Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global _publ_contact_author_name 'Dr Andrew D Bond' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK ; _publ_contact_author_email 'adb29@cam.ac.uk' _publ_contact_author_fax '(01223) 336362' _publ_contact_author_phone '(01223) 336352' _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bond, Andrew D.' 'Jones, W.' _publ_section_title ; Divalent complexes of 3-hydroxy-4-methyl-2(3H)-thiazolethione with Co-Zn: synthesis, X-ray crystal structures and the structure-directing influence of C-H...S interactions ; data_1 _database_code_CSD 168626 _audit_creation_method 'SHELXL-97 plus manual editing' _chemical_name_systematic ; bis(3-hydroxy-4-methyl-2(3H)-thiazolethiolato-S,O)zinc(II) ; _chemical_name_common Zn(MTT)2 _chemical_formula_moiety 'C8 H8 N2 O2 S4 Zn' _chemical_formula_sum 'C8 H8 N2 O2 S4 Zn' _chemical_formula_weight 357.77 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6216(4) _cell_length_b 7.6954(4) _cell_length_c 11.7788(6) _cell_angle_alpha 105.147(3) _cell_angle_beta 96.210(3) _cell_angle_gamma 106.593(3) _cell_volume 626.47(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3011 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 2.614 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Hydrogens placed geometrically and allowed to ride during refinement. ; _diffrn_ambient_temperature 180(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 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 3892 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_full 0.982 _reflns_number_total 2798 _reflns_number_gt 2352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0271P)^2^+0.1537P] 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 2798 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 0.325 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.092 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 Zn1 Zn 0.12600(4) 0.46852(4) 0.74890(2) 0.02251(10) Uani 1 1 d . . . S1 S 0.28983(9) 0.76183(8) 0.88440(6) 0.02538(16) Uani 1 1 d . . . S2 S 0.44855(9) 0.77601(9) 1.13737(5) 0.02554(16) Uani 1 1 d . . . S3 S -0.15462(9) 0.35824(9) 0.61646(6) 0.02539(16) Uani 1 1 d . . . S4 S -0.17824(9) 0.10187(9) 0.36607(5) 0.02526(16) Uani 1 1 d . . . O1 O 0.1326(2) 0.3483(2) 0.87923(14) 0.0248(4) Uani 1 1 d . . . O2 O 0.2499(2) 0.3745(2) 0.61690(14) 0.0249(4) Uani 1 1 d . . . N1 N 0.2414(3) 0.4745(3) 0.98178(17) 0.0187(4) Uani 1 1 d . . . N2 N 0.1223(3) 0.2684(3) 0.51571(16) 0.0183(4) Uani 1 1 d . . . C1 C 0.3169(3) 0.6607(3) 0.9959(2) 0.0193(5) Uani 1 1 d . . . C2 C 0.3982(3) 0.5652(3) 1.1728(2) 0.0231(5) Uani 1 1 d . . . H2 H 0.4449 0.5551 1.2481 0.028 Uiso 1 1 calc R . . C3 C 0.2851(3) 0.4176(3) 1.0811(2) 0.0205(5) Uani 1 1 d . . . C4 C 0.2058(4) 0.2136(3) 1.0736(2) 0.0283(6) Uani 1 1 d . . . H4A H 0.2557 0.1944 1.1480 0.034 Uiso 1 1 calc R . . H4B H 0.2400 0.1346 1.0056 0.034 Uiso 1 1 calc R . . H4C H 0.0694 0.1772 1.0624 0.034 Uiso 1 1 calc R . . C5 C -0.0579(3) 0.2519(3) 0.5055(2) 0.0207(5) Uani 1 1 d . . . C6 C 0.0237(3) 0.0687(3) 0.3260(2) 0.0239(5) Uani 1 1 d . . . H6 H 0.0286 -0.0102 0.2503 0.029 Uiso 1 1 calc R . . C7 C 0.1734(3) 0.1680(3) 0.4150(2) 0.0215(5) Uani 1 1 d . . . C8 C 0.3729(4) 0.1830(4) 0.4183(2) 0.0308(6) Uani 1 1 d . . . H8A H 0.3849 0.0995 0.3431 0.037 Uiso 1 1 calc R . . H8B H 0.4181 0.1444 0.4858 0.037 Uiso 1 1 calc R . . H8C H 0.4470 0.3150 0.4283 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 Zn1 0.02407(18) 0.02529(17) 0.01467(17) 0.00142(13) -0.00069(13) 0.00875(13) S1 0.0338(4) 0.0196(3) 0.0207(3) 0.0044(3) -0.0007(3) 0.0095(3) S2 0.0280(4) 0.0234(3) 0.0164(3) -0.0015(3) -0.0015(3) 0.0043(3) S3 0.0200(3) 0.0344(4) 0.0202(3) 0.0033(3) 0.0012(3) 0.0122(3) S4 0.0220(3) 0.0294(3) 0.0164(3) 0.0031(3) -0.0038(3) 0.0028(3) O1 0.0285(10) 0.0204(8) 0.0153(9) -0.0006(7) -0.0062(7) 0.0021(7) O2 0.0190(9) 0.0326(9) 0.0137(9) -0.0034(7) -0.0034(7) 0.0063(8) N1 0.0189(11) 0.0196(10) 0.0152(10) 0.0020(8) 0.0033(8) 0.0060(8) N2 0.0176(11) 0.0212(10) 0.0135(10) 0.0020(8) 0.0012(8) 0.0063(8) C1 0.0193(13) 0.0197(12) 0.0146(12) -0.0008(9) 0.0003(10) 0.0067(10) C2 0.0230(13) 0.0313(13) 0.0164(12) 0.0068(11) 0.0051(10) 0.0108(11) C3 0.0180(12) 0.0282(13) 0.0182(12) 0.0088(11) 0.0066(10) 0.0091(10) C4 0.0298(15) 0.0286(14) 0.0281(15) 0.0136(12) 0.0065(12) 0.0073(12) C5 0.0214(13) 0.0238(12) 0.0145(12) 0.0053(10) -0.0002(10) 0.0054(10) C6 0.0301(15) 0.0220(12) 0.0157(12) 0.0030(10) 0.0056(11) 0.0051(11) C7 0.0251(14) 0.0218(12) 0.0171(12) 0.0041(10) 0.0054(10) 0.0083(10) C8 0.0259(15) 0.0350(15) 0.0277(15) 0.0021(12) 0.0084(12) 0.0100(12) _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 Zn1 O2 1.9883(17) . ? Zn1 O1 1.9917(15) . ? Zn1 S1 2.2973(7) . ? Zn1 S3 2.2973(7) . ? S1 C1 1.716(2) . ? S2 C1 1.711(2) . ? S2 C2 1.728(2) . ? S3 C5 1.707(3) . ? S4 C5 1.718(2) . ? S4 C6 1.725(3) . ? O1 N1 1.342(2) . ? O2 N2 1.349(2) . ? N1 C1 1.340(3) . ? N1 C3 1.392(3) . ? N2 C5 1.332(3) . ? N2 C7 1.396(3) . ? C2 C3 1.340(3) . ? C2 H2 0.9500 . ? C3 C4 1.488(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.345(3) . ? C6 H6 0.9500 . ? C7 C8 1.487(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 114.53(7) . . ? O2 Zn1 S1 116.25(5) . . ? O1 Zn1 S1 90.16(5) . . ? O2 Zn1 S3 90.43(5) . . ? O1 Zn1 S3 115.13(5) . . ? S1 Zn1 S3 132.14(3) . . ? C1 S1 Zn1 91.14(8) . . ? C1 S2 C2 91.26(11) . . ? C5 S3 Zn1 90.48(8) . . ? C5 S4 C6 91.42(12) . . ? N1 O1 Zn1 111.09(12) . . ? N2 O2 Zn1 110.64(13) . . ? C1 N1 O1 123.28(18) . . ? C1 N1 C3 115.5(2) . . ? O1 N1 C3 121.26(18) . . ? C5 N2 O2 122.74(19) . . ? C5 N2 C7 116.1(2) . . ? O2 N2 C7 121.15(19) . . ? N1 C1 S2 110.08(16) . . ? N1 C1 S1 123.76(18) . . ? S2 C1 S1 126.12(13) . . ? C3 C2 S2 111.76(18) . . ? C3 C2 H2 124.1 . . ? S2 C2 H2 124.1 . . ? C2 C3 N1 111.4(2) . . ? C2 C3 C4 129.5(2) . . ? N1 C3 C4 119.1(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 S3 124.88(18) . . ? N2 C5 S4 109.69(18) . . ? S3 C5 S4 125.40(15) . . ? C7 C6 S4 111.77(19) . . ? C7 C6 H6 124.1 . . ? S4 C6 H6 124.1 . . ? C6 C7 N2 111.0(2) . . ? C6 C7 C8 129.7(2) . . ? N2 C7 C8 119.3(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 O2 Zn1 S1 C1 -112.48(10) . . . . ? O1 Zn1 S1 C1 5.19(9) . . . . ? S3 Zn1 S1 C1 130.31(8) . . . . ? O2 Zn1 S3 C5 6.67(9) . . . . ? O1 Zn1 S3 C5 -110.85(9) . . . . ? S1 Zn1 S3 C5 133.77(8) . . . . ? O2 Zn1 O1 N1 112.06(14) . . . . ? S1 Zn1 O1 N1 -7.11(13) . . . . ? S3 Zn1 O1 N1 -145.05(12) . . . . ? O1 Zn1 O2 N2 109.60(13) . . . . ? S1 Zn1 O2 N2 -147.18(11) . . . . ? S3 Zn1 O2 N2 -8.44(12) . . . . ? Zn1 O1 N1 C1 6.9(3) . . . . ? Zn1 O1 N1 C3 -172.19(16) . . . . ? Zn1 O2 N2 C5 7.4(2) . . . . ? Zn1 O2 N2 C7 -172.25(15) . . . . ? O1 N1 C1 S2 -179.33(16) . . . . ? C3 N1 C1 S2 -0.2(3) . . . . ? O1 N1 C1 S1 -1.7(3) . . . . ? C3 N1 C1 S1 177.49(17) . . . . ? C2 S2 C1 N1 0.52(19) . . . . ? C2 S2 C1 S1 -177.04(17) . . . . ? Zn1 S1 C1 N1 -3.6(2) . . . . ? Zn1 S1 C1 S2 173.66(16) . . . . ? C1 S2 C2 C3 -0.8(2) . . . . ? S2 C2 C3 N1 0.8(3) . . . . ? S2 C2 C3 C4 -179.1(2) . . . . ? C1 N1 C3 C2 -0.5(3) . . . . ? O1 N1 C3 C2 178.7(2) . . . . ? C1 N1 C3 C4 179.4(2) . . . . ? O1 N1 C3 C4 -1.4(3) . . . . ? O2 N2 C5 S3 -0.5(3) . . . . ? C7 N2 C5 S3 179.20(16) . . . . ? O2 N2 C5 S4 -178.59(14) . . . . ? C7 N2 C5 S4 1.1(2) . . . . ? Zn1 S3 C5 N2 -5.42(19) . . . . ? Zn1 S3 C5 S4 172.37(14) . . . . ? C6 S4 C5 N2 -0.52(17) . . . . ? C6 S4 C5 S3 -178.60(15) . . . . ? C5 S4 C6 C7 -0.17(18) . . . . ? S4 C6 C7 N2 0.8(2) . . . . ? S4 C6 C7 C8 -178.9(2) . . . . ? C5 N2 C7 C6 -1.3(3) . . . . ? O2 N2 C7 C6 178.44(18) . . . . ? C5 N2 C7 C8 178.5(2) . . . . ? O2 N2 C7 C8 -1.8(3) . . . . ? #===END data_2 _database_code_CSD 168627 _audit_creation_method 'GSAS plus manual editing' _chemical_name_systematic ; bis(3-hydroxy-4-methyl-2(3H)-thiazolethiolato-S,O)copper(II) ; _chemical_name_common Cu(MTT)2 _chemical_formula_moiety '(C4 H4 N O S2)2 Cu' _chemical_formula_sum 'C8 H8 Cu1 N2 O2 S4' _chemical_formula_weight 355.94 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,+y+1/2,-z+1/2' '-x,-y,-z' '-1/2+x,-y-1/2,+z-1/2' _cell_length_a 4.0859(2) _cell_length_b 12.7571(8) _cell_length_c 11.9876(7) _cell_angle_alpha 90.0 _cell_angle_beta 97.010(7) _cell_angle_gamma 90.0 _cell_volume 620.2(1) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) loop_ _atom_type_symbol _atom_type_number_in_cell CU 2.0 S 8.0 O 4.0 N 4.0 C 16.0 H 16.0 _diffrn_ambient_temperature 298(2) _diffrn_radiation_type Cu-Ka _diffrn_measurement_device_type 'Stoe STADI-P' _diffrn_detector PSD _diffrn_radiation_polarisn_ratio 0.5 _diffrn_radiation_wavelength 1.5406 _diffrn_radiation_monochromator Ge(111) _pd_meas_number_of_points 5699 _pd_proc_number_of_points 5699 _pd_meas_2theta_range_min 8.01 _pd_meas_2theta_range_max 64.99 _pd_meas_2theta_range_inc 0.01 _pd_proc_2theta_range_min 8.01 _pd_proc_2theta_range_max 64.99 _pd_proc_2theta_range_inc 0.01 _pd_proc_ls_profile_function 'pseudo-voigt (Thompson et al.)' _pd_proc_ls_background_function 'linear interpolation (10 terms)' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.044 _pd_proc_ls_prof_wR_factor 0.057 _pd_proc_ls_prof_wR_expected 0.021 _refine_ls_number_parameters 22 _refine_ls_goodness_of_fit_all 2.76 _refine_special_details ; Molecules constrained as rigid bodies, allowed to rotate about Cu positions ; _computing_data_collection 'Stoe WinXpow' _computing_cell_refinement 'GSAS' _computing_structure_solution 'Cerius2' _computing_structure_refinement 'GSAS' _computing_molecular_graphics 'GSAS' _computing_publication_material 'GSAS' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv CU1 CU 0.5000(0) 0.5000(0) 0.5000(0) 0.5 Uiso 0.0269(11) S1 S 0.6726(5) 0.4548(1) 0.6978(1) 1.0 Uiso 0.0269(11) S2 S 1.1000(6) 0.6077(2) 0.8453(1) 1.0 Uiso 0.0269(11) O1 O 0.8143(6) 0.6245(1) 0.5307(1) 1.0 Uiso 0.0269(11) N1 N 0.9386(5) 0.6375(1) 0.6395(1) 1.0 Uiso 0.0269(11) C1 C 0.8922(5) 0.5676(1) 0.7194(1) 1.0 Uiso 0.0269(11) C2 C 1.2427(5) 0.7185(2) 0.7844(2) 1.0 Uiso 0.0269(11) H2 H 1.3804(5) 0.7695(2) 0.8241(2) 1.0 Uiso 0.0269(11) C3 C 1.1364(6) 0.7238(2) 0.6746(2) 1.0 Uiso 0.0269(11) C4 C 1.2050(9) 0.8050(2) 0.5916(2) 1.0 Uiso 0.0269(11) H4A H 1.3725(9) 0.8536(2) 0.6267(2) 1.0 Uiso 0.0269(11) H4B H 1.2857(9) 0.7712(1) 0.5268(2) 1.0 Uiso 0.0269(11) H4C H 1.0019(8) 0.8436(2) 0.5667(2) 1.0 Uiso 0.0269(11) data_5 _database_code_CSD 168628 _audit_creation_method 'SHELXL-97 plus manual editing' _chemical_name_systematic ; bis(3-hydroxy-4-methyl-2(3H)-thiazolethiolato-S,O)nickel(II) ; _chemical_name_common Ni(MTT)2 _chemical_formula_moiety 'Ni3,6(C4 H4 N1 O1 S2)' _chemical_formula_sum 'C24 H24 N6 Ni3 O6 S12' _chemical_formula_weight 1053.34 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.067(5) _cell_length_b 10.167(8) _cell_length_c 11.184(4) _cell_angle_alpha 92.71(6) _cell_angle_beta 114.00(4) _cell_angle_gamma 112.92(5) _cell_volume 933.9(9) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 2.216 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details 'North, Phillips and Mathews (1968)' _exptl_special_details ; Hydrogens placed geometrically and allowed to ride during subsequent refinement. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R 4-circle diffractometer' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4505 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 4266 _reflns_number_gt 2796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractomer Control (1998)' _computing_cell_refinement 'MSC/AFC Diffractomer Control (1998)' _computing_data_reduction 'TeXsan (MSC, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0409P)^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_number_reflns 4266 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.707 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.145 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 0.51145(9) 0.58641(8) 0.76409(7) 0.01691(19) Uani 1 1 d . . . Ni2 Ni 0.5000 0.5000 0.5000 0.0153(2) Uani 1 2 d S . . S1 S 0.46179(18) 0.76928(17) 0.84658(15) 0.0233(3) Uani 1 1 d . . . S2 S 0.73504(19) 1.00454(17) 1.10754(15) 0.0232(3) Uani 1 1 d . . . S3 S 0.33334(18) 0.37587(17) 0.79486(14) 0.0215(3) Uani 1 1 d . . . S4 S -0.01311(19) 0.19700(18) 0.56962(16) 0.0267(4) Uani 1 1 d . . . S5 S 0.34706(18) 0.23926(16) 0.42186(14) 0.0207(3) Uani 1 1 d . . . S6 S 0.4323(2) 0.05060(16) 0.61559(16) 0.0247(3) Uani 1 1 d . . . O1 O 0.7379(5) 0.6966(4) 0.9027(4) 0.0189(9) Uani 1 1 d . . . O2 O 0.3380(5) 0.5300(4) 0.5691(4) 0.0184(8) Uani 1 1 d . . . O3 O 0.6049(5) 0.4695(4) 0.6857(4) 0.0164(8) Uani 1 1 d . . . N1 N 0.7664(6) 0.8133(5) 0.9886(4) 0.0153(10) Uani 1 1 d . . . N2 N 0.1959(6) 0.4148(5) 0.5459(5) 0.0173(10) Uani 1 1 d . . . N3 N 0.5644(5) 0.3254(5) 0.6868(4) 0.0145(9) Uani 1 1 d . . . C1 C 0.6545(7) 0.8554(6) 0.9764(5) 0.0164(11) Uani 1 1 d . . . C2 C 0.9215(7) 1.0019(7) 1.1733(6) 0.0220(13) Uani 1 1 d . . . H2 H 1.0146 1.0699 1.2524 0.026 Uiso 1 1 calc R . . C3 C 0.9198(7) 0.8929(6) 1.0999(5) 0.0173(12) Uani 1 1 d . . . C4 C 1.0511(7) 0.8486(7) 1.1222(6) 0.0286(15) Uani 1 1 d . . . H4A H 1.1533 0.9216 1.1976 0.034 Uiso 1 1 calc R . . H4B H 1.0645 0.8432 1.0403 0.034 Uiso 1 1 calc R . . H4C H 1.0220 0.7520 1.1433 0.034 Uiso 1 1 calc R . . C5 C 0.1829(7) 0.3369(7) 0.6368(6) 0.0217(13) Uani 1 1 d . . . C6 C -0.0693(8) 0.2577(7) 0.4238(6) 0.0270(14) Uani 1 1 d . . . H6 H -0.1764 0.2131 0.3509 0.032 Uiso 1 1 calc R . . C7 C 0.0526(7) 0.3731(7) 0.4242(6) 0.0208(13) Uani 1 1 d . . . C8 C 0.0558(8) 0.4585(8) 0.3207(6) 0.0312(15) Uani 1 1 d . . . H8A H 0.1114 0.4342 0.2752 0.037 Uiso 1 1 calc R . . H8B H 0.1139 0.5640 0.3641 0.037 Uiso 1 1 calc R . . H8C H -0.0559 0.4336 0.2543 0.037 Uiso 1 1 calc R . . C9 C 0.4519(7) 0.2167(6) 0.5760(5) 0.0163(11) Uani 1 1 d . . . C10 C 0.5746(8) 0.1375(7) 0.7827(6) 0.0252(14) Uani 1 1 d . . . H10 H 0.6060 0.0870 0.8502 0.030 Uiso 1 1 calc R . . C11 C 0.6346(7) 0.2834(6) 0.8050(5) 0.0151(11) Uani 1 1 d . . . C12 C 0.7595(8) 0.3973(7) 0.9326(6) 0.0261(14) Uani 1 1 d . . . H12A H 0.8086 0.3508 1.0010 0.031 Uiso 1 1 calc R . . H12B H 0.7082 0.4451 0.9648 0.031 Uiso 1 1 calc R . . H12C H 0.8439 0.4711 0.9164 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0150(4) 0.0156(4) 0.0144(4) 0.0000(3) 0.0036(3) 0.0053(3) Ni2 0.0151(5) 0.0133(5) 0.0117(5) 0.0026(4) 0.0044(4) 0.0029(4) S1 0.0150(7) 0.0229(8) 0.0242(8) -0.0027(6) 0.0019(6) 0.0096(6) S2 0.0249(8) 0.0221(8) 0.0213(7) -0.0033(6) 0.0093(6) 0.0117(7) S3 0.0198(7) 0.0257(8) 0.0172(7) 0.0081(6) 0.0083(6) 0.0083(7) S4 0.0171(8) 0.0248(8) 0.0271(8) 0.0041(6) 0.0086(7) 0.0008(7) S5 0.0184(7) 0.0174(7) 0.0148(7) -0.0009(5) 0.0036(6) 0.0021(6) S6 0.0264(8) 0.0151(7) 0.0296(8) 0.0048(6) 0.0122(7) 0.0073(6) O1 0.018(2) 0.017(2) 0.0161(19) -0.0028(16) 0.0043(17) 0.0063(17) O2 0.017(2) 0.015(2) 0.0182(19) 0.0037(16) 0.0064(17) 0.0046(17) O3 0.016(2) 0.015(2) 0.0134(18) 0.0025(15) 0.0042(16) 0.0048(17) N1 0.016(2) 0.018(2) 0.011(2) -0.0008(18) 0.0049(19) 0.009(2) N2 0.014(2) 0.017(2) 0.017(2) 0.0038(19) 0.004(2) 0.007(2) N3 0.011(2) 0.013(2) 0.018(2) 0.0028(18) 0.0053(19) 0.0046(19) C1 0.019(3) 0.014(3) 0.016(3) 0.002(2) 0.008(2) 0.006(2) C2 0.017(3) 0.023(3) 0.019(3) -0.001(2) 0.003(2) 0.008(3) C3 0.016(3) 0.017(3) 0.015(3) 0.004(2) 0.006(2) 0.005(2) C4 0.013(3) 0.035(4) 0.025(3) -0.005(3) 0.001(3) 0.009(3) C5 0.020(3) 0.021(3) 0.018(3) 0.000(2) 0.007(2) 0.006(3) C6 0.017(3) 0.032(4) 0.026(3) 0.003(3) 0.011(3) 0.004(3) C7 0.018(3) 0.026(3) 0.015(3) -0.001(2) 0.004(2) 0.010(3) C8 0.023(3) 0.043(4) 0.017(3) 0.008(3) 0.002(3) 0.013(3) C9 0.014(3) 0.015(3) 0.019(3) 0.004(2) 0.009(2) 0.005(2) C10 0.028(3) 0.023(3) 0.031(3) 0.017(3) 0.017(3) 0.014(3) C11 0.015(3) 0.023(3) 0.015(3) 0.008(2) 0.009(2) 0.012(2) C12 0.027(3) 0.032(4) 0.018(3) 0.002(3) 0.005(3) 0.017(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 O1 1.956(4) . ? Ni1 O2 2.034(4) . ? Ni1 O3 2.123(4) . ? Ni1 S1 2.344(2) . ? Ni1 S3 2.345(2) . ? Ni1 Ni2 2.9846(15) . ? Ni2 O3 2.014(4) 2_666 ? Ni2 O3 2.014(4) . ? Ni2 O2 2.177(4) . ? Ni2 O2 2.177(4) 2_666 ? Ni2 S5 2.381(3) . ? Ni2 S5 2.381(3) 2_666 ? Ni2 Ni1 2.9846(15) 2_666 ? S1 C1 1.704(6) . ? S2 C1 1.725(6) . ? S2 C2 1.728(6) . ? S3 C5 1.693(6) . ? S4 C6 1.725(7) . ? S4 C5 1.728(6) . ? S5 C9 1.699(6) . ? S6 C9 1.723(6) . ? S6 C10 1.734(7) . ? O1 N1 1.348(6) . ? O2 N2 1.360(6) . ? O3 N3 1.361(6) . ? N1 C1 1.313(7) . ? N1 C3 1.399(7) . ? N2 C5 1.334(7) . ? N2 C7 1.409(7) . ? N3 C9 1.339(7) . ? N3 C11 1.400(7) . ? C2 C3 1.337(8) . ? C2 H2 0.9500 . ? C3 C4 1.490(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.326(8) . ? C6 H6 0.9500 . ? C7 C8 1.482(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C11 1.332(8) . ? C10 H10 0.9500 . ? C11 C12 1.486(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 O1 Ni1 O2 150.17(17) . . ? O1 Ni1 O3 83.73(16) . . ? O2 Ni1 O3 84.44(16) . . ? O1 Ni1 S1 87.32(14) . . ? O2 Ni1 S1 97.53(14) . . ? O3 Ni1 S1 164.80(12) . . ? O1 Ni1 S3 120.38(14) . . ? O2 Ni1 S3 87.66(14) . . ? O3 Ni1 S3 93.81(13) . . ? S1 Ni1 S3 101.31(8) . . ? O1 Ni1 Ni2 109.64(13) . . ? O2 Ni1 Ni2 46.84(11) . . ? O3 Ni1 Ni2 42.41(10) . . ? S1 Ni1 Ni2 131.63(6) . . ? S3 Ni1 Ni2 107.13(9) . . ? O3 Ni2 O3 180.000(1) 2_666 . ? O3 Ni2 O2 96.46(15) 2_666 . ? O3 Ni2 O2 83.54(15) . . ? O3 Ni2 O2 83.54(15) 2_666 2_666 ? O3 Ni2 O2 96.46(15) . 2_666 ? O2 Ni2 O2 180.000(1) . 2_666 ? O3 Ni2 S5 92.49(14) 2_666 . ? O3 Ni2 S5 87.51(14) . . ? O2 Ni2 S5 95.08(12) . . ? O2 Ni2 S5 84.92(12) 2_666 . ? O3 Ni2 S5 87.51(14) 2_666 2_666 ? O3 Ni2 S5 92.49(14) . 2_666 ? O2 Ni2 S5 84.92(12) . 2_666 ? O2 Ni2 S5 95.08(12) 2_666 2_666 ? S5 Ni2 S5 180.0 . 2_666 ? O3 Ni2 Ni1 45.31(11) 2_666 2_666 ? O3 Ni2 Ni1 134.69(11) . 2_666 ? O2 Ni2 Ni1 137.03(11) . 2_666 ? O2 Ni2 Ni1 42.97(10) 2_666 2_666 ? S5 Ni2 Ni1 72.43(8) . 2_666 ? S5 Ni2 Ni1 107.57(8) 2_666 2_666 ? O3 Ni2 Ni1 134.69(11) 2_666 . ? O3 Ni2 Ni1 45.31(11) . . ? O2 Ni2 Ni1 42.97(10) . . ? O2 Ni2 Ni1 137.03(10) 2_666 . ? S5 Ni2 Ni1 107.57(8) . . ? S5 Ni2 Ni1 72.43(8) 2_666 . ? Ni1 Ni2 Ni1 180.0 2_666 . ? C1 S1 Ni1 92.3(2) . . ? C1 S2 C2 90.9(3) . . ? C5 S3 Ni1 92.4(2) . . ? C6 S4 C5 91.0(3) . . ? C9 S5 Ni2 91.3(2) . . ? C9 S6 C10 91.6(3) . . ? N1 O1 Ni1 114.3(3) . . ? N2 O2 Ni1 112.0(3) . . ? N2 O2 Ni2 121.0(3) . . ? Ni1 O2 Ni2 90.19(16) . . ? N3 O3 Ni2 113.3(3) . . ? N3 O3 Ni1 120.9(3) . . ? Ni2 O3 Ni1 92.29(16) . . ? C1 N1 O1 123.2(5) . . ? C1 N1 C3 116.8(5) . . ? O1 N1 C3 119.9(4) . . ? C5 N2 O2 122.5(5) . . ? C5 N2 C7 116.3(5) . . ? O2 N2 C7 121.2(4) . . ? C9 N3 O3 121.8(4) . . ? C9 N3 C11 116.6(5) . . ? O3 N3 C11 121.5(4) . . ? N1 C1 S1 122.4(4) . . ? N1 C1 S2 109.7(4) . . ? S1 C1 S2 127.9(3) . . ? C3 C2 S2 112.2(5) . . ? C3 C2 H2 123.9 . . ? S2 C2 H2 123.9 . . ? C2 C3 N1 110.4(5) . . ? C2 C3 C4 129.9(5) . . ? N1 C3 C4 119.7(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 S3 124.7(5) . . ? N2 C5 S4 109.1(4) . . ? S3 C5 S4 126.1(4) . . ? C7 C6 S4 113.0(5) . . ? C7 C6 H6 123.5 . . ? S4 C6 H6 123.5 . . ? C6 C7 N2 110.5(5) . . ? C6 C7 C8 130.1(6) . . ? N2 C7 C8 119.4(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 S5 125.5(4) . . ? N3 C9 S6 108.8(4) . . ? S5 C9 S6 125.8(3) . . ? C11 C10 S6 111.9(4) . . ? C11 C10 H10 124.1 . . ? S6 C10 H10 124.1 . . ? C10 C11 N3 111.0(5) . . ? C10 C11 C12 128.9(5) . . ? N3 C11 C12 120.1(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 O1 Ni1 Ni2 O3 -124.2(2) . . . 2_666 ? O2 Ni1 Ni2 O3 33.9(2) . . . 2_666 ? O3 Ni1 Ni2 O3 180.000(1) . . . 2_666 ? S1 Ni1 Ni2 O3 -19.72(17) . . . 2_666 ? S3 Ni1 Ni2 O3 103.55(17) . . . 2_666 ? O1 Ni1 Ni2 O3 55.8(2) . . . . ? O2 Ni1 Ni2 O3 -146.1(2) . . . . ? S1 Ni1 Ni2 O3 160.28(17) . . . . ? S3 Ni1 Ni2 O3 -76.45(17) . . . . ? O1 Ni1 Ni2 O2 -158.1(2) . . . . ? O3 Ni1 Ni2 O2 146.1(2) . . . . ? S1 Ni1 Ni2 O2 -53.62(17) . . . . ? S3 Ni1 Ni2 O2 69.65(17) . . . . ? O1 Ni1 Ni2 O2 21.9(2) . . . 2_666 ? O2 Ni1 Ni2 O2 180.000(1) . . . 2_666 ? O3 Ni1 Ni2 O2 -33.9(2) . . . 2_666 ? S1 Ni1 Ni2 O2 126.38(17) . . . 2_666 ? S3 Ni1 Ni2 O2 -110.35(17) . . . 2_666 ? O1 Ni1 Ni2 S5 123.60(14) . . . . ? O2 Ni1 Ni2 S5 -78.26(17) . . . . ? O3 Ni1 Ni2 S5 67.84(17) . . . . ? S1 Ni1 Ni2 S5 -131.88(9) . . . . ? S3 Ni1 Ni2 S5 -8.61(6) . . . . ? O1 Ni1 Ni2 S5 -56.40(14) . . . 2_666 ? O2 Ni1 Ni2 S5 101.74(17) . . . 2_666 ? O3 Ni1 Ni2 S5 -112.16(17) . . . 2_666 ? S1 Ni1 Ni2 S5 48.12(9) . . . 2_666 ? S3 Ni1 Ni2 S5 171.39(6) . . . 2_666 ? O1 Ni1 Ni2 Ni1 -42(100) . . . 2_666 ? O2 Ni1 Ni2 Ni1 116(100) . . . 2_666 ? O3 Ni1 Ni2 Ni1 -98(100) . . . 2_666 ? S1 Ni1 Ni2 Ni1 63(100) . . . 2_666 ? S3 Ni1 Ni2 Ni1 -174(100) . . . 2_666 ? O1 Ni1 S1 C1 -5.2(2) . . . . ? O2 Ni1 S1 C1 -155.6(2) . . . . ? O3 Ni1 S1 C1 -59.0(5) . . . . ? S3 Ni1 S1 C1 115.3(2) . . . . ? Ni2 Ni1 S1 C1 -119.3(2) . . . . ? O1 Ni1 S3 C5 -173.9(2) . . . . ? O2 Ni1 S3 C5 -4.6(2) . . . . ? O3 Ni1 S3 C5 -88.9(2) . . . . ? S1 Ni1 S3 C5 92.6(2) . . . . ? Ni2 Ni1 S3 C5 -47.8(2) . . . . ? O3 Ni2 S5 C9 174.4(2) 2_666 . . . ? O3 Ni2 S5 C9 -5.6(2) . . . . ? O2 Ni2 S5 C9 -88.9(2) . . . . ? O2 Ni2 S5 C9 91.1(2) 2_666 . . . ? S5 Ni2 S5 C9 -166(100) 2_666 . . . ? Ni1 Ni2 S5 C9 133.18(19) 2_666 . . . ? Ni1 Ni2 S5 C9 -46.82(19) . . . . ? O2 Ni1 O1 N1 106.0(4) . . . . ? O3 Ni1 O1 N1 173.2(3) . . . . ? S1 Ni1 O1 N1 5.5(3) . . . . ? S3 Ni1 O1 N1 -96.0(3) . . . . ? Ni2 Ni1 O1 N1 139.1(3) . . . . ? O1 Ni1 O2 N2 168.7(3) . . . . ? O3 Ni1 O2 N2 101.7(3) . . . . ? S1 Ni1 O2 N2 -93.5(3) . . . . ? S3 Ni1 O2 N2 7.6(3) . . . . ? Ni2 Ni1 O2 N2 123.9(4) . . . . ? O1 Ni1 O2 Ni2 44.8(4) . . . . ? O3 Ni1 O2 Ni2 -22.20(14) . . . . ? S1 Ni1 O2 Ni2 142.63(10) . . . . ? S3 Ni1 O2 Ni2 -116.27(12) . . . . ? O3 Ni2 O2 N2 87.4(4) 2_666 . . . ? O3 Ni2 O2 N2 -92.6(4) . . . . ? O2 Ni2 O2 N2 169(100) 2_666 . . . ? S5 Ni2 O2 N2 -5.7(3) . . . . ? S5 Ni2 O2 N2 174.3(3) 2_666 . . . ? Ni1 Ni2 O2 N2 63.9(4) 2_666 . . . ? Ni1 Ni2 O2 N2 -116.1(4) . . . . ? O3 Ni2 O2 Ni1 -156.48(15) 2_666 . . . ? O3 Ni2 O2 Ni1 23.52(15) . . . . ? O2 Ni2 O2 Ni1 -75(100) 2_666 . . . ? S5 Ni2 O2 Ni1 110.43(14) . . . . ? S5 Ni2 O2 Ni1 -69.57(14) 2_666 . . . ? Ni1 Ni2 O2 Ni1 180.000(2) 2_666 . . . ? O3 Ni2 O3 N3 -173(100) 2_666 . . . ? O2 Ni2 O3 N3 102.7(3) . . . . ? O2 Ni2 O3 N3 -77.3(3) 2_666 . . . ? S5 Ni2 O3 N3 7.3(3) . . . . ? S5 Ni2 O3 N3 -172.7(3) 2_666 . . . ? Ni1 Ni2 O3 N3 -54.8(4) 2_666 . . . ? Ni1 Ni2 O3 N3 125.2(4) . . . . ? O3 Ni2 O3 Ni1 62(100) 2_666 . . . ? O2 Ni2 O3 Ni1 -22.49(14) . . . . ? O2 Ni2 O3 Ni1 157.51(14) 2_666 . . . ? S5 Ni2 O3 Ni1 -117.90(13) . . . . ? S5 Ni2 O3 Ni1 62.10(13) 2_666 . . . ? Ni1 Ni2 O3 Ni1 180.000(2) 2_666 . . . ? O1 Ni1 O3 N3 112.6(4) . . . . ? O2 Ni1 O3 N3 -94.9(4) . . . . ? S1 Ni1 O3 N3 166.8(3) . . . . ? S3 Ni1 O3 N3 -7.6(3) . . . . ? Ni2 Ni1 O3 N3 -119.0(4) . . . . ? O1 Ni1 O3 Ni2 -128.44(17) . . . . ? O2 Ni1 O3 Ni2 24.13(15) . . . . ? S1 Ni1 O3 Ni2 -74.2(4) . . . . ? S3 Ni1 O3 Ni2 111.40(14) . . . . ? Ni1 O1 N1 C1 -3.8(6) . . . . ? Ni1 O1 N1 C3 174.0(4) . . . . ? Ni1 O2 N2 C5 -9.0(6) . . . . ? Ni2 O2 N2 C5 95.4(5) . . . . ? Ni1 O2 N2 C7 169.8(4) . . . . ? Ni2 O2 N2 C7 -85.9(5) . . . . ? Ni2 O3 N3 C9 -6.8(6) . . . . ? Ni1 O3 N3 C9 101.2(5) . . . . ? Ni2 O3 N3 C11 175.3(4) . . . . ? Ni1 O3 N3 C11 -76.8(5) . . . . ? O1 N1 C1 S1 -2.0(7) . . . . ? C3 N1 C1 S1 -179.8(4) . . . . ? O1 N1 C1 S2 178.2(4) . . . . ? C3 N1 C1 S2 0.3(6) . . . . ? Ni1 S1 C1 N1 5.3(5) . . . . ? Ni1 S1 C1 S2 -174.9(4) . . . . ? C2 S2 C1 N1 0.2(4) . . . . ? C2 S2 C1 S1 -179.6(4) . . . . ? C1 S2 C2 C3 -0.7(5) . . . . ? S2 C2 C3 N1 1.0(6) . . . . ? S2 C2 C3 C4 -178.1(5) . . . . ? C1 N1 C3 C2 -0.9(7) . . . . ? O1 N1 C3 C2 -178.8(5) . . . . ? C1 N1 C3 C4 178.3(5) . . . . ? O1 N1 C3 C4 0.4(8) . . . . ? O2 N2 C5 S3 4.5(8) . . . . ? C7 N2 C5 S3 -174.3(4) . . . . ? O2 N2 C5 S4 -178.2(4) . . . . ? C7 N2 C5 S4 3.1(6) . . . . ? Ni1 S3 C5 N2 1.8(5) . . . . ? Ni1 S3 C5 S4 -175.1(4) . . . . ? C6 S4 C5 N2 -2.6(5) . . . . ? C6 S4 C5 S3 174.7(4) . . . . ? C5 S4 C6 C7 1.7(5) . . . . ? S4 C6 C7 N2 -0.3(7) . . . . ? S4 C6 C7 C8 -179.4(5) . . . . ? C5 N2 C7 C6 -1.9(7) . . . . ? O2 N2 C7 C6 179.3(5) . . . . ? C5 N2 C7 C8 177.4(5) . . . . ? O2 N2 C7 C8 -1.4(8) . . . . ? O3 N3 C9 S5 0.7(7) . . . . ? C11 N3 C9 S5 178.7(4) . . . . ? O3 N3 C9 S6 -179.7(4) . . . . ? C11 N3 C9 S6 -1.6(6) . . . . ? Ni2 S5 C9 N3 4.5(5) . . . . ? Ni2 S5 C9 S6 -175.1(4) . . . . ? C10 S6 C9 N3 1.5(4) . . . . ? C10 S6 C9 S5 -178.8(4) . . . . ? C9 S6 C10 C11 -1.2(5) . . . . ? S6 C10 C11 N3 0.5(6) . . . . ? S6 C10 C11 C12 -179.2(5) . . . . ? C9 N3 C11 C10 0.7(7) . . . . ? O3 N3 C11 C10 178.8(5) . . . . ? C9 N3 C11 C12 -179.5(5) . . . . ? O3 N3 C11 C12 -1.4(7) . . . . ? #===END