Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'L. R. Nassimbeni' 'M. L. Kilkenny' _publ_contact_author_name 'Prof Luigi R Nassimbeni' _publ_contact_author_address ; Prof Luigi R Nassimbeni Department of Chemistry University of Cape Town Rondebosch 7701 SOUTH AFRICA ; data_COMPOUND 1: Ni(NCS)2(4-aminopyridine)4 _database_code_CSD 155036 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ni(NCS)2(4-aminopyridine)4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 N10 Ni S2' _chemical_formula_weight 551.34 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 17.046(3) _cell_length_b 9.6274(19) _cell_length_c 16.129(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2646.9(9) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 1.382 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6078 _exptl_absorpt_correction_T_max 0.7326 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12674 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 30.24 _reflns_number_total 3517 _reflns_number_gt 2562 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.7237P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3517 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.7500 0.2500 0.067339(17) 0.01677(9) Uani 1 2 d S . . S1 S 0.56909(3) -0.13893(5) 0.07884(3) 0.03556(13) Uani 1 1 d . . . N3 N 0.68833(7) 0.36302(14) 0.15920(8) 0.0196(3) Uani 1 1 d . . . N2 N 0.68567(7) 0.36006(14) -0.02380(8) 0.0187(3) Uani 1 1 d . . . C1 C 0.62477(9) -0.00014(17) 0.07207(9) 0.0203(3) Uani 1 1 d . . . N1 N 0.66442(8) 0.09694(15) 0.06789(8) 0.0236(3) Uani 1 1 d . . . C9 C 0.61388(9) 0.51540(18) 0.28647(10) 0.0225(3) Uani 1 1 d . . . N5 N 0.58049(11) 0.5883(2) 0.34855(11) 0.0378(4) Uani 1 1 d . . . C6 C 0.72136(10) 0.43271(18) -0.08417(10) 0.0236(4) Uani 1 1 d . . . C3 C 0.56285(10) 0.43571(17) -0.08018(10) 0.0218(3) Uani 1 1 d . . . C7 C 0.65507(9) 0.30051(18) 0.22497(10) 0.0206(3) Uani 1 1 d . . . N4 N 0.55824(11) 0.58706(18) -0.19987(12) 0.0332(4) Uani 1 1 d . . . C8 C 0.61835(9) 0.36993(18) 0.28817(11) 0.0227(4) Uani 1 1 d . . . C10 C 0.64702(10) 0.58068(18) 0.21692(10) 0.0237(4) Uani 1 1 d . . . C5 C 0.68189(10) 0.50648(19) -0.14397(10) 0.0249(4) Uani 1 1 d . . . C4 C 0.60019(9) 0.50960(17) -0.14305(10) 0.0214(3) Uani 1 1 d . . . C2 C 0.60696(9) 0.36326(17) -0.02338(10) 0.0198(3) Uani 1 1 d . . . C11 C 0.68258(10) 0.50204(17) 0.15687(10) 0.0213(3) Uani 1 1 d . . . H2 H 0.5075(11) 0.4297(18) -0.0775(10) 0.024(5) Uiso 1 1 d . . . H7 H 0.6583(10) 0.2038(19) 0.2262(10) 0.023(4) Uiso 1 1 d . . . H10 H 0.7033(10) 0.5466(19) 0.1104(11) 0.027(5) Uiso 1 1 d . . . H1 H 0.5829(10) 0.3116(18) 0.0186(11) 0.021(4) Uiso 1 1 d . . . H3 H 0.7086(12) 0.551(2) -0.1841(11) 0.032(5) Uiso 1 1 d . . . H4 H 0.7793(12) 0.4314(19) -0.0832(10) 0.027(5) Uiso 1 1 d . . . H8 H 0.5952(10) 0.3200(19) 0.3332(11) 0.026(5) Uiso 1 1 d . . . H11 H 0.5745(13) 0.675(3) 0.3438(14) 0.049(7) Uiso 1 1 d . . . H5 H 0.5091(15) 0.571(2) -0.1990(13) 0.052(7) Uiso 1 1 d . . . H9 H 0.6466(10) 0.676(2) 0.2100(11) 0.029(5) Uiso 1 1 d . . . H6 H 0.5780(12) 0.594(2) -0.2461(14) 0.037(6) Uiso 1 1 d . . . H12 H 0.5559(12) 0.546(2) 0.3872(14) 0.042(6) Uiso 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 Ni1 0.01691(14) 0.01656(14) 0.01685(16) 0.000 0.000 0.00013(11) S1 0.0388(3) 0.0265(3) 0.0413(3) 0.0022(2) 0.0055(2) -0.0135(2) N3 0.0214(7) 0.0190(7) 0.0183(7) 0.0021(5) 0.0002(5) 0.0019(5) N2 0.0171(6) 0.0220(7) 0.0171(7) -0.0007(5) 0.0017(5) 0.0006(5) C1 0.0203(8) 0.0230(8) 0.0177(8) -0.0003(7) 0.0012(6) 0.0029(6) N1 0.0221(7) 0.0228(7) 0.0259(8) -0.0006(6) 0.0012(6) -0.0018(6) C9 0.0197(8) 0.0273(9) 0.0205(8) -0.0037(7) -0.0024(7) 0.0009(7) N5 0.0494(11) 0.0305(10) 0.0336(10) -0.0061(8) 0.0176(8) 0.0032(8) C6 0.0191(8) 0.0309(10) 0.0207(9) 0.0024(7) 0.0028(7) 0.0001(7) C3 0.0165(7) 0.0214(8) 0.0274(9) -0.0035(7) -0.0009(7) 0.0006(6) C7 0.0212(8) 0.0188(8) 0.0216(9) 0.0040(7) -0.0013(7) 0.0030(7) N4 0.0315(9) 0.0367(9) 0.0315(10) 0.0099(7) -0.0098(8) 0.0007(7) C8 0.0212(8) 0.0276(9) 0.0193(9) 0.0053(7) 0.0009(7) 0.0017(7) C10 0.0273(8) 0.0179(8) 0.0257(9) 0.0004(7) 0.0010(7) 0.0015(7) C5 0.0247(8) 0.0304(9) 0.0195(9) 0.0059(7) 0.0036(7) -0.0017(7) C4 0.0231(8) 0.0197(8) 0.0213(9) -0.0033(7) -0.0050(7) 0.0010(6) C2 0.0189(8) 0.0206(8) 0.0200(9) -0.0008(7) 0.0029(6) -0.0013(6) C11 0.0251(8) 0.0196(8) 0.0193(8) 0.0036(7) 0.0007(7) 0.0017(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 Ni1 N1 2.0735(14) 2_655 ? Ni1 N1 2.0735(14) . ? Ni1 N2 2.1180(13) . ? Ni1 N2 2.1180(13) 2_655 ? Ni1 N3 2.1177(13) 2_655 ? Ni1 N3 2.1177(13) . ? S1 C1 1.6427(17) . ? N3 C7 1.345(2) . ? N3 C11 1.342(2) . ? N2 C2 1.342(2) . ? N2 C6 1.344(2) . ? C1 N1 1.155(2) . ? C9 N5 1.349(2) . ? C9 C10 1.404(2) . ? C9 C8 1.403(2) . ? C6 C5 1.374(2) . ? C3 C2 1.375(2) . ? C3 C4 1.393(2) . ? C7 C8 1.370(2) . ? N4 C4 1.381(2) . ? C10 C11 1.371(2) . ? C5 C4 1.393(2) . ? 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 N1 Ni1 N1 179.51(8) 2_655 . ? N1 Ni1 N2 90.67(5) 2_655 . ? N1 Ni1 N2 89.67(5) . . ? N1 Ni1 N2 89.67(5) 2_655 2_655 ? N1 Ni1 N2 90.67(5) . 2_655 ? N2 Ni1 N2 92.10(7) . 2_655 ? N1 Ni1 N3 90.74(5) 2_655 2_655 ? N1 Ni1 N3 88.92(5) . 2_655 ? N2 Ni1 N3 178.52(5) . 2_655 ? N2 Ni1 N3 88.37(5) 2_655 2_655 ? N1 Ni1 N3 88.92(5) 2_655 . ? N1 Ni1 N3 90.74(5) . . ? N2 Ni1 N3 88.37(5) . . ? N2 Ni1 N3 178.52(5) 2_655 . ? N3 Ni1 N3 91.20(7) 2_655 . ? C7 N3 C11 115.94(14) . . ? C7 N3 Ni1 122.08(11) . . ? C11 N3 Ni1 121.93(11) . . ? C2 N2 C6 116.36(14) . . ? C2 N2 Ni1 121.71(11) . . ? C6 N2 Ni1 121.92(11) . . ? N1 C1 S1 179.32(16) . . ? C1 N1 Ni1 170.64(13) . . ? N5 C9 C10 122.00(17) . . ? N5 C9 C8 121.86(17) . . ? C10 C9 C8 116.14(15) . . ? N2 C6 C5 123.77(16) . . ? C2 C3 C4 119.62(15) . . ? N3 C7 C8 124.13(16) . . ? C7 C8 C9 119.81(16) . . ? C11 C10 C9 119.68(16) . . ? C6 C5 C4 119.56(16) . . ? N4 C4 C3 121.49(16) . . ? N4 C4 C5 121.48(17) . . ? C3 C4 C5 116.97(15) . . ? N2 C2 C3 123.70(15) . . ? N3 C11 C10 124.28(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 N3 C7 -137.16(12) 2_655 . . . ? N1 Ni1 N3 C7 42.49(12) . . . . ? N2 Ni1 N3 C7 132.13(12) . . . . ? N2 Ni1 N3 C7 -119.4(19) 2_655 . . . ? N3 Ni1 N3 C7 -46.45(10) 2_655 . . . ? N1 Ni1 N3 C11 40.32(12) 2_655 . . . ? N1 Ni1 N3 C11 -140.04(12) . . . . ? N2 Ni1 N3 C11 -50.39(12) . . . . ? N2 Ni1 N3 C11 58(2) 2_655 . . . ? N3 Ni1 N3 C11 131.03(14) 2_655 . . . ? N1 Ni1 N2 C2 -143.16(12) 2_655 . . . ? N1 Ni1 N2 C2 36.48(13) . . . . ? N2 Ni1 N2 C2 127.14(14) 2_655 . . . ? N3 Ni1 N2 C2 19(2) 2_655 . . . ? N3 Ni1 N2 C2 -54.26(12) . . . . ? N1 Ni1 N2 C6 35.48(13) 2_655 . . . ? N1 Ni1 N2 C6 -144.87(13) . . . . ? N2 Ni1 N2 C6 -54.21(11) 2_655 . . . ? N3 Ni1 N2 C6 -162.6(19) 2_655 . . . ? N3 Ni1 N2 C6 124.38(13) . . . . ? S1 C1 N1 Ni1 26(17) . . . . ? N1 Ni1 N1 C1 -70.6(8) 2_655 . . . ? N2 Ni1 N1 C1 155.4(8) . . . . ? N2 Ni1 N1 C1 63.3(8) 2_655 . . . ? N3 Ni1 N1 C1 -25.0(8) 2_655 . . . ? N3 Ni1 N1 C1 -116.2(8) . . . . ? C2 N2 C6 C5 -0.7(2) . . . . ? Ni1 N2 C6 C5 -179.38(13) . . . . ? C11 N3 C7 C8 -1.3(2) . . . . ? Ni1 N3 C7 C8 176.29(12) . . . . ? N3 C7 C8 C9 0.0(3) . . . . ? N5 C9 C8 C7 -177.89(17) . . . . ? C10 C9 C8 C7 1.4(2) . . . . ? N5 C9 C10 C11 177.81(17) . . . . ? C8 C9 C10 C11 -1.4(2) . . . . ? N2 C6 C5 C4 0.8(3) . . . . ? C2 C3 C4 N4 -178.05(16) . . . . ? C2 C3 C4 C5 -0.6(2) . . . . ? C6 C5 C4 N4 177.29(17) . . . . ? C6 C5 C4 C3 -0.1(2) . . . . ? C6 N2 C2 C3 -0.2(2) . . . . ? Ni1 N2 C2 C3 178.55(12) . . . . ? C4 C3 C2 N2 0.8(3) . . . . ? C7 N3 C11 C10 1.2(2) . . . . ? Ni1 N3 C11 C10 -176.38(13) . . . . ? C9 C10 C11 N3 0.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 30.24 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.335 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.061 #===END data_COMPOUND 2: Ni(NCS)2(4-aminopyridine)4.EtOH.Acetone _database_code_CSD 155037 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni(NCS)2(4-aminopyridine)4.EtOH.Acetone _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H36 N10 Ni O2 S2' _chemical_formula_weight 655.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.5289(2) _cell_length_b 15.8155(3) _cell_length_c 21.7001(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3613.50(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17030 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.14 _reflns_number_total 7031 _reflns_number_gt 4527 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 7031 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.2001 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.086 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.49620(6) 0.97708(4) 0.97684(3) 0.0360(2) Uani 1 1 d . . . N3 N 0.4857(4) 0.8438(3) 0.98907(18) 0.0369(10) Uani 1 1 d . . . N5 N 0.5159(5) 1.1091(3) 0.9638(2) 0.0421(12) Uani 1 1 d . . . N2 N 0.6524(5) 0.9822(3) 1.0345(2) 0.0431(11) Uani 1 1 d . . . N1 N 0.3367(5) 0.9761(3) 0.9203(2) 0.0417(11) Uani 1 1 d . . . N4 N 0.6138(4) 0.9570(3) 0.8998(2) 0.0385(12) Uani 1 1 d . . . N6 N 0.3781(4) 0.9936(3) 1.0553(2) 0.0374(11) Uani 1 1 d . . . S2 S 0.83859(17) 1.00892(13) 1.12386(7) 0.0619(5) Uani 1 1 d . . . S1 S 0.13629(19) 0.95500(16) 0.83881(9) 0.0794(7) Uani 1 1 d . . . C2 C 0.7289(5) 0.9941(3) 1.0709(2) 0.0354(13) Uani 1 1 d . . . C1 C 0.2560(6) 0.9689(4) 0.8874(3) 0.0399(14) Uani 1 1 d . . . C18 C 0.4072(5) 1.0465(3) 1.1012(2) 0.0386(13) Uani 1 1 d . . . H19 H 0.4787 1.0827 1.0968 0.046 Uiso 1 1 calc R . . C22 C 0.2753(5) 0.9439(4) 1.0634(3) 0.0400(14) Uani 1 1 d . . . H22 H 0.2518 0.9074 1.0305 0.048 Uiso 1 1 calc R . . C14 C 0.4311(8) 1.2485(4) 0.9494(4) 0.069(2) Uani 1 1 d . . . H14 H 0.3584 1.2836 0.9453 0.082 Uiso 1 1 calc R . . C17 C 0.6334(7) 1.1435(4) 0.9569(3) 0.0540(18) Uani 1 1 d . . . H16 H 0.7049 1.1070 0.9589 0.065 Uiso 1 1 calc R . . C13 C 0.4192(7) 1.1636(4) 0.9601(3) 0.0560(18) Uani 1 1 d . . . H13 H 0.3358 1.1417 0.9654 0.067 Uiso 1 1 calc R . . C19 C 0.3349(6) 1.0504(4) 1.1561(2) 0.0418(14) Uani 1 1 d . . . H20 H 0.3563 1.0899 1.1874 0.050 Uiso 1 1 calc R . . C8 C 0.5954(5) 0.9985(4) 0.8461(2) 0.0402(13) Uani 1 1 d . . . H7 H 0.5262 1.0369 0.8437 0.048 Uiso 1 1 calc R . . C5 C 0.4875(5) 0.6668(3) 1.0049(2) 0.0376(12) Uani 1 1 d . . . N10 N 0.1620(5) 0.9973(3) 1.2168(2) 0.0526(13) Uani 1 1 d . . . H23 H 0.1808 1.0327 1.2467 0.063 Uiso 1 1 calc R . . H24 H 0.0974 0.9624 1.2208 0.063 Uiso 1 1 calc R . . C9 C 0.6694(6) 0.9888(4) 0.7957(2) 0.0442(14) Uani 1 1 d . . . H8 H 0.6526 1.0208 0.7596 0.053 Uiso 1 1 calc R . . C20 C 0.2331(5) 0.9965(3) 1.1639(2) 0.0382(13) Uani 1 1 d . . . C16 C 0.6541(7) 1.2277(4) 0.9473(4) 0.066(2) Uani 1 1 d . . . H15 H 0.7385 1.2479 0.9426 0.079 Uiso 1 1 calc R . . C10 C 0.7714(5) 0.9311(4) 0.7968(2) 0.0404(14) Uani 1 1 d . . . C7 C 0.5321(6) 0.8064(4) 1.0403(2) 0.0429(15) Uani 1 1 d . . . H4 H 0.5652 0.8418 1.0719 0.051 Uiso 1 1 calc R . . C11 C 0.7889(6) 0.8868(4) 0.8514(3) 0.0430(14) Uani 1 1 d . . . H9 H 0.8549 0.8461 0.8546 0.052 Uiso 1 1 calc R . . C6 C 0.5346(6) 0.7214(4) 1.0497(3) 0.0467(16) Uani 1 1 d . . . H3 H 0.5686 0.6993 1.0869 0.056 Uiso 1 1 calc R . . C21 C 0.2025(5) 0.9425(3) 1.1157(2) 0.0376(13) Uani 1 1 d . . . H21 H 0.1322 0.9051 1.1190 0.045 Uiso 1 1 calc R . . N7 N 0.4876(5) 0.5826(3) 1.0123(2) 0.0446(11) Uani 1 1 d . . . H6 H 0.5181 0.5602 1.0463 0.053 Uiso 1 1 calc R . . H5 H 0.4571 0.5498 0.9831 0.053 Uiso 1 1 calc R . . N8 N 0.8496(5) 0.9197(4) 0.7464(2) 0.0579(14) Uani 1 1 d . . . H12 H 0.9129 0.8835 0.7482 0.070 Uiso 1 1 calc R . . H11 H 0.8360 0.9487 0.7124 0.070 Uiso 1 1 calc R . . C4 C 0.4370(6) 0.7050(4) 0.9512(3) 0.0452(15) Uani 1 1 d . . . H2 H 0.4021 0.6714 0.9191 0.054 Uiso 1 1 calc R . . C3 C 0.4393(6) 0.7916(4) 0.9464(3) 0.0402(14) Uani 1 1 d . . . H1 H 0.4054 0.8161 0.9100 0.048 Uiso 1 1 calc R . . C15 C 0.5560(8) 1.2824(4) 0.9445(4) 0.070(2) Uani 1 1 d . . . N9 N 0.5726(7) 1.3674(4) 0.9349(4) 0.101(3) Uani 1 1 d . . . H17 H 0.6496 1.3881 0.9304 0.121 Uiso 1 1 calc R . . H18 H 0.5063 1.4012 0.9333 0.121 Uiso 1 1 calc R . . O1 O -0.0104(6) 0.8474(4) 1.2349(3) 0.0924(17) Uiso 1 1 d . . . C23 C 0.0255(10) 0.7794(6) 1.2509(4) 0.087(3) Uiso 1 1 d . . . C12 C 0.7124(5) 0.9017(4) 0.8998(3) 0.0419(14) Uani 1 1 d . . . H10 H 0.7285 0.8712 0.9367 0.050 Uiso 1 1 calc R . . C26 C 1.0412(5) 0.7006(4) 0.7245(3) 0.254(10) Uiso 1 1 d R . . C24 C -0.0392(17) 0.6987(12) 1.2488(8) 0.191(7) Uiso 1 1 d . . . C25 C 0.1751(18) 0.7783(12) 1.2752(9) 0.195(6) Uiso 1 1 d . . . C27 C 1.066(3) 0.663(2) 0.6565(14) 0.146(12) Uiso 0.435(16) 1 d P . . C28 C 1.0270(16) 0.6365(11) 0.7821(7) 0.094(6) Uiso 0.565(16) 1 d P . . O2A O 1.0039(15) 0.7707(8) 0.7584(8) 0.088(5) Uiso 0.435(16) 1 d P . . O2B O 1.0083(13) 0.7774(8) 0.7159(7) 0.110(5) Uiso 0.565(16) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0343(4) 0.0406(4) 0.0329(3) 0.0011(3) -0.0032(3) -0.0019(4) N3 0.041(3) 0.038(2) 0.031(2) 0.0006(17) -0.002(2) 0.001(2) N5 0.046(3) 0.033(2) 0.048(3) 0.0004(19) -0.001(2) -0.006(3) N2 0.040(3) 0.048(3) 0.042(3) 0.002(2) -0.006(2) -0.002(3) N1 0.040(3) 0.049(3) 0.036(2) -0.002(2) -0.004(2) -0.002(3) N4 0.038(3) 0.045(3) 0.033(2) 0.007(2) -0.004(2) 0.005(2) N6 0.035(3) 0.041(3) 0.036(2) -0.003(2) 0.000(2) 0.000(2) S2 0.0527(11) 0.0902(14) 0.0429(9) -0.0171(9) -0.0128(7) 0.0045(10) S1 0.0607(12) 0.1246(19) 0.0530(10) 0.0292(11) -0.0241(9) -0.0422(12) C2 0.036(4) 0.037(3) 0.033(3) -0.002(2) 0.004(3) 0.001(3) C1 0.040(4) 0.047(3) 0.033(3) 0.011(3) -0.001(3) -0.011(3) C18 0.035(3) 0.038(3) 0.043(3) -0.003(2) -0.003(3) -0.005(2) C22 0.038(4) 0.043(3) 0.039(3) -0.007(3) 0.001(3) -0.012(3) C14 0.059(5) 0.040(4) 0.106(6) 0.012(4) 0.023(4) 0.006(4) C17 0.057(5) 0.037(3) 0.068(4) 0.013(3) -0.008(3) -0.010(3) C13 0.054(4) 0.047(4) 0.067(5) 0.006(3) 0.006(3) -0.007(3) C19 0.051(4) 0.039(3) 0.035(3) -0.006(2) 0.000(3) 0.000(3) C8 0.041(4) 0.040(3) 0.039(3) 0.000(2) -0.002(3) 0.009(3) C5 0.028(3) 0.045(3) 0.040(3) 0.000(2) 0.011(3) 0.001(3) N10 0.052(3) 0.055(3) 0.050(3) -0.005(2) 0.014(3) -0.006(3) C9 0.049(4) 0.046(3) 0.037(3) 0.003(3) 0.000(3) 0.000(3) C20 0.042(3) 0.037(3) 0.036(3) 0.000(2) 0.003(3) 0.003(3) C16 0.037(4) 0.056(4) 0.104(6) 0.021(4) -0.001(4) -0.013(3) C10 0.038(4) 0.043(3) 0.040(3) -0.004(3) 0.002(3) 0.004(3) C7 0.050(4) 0.051(3) 0.028(3) 0.003(2) -0.003(2) -0.010(3) C11 0.041(4) 0.050(3) 0.038(3) 0.004(3) -0.004(3) 0.011(3) C6 0.056(4) 0.056(4) 0.028(3) 0.008(3) -0.001(3) -0.006(3) C21 0.032(3) 0.039(3) 0.041(3) 0.000(3) 0.003(2) 0.001(3) N7 0.049(3) 0.037(2) 0.048(3) 0.0014(19) -0.001(3) 0.000(2) N8 0.056(4) 0.078(4) 0.040(3) 0.011(3) 0.010(3) 0.015(3) C4 0.048(4) 0.051(4) 0.037(3) -0.013(3) -0.006(3) -0.003(3) C3 0.049(4) 0.036(3) 0.036(3) -0.005(2) -0.012(3) 0.002(3) C15 0.076(5) 0.038(4) 0.096(6) 0.014(4) 0.009(4) -0.009(4) N9 0.081(5) 0.054(4) 0.168(8) 0.025(5) 0.002(5) -0.006(4) C12 0.033(4) 0.051(4) 0.042(3) 0.013(3) -0.007(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.068(5) . ? Ni1 N1 2.080(5) . ? Ni1 N4 2.104(5) . ? Ni1 N5 2.118(4) . ? Ni1 N3 2.128(4) . ? Ni1 N6 2.125(4) . ? N3 C3 1.333(7) . ? N3 C7 1.351(7) . ? N5 C13 1.337(8) . ? N5 C17 1.359(8) . ? N2 C2 1.143(7) . ? N1 C1 1.116(7) . ? N4 C12 1.358(7) . ? N4 C8 1.351(7) . ? N6 C18 1.337(7) . ? N6 C22 1.348(7) . ? S2 C2 1.647(6) . ? S1 C1 1.658(6) . ? C18 C19 1.415(8) . ? C22 C21 1.371(8) . ? C14 C13 1.368(9) . ? C14 C15 1.425(11) . ? C17 C16 1.365(9) . ? C19 C20 1.381(8) . ? C8 C9 1.352(8) . ? C5 N7 1.342(7) . ? C5 C6 1.391(8) . ? C5 C4 1.416(8) . ? N10 C20 1.370(7) . ? C9 C10 1.410(8) . ? C20 C21 1.387(8) . ? C16 C15 1.349(10) . ? C10 N8 1.382(7) . ? C10 C11 1.388(8) . ? C7 C6 1.359(9) . ? C11 C12 1.343(8) . ? C4 C3 1.373(9) . ? C15 N9 1.371(10) . ? O1 C23 1.191(9) . ? C23 C24 1.447(18) . ? C23 C25 1.66(2) . ? C26 O2B 1.277(13) . ? C26 O2A 1.387(15) . ? C26 C27 1.61(3) . ? C26 C28 1.617(18) . ? O2A O2B 0.928(15) . ? 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 Ni1 N1 177.9(2) . . ? N2 Ni1 N4 91.03(19) . . ? N1 Ni1 N4 90.33(18) . . ? N2 Ni1 N5 88.0(2) . . ? N1 Ni1 N5 90.4(2) . . ? N4 Ni1 N5 89.15(18) . . ? N2 Ni1 N3 90.26(19) . . ? N1 Ni1 N3 91.41(19) . . ? N4 Ni1 N3 88.86(17) . . ? N5 Ni1 N3 177.30(19) . . ? N2 Ni1 N6 88.62(19) . . ? N1 Ni1 N6 90.06(18) . . ? N4 Ni1 N6 178.31(19) . . ? N5 Ni1 N6 92.49(18) . . ? N3 Ni1 N6 89.48(17) . . ? C3 N3 C7 115.7(5) . . ? C3 N3 Ni1 123.1(4) . . ? C7 N3 Ni1 121.1(4) . . ? C13 N5 C17 115.4(5) . . ? C13 N5 Ni1 124.7(4) . . ? C17 N5 Ni1 119.9(4) . . ? C2 N2 Ni1 169.8(5) . . ? C1 N1 Ni1 173.3(5) . . ? C12 N4 C8 114.9(5) . . ? C12 N4 Ni1 123.2(4) . . ? C8 N4 Ni1 121.8(4) . . ? C18 N6 C22 116.9(5) . . ? C18 N6 Ni1 122.7(4) . . ? C22 N6 Ni1 120.1(4) . . ? N2 C2 S2 178.7(6) . . ? N1 C1 S1 178.3(6) . . ? N6 C18 C19 122.1(5) . . ? N6 C22 C21 124.5(5) . . ? C13 C14 C15 117.9(7) . . ? N5 C17 C16 123.5(7) . . ? N5 C13 C14 124.9(7) . . ? C20 C19 C18 119.5(5) . . ? C9 C8 N4 124.1(5) . . ? N7 C5 C6 122.2(5) . . ? N7 C5 C4 121.4(5) . . ? C6 C5 C4 116.4(5) . . ? C8 C9 C10 119.9(5) . . ? N10 C20 C19 121.4(5) . . ? N10 C20 C21 120.6(5) . . ? C19 C20 C21 118.0(5) . . ? C15 C16 C17 120.7(7) . . ? N8 C10 C11 122.1(5) . . ? N8 C10 C9 121.6(5) . . ? C11 C10 C9 116.2(5) . . ? N3 C7 C6 124.2(5) . . ? C12 C11 C10 119.9(5) . . ? C7 C6 C5 120.2(5) . . ? C22 C21 C20 118.9(5) . . ? C3 C4 C5 118.7(5) . . ? N3 C3 C4 124.9(5) . . ? C16 C15 N9 122.6(7) . . ? C16 C15 C14 117.5(6) . . ? N9 C15 C14 119.9(7) . . ? O1 C23 C24 129.5(11) . . ? O1 C23 C25 113.8(10) . . ? C24 C23 C25 116.5(11) . . ? C11 C12 N4 124.9(5) . . ? O2B C26 O2A 40.5(7) . . ? O2B C26 C27 105.2(14) . . ? O2A C26 C27 145.6(14) . . ? O2B C26 C28 133.1(10) . . ? O2A C26 C28 93.7(9) . . ? C27 C26 C28 119.5(14) . . ? O2B O2A C26 63.4(12) . . ? O2A O2B C26 76.1(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N3 C3 -151.0(5) . . . . ? N1 Ni1 N3 C3 30.3(4) . . . . ? N4 Ni1 N3 C3 -60.0(4) . . . . ? N5 Ni1 N3 C3 -103(3) . . . . ? N6 Ni1 N3 C3 120.3(4) . . . . ? N2 Ni1 N3 C7 25.7(4) . . . . ? N1 Ni1 N3 C7 -153.0(4) . . . . ? N4 Ni1 N3 C7 116.7(4) . . . . ? N5 Ni1 N3 C7 74(4) . . . . ? N6 Ni1 N3 C7 -62.9(4) . . . . ? N2 Ni1 N5 C13 -140.9(5) . . . . ? N1 Ni1 N5 C13 37.7(5) . . . . ? N4 Ni1 N5 C13 128.0(5) . . . . ? N3 Ni1 N5 C13 171(3) . . . . ? N6 Ni1 N5 C13 -52.4(5) . . . . ? N2 Ni1 N5 C17 40.9(5) . . . . ? N1 Ni1 N5 C17 -140.5(5) . . . . ? N4 Ni1 N5 C17 -50.2(5) . . . . ? N3 Ni1 N5 C17 -8(4) . . . . ? N6 Ni1 N5 C17 129.4(5) . . . . ? N1 Ni1 N2 C2 13(7) . . . . ? N4 Ni1 N2 C2 143(3) . . . . ? N5 Ni1 N2 C2 54(3) . . . . ? N3 Ni1 N2 C2 -128(3) . . . . ? N6 Ni1 N2 C2 -39(3) . . . . ? N2 Ni1 N1 C1 176(41) . . . . ? N4 Ni1 N1 C1 46(4) . . . . ? N5 Ni1 N1 C1 135(4) . . . . ? N3 Ni1 N1 C1 -43(4) . . . . ? N6 Ni1 N1 C1 -132(4) . . . . ? N2 Ni1 N4 C12 44.9(4) . . . . ? N1 Ni1 N4 C12 -136.7(4) . . . . ? N5 Ni1 N4 C12 132.8(4) . . . . ? N3 Ni1 N4 C12 -45.3(4) . . . . ? N6 Ni1 N4 C12 -33(6) . . . . ? N2 Ni1 N4 C8 -135.6(5) . . . . ? N1 Ni1 N4 C8 42.7(5) . . . . ? N5 Ni1 N4 C8 -47.7(5) . . . . ? N3 Ni1 N4 C8 134.1(4) . . . . ? N6 Ni1 N4 C8 146(6) . . . . ? N2 Ni1 N6 C18 40.1(4) . . . . ? N1 Ni1 N6 C18 -138.3(5) . . . . ? N4 Ni1 N6 C18 118(6) . . . . ? N5 Ni1 N6 C18 -47.8(4) . . . . ? N3 Ni1 N6 C18 130.3(4) . . . . ? N2 Ni1 N6 C22 -133.5(5) . . . . ? N1 Ni1 N6 C22 48.2(4) . . . . ? N4 Ni1 N6 C22 -55(6) . . . . ? N5 Ni1 N6 C22 138.6(4) . . . . ? N3 Ni1 N6 C22 -43.2(4) . . . . ? Ni1 N2 C2 S2 117(23) . . . . ? Ni1 N1 C1 S1 38(21) . . . . ? C22 N6 C18 C19 0.5(8) . . . . ? Ni1 N6 C18 C19 -173.2(4) . . . . ? C18 N6 C22 C21 -2.2(8) . . . . ? Ni1 N6 C22 C21 171.7(4) . . . . ? C13 N5 C17 C16 0.5(9) . . . . ? Ni1 N5 C17 C16 178.9(5) . . . . ? C17 N5 C13 C14 0.9(10) . . . . ? Ni1 N5 C13 C14 -177.4(6) . . . . ? C15 C14 C13 N5 -3.0(12) . . . . ? N6 C18 C19 C20 1.9(8) . . . . ? C12 N4 C8 C9 -1.5(8) . . . . ? Ni1 N4 C8 C9 179.0(4) . . . . ? N4 C8 C9 C10 1.4(9) . . . . ? C18 C19 C20 N10 178.9(5) . . . . ? C18 C19 C20 C21 -2.7(8) . . . . ? N5 C17 C16 C15 0.4(12) . . . . ? C8 C9 C10 N8 -179.6(6) . . . . ? C8 C9 C10 C11 0.1(8) . . . . ? C3 N3 C7 C6 0.6(8) . . . . ? Ni1 N3 C7 C6 -176.4(4) . . . . ? N8 C10 C11 C12 178.3(6) . . . . ? C9 C10 C11 C12 -1.5(8) . . . . ? N3 C7 C6 C5 0.1(9) . . . . ? N7 C5 C6 C7 -179.7(5) . . . . ? C4 C5 C6 C7 -0.9(8) . . . . ? N6 C22 C21 C20 1.4(9) . . . . ? N10 C20 C21 C22 179.5(5) . . . . ? C19 C20 C21 C22 1.1(8) . . . . ? N7 C5 C4 C3 179.8(6) . . . . ? C6 C5 C4 C3 1.0(8) . . . . ? C7 N3 C3 C4 -0.5(9) . . . . ? Ni1 N3 C3 C4 176.4(5) . . . . ? C5 C4 C3 N3 -0.3(10) . . . . ? C17 C16 C15 N9 -180.0(8) . . . . ? C17 C16 C15 C14 -2.5(12) . . . . ? C13 C14 C15 C16 3.7(12) . . . . ? C13 C14 C15 N9 -178.8(7) . . . . ? C10 C11 C12 N4 1.4(9) . . . . ? C8 N4 C12 C11 0.0(8) . . . . ? Ni1 N4 C12 C11 179.6(5) . . . . ? C27 C26 O2A O2B -3(3) . . . . ? C28 C26 O2A O2B -168.2(16) . . . . ? C27 C26 O2B O2A 178.4(17) . . . . ? C28 C26 O2B O2A 16(2) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.746 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.101 #===END data_COMPOUND 3: Ni(NCS)2(4-aminopyridine)4.2DMSO _database_code_CSD 155038 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ni(NCS)2(4-aminopyridine)4.2DMSO' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 N10 Ni O2 S4' _chemical_formula_weight 707.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.2639(2) _cell_length_b 15.7895(3) _cell_length_c 21.8834(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3546.46(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15491 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.10 _reflns_number_total 7790 _reflns_number_gt 7043 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+7.2493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.035(18) _refine_ls_number_reflns 7790 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.99764(5) 0.47972(3) 0.974147(19) 0.01847(12) Uani 1 1 d . . . N2 N 0.8342(3) 0.4853(2) 1.03027(15) 0.0226(7) Uani 1 1 d . . . N4 N 1.0076(4) 0.3475(2) 0.98922(14) 0.0233(7) Uani 1 1 d . . . N1 N 1.1624(3) 0.4780(2) 0.91976(15) 0.0218(7) Uani 1 1 d . . . N3 N 0.8825(3) 0.4576(2) 0.89646(15) 0.0199(7) Uani 1 1 d . . . N5 N 1.1168(3) 0.4959(2) 1.05244(14) 0.0194(7) Uani 1 1 d . . . N6 N 0.9756(3) 0.6118(2) 0.96079(14) 0.0210(7) Uani 1 1 d . . . S2 S 0.64825(11) 0.50360(8) 1.12239(5) 0.0334(3) Uani 1 1 d . . . C2 C 0.7592(4) 0.4937(2) 1.06827(16) 0.0185(8) Uani 1 1 d . . . C22 C 0.8560(4) 0.6452(3) 0.95238(19) 0.0255(9) Uani 1 1 d . . . H22 H 0.7839 0.6075 0.9521 0.031 Uiso 1 1 calc R . . C16 C 1.1558(4) 0.5485(3) 1.15392(18) 0.0223(8) Uani 1 1 d . . . H15 H 1.1333 0.5879 1.1850 0.027 Uiso 1 1 calc R . . C17 C 1.0885(4) 0.5476(2) 1.09956(17) 0.0201(8) Uani 1 1 d . . . H16 H 1.0176 0.5858 1.0950 0.024 Uiso 1 1 calc R . . S1 S 1.36260(12) 0.44261(10) 0.83661(5) 0.0431(3) Uani 1 1 d . . . C3 C 0.9038(4) 0.5004(3) 0.84393(17) 0.0232(8) Uani 1 1 d . . . H1 H 0.9721 0.5410 0.8433 0.028 Uiso 1 1 calc R . . C15 C 1.2573(4) 0.4911(3) 1.16320(17) 0.0201(8) Uani 1 1 d . . . C4 C 0.8323(4) 0.4888(3) 0.79099(19) 0.0331(10) Uani 1 1 d . . . H2 H 0.8513 0.5208 0.7553 0.040 Uiso 1 1 calc R . . C19 C 1.0595(5) 0.7538(3) 0.9532(2) 0.0302(10) Uani 1 1 d . . . H20 H 1.1331 0.7902 0.9537 0.036 Uiso 1 1 calc R . . C18 C 1.0750(4) 0.6676(3) 0.96046(18) 0.0249(9) Uani 1 1 d . . . H19 H 1.1609 0.6464 0.9655 0.030 Uiso 1 1 calc R . . C7 C 0.7852(4) 0.4002(3) 0.89534(18) 0.0221(8) Uani 1 1 d . . . H4 H 0.7680 0.3693 0.9317 0.027 Uiso 1 1 calc R . . C1 C 1.2438(4) 0.4639(2) 0.88534(17) 0.0204(8) Uani 1 1 d . . . C8 C 1.0513(4) 0.2927(3) 0.94631(19) 0.0227(8) Uani 1 1 d . . . H7 H 1.0817 0.3156 0.9088 0.027 Uiso 1 1 calc R . . C6 C 0.7094(4) 0.3838(3) 0.84513(19) 0.0256(9) Uani 1 1 d . . . H3 H 0.6428 0.3421 0.8470 0.031 Uiso 1 1 calc R . . N9 N 1.3268(3) 0.4885(3) 1.21658(15) 0.0269(8) Uani 1 1 d . . . H18 H 1.3079 0.5237 1.2465 0.032 Uiso 1 1 calc R . . H17 H 1.3903 0.4515 1.2210 0.032 Uiso 1 1 calc R . . C10 C 1.0088(4) 0.1704(2) 1.00782(16) 0.0202(7) Uani 1 1 d . . . N7 N 0.6575(4) 0.4156(3) 0.74019(18) 0.0457(12) Uani 1 1 d . . . H6 H 0.6725 0.4445 0.7066 0.055 Uiso 1 1 calc R . . H5 H 0.5945 0.3778 0.7411 0.055 Uiso 1 1 calc R . . C21 C 0.8314(4) 0.7297(3) 0.9443(2) 0.0270(9) Uani 1 1 d . . . H21 H 0.7447 0.7490 0.9382 0.032 Uiso 1 1 calc R . . C14 C 1.2900(4) 0.4376(3) 1.11391(18) 0.0207(8) Uani 1 1 d . . . H14 H 1.3601 0.3986 1.1174 0.025 Uiso 1 1 calc R . . C11 C 0.9628(4) 0.2273(3) 1.05295(18) 0.0235(9) Uani 1 1 d . . . H9 H 0.9305 0.2066 1.0908 0.028 Uiso 1 1 calc R . . C5 C 0.7317(4) 0.4293(3) 0.79086(19) 0.0301(10) Uani 1 1 d . . . C13 C 1.2193(4) 0.4426(3) 1.06096(18) 0.0200(8) Uani 1 1 d . . . H13 H 1.2433 0.4065 1.0281 0.024 Uiso 1 1 calc R . . C12 C 0.9653(4) 0.3124(3) 1.04132(19) 0.0240(9) Uani 1 1 d . . . H10 H 0.9349 0.3494 1.0725 0.029 Uiso 1 1 calc R . . C9 C 1.0549(4) 0.2070(3) 0.95333(19) 0.0240(9) Uani 1 1 d . . . H8 H 1.0882 0.1721 0.9216 0.029 Uiso 1 1 calc R . . S5 S 0.4942(3) 0.19010(12) 0.69129(11) 0.0525(7) Uani 0.677(4) 1 d P A 1 N8 N 1.0072(4) 0.0853(2) 1.01719(15) 0.0248(7) Uani 1 1 d . . . H11 H 1.0357 0.0508 0.9886 0.030 Uiso 1 1 calc R . . H12 H 0.9776 0.0647 1.0519 0.030 Uiso 1 1 calc R . . N10 N 0.9149(4) 0.8720(3) 0.9399(2) 0.0430(11) Uani 1 1 d . . . H24 H 0.8355 0.8922 0.9360 0.052 Uiso 1 1 calc R . . H23 H 0.9819 0.9068 0.9406 0.052 Uiso 1 1 calc R . . C20 C 0.9343(5) 0.7869(3) 0.9450(2) 0.0282(10) Uani 1 1 d . . . S3 S 1.0036(5) 0.7214(2) 0.78105(16) 0.0463(11) Uani 0.365(4) 1 d P B 4 C26 C 0.9934(10) 0.8132(5) 0.7882(4) 0.0462(19) Uiso 0.635(4) 1 d P B 3 S4 S 0.9879(2) 0.74663(13) 0.72263(8) 0.0381(6) Uani 0.635(4) 1 d P B 3 O2A O 0.4797(7) 0.2795(4) 0.7094(3) 0.0505(15) Uiso 0.677(4) 1 d P A 1 S6 S 0.3765(4) 0.2269(3) 0.7289(3) 0.0505(14) Uani 0.323(4) 1 d P A 2 O1A O 0.9885(11) 0.6509(6) 0.7385(4) 0.035(2) Uiso 0.365(4) 1 d P B 4 C25 C 0.8174(10) 0.7311(7) 0.7188(5) 0.059(3) Uiso 0.635(4) 1 d P B 3 C24 C 1.1842(17) 0.7300(12) 0.7891(8) 0.057(4) Uiso 0.365(4) 1 d P B 4 C27 C 0.5221(14) 0.1291(8) 0.7579(6) 0.088(4) Uiso 0.677(4) 1 d P A 1 O2B O 0.4975(13) 0.2744(6) 0.7373(5) 0.031(2) Uiso 0.323(4) 1 d P A 2 C23 C 0.9777(17) 0.8192(10) 0.7384(8) 0.053(4) Uiso 0.365(4) 1 d P B 4 C28 C 0.6525(15) 0.1869(10) 0.6554(7) 0.106(5) Uiso 0.677(4) 1 d P A 1 O1B O 1.0440(9) 0.6628(6) 0.7429(4) 0.070(2) Uiso 0.635(4) 1 d P B 3 C29 C 0.404(3) 0.1403(17) 0.6749(12) 0.080(7) Uiso 0.323(4) 1 d P A 2 C30 C 0.353(2) 0.1649(14) 0.7943(10) 0.062(5) Uiso 0.323(4) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0176(2) 0.0221(2) 0.0157(2) 0.00060(18) 0.0018(2) 0.0029(2) N2 0.0208(15) 0.0250(17) 0.0220(15) -0.0020(16) 0.0010(13) 0.0033(15) N4 0.0243(16) 0.0268(16) 0.0189(15) -0.0006(12) -0.0028(15) -0.0002(17) N1 0.0213(16) 0.0230(17) 0.0212(16) 0.0004(14) 0.0034(13) -0.0004(15) N3 0.0185(16) 0.0205(17) 0.0207(16) 0.0010(13) 0.0013(13) 0.0001(13) N5 0.0208(16) 0.0189(17) 0.0186(14) -0.0015(13) 0.0017(12) 0.0036(13) N6 0.0212(18) 0.0233(16) 0.0186(15) 0.0010(12) 0.0001(13) 0.0022(13) S2 0.0283(5) 0.0455(7) 0.0263(5) -0.0104(5) 0.0107(4) -0.0049(5) C2 0.0237(18) 0.0150(18) 0.0167(17) 0.0003(15) -0.0039(15) -0.0002(15) C22 0.021(2) 0.025(2) 0.030(2) 0.0060(17) 0.0026(17) 0.0003(17) C16 0.025(2) 0.020(2) 0.0210(19) -0.0035(16) 0.0052(16) 0.0018(17) C17 0.0236(19) 0.0184(19) 0.0183(18) 0.0021(15) 0.0057(15) 0.0030(16) S1 0.0300(6) 0.0763(10) 0.0230(5) 0.0128(6) 0.0102(5) 0.0223(6) C3 0.0249(19) 0.025(2) 0.0201(18) 0.0017(16) 0.0014(15) -0.0060(16) C15 0.0207(17) 0.0188(19) 0.0208(18) 0.0019(15) -0.0005(14) -0.0044(16) C4 0.032(2) 0.046(3) 0.021(2) 0.010(2) -0.0027(16) -0.013(2) C19 0.032(2) 0.028(2) 0.030(2) 0.0045(19) -0.0054(19) -0.003(2) C18 0.025(2) 0.029(2) 0.020(2) 0.0003(16) -0.0052(17) 0.0043(18) C7 0.0183(19) 0.027(2) 0.0207(19) 0.0029(16) 0.0057(15) -0.0018(16) C1 0.0240(19) 0.019(2) 0.0184(18) 0.0056(15) -0.0018(16) 0.0032(15) C8 0.0230(19) 0.024(2) 0.0206(19) -0.0006(16) 0.0004(16) 0.0002(17) C6 0.0166(18) 0.036(2) 0.024(2) -0.0002(18) 0.0015(16) -0.0050(17) N9 0.0275(18) 0.033(2) 0.0198(16) -0.0037(16) -0.0044(13) 0.0067(16) C10 0.0150(17) 0.0230(18) 0.0225(17) -0.0007(13) -0.0052(17) 0.0016(18) N7 0.043(2) 0.068(3) 0.026(2) 0.009(2) -0.0107(18) -0.031(2) C21 0.026(2) 0.028(2) 0.027(2) 0.0070(18) 0.0019(17) 0.0092(18) C14 0.0176(18) 0.022(2) 0.0230(19) -0.0001(16) 0.0040(15) 0.0001(16) C11 0.027(2) 0.025(2) 0.0186(18) 0.0039(16) -0.0004(15) 0.0007(16) C5 0.024(2) 0.044(3) 0.022(2) 0.0011(19) -0.0042(17) -0.008(2) C13 0.0204(19) 0.0189(19) 0.0208(19) -0.0033(16) 0.0057(15) 0.0036(16) C12 0.025(2) 0.023(2) 0.023(2) 0.0002(15) -0.0013(15) 0.0049(15) C9 0.026(2) 0.023(2) 0.023(2) -0.0081(16) -0.0005(17) 0.0008(17) S5 0.0493(12) 0.0285(10) 0.0797(15) 0.0039(9) 0.0038(13) -0.0038(11) N8 0.0243(16) 0.0238(15) 0.0264(16) -0.0019(12) 0.0028(17) -0.0017(17) N10 0.043(2) 0.024(2) 0.062(3) 0.009(2) -0.010(2) 0.0056(19) C20 0.043(3) 0.019(2) 0.023(2) 0.0025(17) -0.0047(19) 0.0059(19) S3 0.055(2) 0.046(2) 0.0382(19) -0.0029(14) 0.014(2) -0.010(2) S4 0.0435(12) 0.0437(11) 0.0271(9) -0.0045(7) 0.0082(9) 0.0083(10) S6 0.034(2) 0.034(2) 0.083(4) 0.005(2) 0.000(2) -0.0076(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 Ni1 N1 2.068(3) . ? Ni1 N2 2.081(3) . ? Ni1 N3 2.100(3) . ? Ni1 N4 2.116(3) . ? Ni1 N6 2.117(3) . ? Ni1 N5 2.121(3) . ? N2 C2 1.141(5) . ? N4 C12 1.339(5) . ? N4 C8 1.353(5) . ? N1 C1 1.147(5) . ? N3 C7 1.349(5) . ? N3 C3 1.351(5) . ? N5 C17 1.347(5) . ? N5 C13 1.360(5) . ? N6 C22 1.349(5) . ? N6 C18 1.349(5) . ? S2 C2 1.650(4) . ? C22 C21 1.369(6) . ? C16 C17 1.376(6) . ? C16 C15 1.395(6) . ? S1 C1 1.654(4) . ? C3 C4 1.384(6) . ? C15 N9 1.369(5) . ? C15 C14 1.411(5) . ? C4 C5 1.396(6) . ? C19 C18 1.378(6) . ? C19 C20 1.399(6) . ? C7 C6 1.371(6) . ? C8 C9 1.364(6) . ? C6 C5 1.407(6) . ? C10 N8 1.359(5) . ? C10 C9 1.407(6) . ? C10 C11 1.416(5) . ? N7 C5 1.363(6) . ? C21 C20 1.390(7) . ? C14 C13 1.369(6) . ? C11 C12 1.369(6) . ? S5 O2A 1.473(6) . ? S5 C27 1.771(13) . ? S5 C28 1.806(16) . ? N10 C20 1.364(6) . ? S3 O1A 1.459(11) . ? S3 C23 1.824(17) . ? S3 C24 1.867(19) . ? C26 S4 1.780(8) . ? S4 O1B 1.510(9) . ? S4 C25 1.770(11) . ? S6 O2B 1.463(13) . ? S6 C30 1.75(2) . ? S6 C29 1.83(3) . ? 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 N1 Ni1 N2 178.04(15) . . ? N1 Ni1 N3 89.54(14) . . ? N2 Ni1 N3 91.80(13) . . ? N1 Ni1 N4 92.12(14) . . ? N2 Ni1 N4 89.34(14) . . ? N3 Ni1 N4 89.39(13) . . ? N1 Ni1 N6 91.21(13) . . ? N2 Ni1 N6 87.36(13) . . ? N3 Ni1 N6 89.54(13) . . ? N4 Ni1 N6 176.49(15) . . ? N1 Ni1 N5 89.70(13) . . ? N2 Ni1 N5 89.03(13) . . ? N3 Ni1 N5 177.26(13) . . ? N4 Ni1 N5 88.01(13) . . ? N6 Ni1 N5 93.11(13) . . ? C2 N2 Ni1 168.3(3) . . ? C12 N4 C8 115.8(3) . . ? C12 N4 Ni1 121.6(3) . . ? C8 N4 Ni1 122.6(3) . . ? C1 N1 Ni1 167.5(3) . . ? C7 N3 C3 116.1(3) . . ? C7 N3 Ni1 122.9(3) . . ? C3 N3 Ni1 121.0(3) . . ? C17 N5 C13 115.9(3) . . ? C17 N5 Ni1 124.5(3) . . ? C13 N5 Ni1 118.8(3) . . ? C22 N6 C18 115.6(4) . . ? C22 N6 Ni1 120.1(3) . . ? C18 N6 Ni1 124.3(3) . . ? N2 C2 S2 178.4(4) . . ? N6 C22 C21 124.6(4) . . ? C17 C16 C15 119.7(4) . . ? N5 C17 C16 124.0(4) . . ? N3 C3 C4 124.1(4) . . ? N9 C15 C16 122.2(4) . . ? N9 C15 C14 120.7(4) . . ? C16 C15 C14 117.1(3) . . ? C3 C4 C5 118.9(4) . . ? C18 C19 C20 119.3(4) . . ? N6 C18 C19 123.9(4) . . ? N3 C7 C6 124.2(4) . . ? N1 C1 S1 179.0(4) . . ? N4 C8 C9 124.4(4) . . ? C7 C6 C5 119.2(4) . . ? N8 C10 C9 122.5(4) . . ? N8 C10 C11 121.2(4) . . ? C9 C10 C11 116.3(4) . . ? C22 C21 C20 119.4(4) . . ? C13 C14 C15 119.1(4) . . ? C12 C11 C10 119.1(4) . . ? N7 C5 C4 121.5(4) . . ? N7 C5 C6 121.0(4) . . ? C4 C5 C6 117.5(4) . . ? N5 C13 C14 124.2(4) . . ? N4 C12 C11 124.8(4) . . ? C8 C9 C10 119.6(4) . . ? O2A S5 C27 108.5(5) . . ? O2A S5 C28 103.6(6) . . ? C27 S5 C28 101.4(7) . . ? N10 C20 C21 122.0(4) . . ? N10 C20 C19 120.8(4) . . ? C21 C20 C19 117.2(4) . . ? O1A S3 C23 107.7(7) . . ? O1A S3 C24 102.8(8) . . ? C23 S3 C24 97.6(8) . . ? O1B S4 C25 105.7(5) . . ? O1B S4 C26 105.6(4) . . ? C25 S4 C26 98.7(5) . . ? O2B S6 C30 107.6(9) . . ? O2B S6 C29 109.6(10) . . ? C30 S6 C29 97.6(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 N2 C2 -35(5) . . . . ? N3 Ni1 N2 C2 -167.8(17) . . . . ? N4 Ni1 N2 C2 102.8(17) . . . . ? N6 Ni1 N2 C2 -78.4(17) . . . . ? N5 Ni1 N2 C2 14.8(17) . . . . ? N1 Ni1 N4 C12 149.1(3) . . . . ? N2 Ni1 N4 C12 -29.6(3) . . . . ? N3 Ni1 N4 C12 -121.4(3) . . . . ? N6 Ni1 N4 C12 -49(2) . . . . ? N5 Ni1 N4 C12 59.4(3) . . . . ? N1 Ni1 N4 C8 -33.9(3) . . . . ? N2 Ni1 N4 C8 147.4(3) . . . . ? N3 Ni1 N4 C8 55.6(3) . . . . ? N6 Ni1 N4 C8 128(2) . . . . ? N5 Ni1 N4 C8 -123.5(3) . . . . ? N2 Ni1 N1 C1 180(100) . . . . ? N3 Ni1 N1 C1 -47.4(15) . . . . ? N4 Ni1 N1 C1 42.0(15) . . . . ? N6 Ni1 N1 C1 -136.9(15) . . . . ? N5 Ni1 N1 C1 130.0(15) . . . . ? N1 Ni1 N3 C7 134.7(3) . . . . ? N2 Ni1 N3 C7 -46.7(3) . . . . ? N4 Ni1 N3 C7 42.6(3) . . . . ? N6 Ni1 N3 C7 -134.1(3) . . . . ? N5 Ni1 N3 C7 61(3) . . . . ? N1 Ni1 N3 C3 -44.6(3) . . . . ? N2 Ni1 N3 C3 134.0(3) . . . . ? N4 Ni1 N3 C3 -136.7(3) . . . . ? N6 Ni1 N3 C3 46.7(3) . . . . ? N5 Ni1 N3 C3 -119(3) . . . . ? N1 Ni1 N5 C17 139.7(3) . . . . ? N2 Ni1 N5 C17 -38.8(3) . . . . ? N3 Ni1 N5 C17 -146(3) . . . . ? N4 Ni1 N5 C17 -128.2(3) . . . . ? N6 Ni1 N5 C17 48.5(3) . . . . ? N1 Ni1 N5 C13 -50.3(3) . . . . ? N2 Ni1 N5 C13 131.2(3) . . . . ? N3 Ni1 N5 C13 24(3) . . . . ? N4 Ni1 N5 C13 41.8(3) . . . . ? N6 Ni1 N5 C13 -141.5(3) . . . . ? N1 Ni1 N6 C22 139.8(3) . . . . ? N2 Ni1 N6 C22 -41.6(3) . . . . ? N3 Ni1 N6 C22 50.2(3) . . . . ? N4 Ni1 N6 C22 -22(2) . . . . ? N5 Ni1 N6 C22 -130.5(3) . . . . ? N1 Ni1 N6 C18 -40.8(3) . . . . ? N2 Ni1 N6 C18 137.8(3) . . . . ? N3 Ni1 N6 C18 -130.4(3) . . . . ? N4 Ni1 N6 C18 157.5(19) . . . . ? N5 Ni1 N6 C18 48.9(3) . . . . ? Ni1 N2 C2 S2 -151(13) . . . . ? C18 N6 C22 C21 -0.5(6) . . . . ? Ni1 N6 C22 C21 179.0(3) . . . . ? C13 N5 C17 C16 -0.3(6) . . . . ? Ni1 N5 C17 C16 169.9(3) . . . . ? C15 C16 C17 N5 -2.3(6) . . . . ? C7 N3 C3 C4 0.4(6) . . . . ? Ni1 N3 C3 C4 179.7(4) . . . . ? C17 C16 C15 N9 -179.3(4) . . . . ? C17 C16 C15 C14 3.3(6) . . . . ? N3 C3 C4 C5 -0.2(7) . . . . ? C22 N6 C18 C19 1.1(6) . . . . ? Ni1 N6 C18 C19 -178.4(3) . . . . ? C20 C19 C18 N6 -0.6(7) . . . . ? C3 N3 C7 C6 0.1(6) . . . . ? Ni1 N3 C7 C6 -179.2(3) . . . . ? Ni1 N1 C1 S1 -92(26) . . . . ? C12 N4 C8 C9 -0.3(6) . . . . ? Ni1 N4 C8 C9 -177.5(3) . . . . ? N3 C7 C6 C5 -0.7(7) . . . . ? N6 C22 C21 C20 -0.6(7) . . . . ? N9 C15 C14 C13 -179.3(4) . . . . ? C16 C15 C14 C13 -1.9(6) . . . . ? N8 C10 C11 C12 -179.5(4) . . . . ? C9 C10 C11 C12 0.1(6) . . . . ? C3 C4 C5 N7 179.6(5) . . . . ? C3 C4 C5 C6 -0.4(7) . . . . ? C7 C6 C5 N7 -179.2(5) . . . . ? C7 C6 C5 C4 0.8(7) . . . . ? C17 N5 C13 C14 1.8(6) . . . . ? Ni1 N5 C13 C14 -169.0(3) . . . . ? C15 C14 C13 N5 -0.7(6) . . . . ? C8 N4 C12 C11 -0.7(6) . . . . ? Ni1 N4 C12 C11 176.6(3) . . . . ? C10 C11 C12 N4 0.7(6) . . . . ? N4 C8 C9 C10 1.1(7) . . . . ? N8 C10 C9 C8 178.7(4) . . . . ? C11 C10 C9 C8 -1.0(6) . . . . ? C22 C21 C20 N10 -177.0(4) . . . . ? C22 C21 C20 C19 1.1(7) . . . . ? C18 C19 C20 N10 177.6(4) . . . . ? C18 C19 C20 C21 -0.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.809 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.081 #===END