.85261(16) 0.15230(9) 0.0351(6) Uani 1 1 d . . . H4 H 0.9119 0.7911 0.1627 0.042 Uiso 1 1 calc R . . N5 N 0.6024(2) 0.91940(19) 0.16495(11) 0.0510(7) Uani 1 1 d . . . N6 N 0.48018(18) 0.84774(16) 0.24789(10) 0.0376(6) Uani 1 1 d . . . H6 H 0.5438 0.8518 0.2450 0.045 Uiso 1 1 calc R . . C1 C 0.6983(2) 0.64839(18) 0.20459(11) 0.0284(6) Uani 1 1 d . . . C2 C 0.5900(2) 0.66674(19) 0.21094(12) 0.0311(7) Uani 1 1 d . . . C3 C 0.5645(2) 0.6109(2) 0.17650(13) 0.0394(8) Uani 1 1 d . . . H3 H 0.4919 0.6249 0.1816 0.047 Uiso 1 1 calc R . . C4 C 0.6429(2) 0.5350(2) 0.13479(13) 0.0413(8) Uani 1 1 d . A . C5 C 0.7492(2) 0.5180(2) 0.12923(12) 0.0382(7) Uani 1 1 d . . . H5 H 0.8038 0.4669 0.1019 0.046 Uiso 1 1 calc R . . C6 C 0.7794(2) 0.57234(19) 0.16189(12) 0.0301(6) Uani 1 1 d . . . C7 C 0.8975(2) 0.55134(19) 0.14795(12) 0.0331(7) Uani 1 1 d . . . H7A H 0.9030 0.6124 0.1398 0.040 Uiso 1 1 calc R . . H7B H 0.9354 0.5068 0.1120 0.040 Uiso 1 1 calc R . . C8 C 1.0734(2) 0.4850(2) 0.16477(12) 0.0372(7) Uani 1 1 d . . . H8A H 1.0764 0.5441 0.1499 0.045 Uiso 1 1 calc R . . H8B H 1.0992 0.4363 0.1313 0.045 Uiso 1 1 calc R . . C9 C 1.1506(2) 0.4472(2) 0.20278(13) 0.0430(8) Uani 1 1 d . . . H9A H 1.1578 0.3827 0.2129 0.052 Uiso 1 1 calc R . . H9B H 1.1217 0.4909 0.2389 0.052 Uiso 1 1 calc R . . C10 C 1.2616(2) 0.4407(3) 0.17078(16) 0.0735(12) Uani 1 1 d . . . H10A H 1.2906 0.3967 0.1353 0.110 Uiso 1 1 calc R . . H10B H 1.3097 0.4166 0.1956 0.110 Uiso 1 1 calc R . . H10C H 1.2545 0.5048 0.1612 0.110 Uiso 1 1 calc R . . C11 C 0.9488(2) 0.41552(19) 0.21110(12) 0.0350(7) Uani 1 1 d . . . H11A H 1.0126 0.3590 0.1887 0.042 Uiso 1 1 calc R . . H11B H 0.8854 0.4145 0.2025 0.042 Uiso 1 1 calc R . . C12 C 0.9394(2) 0.40985(19) 0.27623(12) 0.0372(7) Uani 1 1 d . . . H12A H 0.9309 0.3512 0.2877 0.045 Uiso 1 1 calc R . . H12B H 1.0051 0.4059 0.2844 0.045 Uiso 1 1 calc R . . C13 C 0.7405(2) 0.49911(19) 0.30616(12) 0.0346(7) Uani 1 1 d . . . H13A H 0.7390 0.5030 0.2654 0.041 Uiso 1 1 calc R . . H13B H 0.6815 0.5588 0.3285 0.041 Uiso 1 1 calc R . . C14 C 0.7177(2) 0.4133(2) 0.32691(14) 0.0499(9) Uani 1 1 d . . . H14A H 0.7124 0.4112 0.3686 0.060 Uiso 1 1 calc R . . H14B H 0.7769 0.3523 0.3062 0.060 Uiso 1 1 calc R . . C15 C 0.6121(2) 0.4235(2) 0.31579(15) 0.0589(10) Uani 1 1 d . . . H15A H 0.5527 0.4804 0.3394 0.088 Uiso 1 1 calc R . . H15B H 0.6014 0.3660 0.3259 0.088 Uiso 1 1 calc R . . H15C H 0.6155 0.4304 0.2750 0.088 Uiso 1 1 calc R . . C16 C 0.8451(2) 0.5049(2) 0.37344(12) 0.0380(7) Uani 1 1 d . . . H16A H 0.8802 0.4395 0.3847 0.046 Uiso 1 1 calc R . . H16B H 0.7710 0.5359 0.3981 0.046 Uiso 1 1 calc R . . C17 C 0.9050(2) 0.56443(19) 0.38269(12) 0.0368(7) Uani 1 1 d . . . H17A H 0.8968 0.5752 0.4244 0.044 Uiso 1 1 calc R . . H17B H 0.9818 0.5277 0.3634 0.044 Uiso 1 1 calc R . . C18 C 0.7476(2) 0.72541(19) 0.38900(11) 0.0334(7) Uani 1 1 d . . . H18A H 0.7035 0.6950 0.3805 0.040 Uiso 1 1 calc R . . H18B H 0.7271 0.7872 0.3719 0.040 Uiso 1 1 calc R . . C19 C 0.7185(2) 0.7482(2) 0.45579(12) 0.0458(8) Uani 1 1 d . . . H19A H 0.7166 0.6914 0.4746 0.055 Uiso 1 1 calc R . . H19B H 0.7738 0.7620 0.4661 0.055 Uiso 1 1 calc R . . C20 C 0.6086(3) 0.8360(2) 0.47790(14) 0.0590(10) Uani 1 1 d . . . H20A H 0.6104 0.8921 0.4591 0.088 Uiso 1 1 calc R . . H20B H 0.5925 0.8500 0.5196 0.088 Uiso 1 1 calc R . . H20C H 0.5536 0.8215 0.4689 0.088 Uiso 1 1 calc R . . C21 C 0.9325(2) 0.71131(18) 0.36429(12) 0.0301(7) Uani 1 1 d . . . H21A H 0.9261 0.7239 0.4056 0.036 Uiso 1 1 calc R . . H21B H 1.0078 0.6675 0.3454 0.036 Uiso 1 1 calc R . . C22 C 0.9032(2) 0.80620(19) 0.33756(12) 0.0282(6) Uani 1 1 d . . . C23 C 0.9299(2) 0.80456(18) 0.27622(12) 0.0285(6) Uani 1 1 d . . . C24 C 0.9097(2) 0.89404(19) 0.25238(12) 0.0288(6) Uani 1 1 d . . . C25 C 0.8617(2) 0.9815(2) 0.28904(12) 0.0340(7) Uani 1 1 d . . . H25 H 0.8481 1.0401 0.2723 0.041 Uiso 1 1 calc R . . C26 C 0.8336(2) 0.9842(2) 0.34954(13) 0.0363(7) Uani 1 1 d . B . C27 C 0.8561(2) 0.8946(2) 0.37229(12) 0.0341(7) Uani 1 1 d . . . H27 H 0.8385 0.8943 0.4129 0.041 Uiso 1 1 calc R . . C28 C 0.9485(2) 0.8953(2) 0.18674(12) 0.0352(7) Uani 1 1 d . . . H28A H 0.9312 0.9625 0.1783 0.042 Uiso 1 1 calc R . . H28B H 1.0269 0.8580 0.1741 0.042 Uiso 1 1 calc R . . C29 C 0.9451(3) 0.8422(2) 0.08653(12) 0.0490(9) Uani 1 1 d . . . H29A H 0.9212 0.8009 0.0683 0.059 Uiso 1 1 calc R . . H29B H 0.9147 0.9066 0.0731 0.059 Uiso 1 1 calc R . . C30 C 1.0672(3) 0.8000(3) 0.06474(14) 0.0648(10) Uani 1 1 d . . . H30A H 1.0870 0.8001 0.0224 0.078 Uiso 1 1 calc R . . H30B H 1.0911 0.8429 0.0814 0.078 Uiso 1 1 calc R . . C31 C 1.1274(3) 0.6977(3) 0.07906(16) 0.0838(13) Uani 1 1 d . . . H31A H 1.1227 0.6991 0.1203 0.126 Uiso 1 1 calc R . . H31B H 1.2023 0.6718 0.0569 0.126 Uiso 1 1 calc R . . H31C H 1.0958 0.6568 0.0691 0.126 Uiso 1 1 calc R . . C32 C 0.7768(2) 0.9112(2) 0.16986(13) 0.0415(8) Uani 1 1 d . . . H32A H 0.7597 0.9791 0.1633 0.050 Uiso 1 1 calc R . . H32B H 0.7494 0.9094 0.2116 0.050 Uiso 1 1 calc R . . C33 C 0.7188(2) 0.8742(2) 0.13642(13) 0.0478(8) Uani 1 1 d . . . H33A H 0.7318 0.8903 0.0963 0.057 Uiso 1 1 calc R . . H33B H 0.7472 0.8033 0.1354 0.057 Uiso 1 1 calc R . . C34 C 0.5521(3) 1.0246(3) 0.1580(2) 0.0842(13) Uani 1 1 d . . . H34A H 0.4833 1.0405 0.1494 0.101 Uiso 1 1 calc R . . H34B H 0.5985 1.0372 0.1243 0.101 Uiso 1 1 calc R . . C35 C 0.5327(3) 1.0909(3) 0.2094(2) 0.1172(19) Uani 1 1 d . . . H35A H 0.5998 1.0731 0.2204 0.141 Uiso 1 1 calc R . . H35B H 0.4799 1.0846 0.2425 0.141 Uiso 1 1 calc R . . C36 C 0.4889(4) 1.2002(3) 0.1938(3) 0.230(4) Uani 1 1 d . . . H36A H 0.4775 1.2021 0.1554 0.345 Uiso 1 1 calc R . . H36B H 0.5410 1.2251 0.1945 0.345 Uiso 1 1 calc R . . H36C H 0.4214 1.2399 0.2221 0.345 Uiso 1 1 calc R . . C37 C 0.5470(3) 0.8662(2) 0.14477(14) 0.0557(9) Uani 1 1 d . . . H37A H 0.5249 0.8928 0.1102 0.067 Uiso 1 1 calc R . . H37B H 0.5969 0.7973 0.1341 0.067 Uiso 1 1 calc R . . C38 C 0.4505(3) 0.8761(2) 0.19172(14) 0.0526(9) Uani 1 1 d . . . H38A H 0.4205 0.8342 0.1800 0.063 Uiso 1 1 calc R . . H38B H 0.3954 0.9435 0.1977 0.063 Uiso 1 1 calc R . . C39 C 0.3968(3) 0.9184(2) 0.30043(16) 0.0674(11) Uani 1 1 d . . . H39A H 0.3672 0.9840 0.2885 0.081 Uiso 1 1 calc R . . H39B H 0.3376 0.8997 0.3135 0.081 Uiso 1 1 calc R . . C40 C 0.4432(4) 0.9202(3) 0.35055(16) 0.123(2) Uani 1 1 d . . . H40A H 0.4695 0.8557 0.3642 0.148 Uiso 1 1 calc R . . H40B H 0.5042 0.9366 0.3375 0.148 Uiso 1 1 calc R . . C41 C 0.3598(5) 0.9932(4) 0.3989(2) 0.194(3) Uani 1 1 d . . . H41A H 0.3833 0.9818 0.4342 0.291 Uiso 1 1 calc R . . H41B H 0.2929 0.9873 0.4049 0.291 Uiso 1 1 calc R . . H41C H 0.3488 1.0580 0.3892 0.291 Uiso 1 1 calc R . . C42 C 0.4998(2) 0.74380(19) 0.25804(12) 0.0356(7) Uani 1 1 d . . . H42A H 0.4332 0.7374 0.2609 0.043 Uiso 1 1 calc R . . H42B H 0.5170 0.7309 0.2954 0.043 Uiso 1 1 calc R . . C43 C 0.6116(3) 0.4753(3) 0.09741(18) 0.0697(12) Uani 1 1 d D . . C44A C 0.7080(8) 0.3896(6) 0.0636(5) 0.075(3) Uani 0.608(6) 1 d PD A 1 H44A H 0.7510 0.3547 0.0893 0.113 Uiso 0.608(6) 1 calc PR A 1 H44B H 0.7503 0.4111 0.0333 0.113 Uiso 0.608(6) 1 calc PR A 1 H44C H 0.6857 0.3471 0.0461 0.113 Uiso 0.608(6) 1 calc PR A 1 C45A C 0.5503(5) 0.4208(4) 0.1470(3) 0.065(2) Uani 0.608(6) 1 d PD A 1 H45A H 0.5345 0.3760 0.1267 0.098 Uiso 0.608(6) 1 calc PR A 1 H45B H 0.4840 0.4700 0.1719 0.098 Uiso 0.608(6) 1 calc PR A 1 H45C H 0.5978 0.3853 0.1705 0.098 Uiso 0.608(6) 1 calc PR A 1 C46A C 0.5309(8) 0.5358(6) 0.0711(4) 0.101(4) Uani 0.608(6) 1 d PD A 1 H46A H 0.5575 0.5752 0.0459 0.152 Uiso 0.608(6) 1 calc PR A 1 H46B H 0.4673 0.5778 0.1011 0.152 Uiso 0.608(6) 1 calc PR A 1 H46C H 0.5130 0.4956 0.0484 0.152 Uiso 0.608(6) 1 calc PR A 1 C44B C 0.6851(10) 0.3703(8) 0.0822(7) 0.069(5) Uani 0.392(6) 1 d PD A 2 H44D H 0.6648 0.3433 0.0531 0.103 Uiso 0.392(6) 1 calc PR A 2 H44E H 0.6803 0.3367 0.1167 0.103 Uiso 0.392(6) 1 calc PR A 2 H44F H 0.7584 0.3622 0.0668 0.103 Uiso 0.392(6) 1 calc PR A 2 C45B C 0.6407(8) 0.5159(6) 0.0265(3) 0.054(3) Uani 0.392(6) 1 d PD A 2 H45D H 0.7160 0.5026 0.0141 0.081 Uiso 0.392(6) 1 calc PR A 2 H45E H 0.5967 0.5853 0.0287 0.081 Uiso 0.392(6) 1 calc PR A 2 H45F H 0.6248 0.4817 -0.0012 0.081 Uiso 0.392(6) 1 calc PR A 2 C46B C 0.4937(8) 0.5059(8) 0.1049(6) 0.080(5) Uani 0.392(6) 1 d PD A 2 H46D H 0.4846 0.4673 0.0764 0.121 Uiso 0.392(6) 1 calc PR A 2 H46E H 0.4593 0.5742 0.0994 0.121 Uiso 0.392(6) 1 calc PR A 2 H46F H 0.4611 0.4960 0.1437 0.121 Uiso 0.392(6) 1 calc PR A 2 C47 C 0.7777(3) 1.0817(2) 0.38923(14) 0.0505(9) Uani 1 1 d D . . C48A C 0.8450(8) 1.1406(7) 0.3745(4) 0.073(3) Uani 0.523(10) 1 d PD B 1 H48A H 0.8042 1.2052 0.3956 0.109 Uiso 0.523(10) 1 calc PR B 1 H48B H 0.8614 1.1458 0.3331 0.109 Uiso 0.523(10) 1 calc PR B 1 H48C H 0.9113 1.1077 0.3857 0.109 Uiso 0.523(10) 1 calc PR B 1 C49A C 0.7528(9) 1.0743(5) 0.4547(3) 0.083(4) Uani 0.523(10) 1 d PD B 1 H49A H 0.8193 1.0375 0.4652 0.125 Uiso 0.523(10) 1 calc PR B 1 H49B H 0.7063 1.0417 0.4649 0.125 Uiso 0.523(10) 1 calc PR B 1 H49C H 0.7170 1.1391 0.4755 0.125 Uiso 0.523(10) 1 calc PR B 1 C50A C 0.6685(6) 1.1475(6) 0.3734(4) 0.090(5) Uani 0.523(10) 1 d PD B 1 H50A H 0.6143 1.1254 0.3909 0.135 Uiso 0.523(10) 1 calc PR B 1 H50B H 0.6807 1.1424 0.3316 0.135 Uiso 0.523(10) 1 calc PR B 1 H50C H 0.6440 1.2147 0.3882 0.135 Uiso 0.523(10) 1 calc PR B 1 C48B C 0.8485(10) 1.0688(7) 0.4333(5) 0.105(5) Uani 0.477(10) 1 d PD B 2 H48D H 0.8156 1.1265 0.4610 0.158 Uiso 0.477(10) 1 calc PR B 2 H48E H 0.9202 1.0593 0.4119 0.158 Uiso 0.477(10) 1 calc PR B 2 H48F H 0.8531 1.0126 0.4538 0.158 Uiso 0.477(10) 1 calc PR B 2 C49B C 0.6685(6) 1.0929(6) 0.4232(5) 0.079(4) Uani 0.477(10) 1 d PD B 2 H49D H 0.6758 1.0352 0.4427 0.118 Uiso 0.477(10) 1 calc PR B 2 H49E H 0.6239 1.1013 0.3970 0.118 Uiso 0.477(10) 1 calc PR B 2 H49F H 0.6354 1.1494 0.4519 0.118 Uiso 0.477(10) 1 calc PR B 2 C50B C 0.7758(11) 1.1664(7) 0.3565(5) 0.099(6) Uani 0.477(10) 1 d PD B 2 H50D H 0.7471 1.2242 0.3838 0.148 Uiso 0.477(10) 1 calc PR B 2 H50E H 0.7309 1.1770 0.3303 0.148 Uiso 0.477(10) 1 calc PR B 2 H50F H 0.8484 1.1530 0.3344 0.148 Uiso 0.477(10) 1 calc PR B 2 B1 B 1.2330(3) 0.6206(2) 0.41105(14) 0.0334(8) Uani 1 1 d . . . C101 C 1.2723(2) 0.5037(2) 0.39192(12) 0.0340(7) Uani 1 1 d . . . C102 C 1.3548(2) 0.4270(2) 0.40863(13) 0.0418(8) Uani 1 1 d . . . H102 H 1.3933 0.4424 0.4306 0.050 Uiso 1 1 calc R . . C103 C 1.3825(3) 0.3293(2) 0.39430(14) 0.0527(9) Uani 1 1 d . . . H103 H 1.4387 0.2810 0.4064 0.063 Uiso 1 1 calc R . . C104 C 1.3277(3) 0.3027(2) 0.36232(14) 0.0513(9) Uani 1 1 d . . . H104 H 1.3456 0.2369 0.3530 0.062 Uiso 1 1 calc R . . C105 C 1.2460(3) 0.3754(2) 0.34438(14) 0.0488(9) Uani 1 1 d . . . H105 H 1.2080 0.3591 0.3225 0.059 Uiso 1 1 calc R . . C106 C 1.2203(2) 0.4724(2) 0.35866(13) 0.0418(8) Uani 1 1 d . . . H106 H 1.1650 0.5201 0.3455 0.050 Uiso 1 1 calc R . . C201 C 1.3245(2) 0.63646(19) 0.43551(12) 0.0319(7) Uani 1 1 d . . . C202 C 1.3979(2) 0.6677(2) 0.40246(13) 0.0394(8) Uani 1 1 d . . . H202 H 1.3933 0.6835 0.3648 0.047 Uiso 1 1 calc R . . C203 C 1.4779(2) 0.6765(2) 0.42269(13) 0.0434(8) Uani 1 1 d . . . H203 H 1.5249 0.6986 0.3989 0.052 Uiso 1 1 calc R . . C204 C 1.4882(2) 0.6528(2) 0.47763(13) 0.0413(8) Uani 1 1 d . . . H204 H 1.5428 0.6573 0.4912 0.050 Uiso 1 1 calc R . . C205 C 1.4169(2) 0.6225(2) 0.51206(13) 0.0442(8) Uani 1 1 d . . . H205 H 1.4222 0.6067 0.5496 0.053 Uiso 1 1 calc R . . C206 C 1.3369(2) 0.6151(2) 0.49155(13) 0.0434(8) Uani 1 1 d . . . H206 H 1.2889 0.5950 0.5162 0.052 Uiso 1 1 calc R . . C301 C 1.2178(2) 0.6810(2) 0.35269(13) 0.0376(7) Uani 1 1 d . . . C302 C 1.2723(2) 0.6364(2) 0.29564(14) 0.0479(8) Uani 1 1 d . . . H302 H 1.3172 0.5693 0.2901 0.057 Uiso 1 1 calc R . . C303 C 1.2630(3) 0.6870(3) 0.24627(15) 0.0642(11) Uani 1 1 d . . . H303 H 1.3001 0.6532 0.2090 0.077 Uiso 1 1 calc R . . C304 C 1.2000(3) 0.7855(4) 0.2524(2) 0.0768(14) Uani 1 1 d . . . H304 H 1.1941 0.8197 0.2195 0.092 Uiso 1 1 calc R . . C305 C 1.1460(3) 0.8332(3) 0.3071(2) 0.0740(12) Uani 1 1 d . . . H305 H 1.1033 0.9007 0.3118 0.089 Uiso 1 1 calc R . . C306 C 1.1538(3) 0.7821(2) 0.35628(16) 0.0579(10) Uani 1 1 d . . . H306 H 1.1148 0.8168 0.3932 0.069 Uiso 1 1 calc R . . C401 C 1.1189(2) 0.6625(2) 0.46377(12) 0.0372(7) Uani 1 1 d . . . C402 C 1.0569(2) 0.6108(2) 0.48135(12) 0.0388(7) Uani 1 1 d . . . H402 H 1.0825 0.5477 0.4630 0.047 Uiso 1 1 calc R . . C403 C 0.9590(3) 0.6480(3) 0.52462(13) 0.0490(9) Uani 1 1 d . . . H403 H 0.9214 0.6098 0.5352 0.059 Uiso 1 1 calc R . . C404 C 0.9185(3) 0.7403(3) 0.55141(15) 0.0718(12) Uani 1 1 d . . . H404 H 0.8515 0.7669 0.5793 0.086 Uiso 1 1 calc R . . C405 C 0.9771(3) 0.7948(3) 0.53719(17) 0.0908(15) Uani 1 1 d . . . H405 H 0.9505 0.8577 0.5560 0.109 Uiso 1 1 calc R . . C406 C 1.0759(3) 0.7550(3) 0.49460(16) 0.0677(11) Uani 1 1 d . . . H406 H 1.1153 0.7919 0.4863 0.081 Uiso 1 1 calc R . . B2 B 0.1371(3) 0.1067(2) 0.11298(15) 0.0399(9) Uani 1 1 d . . . C502 C 0.2133(2) 0.1738(2) 0.18810(13) 0.0431(8) Uani 1 1 d . . . H502 H 0.2441 0.1997 0.1570 0.052 Uiso 1 1 calc R . . C503 C 0.2275(3) 0.1869(2) 0.24273(16) 0.0541(9) Uani 1 1 d . . . H503 H 0.2670 0.2212 0.2475 0.065 Uiso 1 1 calc R . . C506 C 0.1141(3) 0.0853(2) 0.22665(13) 0.0504(9) Uani 1 1 d . . . H506 H 0.0763 0.0492 0.2222 0.060 Uiso 1 1 calc R . . C501 C 0.1552(2) 0.1237(2) 0.17739(13) 0.0394(7) Uani 1 1 d . . . C504 C 0.1840(3) 0.1498(3) 0.28958(16) 0.0625(11) Uani 1 1 d . . . H504 H 0.1929 0.1590 0.3264 0.075 Uiso 1 1 calc R . . C505 C 0.1271(3) 0.0988(3) 0.28142(14) 0.0603(10) Uani 1 1 d . . . H505 H 0.0969 0.0731 0.3130 0.072 Uiso 1 1 calc R . . C601 C 0.0126(3) 0.1208(2) 0.12127(13) 0.0396(8) Uani 1 1 d . . . C602 C -0.0754(3) 0.1769(2) 0.16885(14) 0.0488(9) Uani 1 1 d . . . H602 H -0.0622 0.2052 0.1990 0.059 Uiso 1 1 calc R . . C603 C -0.1808(3) 0.1923(2) 0.17329(16) 0.0583(10) Uani 1 1 d . . . H603 H -0.2360 0.2290 0.2063 0.070 Uiso 1 1 calc R . . C604 C -0.2045(3) 0.1536(2) 0.12889(17) 0.0583(10) Uani 1 1 d . . . H604 H -0.2753 0.1635 0.1316 0.070 Uiso 1 1 calc R . . C605 C -0.1209(3) 0.0999(2) 0.08051(15) 0.0526(9) Uani 1 1 d . . . H605 H -0.1355 0.0750 0.0495 0.063 Uiso 1 1 calc R . . C606 C -0.0154(3) 0.0828(2) 0.07765(13) 0.0440(8) Uani 1 1 d . . . H606 H 0.0397 0.0440 0.0451 0.053 Uiso 1 1 calc R . . C701 C 0.1552(3) 0.1884(2) 0.07011(13) 0.0448(8) Uani 1 1 d . . . C702 C 0.0715(3) 0.2660(2) 0.05439(13) 0.0509(9) Uani 1 1 d . . . H702 H 0.0009 0.2728 0.0691 0.061 Uiso 1 1 calc R . . C703 C 0.0886(4) 0.3339(3) 0.01766(15) 0.0709(12) Uani 1 1 d . . . H703 H 0.0304 0.3835 0.0078 0.085 Uiso 1 1 calc R . . C704 C 0.1901(5) 0.3274(3) -0.00351(17) 0.0858(15) Uani 1 1 d . . . H704 H 0.2015 0.3729 -0.0276 0.103 Uiso 1 1 calc R . . C705 C 0.2761(4) 0.2534(3) 0.01078(17) 0.0847(14) Uani 1 1 d . . . H705 H 0.3459 0.2489 -0.0033 0.102 Uiso 1 1 calc R . . C706 C 0.2584(3) 0.1852(3) 0.04640(15) 0.0662(11) Uani 1 1 d . . . H706 H 0.3179 0.1349 0.0550 0.079 Uiso 1 1 calc R . . C801 C 0.2229(2) -0.0048(2) 0.08208(13) 0.0409(8) Uani 1 1 d . . . C802 C 0.2495(3) -0.0846(2) 0.11368(14) 0.0534(9) Uani 1 1 d . . . H802 H 0.2190 -0.0738 0.1541 0.064 Uiso 1 1 calc R . . C803 C 0.3189(3) -0.1804(2) 0.08897(17) 0.0650(11) Uani 1 1 d . . . H803 H 0.3328 -0.2311 0.1128 0.078 Uiso 1 1 calc R . . C804 C 0.3663(3) -0.2004(3) 0.03079(17) 0.0666(11) Uani 1 1 d . . . H804 H 0.4150 -0.2639 0.0140 0.080 Uiso 1 1 calc R . . C805 C 0.3408(4) -0.1248(3) -0.00244(17) 0.0975(16) Uani 1 1 d . . . H805 H 0.3711 -0.1368 -0.0429 0.117 Uiso 1 1 calc R . . C806 C 0.2700(3) -0.0296(3) 0.02279(16) 0.0875(14) Uani 1 1 d . . . H806 H 0.2536 0.0200 -0.0018 0.105 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 Ni 0.0283(2) 0.0243(2) 0.0336(2) 0.00525(16) -0.00991(17) -0.01119(17) S1 0.0309(4) 0.0250(4) 0.0371(4) 0.0008(3) -0.0140(3) -0.0088(3) S2 0.0323(4) 0.0259(4) 0.0362(4) 0.0010(3) -0.0044(3) -0.0131(3) N1 0.0270(13) 0.0247(13) 0.0383(14) 0.0054(11) -0.0096(11) -0.0100(11) N2 0.0323(14) 0.0303(13) 0.0376(15) 0.0061(11) -0.0109(12) -0.0157(12) N3 0.0284(13) 0.0261(13) 0.0358(14) 0.0086(11) -0.0133(11) -0.0147(11) N4 0.0450(16) 0.0311(14) 0.0312(14) 0.0049(11) -0.0091(12) -0.0190(13) N5 0.0519(18) 0.0464(18) 0.0611(19) 0.0187(15) -0.0243(15) -0.0226(15) N6 0.0301(14) 0.0341(14) 0.0461(16) 0.0028(12) -0.0096(12) -0.0119(12) C1 0.0309(16) 0.0241(15) 0.0298(16) 0.0074(12) -0.0101(13) -0.0106(13) C2 0.0316(17) 0.0270(16) 0.0361(17) 0.0065(13) -0.0109(14) -0.0130(14) C3 0.0327(17) 0.0379(18) 0.051(2) 0.0009(16) -0.0159(16) -0.0158(15) C4 0.0418(19) 0.0389(19) 0.047(2) -0.0048(16) -0.0152(16) -0.0190(16) C5 0.0419(19) 0.0311(17) 0.0377(18) -0.0045(14) -0.0097(15) -0.0126(15) C6 0.0342(17) 0.0269(16) 0.0300(16) 0.0036(13) -0.0098(14) -0.0133(14) C7 0.0350(17) 0.0289(16) 0.0329(17) -0.0009(13) -0.0058(14) -0.0134(14) C8 0.0276(17) 0.0288(16) 0.050(2) -0.0033(14) -0.0030(15) -0.0108(14) C9 0.0302(18) 0.0304(17) 0.065(2) 0.0040(16) -0.0127(16) -0.0096(14) C10 0.039(2) 0.071(3) 0.109(3) 0.018(2) -0.021(2) -0.022(2) C11 0.0309(16) 0.0232(15) 0.0462(19) 0.0001(14) -0.0086(14) -0.0083(13) C12 0.0356(18) 0.0250(16) 0.053(2) 0.0105(15) -0.0160(16) -0.0129(14) C13 0.0348(17) 0.0348(17) 0.0401(18) 0.0079(14) -0.0105(14) -0.0205(14) C14 0.057(2) 0.053(2) 0.057(2) 0.0217(18) -0.0189(18) -0.0388(19) C15 0.057(2) 0.060(2) 0.074(3) 0.009(2) -0.017(2) -0.039(2) C16 0.0485(19) 0.0352(17) 0.0394(18) 0.0157(14) -0.0187(15) -0.0232(16) C17 0.0430(18) 0.0335(17) 0.0392(18) 0.0142(14) -0.0175(15) -0.0181(15) C18 0.0298(17) 0.0336(17) 0.0378(18) 0.0040(14) -0.0088(14) -0.0148(14) C19 0.045(2) 0.062(2) 0.0347(19) 0.0032(16) -0.0099(16) -0.0265(18) C20 0.062(2) 0.060(2) 0.048(2) -0.0099(18) 0.0012(19) -0.028(2) C21 0.0305(16) 0.0321(16) 0.0356(17) 0.0080(13) -0.0137(13) -0.0183(14) C22 0.0277(16) 0.0298(16) 0.0331(17) 0.0054(13) -0.0124(13) -0.0158(13) C23 0.0250(15) 0.0255(15) 0.0376(17) 0.0038(13) -0.0093(13) -0.0129(13) C24 0.0311(16) 0.0270(16) 0.0313(16) 0.0038(13) -0.0099(13) -0.0146(13) C25 0.0369(17) 0.0247(16) 0.0400(18) 0.0060(14) -0.0096(15) -0.0136(14) C26 0.0373(18) 0.0323(17) 0.0376(18) 0.0002(14) -0.0067(15) -0.0154(15) C27 0.0399(18) 0.0392(18) 0.0273(16) 0.0017(14) -0.0070(14) -0.0221(15) C28 0.0443(18) 0.0292(16) 0.0377(18) 0.0033(14) -0.0120(15) -0.0206(15) C29 0.071(3) 0.055(2) 0.0290(18) 0.0069(16) -0.0119(17) -0.035(2) C30 0.075(3) 0.071(3) 0.038(2) 0.0020(19) 0.0050(19) -0.033(2) C31 0.085(3) 0.060(3) 0.065(3) 0.001(2) 0.022(2) -0.015(2) C32 0.044(2) 0.0353(18) 0.047(2) 0.0090(15) -0.0140(16) -0.0172(16) C33 0.053(2) 0.056(2) 0.046(2) 0.0163(17) -0.0204(18) -0.0302(19) C34 0.058(3) 0.050(3) 0.137(4) 0.003(3) -0.021(3) -0.018(2) C35 0.062(3) 0.061(3) 0.196(6) 0.010(4) -0.007(3) -0.012(3) C36 0.112(5) 0.053(3) 0.401(11) 0.044(5) 0.093(6) -0.010(3) C37 0.060(2) 0.068(2) 0.051(2) 0.0205(19) -0.032(2) -0.031(2) C38 0.052(2) 0.047(2) 0.066(2) 0.0206(18) -0.032(2) -0.0188(18) C39 0.056(2) 0.042(2) 0.078(3) -0.014(2) 0.007(2) -0.0105(19) C40 0.155(5) 0.085(3) 0.037(3) -0.023(2) -0.010(3) 0.027(3) C41 0.266(8) 0.136(5) 0.107(5) -0.016(4) -0.057(5) -0.014(5) C42 0.0348(17) 0.0360(18) 0.0372(18) 0.0046(14) -0.0094(14) -0.0165(15) C43 0.059(3) 0.065(3) 0.091(3) -0.030(2) -0.030(2) -0.027(2) C44A 0.113(7) 0.066(6) 0.071(6) -0.023(5) -0.012(5) -0.067(6) C45A 0.058(4) 0.062(4) 0.085(5) -0.015(4) -0.013(4) -0.038(4) C46A 0.148(11) 0.076(6) 0.117(10) 0.004(6) -0.108(9) -0.043(6) C44B 0.085(10) 0.026(6) 0.131(15) 0.019(7) -0.072(10) -0.033(7) C45B 0.068(7) 0.046(5) 0.055(6) -0.007(5) -0.038(6) -0.019(5) C46B 0.063(8) 0.078(10) 0.110(12) -0.029(8) -0.015(8) -0.045(7) C47 0.057(2) 0.0365(19) 0.049(2) -0.0099(17) 0.0021(19) -0.0203(18) C48A 0.098(8) 0.051(6) 0.078(7) -0.016(5) -0.005(5) -0.049(6) C49A 0.134(11) 0.044(5) 0.040(5) -0.018(4) 0.009(5) -0.025(6) C50A 0.060(6) 0.060(6) 0.108(9) -0.037(6) -0.026(6) 0.017(5) C48B 0.151(11) 0.082(7) 0.092(9) -0.037(6) -0.024(8) -0.063(8) C49B 0.063(6) 0.045(5) 0.092(9) -0.022(6) 0.023(6) -0.012(5) C50B 0.155(16) 0.035(6) 0.071(8) -0.016(5) 0.025(8) -0.039(8) B1 0.0320(19) 0.035(2) 0.034(2) -0.0007(16) -0.0092(16) -0.0153(16) C101 0.0296(16) 0.0429(18) 0.0330(17) 0.0073(14) -0.0081(14) -0.0193(15) C102 0.045(2) 0.043(2) 0.0427(19) 0.0065(16) -0.0186(16) -0.0214(17) C103 0.054(2) 0.039(2) 0.061(2) 0.0100(18) -0.0244(19) -0.0120(18) C104 0.061(2) 0.0355(19) 0.057(2) 0.0027(17) -0.0143(19) -0.0219(19) C105 0.049(2) 0.043(2) 0.058(2) -0.0072(17) -0.0164(18) -0.0216(18) C106 0.0392(19) 0.0396(19) 0.048(2) 0.0015(16) -0.0180(16) -0.0154(16) C201 0.0312(17) 0.0313(16) 0.0326(17) 0.0004(13) -0.0053(14) -0.0148(14) C202 0.0416(19) 0.054(2) 0.0346(18) 0.0126(15) -0.0145(15) -0.0293(17) C203 0.0397(19) 0.052(2) 0.047(2) 0.0120(17) -0.0120(16) -0.0279(17) C204 0.0391(19) 0.0456(19) 0.046(2) 0.0031(16) -0.0179(16) -0.0209(16) C205 0.054(2) 0.058(2) 0.0335(18) 0.0089(16) -0.0180(16) -0.0331(18) C206 0.049(2) 0.059(2) 0.0339(18) 0.0083(16) -0.0081(16) -0.0361(18) C301 0.0310(17) 0.0435(19) 0.046(2) 0.0096(16) -0.0155(15) -0.0209(16) C302 0.045(2) 0.059(2) 0.046(2) 0.0153(18) -0.0173(17) -0.0250(18) C303 0.057(3) 0.105(3) 0.048(2) 0.028(2) -0.022(2) -0.047(3) C304 0.058(3) 0.116(4) 0.090(3) 0.067(3) -0.043(3) -0.057(3) C305 0.058(3) 0.060(3) 0.113(4) 0.049(3) -0.036(3) -0.028(2) C306 0.053(2) 0.053(2) 0.074(3) 0.018(2) -0.022(2) -0.025(2) C401 0.0368(18) 0.0449(19) 0.0352(18) 0.0004(15) -0.0115(15) -0.0217(16) C402 0.0439(19) 0.0453(19) 0.0329(18) 0.0066(15) -0.0127(15) -0.0234(16) C403 0.051(2) 0.070(2) 0.0334(19) 0.0025(18) -0.0054(17) -0.037(2) C404 0.053(2) 0.106(3) 0.053(2) -0.029(2) 0.0179(19) -0.048(2) C405 0.074(3) 0.092(3) 0.091(3) -0.056(3) 0.027(2) -0.048(3) C406 0.057(2) 0.070(3) 0.076(3) -0.024(2) 0.008(2) -0.041(2) B2 0.053(2) 0.035(2) 0.034(2) 0.0075(17) -0.0180(18) -0.0180(19) C502 0.047(2) 0.0334(18) 0.043(2) -0.0005(15) -0.0129(16) -0.0106(16) C503 0.054(2) 0.041(2) 0.062(2) -0.0073(18) -0.029(2) -0.0075(18) C506 0.063(2) 0.053(2) 0.037(2) 0.0064(17) -0.0185(18) -0.0242(19) C501 0.0432(19) 0.0325(17) 0.0380(19) 0.0025(14) -0.0114(15) -0.0120(15) C504 0.065(3) 0.057(2) 0.048(2) -0.0104(19) -0.028(2) -0.003(2) C505 0.070(3) 0.064(3) 0.037(2) 0.0067(18) -0.0157(19) -0.019(2) C601 0.055(2) 0.0290(17) 0.0378(19) 0.0104(14) -0.0173(17) -0.0183(16) C602 0.059(2) 0.040(2) 0.048(2) 0.0057(17) -0.0180(19) -0.0194(18) C603 0.055(2) 0.043(2) 0.065(3) 0.0045(19) -0.010(2) -0.0141(19) C604 0.055(2) 0.049(2) 0.083(3) 0.019(2) -0.027(2) -0.029(2) C605 0.068(3) 0.044(2) 0.060(2) 0.0130(18) -0.033(2) -0.030(2) C606 0.057(2) 0.0397(19) 0.0388(19) 0.0096(15) -0.0166(17) -0.0218(17) C701 0.064(2) 0.046(2) 0.0297(18) 0.0043(15) -0.0136(17) -0.0277(19) C702 0.083(3) 0.041(2) 0.0361(19) 0.0069(16) -0.0213(19) -0.030(2) C703 0.134(4) 0.047(2) 0.040(2) 0.0107(18) -0.028(3) -0.045(3) C704 0.155(5) 0.079(3) 0.048(3) 0.022(2) -0.019(3) -0.079(4) C705 0.108(4) 0.103(4) 0.056(3) 0.012(3) 0.002(3) -0.071(3) C706 0.075(3) 0.078(3) 0.051(2) 0.020(2) -0.012(2) -0.041(2) C801 0.048(2) 0.0430(19) 0.0357(18) 0.0075(15) -0.0174(16) -0.0206(17) C802 0.072(3) 0.041(2) 0.042(2) 0.0070(17) -0.0140(18) -0.0197(19) C803 0.090(3) 0.036(2) 0.065(3) 0.0110(19) -0.035(2) -0.016(2) C804 0.082(3) 0.043(2) 0.060(3) -0.006(2) -0.028(2) -0.008(2) C805 0.134(4) 0.068(3) 0.044(3) -0.002(2) -0.007(3) -0.009(3) C806 0.129(4) 0.048(2) 0.042(2) 0.006(2) -0.010(2) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N3 2.125(2) . ? Ni N1 2.137(2) . ? Ni N2 2.176(2) . ? Ni S1 2.3036(12) . ? Ni S2 2.3321(10) . ? S1 C1 1.754(3) . ? S2 C23 1.754(3) . ? N1 C8 1.492(3) . ? N1 C11 1.499(3) . ? N1 C7 1.508(3) . ? N2 C12 1.480(3) . ? N2 C13 1.489(3) . ? N2 C16 1.494(3) . ? N3 C18 1.483(3) . ? N3 C17 1.489(3) . ? N3 C21 1.500(3) . ? N4 C32 1.499(3) . ? N4 C28 1.508(3) . ? N4 C29 1.513(3) . ? N5 C33 1.459(4) . ? N5 C34 1.469(4) . ? N5 C37 1.484(4) . ? N6 C38 1.495(3) . ? N6 C42 1.502(3) . ? N6 C39 1.518(4) . ? C1 C2 1.399(3) . ? C1 C6 1.409(4) . ? C2 C3 1.384(3) . ? C2 C42 1.511(4) . ? C3 C4 1.384(4) . ? C4 C5 1.381(4) . ? C4 C43 1.527(4) . ? C5 C6 1.385(3) . ? C6 C7 1.506(4) . ? C8 C9 1.507(4) . ? C9 C10 1.521(4) . ? C11 C12 1.517(4) . ? C13 C14 1.512(3) . ? C14 C15 1.519(4) . ? C16 C17 1.517(3) . ? C18 C19 1.532(4) . ? C19 C20 1.519(4) . ? C21 C22 1.496(3) . ? C22 C27 1.377(3) . ? C22 C23 1.403(4) . ? C23 C24 1.402(3) . ? C24 C25 1.388(3) . ? C24 C28 1.515(3) . ? C25 C26 1.382(4) . ? C26 C27 1.389(4) . ? C26 C47 1.531(4) . ? C29 C30 1.509(4) . ? C30 C31 1.499(4) . ? C32 C33 1.522(4) . ? C34 C35 1.476(5) . ? C35 C36 1.575(6) . ? C37 C38 1.479(4) . ? C39 C40 1.494(5) . ? C40 C41 1.472(6) . ? C43 C46A 1.408(7) . ? C43 C44A 1.467(9) . ? C43 C44B 1.468(11) . ? C43 C46B 1.488(9) . ? C43 C45A 1.697(6) . ? C43 C45B 1.791(8) . ? C47 C50B 1.483(9) . ? C47 C49B 1.488(7) . ? C47 C49A 1.514(7) . ? C47 C48A 1.534(8) . ? C47 C48B 1.570(8) . ? C47 C50A 1.577(7) . ? B1 C101 1.640(4) . ? B1 C201 1.640(4) . ? B1 C401 1.643(4) . ? B1 C301 1.656(4) . ? C101 C102 1.390(4) . ? C101 C106 1.402(4) . ? C102 C103 1.379(4) . ? C103 C104 1.373(4) . ? C104 C105 1.370(4) . ? C105 C106 1.375(4) . ? C201 C202 1.380(3) . ? C201 C206 1.396(4) . ? C202 C203 1.384(4) . ? C203 C204 1.370(4) . ? C204 C205 1.363(4) . ? C205 C206 1.376(4) . ? C301 C302 1.388(4) . ? C301 C306 1.398(4) . ? C302 C303 1.393(4) . ? C303 C304 1.360(5) . ? C304 C305 1.355(5) . ? C305 C306 1.391(5) . ? C401 C406 1.390(4) . ? C401 C402 1.391(4) . ? C402 C403 1.386(4) . ? C403 C404 1.355(4) . ? C404 C405 1.378(5) . ? C405 C406 1.387(4) . ? B2 C601 1.637(5) . ? B2 C801 1.642(4) . ? B2 C501 1.644(4) . ? B2 C701 1.652(4) . ? C502 C503 1.383(4) . ? C502 C501 1.391(4) . ? C503 C504 1.364(4) . ? C506 C505 1.380(4) . ? C506 C501 1.402(4) . ? C504 C505 1.369(4) . ? C601 C606 1.397(4) . ? C601 C602 1.400(4) . ? C602 C603 1.379(4) . ? C603 C604 1.380(4) . ? C604 C605 1.377(4) . ? C605 C606 1.382(4) . ? C701 C702 1.395(4) . ? C701 C706 1.403(4) . ? C702 C703 1.397(4) . ? C703 C704 1.354(5) . ? C704 C705 1.374(5) . ? C705 C706 1.388(5) . ? C801 C806 1.372(4) . ? C801 C802 1.377(4) . ? C802 C803 1.388(4) . ? C803 C804 1.346(4) . ? C804 C805 1.352(5) . ? C805 C806 1.389(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni N1 155.72(8) . . ? N3 Ni N2 83.25(8) . . ? N1 Ni N2 83.33(8) . . ? N3 Ni S1 102.76(7) . . ? N1 Ni S1 99.96(7) . . ? N2 Ni S1 103.25(7) . . ? N3 Ni S2 94.19(6) . . ? N1 Ni S2 91.26(7) . . ? N2 Ni S2 159.29(6) . . ? S1 Ni S2 97.37(4) . . ? C1 S1 Ni 105.67(9) . . ? C23 S2 Ni 103.69(9) . . ? C8 N1 C11 109.4(2) . . ? C8 N1 C7 105.4(2) . . ? C11 N1 C7 111.6(2) . . ? C8 N1 Ni 114.01(16) . . ? C11 N1 Ni 107.57(16) . . ? C7 N1 Ni 108.89(15) . . ? C12 N2 C13 111.5(2) . . ? C12 N2 C16 111.4(2) . . ? C13 N2 C16 110.2(2) . . ? C12 N2 Ni 99.25(15) . . ? C13 N2 Ni 116.90(16) . . ? C16 N2 Ni 107.09(15) . . ? C18 N3 C17 113.1(2) . . ? C18 N3 C21 109.9(2) . . ? C17 N3 C21 108.46(19) . . ? C18 N3 Ni 113.04(16) . . ? C17 N3 Ni 99.43(16) . . ? C21 N3 Ni 112.58(16) . . ? C32 N4 C28 109.9(2) . . ? C32 N4 C29 111.9(2) . . ? C28 N4 C29 113.5(2) . . ? C33 N5 C34 111.6(3) . . ? C33 N5 C37 111.6(3) . . ? C34 N5 C37 112.0(3) . . ? C38 N6 C42 113.0(2) . . ? C38 N6 C39 112.0(2) . . ? C42 N6 C39 110.5(2) . . ? C2 C1 C6 117.8(2) . . ? C2 C1 S1 119.7(2) . . ? C6 C1 S1 122.4(2) . . ? C3 C2 C1 120.6(3) . . ? C3 C2 C42 119.0(2) . . ? C1 C2 C42 120.3(2) . . ? C2 C3 C4 122.6(3) . . ? C5 C4 C3 116.0(3) . . ? C5 C4 C43 122.9(3) . . ? C3 C4 C43 121.1(3) . . ? C4 C5 C6 123.9(3) . . ? C5 C6 C1 119.1(3) . . ? C5 C6 C7 118.4(2) . . ? C1 C6 C7 122.4(2) . . ? C6 C7 N1 117.9(2) . . ? N1 C8 C9 116.3(2) . . ? C8 C9 C10 110.6(3) . . ? N1 C11 C12 110.1(2) . . ? N2 C12 C11 109.9(2) . . ? N2 C13 C14 117.1(2) . . ? C13 C14 C15 110.0(2) . . ? N2 C16 C17 110.4(2) . . ? N3 C17 C16 111.5(2) . . ? N3 C18 C19 116.9(2) . . ? C20 C19 C18 110.7(2) . . ? C22 C21 N3 113.5(2) . . ? C27 C22 C23 119.7(2) . . ? C27 C22 C21 120.9(2) . . ? C23 C22 C21 119.4(2) . . ? C24 C23 C22 118.1(2) . . ? C24 C23 S2 121.2(2) . . ? C22 C23 S2 120.6(2) . . ? C25 C24 C23 120.3(3) . . ? C25 C24 C28 119.3(2) . . ? C23 C24 C28 120.2(2) . . ? C26 C25 C24 122.2(3) . . ? C25 C26 C27 116.7(3) . . ? C25 C26 C47 121.4(3) . . ? C27 C26 C47 121.9(3) . . ? C22 C27 C26 123.1(3) . . ? N4 C28 C24 112.6(2) . . ? C30 C29 N4 116.4(3) . . ? C31 C30 C29 115.2(3) . . ? N4 C32 C33 113.5(2) . . ? N5 C33 C32 109.9(3) . . ? N5 C34 C35 114.9(4) . . ? C34 C35 C36 109.4(5) . . ? C38 C37 N5 110.3(3) . . ? C37 C38 N6 110.6(2) . . ? C40 C39 N6 112.8(3) . . ? C41 C40 C39 110.2(4) . . ? N6 C42 C2 114.6(2) . . ? C46A C43 C44A 121.2(6) . . ? C46A C43 C44B 128.9(8) . . ? C44A C43 C44B 24.5(7) . . ? C46A C43 C46B 42.4(5) . . ? C44A C43 C46B 131.3(7) . . ? C44B C43 C46B 117.7(7) . . ? C46A C43 C4 112.0(4) . . ? C44A C43 C4 111.0(5) . . ? C44B C43 C4 117.0(7) . . ? C46B C43 C4 117.4(5) . . ? C46A C43 C45A 105.1(5) . . ? C44A C43 C45A 101.3(4) . . ? C44B C43 C45A 76.8(6) . . ? C46B C43 C45A 62.8(5) . . ? C4 C43 C45A 104.0(3) . . ? C46A C43 C45B 56.4(5) . . ? C44A C43 C45B 76.9(5) . . ? C44B C43 C45B 98.7(7) . . ? C46B C43 C45B 97.3(6) . . ? C4 C43 C45B 102.2(3) . . ? C45A C43 C45B 152.4(4) . . ? C50B C47 C49B 114.0(6) . . ? C50B C47 C49A 130.0(5) . . ? C49B C47 C49A 59.2(4) . . ? C50B C47 C26 112.9(5) . . ? C49B C47 C26 107.9(4) . . ? C49A C47 C26 116.1(4) . . ? C50B C47 C48A 41.9(5) . . ? C49B C47 C48A 140.9(5) . . ? C49A C47 C48A 108.6(5) . . ? C26 C47 C48A 110.4(4) . . ? C50B C47 C48B 108.1(5) . . ? C49B C47 C48B 108.3(5) . . ? C49A C47 C48B 49.2(4) . . ? C26 C47 C48B 105.1(4) . . ? C48A C47 C48B 68.7(5) . . ? C50B C47 C50A 63.4(5) . . ? C49B C47 C50A 55.6(4) . . ? C49A C47 C50A 108.8(5) . . ? C26 C47 C50A 108.3(3) . . ? C48A C47 C50A 104.0(5) . . ? C48B C47 C50A 146.1(5) . . ? C101 B1 C201 110.6(2) . . ? C101 B1 C401 109.4(2) . . ? C201 B1 C401 108.3(2) . . ? C101 B1 C301 108.9(2) . . ? C201 B1 C301 108.3(2) . . ? C401 B1 C301 111.3(2) . . ? C102 C101 C106 113.7(3) . . ? C102 C101 B1 124.6(2) . . ? C106 C101 B1 121.6(3) . . ? C103 C102 C101 123.3(3) . . ? C104 C103 C102 120.6(3) . . ? C105 C104 C103 118.5(3) . . ? C104 C105 C106 120.0(3) . . ? C105 C106 C101 123.8(3) . . ? C202 C201 C206 114.5(3) . . ? C202 C201 B1 123.7(3) . . ? C206 C201 B1 121.8(3) . . ? C201 C202 C203 123.1(3) . . ? C204 C203 C202 120.3(3) . . ? C205 C204 C203 118.7(3) . . ? C204 C205 C206 120.4(3) . . ? C205 C206 C201 123.1(3) . . ? C302 C301 C306 113.9(3) . . ? C302 C301 B1 122.8(3) . . ? C306 C301 B1 123.3(3) . . ? C301 C302 C303 123.3(3) . . ? C304 C303 C302 120.3(4) . . ? C305 C304 C303 118.9(4) . . ? C304 C305 C306 120.7(4) . . ? C305 C306 C301 122.9(4) . . ? C406 C401 C402 114.2(3) . . ? C406 C401 B1 121.6(3) . . ? C402 C401 B1 124.2(3) . . ? C403 C402 C401 123.8(3) . . ? C404 C403 C402 119.5(3) . . ? C403 C404 C405 119.8(3) . . ? C404 C405 C406 119.4(3) . . ? C405 C406 C401 123.2(3) . . ? C601 B2 C801 109.5(2) . . ? C601 B2 C501 109.7(3) . . ? C801 B2 C501 109.4(2) . . ? C601 B2 C701 107.6(3) . . ? C801 B2 C701 109.9(3) . . ? C501 B2 C701 110.6(2) . . ? C503 C502 C501 123.4(3) . . ? C504 C503 C502 120.3(3) . . ? C505 C506 C501 122.9(3) . . ? C502 C501 C506 114.1(3) . . ? C502 C501 B2 124.4(3) . . ? C506 C501 B2 121.5(3) . . ? C503 C504 C505 118.9(3) . . ? C504 C505 C506 120.5(3) . . ? C606 C601 C602 114.2(3) . . ? C606 C601 B2 121.2(3) . . ? C602 C601 B2 124.4(3) . . ? C603 C602 C601 123.4(3) . . ? C602 C603 C604 120.2(3) . . ? C605 C604 C603 118.5(3) . . ? C604 C605 C606 120.4(3) . . ? C605 C606 C601 123.2(3) . . ? C702 C701 C706 114.1(3) . . ? C702 C701 B2 124.1(3) . . ? C706 C701 B2 121.9(3) . . ? C701 C702 C703 123.2(4) . . ? C704 C703 C702 120.0(4) . . ? C703 C704 C705 119.8(4) . . ? C704 C705 C706 119.7(4) . . ? C705 C706 C701 123.2(4) . . ? C806 C801 C802 113.0(3) . . ? C806 C801 B2 124.5(3) . . ? C802 C801 B2 122.3(3) . . ? C801 C802 C803 124.1(3) . . ? C804 C803 C802 120.6(3) . . ? C803 C804 C805 117.6(4) . . ? C804 C805 C806 121.1(4) . . ? C801 C806 C805 123.5(3) . . ? #===END