Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_general _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry ' _publ_contact_author 'Dr Reizo Kato' _publ_contact_author ; Dr Reizo Kato Institute of Molecular Science Myodaiji Okazaki 444-8585 JAPAN ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone 81-48-467-9408 _publ_contact_author_fax 81-48-462-4661 _publ_contact_author_email reizo@postman.riken.go.jp loop_ _publ_author_name _publ_author_address 'Fujiwara, Masahiro' 'Kato, Reizo' 'Watanabe, Eiji' 'Yamaura, Jun-Ichi' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_Ni(edo)2_neutral _database_code_CSD 162731 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Dec 18 22:32:35 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'Mac Denzo' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 355.09 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H8 O4 Ni S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.557(6) _cell_length_b 15.26(1) _cell_length_c 4.451(5) _cell_angle_alpha 90.29(4) _cell_angle_beta 97.90(6) _cell_angle_gamma 86.77(5) _cell_volume 641.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.008 _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 360.00 _exptl_absorpt_coefficient_mu 2.158 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Sience M18X' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imagin Plate' _diffrn_measurement_device 'Mac Science DIP320' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l / / / _diffrn_reflns_number 1738 _reflns_number_total 1738 _reflns_number_observed 748 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.146 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 2 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 16 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 16 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ni(1) 0.0000 0.0000 0.0000 0.052(1) Uani d . 0.50 S Ni(2) -0.5000 0.5000 0.0000 0.045(1) Uani d . 0.50 S S(1) 0.0233(6) 0.1145(3) 0.282(1) 0.064(2) Uani d . 1.00 . S(2) 0.2246(5) -0.0184(3) -0.006(1) 0.063(2) Uani d . 1.00 . S(3) -0.3278(5) 0.5412(3) -0.217(1) 0.059(2) Uani d . 1.00 . S(4) -0.4079(5) 0.3695(3) 0.069(1) 0.050(2) Uani d . 1.00 . O(1) 0.243(1) 0.1963(7) 0.500(3) 0.082(5) Uani d . 1.00 . O(2) 0.435(1) 0.0726(7) 0.239(3) 0.067(5) Uani d . 1.00 . O(3) -0.100(1) 0.4562(7) -0.329(3) 0.074(5) Uani d . 1.00 . O(4) -0.174(1) 0.2973(7) -0.083(3) 0.078(5) Uani d . 1.00 . C(1) 0.197(2) 0.125(1) 0.329(4) 0.066(7) Uani d . 1.00 . C(2) 0.294(2) 0.066(1) 0.200(4) 0.051(6) Uani d . 1.00 . C(3) 0.383(2) 0.215(1) 0.462(5) 0.101(9) Uani d . 1.00 . C(4) 0.485(2) 0.139(1) 0.468(4) 0.064(7) Uani d . 1.00 . C(5) -0.221(1) 0.4489(10) -0.208(4) 0.043(6) Uani d . 1.00 . C(6) -0.258(2) 0.371(1) -0.086(4) 0.050(6) Uani d . 1.00 . C(7) -0.006(2) 0.382(1) -0.277(5) 0.094(9) Uani d . 1.00 . C(8) -0.063(3) 0.301(2) -0.263(6) 0.13(1) Uani d . 1.00 . H(1) 0.3813 0.2433 0.2560 0.1260 Uiso calc . 1.00 . H(2) 0.4181 0.2603 0.6009 0.1260 Uiso calc . 1.00 . H(3) 0.4955 0.1142 0.6752 0.0781 Uiso calc . 1.00 . H(4) 0.5794 0.1562 0.4439 0.0781 Uiso calc . 1.00 . H(5) 0.0624 0.3802 -0.4279 0.1072 Uiso calc . 1.00 . H(6) 0.0570 0.3881 -0.0821 0.1072 Uiso calc . 1.00 . H(7) 0.0094 0.2551 -0.2108 0.1561 Uiso calc . 1.00 . H(8) -0.1019 0.2874 -0.4799 0.1561 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.056(3) 0.049(2) 0.051(3) -0.004(2) 0.003(2) -0.003(2) Ni(2) 0.045(2) 0.043(2) 0.048(3) -0.009(1) 0.005(2) -0.005(2) S(1) 0.073(4) 0.053(3) 0.067(4) -0.002(2) 0.008(3) -0.014(3) S(2) 0.050(4) 0.067(3) 0.067(4) -0.003(2) -0.002(3) -0.011(3) S(3) 0.062(4) 0.052(3) 0.066(4) -0.005(2) 0.018(3) 0.007(3) S(4) 0.052(3) 0.048(3) 0.051(4) -0.005(2) 0.010(2) 0.001(2) O(1) 0.11(1) 0.066(8) 0.07(1) -0.027(7) -0.004(8) -0.026(7) O(2) 0.047(9) 0.083(8) 0.07(1) -0.020(6) 0.013(7) -0.003(7) O(3) 0.09(1) 0.061(8) 0.08(1) 0.009(7) 0.026(8) 0.006(7) O(4) 0.12(1) 0.055(8) 0.06(1) 0.028(7) 0.020(8) 0.001(7) C(1) 0.11(2) 0.05(1) 0.03(1) -0.03(1) -0.01(1) 0.005(10) C(2) 0.05(1) 0.08(1) 0.03(1) -0.021(9) 0.017(9) -0.016(10) C(3) 0.05(2) 0.12(2) 0.14(2) -0.04(1) 0.02(1) -0.06(2) C(4) 0.01(1) 0.10(1) 0.08(2) -0.010(10) 0.015(10) 0.00(1) C(5) 0.02(1) 0.07(1) 0.05(1) -0.021(7) 0.012(8) 0.015(9) C(6) 0.07(1) 0.049(10) 0.02(1) 0.024(9) 0.007(9) -0.021(9) C(7) 0.04(2) 0.10(2) 0.15(2) -0.01(1) 0.05(1) 0.01(1) C(8) 0.11(2) 0.13(2) 0.15(3) 0.07(2) 0.07(2) 0.00(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 748 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0716 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0692 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.003 _refine_ls_shift/esd_max 2.0030 _refine_ls_shift/esd_mean 0.3990 _refine_diff_density_min -0.72 _refine_diff_density_max 0.66 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.149(5) 1_555 1_555 yes Ni(1) S(1) 2.149(5) 1_555 2_555 yes Ni(1) S(2) 2.152(5) 1_555 1_555 yes Ni(1) S(2) 2.152(5) 1_555 2_555 yes Ni(2) S(3) 2.145(5) 1_555 1_555 yes Ni(2) S(3) 2.145(5) 1_555 2_465 yes Ni(2) S(4) 2.138(4) 1_555 1_555 yes Ni(2) S(4) 2.138(4) 1_555 2_465 yes S(1) C(1) 1.66(2) 1_555 1_555 yes S(2) C(2) 1.69(2) 1_555 1_555 yes S(3) C(5) 1.69(2) 1_555 1_555 yes S(4) C(6) 1.68(2) 1_555 1_555 yes O(1) C(1) 1.38(2) 1_555 1_555 yes O(1) C(3) 1.42(2) 1_555 1_555 yes O(2) C(2) 1.34(2) 1_555 1_555 yes O(2) C(4) 1.48(2) 1_555 1_555 yes O(3) C(5) 1.36(2) 1_555 1_555 yes O(3) C(7) 1.40(2) 1_555 1_555 yes O(4) C(6) 1.34(2) 1_555 1_555 yes O(4) C(8) 1.42(3) 1_555 1_555 yes C(1) C(2) 1.43(2) 1_555 1_555 yes C(3) C(4) 1.46(2) 1_555 1_555 yes C(5) C(6) 1.38(2) 1_555 1_555 yes C(7) C(8) 1.38(3) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(1) 180.0 1_555 1_555 2_555 yes S(1) Ni(1) S(2) 92.5(2) 1_555 1_555 1_555 yes S(1) Ni(1) S(2) 87.5(2) 1_555 1_555 2_555 yes S(1) Ni(1) S(2) 87.5(2) 2_555 1_555 1_555 yes S(1) Ni(1) S(2) 92.5(2) 2_555 1_555 2_555 yes S(2) Ni(1) S(2) 180.0 1_555 1_555 2_555 yes S(3) Ni(2) S(3) 180.0 1_555 1_555 2_465 yes S(3) Ni(2) S(4) 92.7(2) 1_555 1_555 1_555 yes S(3) Ni(2) S(4) 87.3(2) 1_555 1_555 2_465 yes S(3) Ni(2) S(4) 87.3(2) 2_465 1_555 1_555 yes S(3) Ni(2) S(4) 92.7(2) 2_465 1_555 2_465 yes S(4) Ni(2) S(4) 180.0 1_555 1_555 2_465 yes Ni(1) S(1) C(1) 102.7(7) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 104.5(7) 1_555 1_555 1_555 yes Ni(2) S(3) C(5) 102.3(5) 1_555 1_555 1_555 yes Ni(2) S(4) C(6) 103.6(5) 1_555 1_555 1_555 yes C(1) O(1) C(3) 111(1) 1_555 1_555 1_555 yes C(2) O(2) C(4) 113(1) 1_555 1_555 1_555 yes C(5) O(3) C(7) 113(1) 1_555 1_555 1_555 yes C(6) O(4) C(8) 114(1) 1_555 1_555 1_555 yes S(1) C(1) O(1) 115(1) 1_555 1_555 1_555 yes S(1) C(1) C(2) 123(1) 1_555 1_555 1_555 yes O(1) C(1) C(2) 121(1) 1_555 1_555 1_555 yes S(2) C(2) O(2) 118(1) 1_555 1_555 1_555 yes S(2) C(2) C(1) 116(1) 1_555 1_555 1_555 yes O(2) C(2) C(1) 124(1) 1_555 1_555 1_555 yes O(1) C(3) C(4) 116(1) 1_555 1_555 1_555 yes O(1) C(3) H(1) 108(1) 1_555 1_555 1_555 no O(1) C(3) H(2) 110(1) 1_555 1_555 1_555 no C(4) C(3) H(1) 105(1) 1_555 1_555 1_555 no C(4) C(3) H(2) 111(1) 1_555 1_555 1_555 no H(1) C(3) H(2) 102(1) 1_555 1_555 1_555 no O(2) C(4) C(3) 111(1) 1_555 1_555 1_555 yes O(2) C(4) H(3) 110(1) 1_555 1_555 1_555 no O(2) C(4) H(4) 111(1) 1_555 1_555 1_555 no C(3) C(4) H(3) 106(1) 1_555 1_555 1_555 no C(3) C(4) H(4) 111(1) 1_555 1_555 1_555 no H(3) C(4) H(4) 104(1) 1_555 1_555 1_555 no S(3) C(5) O(3) 115.4(10) 1_555 1_555 1_555 yes S(3) C(5) C(6) 121(1) 1_555 1_555 1_555 yes O(3) C(5) C(6) 122(1) 1_555 1_555 1_555 yes S(4) C(6) O(4) 118(1) 1_555 1_555 1_555 yes S(4) C(6) C(5) 119(1) 1_555 1_555 1_555 yes O(4) C(6) C(5) 121(1) 1_555 1_555 1_555 yes O(3) C(7) C(8) 117(1) 1_555 1_555 1_555 yes O(3) C(7) H(5) 109(1) 1_555 1_555 1_555 no O(3) C(7) H(6) 110(1) 1_555 1_555 1_555 no C(8) C(7) H(5) 109(2) 1_555 1_555 1_555 no C(8) C(7) H(6) 105(2) 1_555 1_555 1_555 no H(5) C(7) H(6) 102(1) 1_555 1_555 1_555 no O(4) C(8) C(7) 115(1) 1_555 1_555 1_555 yes O(4) C(8) H(7) 111(2) 1_555 1_555 1_555 no O(4) C(8) H(8) 108(2) 1_555 1_555 1_555 no C(7) C(8) H(7) 111(2) 1_555 1_555 1_555 no C(7) C(8) H(8) 104(2) 1_555 1_555 1_555 no H(7) C(8) H(8) 103(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(1) O(4) 3.55(1) 1_555 1_555 ? O(1) C(8) 3.54(3) 1_555 1_556 ? O(2) O(2) 3.29(2) 1_555 2_656 ? O(2) O(2) 3.37(3) 1_555 2_655 ? O(2) C(4) 3.49(2) 1_555 2_656 ? O(3) O(3) 2.98(2) 1_555 2_564 ? O(3) C(7) 3.32(3) 1_555 2_564 ? O(3) O(3) 3.57(3) 1_555 2_565 ? #------------------------------------------------------------------------------ data_Ni(dmit)(edo) neutral _database_code_CSD 162732 #------------------------------------------------------------------------------ _audit_creation_date 'Wed May 26 23:44:35 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'Mac Denzo' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 403.23 _chemical_formula_analytical ? _chemical_formula_sum 'C7 H4 O2 Ni S7 ' _chemical_formula_moiety 'C7 H4 O2 Ni S7 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.913(2) _cell_length_b 15.882(3) _cell_length_c 8.240(1) _cell_angle_alpha 90 _cell_angle_beta 124.06(1) _cell_angle_gamma 90 _cell_volume 1291.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c ' _symmetry_Int_Tables_number 9 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,1/2+z 1/2+x,1/2+y,z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.740 _exptl_crystal_size_mid 0.455 _exptl_crystal_size_min 0.455 _exptl_crystal_density_diffrn 2.074 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 808.00 _exptl_absorpt_coefficient_mu 2.614 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Sience M18X' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imagin Plate' _diffrn_measurement_device 'Mac Science DIP320' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 1647 _reflns_number_total 1647 _reflns_number_observed 1087 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 4 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 28 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 28 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 16 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ni 0.749(4) 0.09142(3) 0.661(5) 0.0481(2) Uani d . 1.00 . S(1) 0.897(4) -0.0007(2) 0.703(5) 0.0568(9) Uani d . 1.00 . S(2) 0.609(4) -0.0015(3) 0.630(5) 0.0557(10) Uani d . 1.00 . S(3) 0.889(4) 0.1839(2) 0.685(5) 0.0575(10) Uani d . 1.00 . S(4) 0.616(4) 0.1859(2) 0.648(5) 0.055(1) Uani d . 1.00 . S(5) 0.886(4) -0.1910(3) 0.700(5) 0.057(1) Uani d . 1.00 . S(6) 0.618(4) -0.1921(2) 0.626(5) 0.059(1) Uani d . 1.00 . S(7) 0.749(4) -0.35465(8) 0.659(5) 0.0733(4) Uani d . 1.00 . O(1) 0.872(4) 0.3506(6) 0.675(5) 0.053(2) Uani d . 1.00 . O(2) 0.628(4) 0.3458(6) 0.659(5) 0.067(3) Uani d . 1.00 . C(1) 0.819(4) -0.0939(7) 0.680(5) 0.060(2) Uani d . 1.00 . C(2) 0.692(4) -0.0929(7) 0.649(5) 0.034(3) Uani d . 1.00 . C(3) 0.816(4) 0.2789(9) 0.677(5) 0.058(3) Uani d . 1.00 . C(4) 0.695(4) 0.2739(10) 0.667(5) 0.038(3) Uani d . 1.00 . C(5) 0.746(4) -0.2516(2) 0.650(6) 0.049(1) Uani d . 1.00 . C(6) 0.792(4) 0.4201(8) 0.620(5) 0.068(3) Uani d . 1.00 . C(7) 0.717(4) 0.4266(8) 0.713(5) 0.075(4) Uani d . 1.00 . H(1) 0.8319 0.4708 0.6022 0.0733 Uiso calc . 1.00 . H(2) 0.7154 0.4154 0.4403 0.0733 Uiso calc . 1.00 . H(3) 0.6410 0.4779 0.6206 0.0944 Uiso calc . 1.00 . H(4) 0.7632 0.4400 0.8127 0.0944 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0486(3) 0.0344(3) 0.0655(4) 0.0079(8) 0.0346(3) 0.005(1) S(1) 0.048(2) 0.036(1) 0.084(2) 0.005(1) 0.035(2) 0.002(2) S(2) 0.054(2) 0.039(2) 0.095(3) 0.005(1) 0.054(2) 0.000(2) S(3) 0.048(2) 0.042(1) 0.079(3) 0.004(1) 0.033(2) 0.009(2) S(4) 0.059(2) 0.031(2) 0.095(3) 0.000(1) 0.056(2) -0.003(2) S(5) 0.061(2) 0.034(2) 0.089(3) -0.006(2) 0.050(2) -0.007(2) S(6) 0.056(2) 0.042(2) 0.083(3) -0.018(2) 0.043(2) -0.015(2) S(7) 0.0997(10) 0.0352(6) 0.098(1) 0.007(3) 0.0631(9) 0.004(3) O(1) 0.051(4) 0.028(4) 0.078(6) 0.003(3) 0.035(4) 0.023(5) O(2) 0.079(6) 0.036(3) 0.120(7) 0.000(3) 0.076(6) 0.009(5) C(1) 0.047(5) 0.039(2) 0.094(8) -0.006(2) 0.040(7) -0.021(4) C(2) 0.056(5) 0.035(2) 0.027(9) -0.012(2) 0.033(7) -0.021(5) C(3) 0.050(5) 0.031(3) 0.090(7) -0.018(3) 0.037(6) -0.012(5) C(4) 0.056(6) 0.041(3) 0.028(7) -0.013(4) 0.030(7) -0.011(6) C(5) 0.055(3) 0.036(1) 0.048(3) -0.012(3) 0.024(3) -0.005(7) C(6) 0.059(6) 0.023(3) 0.13(1) -0.007(3) 0.053(6) 0.005(5) C(7) 0.114(8) 0.045(5) 0.10(1) -0.038(5) 0.084(8) -0.035(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1087 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0443 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0457 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.387 _refine_ls_shift/esd_max 7.5460 _refine_ls_shift/esd_mean 1.6020 _refine_diff_density_min -0.50 _refine_diff_density_max 0.85 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S(1) 2.161(9) 1_555 1_555 yes Ni S(2) 2.137(10) 1_555 1_555 yes Ni S(3) 2.145(9) 1_555 1_555 yes Ni S(4) 2.140(8) 1_555 1_555 yes S(1) C(1) 1.70(3) 1_555 1_555 yes S(2) C(2) 1.72(3) 1_555 1_555 yes S(3) C(3) 1.72(3) 1_555 1_555 yes S(4) C(4) 1.64(3) 1_555 1_555 yes S(5) C(1) 1.70(2) 1_555 1_555 yes S(5) C(5) 1.76(2) 1_555 1_555 yes S(6) C(2) 1.76(2) 1_555 1_555 yes S(6) C(5) 1.71(3) 1_555 1_555 yes S(7) C(5) 1.638(8) 1_555 1_555 yes O(1) C(3) 1.32(3) 1_555 1_555 yes O(1) C(6) 1.36(3) 1_555 1_555 yes O(2) C(4) 1.37(3) 1_555 1_555 yes O(2) C(7) 1.56(3) 1_555 1_555 yes C(1) C(2) 1.380(10) 1_555 1_555 yes C(3) C(4) 1.406(10) 1_555 1_555 yes C(6) C(7) 1.47(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni S(2) 93.70(8) 1_555 1_555 1_555 yes S(1) Ni S(3) 85.9(4) 1_555 1_555 1_555 yes S(1) Ni S(4) 174.6(5) 1_555 1_555 1_555 yes S(2) Ni S(3) 178.5(5) 1_555 1_555 1_555 yes S(2) Ni S(4) 88.3(3) 1_555 1_555 1_555 yes S(3) Ni S(4) 92.22(9) 1_555 1_555 1_555 yes Ni S(1) C(1) 102(1) 1_555 1_555 1_555 yes Ni S(2) C(2) 101(1) 1_555 1_555 1_555 yes Ni S(3) C(3) 104(1) 1_555 1_555 1_555 yes Ni S(4) C(4) 103(1) 1_555 1_555 1_555 yes C(1) S(5) C(5) 98(1) 1_555 1_555 1_555 yes C(2) S(6) C(5) 96(1) 1_555 1_555 1_555 yes C(3) O(1) C(6) 116(2) 1_555 1_555 1_555 yes C(4) O(2) C(7) 113(2) 1_555 1_555 1_555 yes S(1) C(1) S(5) 125(2) 1_555 1_555 1_555 yes S(1) C(1) C(2) 118(2) 1_555 1_555 1_555 yes S(5) C(1) C(2) 115(2) 1_555 1_555 1_555 yes S(2) C(2) S(6) 121(2) 1_555 1_555 1_555 yes S(2) C(2) C(1) 122(2) 1_555 1_555 1_555 yes S(6) C(2) C(1) 116(2) 1_555 1_555 1_555 yes S(3) C(3) O(1) 120(2) 1_555 1_555 1_555 yes S(3) C(3) C(4) 115(2) 1_555 1_555 1_555 yes O(1) C(3) C(4) 123(3) 1_555 1_555 1_555 yes S(4) C(4) O(2) 115(2) 1_555 1_555 1_555 yes S(4) C(4) C(3) 124(3) 1_555 1_555 1_555 yes O(2) C(4) C(3) 120(3) 1_555 1_555 1_555 yes S(5) C(5) S(6) 113.0(5) 1_555 1_555 1_555 yes S(5) C(5) S(7) 122(1) 1_555 1_555 1_555 yes S(6) C(5) S(7) 123(1) 1_555 1_555 1_555 yes O(1) C(6) C(7) 113(2) 1_555 1_555 1_555 yes O(1) C(6) H(1) 114(4) 1_555 1_555 1_555 no O(1) C(6) H(2) 105(3) 1_555 1_555 1_555 no C(7) C(6) H(1) 120(4) 1_555 1_555 1_555 no C(7) C(6) H(2) 111(4) 1_555 1_555 1_555 no H(1) C(6) H(2) 88(4) 1_555 1_555 1_555 no O(2) C(7) C(6) 107(2) 1_555 1_555 1_555 yes O(2) C(7) H(3) 103(3) 1_555 1_555 1_555 no O(2) C(7) H(4) 122(5) 1_555 1_555 1_555 no C(6) C(7) H(3) 101(4) 1_555 1_555 1_555 no C(6) C(7) H(4) 108(7) 1_555 1_555 1_555 no H(3) C(7) H(4) 111(4) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(3) O(2) 3.34(2) 1_555 4_555 ? S(4) O(1) 3.36(2) 1_555 4_454 ? S(4) C(3) 3.55(3) 1_555 4_454 ? S(4) S(5) 3.587(10) 1_555 3_455 ? S(5) O(2) 3.15(2) 1_555 3_545 ? S(5) S(6) 3.544(3) 1_555 4_545 ? S(6) O(1) 3.25(2) 1_555 3_445 ? S(7) O(2) 3.53(3) 1_555 2_554 ? S(7) C(7) 3.55(3) 1_555 1_545 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_Ni(edo)(mnt) _database_code_CSD 162733 _audit_creation_date 'Thu Nov 25 18:34:33 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C8 H4 N2 O2 Ni S4 ' _chemical_formula_moiety 'C8 H4 N2 O2 Ni S4 ' _chemical_formula_weight 347.07 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 25.420(4) _cell_length_b 7.7460(8) _cell_length_c 6.0710(8) _cell_angle_alpha 90 _cell_angle_beta 91.670(7) _cell_angle_gamma 90 _cell_volume 1194.9(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.580 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.309 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type Imaging Plate _diffrn_reflns_number 2931 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 30.25 _diffrn_measured_fraction_theta_max 0.7568 _diffrn_reflns_theta_full 30.25 _diffrn_measured_fraction_theta_full 0.7568 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2693 _reflns_number_gt 1713 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.1820 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1713 _refine_ls_number_parameters 155 _refine_ls_goodness_of_fit_ref 2.583 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 3.2805 _refine_diff_density_max 2.60 _refine_diff_density_min -0.76 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 0.21761(4) 0.3166(1) 0.5502(2) 0.0371(3) Uani 1.00 d . . . S(1) S 0.14528(8) 0.3940(3) 0.3807(4) 0.0460(7) Uani 1.00 d . . . S(2) S 0.17520(8) 0.2164(3) 0.8241(3) 0.0443(6) Uani 1.00 d . . . S(3) S 0.25936(8) 0.4092(3) 0.2735(3) 0.0385(6) Uani 1.00 d . . . S(4) S 0.28703(8) 0.2245(3) 0.7144(3) 0.0415(6) Uani 1.00 d . . . O(1) O 0.0482(2) 0.3416(9) 0.480(1) 0.060(2) Uani 1.00 d . . . O(2) O 0.0765(2) 0.1730(9) 0.881(1) 0.057(2) Uani 1.00 d . . . N(1) N 0.3978(3) 0.428(1) 0.076(1) 0.060(3) Uani 1.00 d . . . N(2) N 0.4299(3) 0.169(1) 0.629(2) 0.077(3) Uani 1.00 d . . . C(1) C 0.0983(3) 0.322(1) 0.544(1) 0.040(2) Uani 1.00 d . . . C(2) C 0.1127(3) 0.240(1) 0.749(1) 0.039(2) Uani 1.00 d . . . C(3) C 0.3230(3) 0.348(1) 0.336(1) 0.037(2) Uani 1.00 d . . . C(4) C 0.3353(3) 0.2674(9) 0.529(1) 0.032(2) Uani 1.00 d . . . C(5) C 0.0104(4) 0.302(1) 0.647(2) 0.081(4) Uani 1.00 d . . . C(6) C 0.0232(4) 0.161(2) 0.779(2) 0.081(4) Uani 1.00 d . . . C(7) C 0.3638(3) 0.393(1) 0.186(1) 0.042(2) Uani 1.00 d . . . C(8) C 0.3877(3) 0.217(1) 0.585(1) 0.044(3) Uani 1.00 d . . . H(1) H 0.0073 0.4006 0.7391 0.0972 Uiso 1.00 calc . . . H(2) H -0.0226 0.2798 0.5745 0.0972 Uiso 1.00 calc . . . H(3) H 0.0212 0.0595 0.6915 0.0975 Uiso 1.00 calc . . . H(4) H -0.0016 0.1536 0.8931 0.0975 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0293(5) 0.0487(9) 0.0332(5) -0.0016(4) 0.0002(4) 0.0035(4) S(1) 0.036(1) 0.059(2) 0.043(1) 0.0016(9) -0.0030(8) 0.0106(10) S(2) 0.034(1) 0.059(2) 0.040(1) -0.0024(9) -0.0011(8) 0.0085(9) S(3) 0.037(1) 0.042(2) 0.037(1) 0.0009(8) 0.0013(8) 0.0065(8) S(4) 0.0322(10) 0.054(2) 0.038(1) 0.0016(9) -0.0014(8) 0.0091(9) O(1) 0.031(3) 0.077(5) 0.070(4) 0.003(3) -0.005(3) 0.013(4) O(2) 0.042(3) 0.074(5) 0.057(4) -0.001(3) 0.014(3) 0.011(3) N(1) 0.050(5) 0.068(6) 0.064(5) 0.003(4) 0.018(4) 0.011(4) N(2) 0.039(4) 0.118(8) 0.073(6) 0.018(5) 0.000(4) 0.021(5) C(1) 0.037(4) 0.032(5) 0.052(5) 0.005(3) -0.007(3) 0.007(4) C(2) 0.042(4) 0.030(5) 0.044(5) -0.002(3) 0.002(3) -0.008(3) C(3) 0.034(4) 0.038(5) 0.039(4) -0.008(3) 0.003(3) -0.001(3) C(4) 0.035(4) 0.013(4) 0.049(4) 0.001(3) -0.004(3) -0.006(3) C(5) 0.038(5) 0.074(9) 0.13(1) -0.009(5) 0.014(6) 0.029(7) C(6) 0.038(5) 0.104(10) 0.103(10) 0.002(6) 0.010(6) 0.021(7) C(7) 0.040(4) 0.043(6) 0.043(4) 0.005(4) 0.007(3) 0.003(4) C(8) 0.038(4) 0.045(6) 0.048(5) -0.003(4) 0.002(4) 0.006(4) #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.165(2) . . yes Ni(1) S(2) 2.153(2) . . yes Ni(1) S(3) 2.137(2) . . yes Ni(1) S(4) 2.125(2) . . yes S(1) C(1) 1.671(9) . . yes S(2) C(2) 1.652(8) . . yes S(3) C(3) 1.717(8) . . yes S(4) C(4) 1.722(8) . . yes O(1) C(1) 1.331(9) . . yes O(1) C(5) 1.45(1) . . yes O(2) C(2) 1.343(9) . . yes O(2) C(6) 1.47(1) . . yes N(1) C(7) 1.142(10) . . yes N(2) C(8) 1.16(1) . . yes C(1) C(2) 1.43(1) . . yes C(3) C(4) 1.35(1) . . yes C(3) C(7) 1.44(1) . . yes C(4) C(8) 1.42(1) . . yes C(5) C(6) 1.39(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(2) 91.69(8) 1_555 1_555 1_555 yes S(1) Ni(1) S(3) 88.15(8) 1_555 1_555 1_555 yes S(1) Ni(1) S(4) 176.4(1) 1_555 1_555 1_555 yes S(2) Ni(1) S(3) 178.4(1) 1_555 1_555 1_555 yes S(2) Ni(1) S(4) 86.80(8) 1_555 1_555 1_555 yes S(3) Ni(1) S(4) 93.26(8) 1_555 1_555 1_555 yes Ni(1) S(1) C(1) 103.7(3) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 104.2(3) 1_555 1_555 1_555 yes Ni(1) S(3) C(3) 102.7(3) 1_555 1_555 1_555 yes Ni(1) S(4) C(4) 103.1(3) 1_555 1_555 1_555 yes C(1) O(1) C(5) 115.0(8) 1_555 1_555 1_555 yes C(2) O(2) C(6) 114.3(7) 1_555 1_555 1_555 yes S(1) C(1) O(1) 118.9(6) 1_555 1_555 1_555 yes S(1) C(1) C(2) 119.7(6) 1_555 1_555 1_555 yes O(1) C(1) C(2) 121.4(7) 1_555 1_555 1_555 yes S(2) C(2) O(2) 117.5(6) 1_555 1_555 1_555 yes S(2) C(2) C(1) 120.5(6) 1_555 1_555 1_555 yes O(2) C(2) C(1) 121.9(7) 1_555 1_555 1_555 yes S(3) C(3) C(4) 120.8(6) 1_555 1_555 1_555 yes S(3) C(3) C(7) 118.9(6) 1_555 1_555 1_555 yes C(4) C(3) C(7) 120.3(7) 1_555 1_555 1_555 yes S(4) C(4) C(3) 120.2(6) 1_555 1_555 1_555 yes S(4) C(4) C(8) 118.1(6) 1_555 1_555 1_555 yes C(3) C(4) C(8) 121.7(7) 1_555 1_555 1_555 yes O(1) C(5) C(6) 114.8(9) 1_555 1_555 1_555 yes O(1) C(5) H(1) 109.6(9) 1_555 1_555 1_555 no O(1) C(5) H(2) 109(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 107(1) 1_555 1_555 1_555 no C(6) C(5) H(2) 109.1(10) 1_555 1_555 1_555 no H(1) C(5) H(2) 105(1) 1_555 1_555 1_555 no O(2) C(6) C(5) 112.9(9) 1_555 1_555 1_555 yes O(2) C(6) H(3) 109.4(9) 1_555 1_555 1_555 no O(2) C(6) H(4) 109(1) 1_555 1_555 1_555 no C(5) C(6) H(3) 108(1) 1_555 1_555 1_555 no C(5) C(6) H(4) 110(1) 1_555 1_555 1_555 no H(3) C(6) H(4) 105(1) 1_555 1_555 1_555 no N(1) C(7) C(3) 176.6(9) 1_555 1_555 1_555 yes N(2) C(8) C(4) 177(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Ni(1) S(1) C(1) O(1) -176.6(6) 1_555 1_555 1_555 1_555 yes Ni(1) S(1) C(1) C(2) 2.9(8) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) O(2) 174.0(6) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) C(1) -3.3(7) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(3) C(4) -2.1(7) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(3) C(7) -178.6(6) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(4) C(3) 2.1(7) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(4) C(8) -178.5(6) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(2) C(2) 3.9(3) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(3) C(3) -174.1(3) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(4) C(4) 110(1) 1_555 1_555 1_555 1_555 yes S(1) C(1) O(1) C(5) -170.2(7) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) S(2) 0(1) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) O(2) -176.9(6) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(1) C(1) -3.8(3) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(3) C(3) -89(3) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(4) C(4) 175.7(3) 1_555 1_555 1_555 1_555 yes S(2) C(2) O(2) C(6) -165.9(7) 1_555 1_555 1_555 1_555 yes S(2) C(2) C(1) O(1) 179.7(6) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(1) C(1) 174.6(3) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(2) C(2) -80(3) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(4) C(4) -2.6(3) 1_555 1_555 1_555 1_555 yes S(3) C(3) C(4) S(4) 0.1(10) 1_555 1_555 1_555 1_555 yes S(3) C(3) C(4) C(8) -179.3(6) 1_555 1_555 1_555 1_555 yes S(3) C(3) C(7) N(1) 156(15) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(1) C(1) 61(1) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(2) C(2) -172.9(3) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(3) C(3) 2.6(3) 1_555 1_555 1_555 1_555 yes S(4) C(4) C(3) C(7) 176.5(6) 1_555 1_555 1_555 1_555 yes S(4) C(4) C(8) N(2) 78(18) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) O(2) 2(1) 1_555 1_555 1_555 1_555 yes O(1) C(5) C(6) O(2) 52(1) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(3) C(4) -19(16) 1_555 1_555 1_555 1_555 yes N(2) C(8) C(4) C(3) -102(17) 1_555 1_555 1_555 1_555 yes C(1) O(1) C(5) C(6) -38(1) 1_555 1_555 1_555 1_555 yes C(1) C(2) O(2) C(6) 11(1) 1_555 1_555 1_555 1_555 yes C(2) O(2) C(6) C(5) -38(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) O(1) C(5) 10(1) 1_555 1_555 1_555 1_555 yes C(7) C(3) C(4) C(8) -2(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni(1) S(4) 3.471(3) . 2_556 ? S(2) C(3) 3.519(8) . 2_546 ? O(1) C(5) 3.22(1) . 3_566 ? O(1) O(1) 3.48(1) . 3_566 ? O(1) N(1) 3.51(1) . 2_545 ? O(1) N(2) 3.51(1) . 2_556 ? O(2) N(1) 3.44(1) . 2_545 ? N(1) C(2) 3.13(1) . 2_555 ? N(1) C(1) 3.14(1) . 2_555 ? N(1) C(5) 3.39(1) . 4_554 ? N(1) C(8) 3.40(1) . 1_554 ? N(1) C(6) 3.45(1) . 4_554 ? N(1) N(2) 3.49(1) . 1_554 ? N(1) C(6) 3.49(1) . 2_555 ? N(2) C(1) 3.43(1) . 2_546 ? N(2) C(5) 3.48(2) . 2_546 ? N(2) C(6) 3.49(2) . 4_554 ? N(2) C(2) 3.58(1) . 2_546 ? C(5) C(5) 3.58(2) . 3_566 ? #------------------------------------------------------------------------------ data_[Ni(edo)2]3(PF6)2 _database_code_CSD 162734 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 18 21:28:49 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'Mac Denzo' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1355.19 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H24 F12 O12 Ni3 P2 S12 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 16.760(1) _cell_length_b 12.292(1) _cell_length_c 10.8640(7) _cell_angle_alpha 90 _cell_angle_beta 104.073(5) _cell_angle_gamma 90 _cell_volume 2171.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.520 _exptl_crystal_size_mid 0.480 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1356.00 _exptl_absorpt_coefficient_mu 2.046 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Sience M18X' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imagin Plate' _diffrn_measurement_device 'Mac Science DIP320' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 5592 _reflns_number_total 5592 _reflns_number_observed 3371 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.068 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 6 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 24 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 24 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 48 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 24 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ni(1) 0.07685(3) 0.27791(5) 0.18132(5) 0.0342(2) Uani d . 1.00 . Ni(2) 0.0000 0.5000 0.0000 0.0329(2) Uani d . 0.50 S S(1) 0.01818(7) 0.14066(10) 0.0700(1) 0.0416(3) Uani d . 1.00 . S(2) -0.04030(7) 0.34107(10) 0.2017(1) 0.0375(3) Uani d . 1.00 . S(3) 0.19372(7) 0.19737(10) 0.1893(1) 0.0411(3) Uani d . 1.00 . S(4) 0.13256(7) 0.38872(10) 0.3330(1) 0.0349(3) Uani d . 1.00 . S(5) 0.09107(6) 0.38140(9) -0.0300(1) 0.0360(3) Uani d . 1.00 . S(6) 0.09703(6) 0.59315(9) 0.1282(1) 0.0333(3) Uani d . 1.00 . P(1) 0.43792(8) 0.6317(1) -0.2142(1) 0.0635(5) Uani d . 1.00 . F(1) 0.3721(2) 0.5370(3) -0.2307(4) 0.107(1) Uani d . 1.00 . F(2) 0.5036(3) 0.5441(4) -0.2272(5) 0.153(2) Uani d . 1.00 . F(3) 0.5054(3) 0.7191(4) -0.2010(4) 0.141(2) Uani d . 1.00 . F(4) 0.3678(3) 0.7105(4) -0.2079(5) 0.142(2) Uani d . 1.00 . F(5) 0.4595(2) 0.6171(4) -0.0658(3) 0.112(2) Uani d . 1.00 . F(6) 0.4154(2) 0.6489(4) -0.3626(3) 0.114(2) Uani d . 1.00 . O(1) -0.1344(2) 0.1015(3) -0.0270(3) 0.0462(10) Uani d . 1.00 . O(2) -0.1883(2) 0.2700(3) 0.1120(3) 0.0428(9) Uani d . 1.00 . O(3) 0.3392(2) 0.2425(3) 0.3233(3) 0.051(1) Uani d . 1.00 . O(4) 0.2847(2) 0.4151(3) 0.4525(3) 0.051(1) Uani d . 1.00 . O(5) 0.2489(2) 0.4052(2) -0.0045(3) 0.0430(9) Uani d . 1.00 . O(6) 0.2537(2) 0.5972(2) 0.1439(3) 0.0393(9) Uani d . 1.00 . C(1) -0.0819(3) 0.1660(4) 0.0515(4) 0.036(1) Uani d . 1.00 . C(2) -0.1087(2) 0.2538(3) 0.1172(4) 0.032(1) Uani d . 1.00 . C(3) 0.2605(2) 0.2710(4) 0.2984(4) 0.035(1) Uani d . 1.00 . C(4) 0.2329(3) 0.3573(4) 0.3625(4) 0.036(1) Uani d . 1.00 . C(5) -0.2202(3) 0.1398(5) -0.0598(5) 0.048(2) Uani d . 1.00 . C(6) -0.2430(3) 0.1811(5) 0.0545(6) 0.051(2) Uani d . 1.00 . C(7) 0.3957(3) 0.3042(5) 0.4204(6) 0.068(2) Uani d . 1.00 . C(8) 0.3622(4) 0.3599(7) 0.5039(8) 0.135(3) Uani d . 1.00 . C(9) 0.1809(2) 0.4501(4) 0.0211(4) 0.033(1) Uani d . 1.00 . C(10) 0.1834(2) 0.5436(3) 0.0936(4) 0.030(1) Uani d . 1.00 . C(11) 0.3191(3) 0.4733(6) 0.0302(7) 0.104(3) Uani d . 1.00 . C(12) 0.3255(3) 0.5510(5) 0.1146(8) 0.100(2) Uani d . 1.00 . H(1) -0.223(2) 0.191(3) -0.118(4) 0.04(1) Uiso calc . 1.00 . H(2) -0.256(3) 0.075(4) -0.101(4) 0.06(1) Uiso calc . 1.00 . H(3) -0.296(3) 0.213(3) 0.038(4) 0.05(1) Uiso calc . 1.00 . H(4) -0.239(3) 0.123(4) 0.125(4) 0.06(1) Uiso calc . 1.00 . H(5) 0.4223 0.3590 0.3775 0.0828 Uiso calc . 1.00 . H(6) 0.4387 0.2576 0.4651 0.0828 Uiso calc . 1.00 . H(7) 0.3551 0.3069 0.5669 0.1593 Uiso calc . 1.00 . H(8) 0.4027 0.4116 0.5492 0.1593 Uiso calc . 1.00 . H(9) 0.3252 0.5089 -0.0463 0.1228 Uiso calc . 1.00 . H(10) 0.3661 0.4261 0.0577 0.1228 Uiso calc . 1.00 . H(11) 0.3595 0.5208 0.1939 0.1164 Uiso calc . 1.00 . H(12) 0.3573 0.6089 0.0908 0.1164 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0302(3) 0.0330(3) 0.0377(3) -0.0010(2) 0.0047(2) -0.0028(3) Ni(2) 0.0257(4) 0.0353(5) 0.0359(5) 0.0018(3) 0.0039(3) -0.0076(4) S(1) 0.0363(6) 0.0373(7) 0.0499(7) -0.0034(5) 0.0080(5) -0.0078(6) S(2) 0.0325(6) 0.0407(7) 0.0379(7) 0.0000(5) 0.0061(5) -0.0036(6) S(3) 0.0363(6) 0.0407(7) 0.0437(7) 0.0042(5) 0.0049(5) -0.0055(6) S(4) 0.0330(6) 0.0371(7) 0.0340(6) -0.0013(5) 0.0069(5) -0.0015(6) S(5) 0.0293(6) 0.0327(7) 0.0446(7) 0.0011(5) 0.0067(5) -0.0086(6) S(6) 0.0299(6) 0.0347(7) 0.0334(6) 0.0004(5) 0.0043(4) -0.0052(6) P(1) 0.0321(7) 0.097(1) 0.0569(10) 0.0010(8) 0.0015(6) 0.0135(9) F(1) 0.099(3) 0.110(3) 0.101(3) -0.034(2) 0.003(2) 0.012(3) F(2) 0.098(3) 0.184(5) 0.173(5) 0.069(3) 0.024(3) 0.019(4) F(3) 0.132(3) 0.201(5) 0.081(3) -0.113(3) 0.007(2) 0.002(3) F(4) 0.134(4) 0.147(4) 0.147(4) 0.069(3) 0.041(3) -0.009(3) F(5) 0.100(3) 0.171(4) 0.058(2) -0.044(3) 0.003(2) 0.017(3) F(6) 0.075(2) 0.201(4) 0.059(2) -0.011(3) 0.000(2) 0.034(3) O(1) 0.040(2) 0.039(2) 0.051(2) -0.006(1) -0.003(1) -0.006(2) O(2) 0.029(2) 0.048(2) 0.049(2) -0.002(1) 0.006(1) 0.001(2) O(3) 0.032(2) 0.062(2) 0.057(2) 0.004(2) 0.006(2) -0.010(2) O(4) 0.034(2) 0.057(2) 0.055(2) -0.004(2) -0.001(1) -0.015(2) O(5) 0.028(2) 0.046(2) 0.056(2) 0.001(1) 0.013(1) -0.007(2) O(6) 0.029(2) 0.038(2) 0.048(2) -0.005(1) 0.005(1) -0.008(2) C(1) 0.038(2) 0.032(3) 0.034(3) -0.006(2) 0.004(2) 0.007(2) C(2) 0.028(2) 0.035(3) 0.032(2) 0.000(2) 0.005(2) 0.012(2) C(3) 0.029(2) 0.042(3) 0.035(3) 0.004(2) 0.006(2) 0.006(2) C(4) 0.038(2) 0.037(3) 0.033(3) -0.006(2) 0.007(2) 0.000(2) C(5) 0.040(3) 0.049(3) 0.047(3) -0.009(2) -0.003(2) 0.010(3) C(6) 0.032(3) 0.056(4) 0.061(4) -0.013(2) 0.004(2) 0.000(3) C(7) 0.040(3) 0.088(5) 0.069(4) 0.003(3) -0.002(3) -0.016(4) C(8) 0.044(4) 0.183(8) 0.148(7) 0.039(4) -0.035(4) -0.097(6) C(9) 0.030(2) 0.034(3) 0.036(3) 0.003(2) 0.008(2) 0.000(2) C(10) 0.030(2) 0.028(2) 0.031(2) -0.003(2) 0.003(2) 0.005(2) C(11) 0.040(3) 0.135(6) 0.150(6) -0.035(3) 0.046(3) -0.094(5) C(12) 0.030(3) 0.085(5) 0.184(7) -0.010(3) 0.028(4) -0.063(5) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0001(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3371 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0443 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0428 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.787 _refine_ls_shift/esd_max 0.0340 _refine_ls_shift/esd_mean 0.0030 _refine_diff_density_min -0.69 _refine_diff_density_max 0.70 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.168(1) 1_555 1_555 yes Ni(1) S(2) 2.172(1) 1_555 1_555 yes Ni(1) S(3) 2.178(1) 1_555 1_555 yes Ni(1) S(4) 2.167(1) 1_555 1_555 yes Ni(2) S(5) 2.192(1) 1_555 1_555 yes Ni(2) S(5) 2.192(1) 1_555 3_565 yes Ni(2) S(6) 2.190(1) 1_555 1_555 yes Ni(2) S(6) 2.190(1) 1_555 3_565 yes S(1) C(1) 1.669(4) 1_555 1_555 yes S(2) C(2) 1.672(4) 1_555 1_555 yes S(3) C(3) 1.683(4) 1_555 1_555 yes S(4) C(4) 1.678(4) 1_555 1_555 yes S(5) C(9) 1.697(4) 1_555 1_555 yes S(6) C(10) 1.694(4) 1_555 1_555 yes P(1) F(1) 1.584(4) 1_555 1_555 yes P(1) F(2) 1.571(4) 1_555 1_555 yes P(1) F(3) 1.541(4) 1_555 1_555 yes P(1) F(4) 1.536(4) 1_555 1_555 yes P(1) F(5) 1.574(4) 1_555 1_555 yes P(1) F(6) 1.578(4) 1_555 1_555 yes O(1) C(1) 1.328(5) 1_555 1_555 yes O(1) C(5) 1.472(6) 1_555 1_555 yes O(2) C(2) 1.337(4) 1_555 1_555 yes O(2) C(6) 1.465(5) 1_555 1_555 yes O(3) C(3) 1.328(5) 1_555 1_555 yes O(3) C(7) 1.450(6) 1_555 1_555 yes O(4) C(4) 1.342(5) 1_555 1_555 yes O(4) C(8) 1.451(7) 1_555 1_555 yes O(5) C(9) 1.354(5) 1_555 1_555 yes O(5) C(11) 1.418(6) 1_555 1_555 yes O(6) C(10) 1.345(4) 1_555 1_555 yes O(6) C(12) 1.435(6) 1_555 1_555 yes C(1) C(2) 1.426(6) 1_555 1_555 yes C(3) C(4) 1.408(6) 1_555 1_555 yes C(5) C(6) 1.474(8) 1_555 1_555 yes C(7) C(8) 1.362(9) 1_555 1_555 yes C(9) C(10) 1.389(6) 1_555 1_555 yes C(11) C(12) 1.311(8) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(2) 92.09(5) 1_555 1_555 1_555 yes S(1) Ni(1) S(3) 87.13(5) 1_555 1_555 1_555 yes S(1) Ni(1) S(4) 165.22(5) 1_555 1_555 1_555 yes S(2) Ni(1) S(3) 170.11(5) 1_555 1_555 1_555 yes S(2) Ni(1) S(4) 86.04(5) 1_555 1_555 1_555 yes S(3) Ni(1) S(4) 92.21(5) 1_555 1_555 1_555 yes S(5) Ni(2) S(5) 180.0000(1) 1_555 1_555 3_565 yes S(5) Ni(2) S(6) 90.34(4) 1_555 1_555 1_555 yes S(5) Ni(2) S(6) 89.66(4) 1_555 1_555 3_565 yes S(5) Ni(2) S(6) 89.66(4) 3_565 1_555 1_555 yes S(5) Ni(2) S(6) 90.34(4) 3_565 1_555 3_565 yes S(6) Ni(2) S(6) 180.0 1_555 1_555 3_565 yes Ni(1) S(1) C(1) 103.2(2) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 103.4(2) 1_555 1_555 1_555 yes Ni(1) S(3) C(3) 102.8(2) 1_555 1_555 1_555 yes Ni(1) S(4) C(4) 103.1(2) 1_555 1_555 1_555 yes Ni(2) S(5) C(9) 102.4(2) 1_555 1_555 1_555 yes Ni(2) S(6) C(10) 102.3(1) 1_555 1_555 1_555 yes F(1) P(1) F(2) 88.3(3) 1_555 1_555 1_555 yes F(1) P(1) F(3) 176.5(3) 1_555 1_555 1_555 yes F(1) P(1) F(4) 87.1(3) 1_555 1_555 1_555 yes F(1) P(1) F(5) 90.7(2) 1_555 1_555 1_555 yes F(1) P(1) F(6) 89.7(2) 1_555 1_555 1_555 yes F(2) P(1) F(3) 88.4(3) 1_555 1_555 1_555 yes F(2) P(1) F(4) 174.9(3) 1_555 1_555 1_555 yes F(2) P(1) F(5) 91.3(3) 1_555 1_555 1_555 yes F(2) P(1) F(6) 89.9(3) 1_555 1_555 1_555 yes F(3) P(1) F(4) 96.3(3) 1_555 1_555 1_555 yes F(3) P(1) F(5) 90.2(2) 1_555 1_555 1_555 yes F(3) P(1) F(6) 89.4(2) 1_555 1_555 1_555 yes F(4) P(1) F(5) 90.9(3) 1_555 1_555 1_555 yes F(4) P(1) F(6) 88.0(2) 1_555 1_555 1_555 yes F(5) P(1) F(6) 178.8(3) 1_555 1_555 1_555 yes C(1) O(1) C(5) 114.9(4) 1_555 1_555 1_555 yes C(2) O(2) C(6) 114.9(4) 1_555 1_555 1_555 yes C(3) O(3) C(7) 116.8(4) 1_555 1_555 1_555 yes C(4) O(4) C(8) 113.1(4) 1_555 1_555 1_555 yes C(9) O(5) C(11) 113.0(4) 1_555 1_555 1_555 yes C(10) O(6) C(12) 114.6(4) 1_555 1_555 1_555 yes S(1) C(1) O(1) 117.1(3) 1_555 1_555 1_555 yes S(1) C(1) C(2) 120.7(3) 1_555 1_555 1_555 yes O(1) C(1) C(2) 122.1(4) 1_555 1_555 1_555 yes S(2) C(2) O(2) 118.2(3) 1_555 1_555 1_555 yes S(2) C(2) C(1) 120.2(3) 1_555 1_555 1_555 yes O(2) C(2) C(1) 121.6(4) 1_555 1_555 1_555 yes S(3) C(3) O(3) 117.3(3) 1_555 1_555 1_555 yes S(3) C(3) C(4) 120.8(3) 1_555 1_555 1_555 yes O(3) C(3) C(4) 121.9(4) 1_555 1_555 1_555 yes S(4) C(4) O(4) 117.3(3) 1_555 1_555 1_555 yes S(4) C(4) C(3) 120.9(3) 1_555 1_555 1_555 yes O(4) C(4) C(3) 121.8(4) 1_555 1_555 1_555 yes O(1) C(5) C(6) 110.1(4) 1_555 1_555 1_555 yes O(1) C(5) H(1) 106(2) 1_555 1_555 1_555 no O(1) C(5) H(2) 106(2) 1_555 1_555 1_555 no C(6) C(5) H(1) 112(2) 1_555 1_555 1_555 no C(6) C(5) H(2) 113(2) 1_555 1_555 1_555 no H(1) C(5) H(2) 107(3) 1_555 1_555 1_555 no O(2) C(6) C(5) 110.7(4) 1_555 1_555 1_555 yes O(2) C(6) H(3) 103(2) 1_555 1_555 1_555 no O(2) C(6) H(4) 106(2) 1_555 1_555 1_555 no C(5) C(6) H(3) 114(2) 1_555 1_555 1_555 no C(5) C(6) H(4) 113(2) 1_555 1_555 1_555 no H(3) C(6) H(4) 107(3) 1_555 1_555 1_555 no O(3) C(7) C(8) 116.4(5) 1_555 1_555 1_555 yes O(3) C(7) H(5) 107.7(5) 1_555 1_555 1_555 no O(3) C(7) H(6) 109.6(5) 1_555 1_555 1_555 no C(8) C(7) H(5) 106.2(7) 1_555 1_555 1_555 no C(8) C(7) H(6) 110.2(6) 1_555 1_555 1_555 no H(5) C(7) H(6) 106.2(5) 1_555 1_555 1_555 no O(4) C(8) C(7) 117.0(6) 1_555 1_555 1_555 yes O(4) C(8) H(7) 109.4(6) 1_555 1_555 1_555 no O(4) C(8) H(8) 109.8(7) 1_555 1_555 1_555 no C(7) C(8) H(7) 105.9(7) 1_555 1_555 1_555 no C(7) C(8) H(8) 108.4(7) 1_555 1_555 1_555 no H(7) C(8) H(8) 105.8(7) 1_555 1_555 1_555 no S(5) C(9) O(5) 117.0(3) 1_555 1_555 1_555 yes S(5) C(9) C(10) 120.0(3) 1_555 1_555 1_555 yes O(5) C(9) C(10) 122.9(4) 1_555 1_555 1_555 yes S(6) C(10) O(6) 116.5(3) 1_555 1_555 1_555 yes S(6) C(10) C(9) 120.9(3) 1_555 1_555 1_555 yes O(6) C(10) C(9) 122.6(4) 1_555 1_555 1_555 yes O(5) C(11) C(12) 122.5(5) 1_555 1_555 1_555 yes O(5) C(11) H(9) 107.0(6) 1_555 1_555 1_555 no O(5) C(11) H(10) 106.9(6) 1_555 1_555 1_555 no C(12) C(11) H(9) 105.3(7) 1_555 1_555 1_555 no C(12) C(11) H(10) 107.4(6) 1_555 1_555 1_555 no H(9) C(11) H(10) 106.8(5) 1_555 1_555 1_555 no O(6) C(12) C(11) 120.9(5) 1_555 1_555 1_555 yes O(6) C(12) H(11) 107.0(6) 1_555 1_555 1_555 no O(6) C(12) H(12) 108.4(5) 1_555 1_555 1_555 no C(11) C(12) H(11) 105.6(7) 1_555 1_555 1_555 no C(11) C(12) H(12) 108.0(7) 1_555 1_555 1_555 no H(11) C(12) H(12) 106.0(5) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni(1) S(5) 2.685(1) 1_555 1_555 ? Ni(1) Ni(2) 3.4290(6) 1_555 1_555 ? Ni(1) C(9) 3.468(4) 1_555 1_555 ? Ni(2) S(2) 3.129(1) 1_555 1_555 ? Ni(2) S(2) 3.129(1) 1_555 3_565 ? S(1) S(5) 3.475(2) 1_555 1_555 ? S(1) S(4) 3.582(2) 1_555 4_554 ? S(2) S(6) 3.570(2) 1_555 3_565 ? S(3) S(5) 3.429(2) 1_555 1_555 ? S(3) O(5) 3.467(3) 1_555 4_555 ? S(3) O(5) 3.572(3) 1_555 1_555 ? S(3) O(4) 3.573(4) 1_555 4_554 ? S(3) C(9) 3.584(4) 1_555 1_555 ? S(4) S(6) 3.313(2) 1_555 1_555 ? S(4) O(1) 3.354(3) 1_555 2_555 ? S(4) C(10) 3.492(4) 1_555 1_555 ? S(6) C(2) 3.307(4) 1_555 3_565 ? S(6) C(2) 3.365(4) 1_555 2_555 ? S(6) C(1) 3.521(4) 1_555 3_565 ? S(6) O(2) 3.596(3) 1_555 2_555 ? F(1) C(5) 3.230(6) 1_555 2_554 ? F(1) C(11) 3.265(8) 1_555 1_555 ? F(1) O(3) 3.551(5) 1_555 4_554 ? F(1) C(8) 3.584(9) 1_555 1_554 ? F(2) C(12) 3.059(7) 1_555 3_665 ? F(2) C(11) 3.219(8) 1_555 3_665 ? F(2) C(7) 3.529(8) 1_555 3_665 ? F(3) C(8) 3.193(8) 1_555 2_655 ? F(3) C(7) 3.229(8) 1_555 3_665 ? F(3) O(3) 3.233(5) 1_555 3_665 ? F(3) C(7) 3.268(7) 1_555 2_655 ? F(4) C(5) 3.195(7) 1_555 2_554 ? F(4) O(6) 3.216(5) 1_555 4_564 ? F(4) C(6) 3.261(7) 1_555 3_565 ? F(4) O(2) 3.423(5) 1_555 3_565 ? F(4) C(12) 3.485(8) 1_555 4_564 ? F(5) C(11) 3.308(8) 1_555 1_555 ? F(5) F(5) 3.350(9) 1_555 3_665 ? F(5) C(12) 3.418(8) 1_555 1_555 ? F(5) C(7) 3.437(7) 1_555 2_655 ? F(6) C(6) 3.150(6) 1_555 2_554 ? F(6) C(5) 3.175(6) 1_555 2_554 ? F(6) C(7) 3.422(7) 1_555 3_665 ? O(2) O(6) 3.180(4) 1_555 3_565 ? O(2) C(10) 3.215(5) 1_555 3_565 ? O(3) O(5) 3.235(4) 1_555 4_555 ? O(3) C(11) 3.545(7) 1_555 4_555 ? O(4) C(5) 3.282(7) 1_555 2_555 ? O(4) C(6) 3.341(6) 1_555 2_555 ? O(5) C(3) 3.086(5) 1_555 4_554 ? O(5) C(4) 3.519(5) 1_555 4_554 ? O(6) C(5) 3.369(6) 1_555 3_565 ? O(6) C(6) 3.452(7) 1_555 3_565 ? O(6) C(6) 3.481(7) 1_555 2_555 ? C(2) C(10) 3.408(6) 1_555 3_565 ? #------------------------------------------------------------------------------ data_Ni(edo)2FeCl4 _database_code_CSD 162735 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Feb 15 00:43:37 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MXC18' _computing_cell_refinement 'MXC18' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 907.84 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H16 Cl4 Fe O8 Ni2 S8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 13.444(4) _cell_length_b 16.143(2) _cell_length_c 7.508(1) _cell_angle_alpha 101.34(1) _cell_angle_beta 102.42(2) _cell_angle_gamma 92.10(2) _cell_volume 1555.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.6 _cell_measurement_theta_max 14.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 908.00 _exptl_absorpt_coefficient_mu 2.578 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Science M18X' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'four circle diffractometer' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% -5.17 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 3 -3 0 4 4 5 -5 -3 _diffrn_reflns_number 9521 _reflns_number_total 9062 _reflns_number_observed 5782 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_av_sigmaI/netI 0.077 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02221 _diffrn_orient_matrix_UB_12 0.01505 _diffrn_orient_matrix_UB_13 0.12038 _diffrn_orient_matrix_UB_21 -0.01099 _diffrn_orient_matrix_UB_22 -0.06158 _diffrn_orient_matrix_UB_23 0.00023 _diffrn_orient_matrix_UB_31 0.07229 _diffrn_orient_matrix_UB_32 0.00078 _diffrn_orient_matrix_UB_33 0.07046 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 4 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 32 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 16 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 2 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 32 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ni(1) 0.0000 0.0000 0.0000 0.0440(2) Uani d . 0.50 S Ni(2) 0.23764(4) 0.06568(4) 0.28095(7) 0.0425(1) Uani d . 1.00 . Ni(3) 0.5000 0.0000 0.5000 0.0518(2) Uani d . 0.50 S Fe(1) 0.76204(6) 0.47627(5) 0.3550(1) 0.0659(3) Uani d . 1.00 . Cl(1) 0.7881(1) 0.4625(1) 0.6462(2) 0.0868(5) Uani d . 1.00 . Cl(2) 0.7810(2) 0.3562(1) 0.1800(2) 0.1015(7) Uani d . 1.00 . Cl(3) 0.6047(1) 0.5059(1) 0.2527(3) 0.1021(7) Uani d . 1.00 . Cl(4) 0.8709(2) 0.5734(2) 0.3304(3) 0.1462(10) Uani d . 1.00 . S(1) 0.03536(8) 0.08405(7) -0.1784(2) 0.0483(3) Uani d . 1.00 . S(2) 0.02930(9) 0.10507(8) 0.2393(2) 0.0502(3) Uani d . 1.00 . S(3) 0.27062(8) 0.08179(7) 0.0201(1) 0.0439(3) Uani d . 1.00 . S(4) 0.27493(8) 0.19944(7) 0.4071(1) 0.0456(3) Uani d . 1.00 . S(5) 0.22823(8) -0.06988(7) 0.1734(1) 0.0459(3) Uani d . 1.00 . S(6) 0.22819(9) 0.04796(7) 0.5535(1) 0.0483(3) Uani d . 1.00 . S(7) 0.52578(9) 0.09245(8) 0.3421(2) 0.0571(4) Uani d . 1.00 . S(8) 0.50769(10) 0.09498(9) 0.7486(2) 0.0607(4) Uani d . 1.00 . O(1) 0.0367(3) 0.2485(2) -0.1280(5) 0.059(1) Uani d . 1.00 . O(2) 0.0295(3) 0.2661(2) 0.2540(5) 0.059(1) Uani d . 1.00 . O(3) 0.3079(3) 0.2174(2) -0.0944(5) 0.067(1) Uani d . 1.00 . O(4) 0.3171(3) 0.3238(2) 0.2576(5) 0.061(1) Uani d . 1.00 . O(5) 0.1973(3) -0.1953(2) 0.3285(4) 0.0549(10) Uani d . 1.00 . O(6) 0.2058(3) -0.0870(2) 0.6785(4) 0.057(1) Uani d . 1.00 . O(7) 0.5506(3) 0.2567(2) 0.4356(5) 0.068(1) Uani d . 1.00 . O(8) 0.5432(3) 0.2588(2) 0.8126(5) 0.076(1) Uani d . 1.00 . C(1) 0.0332(3) 0.1807(3) -0.0459(6) 0.046(1) Uani d . 1.00 . C(2) 0.0292(3) 0.1907(3) 0.1410(6) 0.046(1) Uani d . 1.00 . C(3) 0.0016(5) 0.3239(4) -0.0252(9) 0.065(2) Uani d . 1.00 . C(4) 0.0514(5) 0.3384(3) 0.1754(9) 0.064(2) Uani d . 1.00 . C(5) 0.2922(3) 0.1862(3) 0.0512(6) 0.046(1) Uani d . 1.00 . C(6) 0.2944(3) 0.2403(3) 0.2256(6) 0.045(1) Uani d . 1.00 . C(7) 0.2122(3) -0.1112(3) 0.3540(6) 0.044(1) Uani d . 1.00 . C(8) 0.2137(3) -0.0566(3) 0.5289(6) 0.044(1) Uani d . 1.00 . C(9) 0.3166(7) 0.3068(4) -0.066(1) 0.123(3) Uani d . 1.00 . C(10) 0.3557(6) 0.3519(4) 0.1098(9) 0.113(3) Uani d . 1.00 . C(11) 0.1568(5) -0.2236(4) 0.4769(8) 0.063(2) Uani d . 1.00 . C(12) 0.2136(5) -0.1767(4) 0.6635(8) 0.060(2) Uani d . 1.00 . C(13) 0.5353(3) 0.1846(3) 0.4976(7) 0.056(1) Uani d . 1.00 . C(14) 0.5307(3) 0.1860(3) 0.6817(7) 0.057(1) Uani d . 1.00 . C(15) 0.5384(5) 0.3338(4) 0.5651(10) 0.073(2) Uani d . 1.00 . C(16) 0.5897(6) 0.3295(4) 0.758(1) 0.080(2) Uani d . 1.00 . H(1) 0.012(4) 0.367(3) -0.085(7) 0.06(1) Uiso calc . 1.00 . H(2) -0.076(3) 0.312(3) -0.046(6) 0.05(1) Uiso calc . 1.00 . H(3) 0.035(3) 0.381(3) 0.248(6) 0.04(1) Uiso calc . 1.00 . H(4) 0.140(4) 0.348(3) 0.200(7) 0.08(2) Uiso calc . 1.00 . H(5) 0.3500 0.3228 -0.1524 0.1510 Uiso calc . 1.00 . H(6) 0.2449 0.3229 -0.0989 0.1510 Uiso calc . 1.00 . H(7) 0.3496 0.4088 0.1146 0.1362 Uiso calc . 1.00 . H(8) 0.4292 0.3420 0.1307 0.1362 Uiso calc . 1.00 . H(9) 0.161(4) -0.285(3) 0.452(7) 0.07(1) Uiso calc . 1.00 . H(10) 0.090(4) -0.207(3) 0.469(7) 0.07(2) Uiso calc . 1.00 . H(11) 0.191(4) -0.196(3) 0.759(7) 0.07(2) Uiso calc . 1.00 . H(12) 0.284(4) -0.190(3) 0.685(6) 0.06(1) Uiso calc . 1.00 . H(13) 0.567(4) 0.376(3) 0.517(7) 0.07(1) Uiso calc . 1.00 . H(14) 0.454(4) 0.337(3) 0.551(7) 0.09(2) Uiso calc . 1.00 . H(15) 0.580(4) 0.376(3) 0.836(7) 0.07(2) Uiso calc . 1.00 . H(16) 0.656(4) 0.320(4) 0.746(8) 0.09(2) Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0359(4) 0.0435(4) 0.0517(5) -0.0020(3) 0.0112(3) 0.0078(4) Ni(2) 0.0455(3) 0.0492(3) 0.0318(3) -0.0054(2) 0.0056(2) 0.0113(2) Ni(3) 0.0358(4) 0.0530(5) 0.0650(6) 0.0028(4) 0.0075(4) 0.0130(4) Fe(1) 0.0672(5) 0.0636(5) 0.0721(5) -0.0005(4) 0.0168(4) 0.0268(4) Cl(1) 0.114(1) 0.077(1) 0.0688(9) -0.0192(9) 0.0201(9) 0.0192(8) Cl(2) 0.130(2) 0.104(1) 0.080(1) 0.056(1) 0.031(1) 0.0263(10) Cl(3) 0.081(1) 0.086(1) 0.139(2) 0.0289(9) 0.019(1) 0.024(1) Cl(4) 0.138(2) 0.177(2) 0.128(2) -0.073(2) 0.003(1) 0.088(2) S(1) 0.0396(5) 0.0516(7) 0.0546(7) -0.0014(5) 0.0146(5) 0.0098(5) S(2) 0.0522(7) 0.0474(6) 0.0486(6) -0.0026(5) 0.0076(5) 0.0095(5) S(3) 0.0467(6) 0.0518(6) 0.0350(5) 0.0016(5) 0.0103(4) 0.0128(5) S(4) 0.0442(6) 0.0534(7) 0.0369(5) -0.0035(5) 0.0063(4) 0.0089(5) S(5) 0.0472(6) 0.0531(7) 0.0376(5) -0.0008(5) 0.0102(4) 0.0099(5) S(6) 0.0608(7) 0.0504(7) 0.0356(5) -0.0001(5) 0.0135(5) 0.0117(5) S(7) 0.0440(6) 0.0593(8) 0.0678(8) 0.0040(5) 0.0122(6) 0.0135(6) S(8) 0.0551(7) 0.0611(8) 0.0654(8) 0.0028(6) 0.0118(6) 0.0144(6) O(1) 0.061(2) 0.052(2) 0.071(2) 0.006(2) 0.022(2) 0.023(2) O(2) 0.067(2) 0.043(2) 0.062(2) 0.002(2) 0.012(2) 0.003(2) O(3) 0.098(3) 0.063(2) 0.055(2) 0.009(2) 0.036(2) 0.027(2) O(4) 0.076(2) 0.051(2) 0.055(2) -0.010(2) 0.012(2) 0.013(2) O(5) 0.067(2) 0.049(2) 0.051(2) 0.002(2) 0.020(2) 0.011(2) O(6) 0.079(2) 0.053(2) 0.049(2) 0.003(2) 0.025(2) 0.021(2) O(7) 0.066(2) 0.059(2) 0.083(3) 0.003(2) 0.020(2) 0.020(2) O(8) 0.086(3) 0.059(2) 0.076(3) -0.008(2) 0.014(2) 0.002(2) C(1) 0.031(2) 0.050(3) 0.059(3) 0.002(2) 0.009(2) 0.017(2) C(2) 0.034(2) 0.044(2) 0.056(3) 0.001(2) 0.005(2) 0.008(2) C(3) 0.069(4) 0.052(3) 0.083(4) 0.010(3) 0.024(3) 0.026(3) C(4) 0.065(3) 0.042(3) 0.083(4) 0.001(2) 0.020(3) 0.005(3) C(5) 0.040(2) 0.056(3) 0.043(2) 0.001(2) 0.009(2) 0.019(2) C(6) 0.036(2) 0.047(3) 0.050(2) -0.002(2) 0.005(2) 0.015(2) C(7) 0.032(2) 0.052(3) 0.048(2) 0.003(2) 0.008(2) 0.016(2) C(8) 0.037(2) 0.055(3) 0.042(2) 0.002(2) 0.010(2) 0.019(2) C(9) 0.24(1) 0.056(4) 0.102(5) 0.004(5) 0.095(6) 0.030(4) C(10) 0.173(7) 0.089(5) 0.073(4) -0.069(5) 0.019(5) 0.026(4) C(11) 0.077(4) 0.050(3) 0.065(3) -0.005(3) 0.017(3) 0.022(3) C(12) 0.067(3) 0.062(3) 0.060(3) 0.006(3) 0.022(3) 0.026(3) C(13) 0.037(2) 0.055(3) 0.075(3) 0.004(2) 0.009(2) 0.017(3) C(14) 0.043(2) 0.054(3) 0.071(3) 0.003(2) 0.007(2) 0.011(3) C(15) 0.066(4) 0.052(3) 0.095(5) -0.004(3) 0.007(3) 0.015(3) C(16) 0.077(4) 0.054(4) 0.098(5) -0.005(3) 0.005(4) 0.007(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5782 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0450 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0491 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.087 _refine_ls_shift/esd_max 2.8030 _refine_ls_shift/esd_mean 0.0370 _refine_diff_density_min -0.62 _refine_diff_density_max 0.79 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.191(1) 1_555 1_555 yes Ni(1) S(1) 2.191(1) 1_555 2_555 yes Ni(1) S(2) 2.170(1) 1_555 1_555 yes Ni(1) S(2) 2.170(1) 1_555 2_555 yes Ni(2) S(3) 2.160(1) 1_555 1_555 yes Ni(2) S(4) 2.173(1) 1_555 1_555 yes Ni(2) S(5) 2.168(1) 1_555 1_555 yes Ni(2) S(6) 2.151(1) 1_555 1_555 yes Ni(3) S(7) 2.142(1) 1_555 1_555 yes Ni(3) S(7) 2.142(1) 1_555 2_656 yes Ni(3) S(8) 2.150(1) 1_555 1_555 yes Ni(3) S(8) 2.150(1) 1_555 2_656 yes Fe(1) Cl(1) 2.195(2) 1_555 1_555 yes Fe(1) Cl(2) 2.175(2) 1_555 1_555 yes Fe(1) Cl(3) 2.194(2) 1_555 1_555 yes Fe(1) Cl(4) 2.167(2) 1_555 1_555 yes S(1) C(1) 1.683(5) 1_555 1_555 yes S(2) C(2) 1.689(4) 1_555 1_555 yes S(3) C(5) 1.662(4) 1_555 1_555 yes S(4) C(6) 1.689(4) 1_555 1_555 yes S(5) C(7) 1.673(4) 1_555 1_555 yes S(6) C(8) 1.662(4) 1_555 1_555 yes S(7) C(13) 1.683(5) 1_555 1_555 yes S(8) C(14) 1.682(5) 1_555 1_555 yes O(1) C(1) 1.361(5) 1_555 1_555 yes O(1) C(3) 1.460(6) 1_555 1_555 yes O(2) C(2) 1.340(5) 1_555 1_555 yes O(2) C(4) 1.456(6) 1_555 1_555 yes O(3) C(5) 1.342(5) 1_555 1_555 yes O(3) C(9) 1.413(7) 1_555 1_555 yes O(4) C(6) 1.335(5) 1_555 1_555 yes O(4) C(10) 1.460(7) 1_555 1_555 yes O(5) C(7) 1.335(5) 1_555 1_555 yes O(5) C(11) 1.480(6) 1_555 1_555 yes O(6) C(8) 1.333(5) 1_555 1_555 yes O(6) C(12) 1.440(6) 1_555 1_555 yes O(7) C(13) 1.361(6) 1_555 1_555 yes O(7) C(15) 1.459(7) 1_555 1_555 yes O(8) C(14) 1.355(6) 1_555 1_555 yes O(8) C(16) 1.451(7) 1_555 1_555 yes C(1) C(2) 1.394(6) 1_555 1_555 yes C(3) C(4) 1.479(8) 1_555 1_555 yes C(5) C(6) 1.418(6) 1_555 1_555 yes C(7) C(8) 1.425(6) 1_555 1_555 yes C(9) C(10) 1.357(9) 1_555 1_555 yes C(11) C(12) 1.483(8) 1_555 1_555 yes C(13) C(14) 1.393(7) 1_555 1_555 yes C(15) C(16) 1.480(9) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(1) 180.0 1_555 1_555 2_555 yes S(1) Ni(1) S(2) 90.84(4) 1_555 1_555 1_555 yes S(1) Ni(1) S(2) 89.16(4) 1_555 1_555 2_555 yes S(1) Ni(1) S(2) 89.16(4) 2_555 1_555 1_555 yes S(1) Ni(1) S(2) 90.84(4) 2_555 1_555 2_555 yes S(2) Ni(1) S(2) 180.0 1_555 1_555 2_555 yes S(3) Ni(2) S(4) 92.53(5) 1_555 1_555 1_555 yes S(3) Ni(2) S(5) 87.36(5) 1_555 1_555 1_555 yes S(3) Ni(2) S(6) 171.67(5) 1_555 1_555 1_555 yes S(4) Ni(2) S(5) 170.08(5) 1_555 1_555 1_555 yes S(4) Ni(2) S(6) 86.79(5) 1_555 1_555 1_555 yes S(5) Ni(2) S(6) 91.88(5) 1_555 1_555 1_555 yes S(7) Ni(3) S(7) 180.0 1_555 1_555 2_656 yes S(7) Ni(3) S(8) 92.69(5) 1_555 1_555 1_555 yes S(7) Ni(3) S(8) 87.31(5) 1_555 1_555 2_656 yes S(7) Ni(3) S(8) 87.31(5) 2_656 1_555 1_555 yes S(7) Ni(3) S(8) 92.69(5) 2_656 1_555 2_656 yes S(8) Ni(3) S(8) 180.0 1_555 1_555 2_656 yes Cl(1) Fe(1) Cl(2) 109.21(7) 1_555 1_555 1_555 yes Cl(1) Fe(1) Cl(3) 111.12(8) 1_555 1_555 1_555 yes Cl(1) Fe(1) Cl(4) 109.70(8) 1_555 1_555 1_555 yes Cl(2) Fe(1) Cl(3) 106.28(8) 1_555 1_555 1_555 yes Cl(2) Fe(1) Cl(4) 109.6(1) 1_555 1_555 1_555 yes Cl(3) Fe(1) Cl(4) 110.90(9) 1_555 1_555 1_555 yes Ni(1) S(1) C(1) 102.2(2) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 102.9(2) 1_555 1_555 1_555 yes Ni(2) S(3) C(5) 103.2(2) 1_555 1_555 1_555 yes Ni(2) S(4) C(6) 102.3(2) 1_555 1_555 1_555 yes Ni(2) S(5) C(7) 103.5(2) 1_555 1_555 1_555 yes Ni(2) S(6) C(8) 104.1(2) 1_555 1_555 1_555 yes Ni(3) S(7) C(13) 102.9(2) 1_555 1_555 1_555 yes Ni(3) S(8) C(14) 103.2(2) 1_555 1_555 1_555 yes C(1) O(1) C(3) 112.5(4) 1_555 1_555 1_555 yes C(2) O(2) C(4) 114.3(4) 1_555 1_555 1_555 yes C(5) O(3) C(9) 115.3(4) 1_555 1_555 1_555 yes C(6) O(4) C(10) 114.0(4) 1_555 1_555 1_555 yes C(7) O(5) C(11) 113.6(4) 1_555 1_555 1_555 yes C(8) O(6) C(12) 116.3(4) 1_555 1_555 1_555 yes C(13) O(7) C(15) 113.5(4) 1_555 1_555 1_555 yes C(14) O(8) C(16) 113.0(5) 1_555 1_555 1_555 yes S(1) C(1) O(1) 117.3(3) 1_555 1_555 1_555 yes S(1) C(1) C(2) 121.0(3) 1_555 1_555 1_555 yes O(1) C(1) C(2) 121.6(4) 1_555 1_555 1_555 yes S(2) C(2) O(2) 116.3(3) 1_555 1_555 1_555 yes S(2) C(2) C(1) 120.0(3) 1_555 1_555 1_555 yes O(2) C(2) C(1) 123.6(4) 1_555 1_555 1_555 yes O(1) C(3) C(4) 110.4(5) 1_555 1_555 1_555 yes O(1) C(3) H(1) 105(3) 1_555 1_555 1_555 no O(1) C(3) H(2) 105(2) 1_555 1_555 1_555 no C(4) C(3) H(1) 116(3) 1_555 1_555 1_555 no C(4) C(3) H(2) 111(2) 1_555 1_555 1_555 no H(1) C(3) H(2) 106(3) 1_555 1_555 1_555 no O(2) C(4) C(3) 111.1(4) 1_555 1_555 1_555 yes O(2) C(4) H(3) 104(3) 1_555 1_555 1_555 no O(2) C(4) H(4) 106(2) 1_555 1_555 1_555 no C(3) C(4) H(3) 117(3) 1_555 1_555 1_555 no C(3) C(4) H(4) 111(2) 1_555 1_555 1_555 no H(3) C(4) H(4) 104(3) 1_555 1_555 1_555 no S(3) C(5) O(3) 117.6(3) 1_555 1_555 1_555 yes S(3) C(5) C(6) 121.1(3) 1_555 1_555 1_555 yes O(3) C(5) C(6) 121.3(4) 1_555 1_555 1_555 yes S(4) C(6) O(4) 117.1(3) 1_555 1_555 1_555 yes S(4) C(6) C(5) 120.4(3) 1_555 1_555 1_555 yes O(4) C(6) C(5) 122.4(4) 1_555 1_555 1_555 yes S(5) C(7) O(5) 118.3(3) 1_555 1_555 1_555 yes S(5) C(7) C(8) 119.9(3) 1_555 1_555 1_555 yes O(5) C(7) C(8) 121.8(4) 1_555 1_555 1_555 yes S(6) C(8) O(6) 117.7(3) 1_555 1_555 1_555 yes S(6) C(8) C(7) 120.5(3) 1_555 1_555 1_555 yes O(6) C(8) C(7) 121.8(4) 1_555 1_555 1_555 yes O(3) C(9) C(10) 118.0(6) 1_555 1_555 1_555 yes O(3) C(9) H(5) 109.0(6) 1_555 1_555 1_555 no O(3) C(9) H(6) 105.1(7) 1_555 1_555 1_555 no C(10) C(9) H(5) 112.1(8) 1_555 1_555 1_555 no C(10) C(9) H(6) 105.1(7) 1_555 1_555 1_555 no H(5) C(9) H(6) 106.6(7) 1_555 1_555 1_555 no O(4) C(10) C(9) 115.9(5) 1_555 1_555 1_555 yes O(4) C(10) H(7) 111.5(7) 1_555 1_555 1_555 no O(4) C(10) H(8) 107.0(6) 1_555 1_555 1_555 no C(9) C(10) H(7) 110.3(7) 1_555 1_555 1_555 no C(9) C(10) H(8) 103.2(8) 1_555 1_555 1_555 no H(7) C(10) H(8) 108.4(6) 1_555 1_555 1_555 no O(5) C(11) C(12) 110.5(4) 1_555 1_555 1_555 yes O(5) C(11) H(9) 104(2) 1_555 1_555 1_555 no O(5) C(11) H(10) 108(3) 1_555 1_555 1_555 no C(12) C(11) H(9) 115(2) 1_555 1_555 1_555 no C(12) C(11) H(10) 103(3) 1_555 1_555 1_555 no H(9) C(11) H(10) 114(4) 1_555 1_555 1_555 no O(6) C(12) C(11) 110.1(4) 1_555 1_555 1_555 yes O(6) C(12) H(11) 111(3) 1_555 1_555 1_555 no O(6) C(12) H(12) 111(2) 1_555 1_555 1_555 no C(11) C(12) H(11) 111(3) 1_555 1_555 1_555 no C(11) C(12) H(12) 109(2) 1_555 1_555 1_555 no H(11) C(12) H(12) 102(3) 1_555 1_555 1_555 no S(7) C(13) O(7) 116.7(4) 1_555 1_555 1_555 yes S(7) C(13) C(14) 121.1(4) 1_555 1_555 1_555 yes O(7) C(13) C(14) 122.2(5) 1_555 1_555 1_555 yes S(8) C(14) O(8) 117.4(4) 1_555 1_555 1_555 yes S(8) C(14) C(13) 120.0(4) 1_555 1_555 1_555 yes O(8) C(14) C(13) 122.5(5) 1_555 1_555 1_555 yes O(7) C(15) C(16) 110.1(5) 1_555 1_555 1_555 yes O(7) C(15) H(13) 102(3) 1_555 1_555 1_555 no O(7) C(15) H(14) 106(2) 1_555 1_555 1_555 no C(16) C(15) H(13) 115(3) 1_555 1_555 1_555 no C(16) C(15) H(14) 110(2) 1_555 1_555 1_555 no H(13) C(15) H(14) 111(4) 1_555 1_555 1_555 no O(8) C(16) C(15) 110.0(5) 1_555 1_555 1_555 yes O(8) C(16) H(15) 106(3) 1_555 1_555 1_555 no O(8) C(16) H(16) 110(3) 1_555 1_555 1_555 no C(15) C(16) H(15) 109(3) 1_555 1_555 1_555 no C(15) C(16) H(16) 102(3) 1_555 1_555 1_555 no H(15) C(16) H(16) 118(4) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni(1) S(5) 3.391(1) 1_555 1_555 ? Ni(1) S(5) 3.391(1) 1_555 2_555 ? Ni(1) Ni(2) 3.4285(9) 1_555 1_555 ? Ni(1) Ni(2) 3.4285(9) 1_555 2_555 ? Ni(2) S(2) 2.860(2) 1_555 1_555 ? Cl(2) C(12) 3.330(6) 1_555 2_656 ? Cl(2) C(16) 3.566(7) 1_555 1_554 ? Cl(3) C(15) 3.517(7) 1_555 2_666 ? S(1) S(3) 3.198(2) 1_555 1_555 ? S(1) C(7) 3.384(4) 1_555 2_555 ? S(1) S(5) 3.552(2) 1_555 2_555 ? S(2) O(6) 3.361(4) 1_555 2_556 ? S(2) S(6) 3.448(2) 1_555 1_555 ? S(2) S(4) 3.450(2) 1_555 1_555 ? S(3) O(6) 3.299(3) 1_555 1_554 ? S(3) S(6) 3.355(2) 1_555 1_554 ? S(4) C(13) 3.446(5) 1_555 1_555 ? S(4) C(2) 3.455(4) 1_555 1_555 ? S(4) O(2) 3.534(4) 1_555 1_555 ? S(5) S(8) 3.524(2) 1_555 2_656 ? S(6) O(3) 3.368(4) 1_555 1_556 ? S(7) C(8) 3.529(4) 1_555 2_656 ? O(1) O(5) 3.187(5) 1_555 2_555 ? O(1) C(11) 3.220(7) 1_555 2_555 ? O(3) O(8) 3.453(5) 1_555 1_554 ? O(4) C(15) 3.327(7) 1_555 1_555 ? O(4) O(7) 3.439(5) 1_555 1_555 ? O(4) C(4) 3.517(7) 1_555 1_555 ? O(5) C(1) 3.403(5) 1_555 2_555 ? O(5) C(3) 3.429(7) 1_555 2_555 ? O(5) C(13) 3.536(6) 1_555 2_656 ? O(7) C(6) 3.443(5) 1_555 1_555 ? O(8) C(9) 3.436(10) 1_555 1_556 ? C(1) C(5) 3.395(6) 1_555 1_555 ? C(1) C(7) 3.594(6) 1_555 2_555 ? C(2) C(6) 3.517(6) 1_555 1_555 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_[Ni(edo)2]2FeBr4 _database_code_CSD 162736 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C16 H16 Br4 Fe O8 Ni2 S8 ' _chemical_formula_moiety '?' _chemical_formula_weight 1085.64 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 14.989(2) _cell_length_b 31.944(4) _cell_length_c 14.3620(9) _cell_angle_alpha 90 _cell_angle_beta 112.525(7) _cell_angle_gamma 90 _cell_volume 6352(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.015 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 7.236 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type Imaging Plate (DIP320) _diffrn_reflns_number 11751 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 30.17 _diffrn_measured_fraction_theta_max 0.3110 _diffrn_reflns_theta_full 30.17 _diffrn_measured_fraction_theta_full 0.3110 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3858 _reflns_number_gt 3854 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0490 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3854 _refine_ls_number_parameters 710 _refine_ls_goodness_of_fit_ref 2.779 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_shift/su_max 5.0223 _refine_diff_density_max 0.87 _refine_diff_density_min -0.67 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Fe' 'Fe' 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.1096(2) 0.27408(9) 0.2191(2) 0.106(1) Uani 1.00 d . . . Br(2) Br 0.3777(2) 0.25231(7) 0.3135(2) 0.0857(9) Uani 1.00 d . . . Br(3) Br 0.2515(2) 0.25111(7) 0.4994(1) 0.0851(10) Uani 1.00 d . . . Br(4) Br 0.2023(2) 0.16448(7) 0.3074(2) 0.0884(9) Uani 1.00 d . . . Br(5) Br 0.1108(2) 0.26510(8) 0.7158(2) 0.1040(10) Uani 1.00 d . . . Br(6) Br 0.3816(2) 0.24412(7) 0.8340(2) 0.0859(9) Uani 1.00 d . . . Br(7) Br 0.2429(2) 0.24975(7) 1.0029(1) 0.0853(10) Uani 1.00 d . . . Br(8) Br 0.2006(2) 0.15767(7) 0.8210(2) 0.0893(9) Uani 1.00 d . . . Ni(1) Ni 0.0000 0.0000 0.0000 0.057(1) Uani 1.00 d S . . Ni(2) Ni 0.0054(2) 0.00838(8) 0.2580(2) 0.0584(9) Uani 1.00 d . . . Ni(3) Ni 0.0000 0.0000 0.5000 0.052(1) Uani 1.00 d S . . Ni(4) Ni 0.5000 0.0000 0.0000 0.051(1) Uani 1.00 d S . . Ni(5) Ni 0.5191(2) 0.00322(8) 0.2733(1) 0.0503(8) Uani 1.00 d . . . Ni(6) Ni 0.5000 0.0000 0.5000 0.051(1) Uani 1.00 d S . . Fe(1) Fe 0.2338(2) 0.23484(9) 0.3341(2) 0.061(1) Uani 1.00 d . . . Fe(2) Fe 0.2318(2) 0.22867(9) 0.8422(2) 0.061(1) Uani 1.00 d . . . S(1) S 0.1102(4) 0.0456(2) 0.0138(3) 0.063(2) Uani 1.00 d . . . S(2) S -0.1058(4) 0.0476(2) -0.0114(3) 0.058(2) Uani 1.00 d . . . S(3) S 0.0419(4) 0.0736(2) 0.2529(3) 0.056(2) Uani 1.00 d . . . S(4) S -0.1390(4) 0.0231(2) 0.2454(3) 0.063(2) Uani 1.00 d . . . S(5) S 0.1508(4) -0.0061(2) 0.2716(4) 0.073(2) Uani 1.00 d . . . S(6) S -0.0337(4) -0.0570(2) 0.2495(3) 0.061(2) Uani 1.00 d . . . S(7) S 0.1031(4) 0.0472(2) 0.4983(3) 0.057(2) Uani 1.00 d . . . S(8) S -0.1092(4) 0.0471(2) 0.4882(3) 0.055(2) Uani 1.00 d . . . S(9) S 0.6363(4) 0.0261(2) 0.0117(3) 0.057(2) Uani 1.00 d . . . S(10) S 0.4244(4) 0.0580(2) -0.0520(3) 0.057(2) Uani 1.00 d . . . S(11) S 0.5770(4) 0.0582(1) 0.2308(3) 0.048(2) Uani 1.00 d . . . S(12) S 0.3756(3) 0.0301(2) 0.2231(3) 0.048(2) Uani 1.00 d . . . S(13) S 0.6578(4) -0.0266(2) 0.3077(3) 0.056(2) Uani 1.00 d . . . S(14) S 0.4527(4) -0.0553(2) 0.2869(3) 0.052(2) Uani 1.00 d . . . S(15) S 0.6191(4) 0.0326(2) 0.4835(3) 0.066(2) Uani 1.00 d . . . S(16) S 0.4075(4) 0.0548(2) 0.4502(3) 0.063(2) Uani 1.00 d . . . O(1) O 0.104(1) 0.1271(5) 0.0120(8) 0.066(5) Uani 1.00 d . . . O(2) O -0.0898(9) 0.1280(5) -0.0050(8) 0.059(5) Uani 1.00 d . . . O(3) O -0.064(1) 0.1399(5) 0.2329(9) 0.072(5) Uani 1.00 d . . . O(4) O -0.224(1) 0.0932(6) 0.2364(10) 0.082(6) Uani 1.00 d . . . O(5) O 0.233(1) -0.0757(6) 0.2807(10) 0.087(6) Uani 1.00 d . . . O(6) O 0.073(1) -0.1234(5) 0.2709(10) 0.080(6) Uani 1.00 d . . . O(7) O 0.0937(10) 0.1275(5) 0.4967(8) 0.065(5) Uani 1.00 d . . . O(8) O -0.0953(10) 0.1285(5) 0.4975(8) 0.059(5) Uani 1.00 d . . . O(9) O 0.6809(10) 0.1010(4) -0.0244(8) 0.061(5) Uani 1.00 d . . . O(10) O 0.4882(10) 0.1306(4) -0.0781(8) 0.065(5) Uani 1.00 d . . . O(11) O 0.4971(9) 0.1287(4) 0.1608(8) 0.056(5) Uani 1.00 d . . . O(12) O 0.3151(10) 0.1040(5) 0.1591(9) 0.072(5) Uani 1.00 d . . . O(13) O 0.7105(10) -0.1033(4) 0.3514(8) 0.066(5) Uani 1.00 d . . . O(14) O 0.5243(9) -0.1292(4) 0.3318(8) 0.062(5) Uani 1.00 d . . . O(15) O 0.646(1) 0.1110(6) 0.4619(9) 0.091(6) Uani 1.00 d . . . O(16) O 0.455(1) 0.1323(5) 0.4377(10) 0.097(6) Uani 1.00 d . . . C(1) C 0.057(2) 0.0919(7) 0.008(1) 0.052(8) Uani 1.00 d . . . C(2) C -0.041(2) 0.0917(6) -0.002(1) 0.050(8) Uani 1.00 d . . . C(3) C 0.046(2) 0.1649(7) -0.014(2) 0.081(10) Uani 1.00 d . . . C(4) C -0.029(2) 0.1642(8) 0.026(2) 0.08(1) Uani 1.00 d . . . C(5) C -0.060(2) 0.0988(8) 0.243(1) 0.059(8) Uani 1.00 d . . . C(6) C -0.141(2) 0.0756(7) 0.240(1) 0.058(8) Uani 1.00 d . . . C(7) C 0.151(2) -0.0573(8) 0.273(1) 0.062(8) Uani 1.00 d . . . C(8) C 0.070(2) -0.0819(8) 0.264(1) 0.067(9) Uani 1.00 d . . . C(9) C -0.163(2) 0.1558(6) 0.187(1) 0.071(8) Uani 1.00 d . . . C(10) C -0.223(2) 0.1369(8) 0.240(2) 0.080(9) Uani 1.00 d . . . C(11) C 0.232(2) -0.120(1) 0.269(1) 0.09(1) Uani 1.00 d . . . C(12) C 0.170(2) -0.1399(7) 0.314(2) 0.082(10) Uani 1.00 d . . . C(13) C 0.044(2) 0.0921(6) 0.496(1) 0.045(8) Uani 1.00 d . . . C(14) C -0.051(2) 0.0925(7) 0.492(1) 0.050(8) Uani 1.00 d . . . C(15) C 0.040(2) 0.1657(7) 0.484(1) 0.067(9) Uani 1.00 d . . . C(16) C -0.031(2) 0.1637(6) 0.531(1) 0.067(8) Uani 1.00 d . . . C(17) C 0.607(2) 0.0757(6) -0.024(1) 0.053(8) Uani 1.00 d . . . C(18) C 0.512(2) 0.0911(6) -0.053(1) 0.054(8) Uani 1.00 d . . . C(19) C 0.648(2) 0.1382(7) -0.080(1) 0.066(8) Uani 1.00 d . . . C(20) C 0.572(2) 0.1586(6) -0.052(1) 0.074(9) Uani 1.00 d . . . C(21) C 0.483(1) 0.0909(6) 0.191(1) 0.039(7) Uani 1.00 d . . . C(22) C 0.393(2) 0.0783(6) 0.190(1) 0.045(7) Uani 1.00 d . . . C(23) C 0.638(2) -0.0761(6) 0.326(1) 0.052(7) Uani 1.00 d . . . C(24) C 0.545(1) -0.0898(6) 0.317(1) 0.047(7) Uani 1.00 d . . . C(25) C 0.409(2) 0.1527(7) 0.109(1) 0.077(9) Uani 1.00 d . . . C(26) C 0.338(2) 0.1465(8) 0.144(2) 0.11(1) Uani 1.00 d . . . C(27) C 0.689(2) -0.1443(8) 0.377(3) 0.17(2) Uani 1.00 d . . . C(28) C 0.606(2) -0.1576(7) 0.358(3) 0.15(1) Uani 1.00 d . . . C(29) C 0.580(2) 0.0821(7) 0.469(1) 0.064(9) Uani 1.00 d . . . C(30) C 0.488(2) 0.0926(7) 0.453(1) 0.070(9) Uani 1.00 d . . . C(31) C 0.601(3) 0.1512(9) 0.419(2) 0.13(1) Uani 1.00 d . . . C(32) C 0.531(2) 0.1628(8) 0.466(2) 0.11(1) Uani 1.00 d . . . H(1) H 0.0860 0.1898 0.0089 0.0972 Uiso 1.00 calc . . . H(2) H 0.0131 0.1678 -0.0861 0.0972 Uiso 1.00 calc . . . H(3) H -0.0643 0.1907 0.0105 0.0964 Uiso 1.00 calc . . . H(4) H 0.0056 0.1653 0.1013 0.0964 Uiso 1.00 calc . . . H(5) H -0.1644 0.1867 0.1869 0.0837 Uiso 1.00 calc . . . H(6) H -0.1934 0.1482 0.1157 0.0837 Uiso 1.00 calc . . . H(7) H -0.2884 0.1499 0.2141 0.0979 Uiso 1.00 calc . . . H(8) H -0.1952 0.1481 0.3113 0.0979 Uiso 1.00 calc . . . H(9) H 0.2062 -0.1289 0.1969 0.1027 Uiso 1.00 calc . . . H(10) H 0.2976 -0.1328 0.2953 0.1027 Uiso 1.00 calc . . . H(11) H 0.2007 -0.1350 0.3886 0.1000 Uiso 1.00 calc . . . H(12) H 0.1718 -0.1711 0.3105 0.1000 Uiso 1.00 calc . . . H(13) H 0.0817 0.1901 0.5126 0.0804 Uiso 1.00 calc . . . H(14) H 0.0042 0.1728 0.4137 0.0804 Uiso 1.00 calc . . . H(15) H -0.0706 0.1899 0.5185 0.0810 Uiso 1.00 calc . . . H(16) H 0.0018 0.1630 0.6041 0.0810 Uiso 1.00 calc . . . H(17) H 0.7036 0.1578 -0.0684 0.0761 Uiso 1.00 calc . . . H(18) H 0.6229 0.1333 -0.1521 0.0761 Uiso 1.00 calc . . . H(19) H 0.5551 0.1858 -0.0847 0.0869 Uiso 1.00 calc . . . H(20) H 0.6010 0.1647 0.0202 0.0869 Uiso 1.00 calc . . . H(21) H 0.4254 0.1826 0.1115 0.0847 Uiso 1.00 calc . . . H(22) H 0.3820 0.1456 0.0381 0.0847 Uiso 1.00 calc . . . H(23) H 0.2804 0.1621 0.0989 0.1278 Uiso 1.00 calc . . . H(24) H 0.3582 0.1629 0.2077 0.1278 Uiso 1.00 calc . . . H(25) H 0.7205 -0.1645 0.3496 0.1845 Uiso 1.00 calc . . . H(26) H 0.7207 -0.1471 0.4505 0.1845 Uiso 1.00 calc . . . H(27) H 0.6079 -0.1754 0.4150 0.1686 Uiso 1.00 calc . . . H(28) H 0.5934 -0.1781 0.3023 0.1686 Uiso 1.00 calc . . . H(29) H 0.6527 0.1730 0.4316 0.1361 Uiso 1.00 calc . . . H(30) H 0.5704 0.1498 0.3465 0.1361 Uiso 1.00 calc . . . H(31) H 0.5078 0.1907 0.4444 0.1193 Uiso 1.00 calc . . . H(32) H 0.5671 0.1639 0.5376 0.1193 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.091(2) 0.122(2) 0.093(2) 0.052(2) 0.021(1) 0.028(2) Br(2) 0.076(2) 0.065(2) 0.117(2) -0.006(1) 0.038(1) 0.003(1) Br(3) 0.118(3) 0.059(2) 0.072(1) 0.001(1) 0.029(1) 0.000(1) Br(4) 0.083(2) 0.058(2) 0.115(2) -0.019(1) 0.028(1) -0.019(1) Br(5) 0.082(2) 0.104(2) 0.102(2) 0.024(2) 0.008(1) 0.025(2) Br(6) 0.069(2) 0.064(2) 0.130(2) -0.003(1) 0.044(2) -0.008(1) Br(7) 0.122(3) 0.058(2) 0.080(1) 0.012(1) 0.043(1) 0.003(1) Br(8) 0.095(2) 0.052(2) 0.118(2) -0.014(1) 0.037(1) -0.011(1) Ni(1) 0.050(3) 0.054(3) 0.075(2) -0.002(2) 0.031(2) -0.005(2) Ni(2) 0.039(2) 0.075(2) 0.061(1) -0.005(1) 0.019(1) 0.012(1) Ni(3) 0.046(3) 0.051(3) 0.059(2) -0.006(2) 0.020(2) 0.003(2) Ni(4) 0.047(3) 0.050(3) 0.050(2) -0.004(2) 0.011(2) -0.001(2) Ni(5) 0.040(2) 0.046(2) 0.068(1) 0.007(1) 0.024(1) 0.011(1) Ni(6) 0.064(3) 0.040(2) 0.047(2) -0.006(2) 0.018(2) 0.003(2) Fe(1) 0.059(2) 0.049(2) 0.065(2) 0.007(2) 0.014(1) 0.001(1) Fe(2) 0.061(2) 0.048(2) 0.070(2) 0.007(2) 0.023(2) 0.002(1) S(1) 0.049(4) 0.062(4) 0.082(4) -0.001(3) 0.030(3) 0.002(3) S(2) 0.048(4) 0.061(4) 0.068(3) 0.002(3) 0.024(3) -0.001(3) S(3) 0.039(4) 0.069(4) 0.062(3) -0.007(3) 0.020(3) 0.001(3) S(4) 0.035(4) 0.087(5) 0.070(3) -0.013(3) 0.021(3) 0.001(3) S(5) 0.051(4) 0.081(5) 0.098(4) 0.005(3) 0.039(3) 0.024(3) S(6) 0.047(4) 0.072(4) 0.062(3) -0.006(3) 0.020(3) 0.007(3) S(7) 0.046(4) 0.052(4) 0.070(3) -0.003(3) 0.018(3) 0.010(3) S(8) 0.045(4) 0.062(4) 0.056(3) -0.006(3) 0.018(3) 0.004(3) S(9) 0.046(4) 0.049(4) 0.074(3) -0.003(3) 0.021(3) 0.001(3) S(10) 0.054(4) 0.046(4) 0.057(3) -0.003(3) 0.007(3) 0.003(2) S(11) 0.038(4) 0.054(4) 0.050(3) 0.000(3) 0.014(2) 0.005(2) S(12) 0.041(4) 0.046(4) 0.057(3) 0.002(3) 0.019(2) 0.006(2) S(13) 0.042(4) 0.044(4) 0.083(3) 0.005(3) 0.025(3) 0.009(3) S(14) 0.036(4) 0.046(4) 0.072(3) 0.000(3) 0.018(3) 0.007(3) S(15) 0.077(5) 0.057(4) 0.069(3) -0.014(3) 0.035(3) -0.004(3) S(16) 0.072(5) 0.052(4) 0.055(3) 0.001(3) 0.013(3) 0.005(3) O(1) 0.05(1) 0.06(1) 0.086(9) -0.019(10) 0.029(8) 0.008(8) O(2) 0.05(1) 0.05(1) 0.077(9) -0.002(9) 0.025(8) 0.000(8) O(3) 0.05(1) 0.07(1) 0.090(9) -0.006(9) 0.018(8) 0.008(8) O(4) 0.05(1) 0.09(1) 0.12(1) 0.02(1) 0.038(9) 0.004(10) O(5) 0.08(1) 0.09(1) 0.10(1) 0.02(1) 0.045(9) 0.007(9) O(6) 0.06(1) 0.07(1) 0.099(10) -0.01(1) 0.020(9) -0.004(9) O(7) 0.06(1) 0.04(1) 0.080(9) -0.002(9) 0.021(8) 0.019(8) O(8) 0.06(1) 0.06(1) 0.054(8) -0.005(10) 0.017(7) -0.006(7) O(9) 0.05(1) 0.046(10) 0.072(8) -0.005(8) 0.011(7) 0.015(7) O(10) 0.07(1) 0.038(10) 0.086(9) 0.000(8) 0.026(8) 0.018(7) O(11) 0.046(10) 0.038(9) 0.079(8) 0.005(7) 0.020(7) 0.026(7) O(12) 0.05(1) 0.05(1) 0.12(1) 0.011(8) 0.026(8) 0.015(8) O(13) 0.05(1) 0.05(1) 0.097(9) 0.001(8) 0.021(8) 0.001(8) O(14) 0.04(1) 0.036(10) 0.095(9) -0.009(8) 0.011(7) 0.005(7) O(15) 0.11(1) 0.07(1) 0.087(10) -0.03(1) 0.029(9) 0.009(9) O(16) 0.11(1) 0.04(1) 0.10(1) 0.00(1) -0.009(9) -0.007(9) C(1) 0.03(2) 0.09(2) 0.05(1) 0.01(1) 0.02(1) 0.02(1) C(2) 0.07(2) 0.04(2) 0.04(1) 0.01(1) 0.02(1) 0.005(10) C(3) 0.08(2) 0.06(2) 0.11(2) 0.01(2) 0.04(2) 0.00(1) C(4) 0.07(2) 0.08(2) 0.11(2) 0.01(2) 0.04(2) 0.01(1) C(5) 0.05(2) 0.07(2) 0.06(1) -0.01(2) 0.02(1) 0.01(1) C(6) 0.07(2) 0.06(2) 0.05(1) 0.01(2) 0.03(1) 0.009(10) C(7) 0.04(2) 0.09(2) 0.06(1) 0.03(2) 0.03(1) 0.01(1) C(8) 0.08(2) 0.06(2) 0.08(1) -0.01(2) 0.04(1) 0.02(1) C(9) 0.07(2) 0.07(2) 0.06(1) 0.00(1) 0.02(1) 0.00(1) C(10) 0.07(2) 0.08(2) 0.09(2) 0.02(1) 0.03(1) 0.00(1) C(11) 0.07(2) 0.16(3) 0.07(1) 0.03(2) 0.04(1) -0.02(2) C(12) 0.07(2) 0.07(2) 0.10(2) 0.02(2) 0.03(2) -0.01(1) C(13) 0.07(2) 0.04(2) 0.03(1) -0.01(1) 0.02(1) 0.003(9) C(14) 0.04(2) 0.06(2) 0.04(1) -0.02(1) 0.01(1) 0.00(1) C(15) 0.06(2) 0.07(2) 0.06(1) -0.01(1) 0.02(1) 0.01(1) C(16) 0.07(2) 0.03(2) 0.09(1) -0.01(1) 0.02(1) -0.01(1) C(17) 0.07(2) 0.06(2) 0.02(1) -0.01(1) 0.01(1) 0.004(9) C(18) 0.07(2) 0.03(1) 0.06(1) 0.00(1) 0.02(1) 0.00(1) C(19) 0.08(2) 0.07(2) 0.04(1) -0.03(1) 0.02(1) 0.00(1) C(20) 0.10(2) 0.04(2) 0.08(1) 0.00(1) 0.03(1) 0.01(1) C(21) 0.04(2) 0.03(1) 0.03(1) -0.01(1) 0.003(9) -0.001(8) C(22) 0.03(2) 0.05(1) 0.06(1) 0.00(1) 0.02(1) 0.003(9) C(23) 0.05(2) 0.04(1) 0.07(1) 0.00(1) 0.03(1) 0.00(1) C(24) 0.03(2) 0.03(1) 0.07(1) 0.00(1) 0.01(1) -0.015(10) C(25) 0.08(2) 0.07(2) 0.08(1) -0.01(2) 0.02(1) 0.02(1) C(26) 0.10(2) 0.06(2) 0.21(3) 0.05(2) 0.09(2) 0.05(2) C(27) 0.10(3) 0.04(2) 0.38(4) 0.02(2) 0.10(3) 0.09(2) C(28) 0.06(2) 0.02(2) 0.35(4) 0.00(2) 0.06(3) 0.03(2) C(29) 0.11(2) 0.03(2) 0.05(1) -0.02(2) 0.03(1) -0.01(1) C(30) 0.09(2) 0.04(2) 0.06(1) 0.02(2) 0.01(1) 0.00(1) C(31) 0.21(4) 0.07(2) 0.07(2) -0.08(2) 0.01(2) 0.01(2) C(32) 0.18(3) 0.05(2) 0.06(2) 0.00(2) -0.01(2) -0.01(1) #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Fe(1) 2.326(3) . . yes Br(2) Fe(1) 2.354(4) . . yes Br(3) Fe(1) 2.344(3) . . yes Br(4) Fe(1) 2.299(4) . . yes Br(5) Fe(2) 2.328(3) . . yes Br(6) Fe(2) 2.345(4) . . yes Br(7) Fe(2) 2.348(3) . . yes Br(8) Fe(2) 2.312(4) . . yes Ni(1) S(1) 2.155(5) . . yes Ni(1) S(1) 2.155(5) . 3_555 yes Ni(1) S(2) 2.157(5) . . yes Ni(1) S(2) 2.157(5) . 3_555 yes Ni(2) S(3) 2.161(6) . . yes Ni(2) S(4) 2.155(6) . . yes Ni(2) S(5) 2.161(6) . . yes Ni(2) S(6) 2.161(6) . . yes Ni(3) S(7) 2.164(5) . . yes Ni(3) S(7) 2.164(5) . 3_556 yes Ni(3) S(8) 2.182(5) . . yes Ni(3) S(8) 2.182(5) . 3_556 yes Ni(4) S(9) 2.152(5) . . yes Ni(4) S(9) 2.152(5) . 3_655 yes Ni(4) S(10) 2.151(5) . . yes Ni(4) S(10) 2.151(5) . 3_655 yes Ni(5) S(11) 2.148(5) . . yes Ni(5) S(12) 2.166(5) . . yes Ni(5) S(13) 2.166(6) . . yes Ni(5) S(14) 2.160(5) . . yes Ni(6) S(15) 2.156(5) . . yes Ni(6) S(15) 2.156(5) . 3_656 yes Ni(6) S(16) 2.176(5) . . yes Ni(6) S(16) 2.176(5) . 3_656 yes S(1) C(1) 1.67(2) . . yes S(2) C(2) 1.68(2) . . yes S(3) C(5) 1.69(2) . . yes S(4) C(6) 1.68(2) . . yes S(5) C(7) 1.64(2) . . yes S(6) C(8) 1.68(2) . . yes S(7) C(13) 1.68(2) . . yes S(8) C(14) 1.68(2) . . yes S(9) C(17) 1.67(2) . . yes S(10) C(18) 1.68(2) . . yes S(11) C(21) 1.67(2) . . yes S(12) C(22) 1.66(2) . . yes S(13) C(23) 1.65(2) . . yes S(14) C(24) 1.69(2) . . yes S(15) C(29) 1.67(2) . . yes S(16) C(30) 1.70(3) . . yes O(1) C(1) 1.32(2) . . yes O(1) C(3) 1.46(2) . . yes O(2) C(2) 1.36(2) . . yes O(2) C(4) 1.44(2) . . yes O(3) C(5) 1.32(2) . . yes O(3) C(9) 1.46(2) . . yes O(4) C(6) 1.34(2) . . yes O(4) C(10) 1.40(2) . . yes O(5) C(7) 1.33(2) . . yes O(5) C(11) 1.42(3) . . yes O(6) C(8) 1.33(2) . . yes O(6) C(12) 1.45(2) . . yes O(7) C(13) 1.35(2) . . yes O(7) C(15) 1.44(2) . . yes O(8) C(14) 1.35(2) . . yes O(8) C(16) 1.44(2) . . yes O(9) C(17) 1.37(2) . . yes O(9) C(19) 1.41(2) . . yes O(10) C(18) 1.33(2) . . yes O(10) C(20) 1.47(2) . . yes O(11) C(21) 1.33(2) . . yes O(11) C(25) 1.45(2) . . yes O(12) C(22) 1.35(2) . . yes O(12) C(26) 1.43(3) . . yes O(13) C(23) 1.33(2) . . yes O(13) C(27) 1.43(2) . . yes O(14) C(24) 1.33(2) . . yes O(14) C(28) 1.45(3) . . yes O(15) C(29) 1.39(2) . . yes O(15) C(31) 1.47(3) . . yes O(16) C(30) 1.35(2) . . yes O(16) C(32) 1.44(3) . . yes C(1) C(2) 1.42(2) . . yes C(3) C(4) 1.43(3) . . yes C(5) C(6) 1.41(3) . . yes C(7) C(8) 1.41(3) . . yes C(9) C(10) 1.50(3) . . yes C(11) C(12) 1.48(3) . . yes C(13) C(14) 1.41(2) . . yes C(15) C(16) 1.46(3) . . yes C(17) C(18) 1.42(3) . . yes C(19) C(20) 1.50(3) . . yes C(21) C(22) 1.40(2) . . yes C(23) C(24) 1.41(2) . . yes C(25) C(26) 1.36(3) . . yes C(27) C(28) 1.24(3) . . yes C(29) C(30) 1.34(3) . . yes C(31) C(32) 1.49(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(1) 180.0 1_555 1_555 3_555 yes S(1) Ni(1) S(2) 92.6(2) 1_555 1_555 1_555 yes S(1) Ni(1) S(2) 87.4(2) 1_555 1_555 3_555 yes S(1) Ni(1) S(2) 87.4(2) 3_555 1_555 1_555 yes S(1) Ni(1) S(2) 92.6(2) 3_555 1_555 3_555 yes S(2) Ni(1) S(2) 180.0 1_555 1_555 3_555 yes S(3) Ni(2) S(4) 92.6(2) 1_555 1_555 1_555 yes S(3) Ni(2) S(5) 87.1(2) 1_555 1_555 1_555 yes S(3) Ni(2) S(6) 175.1(2) 1_555 1_555 1_555 yes S(4) Ni(2) S(5) 179.6(2) 1_555 1_555 1_555 yes S(4) Ni(2) S(6) 87.9(2) 1_555 1_555 1_555 yes S(5) Ni(2) S(6) 92.4(2) 1_555 1_555 1_555 yes S(7) Ni(3) S(7) 180.0 1_555 1_555 3_556 yes S(7) Ni(3) S(8) 92.1(2) 1_555 1_555 1_555 yes S(7) Ni(3) S(8) 87.9(2) 1_555 1_555 3_556 yes S(7) Ni(3) S(8) 87.9(2) 3_556 1_555 1_555 yes S(7) Ni(3) S(8) 92.1(2) 3_556 1_555 3_556 yes S(8) Ni(3) S(8) 180.0 1_555 1_555 3_556 yes S(9) Ni(4) S(9) 180.0 1_555 1_555 3_655 yes S(9) Ni(4) S(10) 93.0(2) 1_555 1_555 1_555 yes S(9) Ni(4) S(10) 87.0(2) 1_555 1_555 3_655 yes S(9) Ni(4) S(10) 87.0(2) 3_655 1_555 1_555 yes S(9) Ni(4) S(10) 93.0(2) 3_655 1_555 3_655 yes S(10) Ni(4) S(10) 180.0 1_555 1_555 3_655 yes S(11) Ni(5) S(12) 92.3(2) 1_555 1_555 1_555 yes S(11) Ni(5) S(13) 88.1(2) 1_555 1_555 1_555 yes S(11) Ni(5) S(14) 169.3(2) 1_555 1_555 1_555 yes S(12) Ni(5) S(13) 173.9(2) 1_555 1_555 1_555 yes S(12) Ni(5) S(14) 86.5(2) 1_555 1_555 1_555 yes S(13) Ni(5) S(14) 91.9(2) 1_555 1_555 1_555 yes S(15) Ni(6) S(15) 180.0 1_555 1_555 3_656 yes S(15) Ni(6) S(16) 91.5(2) 1_555 1_555 1_555 yes S(15) Ni(6) S(16) 88.5(2) 1_555 1_555 3_656 yes S(15) Ni(6) S(16) 88.5(2) 3_656 1_555 1_555 yes S(15) Ni(6) S(16) 91.5(2) 3_656 1_555 3_656 yes S(16) Ni(6) S(16) 180.0 1_555 1_555 3_656 yes Br(1) Fe(1) Br(2) 107.8(1) 1_555 1_555 1_555 yes Br(1) Fe(1) Br(3) 110.4(1) 1_555 1_555 1_555 yes Br(1) Fe(1) Br(4) 110.6(1) 1_555 1_555 1_555 yes Br(2) Fe(1) Br(3) 108.7(1) 1_555 1_555 1_555 yes Br(2) Fe(1) Br(4) 110.5(1) 1_555 1_555 1_555 yes Br(3) Fe(1) Br(4) 108.8(1) 1_555 1_555 1_555 yes Br(5) Fe(2) Br(6) 109.3(1) 1_555 1_555 1_555 yes Br(5) Fe(2) Br(7) 111.3(1) 1_555 1_555 1_555 yes Br(5) Fe(2) Br(8) 109.2(1) 1_555 1_555 1_555 yes Br(6) Fe(2) Br(7) 106.3(1) 1_555 1_555 1_555 yes Br(6) Fe(2) Br(8) 110.4(1) 1_555 1_555 1_555 yes Br(7) Fe(2) Br(8) 110.2(1) 1_555 1_555 1_555 yes Ni(1) S(1) C(1) 105.0(9) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 101.5(9) 1_555 1_555 1_555 yes Ni(2) S(3) C(5) 103.4(9) 1_555 1_555 1_555 yes Ni(2) S(4) C(6) 102(1) 1_555 1_555 1_555 yes Ni(2) S(5) C(7) 102.0(9) 1_555 1_555 1_555 yes Ni(2) S(6) C(8) 103.3(9) 1_555 1_555 1_555 yes Ni(3) S(7) C(13) 102.9(9) 1_555 1_555 1_555 yes Ni(3) S(8) C(14) 103(1) 1_555 1_555 1_555 yes Ni(4) S(9) C(17) 102.3(10) 1_555 1_555 1_555 yes Ni(4) S(10) C(18) 103.5(8) 1_555 1_555 1_555 yes Ni(5) S(11) C(21) 103.1(8) 1_555 1_555 1_555 yes Ni(5) S(12) C(22) 102.7(8) 1_555 1_555 1_555 yes Ni(5) S(13) C(23) 103.9(9) 1_555 1_555 1_555 yes Ni(5) S(14) C(24) 103.1(8) 1_555 1_555 1_555 yes Ni(6) S(15) C(29) 101(1) 1_555 1_555 1_555 yes Ni(6) S(16) C(30) 101.9(9) 1_555 1_555 1_555 yes C(1) O(1) C(3) 115(1) 1_555 1_555 1_555 yes C(2) O(2) C(4) 113(1) 1_555 1_555 1_555 yes C(5) O(3) C(9) 113(1) 1_555 1_555 1_555 yes C(6) O(4) C(10) 114(1) 1_555 1_555 1_555 yes C(7) O(5) C(11) 117(2) 1_555 1_555 1_555 yes C(8) O(6) C(12) 113(1) 1_555 1_555 1_555 yes C(13) O(7) C(15) 115(1) 1_555 1_555 1_555 yes C(14) O(8) C(16) 114(1) 1_555 1_555 1_555 yes C(17) O(9) C(19) 113(1) 1_555 1_555 1_555 yes C(18) O(10) C(20) 113(1) 1_555 1_555 1_555 yes C(21) O(11) C(25) 114(1) 1_555 1_555 1_555 yes C(22) O(12) C(26) 113(1) 1_555 1_555 1_555 yes C(23) O(13) C(27) 115(1) 1_555 1_555 1_555 yes C(24) O(14) C(28) 113(1) 1_555 1_555 1_555 yes C(29) O(15) C(31) 112(2) 1_555 1_555 1_555 yes C(30) O(16) C(32) 112(2) 1_555 1_555 1_555 yes S(1) C(1) O(1) 120(1) 1_555 1_555 1_555 yes S(1) C(1) C(2) 117(1) 1_555 1_555 1_555 yes O(1) C(1) C(2) 121(2) 1_555 1_555 1_555 yes S(2) C(2) O(2) 115(1) 1_555 1_555 1_555 yes S(2) C(2) C(1) 123(1) 1_555 1_555 1_555 yes O(2) C(2) C(1) 121(2) 1_555 1_555 1_555 yes O(1) C(3) C(4) 112(1) 1_555 1_555 1_555 yes O(1) C(3) H(1) 110(2) 1_555 1_555 1_555 no O(1) C(3) H(2) 110(2) 1_555 1_555 1_555 no C(4) C(3) H(1) 111(2) 1_555 1_555 1_555 no C(4) C(3) H(2) 106(2) 1_555 1_555 1_555 no H(1) C(3) H(2) 105(2) 1_555 1_555 1_555 no O(2) C(4) C(3) 112(2) 1_555 1_555 1_555 yes O(2) C(4) H(3) 113(2) 1_555 1_555 1_555 no O(2) C(4) H(4) 111(2) 1_555 1_555 1_555 no C(3) C(4) H(3) 109(2) 1_555 1_555 1_555 no C(3) C(4) H(4) 105(2) 1_555 1_555 1_555 no H(3) C(4) H(4) 103(2) 1_555 1_555 1_555 no S(3) C(5) O(3) 119(1) 1_555 1_555 1_555 yes S(3) C(5) C(6) 119(2) 1_555 1_555 1_555 yes O(3) C(5) C(6) 120(2) 1_555 1_555 1_555 yes S(4) C(6) O(4) 114(2) 1_555 1_555 1_555 yes S(4) C(6) C(5) 121(2) 1_555 1_555 1_555 yes O(4) C(6) C(5) 123(2) 1_555 1_555 1_555 yes S(5) C(7) O(5) 115(2) 1_555 1_555 1_555 yes S(5) C(7) C(8) 124(1) 1_555 1_555 1_555 yes O(5) C(7) C(8) 119(2) 1_555 1_555 1_555 yes S(6) C(8) O(6) 118(1) 1_555 1_555 1_555 yes S(6) C(8) C(7) 117(1) 1_555 1_555 1_555 yes O(6) C(8) C(7) 123(2) 1_555 1_555 1_555 yes O(3) C(9) C(10) 109(1) 1_555 1_555 1_555 yes O(3) C(9) H(5) 111(2) 1_555 1_555 1_555 no O(3) C(9) H(6) 111(2) 1_555 1_555 1_555 no C(10) C(9) H(5) 112(2) 1_555 1_555 1_555 no C(10) C(9) H(6) 107(2) 1_555 1_555 1_555 no H(5) C(9) H(6) 104(1) 1_555 1_555 1_555 no O(4) C(10) C(9) 112(1) 1_555 1_555 1_555 yes O(4) C(10) H(7) 113(2) 1_555 1_555 1_555 no O(4) C(10) H(8) 112(2) 1_555 1_555 1_555 no C(9) C(10) H(7) 109(2) 1_555 1_555 1_555 no C(9) C(10) H(8) 106(2) 1_555 1_555 1_555 no H(7) C(10) H(8) 100(1) 1_555 1_555 1_555 no O(5) C(11) C(12) 110(1) 1_555 1_555 1_555 yes O(5) C(11) H(9) 113(2) 1_555 1_555 1_555 no O(5) C(11) H(10) 113(2) 1_555 1_555 1_555 no C(12) C(11) H(9) 105(2) 1_555 1_555 1_555 no C(12) C(11) H(10) 110(2) 1_555 1_555 1_555 no H(9) C(11) H(10) 102(1) 1_555 1_555 1_555 no O(6) C(12) C(11) 110(1) 1_555 1_555 1_555 yes O(6) C(12) H(11) 112(2) 1_555 1_555 1_555 no O(6) C(12) H(12) 112(2) 1_555 1_555 1_555 no C(11) C(12) H(11) 107(2) 1_555 1_555 1_555 no C(11) C(12) H(12) 112(2) 1_555 1_555 1_555 no H(11) C(12) H(12) 101(2) 1_555 1_555 1_555 no S(7) C(13) O(7) 115(1) 1_555 1_555 1_555 yes S(7) C(13) C(14) 121(1) 1_555 1_555 1_555 yes O(7) C(13) C(14) 122(2) 1_555 1_555 1_555 yes S(8) C(14) O(8) 118(2) 1_555 1_555 1_555 yes S(8) C(14) C(13) 119(2) 1_555 1_555 1_555 yes O(8) C(14) C(13) 121(1) 1_555 1_555 1_555 yes O(7) C(15) C(16) 112(1) 1_555 1_555 1_555 yes O(7) C(15) H(13) 112(2) 1_555 1_555 1_555 no O(7) C(15) H(14) 112(2) 1_555 1_555 1_555 no C(16) C(15) H(13) 107(2) 1_555 1_555 1_555 no C(16) C(15) H(14) 106(2) 1_555 1_555 1_555 no H(13) C(15) H(14) 104(1) 1_555 1_555 1_555 no O(8) C(16) C(15) 113(1) 1_555 1_555 1_555 yes O(8) C(16) H(15) 108(2) 1_555 1_555 1_555 no O(8) C(16) H(16) 109(1) 1_555 1_555 1_555 no C(15) C(16) H(15) 111(2) 1_555 1_555 1_555 no C(15) C(16) H(16) 109(2) 1_555 1_555 1_555 no H(15) C(16) H(16) 103(1) 1_555 1_555 1_555 no S(9) C(17) O(9) 116(1) 1_555 1_555 1_555 yes S(9) C(17) C(18) 122(1) 1_555 1_555 1_555 yes O(9) C(17) C(18) 121(1) 1_555 1_555 1_555 yes S(10) C(18) O(10) 118(1) 1_555 1_555 1_555 yes S(10) C(18) C(17) 118(1) 1_555 1_555 1_555 yes O(10) C(18) C(17) 122(1) 1_555 1_555 1_555 yes O(9) C(19) C(20) 110(1) 1_555 1_555 1_555 yes O(9) C(19) H(17) 110(2) 1_555 1_555 1_555 no O(9) C(19) H(18) 112(1) 1_555 1_555 1_555 no C(20) C(19) H(17) 110(2) 1_555 1_555 1_555 no C(20) C(19) H(18) 109(2) 1_555 1_555 1_555 no H(17) C(19) H(18) 103(1) 1_555 1_555 1_555 no O(10) C(20) C(19) 109(1) 1_555 1_555 1_555 yes O(10) C(20) H(19) 112(2) 1_555 1_555 1_555 no O(10) C(20) H(20) 112(1) 1_555 1_555 1_555 no C(19) C(20) H(19) 109(2) 1_555 1_555 1_555 no C(19) C(20) H(20) 107(2) 1_555 1_555 1_555 no H(19) C(20) H(20) 105(1) 1_555 1_555 1_555 no S(11) C(21) O(11) 117(1) 1_555 1_555 1_555 yes S(11) C(21) C(22) 120(1) 1_555 1_555 1_555 yes O(11) C(21) C(22) 122(1) 1_555 1_555 1_555 yes S(12) C(22) O(12) 116(1) 1_555 1_555 1_555 yes S(12) C(22) C(21) 121(1) 1_555 1_555 1_555 yes O(12) C(22) C(21) 122(1) 1_555 1_555 1_555 yes S(13) C(23) O(13) 119(1) 1_555 1_555 1_555 yes S(13) C(23) C(24) 121(1) 1_555 1_555 1_555 yes O(13) C(23) C(24) 119(1) 1_555 1_555 1_555 yes S(14) C(24) O(14) 115(1) 1_555 1_555 1_555 yes S(14) C(24) C(23) 119(1) 1_555 1_555 1_555 yes O(14) C(24) C(23) 124(1) 1_555 1_555 1_555 yes O(11) C(25) C(26) 115(1) 1_555 1_555 1_555 yes O(11) C(25) H(21) 109(2) 1_555 1_555 1_555 no O(11) C(25) H(22) 110(2) 1_555 1_555 1_555 no C(26) C(25) H(21) 110(2) 1_555 1_555 1_555 no C(26) C(25) H(22) 105(2) 1_555 1_555 1_555 no H(21) C(25) H(22) 104(1) 1_555 1_555 1_555 no O(12) C(26) C(25) 117(2) 1_555 1_555 1_555 yes O(12) C(26) H(23) 112(2) 1_555 1_555 1_555 no O(12) C(26) H(24) 111(2) 1_555 1_555 1_555 no C(25) C(26) H(23) 107(2) 1_555 1_555 1_555 no C(25) C(26) H(24) 104(2) 1_555 1_555 1_555 no H(23) C(26) H(24) 102(2) 1_555 1_555 1_555 no O(13) C(27) C(28) 124(2) 1_555 1_555 1_555 yes O(13) C(27) H(25) 108(2) 1_555 1_555 1_555 no O(13) C(27) H(26) 106(2) 1_555 1_555 1_555 no C(28) C(27) H(25) 106(3) 1_555 1_555 1_555 no C(28) C(27) H(26) 104(3) 1_555 1_555 1_555 no H(25) C(27) H(26) 104(2) 1_555 1_555 1_555 no O(14) C(28) C(27) 121(2) 1_555 1_555 1_555 yes O(14) C(28) H(27) 108(2) 1_555 1_555 1_555 no O(14) C(28) H(28) 109(2) 1_555 1_555 1_555 no C(27) C(28) H(27) 107(3) 1_555 1_555 1_555 no C(27) C(28) H(28) 105(3) 1_555 1_555 1_555 no H(27) C(28) H(28) 102(2) 1_555 1_555 1_555 no S(15) C(29) O(15) 114(2) 1_555 1_555 1_555 yes S(15) C(29) C(30) 123(2) 1_555 1_555 1_555 yes O(15) C(29) C(30) 122(2) 1_555 1_555 1_555 yes S(16) C(30) O(16) 116(2) 1_555 1_555 1_555 yes S(16) C(30) C(29) 119(2) 1_555 1_555 1_555 yes O(16) C(30) C(29) 123(2) 1_555 1_555 1_555 yes O(15) C(31) C(32) 108(2) 1_555 1_555 1_555 yes O(15) C(31) H(29) 109(3) 1_555 1_555 1_555 no O(15) C(31) H(30) 111(2) 1_555 1_555 1_555 no C(32) C(31) H(29) 111(3) 1_555 1_555 1_555 no C(32) C(31) H(30) 112(3) 1_555 1_555 1_555 no H(29) C(31) H(30) 103(2) 1_555 1_555 1_555 no O(16) C(32) C(31) 108(2) 1_555 1_555 1_555 yes O(16) C(32) H(31) 112(2) 1_555 1_555 1_555 no O(16) C(32) H(32) 112(2) 1_555 1_555 1_555 no C(31) C(32) H(31) 108(3) 1_555 1_555 1_555 no C(31) C(32) H(32) 106(3) 1_555 1_555 1_555 no H(31) C(32) H(32) 107(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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 Ni(1) S(1) C(1) O(1) -178(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(1) C(1) C(2) 1(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(1) C(1) O(1) 178(1) 1_555 3_555 3_555 3_555 yes Ni(1) S(1) C(1) C(2) -1(1) 1_555 3_555 3_555 3_555 yes Ni(1) S(2) C(2) O(2) -179(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) C(1) 1(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) O(2) 179(1) 1_555 3_555 3_555 3_555 yes Ni(1) S(2) C(2) C(1) -1(1) 1_555 3_555 3_555 3_555 yes Ni(2) S(3) C(5) O(3) -176(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(3) C(5) C(6) 0(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(4) C(6) O(4) -177(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(4) C(6) C(5) 0(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(5) C(7) O(5) 179(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(5) C(7) C(8) 1(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(6) C(8) O(6) 174(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(6) C(8) C(7) -3(1) 1_555 1_555 1_555 1_555 yes Ni(3) S(7) C(13) O(7) 178(1) 1_555 1_555 1_555 1_555 yes Ni(3) S(7) C(13) C(14) -2(1) 1_555 1_555 1_555 1_555 yes Ni(3) S(7) C(13) O(7) -178(1) 1_555 3_556 3_556 3_556 yes Ni(3) S(7) C(13) C(14) 2(1) 1_555 3_556 3_556 3_556 yes Ni(3) S(8) C(14) O(8) -172(1) 1_555 1_555 1_555 1_555 yes Ni(3) S(8) C(14) C(13) 2(1) 1_555 1_555 1_555 1_555 yes Ni(3) S(8) C(14) O(8) 172(1) 1_555 3_556 3_556 3_556 yes Ni(3) S(8) C(14) C(13) -2(1) 1_555 3_556 3_556 3_556 yes Ni(4) S(9) C(17) O(9) -179(1) 1_555 1_555 1_555 1_555 yes Ni(4) S(9) C(17) C(18) 0(1) 1_555 1_555 1_555 1_555 yes Ni(4) S(9) C(17) O(9) 179(1) 1_555 3_655 3_655 3_655 yes Ni(4) S(9) C(17) C(18) 0(1) 1_555 3_655 3_655 3_655 yes Ni(4) S(10) C(18) O(10) -177(1) 1_555 1_555 1_555 1_555 yes Ni(4) S(10) C(18) C(17) 1(1) 1_555 1_555 1_555 1_555 yes Ni(4) S(10) C(18) O(10) 177(1) 1_555 3_655 3_655 3_655 yes Ni(4) S(10) C(18) C(17) -1(1) 1_555 3_655 3_655 3_655 yes Ni(5) S(11) C(21) O(11) 179(1) 1_555 1_555 1_555 1_555 yes Ni(5) S(11) C(21) C(22) -1(1) 1_555 1_555 1_555 1_555 yes Ni(5) S(12) C(22) O(12) -177(1) 1_555 1_555 1_555 1_555 yes Ni(5) S(12) C(22) C(21) 5(1) 1_555 1_555 1_555 1_555 yes Ni(5) S(13) C(23) O(13) -178(1) 1_555 1_555 1_555 1_555 yes Ni(5) S(13) C(23) C(24) 0(1) 1_555 1_555 1_555 1_555 yes Ni(5) S(14) C(24) O(14) 179(1) 1_555 1_555 1_555 1_555 yes Ni(5) S(14) C(24) C(23) 0(1) 1_555 1_555 1_555 1_555 yes Ni(6) S(15) C(29) O(15) 176(1) 1_555 1_555 1_555 1_555 yes Ni(6) S(15) C(29) C(30) -11(1) 1_555 1_555 1_555 1_555 yes Ni(6) S(15) C(29) O(15) -176(1) 1_555 3_656 3_656 3_656 yes Ni(6) S(15) C(29) C(30) 11(1) 1_555 3_656 3_656 3_656 yes Ni(6) S(16) C(30) O(16) -172(1) 1_555 1_555 1_555 1_555 yes Ni(6) S(16) C(30) C(29) 8(1) 1_555 1_555 1_555 1_555 yes Ni(6) S(16) C(30) O(16) 172(1) 1_555 3_656 3_656 3_656 yes Ni(6) S(16) C(30) C(29) -8(1) 1_555 3_656 3_656 3_656 yes S(1) Ni(1) S(2) C(2) -0.6(6) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(2) C(2) -179.4(6) 1_555 1_555 3_555 3_555 yes S(1) C(1) O(1) C(3) 168(1) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) S(2) -1(1) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) O(2) 178(1) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(1) C(1) -0.2(6) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(1) C(1) -179.8(6) 1_555 1_555 3_555 3_555 yes S(2) C(2) O(2) C(4) 166(1) 1_555 1_555 1_555 1_555 yes S(2) C(2) C(1) O(1) 177(1) 1_555 1_555 1_555 1_555 yes S(3) Ni(2) S(4) C(6) -0.6(6) 1_555 1_555 1_555 1_555 yes S(3) Ni(2) S(5) C(7) -177.4(6) 1_555 1_555 1_555 1_555 yes S(3) Ni(2) S(6) C(8) 86(3) 1_555 1_555 1_555 1_555 yes S(3) C(5) O(3) C(9) 157(1) 1_555 1_555 1_555 1_555 yes S(3) C(5) C(6) S(4) 0(2) 1_555 1_555 1_555 1_555 yes S(3) C(5) C(6) O(4) 177(1) 1_555 1_555 1_555 1_555 yes S(4) Ni(2) S(3) C(5) 0.2(6) 1_555 1_555 1_555 1_555 yes S(4) Ni(2) S(5) C(7) 132(30) 1_555 1_555 1_555 1_555 yes S(4) Ni(2) S(6) C(8) -176.7(7) 1_555 1_555 1_555 1_555 yes S(4) C(6) O(4) C(10) 175(1) 1_555 1_555 1_555 1_555 yes S(4) C(6) C(5) O(3) 176(1) 1_555 1_555 1_555 1_555 yes S(5) Ni(2) S(3) C(5) -179.4(6) 1_555 1_555 1_555 1_555 yes S(5) Ni(2) S(4) C(6) 49(30) 1_555 1_555 1_555 1_555 yes S(5) Ni(2) S(6) C(8) 3.0(7) 1_555 1_555 1_555 1_555 yes S(5) C(7) O(5) C(11) -171(1) 1_555 1_555 1_555 1_555 yes S(5) C(7) C(8) S(6) 1(2) 1_555 1_555 1_555 1_555 yes S(5) C(7) C(8) O(6) -176(1) 1_555 1_555 1_555 1_555 yes S(6) Ni(2) S(3) C(5) 96(3) 1_555 1_555 1_555 1_555 yes S(6) Ni(2) S(4) C(6) -175.7(6) 1_555 1_555 1_555 1_555 yes S(6) Ni(2) S(5) C(7) -2.3(6) 1_555 1_555 1_555 1_555 yes S(6) C(8) O(6) C(12) -161(1) 1_555 1_555 1_555 1_555 yes S(6) C(8) C(7) O(5) -177(1) 1_555 1_555 1_555 1_555 yes S(7) Ni(3) S(8) C(14) -3.5(6) 1_555 1_555 1_555 1_555 yes S(7) Ni(3) S(8) C(14) -176.5(6) 1_555 1_555 3_556 3_556 yes S(7) C(13) O(7) C(15) 173(1) 1_555 1_555 1_555 1_555 yes S(7) C(13) C(14) S(8) 0(1) 1_555 1_555 1_555 1_555 yes S(7) C(13) C(14) O(8) 175(1) 1_555 1_555 1_555 1_555 yes S(8) Ni(3) S(7) C(13) 3.3(5) 1_555 1_555 1_555 1_555 yes S(8) Ni(3) S(7) C(13) 176.7(5) 1_555 1_555 3_556 3_556 yes S(8) C(14) O(8) C(16) 162(1) 1_555 1_555 1_555 1_555 yes S(8) C(14) C(13) O(7) 178(1) 1_555 1_555 1_555 1_555 yes S(9) Ni(4) S(10) C(18) -1.0(6) 1_555 1_555 1_555 1_555 yes S(9) Ni(4) S(10) C(18) -179.0(6) 1_555 1_555 3_655 3_655 yes S(9) C(17) O(9) C(19) 163(1) 1_555 1_555 1_555 1_555 yes S(9) C(17) C(18) S(10) 0(2) 1_555 1_555 1_555 1_555 yes S(9) C(17) C(18) O(10) 178(1) 1_555 1_555 1_555 1_555 yes S(10) Ni(4) S(9) C(17) 0.8(6) 1_555 1_555 1_555 1_555 yes S(10) Ni(4) S(9) C(17) 179.2(6) 1_555 1_555 3_655 3_655 yes S(10) C(18) O(10) C(20) 165(1) 1_555 1_555 1_555 1_555 yes S(10) C(18) C(17) O(9) 178(1) 1_555 1_555 1_555 1_555 yes S(11) Ni(5) S(12) C(22) -4.7(6) 1_555 1_555 1_555 1_555 yes S(11) Ni(5) S(13) C(23) -169.9(7) 1_555 1_555 1_555 1_555 yes S(11) Ni(5) S(14) C(24) 90(1) 1_555 1_555 1_555 1_555 yes S(11) C(21) O(11) C(25) 168(1) 1_555 1_555 1_555 1_555 yes S(11) C(21) C(22) S(12) -2(1) 1_555 1_555 1_555 1_555 yes S(11) C(21) C(22) O(12) 179(1) 1_555 1_555 1_555 1_555 yes S(12) Ni(5) S(11) C(21) 3.6(6) 1_555 1_555 1_555 1_555 yes S(12) Ni(5) S(13) C(23) -75(2) 1_555 1_555 1_555 1_555 yes S(12) Ni(5) S(14) C(24) 174.8(6) 1_555 1_555 1_555 1_555 yes S(12) C(22) O(12) C(26) 172(1) 1_555 1_555 1_555 1_555 yes S(12) C(22) C(21) O(11) 176(1) 1_555 1_555 1_555 1_555 yes S(13) Ni(5) S(11) C(21) 177.5(5) 1_555 1_555 1_555 1_555 yes S(13) Ni(5) S(12) C(22) -98(2) 1_555 1_555 1_555 1_555 yes S(13) Ni(5) S(14) C(24) 0.7(6) 1_555 1_555 1_555 1_555 yes S(13) C(23) O(13) C(27) 173(1) 1_555 1_555 1_555 1_555 yes S(13) C(23) C(24) S(14) 0(2) 1_555 1_555 1_555 1_555 yes S(13) C(23) C(24) O(14) -179(1) 1_555 1_555 1_555 1_555 yes S(14) Ni(5) S(11) C(21) 86(1) 1_555 1_555 1_555 1_555 yes S(14) Ni(5) S(12) C(22) -174.0(6) 1_555 1_555 1_555 1_555 yes S(14) Ni(5) S(13) C(23) -0.6(7) 1_555 1_555 1_555 1_555 yes S(14) C(24) O(14) C(28) 179(1) 1_555 1_555 1_555 1_555 yes S(14) C(24) C(23) O(13) 179(1) 1_555 1_555 1_555 1_555 yes S(15) Ni(6) S(16) C(30) -12.0(7) 1_555 1_555 1_555 1_555 yes S(15) Ni(6) S(16) C(30) -168.0(7) 1_555 1_555 3_656 3_656 yes S(15) C(29) O(15) C(31) 162(1) 1_555 1_555 1_555 1_555 yes S(15) C(29) C(30) S(16) 1(2) 1_555 1_555 1_555 1_555 yes S(15) C(29) C(30) O(16) -177(1) 1_555 1_555 1_555 1_555 yes S(16) Ni(6) S(15) C(29) 12.5(7) 1_555 1_555 1_555 1_555 yes S(16) Ni(6) S(15) C(29) 167.5(7) 1_555 1_555 3_656 3_656 yes S(16) C(30) O(16) C(32) 165(1) 1_555 1_555 1_555 1_555 yes S(16) C(30) C(29) O(15) 172(1) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) O(2) -1(2) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) O(2) -55(2) 1_555 1_555 1_555 1_555 yes O(3) C(5) C(6) O(4) -5(2) 1_555 1_555 1_555 1_555 yes O(3) C(9) C(10) O(4) -58(2) 1_555 1_555 1_555 1_555 yes O(5) C(7) C(8) O(6) 4(2) 1_555 1_555 1_555 1_555 yes O(5) C(11) C(12) O(6) 57(2) 1_555 1_555 1_555 1_555 yes O(7) C(13) C(14) O(8) -6(2) 1_555 1_555 1_555 1_555 yes O(7) C(15) C(16) O(8) -54(2) 1_555 1_555 1_555 1_555 yes O(9) C(17) C(18) O(10) -2(2) 1_555 1_555 1_555 1_555 yes O(9) C(19) C(20) O(10) -62(1) 1_555 1_555 1_555 1_555 yes O(11) C(21) C(22) O(12) 0(2) 1_555 1_555 1_555 1_555 yes O(11) C(25) C(26) O(12) -46(3) 1_555 1_555 1_555 1_555 yes O(13) C(23) C(24) O(14) 0(2) 1_555 1_555 1_555 1_555 yes O(13) C(27) C(28) O(14) -17(6) 1_555 1_555 1_555 1_555 yes O(15) C(29) C(30) O(16) -5(3) 1_555 1_555 1_555 1_555 yes O(15) C(31) C(32) O(16) -64(2) 1_555 1_555 1_555 1_555 yes C(1) O(1) C(3) C(4) 39(2) 1_555 1_555 1_555 1_555 yes C(1) C(2) O(2) C(4) -14(2) 1_555 1_555 1_555 1_555 yes C(2) O(2) C(4) C(3) 42(2) 1_555 1_555 1_555 1_555 yes C(2) C(1) O(1) C(3) -11(2) 1_555 1_555 1_555 1_555 yes C(5) O(3) C(9) C(10) 49(2) 1_555 1_555 1_555 1_555 yes C(5) C(6) O(4) C(10) -2(2) 1_555 1_555 1_555 1_555 yes C(6) O(4) C(10) C(9) 34(2) 1_555 1_555 1_555 1_555 yes C(6) C(5) O(3) C(9) -19(2) 1_555 1_555 1_555 1_555 yes C(7) O(5) C(11) C(12) -37(2) 1_555 1_555 1_555 1_555 yes C(7) C(8) O(6) C(12) 16(2) 1_555 1_555 1_555 1_555 yes C(8) O(6) C(12) C(11) -46(2) 1_555 1_555 1_555 1_555 yes C(8) C(7) O(5) C(11) 7(2) 1_555 1_555 1_555 1_555 yes C(13) O(7) C(15) C(16) 34(2) 1_555 1_555 1_555 1_555 yes C(13) C(14) O(8) C(16) -13(2) 1_555 1_555 1_555 1_555 yes C(14) O(8) C(16) C(15) 43(2) 1_555 1_555 1_555 1_555 yes C(14) C(13) O(7) C(15) -5(2) 1_555 1_555 1_555 1_555 yes C(17) O(9) C(19) C(20) 47(2) 1_555 1_555 1_555 1_555 yes C(17) C(18) O(10) C(20) -13(2) 1_555 1_555 1_555 1_555 yes C(18) O(10) C(20) C(19) 43(2) 1_555 1_555 1_555 1_555 yes C(18) C(17) O(9) C(19) -15(2) 1_555 1_555 1_555 1_555 yes C(21) O(11) C(25) C(26) 34(2) 1_555 1_555 1_555 1_555 yes C(21) C(22) O(12) C(26) -9(2) 1_555 1_555 1_555 1_555 yes C(22) O(12) C(26) C(25) 33(2) 1_555 1_555 1_555 1_555 yes C(22) C(21) O(11) C(25) -10(2) 1_555 1_555 1_555 1_555 yes C(23) O(13) C(27) C(28) 15(5) 1_555 1_555 1_555 1_555 yes C(23) C(24) O(14) C(28) 0(2) 1_555 1_555 1_555 1_555 yes C(24) O(14) C(28) C(27) 9(4) 1_555 1_555 1_555 1_555 yes C(24) C(23) O(13) C(27) -5(2) 1_555 1_555 1_555 1_555 yes C(29) O(15) C(31) C(32) 43(2) 1_555 1_555 1_555 1_555 yes C(29) C(30) O(16) C(32) -15(2) 1_555 1_555 1_555 1_555 yes C(30) O(16) C(32) C(31) 50(2) 1_555 1_555 1_555 1_555 yes C(30) C(29) O(15) C(31) -9(2) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni(2) S(7) 3.422(5) . . ? Ni(2) Ni(3) 3.518(2) . . ? Ni(3) S(4) 3.525(4) . . ? Ni(3) S(4) 3.525(4) . 3_556 ? Ni(4) S(11) 3.584(4) . . ? Ni(4) S(11) 3.584(4) . 3_655 ? Ni(5) S(15) 2.961(5) . . ? Ni(5) Ni(6) 3.377(2) . . ? Ni(6) S(14) 3.365(5) . . ? Ni(6) S(14) 3.365(5) . 3_656 ? S(1) O(12) 3.52(1) . . ? S(1) S(6) 3.525(6) . 3_555 ? S(2) C(7) 3.56(2) . 3_555 ? S(2) O(9) 3.57(1) . 1_455 ? S(3) S(7) 3.391(6) . . ? S(3) C(2) 3.43(2) . . ? S(3) C(13) 3.53(2) . . ? S(4) S(8) 3.429(6) . . ? S(6) S(8) 3.563(6) . 3_556 ? S(7) O(13) 3.33(1) . 3_656 ? S(8) C(6) 3.53(2) . . ? S(8) C(8) 3.55(2) . 3_556 ? S(10) C(21) 3.43(1) . . ? S(10) S(13) 3.542(6) . 3_655 ? S(11) O(4) 3.16(2) . 1_655 ? S(11) C(29) 3.49(2) . . ? S(11) O(15) 3.51(1) . . ? S(11) S(15) 3.533(6) . . ? S(12) S(16) 3.208(6) . . ? S(13) S(15) 3.378(7) . . ? S(14) O(5) 3.32(2) . . ? S(14) S(16) 3.548(6) . 3_656 ? S(14) C(17) 3.59(2) . 3_655 ? S(15) O(5) 3.54(2) . 3_656 ? S(16) C(24) 3.33(2) . 3_656 ? S(16) C(23) 3.59(2) . 3_656 ? O(1) O(12) 3.14(2) . . ? O(1) C(26) 3.34(3) . . ? O(2) O(3) 3.31(2) . . ? O(2) O(9) 3.45(2) . 1_455 ? O(2) C(9) 3.45(3) . . ? O(2) C(5) 3.54(2) . . ? O(2) C(11) 3.57(2) . 3_555 ? O(3) C(4) 3.30(3) . . ? O(3) C(15) 3.43(2) . . ? O(4) O(9) 3.47(2) . 1_455 ? O(4) C(14) 3.59(2) . . ? O(6) O(8) 3.22(2) . 3_556 ? O(6) C(16) 3.40(3) . 3_556 ? O(7) O(13) 3.01(2) . 3_656 ? O(7) C(27) 3.11(4) . 3_656 ? O(8) C(12) 3.32(3) . 3_556 ? O(8) C(10) 3.46(2) . . ? O(9) C(9) 3.51(2) . 1_655 ? O(10) O(11) 3.38(2) . . ? O(10) C(25) 3.40(3) . . ? O(10) C(24) 3.53(2) . 3_655 ? O(10) O(14) 3.58(2) . 3_655 ? O(11) C(18) 3.38(2) . . ? O(11) C(31) 3.51(3) . . ? O(13) C(13) 3.50(3) . 3_656 ? O(14) O(16) 3.20(2) . 3_656 ? O(14) C(30) 3.37(3) . 3_656 ? O(14) C(32) 3.48(3) . 3_656 ? O(14) C(19) 3.57(2) . 3_655 ? O(15) C(12) 3.46(3) . 3_656 ? O(16) C(28) 3.49(4) . 3_656 ? C(5) C(13) 3.37(2) . . ? C(5) C(14) 3.54(3) . . ? C(6) C(14) 3.39(2) . . ? C(18) C(24) 3.56(2) . 3_655 ? C(22) C(30) 3.52(2) . . ? C(24) C(30) 3.52(3) . 3_656 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_[Ni(ddt)(edo)]2BF4 _database_code_CSD 162737 _audit_creation_date 'Thu Jul 15 06:49:53 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C16 H12 B F4 O4 Ni2 S12 ' _chemical_formula_moiety '?' _chemical_formula_weight 857.19 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,1/2+z 1/2+x,1/2+y,z 1/2+x,1/2-y,1/2+z _cell_length_a 31.620(5) _cell_length_b 6.898(1) _cell_length_c 13.270(2) _cell_angle_alpha 90 _cell_angle_beta 92.640(9) _cell_angle_gamma 90 _cell_volume 2891.3(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type Imagine Plate(DIP320) _diffrn_reflns_number 3269 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 30.38 _diffrn_measured_fraction_theta_max 0.6979 _diffrn_reflns_theta_full 30.38 _diffrn_measured_fraction_theta_full 0.6979 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3044 _reflns_number_gt 2198 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.1525 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2198 _refine_ls_number_parameters 358 _refine_ls_goodness_of_fit_ref 2.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.4659 _refine_diff_density_max 0.83 _refine_diff_density_min -0.92 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0056(6) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 0.2812 1.0143(2) 0.3467 0.0443(4) Uani 1.00 d . . . Ni(2) Ni 0.24413(7) 0.5549(3) 0.2385(2) 0.0458(5) Uani 1.00 d . . . S(1) S 0.3373(1) 1.0068(5) 0.2563(3) 0.051(1) Uani 1.00 d . . . S(2) S 0.3191(1) 0.9949(7) 0.4866(3) 0.065(1) Uani 1.00 d . . . S(3) S 0.2430(1) 1.0385(6) 0.2101(3) 0.051(1) Uani 1.00 d . . . S(4) S 0.2270(1) 1.0455(5) 0.4359(3) 0.050(1) Uani 1.00 d . . . S(5) S 0.1554(1) 1.1023(5) 0.1502(3) 0.052(1) Uani 1.00 d . . . S(6) S 0.1381(1) 1.1152(5) 0.4068(3) 0.051(1) Uani 1.00 d . . . S(7) S 0.2812(1) 0.5429(6) 0.1061(3) 0.058(1) Uani 1.00 d . . . S(8) S 0.3004(1) 0.5185(6) 0.3377(3) 0.050(1) Uani 1.00 d . . . S(9) S 0.1896(1) 0.5902(5) 0.1389(3) 0.0483(10) Uani 1.00 d . . . S(10) S 0.2071(1) 0.5636(5) 0.3693(3) 0.0453(10) Uani 1.00 d . . . S(11) S 0.1009(1) 0.6477(5) 0.1514(3) 0.056(1) Uani 1.00 d . . . S(12) S 0.1196(1) 0.6297(5) 0.4124(3) 0.053(1) Uani 1.00 d . . . F(1) F 0.5367(8) 0.390(4) 0.531(2) 0.33(1) Uani 1.00 d . . . F(2) F 0.4958(5) 0.593(3) 0.597(1) 0.173(7) Uani 1.00 d . . . F(3) F 0.4847(4) 0.476(2) 0.442(1) 0.123(5) Uani 1.00 d . . . F(4) F 0.5375(7) 0.634(5) 0.488(2) 0.32(1) Uani 1.00 d . . . O(1) O 0.4167(4) 0.988(2) 0.313(1) 0.079(4) Uani 1.00 d . . . O(2) O 0.4011(4) 0.985(2) 0.5210(10) 0.086(4) Uani 1.00 d . . . O(3) O 0.3625(3) 0.525(2) 0.0846(9) 0.078(4) Uani 1.00 d . . . O(4) O 0.3804(3) 0.498(2) 0.2975(10) 0.071(4) Uani 1.00 d . . . C(1) C 0.3778(5) 0.993(2) 0.345(2) 0.066(5) Uani 1.00 d . . . C(2) C 0.3700(5) 0.990(2) 0.448(1) 0.063(5) Uani 1.00 d . . . C(3) C 0.1944(5) 1.072(2) 0.247(1) 0.047(4) Uani 1.00 d . . . C(4) C 0.1867(4) 1.074(2) 0.3510(10) 0.041(4) Uani 1.00 d . . . C(5) C 0.4484(9) 0.967(5) 0.385(3) 0.16(1) Uani 1.00 d . . . C(6) C 0.4405(6) 0.987(4) 0.484(2) 0.13(1) Uani 1.00 d . . . C(7) C 0.1083(5) 1.139(2) 0.206(1) 0.059(5) Uani 1.00 d . . . C(8) C 0.1021(5) 1.139(2) 0.306(1) 0.059(5) Uani 1.00 d . . . C(9) C 0.3309(5) 0.525(2) 0.150(1) 0.048(4) Uani 1.00 d . . . C(10) C 0.3400(5) 0.514(2) 0.259(1) 0.047(4) Uani 1.00 d . . . C(11) C 0.1494(4) 0.613(2) 0.2178(9) 0.040(4) Uani 1.00 d . . . C(12) C 0.1571(4) 0.605(2) 0.319(1) 0.045(4) Uani 1.00 d . . . C(13A) C 0.405(2) 0.40(1) 0.139(6) 0.0924 Uani 0.27 d P . . C(13B) C 0.4042(8) 0.557(5) 0.130(2) 0.092(9) Uani 0.73 d P . . C(14A) C 0.411(2) 0.54(1) 0.217(8) 0.0837 Uani 0.27 d P . . C(14B) C 0.4108(9) 0.449(5) 0.221(3) 0.084(9) Uani 0.73 d P . . C(15) C 0.0642(5) 0.673(2) 0.247(1) 0.070(5) Uani 1.00 d . . . C(16) C 0.0724(5) 0.662(2) 0.344(1) 0.065(5) Uani 1.00 d . . . B(1) B 0.5120(6) 0.521(4) 0.515(2) 0.080(7) Uani 1.00 d . . . H(1) H 0.4601 0.8426 0.3770 0.2041 Uiso 1.00 calc . . . H(2) H 0.4692 1.0633 0.3717 0.2041 Uiso 1.00 calc . . . H(3) H 0.4529 1.1054 0.5053 0.1493 Uiso 1.00 calc . . . H(4) H 0.4552 0.8819 0.5173 0.1493 Uiso 1.00 calc . . . H(5) H 0.0840 1.1625 0.1631 0.0718 Uiso 1.00 calc . . . H(6) H 0.0735 1.1539 0.3243 0.0693 Uiso 1.00 calc . . . H(7A) H 0.3987 0.2900 0.1558 0.1044 Uiso 0.27 calc P . . H(7B) H 0.4252 0.5307 0.0824 0.1044 Uiso 0.73 calc P . . H(8A) H 0.4277 0.4239 0.0953 0.1044 Uiso 0.27 calc P . . H(8B) H 0.4070 0.6962 0.1467 0.1044 Uiso 0.73 calc P . . H(9A) H 0.4099 0.6628 0.1994 0.0996 Uiso 0.27 calc P . . H(9B) H 0.4386 0.4584 0.2489 0.0996 Uiso 0.73 calc P . . H(10A) H 0.4389 0.5030 0.2474 0.0996 Uiso 0.27 calc P . . H(10B) H 0.4063 0.3091 0.2041 0.0996 Uiso 0.73 calc P . . H(11) H 0.0355 0.6962 0.2253 0.0849 Uiso 1.00 calc . . . H(12) H 0.0483 0.6743 0.3831 0.0790 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0493(8) 0.0474(9) 0.0358(8) 0.0014(8) -0.0023(7) -0.0012(8) Ni(2) 0.0479(9) 0.054(1) 0.0360(8) -0.0024(8) 0.0073(7) 0.0009(9) S(1) 0.056(2) 0.053(2) 0.044(2) 0.000(2) -0.001(2) 0.000(2) S(2) 0.065(3) 0.091(3) 0.037(2) 0.009(2) -0.008(2) -0.003(2) S(3) 0.053(2) 0.065(2) 0.034(2) -0.003(2) 0.001(2) 0.001(2) S(4) 0.054(2) 0.062(2) 0.033(2) 0.005(2) -0.001(2) -0.003(2) S(5) 0.074(2) 0.044(2) 0.038(2) -0.004(2) -0.008(2) -0.001(2) S(6) 0.063(2) 0.048(2) 0.043(2) -0.002(2) 0.003(2) -0.001(2) S(7) 0.052(2) 0.081(3) 0.041(2) 0.000(2) 0.009(2) -0.002(2) S(8) 0.048(2) 0.059(2) 0.044(2) -0.003(2) 0.006(2) 0.006(2) S(9) 0.059(2) 0.051(2) 0.035(2) -0.004(2) 0.011(1) -0.004(2) S(10) 0.058(2) 0.045(2) 0.033(2) -0.003(2) 0.003(1) 0.004(1) S(11) 0.057(2) 0.055(2) 0.057(2) 0.004(2) 0.000(2) 0.000(2) S(12) 0.069(2) 0.047(2) 0.043(2) 0.004(2) 0.016(2) -0.002(2) F(1) 0.38(2) 0.40(2) 0.20(2) 0.30(2) -0.18(2) -0.15(2) F(2) 0.12(1) 0.25(2) 0.15(1) -0.01(1) 0.023(9) -0.10(1) F(3) 0.107(9) 0.13(1) 0.12(1) -0.002(8) -0.051(8) -0.022(8) F(4) 0.21(2) 0.54(4) 0.22(2) -0.24(2) 0.05(2) -0.10(3) O(1) 0.057(7) 0.091(9) 0.089(9) -0.001(6) -0.003(6) -0.001(6) O(2) 0.067(7) 0.12(1) 0.066(8) 0.022(7) -0.012(6) -0.010(7) O(3) 0.047(6) 0.14(1) 0.050(7) 0.006(6) 0.015(5) -0.011(7) O(4) 0.048(6) 0.080(7) 0.085(8) 0.008(5) -0.003(6) 0.009(6) C(1) 0.055(9) 0.064(10) 0.08(1) 0.002(8) 0.000(8) -0.008(8) C(2) 0.055(9) 0.09(1) 0.041(9) 0.018(8) -0.012(7) -0.003(7) C(3) 0.067(9) 0.036(7) 0.038(8) -0.019(6) -0.006(6) -0.012(6) C(4) 0.055(8) 0.032(7) 0.037(8) -0.003(6) -0.004(6) -0.002(6) C(5) 0.08(2) 0.24(4) 0.15(3) 0.01(2) -0.01(2) 0.05(2) C(6) 0.05(1) 0.27(4) 0.08(2) 0.02(1) -0.014(10) 0.00(2) C(7) 0.062(9) 0.055(9) 0.060(10) -0.004(8) -0.004(7) 0.009(8) C(8) 0.08(1) 0.044(8) 0.053(10) 0.003(8) 0.006(8) 0.005(8) C(9) 0.060(9) 0.043(8) 0.044(8) -0.007(6) 0.022(6) 0.004(6) C(10) 0.057(8) 0.025(6) 0.061(9) 0.003(6) 0.007(7) -0.001(6) C(11) 0.064(8) 0.028(7) 0.028(7) -0.009(6) 0.003(6) -0.010(6) C(12) 0.049(8) 0.031(7) 0.055(9) 0.002(6) 0.013(6) 0.003(6) C(13A) 0.0562 0.1352 0.0882 0.0131 0.0295 0.0349 C(13B) 0.06(1) 0.14(2) 0.09(2) 0.01(2) 0.03(1) 0.03(2) C(14A) 0.0406 0.1223 0.0898 0.0058 0.0218 0.0009 C(14B) 0.041(9) 0.12(3) 0.09(2) 0.01(2) 0.022(10) 0.00(2) C(15) 0.057(9) 0.07(1) 0.08(1) 0.001(8) -0.009(8) -0.015(10) C(16) 0.053(8) 0.064(10) 0.08(1) 0.008(8) 0.010(8) -0.011(9) B(1) 0.038(9) 0.13(2) 0.07(1) 0.01(1) -0.012(10) -0.02(1) #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.189(4) . . yes Ni(1) S(2) 2.166(4) . . yes Ni(1) S(3) 2.137(4) . . yes Ni(1) S(4) 2.137(4) . . yes Ni(2) S(7) 2.159(4) . . yes Ni(2) S(8) 2.179(4) . . yes Ni(2) S(9) 2.138(4) . . yes Ni(2) S(10) 2.139(4) . . yes S(1) C(1) 1.70(2) . . yes S(2) C(2) 1.71(2) . . yes S(3) C(3) 1.65(2) . . yes S(4) C(4) 1.67(1) . . yes S(5) C(3) 1.75(1) . . yes S(5) C(7) 1.72(2) . . yes S(6) C(4) 1.76(1) . . yes S(6) C(8) 1.72(2) . . yes S(7) C(9) 1.66(2) . . yes S(8) C(10) 1.67(2) . . yes S(9) C(11) 1.69(1) . . yes S(10) C(12) 1.71(1) . . yes S(11) C(11) 1.75(1) . . yes S(11) C(15) 1.77(2) . . yes S(12) C(12) 1.76(1) . . yes S(12) C(16) 1.73(2) . . yes F(1) B(1) 1.21(3) . . yes F(2) B(1) 1.32(3) . . yes F(3) B(1) 1.31(2) . . yes F(4) B(1) 1.19(3) . . yes O(1) C(1) 1.32(2) . . yes O(1) C(5) 1.36(3) . . yes O(2) C(2) 1.35(2) . . yes O(2) C(6) 1.36(3) . . yes O(3) C(9) 1.36(2) . . yes O(3) C(13A) 1.73(7) . . yes O(3) C(13B) 1.44(3) . . yes O(4) C(10) 1.36(2) . . yes O(4) C(14A) 1.51(9) . . yes O(4) C(14B) 1.47(3) . . yes C(1) C(2) 1.40(3) . . yes C(3) C(4) 1.41(2) . . yes C(5) C(6) 1.36(4) . . yes C(7) C(8) 1.35(2) . . yes C(9) C(10) 1.45(2) . . yes C(11) C(12) 1.36(2) . . yes C(13A) C(13B) 1.09(8) . . yes C(13A) C(14A) 1.4(1) . . yes C(13A) C(14B) 1.15(9) . . yes C(13B) C(14A) 1.2(1) . . yes C(13B) C(14B) 1.43(5) . . yes C(14A) C(14B) 0.7(1) . . yes C(15) C(16) 1.30(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(2) 92.2(2) 1_555 1_555 1_555 yes S(1) Ni(1) S(3) 88.7(2) 1_555 1_555 1_555 yes S(1) Ni(1) S(4) 175.5(2) 1_555 1_555 1_555 yes S(2) Ni(1) S(3) 178.7(2) 1_555 1_555 1_555 yes S(2) Ni(1) S(4) 87.5(2) 1_555 1_555 1_555 yes S(3) Ni(1) S(4) 91.5(1) 1_555 1_555 1_555 yes S(7) Ni(2) S(8) 91.6(2) 1_555 1_555 1_555 yes S(7) Ni(2) S(9) 87.4(2) 1_555 1_555 1_555 yes S(7) Ni(2) S(10) 179.3(2) 1_555 1_555 1_555 yes S(8) Ni(2) S(9) 179.0(2) 1_555 1_555 1_555 yes S(8) Ni(2) S(10) 88.6(2) 1_555 1_555 1_555 yes S(9) Ni(2) S(10) 92.4(2) 1_555 1_555 1_555 yes Ni(1) S(1) C(1) 103.1(7) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 103.5(6) 1_555 1_555 1_555 yes Ni(1) S(3) C(3) 104.7(5) 1_555 1_555 1_555 yes Ni(1) S(4) C(4) 104.1(5) 1_555 1_555 1_555 yes C(3) S(5) C(7) 107.0(7) 1_555 1_555 1_555 yes C(4) S(6) C(8) 104.4(7) 1_555 1_555 1_555 yes Ni(2) S(7) C(9) 104.8(5) 1_555 1_555 1_555 yes Ni(2) S(8) C(10) 103.7(6) 1_555 1_555 1_555 yes Ni(2) S(9) C(11) 103.6(5) 1_555 1_555 1_555 yes Ni(2) S(10) C(12) 102.7(5) 1_555 1_555 1_555 yes C(11) S(11) C(15) 104.0(7) 1_555 1_555 1_555 yes C(12) S(12) C(16) 103.6(7) 1_555 1_555 1_555 yes C(1) O(1) C(5) 116(1) 1_555 1_555 1_555 yes C(2) O(2) C(6) 112(1) 1_555 1_555 1_555 yes C(9) O(3) C(13A) 108(2) 1_555 1_555 1_555 yes C(9) O(3) C(13B) 114(1) 1_555 1_555 1_555 yes C(13A) O(3) C(13B) 38(2) 1_555 1_555 1_555 yes C(10) O(4) C(14A) 109(3) 1_555 1_555 1_555 yes C(10) O(4) C(14B) 113(1) 1_555 1_555 1_555 yes C(14A) O(4) C(14B) 25(3) 1_555 1_555 1_555 yes S(1) C(1) O(1) 117(1) 1_555 1_555 1_555 yes S(1) C(1) C(2) 120(1) 1_555 1_555 1_555 yes O(1) C(1) C(2) 121(1) 1_555 1_555 1_555 yes S(2) C(2) O(2) 116(1) 1_555 1_555 1_555 yes S(2) C(2) C(1) 120(1) 1_555 1_555 1_555 yes O(2) C(2) C(1) 123(1) 1_555 1_555 1_555 yes S(3) C(3) S(5) 115.4(8) 1_555 1_555 1_555 yes S(3) C(3) C(4) 119(1) 1_555 1_555 1_555 yes S(5) C(3) C(4) 124(1) 1_555 1_555 1_555 yes S(4) C(4) S(6) 112.9(8) 1_555 1_555 1_555 yes S(4) C(4) C(3) 119(1) 1_555 1_555 1_555 yes S(6) C(4) C(3) 127(1) 1_555 1_555 1_555 yes O(1) C(5) C(6) 120(2) 1_555 1_555 1_555 yes O(1) C(5) H(1) 107(3) 1_555 1_555 1_555 no O(1) C(5) H(2) 106(2) 1_555 1_555 1_555 no C(6) C(5) H(1) 106(2) 1_555 1_555 1_555 no C(6) C(5) H(2) 105(3) 1_555 1_555 1_555 no H(1) C(5) H(2) 109(2) 1_555 1_555 1_555 no O(2) C(6) C(5) 123(2) 1_555 1_555 1_555 yes O(2) C(6) H(3) 106(2) 1_555 1_555 1_555 no O(2) C(6) H(4) 104(2) 1_555 1_555 1_555 no C(5) C(6) H(3) 106(2) 1_555 1_555 1_555 no C(5) C(6) H(4) 105(2) 1_555 1_555 1_555 no H(3) C(6) H(4) 109(2) 1_555 1_555 1_555 no S(5) C(7) C(8) 126(1) 1_555 1_555 1_555 yes S(5) C(7) H(5) 116(1) 1_555 1_555 1_555 no C(8) C(7) H(5) 116(1) 1_555 1_555 1_555 no S(6) C(8) C(7) 129(1) 1_555 1_555 1_555 yes S(6) C(8) H(6) 114(1) 1_555 1_555 1_555 no C(7) C(8) H(6) 115(1) 1_555 1_555 1_555 no S(7) C(9) O(3) 119(1) 1_555 1_555 1_555 yes S(7) C(9) C(10) 119(1) 1_555 1_555 1_555 yes O(3) C(9) C(10) 121(1) 1_555 1_555 1_555 yes S(8) C(10) O(4) 118(1) 1_555 1_555 1_555 yes S(8) C(10) C(9) 120(1) 1_555 1_555 1_555 yes O(4) C(10) C(9) 121(1) 1_555 1_555 1_555 yes S(9) C(11) S(11) 111.6(7) 1_555 1_555 1_555 yes S(9) C(11) C(12) 120(1) 1_555 1_555 1_555 yes S(11) C(11) C(12) 128(1) 1_555 1_555 1_555 yes S(10) C(12) S(12) 112.6(8) 1_555 1_555 1_555 yes S(10) C(12) C(11) 120(1) 1_555 1_555 1_555 yes S(12) C(12) C(11) 126(1) 1_555 1_555 1_555 yes O(3) C(13A) C(13B) 55(3) 1_555 1_555 1_555 yes O(3) C(13A) C(14A) 91(5) 1_555 1_555 1_555 yes O(3) C(13A) C(14B) 109(5) 1_555 1_555 1_555 yes O(3) C(13A) H(7A) 111(5) 1_555 1_555 1_555 no O(3) C(13A) H(8A) 104(5) 1_555 1_555 1_555 no O(3) C(13A) H(10B) 127(4) 1_555 1_555 1_555 no C(13B) C(13A) C(14A) 53(5) 1_555 1_555 1_555 yes C(13B) C(13A) C(14B) 79(6) 1_555 1_555 1_555 yes C(13B) C(13A) H(7A) 159(8) 1_555 1_555 1_555 no C(13B) C(13A) H(8A) 77(5) 1_555 1_555 1_555 no C(13B) C(13A) H(10B) 132(8) 1_555 1_555 1_555 no C(14A) C(13A) C(14B) 26(4) 1_555 1_555 1_555 yes C(14A) C(13A) H(7A) 117(8) 1_555 1_555 1_555 no C(14A) C(13A) H(8A) 104(7) 1_555 1_555 1_555 no C(14A) C(13A) H(10B) 79(6) 1_555 1_555 1_555 no C(14B) C(13A) H(7A) 92(6) 1_555 1_555 1_555 no C(14B) C(13A) H(8A) 116(7) 1_555 1_555 1_555 no C(14B) C(13A) H(10B) 53(4) 1_555 1_555 1_555 no H(7A) C(13A) H(8A) 122(9) 1_555 1_555 1_555 no H(7A) C(13A) H(10B) 39(3) 1_555 1_555 1_555 no H(8A) C(13A) H(10B) 127(7) 1_555 1_555 1_555 no O(3) C(13B) C(13A) 85(4) 1_555 1_555 1_555 yes O(3) C(13B) C(14A) 121(4) 1_555 1_555 1_555 yes O(3) C(13B) C(14B) 111(2) 1_555 1_555 1_555 yes O(3) C(13B) H(7B) 110(2) 1_555 1_555 1_555 no O(3) C(13B) H(8A) 105(2) 1_555 1_555 1_555 no O(3) C(13B) H(8B) 108(2) 1_555 1_555 1_555 no O(3) C(13B) H(9A) 121(2) 1_555 1_555 1_555 no C(13A) C(13B) C(14A) 78(6) 1_555 1_555 1_555 yes C(13A) C(13B) C(14B) 52(4) 1_555 1_555 1_555 yes C(13A) C(13B) H(7B) 81(4) 1_555 1_555 1_555 no C(13A) C(13B) H(8A) 46(3) 1_555 1_555 1_555 no C(13A) C(13B) H(8B) 159(5) 1_555 1_555 1_555 no C(13A) C(13B) H(9A) 121(5) 1_555 1_555 1_555 no C(14A) C(13B) C(14B) 26(4) 1_555 1_555 1_555 yes C(14A) C(13B) H(7B) 122(4) 1_555 1_555 1_555 no C(14A) C(13B) H(8A) 101(4) 1_555 1_555 1_555 no C(14A) C(13B) H(8B) 80(5) 1_555 1_555 1_555 no C(14A) C(13B) H(9A) 42(4) 1_555 1_555 1_555 no C(14B) C(13B) H(7B) 112(2) 1_555 1_555 1_555 no C(14B) C(13B) H(8A) 82(2) 1_555 1_555 1_555 no C(14B) C(13B) H(8B) 107(3) 1_555 1_555 1_555 no C(14B) C(13B) H(9A) 69(2) 1_555 1_555 1_555 no H(7B) C(13B) H(8A) 36(1) 1_555 1_555 1_555 no H(7B) C(13B) H(8B) 106(2) 1_555 1_555 1_555 no H(7B) C(13B) H(9A) 123(2) 1_555 1_555 1_555 no H(8A) C(13B) H(8B) 137(2) 1_555 1_555 1_555 no H(8A) C(13B) H(9A) 130(2) 1_555 1_555 1_555 no H(8B) C(13B) H(9A) 38(1) 1_555 1_555 1_555 no O(4) C(14A) C(13A) 107(6) 1_555 1_555 1_555 yes O(4) C(14A) C(13B) 128(6) 1_555 1_555 1_555 yes O(4) C(14A) C(14B) 73(9) 1_555 1_555 1_555 yes O(4) C(14A) H(9A) 111(7) 1_555 1_555 1_555 no O(4) C(14A) H(9B) 98(6) 1_555 1_555 1_555 no O(4) C(14A) H(10A) 104(7) 1_555 1_555 1_555 no C(13A) C(14A) C(13B) 47(4) 1_555 1_555 1_555 yes C(13A) C(14A) C(14B) 51(9) 1_555 1_555 1_555 yes C(13A) C(14A) H(9A) 117(9) 1_555 1_555 1_555 no C(13A) C(14A) H(9B) 89(6) 1_555 1_555 1_555 no C(13A) C(14A) H(10A) 100(7) 1_555 1_555 1_555 no C(13B) C(14A) C(14B) 99(12) 1_555 1_555 1_555 yes C(13B) C(14A) H(9A) 69(7) 1_555 1_555 1_555 no C(13B) C(14A) H(9B) 121(7) 1_555 1_555 1_555 no C(13B) C(14A) H(10A) 123(8) 1_555 1_555 1_555 no C(14B) C(14A) H(9A) 168(17) 1_555 1_555 1_555 no C(14B) C(14A) H(9B) 57(7) 1_555 1_555 1_555 no C(14B) C(14A) H(10A) 72(9) 1_555 1_555 1_555 no H(9A) C(14A) H(9B) 129(8) 1_555 1_555 1_555 no H(9A) C(14A) H(10A) 114(8) 1_555 1_555 1_555 no H(9B) C(14A) H(10A) 15(1) 1_555 1_555 1_555 no O(4) C(14B) C(13A) 130(3) 1_555 1_555 1_555 yes O(4) C(14B) C(13B) 113(2) 1_555 1_555 1_555 yes O(4) C(14B) C(14A) 80(9) 1_555 1_555 1_555 yes O(4) C(14B) H(9B) 110(3) 1_555 1_555 1_555 no O(4) C(14B) H(10A) 105(2) 1_555 1_555 1_555 no O(4) C(14B) H(10B) 106(2) 1_555 1_555 1_555 no C(13A) C(14B) C(13B) 48(4) 1_555 1_555 1_555 yes C(13A) C(14B) C(14A) 102(12) 1_555 1_555 1_555 yes C(13A) C(14B) H(9B) 119(4) 1_555 1_555 1_555 no C(13A) C(14B) H(10A) 121(4) 1_555 1_555 1_555 no C(13A) C(14B) H(10B) 59(4) 1_555 1_555 1_555 no C(13B) C(14B) C(14A) 54(10) 1_555 1_555 1_555 yes C(13B) C(14B) H(9B) 113(2) 1_555 1_555 1_555 no C(13B) C(14B) H(10A) 101(2) 1_555 1_555 1_555 no C(13B) C(14B) H(10B) 107(3) 1_555 1_555 1_555 no C(14A) C(14B) H(9B) 87(9) 1_555 1_555 1_555 no C(14A) C(14B) H(10A) 69(8) 1_555 1_555 1_555 no C(14A) C(14B) H(10B) 160(12) 1_555 1_555 1_555 no H(9B) C(14B) H(10A) 17.8(6) 1_555 1_555 1_555 no H(9B) C(14B) H(10B) 105(2) 1_555 1_555 1_555 no H(10A) C(14B) H(10B) 123(2) 1_555 1_555 1_555 no S(11) C(15) C(16) 126(1) 1_555 1_555 1_555 yes S(11) C(15) H(11) 116(1) 1_555 1_555 1_555 no C(16) C(15) H(11) 116(1) 1_555 1_555 1_555 no S(12) C(16) C(15) 131(1) 1_555 1_555 1_555 yes S(12) C(16) H(12) 114(1) 1_555 1_555 1_555 no C(15) C(16) H(12) 114(1) 1_555 1_555 1_555 no F(1) B(1) F(2) 114(2) 1_555 1_555 1_555 yes F(1) B(1) F(3) 110(2) 1_555 1_555 1_555 yes F(1) B(1) F(4) 95(2) 1_555 1_555 1_555 yes F(2) B(1) F(3) 115(1) 1_555 1_555 1_555 yes F(2) B(1) F(4) 107(2) 1_555 1_555 1_555 yes F(3) B(1) F(4) 111(2) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Ni(1) S(1) C(1) O(1) -179(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(1) C(1) C(2) 0(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) O(2) 177(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) C(1) -1(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(3) S(5) 178.8(6) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(3) C(4) -1(1) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(4) S(6) -177.1(5) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(4) C(3) 0(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(7) C(9) O(3) -176.7(10) 1_555 1_555 1_555 1_555 yes Ni(2) S(7) C(9) C(10) 2(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(8) C(10) O(4) 178.4(9) 1_555 1_555 1_555 1_555 yes Ni(2) S(8) C(10) C(9) -2(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(9) C(11) S(11) 179.1(5) 1_555 1_555 1_555 1_555 yes Ni(2) S(9) C(11) C(12) 0(1) 1_555 1_555 1_555 1_555 yes Ni(2) S(10) C(12) S(12) -177.3(5) 1_555 1_555 1_555 1_555 yes Ni(2) S(10) C(12) C(11) 3(1) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(2) C(2) 1.3(6) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(3) C(3) -174.3(5) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(4) C(4) 91(2) 1_555 1_555 1_555 1_555 yes S(1) C(1) O(1) C(5) -176(1) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) S(2) 1(2) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) O(2) -178(1) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(1) C(1) -0.6(6) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(3) C(3) -40(8) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(4) C(4) 178.2(5) 1_555 1_555 1_555 1_555 yes S(2) C(2) O(2) C(6) -178(1) 1_555 1_555 1_555 1_555 yes S(2) C(2) C(1) O(1) -179(1) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(1) C(1) 178.5(6) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(2) C(2) -132(8) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(4) C(4) -1.0(5) 1_555 1_555 1_555 1_555 yes S(3) C(3) S(5) C(7) -178.8(8) 1_555 1_555 1_555 1_555 yes S(3) C(3) C(4) S(4) 0(1) 1_555 1_555 1_555 1_555 yes S(3) C(3) C(4) S(6) 177.8(8) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(1) C(1) 85(2) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(2) C(2) -174.3(6) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(3) C(3) 1.2(5) 1_555 1_555 1_555 1_555 yes S(4) C(4) S(6) C(8) -179.8(7) 1_555 1_555 1_555 1_555 yes S(4) C(4) C(3) S(5) -179.5(7) 1_555 1_555 1_555 1_555 yes S(5) C(3) C(4) S(6) -2(1) 1_555 1_555 1_555 1_555 yes S(5) C(7) C(8) S(6) 3(2) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(8) C(10) 3.0(5) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(9) C(11) -178.6(5) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(10) C(12) -73(15) 1_555 1_555 1_555 1_555 yes S(7) C(9) O(3) C(13A) -153(3) 1_555 1_555 1_555 1_555 yes S(7) C(9) O(3) C(13B) 165(1) 1_555 1_555 1_555 1_555 yes S(7) C(9) C(10) S(8) 0(1) 1_555 1_555 1_555 1_555 yes S(7) C(9) C(10) O(4) 179.2(10) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(7) C(9) -3.0(5) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(9) C(11) 178(9) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(10) C(12) 177.2(5) 1_555 1_555 1_555 1_555 yes S(8) C(10) O(4) C(14A) -166(3) 1_555 1_555 1_555 1_555 yes S(8) C(10) O(4) C(14B) 166(1) 1_555 1_555 1_555 1_555 yes S(8) C(10) C(9) O(3) 179(1) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(7) C(9) 177.1(5) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(8) C(10) 5(9) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(10) C(12) -2.8(5) 1_555 1_555 1_555 1_555 yes S(9) C(11) S(11) C(15) -178.8(8) 1_555 1_555 1_555 1_555 yes S(9) C(11) C(12) S(10) -2(1) 1_555 1_555 1_555 1_555 yes S(9) C(11) C(12) S(12) 178.8(7) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(7) C(9) -112(15) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(8) C(10) -177.6(5) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(9) C(11) 2.0(5) 1_555 1_555 1_555 1_555 yes S(10) C(12) S(12) C(16) -178.1(8) 1_555 1_555 1_555 1_555 yes S(10) C(12) C(11) S(11) 178.4(7) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) S(12) 0(1) 1_555 1_555 1_555 1_555 yes S(11) C(15) C(16) S(12) 2(2) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) O(2) 0(2) 1_555 1_555 1_555 1_555 yes O(1) C(5) C(6) O(2) 15(4) 1_555 1_555 1_555 1_555 yes O(3) C(9) C(10) O(4) -1(1) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(13B) C(14A) 123(4) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(13B) C(14B) 121(3) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(14A) O(4) 81(5) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(14A) C(13B) -43(3) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(14A) C(14B) 132(9) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(14B) O(4) 37(8) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(14B) C(13B) -48(3) 1_555 1_555 1_555 1_555 yes O(3) C(13A) C(14B) C(14A) -50(10) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(13A) C(14A) -123(4) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(13A) C(14B) -121(3) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(14A) O(4) -2(11) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(14A) C(13A) 77(5) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(14A) C(14B) 74(10) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(14B) O(4) -59(3) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(14B) C(13A) 65(4) 1_555 1_555 1_555 1_555 yes O(3) C(13B) C(14B) C(14A) -117(10) 1_555 1_555 1_555 1_555 yes O(4) C(14A) C(13A) C(13B) 125(6) 1_555 1_555 1_555 1_555 yes O(4) C(14A) C(13A) C(14B) -50(7) 1_555 1_555 1_555 1_555 yes O(4) C(14A) C(13B) C(13A) -79(8) 1_555 1_555 1_555 1_555 yes O(4) C(14A) C(13B) C(14B) -76(11) 1_555 1_555 1_555 1_555 yes O(4) C(14A) C(14B) C(13A) 129(4) 1_555 1_555 1_555 1_555 yes O(4) C(14A) C(14B) C(13B) 127(5) 1_555 1_555 1_555 1_555 yes O(4) C(14B) C(13A) C(13B) 85(5) 1_555 1_555 1_555 1_555 yes O(4) C(14B) C(13A) C(14A) 88(10) 1_555 1_555 1_555 1_555 yes O(4) C(14B) C(13B) C(13A) -124(5) 1_555 1_555 1_555 1_555 yes O(4) C(14B) C(13B) C(14A) 58(9) 1_555 1_555 1_555 1_555 yes O(4) C(14B) C(14A) C(13A) -129(4) 1_555 1_555 1_555 1_555 yes O(4) C(14B) C(14A) C(13B) -127(5) 1_555 1_555 1_555 1_555 yes C(1) O(1) C(5) C(6) -12(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) O(2) C(6) 1(2) 1_555 1_555 1_555 1_555 yes C(2) O(2) C(6) C(5) -9(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) O(1) C(5) 4(2) 1_555 1_555 1_555 1_555 yes C(3) S(5) C(7) C(8) -1(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) S(6) C(8) 2(1) 1_555 1_555 1_555 1_555 yes C(4) S(6) C(8) C(7) -3(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) S(5) C(7) 1(1) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13A) C(13B) -106(3) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13A) C(14A) -64(4) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13A) C(14B) -44(6) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13B) C(13A) 89(4) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13B) C(14A) 15(6) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13B) C(14B) 43(3) 1_555 1_555 1_555 1_555 yes C(9) C(10) O(4) C(14A) 14(4) 1_555 1_555 1_555 1_555 yes C(9) C(10) O(4) C(14B) -12(2) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14A) C(13A) -63(6) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14A) C(13B) -13(10) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14A) C(14B) -102(9) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14B) C(13A) -10(7) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14B) C(13B) 43(2) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14B) C(14A) 87(9) 1_555 1_555 1_555 1_555 yes C(10) C(9) O(3) C(13A) 27(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) O(3) C(13B) -13(2) 1_555 1_555 1_555 1_555 yes C(11) S(11) C(15) C(16) -1(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) S(12) C(16) 1(1) 1_555 1_555 1_555 1_555 yes C(12) S(12) C(16) C(15) -2(1) 1_555 1_555 1_555 1_555 yes C(12) C(11) S(11) C(15) 0(1) 1_555 1_555 1_555 1_555 yes C(13A) O(3) C(13B) C(14A) -73(6) 1_555 1_555 1_555 1_555 yes C(13A) O(3) C(13B) C(14B) -46(4) 1_555 1_555 1_555 1_555 yes C(13A) C(13B) C(14A) C(14B) -2(9) 1_555 1_555 1_555 1_555 yes C(13A) C(13B) C(14B) C(14A) 176(11) 1_555 1_555 1_555 1_555 yes C(13A) C(14A) O(4) C(14B) 39(7) 1_555 1_555 1_555 1_555 yes C(13A) C(14A) C(13B) C(14B) 2(9) 1_555 1_555 1_555 1_555 yes C(13A) C(14A) C(14B) C(13B) -2(8) 1_555 1_555 1_555 1_555 yes C(13A) C(14B) O(4) C(14A) -98(12) 1_555 1_555 1_555 1_555 yes C(13A) C(14B) C(13B) C(14A) -176(11) 1_555 1_555 1_555 1_555 yes C(13A) C(14B) C(14A) C(13B) 2(8) 1_555 1_555 1_555 1_555 yes C(13B) O(3) C(13A) C(14A) 42(4) 1_555 1_555 1_555 1_555 yes C(13B) O(3) C(13A) C(14B) 62(5) 1_555 1_555 1_555 1_555 yes C(13B) C(13A) C(14A) C(14B) 176(11) 1_555 1_555 1_555 1_555 yes C(13B) C(13A) C(14B) C(14A) -2(9) 1_555 1_555 1_555 1_555 yes C(13B) C(14A) O(4) C(14B) 89(13) 1_555 1_555 1_555 1_555 yes C(13B) C(14A) C(13A) C(14B) -176(11) 1_555 1_555 1_555 1_555 yes C(13B) C(14B) O(4) C(14A) -44(9) 1_555 1_555 1_555 1_555 yes C(13B) C(14B) C(13A) C(14A) 2(9) 1_555 1_555 1_555 1_555 yes C(14A) C(13A) C(13B) C(14B) -1(5) 1_555 1_555 1_555 1_555 yes C(14A) C(13B) C(13A) C(14B) 1(5) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni(1) S(8) 3.477(4) . . ? Ni(1) S(8) 3.534(4) . 1_565 ? Ni(2) S(3) 3.357(4) . . ? Ni(2) S(3) 3.582(4) . 1_545 ? S(1) C(10) 3.40(1) . . ? S(1) C(10) 3.50(1) . 1_565 ? S(1) S(2) 3.599(6) . 2_574 ? S(4) S(10) 3.490(5) . . ? S(5) C(11) 3.50(1) . . ? S(5) S(9) 3.540(5) . 1_565 ? S(5) S(11) 3.579(5) . . ? S(5) S(6) 3.580(5) . 2_574 ? S(6) S(12) 3.401(5) . . ? S(6) F(4) 3.41(2) . 3_455 ? S(6) S(12) 3.598(5) . 1_565 ? S(10) C(4) 3.44(1) . 1_545 ? S(10) C(4) 3.59(1) . . ? S(11) F(4) 3.26(2) . 4_464 ? S(11) C(7) 3.47(2) . . ? S(11) C(7) 3.59(2) . 1_545 ? S(12) F(1) 3.60(2) . 3_455 ? F(1) C(7) 3.18(2) . 4_565 ? F(1) C(16) 3.19(2) . 3_545 ? F(2) C(13A) 2.93(6) . 2_565 ? F(2) C(13B) 3.12(3) . 2_565 ? F(2) C(14B) 3.23(3) . 2_565 ? F(2) C(15) 3.29(2) . 4_565 ? F(2) C(14A) 3.31(9) . 2_565 ? F(2) C(6) 3.53(3) . . ? F(4) C(8) 3.23(3) . 3_545 ? O(1) C(14A) 3.32(9) . . ? O(1) C(14B) 3.40(3) . 1_565 ? O(1) O(4) 3.58(2) . . ? O(2) C(13A) 3.08(9) . 2_565 ? O(2) C(13B) 3.47(3) . 2_575 ? O(4) C(1) 3.48(2) . . ? O(4) C(1) 3.54(2) . 1_545 ? C(3) C(11) 3.49(2) . . ? C(3) C(12) 3.58(2) . . ? C(4) C(12) 3.39(2) . . ? C(6) C(13A) 3.58(9) . 2_565 ? C(7) C(11) 3.52(2) . 1_565 ? C(7) C(15) 3.56(2) . . ? C(8) C(16) 3.47(2) . . ? C(8) C(15) 3.51(2) . . ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_[Ni(dddt)(edo)]3(FeCl4)2 _database_code_CSD 162738 _audit_creation_date 'Fri Feb 23 17:12:13 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H24 Cl8 Fe2 O6 Ni3 S18 ' _chemical_formula_moiety '?' _chemical_formula_weight 1556.95 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' _symmetry_Int_Tables_number 5 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,-z 1/2+x,1/2+y,z 1/2-x,1/2+y,-z _cell_length_a 34.214(3) _cell_length_b 7.7180(6) _cell_length_c 23.381(2) _cell_angle_alpha 90 _cell_angle_beta 120.889(4) _cell_angle_gamma 90 _cell_volume 5298.4(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.120 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.730 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type Imaging Plate _diffrn_reflns_number 7004 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.33 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7003 _reflns_number_gt 4642 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.3669 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4642 _refine_ls_number_parameters 550 _refine_ls_goodness_of_fit_ref 1.459 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1949P)^2^+21.5726P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -5.2070 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.09(4) _refine_diff_density_max 3.04 _refine_diff_density_min -1.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Fe' 'Fe' 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni -0.03975(3) 0.7168(1) 0.07330(4) 0.0455(3) Uani 1.00 d . . . Ni(2) Ni 0.00050(4) 0.8046(3) 0.24934(5) 0.0823(4) Uani 1.00 d . . . Ni(3) Ni 0.03977(3) 0.8871(2) 0.42657(4) 0.0475(3) Uani 1.00 d . . . Fe(1) Fe 0.23681(4) 0.7891(2) 0.13492(5) 0.0636(4) Uani 1.00 d . . . Fe(2) Fe 0.26295(4) 0.3065(2) 0.36463(5) 0.0644(4) Uani 1.00 d . . . Cl(1) Cl 0.17423(7) 0.9487(5) 0.1021(1) 0.0840(9) Uani 1.00 d . . . Cl(2) Cl 0.27602(8) 0.9227(5) 0.0972(1) 0.0916(10) Uani 1.00 d . . . Cl(3) Cl 0.21992(9) 0.5320(6) 0.0918(1) 0.102(1) Uani 1.00 d . . . Cl(4) Cl 0.27407(9) 0.7853(6) 0.2436(1) 0.106(1) Uani 1.00 d . . . Cl(5) Cl 0.27959(9) 0.5728(6) 0.4075(1) 0.095(1) Uani 1.00 d . . . Cl(6) Cl 0.22375(9) 0.3204(6) 0.2559(1) 0.099(1) Uani 1.00 d . . . Cl(7) Cl 0.32608(7) 0.1739(5) 0.3981(1) 0.0774(8) Uani 1.00 d . . . Cl(8) Cl 0.22341(8) 0.1792(6) 0.3999(1) 0.0918(10) Uani 1.00 d . . . S(1) S -0.10042(6) 0.6695(3) 0.07944(8) 0.0531(6) Uani 1.00 d . . . S(2) S -0.05333(7) 0.9947(4) 0.0606(1) 0.0603(7) Uani 1.00 d . . . S(3) S -0.02124(6) 0.4488(3) 0.09316(9) 0.0504(6) Uani 1.00 d . . . S(4) S 0.02350(5) 0.7782(3) 0.08004(8) 0.0440(5) Uani 1.00 d . . . S(5) S 0.04599(7) 0.2246(4) 0.0928(1) 0.0694(8) Uani 1.00 d . . . S(6) S 0.09057(6) 0.6027(3) 0.06720(8) 0.0545(6) Uani 1.00 d . . . S(7) S 0.04833(9) 0.6151(5) 0.2594(1) 0.0850(10) Uani 1.00 d . . . S(8) S 0.04293(9) 1.0140(5) 0.2456(1) 0.086(1) Uani 1.00 d . . . S(9) S -0.0399(1) 0.6126(5) 0.2532(1) 0.089(1) Uani 1.00 d . . . S(10) S -0.04648(9) 1.0041(5) 0.2399(1) 0.0825(10) Uani 1.00 d . . . S(11) S -0.1225(1) 0.5862(7) 0.2460(2) 0.125(2) Uani 1.00 d . . . S(12) S -0.1299(1) 1.0141(8) 0.2381(2) 0.122(2) Uani 1.00 d . . . S(13) S 0.05344(6) 0.6148(4) 0.44049(9) 0.0577(6) Uani 1.00 d . . . S(14) S 0.10027(6) 0.9341(3) 0.42114(8) 0.0493(6) Uani 1.00 d . . . S(15) S -0.02368(6) 0.8282(3) 0.42031(9) 0.0472(5) Uani 1.00 d . . . S(16) S 0.02144(5) 1.1578(3) 0.40787(8) 0.0414(5) Uani 1.00 d . . . S(17) S -0.09153(6) 1.0120(3) 0.43316(9) 0.0534(6) Uani 1.00 d . . . S(18) S -0.04551(7) 1.3801(4) 0.4116(1) 0.0604(7) Uani 1.00 d . . . O(1) O -0.1627(2) 0.886(1) 0.0665(3) 0.073(2) Uani 1.00 d . . . O(2) O -0.1176(2) 1.179(1) 0.0576(3) 0.075(2) Uani 1.00 d . . . O(3) O 0.1272(1) 0.5767(6) 0.2587(2) 0.030(1) Uani 1.00 d . . . O(4) O 0.1270(1) 1.0267(7) 0.2569(2) 0.038(1) Uani 1.00 d . . . O(5) O 0.1184(2) 0.428(1) 0.4478(2) 0.062(2) Uani 1.00 d . . . O(6) O 0.1622(2) 0.725(1) 0.4289(3) 0.074(2) Uani 1.00 d . . . C(1) C 0.0233(2) 0.437(1) 0.0811(3) 0.043(2) Uani 1.00 d . . . C(2) C 0.0452(2) 0.5809(8) 0.0779(2) 0.024(1) Uani 1.00 d . . . C(3) C -0.1219(2) 0.872(1) 0.0698(4) 0.049(2) Uani 1.00 d . . . C(4) C -0.1003(2) 1.015(1) 0.0605(3) 0.044(2) Uani 1.00 d . . . C(5) C 0.1049(3) 0.268(2) 0.1216(4) 0.076(3) Uani 1.00 d . . . C(6) C 0.1123(2) 0.385(1) 0.0725(4) 0.059(2) Uani 1.00 d . . . C(7) C -0.1804(3) 1.048(2) 0.0622(4) 0.068(3) Uani 1.00 d . . . C(8) C -0.1588(4) 1.202(3) 0.0532(6) 0.131(6) Uani 1.00 d . . . C(9) C 0.0932(2) 0.719(1) 0.2559(3) 0.052(2) Uani 1.00 d . . . C(10) C 0.0945(3) 0.898(2) 0.2530(4) 0.081(4) Uani 1.00 d . . . C(11) C -0.0830(3) 0.703(2) 0.2499(4) 0.061(3) Uani 1.00 d . . . C(12) C -0.0833(4) 0.899(2) 0.2424(5) 0.100(5) Uani 1.00 d . . . C(13) C 0.1569(4) 0.721(2) 0.2446(5) 0.112(5) Uani 1.00 d . . . C(14) C 0.1647(4) 0.895(2) 0.2698(5) 0.104(5) Uani 1.00 d . . . C(15) C -0.1646(4) 0.705(3) 0.2548(6) 0.126(6) Uani 1.00 d . . . C(16) C -0.1697(4) 0.854(2) 0.2331(6) 0.103(4) Uani 1.00 d . . . C(17) C 0.1011(3) 0.588(2) 0.4355(4) 0.071(3) Uani 1.00 d . . . C(18) C 0.1243(2) 0.749(2) 0.4313(4) 0.053(3) Uani 1.00 d . . . C(19) C -0.0470(3) 1.022(1) 0.4195(4) 0.058(3) Uani 1.00 d . . . C(20) C -0.0277(2) 1.177(1) 0.4100(3) 0.034(2) Uani 1.00 d . . . C(21) C 0.1530(5) 0.411(4) 0.4282(8) 0.149(8) Uani 1.00 d . . . C(22) C 0.1811(4) 0.533(2) 0.4514(7) 0.135(6) Uani 1.00 d . . . C(23) C -0.1135(3) 1.245(2) 0.4228(5) 0.088(4) Uani 1.00 d . . . C(24) C -0.1057(3) 1.336(2) 0.3801(4) 0.073(3) Uani 1.00 d . . . H(1) H 0.1180 0.3255 0.1634 0.0909 Uiso 1.00 calc . . . H(2) H 0.1200 0.1607 0.1270 0.0909 Uiso 1.00 calc . . . H(3) H 0.0968 0.3338 0.0294 0.0707 Uiso 1.00 calc . . . H(4) H 0.1439 0.3909 0.0882 0.0707 Uiso 1.00 calc . . . H(5) H -0.2108 1.0448 0.0255 0.0812 Uiso 1.00 calc . . . H(6) H -0.1807 1.0649 0.1022 0.0812 Uiso 1.00 calc . . . H(7) H -0.1545 1.2838 0.0864 0.1571 Uiso 1.00 calc . . . H(8) H -0.1793 1.2481 0.0103 0.1571 Uiso 1.00 calc . . . H(9) H 0.1863 0.6715 0.2615 0.1346 Uiso 1.00 calc . . . H(10) H 0.1422 0.7312 0.1975 0.1346 Uiso 1.00 calc . . . H(11) H 0.1820 0.9487 0.2535 0.1251 Uiso 1.00 calc . . . H(12) H 0.1828 0.8840 0.3169 0.1251 Uiso 1.00 calc . . . H(13) H -0.1928 0.6459 0.2311 0.1517 Uiso 1.00 calc . . . H(14) H -0.1551 0.7101 0.3007 0.1517 Uiso 1.00 calc . . . H(15) H -0.1850 0.9111 0.2520 0.1235 Uiso 1.00 calc . . . H(16) H -0.1899 0.8406 0.1865 0.1235 Uiso 1.00 calc . . . H(17) H 0.1686 0.3041 0.4446 0.1788 Uiso 1.00 calc . . . H(18) H 0.1382 0.4121 0.3809 0.1788 Uiso 1.00 calc . . . H(19) H 0.2031 0.5127 0.4389 0.1619 Uiso 1.00 calc . . . H(20) H 0.1954 0.5279 0.4986 0.1619 Uiso 1.00 calc . . . H(21) H -0.1453 1.2420 0.4060 0.1050 Uiso 1.00 calc . . . H(22) H -0.0984 1.3003 0.4650 0.1050 Uiso 1.00 calc . . . H(23) H -0.1213 1.4437 0.3713 0.0872 Uiso 1.00 calc . . . H(24) H -0.1176 1.2722 0.3398 0.0872 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0449(4) 0.0437(5) 0.0533(4) 0.0028(4) 0.0291(3) 0.0012(4) Ni(2) 0.0856(7) 0.0824(8) 0.0714(6) 0.0113(6) 0.0349(5) -0.0055(5) Ni(3) 0.0463(4) 0.0461(6) 0.0555(4) 0.0045(4) 0.0300(3) 0.0004(4) Fe(1) 0.0575(5) 0.0691(9) 0.0690(6) 0.0027(6) 0.0359(4) -0.0035(6) Fe(2) 0.0575(5) 0.0707(10) 0.0694(6) 0.0022(7) 0.0357(4) -0.0022(7) Cl(1) 0.076(1) 0.096(2) 0.088(1) 0.016(1) 0.0481(8) -0.003(1) Cl(2) 0.087(1) 0.103(2) 0.103(1) -0.006(2) 0.0622(9) 0.001(2) Cl(3) 0.102(2) 0.094(2) 0.112(1) -0.011(2) 0.057(1) -0.019(2) Cl(4) 0.098(2) 0.109(3) 0.104(1) 0.003(2) 0.047(1) 0.004(2) Cl(5) 0.096(1) 0.089(2) 0.110(1) -0.013(2) 0.059(1) -0.019(2) Cl(6) 0.094(1) 0.097(3) 0.095(1) -0.002(2) 0.041(1) 0.004(2) Cl(7) 0.0680(10) 0.093(2) 0.081(1) 0.012(1) 0.0448(7) 0.000(1) Cl(8) 0.090(1) 0.098(2) 0.106(1) 0.001(2) 0.0632(9) -0.009(2) S(1) 0.0543(7) 0.058(1) 0.0570(8) -0.0005(9) 0.0355(6) 0.0027(9) S(2) 0.0570(9) 0.051(1) 0.077(1) 0.0026(10) 0.0375(7) -0.0010(10) S(3) 0.0496(7) 0.051(1) 0.0572(8) -0.0003(9) 0.0324(6) 0.0033(8) S(4) 0.0438(7) 0.0398(9) 0.0498(8) -0.0015(7) 0.0250(5) -0.0033(7) S(5) 0.067(1) 0.054(1) 0.089(1) 0.009(1) 0.0410(9) 0.003(1) S(6) 0.0487(7) 0.059(1) 0.0623(8) -0.0063(9) 0.0332(6) -0.0029(9) S(7) 0.092(1) 0.080(2) 0.079(1) 0.009(2) 0.0421(10) -0.001(1) S(8) 0.093(1) 0.075(2) 0.081(1) 0.013(2) 0.037(1) -0.005(1) S(9) 0.090(1) 0.085(2) 0.083(1) 0.017(2) 0.039(1) -0.009(2) S(10) 0.085(1) 0.079(2) 0.080(1) 0.011(2) 0.039(1) -0.003(1) S(11) 0.127(2) 0.109(3) 0.131(2) -0.011(3) 0.060(2) 0.011(3) S(12) 0.121(2) 0.131(4) 0.113(2) 0.003(3) 0.061(2) 0.002(3) S(13) 0.0547(8) 0.051(1) 0.0753(10) 0.0056(10) 0.0390(7) 0.001(1) S(14) 0.0476(7) 0.052(1) 0.0545(8) 0.0030(9) 0.0305(6) 0.0015(9) S(15) 0.0482(7) 0.042(1) 0.0522(8) -0.0021(8) 0.0260(6) -0.0022(8) S(16) 0.0406(6) 0.0397(10) 0.0485(7) 0.0025(7) 0.0263(5) 0.0000(7) S(17) 0.0492(7) 0.058(1) 0.0599(8) -0.0038(10) 0.0331(6) -0.0043(9) S(18) 0.0580(9) 0.047(1) 0.081(1) 0.005(1) 0.0385(8) 0.002(1) O(1) 0.074(3) 0.082(5) 0.084(3) 0.018(4) 0.055(2) 0.010(4) O(2) 0.073(3) 0.072(5) 0.082(3) 0.004(4) 0.040(2) 0.010(3) O(3) 0.026(1) 0.042(2) 0.028(2) 0.008(2) 0.019(1) -0.002(2) O(4) 0.031(2) 0.028(2) 0.054(2) -0.004(2) 0.022(1) 0.007(2) O(5) 0.064(2) 0.061(4) 0.075(3) 0.021(3) 0.045(2) 0.016(3) O(6) 0.068(3) 0.074(5) 0.081(3) 0.016(4) 0.038(2) 0.009(4) C(1) 0.044(3) 0.034(3) 0.046(3) -0.001(3) 0.019(2) 0.006(3) C(2) 0.028(2) 0.028(3) 0.024(2) 0.000(2) 0.018(1) 0.000(2) C(3) 0.049(3) 0.054(5) 0.047(3) 0.008(3) 0.026(2) 0.003(3) C(4) 0.042(3) 0.045(4) 0.049(3) 0.007(3) 0.026(2) -0.003(3) C(5) 0.068(5) 0.070(7) 0.084(5) 0.010(6) 0.035(4) 0.012(5) C(6) 0.050(3) 0.058(5) 0.073(4) 0.013(4) 0.035(3) -0.008(4) C(7) 0.065(4) 0.067(6) 0.085(4) 0.006(5) 0.049(3) 0.006(5) C(8) 0.144(8) 0.13(2) 0.166(7) 0.02(1) 0.111(6) 0.02(1) C(9) 0.061(3) 0.049(4) 0.043(3) 0.002(4) 0.023(3) -0.002(3) C(10) 0.080(5) 0.076(7) 0.077(5) 0.016(6) 0.034(4) -0.002(5) C(11) 0.058(3) 0.072(6) 0.059(4) 0.012(4) 0.034(3) -0.005(4) C(12) 0.106(6) 0.11(1) 0.086(5) 0.020(8) 0.055(5) -0.027(7) C(13) 0.112(7) 0.08(1) 0.100(6) -0.014(9) 0.026(5) -0.010(8) C(14) 0.125(7) 0.11(1) 0.098(6) -0.013(9) 0.069(5) -0.014(8) C(15) 0.135(8) 0.12(2) 0.153(8) -0.01(1) 0.093(6) -0.01(1) C(16) 0.091(5) 0.10(1) 0.140(6) -0.012(7) 0.078(4) 0.021(7) C(17) 0.074(4) 0.083(8) 0.069(4) 0.016(6) 0.045(3) 0.005(5) C(18) 0.050(3) 0.075(6) 0.057(3) -0.001(4) 0.044(2) -0.001(4) C(19) 0.054(4) 0.057(6) 0.055(4) -0.007(4) 0.023(3) -0.010(4) C(20) 0.038(2) 0.040(3) 0.031(3) 0.003(3) 0.023(2) -0.004(2) C(21) 0.149(10) 0.14(2) 0.18(1) 0.03(1) 0.105(8) -0.02(1) C(22) 0.095(7) 0.11(1) 0.171(9) 0.049(8) 0.044(7) -0.043(9) C(23) 0.076(5) 0.088(9) 0.103(5) 0.007(7) 0.050(4) 0.007(7) C(24) 0.071(4) 0.076(7) 0.078(4) 0.018(5) 0.044(3) -0.010(5) #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.184(3) . . yes Ni(1) S(2) 2.182(3) . . yes Ni(1) S(3) 2.143(3) . . yes Ni(1) S(4) 2.141(2) . . yes Ni(2) S(7) 2.116(4) . . yes Ni(2) S(8) 2.204(4) . . yes Ni(2) S(9) 2.060(4) . . yes Ni(2) S(10) 2.154(4) . . yes Ni(3) S(13) 2.142(3) . . yes Ni(3) S(14) 2.168(3) . . yes Ni(3) S(15) 2.148(3) . . yes Ni(3) S(16) 2.160(2) . . yes Fe(1) Cl(1) 2.237(3) . . yes Fe(1) Cl(2) 2.203(4) . . yes Fe(1) Cl(3) 2.166(4) . . yes Fe(1) Cl(4) 2.181(3) . . yes Fe(2) Cl(5) 2.229(4) . . yes Fe(2) Cl(6) 2.184(3) . . yes Fe(2) Cl(7) 2.142(3) . . yes Fe(2) Cl(8) 2.149(4) . . yes S(1) C(3) 1.69(1) . . yes S(2) C(4) 1.613(8) . . yes S(3) C(1) 1.688(9) . . yes S(4) C(2) 1.705(7) . . yes S(5) C(1) 1.772(8) . . yes S(5) C(5) 1.800(10) . . yes S(6) C(2) 1.703(7) . . yes S(6) C(6) 1.82(1) . . yes S(7) C(9) 1.77(1) . . yes S(8) C(10) 1.91(1) . . yes S(9) C(11) 1.59(1) . . yes S(10) C(12) 1.52(2) . . yes S(11) C(11) 1.59(1) . . yes S(11) C(15) 1.81(2) . . yes S(12) C(12) 1.78(2) . . yes S(12) C(16) 1.80(2) . . yes S(13) C(17) 1.71(1) . . yes S(14) C(18) 1.60(1) . . yes S(15) C(19) 1.69(1) . . yes S(16) C(20) 1.712(7) . . yes S(17) C(19) 1.71(1) . . yes S(17) C(23) 1.91(2) . . yes S(18) C(20) 1.690(8) . . yes S(18) C(24) 1.829(9) . . yes O(1) C(3) 1.36(1) . . yes O(1) C(7) 1.36(1) . . yes O(2) C(4) 1.38(1) . . yes O(2) C(8) 1.37(2) . . yes O(3) C(9) 1.58(1) . . yes O(3) C(13) 1.65(2) . . yes O(4) C(10) 1.45(1) . . yes O(4) C(14) 1.55(2) . . yes O(5) C(17) 1.33(2) . . yes O(5) C(21) 1.48(2) . . yes O(6) C(18) 1.34(1) . . yes O(6) C(22) 1.60(2) . . yes C(1) C(2) 1.37(1) . . yes C(3) C(4) 1.41(1) . . yes C(5) C(6) 1.58(2) . . yes C(7) C(8) 1.47(3) . . yes C(9) C(10) 1.39(2) . . yes C(11) C(12) 1.52(2) . . yes C(13) C(14) 1.43(3) . . yes C(15) C(16) 1.23(3) . . yes C(17) C(18) 1.51(2) . . yes C(19) C(20) 1.44(1) . . yes C(21) C(22) 1.25(3) . . yes C(23) C(24) 1.35(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(2) 91.7(1) . 1_555 1_555 yes S(1) Ni(1) S(3) 90.5(1) . 1_555 1_555 yes S(1) Ni(1) S(4) 172.45(8) . 1_555 1_555 yes S(2) Ni(1) S(3) 175.28(7) . 1_555 1_555 yes S(2) Ni(1) S(4) 85.94(10) . 1_555 1_555 yes S(3) Ni(1) S(4) 91.28(9) . 1_555 1_555 yes S(7) Ni(2) S(8) 91.4(1) . 1_555 1_555 yes S(7) Ni(2) S(9) 89.8(2) . 1_555 1_555 yes S(7) Ni(2) S(10) 178.1(2) . 1_555 1_555 yes S(8) Ni(2) S(9) 178.8(2) . 1_555 1_555 yes S(8) Ni(2) S(10) 86.8(2) . 1_555 1_555 yes S(9) Ni(2) S(10) 92.1(2) . 1_555 1_555 yes S(13) Ni(3) S(14) 91.85(10) . 1_555 1_555 yes S(13) Ni(3) S(15) 86.38(9) . 1_555 1_555 yes S(13) Ni(3) S(16) 176.29(7) . 1_555 1_555 yes S(14) Ni(3) S(15) 173.24(9) . 1_555 1_555 yes S(14) Ni(3) S(16) 90.77(9) . 1_555 1_555 yes S(15) Ni(3) S(16) 90.72(9) . 1_555 1_555 yes Cl(1) Fe(1) Cl(2) 106.1(1) . 1_555 1_555 yes Cl(1) Fe(1) Cl(3) 111.4(1) . 1_555 1_555 yes Cl(1) Fe(1) Cl(4) 106.9(1) . 1_555 1_555 yes Cl(2) Fe(1) Cl(3) 108.3(2) . 1_555 1_555 yes Cl(2) Fe(1) Cl(4) 111.1(1) . 1_555 1_555 yes Cl(3) Fe(1) Cl(4) 112.7(2) . 1_555 1_555 yes Cl(5) Fe(2) Cl(6) 109.9(1) . 1_555 1_555 yes Cl(5) Fe(2) Cl(7) 107.4(1) . 1_555 1_555 yes Cl(5) Fe(2) Cl(8) 108.4(2) . 1_555 1_555 yes Cl(6) Fe(2) Cl(7) 110.5(1) . 1_555 1_555 yes Cl(6) Fe(2) Cl(8) 109.7(1) . 1_555 1_555 yes Cl(7) Fe(2) Cl(8) 110.9(1) . 1_555 1_555 yes Ni(1) S(1) C(3) 101.5(3) . 1_555 1_555 yes Ni(1) S(2) C(4) 103.7(3) . 1_555 1_555 yes Ni(1) S(3) C(1) 102.1(3) . 1_555 1_555 yes Ni(1) S(4) C(2) 103.8(2) . 1_555 1_555 yes C(1) S(5) C(5) 101.7(5) . 1_555 1_555 yes C(2) S(6) C(6) 105.6(4) . 1_555 1_555 yes Ni(2) S(7) C(9) 108.7(4) . 1_555 1_555 yes Ni(2) S(8) C(10) 104.6(5) . 1_555 1_555 yes Ni(2) S(9) C(11) 107.9(5) . 1_555 1_555 yes Ni(2) S(10) C(12) 101.8(6) . 1_555 1_555 yes C(11) S(11) C(15) 114.2(9) . 1_555 1_555 yes C(12) S(12) C(16) 106.8(8) . 1_555 1_555 yes Ni(3) S(13) C(17) 104.5(5) . 1_555 1_555 yes Ni(3) S(14) C(18) 106.0(4) . 1_555 1_555 yes Ni(3) S(15) C(19) 105.6(4) . 1_555 1_555 yes Ni(3) S(16) C(20) 105.4(3) . 1_555 1_555 yes C(19) S(17) C(23) 105.3(5) . 1_555 1_555 yes C(20) S(18) C(24) 99.4(5) . 1_555 1_555 yes C(3) O(1) C(7) 119.0(9) . 1_555 1_555 yes C(4) O(2) C(8) 121(1) . 1_555 1_555 yes C(9) O(3) C(13) 92.2(7) . 1_555 1_555 yes C(10) O(4) C(14) 95.6(9) . 1_555 1_555 yes C(17) O(5) C(21) 110(1) . 1_555 1_555 yes C(18) O(6) C(22) 110.4(10) . 1_555 1_555 yes S(3) C(1) S(5) 112.8(5) . 1_555 1_555 yes S(3) C(1) C(2) 122.1(6) . 1_555 1_555 yes S(5) C(1) C(2) 123.5(6) . 1_555 1_555 yes S(4) C(2) S(6) 111.0(4) . 1_555 1_555 yes S(4) C(2) C(1) 117.8(5) . 1_555 1_555 yes S(6) C(2) C(1) 131.0(6) . 1_555 1_555 yes S(1) C(3) O(1) 116.6(8) . 1_555 1_555 yes S(1) C(3) C(4) 121.2(7) . 1_555 1_555 yes O(1) C(3) C(4) 122.0(9) . 1_555 1_555 yes S(2) C(4) O(2) 119.3(6) . 1_555 1_555 yes S(2) C(4) C(3) 121.8(7) . 1_555 1_555 yes O(2) C(4) C(3) 118.7(8) . 1_555 1_555 yes S(5) C(5) C(6) 113.7(5) . 1_555 1_555 yes S(6) C(6) C(5) 111.5(7) . 1_555 1_555 yes O(1) C(7) C(8) 120(1) . 1_555 1_555 yes O(2) C(8) C(7) 117(1) . 1_555 1_555 yes S(7) C(9) O(3) 108.8(6) . 1_555 1_555 yes S(7) C(9) C(10) 120.4(8) . 1_555 1_555 yes O(3) C(9) C(10) 130.9(8) . 1_555 1_555 yes S(8) C(10) O(4) 109.2(8) . 1_555 1_555 yes S(8) C(10) C(9) 114.8(9) . 1_555 1_555 yes O(4) C(10) C(9) 136(1) . 1_555 1_555 yes S(9) C(11) S(11) 119.4(8) . 1_555 1_555 yes S(9) C(11) C(12) 113.1(8) . 1_555 1_555 yes S(11) C(11) C(12) 127.0(8) . 1_555 1_555 yes S(10) C(12) S(12) 117(1) . 1_555 1_555 yes S(10) C(12) C(11) 125(1) . 1_555 1_555 yes S(12) C(12) C(11) 117.0(10) . 1_555 1_555 yes O(3) C(13) C(14) 123(1) . 1_555 1_555 yes O(4) C(14) C(13) 125.2(9) . 1_555 1_555 yes S(11) C(15) C(16) 112(1) . 1_555 1_555 yes S(12) C(16) C(15) 132(1) . 1_555 1_555 yes S(13) C(17) O(5) 115.6(9) . 1_555 1_555 yes S(13) C(17) C(18) 117.2(9) . 1_555 1_555 yes O(5) C(17) C(18) 126.0(9) . 1_555 1_555 yes S(14) C(18) O(6) 123.4(9) . 1_555 1_555 yes S(14) C(18) C(17) 119.9(7) . 1_555 1_555 yes O(6) C(18) C(17) 116(1) . 1_555 1_555 yes S(15) C(19) S(17) 114.8(6) . 1_555 1_555 yes S(15) C(19) C(20) 119.0(7) . 1_555 1_555 yes S(17) C(19) C(20) 126.1(8) . 1_555 1_555 yes S(16) C(20) S(18) 116.9(4) . 1_555 1_555 yes S(16) C(20) C(19) 117.9(6) . 1_555 1_555 yes S(18) C(20) C(19) 124.6(6) . 1_555 1_555 yes O(5) C(21) C(22) 110(2) . 1_555 1_555 yes O(6) C(22) C(21) 117(1) . 1_555 1_555 yes S(17) C(23) C(24) 111(1) . 1_555 1_555 yes S(18) C(24) C(23) 113.9(6) . 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Ni(1) S(1) C(3) O(1) 175.5(5) 1_555 1_555 1_555 1_555 yes Ni(1) S(1) C(3) C(4) 0.4(6) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(4) O(2) 175.8(4) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(4) C(3) 2.2(6) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(1) S(5) -179.0(3) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(1) C(2) 14.9(5) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(2) S(6) 168.7(2) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(2) C(1) -7.9(5) 1_555 1_555 1_555 1_555 yes Ni(2) S(7) C(9) O(3) -176.4(3) 1_555 1_555 1_555 1_555 yes Ni(2) S(7) C(9) C(10) 5.2(7) 1_555 1_555 1_555 1_555 yes Ni(2) S(8) C(10) O(4) -175.1(5) 1_555 1_555 1_555 1_555 yes Ni(2) S(8) C(10) C(9) 2.6(7) 1_555 1_555 1_555 1_555 yes Ni(2) S(9) C(11) S(11) 175.1(4) 1_555 1_555 1_555 1_555 yes Ni(2) S(9) C(11) C(12) 2.1(7) 1_555 1_555 1_555 1_555 yes Ni(2) S(10) C(12) S(12) 178.6(5) 1_555 1_555 1_555 1_555 yes Ni(2) S(10) C(12) C(11) 0.0(9) 1_555 1_555 1_555 1_555 yes Ni(3) S(13) C(17) O(5) 175.1(5) 1_555 1_555 1_555 1_555 yes Ni(3) S(13) C(17) C(18) 6.9(6) 1_555 1_555 1_555 1_555 yes Ni(3) S(14) C(18) O(6) 177.7(5) 1_555 1_555 1_555 1_555 yes Ni(3) S(14) C(18) C(17) 5.7(7) 1_555 1_555 1_555 1_555 yes Ni(3) S(15) C(19) S(17) -166.3(3) 1_555 1_555 1_555 1_555 yes Ni(3) S(15) C(19) C(20) 11.8(6) 1_555 1_555 1_555 1_555 yes Ni(3) S(16) C(20) S(18) 168.7(3) 1_555 1_555 1_555 1_555 yes Ni(3) S(16) C(20) C(19) -2.9(5) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(2) C(4) -1.5(2) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(3) C(1) 172.5(2) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(4) C(2) 117.1(8) 1_555 1_555 1_555 1_555 yes S(1) C(3) O(1) C(7) 176.7(5) 1_555 1_555 1_555 1_555 yes S(1) C(3) C(4) S(2) -1.8(9) 1_555 1_555 1_555 1_555 yes S(1) C(3) C(4) O(2) -175.5(5) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(1) C(3) 0.7(3) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(3) C(1) -68(1) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(4) C(2) -170.6(2) 1_555 1_555 1_555 1_555 yes S(2) C(4) O(2) C(8) 175.9(7) 1_555 1_555 1_555 1_555 yes S(2) C(4) C(3) O(1) -176.7(5) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(1) C(3) 176.6(3) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(2) C(4) -120(1) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(4) C(2) 13.2(2) 1_555 1_555 1_555 1_555 yes S(3) C(1) S(5) C(5) -150.1(4) 1_555 1_555 1_555 1_555 yes S(3) C(1) C(2) S(4) -5.0(7) 1_555 1_555 1_555 1_555 yes S(3) C(1) C(2) S(6) 179.3(3) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(1) C(3) 72.6(8) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(2) C(4) -174.3(2) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(3) C(1) -14.9(2) 1_555 1_555 1_555 1_555 yes S(4) C(2) S(6) C(6) 175.7(3) 1_555 1_555 1_555 1_555 yes S(4) C(2) C(1) S(5) -169.6(4) 1_555 1_555 1_555 1_555 yes S(5) C(1) C(2) S(6) 14.7(8) 1_555 1_555 1_555 1_555 yes S(5) C(5) C(6) S(6) 66.5(8) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(8) C(10) 0.3(3) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(9) C(11) 177.7(3) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(10) C(12) -163(3) 1_555 1_555 1_555 1_555 yes S(7) C(9) O(3) C(13) 173.2(5) 1_555 1_555 1_555 1_555 yes S(7) C(9) C(10) S(8) -5.1(9) 1_555 1_555 1_555 1_555 yes S(7) C(9) C(10) O(4) 171.7(8) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(7) C(9) -2.5(3) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(9) C(11) 11(5) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(10) C(12) -178.6(4) 1_555 1_555 1_555 1_555 yes S(8) C(10) O(4) C(14) 174.3(6) 1_555 1_555 1_555 1_555 yes S(8) C(10) C(9) O(3) 176.9(5) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(7) C(9) 177.8(3) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(8) C(10) 166(4) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(10) C(12) 1.1(4) 1_555 1_555 1_555 1_555 yes S(9) C(11) S(11) C(15) 171.4(6) 1_555 1_555 1_555 1_555 yes S(9) C(11) C(12) S(10) -1(1) 1_555 1_555 1_555 1_555 yes S(9) C(11) C(12) S(12) 179.9(5) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(7) C(9) -17(3) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(8) C(10) 179.8(3) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(9) C(11) -1.8(3) 1_555 1_555 1_555 1_555 yes S(10) C(12) S(12) C(16) 173.8(7) 1_555 1_555 1_555 1_555 yes S(10) C(12) C(11) S(11) -173.8(6) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) S(12) 7(1) 1_555 1_555 1_555 1_555 yes S(11) C(15) C(16) S(12) -40(1) 1_555 1_555 1_555 1_555 yes S(13) Ni(3) S(14) C(18) -1.1(3) 1_555 1_555 1_555 1_555 yes S(13) Ni(3) S(15) C(19) 171.9(3) 1_555 1_555 1_555 1_555 yes S(13) Ni(3) S(16) C(20) 46(1) 1_555 1_555 1_555 1_555 yes S(13) C(17) O(5) C(21) 167.9(7) 1_555 1_555 1_555 1_555 yes S(13) C(17) C(18) S(14) -8.9(9) 1_555 1_555 1_555 1_555 yes S(13) C(17) C(18) O(6) 178.6(5) 1_555 1_555 1_555 1_555 yes S(14) Ni(3) S(13) C(17) -2.8(3) 1_555 1_555 1_555 1_555 yes S(14) Ni(3) S(15) C(19) -113.2(9) 1_555 1_555 1_555 1_555 yes S(14) Ni(3) S(16) C(20) -178.8(2) 1_555 1_555 1_555 1_555 yes S(14) C(18) O(6) C(22) 171.8(7) 1_555 1_555 1_555 1_555 yes S(14) C(18) C(17) O(5) -175.7(7) 1_555 1_555 1_555 1_555 yes S(15) Ni(3) S(13) C(17) 170.6(3) 1_555 1_555 1_555 1_555 yes S(15) Ni(3) S(14) C(18) -75.7(9) 1_555 1_555 1_555 1_555 yes S(15) Ni(3) S(16) C(20) 7.8(2) 1_555 1_555 1_555 1_555 yes S(15) C(19) S(17) C(23) -175.7(4) 1_555 1_555 1_555 1_555 yes S(15) C(19) C(20) S(16) -6.1(7) 1_555 1_555 1_555 1_555 yes S(15) C(19) C(20) S(18) -177.0(3) 1_555 1_555 1_555 1_555 yes S(16) Ni(3) S(13) C(17) 131(1) 1_555 1_555 1_555 1_555 yes S(16) Ni(3) S(14) C(18) -178.4(3) 1_555 1_555 1_555 1_555 yes S(16) Ni(3) S(15) C(19) -10.5(3) 1_555 1_555 1_555 1_555 yes S(16) C(20) S(18) C(24) 158.2(4) 1_555 1_555 1_555 1_555 yes S(16) C(20) C(19) S(17) 171.7(4) 1_555 1_555 1_555 1_555 yes S(17) C(19) C(20) S(18) 0.8(8) 1_555 1_555 1_555 1_555 yes S(17) C(23) C(24) S(18) -68.3(10) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) O(2) 9.7(10) 1_555 1_555 1_555 1_555 yes O(1) C(7) C(8) O(2) -7(1) 1_555 1_555 1_555 1_555 yes O(3) C(9) C(10) O(4) -6(1) 1_555 1_555 1_555 1_555 yes O(3) C(13) C(14) O(4) -56(1) 1_555 1_555 1_555 1_555 yes O(5) C(17) C(18) O(6) 11(1) 1_555 1_555 1_555 1_555 yes O(5) C(21) C(22) O(6) -61(1) 1_555 1_555 1_555 1_555 yes C(1) S(5) C(5) C(6) -56.0(9) 1_555 1_555 1_555 1_555 yes C(1) C(2) S(6) C(6) -8.4(6) 1_555 1_555 1_555 1_555 yes C(2) S(6) C(6) C(5) -31.9(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) S(5) C(5) 15.8(7) 1_555 1_555 1_555 1_555 yes C(3) O(1) C(7) C(8) 7(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) O(2) C(8) -10(1) 1_555 1_555 1_555 1_555 yes C(4) O(2) C(8) C(7) 9(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) O(1) C(7) -8(1) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13) C(14) 35.4(9) 1_555 1_555 1_555 1_555 yes C(9) C(10) O(4) C(14) -2(1) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14) C(13) 31(1) 1_555 1_555 1_555 1_555 yes C(10) C(9) O(3) C(13) -8.6(8) 1_555 1_555 1_555 1_555 yes C(11) S(11) C(15) C(16) 30(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) S(12) C(16) -7.4(9) 1_555 1_555 1_555 1_555 yes C(12) S(12) C(16) C(15) 29(1) 1_555 1_555 1_555 1_555 yes C(12) C(11) S(11) C(15) -16.7(10) 1_555 1_555 1_555 1_555 yes C(17) O(5) C(21) C(22) 49(1) 1_555 1_555 1_555 1_555 yes C(17) C(18) O(6) C(22) -16.0(9) 1_555 1_555 1_555 1_555 yes C(18) O(6) C(22) C(21) 45(1) 1_555 1_555 1_555 1_555 yes C(18) C(17) O(5) C(21) -25(1) 1_555 1_555 1_555 1_555 yes C(19) S(17) C(23) C(24) 28.5(7) 1_555 1_555 1_555 1_555 yes C(19) C(20) S(18) C(24) -30.8(6) 1_555 1_555 1_555 1_555 yes C(20) S(18) C(24) C(23) 68(1) 1_555 1_555 1_555 1_555 yes C(20) C(19) S(17) C(23) 6.3(7) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni(1) S(6) 2.954(2) . 2_555 ? Ni(3) S(17) 2.976(2) . 2_556 ? Cl(1) C(4) 3.353(6) . 2_555 ? Cl(1) C(3) 3.512(8) . 2_555 ? Cl(2) C(8) 3.36(2) . 3_545 ? Cl(2) C(7) 3.54(1) . 3_545 ? Cl(7) C(17) 3.440(8) . 4_546 ? Cl(7) C(18) 3.488(8) . 4_546 ? Cl(7) C(15) 3.53(2) . 3_545 ? Cl(8) C(21) 3.33(2) . . ? Cl(8) C(14) 3.44(1) . 1_545 ? Cl(8) O(4) 3.482(4) . 1_545 ? Cl(8) C(22) 3.52(1) . 4_546 ? Cl(8) C(22) 3.57(2) . . ? S(1) S(9) 3.513(3) . . ? S(2) S(5) 3.554(4) . 1_565 ? S(3) S(6) 3.459(2) . 2_555 ? S(3) C(6) 3.545(6) . 2_555 ? S(3) S(7) 3.595(3) . . ? S(4) S(4) 3.227(3) . 2_555 ? S(4) S(5) 3.509(4) . 1_565 ? S(4) C(2) 3.546(5) . 2_555 ? S(4) C(9) 3.568(6) . . ? S(7) C(17) 3.551(9) . . ? S(8) S(14) 3.579(3) . . ? S(10) S(16) 3.587(3) . . ? S(11) C(24) 3.47(1) . 1_545 ? S(12) C(7) 3.559(9) . . ? S(13) S(18) 3.585(4) . 1_545 ? S(15) S(15) 3.211(4) . 2_556 ? S(15) S(18) 3.522(3) . 1_545 ? S(15) C(11) 3.554(8) . . ? S(15) C(19) 3.578(8) . 2_556 ? S(16) S(17) 3.418(2) . 2_556 ? O(1) C(12) 3.58(1) . . ? O(2) C(6) 3.52(1) . 2_565 ? O(4) C(5) 3.41(1) . 1_565 ? O(5) C(23) 3.42(1) . 2_546 ? O(6) C(9) 3.483(8) . . ? C(1) C(1) 3.27(1) . 2_555 ? C(1) C(2) 3.408(8) . 2_555 ? C(2) C(2) 3.358(8) . 2_555 ? C(3) C(12) 3.55(1) . . ? C(19) C(19) 3.47(1) . 2_556 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_[Ni(edo)(dtm)]2ClO4 _database_code_CSD 162739 _audit_creation_date 'Thu Nov 25 01:50:28 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C16 H20 Cl O8 Ni2 S12 ' _chemical_formula_moiety 'C16 H20 Cl O8 Ni2 S12 ' _chemical_formula_weight 877.90 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pccn' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,z 1/2+x,-y,1/2-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2+y,-z 1/2-x,y,1/2+z x,1/2-y,1/2+z _cell_length_a 27.211(4) _cell_length_b 16.473(3) _cell_length_c 13.801(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6186(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.750 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.120 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.154 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type Imaging Plate(DIP320) _diffrn_reflns_number 6645 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.08 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 0 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6089 _reflns_number_gt 2458 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.2180 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2458 _refine_ls_number_parameters 352 _refine_ls_goodness_of_fit_ref 0.776 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1091P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -4.7020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_diff_density_max 0.92 _refine_diff_density_min -0.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 0.27816(2) -0.02855(4) 0.40811(4) 0.0494(2) Uani 1.00 d . . . Ni(2) Ni 0.27216(2) 0.02024(4) 0.17072(4) 0.0500(2) Uani 1.00 d . . . Cl(1) Cl 0.48727(6) 0.2751(1) 0.3770(1) 0.0907(6) Uani 1.00 d . . . S(1) S 0.31280(5) -0.14653(8) 0.41847(9) 0.0601(4) Uani 1.00 d . . . S(2) S 0.34798(5) 0.03464(8) 0.41346(8) 0.0545(4) Uani 1.00 d . . . S(3) S 0.20795(5) -0.08792(8) 0.42108(8) 0.0537(4) Uani 1.00 d . . . S(4) S 0.24375(5) 0.08740(8) 0.39855(8) 0.0516(4) Uani 1.00 d . . . S(5) S 0.10386(5) -0.02754(9) 0.42481(9) 0.0627(4) Uani 1.00 d . . . S(6) S 0.13908(5) 0.14415(9) 0.39674(9) 0.0585(4) Uani 1.00 d . . . S(7) S 0.33498(5) -0.05933(8) 0.17652(8) 0.0557(4) Uani 1.00 d . . . S(8) S 0.31791(5) 0.12713(9) 0.15910(9) 0.0609(4) Uani 1.00 d . . . S(9) S 0.22755(5) -0.08608(8) 0.17723(8) 0.0553(4) Uani 1.00 d . . . S(10) S 0.20888(5) 0.09666(8) 0.15505(8) 0.0541(4) Uani 1.00 d . . . S(11) S 0.11902(5) -0.11699(9) 0.17829(9) 0.0629(4) Uani 1.00 d . . . S(12) S 0.10077(5) 0.06564(9) 0.16663(9) 0.0632(4) Uani 1.00 d . . . O(1) O 0.4041(1) -0.1855(2) 0.4123(3) 0.080(1) Uani 1.00 d . . . O(2) O 0.4371(1) -0.0212(2) 0.4257(2) 0.065(1) Uani 1.00 d . . . O(3) O 0.4280(1) -0.0275(2) 0.1816(2) 0.073(1) Uani 1.00 d . . . O(4) O 0.4122(1) 0.1412(2) 0.1659(3) 0.086(1) Uani 1.00 d . . . O(5) O 0.5308(2) 0.2357(4) 0.3609(5) 0.195(3) Uani 1.00 d . . . O(6) O 0.4765(2) 0.3260(4) 0.3054(4) 0.183(3) Uani 1.00 d . . . O(7) O 0.4480(2) 0.2181(4) 0.3903(5) 0.189(3) Uani 1.00 d . . . O(8) O 0.4899(3) 0.3179(6) 0.4594(5) 0.258(5) Uani 1.00 d . . . C(1) C 0.3734(2) -0.1214(3) 0.4150(3) 0.056(2) Uani 1.00 d . . . C(2) C 0.3885(2) -0.0428(3) 0.4193(3) 0.058(2) Uani 1.00 d . . . C(3) C 0.1666(2) -0.0110(3) 0.4153(3) 0.052(1) Uani 1.00 d . . . C(4) C 0.1829(2) 0.0692(3) 0.4046(3) 0.042(1) Uani 1.00 d . . . C(5) C 0.4556(2) -0.1613(4) 0.3916(4) 0.097(2) Uani 1.00 d . . . C(6) C 0.4695(2) -0.0904(4) 0.4487(4) 0.084(2) Uani 1.00 d . . . C(7) C 0.0998(2) -0.1369(3) 0.4485(4) 0.072(2) Uani 1.00 d . . . C(8) C 0.1742(2) 0.2344(4) 0.3939(4) 0.076(2) Uani 1.00 d . . . C(9) C 0.3827(2) 0.0050(3) 0.1742(3) 0.058(2) Uani 1.00 d . . . C(10) C 0.3749(2) 0.0885(3) 0.1677(3) 0.056(2) Uani 1.00 d . . . C(11) C 0.1699(2) -0.0497(3) 0.1741(3) 0.047(1) Uani 1.00 d . . . C(12) C 0.1608(2) 0.0342(3) 0.1645(3) 0.048(1) Uani 1.00 d . . . C(13) C 0.4688(3) 0.0313(5) 0.1722(6) 0.133(3) Uani 1.00 d . . . C(14) C 0.4611(3) 0.1060(6) 0.1822(9) 0.186(5) Uani 1.00 d . . . C(15) C 0.1462(2) -0.2170(4) 0.1821(4) 0.076(2) Uani 1.00 d . . . C(16) C 0.1052(2) 0.1698(4) 0.1330(4) 0.072(2) Uani 1.00 d . . . H(1) H 0.4769 -0.2062 0.4056 0.1158 Uiso 1.00 calc . . . H(2) H 0.4588 -0.1492 0.3236 0.1158 Uiso 1.00 calc . . . H(3) H 0.5031 -0.0765 0.4341 0.0974 Uiso 1.00 calc . . . H(4) H 0.4674 -0.1037 0.5156 0.0974 Uiso 1.00 calc . . . H(5) H 0.0659 -0.1527 0.4542 0.0824 Uiso 1.00 calc . . . H(6) H 0.1138 -0.1665 0.3955 0.0824 Uiso 1.00 calc . . . H(7) H 0.1165 -0.1504 0.5062 0.0824 Uiso 1.00 calc . . . H(8) H 0.1931 0.2395 0.4515 0.0899 Uiso 1.00 calc . . . H(9) H 0.1957 0.2341 0.3394 0.0899 Uiso 1.00 calc . . . H(10) H 0.1529 0.2806 0.3887 0.0899 Uiso 1.00 calc . . . H(11) H 0.4941 0.0169 0.2184 0.1539 Uiso 1.00 calc . . . H(12) H 0.4833 0.0245 0.1084 0.1539 Uiso 1.00 calc . . . H(13) H 0.4840 0.1338 0.1380 0.2043 Uiso 1.00 calc . . . H(14) H 0.4716 0.1199 0.2465 0.2043 Uiso 1.00 calc . . . H(15) H 0.1212 -0.2576 0.1857 0.0869 Uiso 1.00 calc . . . H(16) H 0.1657 -0.2263 0.1261 0.0869 Uiso 1.00 calc . . . H(17) H 0.1667 -0.2221 0.2384 0.0869 Uiso 1.00 calc . . . H(18) H 0.1249 0.1986 0.1781 0.0853 Uiso 1.00 calc . . . H(19) H 0.1190 0.1747 0.0700 0.0853 Uiso 1.00 calc . . . H(20) H 0.0729 0.1936 0.1323 0.0853 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0466(4) 0.0492(4) 0.0523(3) 0.0030(3) -0.0010(3) 0.0004(3) Ni(2) 0.0457(4) 0.0532(4) 0.0512(3) -0.0017(3) 0.0026(3) -0.0012(3) Cl(1) 0.0614(9) 0.109(1) 0.102(1) 0.0091(9) -0.0104(8) 0.0150(9) S(1) 0.0583(8) 0.0538(8) 0.0681(8) 0.0023(7) 0.0019(6) 0.0034(7) S(2) 0.0515(7) 0.0530(8) 0.0589(7) 0.0035(6) -0.0008(6) -0.0038(6) S(3) 0.0523(7) 0.0501(8) 0.0587(7) -0.0001(6) -0.0045(6) 0.0028(6) S(4) 0.0465(7) 0.0461(8) 0.0624(7) 0.0014(6) -0.0038(6) -0.0022(6) S(5) 0.0527(8) 0.0648(9) 0.0706(8) -0.0057(7) 0.0024(6) 0.0024(7) S(6) 0.0507(7) 0.0545(9) 0.0703(8) 0.0035(7) -0.0017(6) -0.0020(7) S(7) 0.0540(7) 0.0556(8) 0.0575(7) -0.0002(7) 0.0015(6) -0.0014(6) S(8) 0.0545(8) 0.0602(9) 0.0678(8) -0.0041(7) 0.0008(6) 0.0033(7) S(9) 0.0518(7) 0.0542(8) 0.0600(7) -0.0005(6) 0.0024(6) -0.0055(6) S(10) 0.0502(7) 0.0566(8) 0.0555(7) -0.0023(6) 0.0040(6) 0.0009(6) S(11) 0.0542(8) 0.0617(9) 0.0727(8) -0.0071(7) 0.0021(7) -0.0025(7) S(12) 0.0509(8) 0.0645(9) 0.0742(8) 0.0030(7) -0.0028(6) 0.0014(7) O(1) 0.065(2) 0.062(3) 0.113(3) 0.016(2) 0.008(2) 0.001(2) O(2) 0.056(2) 0.063(2) 0.076(2) 0.002(2) 0.009(2) -0.001(2) O(3) 0.054(2) 0.071(3) 0.095(2) 0.007(2) -0.001(2) -0.005(2) O(4) 0.074(3) 0.067(3) 0.119(3) -0.013(2) -0.004(2) 0.009(2) O(5) 0.130(4) 0.187(6) 0.267(6) 0.089(4) 0.058(4) 0.046(5) O(6) 0.132(5) 0.257(7) 0.161(4) 0.063(5) 0.016(3) 0.088(4) O(7) 0.133(5) 0.151(6) 0.283(7) -0.023(5) 0.065(5) 0.001(5) O(8) 0.153(6) 0.40(1) 0.217(6) 0.015(7) -0.047(5) -0.083(7) C(1) 0.054(3) 0.054(3) 0.060(3) 0.008(3) -0.003(2) 0.003(3) C(2) 0.050(3) 0.067(4) 0.056(3) 0.001(3) 0.002(2) -0.004(3) C(3) 0.049(3) 0.060(3) 0.046(2) -0.003(2) 0.007(2) -0.009(2) C(4) 0.050(3) 0.037(3) 0.039(2) -0.001(2) 0.007(2) 0.001(2) C(5) 0.066(4) 0.076(5) 0.150(5) 0.021(4) 0.026(4) 0.015(4) C(6) 0.057(4) 0.087(5) 0.108(4) 0.016(3) 0.001(3) -0.001(3) C(7) 0.062(3) 0.067(4) 0.087(3) -0.013(3) 0.003(3) 0.012(3) C(8) 0.065(3) 0.063(4) 0.099(4) -0.004(3) 0.007(3) 0.003(3) C(9) 0.052(3) 0.063(3) 0.059(3) -0.001(3) -0.001(2) 0.007(3) C(10) 0.061(3) 0.053(3) 0.053(3) -0.005(3) 0.005(2) 0.007(2) C(11) 0.052(3) 0.048(3) 0.040(2) -0.004(2) 0.000(2) -0.001(2) C(12) 0.050(3) 0.054(3) 0.039(2) 0.005(2) 0.003(2) -0.006(2) C(13) 0.071(5) 0.103(6) 0.226(8) -0.018(4) 0.003(5) 0.005(5) C(14) 0.052(5) 0.103(7) 0.40(1) 0.004(5) -0.012(7) -0.034(8) C(15) 0.088(4) 0.060(4) 0.079(4) 0.003(3) 0.004(3) -0.005(3) C(16) 0.073(4) 0.066(4) 0.077(3) 0.004(3) -0.002(3) -0.006(3) #------------------------------------------------------------------------------ _computing_data_collection 'Mac Science DIP320' _computing_cell_refinement 'Mac Denzo' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.165(2) . . yes Ni(1) S(2) 2.168(2) . . yes Ni(1) S(3) 2.154(2) . . yes Ni(1) S(4) 2.131(2) . . yes Ni(2) S(7) 2.156(2) . . yes Ni(2) S(8) 2.162(2) . . yes Ni(2) S(9) 2.133(2) . . yes Ni(2) S(10) 2.144(2) . . yes Cl(1) O(5) 1.370(6) . . yes Cl(1) O(6) 1.329(6) . . yes Cl(1) O(7) 1.434(7) . . yes Cl(1) O(8) 1.340(8) . . yes S(1) C(1) 1.702(5) . . yes S(2) C(2) 1.688(5) . . yes S(3) C(3) 1.696(5) . . yes S(4) C(4) 1.685(5) . . yes S(5) C(3) 1.734(5) . . yes S(5) C(7) 1.834(6) . . yes S(6) C(4) 1.720(5) . . yes S(6) C(8) 1.769(6) . . yes S(7) C(9) 1.676(5) . . yes S(8) C(10) 1.680(5) . . yes S(9) C(11) 1.680(5) . . yes S(10) C(12) 1.669(5) . . yes S(11) C(11) 1.775(5) . . yes S(11) C(15) 1.807(6) . . yes S(12) C(12) 1.715(5) . . yes S(12) C(16) 1.781(6) . . yes O(1) C(1) 1.346(6) . . yes O(1) C(5) 1.484(7) . . yes O(2) C(2) 1.372(6) . . yes O(2) C(6) 1.475(7) . . yes O(3) C(9) 1.348(6) . . yes O(3) C(13) 1.480(9) . . yes O(4) C(10) 1.337(6) . . yes O(4) C(14) 1.468(9) . . yes C(1) C(2) 1.360(7) . . yes C(3) C(4) 1.401(7) . . yes C(5) C(6) 1.460(9) . . yes C(9) C(10) 1.394(8) . . yes C(11) C(12) 1.409(7) . . yes C(13) C(14) 1.26(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(2) 92.71(5) 1_555 1_555 1_555 yes S(1) Ni(1) S(3) 88.46(6) 1_555 1_555 1_555 yes S(1) Ni(1) S(4) 179.66(6) 1_555 1_555 1_555 yes S(2) Ni(1) S(3) 173.09(5) 1_555 1_555 1_555 yes S(2) Ni(1) S(4) 87.52(6) 1_555 1_555 1_555 yes S(3) Ni(1) S(4) 91.28(6) 1_555 1_555 1_555 yes S(7) Ni(2) S(8) 92.37(6) 1_555 1_555 1_555 yes S(7) Ni(2) S(9) 87.16(6) 1_555 1_555 1_555 yes S(7) Ni(2) S(10) 176.11(5) 1_555 1_555 1_555 yes S(8) Ni(2) S(9) 178.09(5) 1_555 1_555 1_555 yes S(8) Ni(2) S(10) 88.67(6) 1_555 1_555 1_555 yes S(9) Ni(2) S(10) 91.68(6) 1_555 1_555 1_555 yes O(5) Cl(1) O(6) 111.7(4) 1_555 1_555 1_555 yes O(5) Cl(1) O(7) 110.8(4) 1_555 1_555 1_555 yes O(5) Cl(1) O(8) 110.0(4) 1_555 1_555 1_555 yes O(6) Cl(1) O(7) 110.1(4) 1_555 1_555 1_555 yes O(6) Cl(1) O(8) 108.1(5) 1_555 1_555 1_555 yes O(7) Cl(1) O(8) 106.0(5) 1_555 1_555 1_555 yes Ni(1) S(1) C(1) 101.7(2) 1_555 1_555 1_555 yes Ni(1) S(2) C(2) 102.2(2) 1_555 1_555 1_555 yes Ni(1) S(3) C(3) 104.2(2) 1_555 1_555 1_555 yes Ni(1) S(4) C(4) 105.6(2) 1_555 1_555 1_555 yes C(3) S(5) C(7) 103.1(2) 1_555 1_555 1_555 yes C(4) S(6) C(8) 103.3(2) 1_555 1_555 1_555 yes Ni(2) S(7) C(9) 103.2(2) 1_555 1_555 1_555 yes Ni(2) S(8) C(10) 102.5(2) 1_555 1_555 1_555 yes Ni(2) S(9) C(11) 103.7(2) 1_555 1_555 1_555 yes Ni(2) S(10) C(12) 105.0(2) 1_555 1_555 1_555 yes C(11) S(11) C(15) 104.6(3) 1_555 1_555 1_555 yes C(12) S(12) C(16) 102.8(3) 1_555 1_555 1_555 yes C(1) O(1) C(5) 112.3(4) 1_555 1_555 1_555 yes C(2) O(2) C(6) 112.9(4) 1_555 1_555 1_555 yes C(9) O(3) C(13) 114.8(5) 1_555 1_555 1_555 yes C(10) O(4) C(14) 115.4(5) 1_555 1_555 1_555 yes S(1) C(1) O(1) 114.3(4) 1_555 1_555 1_555 yes S(1) C(1) C(2) 121.5(4) 1_555 1_555 1_555 yes O(1) C(1) C(2) 124.2(5) 1_555 1_555 1_555 yes S(2) C(2) O(2) 115.9(4) 1_555 1_555 1_555 yes S(2) C(2) C(1) 121.3(4) 1_555 1_555 1_555 yes O(2) C(2) C(1) 122.7(5) 1_555 1_555 1_555 yes S(3) C(3) S(5) 122.2(3) 1_555 1_555 1_555 yes S(3) C(3) C(4) 120.0(4) 1_555 1_555 1_555 yes S(5) C(3) C(4) 117.9(4) 1_555 1_555 1_555 yes S(4) C(4) S(6) 123.4(3) 1_555 1_555 1_555 yes S(4) C(4) C(3) 118.9(4) 1_555 1_555 1_555 yes S(6) C(4) C(3) 117.7(3) 1_555 1_555 1_555 yes O(1) C(5) C(6) 110.8(5) 1_555 1_555 1_555 yes O(1) C(5) H(1) 108.9(6) 1_555 1_555 1_555 no O(1) C(5) H(2) 109.1(5) 1_555 1_555 1_555 no C(6) C(5) H(1) 110.6(6) 1_555 1_555 1_555 no C(6) C(5) H(2) 109.7(6) 1_555 1_555 1_555 no H(1) C(5) H(2) 107.6(6) 1_555 1_555 1_555 no O(2) C(6) C(5) 110.3(5) 1_555 1_555 1_555 yes O(2) C(6) H(3) 109.8(5) 1_555 1_555 1_555 no O(2) C(6) H(4) 110.7(5) 1_555 1_555 1_555 no C(5) C(6) H(3) 108.8(5) 1_555 1_555 1_555 no C(5) C(6) H(4) 108.9(6) 1_555 1_555 1_555 no H(3) C(6) H(4) 108.2(5) 1_555 1_555 1_555 no S(5) C(7) H(5) 109.8(4) 1_555 1_555 1_555 no S(5) C(7) H(6) 109.8(4) 1_555 1_555 1_555 no S(5) C(7) H(7) 110.7(4) 1_555 1_555 1_555 no H(5) C(7) H(6) 107.9(5) 1_555 1_555 1_555 no H(5) C(7) H(7) 109.2(5) 1_555 1_555 1_555 no H(6) C(7) H(7) 109.4(5) 1_555 1_555 1_555 no S(6) C(8) H(8) 110.4(5) 1_555 1_555 1_555 no S(6) C(8) H(9) 110.2(5) 1_555 1_555 1_555 no S(6) C(8) H(10) 110.0(4) 1_555 1_555 1_555 no H(8) C(8) H(9) 109.2(5) 1_555 1_555 1_555 no H(8) C(8) H(10) 108.7(6) 1_555 1_555 1_555 no H(9) C(8) H(10) 108.4(6) 1_555 1_555 1_555 no S(7) C(9) O(3) 117.1(4) 1_555 1_555 1_555 yes S(7) C(9) C(10) 120.4(4) 1_555 1_555 1_555 yes O(3) C(9) C(10) 122.5(5) 1_555 1_555 1_555 yes S(8) C(10) O(4) 117.0(4) 1_555 1_555 1_555 yes S(8) C(10) C(9) 121.3(4) 1_555 1_555 1_555 yes O(4) C(10) C(9) 121.7(4) 1_555 1_555 1_555 yes S(9) C(11) S(11) 120.3(3) 1_555 1_555 1_555 yes S(9) C(11) C(12) 121.1(4) 1_555 1_555 1_555 yes S(11) C(11) C(12) 118.6(4) 1_555 1_555 1_555 yes S(10) C(12) S(12) 124.1(3) 1_555 1_555 1_555 yes S(10) C(12) C(11) 118.3(4) 1_555 1_555 1_555 yes S(12) C(12) C(11) 117.5(4) 1_555 1_555 1_555 yes O(3) C(13) C(14) 120.5(7) 1_555 1_555 1_555 yes O(3) C(13) H(11) 108.4(7) 1_555 1_555 1_555 no O(3) C(13) H(12) 108.0(7) 1_555 1_555 1_555 no C(14) C(13) H(11) 106.7(8) 1_555 1_555 1_555 no C(14) C(13) H(12) 106.4(9) 1_555 1_555 1_555 no H(11) C(13) H(12) 106.2(7) 1_555 1_555 1_555 no O(4) C(14) C(13) 121.3(7) 1_555 1_555 1_555 yes O(4) C(14) H(13) 107.1(8) 1_555 1_555 1_555 no O(4) C(14) H(14) 108.5(8) 1_555 1_555 1_555 no C(13) C(14) H(13) 106.4(9) 1_555 1_555 1_555 no C(13) C(14) H(14) 106.7(9) 1_555 1_555 1_555 no H(13) C(14) H(14) 105.9(8) 1_555 1_555 1_555 no S(11) C(15) H(15) 110.4(5) 1_555 1_555 1_555 no S(11) C(15) H(16) 110.6(4) 1_555 1_555 1_555 no S(11) C(15) H(17) 109.9(4) 1_555 1_555 1_555 no H(15) C(15) H(16) 109.1(5) 1_555 1_555 1_555 no H(15) C(15) H(17) 108.2(5) 1_555 1_555 1_555 no H(16) C(15) H(17) 108.5(6) 1_555 1_555 1_555 no S(12) C(16) H(18) 110.5(4) 1_555 1_555 1_555 no S(12) C(16) H(19) 110.4(4) 1_555 1_555 1_555 no S(12) C(16) H(20) 109.5(4) 1_555 1_555 1_555 no H(18) C(16) H(19) 109.6(6) 1_555 1_555 1_555 no H(18) C(16) H(20) 108.5(5) 1_555 1_555 1_555 no H(19) C(16) H(20) 108.3(5) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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 Ni(1) S(1) C(1) O(1) -174.8(3) 1_555 1_555 1_555 1_555 yes Ni(1) S(1) C(1) C(2) 8.2(4) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) O(2) -178.7(3) 1_555 1_555 1_555 1_555 yes Ni(1) S(2) C(2) C(1) 3.3(4) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(3) S(5) -178.8(2) 1_555 1_555 1_555 1_555 yes Ni(1) S(3) C(3) C(4) -0.2(4) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(4) S(6) -178.2(2) 1_555 1_555 1_555 1_555 yes Ni(1) S(4) C(4) C(3) 0.8(3) 1_555 1_555 1_555 1_555 yes Ni(2) S(7) C(9) O(3) 177.0(3) 1_555 1_555 1_555 1_555 yes Ni(2) S(7) C(9) C(10) -1.2(4) 1_555 1_555 1_555 1_555 yes Ni(2) S(8) C(10) O(4) -178.0(3) 1_555 1_555 1_555 1_555 yes Ni(2) S(8) C(10) C(9) 3.4(4) 1_555 1_555 1_555 1_555 yes Ni(2) S(9) C(11) S(11) -179.8(2) 1_555 1_555 1_555 1_555 yes Ni(2) S(9) C(11) C(12) 2.5(3) 1_555 1_555 1_555 1_555 yes Ni(2) S(10) C(12) S(12) 174.6(2) 1_555 1_555 1_555 1_555 yes Ni(2) S(10) C(12) C(11) -3.5(3) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(2) C(2) 1.5(2) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(3) C(3) -179.7(2) 1_555 1_555 1_555 1_555 yes S(1) Ni(1) S(4) C(4) -40(9) 1_555 1_555 1_555 1_555 yes S(1) C(1) O(1) C(5) 169.7(3) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) S(2) -8.2(6) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(2) O(2) 173.8(3) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(1) C(1) -4.6(2) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(3) C(3) 80.5(5) 1_555 1_555 1_555 1_555 yes S(2) Ni(1) S(4) C(4) -173.9(1) 1_555 1_555 1_555 1_555 yes S(2) C(2) O(2) C(6) 169.3(3) 1_555 1_555 1_555 1_555 yes S(2) C(2) C(1) O(1) 175.0(3) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(1) C(1) -177.8(2) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(2) C(2) 101.1(5) 1_555 1_555 1_555 1_555 yes S(3) Ni(1) S(4) C(4) -0.7(1) 1_555 1_555 1_555 1_555 yes S(3) C(3) S(5) C(7) 3.6(3) 1_555 1_555 1_555 1_555 yes S(3) C(3) C(4) S(4) -0.4(5) 1_555 1_555 1_555 1_555 yes S(3) C(3) C(4) S(6) 178.7(2) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(1) C(1) -137(9) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(2) C(2) -178.8(2) 1_555 1_555 1_555 1_555 yes S(4) Ni(1) S(3) C(3) 0.5(2) 1_555 1_555 1_555 1_555 yes S(4) C(4) S(6) C(8) -5.4(3) 1_555 1_555 1_555 1_555 yes S(4) C(4) C(3) S(5) 178.2(2) 1_555 1_555 1_555 1_555 yes S(5) C(3) C(4) S(6) -2.7(4) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(8) C(10) -3.2(2) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(9) C(11) -179.9(1) 1_555 1_555 1_555 1_555 yes S(7) Ni(2) S(10) C(12) 76.5(9) 1_555 1_555 1_555 1_555 yes S(7) C(9) O(3) C(13) 175.9(4) 1_555 1_555 1_555 1_555 yes S(7) C(9) C(10) S(8) -1.6(5) 1_555 1_555 1_555 1_555 yes S(7) C(9) C(10) O(4) 179.9(3) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(7) C(9) 2.5(2) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(9) C(11) -104(1) 1_555 1_555 1_555 1_555 yes S(8) Ni(2) S(10) C(12) -177.9(2) 1_555 1_555 1_555 1_555 yes S(8) C(10) O(4) C(14) 174.8(6) 1_555 1_555 1_555 1_555 yes S(8) C(10) C(9) O(3) -179.7(3) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(7) C(9) -179.3(2) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(8) C(10) -78(1) 1_555 1_555 1_555 1_555 yes S(9) Ni(2) S(10) C(12) 4.0(2) 1_555 1_555 1_555 1_555 yes S(9) C(11) S(11) C(15) -1.6(3) 1_555 1_555 1_555 1_555 yes S(9) C(11) C(12) S(10) 0.7(5) 1_555 1_555 1_555 1_555 yes S(9) C(11) C(12) S(12) -177.6(2) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(7) C(9) 108.0(9) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(8) C(10) -179.4(2) 1_555 1_555 1_555 1_555 yes S(10) Ni(2) S(9) C(11) -3.6(1) 1_555 1_555 1_555 1_555 yes S(10) C(12) S(12) C(16) 11.0(3) 1_555 1_555 1_555 1_555 yes S(10) C(12) C(11) S(11) -177.0(2) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) S(12) 4.7(4) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) O(2) -2.9(7) 1_555 1_555 1_555 1_555 yes O(1) C(5) C(6) O(2) -60.0(6) 1_555 1_555 1_555 1_555 yes O(3) C(9) C(10) O(4) 1.8(7) 1_555 1_555 1_555 1_555 yes O(3) C(13) C(14) O(4) -24(1) 1_555 1_555 1_555 1_555 yes C(1) O(1) C(5) C(6) 44.4(6) 1_555 1_555 1_555 1_555 yes C(1) C(2) O(2) C(6) -12.6(6) 1_555 1_555 1_555 1_555 yes C(2) O(2) C(6) C(5) 43.5(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) O(1) C(5) -13.3(6) 1_555 1_555 1_555 1_555 yes C(3) C(4) S(6) C(8) 175.5(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) S(5) C(7) -175.0(3) 1_555 1_555 1_555 1_555 yes C(9) O(3) C(13) C(14) 17(1) 1_555 1_555 1_555 1_555 yes C(9) C(10) O(4) C(14) -6.7(7) 1_555 1_555 1_555 1_555 yes C(10) O(4) C(14) C(13) 18(1) 1_555 1_555 1_555 1_555 yes C(10) C(9) O(3) C(13) -6.0(6) 1_555 1_555 1_555 1_555 yes C(11) C(12) S(12) C(16) -170.8(3) 1_555 1_555 1_555 1_555 yes C(12) C(11) S(11) C(15) 176.1(3) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(2) C(12) 3.473(4) . 7_555 ? S(5) C(9) 3.503(4) . 7_555 ? S(6) O(7) 3.282(7) . 2_555 ? S(6) O(6) 3.423(6) . 2_555 ? S(11) O(5) 3.143(7) . 3_455 ? S(12) O(6) 3.357(6) . 2_555 ? O(1) C(7) 2.970(7) . 2_545 ? O(2) C(6) 3.584(7) . 5_656 ? O(3) O(6) 3.552(7) . 4_645 ? O(4) C(16) 3.183(7) . 2_555 ? O(5) C(15) 3.209(8) . 3_555 ? O(5) C(6) 3.555(9) . 5_656 ? O(6) C(16) 3.257(8) . 2_555 ? O(6) C(5) 3.294(8) . 4_655 ? O(7) C(8) 3.417(9) . 2_555 ? O(8) C(7) 3.334(9) . 6_556 ? O(8) C(14) 3.41(1) . 8_555 ? #------------------------------------------------------------------------------