# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Ren, XiaoMing' _publ_contact_author_name 'Ren, XiaoMing' _publ_contact_author_email xmren@njut.edu.cn _publ_section_title ; A low-dimensional molecular spin system with two steps of magnetic transitions and liquid crystal property ; data_090506-105k _database_code_depnum_ccdc_archive 'CCDC 803771' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 N6 Ni S4' _chemical_formula_weight 518.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 4.4540(5) _cell_length_b 13.6238(15) _cell_length_c 20.238(2) _cell_angle_alpha 84.472(9) _cell_angle_beta 85.962(8) _cell_angle_gamma 82.683(9) _cell_volume 1210.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 105(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 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 4.528 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\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 10060 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 62.64 _reflns_number_total 3831 _reflns_number_gt 2984 _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^)+(0.0427P)^2^+2.8708P] 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 3831 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_restrained_S_all 1.226 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 1.0000 0.5000 0.0264(3) Uani 1 2 d S . . Ni2 Ni 1.0000 1.0000 0.0000 0.0258(3) Uani 1 2 d S . . S1 S 0.5237(3) 0.88006(10) 0.43722(6) 0.0312(3) Uani 1 1 d . . . S2 S 0.7883(3) 1.07024(9) 0.42563(6) 0.0286(3) Uani 1 1 d . . . S3 S 0.7262(3) 0.91112(9) 0.06756(6) 0.0281(3) Uani 1 1 d . . . S4 S 0.9859(3) 1.09894(9) 0.07635(6) 0.0301(3) Uani 1 1 d . . . N1 N 0.2387(11) 0.6401(4) 0.4271(2) 0.0458(12) Uani 1 1 d . . . N2 N 1.1716(11) 1.2962(3) 0.3877(2) 0.0402(11) Uani 1 1 d . . . N3 N 0.3371(11) 0.6855(3) 0.0777(2) 0.0406(11) Uani 1 1 d . . . N4 N 1.2888(11) 1.3240(3) 0.1166(2) 0.0426(12) Uani 1 1 d . . . N5 N 0.9392(8) 0.6099(3) 0.25281(19) 0.0232(9) Uani 1 1 d . . . N6 N 0.4024(9) 0.3860(3) 0.2528(2) 0.0276(9) Uani 1 1 d . . . H6A H 0.3570 0.3663 0.2150 0.033 Uiso 1 1 calc R . . H6B H 0.3310 0.3581 0.2907 0.033 Uiso 1 1 calc R . . C1 C 0.3004(11) 0.7993(4) 0.4821(2) 0.0282(11) Uani 1 1 d . . . C2 C 0.2642(12) 0.7093(4) 0.4521(2) 0.0345(12) Uani 1 1 d . . . C3 C 0.8352(11) 1.1789(4) 0.4582(2) 0.0276(11) Uani 1 1 d . . . C4 C 1.0226(12) 1.2445(4) 0.4197(2) 0.0294(11) Uani 1 1 d . . . C5 C 0.6702(11) 0.8163(4) 0.0212(2) 0.0265(11) Uani 1 1 d . . . C6 C 0.4844(12) 0.7425(4) 0.0522(2) 0.0304(11) Uani 1 1 d . . . C7 C 1.2051(11) 1.1878(4) 0.0421(2) 0.0276(11) Uani 1 1 d . . . C8 C 1.2512(12) 1.2654(4) 0.0823(2) 0.0312(12) Uani 1 1 d . . . C9 C 0.8731(11) 0.5789(3) 0.1946(2) 0.0258(11) Uani 1 1 d . . . H9A H 0.9506 0.6099 0.1540 0.031 Uiso 1 1 calc R . . C10 C 0.6982(10) 0.5044(3) 0.1929(2) 0.0245(10) Uani 1 1 d . . . H10A H 0.6559 0.4835 0.1514 0.029 Uiso 1 1 calc R . . C11 C 0.5798(10) 0.4581(3) 0.2527(2) 0.0228(10) Uani 1 1 d . . . C12 C 0.6547(11) 0.4912(3) 0.3131(2) 0.0239(10) Uani 1 1 d . . . H12A H 0.5817 0.4614 0.3546 0.029 Uiso 1 1 calc R . . C13 C 0.8324(11) 0.5661(3) 0.3113(2) 0.0255(11) Uani 1 1 d . . . H13A H 0.8823 0.5880 0.3519 0.031 Uiso 1 1 calc R . . C14 C 1.1133(11) 0.6965(3) 0.2527(2) 0.0269(11) Uani 1 1 d . . . H14A H 1.2542 0.6990 0.2127 0.032 Uiso 1 1 calc R . . H14B H 1.2356 0.6880 0.2923 0.032 Uiso 1 1 calc R . . C15 C 0.9031(10) 0.7936(3) 0.2533(2) 0.0232(10) Uani 1 1 d . . . H15A H 0.7630 0.7912 0.2935 0.028 Uiso 1 1 calc R . . H15B H 0.7798 0.8018 0.2138 0.028 Uiso 1 1 calc R . . C16 C 1.0810(10) 0.8831(3) 0.2528(2) 0.0254(11) Uani 1 1 d . . . H16A H 1.2013 0.8752 0.2927 0.031 Uiso 1 1 calc R . . H16B H 1.2243 0.8843 0.2131 0.031 Uiso 1 1 calc R . . C17 C 0.8760(11) 0.9812(3) 0.2519(2) 0.0249(10) Uani 1 1 d . . . H17A H 0.7280 0.9788 0.2907 0.030 Uiso 1 1 calc R . . H17B H 0.7607 0.9900 0.2112 0.030 Uiso 1 1 calc R . . C18 C 1.0496(11) 1.0708(3) 0.2537(2) 0.0251(10) Uani 1 1 d . . . H18A H 1.1590 1.0633 0.2952 0.030 Uiso 1 1 calc R . . H18B H 1.2026 1.0718 0.2158 0.030 Uiso 1 1 calc R . . C19 C 0.8443(11) 1.1695(3) 0.2504(2) 0.0295(11) Uani 1 1 d . . . H19A H 0.9669 1.2240 0.2519 0.044 Uiso 1 1 calc R . . H19B H 0.6946 1.1695 0.2883 0.044 Uiso 1 1 calc R . . H19C H 0.7394 1.1783 0.2089 0.044 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 0.0282(7) 0.0286(7) 0.0226(6) -0.0024(5) 0.0009(5) -0.0062(5) Ni2 0.0290(7) 0.0273(6) 0.0221(6) -0.0038(5) 0.0014(5) -0.0082(5) S1 0.0339(7) 0.0359(7) 0.0259(6) -0.0076(5) 0.0043(5) -0.0119(6) S2 0.0340(7) 0.0295(7) 0.0229(6) -0.0027(5) 0.0033(5) -0.0085(5) S3 0.0327(7) 0.0296(7) 0.0228(6) -0.0034(5) 0.0022(5) -0.0087(5) S4 0.0354(7) 0.0330(7) 0.0243(6) -0.0069(5) 0.0038(5) -0.0128(6) N1 0.051(3) 0.048(3) 0.043(3) -0.018(2) 0.002(2) -0.017(3) N2 0.043(3) 0.038(3) 0.040(3) 0.000(2) 0.006(2) -0.011(2) N3 0.041(3) 0.042(3) 0.039(3) 0.001(2) 0.003(2) -0.013(2) N4 0.052(3) 0.038(3) 0.040(3) -0.008(2) -0.002(2) -0.013(2) N5 0.018(2) 0.022(2) 0.030(2) -0.0039(16) -0.0004(16) -0.0014(17) N6 0.030(2) 0.025(2) 0.029(2) -0.0038(17) 0.0011(17) -0.0083(18) C1 0.023(3) 0.033(3) 0.030(3) -0.002(2) -0.006(2) -0.009(2) C2 0.034(3) 0.041(3) 0.029(3) -0.005(2) 0.001(2) -0.009(3) C3 0.029(3) 0.027(3) 0.027(3) 0.002(2) -0.007(2) -0.005(2) C4 0.032(3) 0.027(3) 0.031(3) -0.006(2) -0.004(2) -0.005(2) C5 0.026(3) 0.024(3) 0.031(3) -0.001(2) -0.007(2) -0.005(2) C6 0.032(3) 0.030(3) 0.029(3) -0.003(2) -0.002(2) -0.006(2) C7 0.028(3) 0.027(3) 0.030(3) -0.005(2) -0.002(2) -0.007(2) C8 0.033(3) 0.030(3) 0.031(3) -0.003(2) 0.002(2) -0.007(2) C9 0.024(3) 0.024(3) 0.028(2) -0.001(2) 0.002(2) -0.001(2) C10 0.024(3) 0.023(3) 0.027(2) -0.0042(19) 0.0002(19) -0.002(2) C11 0.021(2) 0.017(2) 0.030(2) -0.0036(19) -0.0002(19) 0.0005(19) C12 0.026(3) 0.019(2) 0.026(2) -0.0008(19) 0.0014(19) -0.002(2) C13 0.025(3) 0.025(3) 0.026(2) -0.004(2) -0.002(2) 0.001(2) C14 0.023(3) 0.022(3) 0.036(3) -0.003(2) 0.001(2) -0.005(2) C15 0.019(2) 0.019(2) 0.032(3) -0.003(2) -0.001(2) -0.0029(19) C16 0.019(2) 0.022(3) 0.035(3) -0.003(2) 0.001(2) -0.002(2) C17 0.024(3) 0.024(3) 0.026(2) -0.004(2) 0.001(2) -0.005(2) C18 0.025(3) 0.024(3) 0.027(2) -0.004(2) 0.002(2) -0.006(2) C19 0.034(3) 0.023(3) 0.032(3) -0.004(2) 0.001(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S2 2.1431(12) 2_676 ? Ni1 S2 2.1431(12) . ? Ni1 S1 2.1524(12) . ? Ni1 S1 2.1524(12) 2_676 ? Ni2 S4 2.1388(12) 2_775 ? Ni2 S4 2.1388(12) . ? Ni2 S3 2.1551(12) . ? Ni2 S3 2.1551(12) 2_775 ? S1 C1 1.727(5) . ? S2 C3 1.719(5) . ? S3 C5 1.720(5) . ? S4 C7 1.716(5) . ? N1 C2 1.134(7) . ? N2 C4 1.152(6) . ? N3 C6 1.142(6) . ? N4 C8 1.142(6) . ? N5 C9 1.352(6) . ? N5 C13 1.357(6) . ? N5 C14 1.492(6) . ? N6 C11 1.337(6) . ? C1 C3 1.355(7) 2_676 ? C1 C2 1.450(7) . ? C3 C1 1.355(7) 2_676 ? C3 C4 1.437(7) . ? C5 C7 1.363(7) 2_775 ? C5 C6 1.450(7) . ? C7 C5 1.363(7) 2_775 ? C7 C8 1.437(7) . ? C9 C10 1.361(7) . ? C10 C11 1.410(6) . ? C11 C12 1.418(7) . ? C12 C13 1.365(7) . ? C14 C15 1.521(6) . ? C15 C16 1.535(6) . ? C16 C17 1.520(6) . ? C17 C18 1.531(6) . ? C18 C19 1.525(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 S2 Ni1 S2 180.000(1) 2_676 . ? S2 Ni1 S1 92.77(5) 2_676 . ? S2 Ni1 S1 87.23(5) . . ? S2 Ni1 S1 87.23(5) 2_676 2_676 ? S2 Ni1 S1 92.77(5) . 2_676 ? S1 Ni1 S1 180.00(5) . 2_676 ? S4 Ni2 S4 180.00(6) 2_775 . ? S4 Ni2 S3 92.69(5) 2_775 . ? S4 Ni2 S3 87.31(5) . . ? S4 Ni2 S3 87.31(5) 2_775 2_775 ? S4 Ni2 S3 92.69(5) . 2_775 ? S3 Ni2 S3 180.00(5) . 2_775 ? C1 S1 Ni1 102.76(17) . . ? C3 S2 Ni1 103.24(17) . . ? C5 S3 Ni2 102.81(17) . . ? C7 S4 Ni2 103.50(16) . . ? C9 N5 C13 120.1(4) . . ? C9 N5 C14 120.0(4) . . ? C13 N5 C14 119.8(4) . . ? C3 C1 C2 122.6(4) 2_676 . ? C3 C1 S1 120.6(4) 2_676 . ? C2 C1 S1 116.8(4) . . ? N1 C2 C1 178.1(6) . . ? C1 C3 C4 121.9(4) 2_676 . ? C1 C3 S2 120.6(4) 2_676 . ? C4 C3 S2 117.5(4) . . ? N2 C4 C3 178.5(5) . . ? C7 C5 C6 122.1(4) 2_775 . ? C7 C5 S3 120.6(4) 2_775 . ? C6 C5 S3 117.2(4) . . ? N3 C6 C5 178.6(5) . . ? C5 C7 C8 121.9(4) 2_775 . ? C5 C7 S4 120.3(4) 2_775 . ? C8 C7 S4 117.8(4) . . ? N4 C8 C7 177.0(6) . . ? N5 C9 C10 121.5(4) . . ? C9 C10 C11 119.9(4) . . ? N6 C11 C10 121.5(4) . . ? N6 C11 C12 120.9(4) . . ? C10 C11 C12 117.5(4) . . ? C13 C12 C11 119.5(4) . . ? N5 C13 C12 121.4(4) . . ? N5 C14 C15 111.4(4) . . ? C14 C15 C16 111.6(4) . . ? C17 C16 C15 112.6(4) . . ? C16 C17 C18 113.1(4) . . ? C19 C18 C17 113.0(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 62.64 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.402 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.077 #=====================END data_293K _database_code_depnum_ccdc_archive 'CCDC 803772' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 N6 Ni S4' _chemical_formula_weight 518.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 4.5025(6) _cell_length_b 13.6474(13) _cell_length_c 20.5060(19) _cell_angle_alpha 84.901(8) _cell_angle_beta 85.132(9) _cell_angle_gamma 83.759(9) _cell_volume 1244.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(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 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 4.405 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 12745 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 63.54 _reflns_number_total 3939 _reflns_number_gt 2728 _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^)+(0.0706P)^2^+1.4529P] 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 3939 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.5000 0.5000 0.0627(4) Uani 1 2 d S . . Ni2 Ni 0.5000 0.5000 0.0000 0.0645(4) Uani 1 2 d S . . S1 S 0.0044(3) 0.40247(11) 0.42404(6) 0.0748(4) Uani 1 1 d . . . S2 S 0.2688(3) 0.59002(11) 0.43280(6) 0.0713(4) Uani 1 1 d . . . S3 S 0.2174(3) 0.42813(11) 0.07404(6) 0.0728(4) Uani 1 1 d . . . S4 S 0.4872(4) 0.61809(11) 0.06338(7) 0.0770(4) Uani 1 1 d . . . N1 N -0.3008(14) 0.1790(4) 0.3848(3) 0.1065(19) Uani 1 1 d . . . N2 N 0.6540(14) 0.8154(4) 0.4214(3) 0.1061(19) Uani 1 1 d . . . N3 N -0.1609(13) 0.2019(4) 0.1117(3) 0.1007(17) Uani 1 1 d . . . N4 N 0.7797(16) 0.8556(5) 0.0746(3) 0.117(2) Uani 1 1 d . . . N5 N 0.5954(9) 1.1185(3) 0.2477(2) 0.0675(11) Uani 1 1 d . . . H5A H 0.6352 1.1385 0.2843 0.081 Uiso 1 1 calc R . . H5B H 0.6671 1.1458 0.2112 0.081 Uiso 1 1 calc R . . N6 N 0.0674(8) 0.8917(3) 0.2476(2) 0.0576(10) Uani 1 1 d . . . C1 C -0.2619(14) 0.2362(4) 0.4187(3) 0.0771(16) Uani 1 1 d . . . C2 C -0.2110(12) 0.3122(4) 0.4593(3) 0.0676(14) Uani 1 1 d . . . C3 C 0.3295(12) 0.6841(4) 0.4786(3) 0.0649(13) Uani 1 1 d . . . C4 C 0.5090(14) 0.7592(4) 0.4478(3) 0.0771(15) Uani 1 1 d . . . C5 C -0.0200(13) 0.2546(4) 0.0796(3) 0.0734(15) Uani 1 1 d . . . C6 C 0.1642(12) 0.3208(4) 0.0410(3) 0.0677(14) Uani 1 1 d . . . C7 C 0.7081(12) 0.6992(4) 0.0186(3) 0.0687(14) Uani 1 1 d . . . C8 C 0.7486(15) 0.7877(5) 0.0486(3) 0.0859(18) Uani 1 1 d . . . C9 C 0.1279(11) 0.9238(4) 0.3047(3) 0.0621(12) Uani 1 1 d . . . H9A H 0.0492 0.8940 0.3440 0.074 Uiso 1 1 calc R . . C10 C 0.3019(11) 0.9991(3) 0.3062(2) 0.0612(12) Uani 1 1 d . . . H10A H 0.3411 1.0199 0.3463 0.073 Uiso 1 1 calc R . . C11 C 0.4222(10) 1.0451(3) 0.2476(2) 0.0544(11) Uani 1 1 d . . . C12 C 0.3532(11) 1.0107(3) 0.1886(2) 0.0593(12) Uani 1 1 d . . . H12A H 0.4266 1.0396 0.1485 0.071 Uiso 1 1 calc R . . C13 C 0.1792(11) 0.9352(3) 0.1903(2) 0.0601(12) Uani 1 1 d . . . H13A H 0.1357 0.9128 0.1510 0.072 Uiso 1 1 calc R . . C14 C -0.1051(11) 0.8045(3) 0.2474(3) 0.0641(13) Uani 1 1 d . . . H14A H -0.2197 0.8121 0.2089 0.077 Uiso 1 1 calc R . . H14B H -0.2452 0.8020 0.2859 0.077 Uiso 1 1 calc R . . C15 C 0.0965(10) 0.7093(3) 0.2468(3) 0.0594(12) Uani 1 1 d . . . H15A H 0.2142 0.7026 0.2847 0.071 Uiso 1 1 calc R . . H15B H 0.2340 0.7115 0.2078 0.071 Uiso 1 1 calc R . . C16 C -0.0769(10) 0.6195(3) 0.2480(3) 0.0620(13) Uani 1 1 d . . . H16A H -0.2157 0.6179 0.2868 0.074 Uiso 1 1 calc R . . H16B H -0.1937 0.6263 0.2099 0.074 Uiso 1 1 calc R . . C17 C 0.1209(11) 0.5228(3) 0.2480(2) 0.0561(11) Uani 1 1 d . . . H17A H 0.2325 0.5148 0.2869 0.067 Uiso 1 1 calc R . . H17B H 0.2643 0.5251 0.2099 0.067 Uiso 1 1 calc R . . C18 C -0.0551(11) 0.4334(3) 0.2467(2) 0.0593(12) Uani 1 1 d . . . H18A H -0.1592 0.4397 0.2068 0.071 Uiso 1 1 calc R . . H18B H -0.2044 0.4325 0.2837 0.071 Uiso 1 1 calc R . . C19 C 0.1484(13) 0.3357(4) 0.2499(3) 0.0728(15) Uani 1 1 d . . . H19A H 0.0296 0.2816 0.2488 0.109 Uiso 1 1 calc R . . H19B H 0.2484 0.3285 0.2898 0.109 Uiso 1 1 calc R . . H19C H 0.2944 0.3358 0.2129 0.109 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 0.0755(8) 0.0673(8) 0.0483(6) -0.0088(5) -0.0013(5) -0.0200(6) Ni2 0.0761(8) 0.0696(8) 0.0491(6) -0.0043(5) 0.0002(6) -0.0181(6) S1 0.0940(10) 0.0825(9) 0.0534(7) -0.0165(6) 0.0072(7) -0.0342(8) S2 0.0891(10) 0.0770(9) 0.0509(7) -0.0083(6) 0.0032(6) -0.0264(7) S3 0.0910(10) 0.0773(9) 0.0521(7) -0.0069(6) 0.0071(7) -0.0253(8) S4 0.0922(10) 0.0873(10) 0.0560(7) -0.0153(7) 0.0063(7) -0.0314(8) N1 0.133(5) 0.097(4) 0.099(4) -0.032(3) -0.007(4) -0.036(4) N2 0.119(5) 0.102(4) 0.099(4) 0.010(3) 0.006(3) -0.043(4) N3 0.112(4) 0.093(4) 0.097(4) 0.006(3) 0.007(3) -0.036(3) N4 0.153(6) 0.108(5) 0.103(4) -0.031(4) -0.009(4) -0.051(4) N5 0.076(3) 0.054(2) 0.074(3) -0.008(2) 0.000(2) -0.018(2) N6 0.053(2) 0.048(2) 0.073(3) -0.0074(19) -0.004(2) -0.0092(18) C1 0.092(4) 0.073(4) 0.073(4) -0.014(3) -0.009(3) -0.028(3) C2 0.080(4) 0.066(3) 0.061(3) -0.008(2) -0.010(3) -0.020(3) C3 0.069(3) 0.067(3) 0.062(3) -0.004(2) -0.010(3) -0.018(3) C4 0.090(4) 0.074(4) 0.069(3) 0.003(3) -0.003(3) -0.023(3) C5 0.080(4) 0.075(4) 0.067(3) -0.002(3) -0.002(3) -0.023(3) C6 0.076(3) 0.069(3) 0.060(3) 0.003(3) -0.012(3) -0.017(3) C7 0.075(4) 0.077(4) 0.058(3) -0.003(3) -0.012(3) -0.022(3) C8 0.100(5) 0.094(5) 0.070(4) -0.018(3) -0.002(3) -0.033(4) C9 0.067(3) 0.058(3) 0.060(3) -0.001(2) 0.003(2) -0.009(2) C10 0.067(3) 0.057(3) 0.061(3) -0.010(2) -0.004(2) -0.010(2) C11 0.056(3) 0.043(2) 0.065(3) -0.006(2) -0.004(2) -0.006(2) C12 0.063(3) 0.054(3) 0.061(3) -0.002(2) 0.000(2) -0.010(2) C13 0.063(3) 0.058(3) 0.061(3) -0.006(2) -0.006(2) -0.008(2) C14 0.052(3) 0.052(3) 0.091(4) -0.006(3) -0.007(3) -0.013(2) C15 0.053(3) 0.050(3) 0.075(3) -0.005(2) -0.004(2) -0.008(2) C16 0.051(3) 0.056(3) 0.080(3) -0.006(2) -0.007(2) -0.009(2) C17 0.055(3) 0.053(3) 0.062(3) -0.008(2) -0.002(2) -0.011(2) C18 0.062(3) 0.055(3) 0.063(3) -0.006(2) -0.005(2) -0.016(2) C19 0.092(4) 0.050(3) 0.078(4) -0.004(3) -0.005(3) -0.013(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 S1 2.1343(13) . ? Ni1 S1 2.1343(13) 2_566 ? Ni1 S2 2.1477(13) 2_566 ? Ni1 S2 2.1477(13) . ? Ni2 S3 2.1366(13) 2_665 ? Ni2 S3 2.1366(13) . ? Ni2 S4 2.1516(14) 2_665 ? Ni2 S4 2.1516(14) . ? S1 C2 1.721(5) . ? S2 C3 1.714(5) . ? S3 C6 1.716(5) . ? S4 C7 1.721(5) . ? N1 C1 1.126(7) . ? N2 C4 1.133(7) . ? N3 C5 1.139(7) . ? N4 C8 1.137(7) . ? N5 C11 1.336(6) . ? N6 C9 1.344(6) . ? N6 C13 1.353(6) . ? N6 C14 1.490(6) . ? C1 C2 1.435(7) . ? C2 C3 1.342(7) 2_566 ? C3 C2 1.342(7) 2_566 ? C3 C4 1.443(7) . ? C5 C6 1.434(7) . ? C6 C7 1.343(7) 2_665 ? C7 C6 1.343(7) 2_665 ? C7 C8 1.438(8) . ? C9 C10 1.362(6) . ? C10 C11 1.401(7) . ? C11 C12 1.406(7) . ? C12 C13 1.357(6) . ? C14 C15 1.503(6) . ? C15 C16 1.520(6) . ? C16 C17 1.509(7) . ? C17 C18 1.529(6) . ? C18 C19 1.533(7) . ? 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 S1 Ni1 S1 180.00(4) . 2_566 ? S1 Ni1 S2 92.42(5) . 2_566 ? S1 Ni1 S2 87.58(5) 2_566 2_566 ? S1 Ni1 S2 87.58(5) . . ? S1 Ni1 S2 92.42(5) 2_566 . ? S2 Ni1 S2 180.00(6) 2_566 . ? S3 Ni2 S3 180.00(5) 2_665 . ? S3 Ni2 S4 87.44(5) 2_665 2_665 ? S3 Ni2 S4 92.56(5) . 2_665 ? S3 Ni2 S4 92.56(5) 2_665 . ? S3 Ni2 S4 87.44(5) . . ? S4 Ni2 S4 180.00(7) 2_665 . ? C2 S1 Ni1 103.33(18) . . ? C3 S2 Ni1 103.01(18) . . ? C6 S3 Ni2 103.30(19) . . ? C7 S4 Ni2 102.67(19) . . ? C9 N6 C13 119.6(4) . . ? C9 N6 C14 120.4(4) . . ? C13 N6 C14 119.9(4) . . ? N1 C1 C2 177.4(7) . . ? C3 C2 C1 122.7(5) 2_566 . ? C3 C2 S1 120.4(4) 2_566 . ? C1 C2 S1 116.9(4) . . ? C2 C3 C4 121.4(5) 2_566 . ? C2 C3 S2 120.9(4) 2_566 . ? C4 C3 S2 117.7(4) . . ? N2 C4 C3 176.9(7) . . ? N3 C5 C6 178.0(6) . . ? C7 C6 C5 122.2(5) 2_665 . ? C7 C6 S3 120.6(4) 2_665 . ? C5 C6 S3 117.1(4) . . ? C6 C7 C8 122.6(5) 2_665 . ? C6 C7 S4 120.8(4) 2_665 . ? C8 C7 S4 116.6(4) . . ? N4 C8 C7 177.3(7) . . ? N6 C9 C10 121.5(5) . . ? C9 C10 C11 120.1(5) . . ? N5 C11 C10 121.4(4) . . ? N5 C11 C12 121.3(4) . . ? C10 C11 C12 117.3(4) . . ? C13 C12 C11 119.8(5) . . ? N6 C13 C12 121.8(5) . . ? N6 C14 C15 111.9(4) . . ? C14 C15 C16 112.5(4) . . ? C17 C16 C15 113.5(4) . . ? C16 C17 C18 113.0(4) . . ? C17 C18 C19 112.1(4) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 63.54 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.279 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.056 #==============================END data_trapped-phase293K _database_code_depnum_ccdc_archive 'CCDC 803773' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 N6 Ni S4' _chemical_formula_weight 518.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 4.4980(3) _cell_length_b 20.5770(14) _cell_length_c 13.6962(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.193(6) _cell_angle_gamma 90.00 _cell_volume 1260.24(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(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 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 4.348 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\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 1143 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.45 _reflns_number_total 247 _reflns_number_gt 246 _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 247 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 1.435 _refine_ls_restrained_S_all 1.435 _refine_ls_shift/su_max 0.310 _refine_ls_shift/su_mean 0.058 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 0.5000 0.5000 0.5000 0.0804(16) Uani 1 2 d S . . S1 S 0.2576(8) 0.56639(18) 0.5814(3) 0.0787(18) Uani 1 1 d . . . S2 S 0.5292(8) 0.57615(17) 0.3954(3) 0.085(2) Uani 1 1 d . . . N1 N -0.110(2) 0.5764(5) 0.8068(7) 0.109(6) Uani 1 1 d . . . N2 N 0.859(3) 0.6170(5) 0.1697(8) 0.124(6) Uani 1 1 d . . . N3 N 0.456(3) 0.2500 0.1342(10) 0.064(7) Uani 1 2 d S . . N4 N 0.984(2) 0.2500 -0.0930(8) 0.071(7) Uani 1 2 d S . . H4A H 1.0448 0.2121 -0.1171 0.085 Uiso 1 1 d R . . C1 C 0.010(3) 0.5500(7) 0.7467(10) 0.085(8) Uani 1 1 d . . . C2 C 0.181(3) 0.5218(7) 0.6776(12) 0.073(8) Uani 1 1 d . . . C3 C 0.804(3) 0.5834(7) 0.2318(11) 0.095(8) Uani 1 1 d . . . C4 C 0.723(4) 0.5393(8) 0.3069(10) 0.074(7) Uani 1 1 d . . . C5 C 0.798(4) 0.2500 -0.0208(11) 0.038(9) Uani 1 2 d S . . C6 C 0.722(3) 0.3091(7) 0.0203(8) 0.067(6) Uani 1 1 d . . . H6A H 0.7762 0.3499 -0.0067 0.081 Uiso 1 1 d R . . C7 C 0.534(3) 0.3044(7) 0.0951(9) 0.073(7) Uani 1 1 d . . . H7A H 0.4754 0.3444 0.1238 0.088 Uiso 1 1 d R . . C8 C 0.268(4) 0.2500 0.2234(10) 0.073(9) Uani 1 2 d S . . H8A H 0.1424 0.2122 0.2210 0.087 Uiso 1 1 d R . . C9 C 0.486(3) 0.2500 0.3155(9) 0.050(8) Uani 1 2 d S . . H9A H 0.6121 0.2878 0.3177 0.060 Uiso 1 1 d R . . C10 C 0.314(4) 0.2500 0.4064(11) 0.081(10) Uani 1 2 d S . . H10A H 0.1877 0.2123 0.4036 0.098 Uiso 1 1 d R . . C11 C 0.511(4) 0.2500 0.5004(10) 0.060(9) Uani 1 2 d S . . H11A H 0.6371 0.2878 0.5033 0.073 Uiso 1 1 d R . . C12 C 0.346(4) 0.2500 0.5942(12) 0.080(9) Uani 1 2 d S . . H12A H 0.2208 0.2122 0.5919 0.096 Uiso 1 1 d R . . C13 C 0.542(4) 0.2500 0.6920(11) 0.095(10) Uani 1 2 d S . . H13A H 0.4277 0.2500 0.7473 0.142 Uiso 1 2 d SR . . H13B H 0.6657 0.2119 0.6941 0.142 Uiso 1 1 d 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 0.082(3) 0.079(3) 0.083(3) 0.005(2) 0.024(3) 0.006(2) S1 0.082(3) 0.062(3) 0.099(3) -0.005(3) 0.043(4) 0.003(3) S2 0.102(4) 0.067(3) 0.093(4) 0.020(3) 0.043(4) 0.016(3) N1 0.104(11) 0.121(11) 0.106(10) -0.013(9) 0.024(10) 0.008(9) N2 0.157(10) 0.098(10) 0.130(11) 0.020(9) 0.066(10) 0.002(9) N3 0.050(12) 0.057(12) 0.078(13) 0.000 -0.017(11) 0.000 N4 0.079(13) 0.105(12) 0.027(11) 0.000 -0.002(11) 0.000 C1 0.095(13) 0.038(15) 0.125(14) -0.007(13) 0.029(12) 0.000(13) C2 0.051(13) 0.061(14) 0.117(16) 0.027(14) 0.048(13) 0.025(12) C3 0.074(13) 0.094(16) 0.124(16) -0.015(13) 0.037(15) -0.006(13) C4 0.097(15) 0.072(15) 0.052(13) -0.019(17) 0.001(12) -0.010(15) C5 0.048(16) 0.062(17) 0.000(15) 0.000 -0.012(14) 0.000 C6 0.099(13) 0.061(11) 0.040(11) 0.014(12) -0.005(11) 0.010(13) C7 0.074(13) 0.061(11) 0.082(13) 0.008(13) -0.006(12) 0.010(11) C8 0.009(14) 0.19(2) 0.022(15) 0.000 0.016(14) 0.000 C9 0.053(16) 0.077(17) 0.014(15) 0.000 -0.028(15) 0.000 C10 0.054(18) 0.15(2) 0.053(17) 0.000 0.044(16) 0.000 C11 0.12(2) 0.017(17) 0.053(18) 0.000 0.048(18) 0.000 C12 0.091(18) 0.11(2) 0.039(17) 0.000 0.000(18) 0.000 C13 0.14(2) 0.11(2) 0.042(17) 0.000 0.047(18) 0.000 _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 S1 2.135(4) 3_666 ? Ni1 S1 2.135(4) . ? Ni1 S2 2.137(4) . ? Ni1 S2 2.137(4) 3_666 ? S1 C2 1.671(15) . ? S2 C4 1.741(16) . ? N1 C1 1.166(16) . ? N2 C3 1.144(18) . ? N3 C7 1.304(15) 4_565 ? N3 C7 1.304(15) . ? N3 C8 1.560(18) . ? N4 C5 1.363(18) . ? C1 C2 1.409(18) . ? C2 C4 1.34(2) 3_666 ? C3 C4 1.447(18) . ? C4 C2 1.34(2) 3_666 ? C5 C6 1.398(15) . ? C5 C6 1.398(15) 4_565 ? C6 C7 1.400(16) . ? C8 C9 1.512(18) . ? C9 C10 1.537(18) . ? C10 C11 1.483(19) . ? C11 C12 1.550(19) . ? C12 C13 1.52(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 S1 Ni1 S1 180.000(2) 3_666 . ? S1 Ni1 S2 92.72(15) 3_666 . ? S1 Ni1 S2 87.28(15) . . ? S1 Ni1 S2 87.28(15) 3_666 3_666 ? S1 Ni1 S2 92.72(15) . 3_666 ? S2 Ni1 S2 180.00(13) . 3_666 ? C2 S1 Ni1 102.7(5) . . ? C4 S2 Ni1 102.6(5) . . ? C7 N3 C7 118.2(17) 4_565 . ? C7 N3 C8 120.9(9) 4_565 . ? C7 N3 C8 120.9(9) . . ? N1 C1 C2 174.3(16) . . ? C4 C2 C1 118.1(15) 3_666 . ? C4 C2 S1 123.4(13) 3_666 . ? C1 C2 S1 118.5(11) . . ? N2 C3 C4 177.1(16) . . ? C2 C4 C3 126.9(16) 3_666 . ? C2 C4 S2 118.4(13) 3_666 . ? C3 C4 S2 113.8(12) . . ? N4 C5 C6 119.3(9) . . ? N4 C5 C6 119.3(9) . 4_565 ? C6 C5 C6 120.8(17) . 4_565 ? C7 C6 C5 115.4(14) . . ? N3 C7 C6 124.6(14) . . ? C9 C8 N3 107.1(12) . . ? C8 C9 C10 109.6(13) . . ? C11 C10 C9 113.4(13) . . ? C10 C11 C12 115.1(14) . . ? C13 C12 C11 116.6(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.375 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.084 #======================END