# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1157 data_Cu(3mpSO3)(1) #------------------------------------------------------------------------------ _audit_creation_date 'Tue Nov 17 20:38:30 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 407.90 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H12 Cu N2 O6 S2 ' _chemical_formula_moiety 'C12 H12 Cu N2 O6 S2 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 7.7242(8) _cell_length_b 9.7417(8) _cell_length_c 4.9584(7) _cell_angle_alpha 103.837(9) _cell_angle_beta 98.12(1) _cell_angle_gamma 93.227(8) _cell_volume 357.07(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _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 'prismatic' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 207.00 _exptl_absorpt_coefficient_mu 1.855 _exptl_absorpt_correction_type '_y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.874 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K_a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method '_w-2_q' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.13 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 -1 2 1 0 1 -1 0 _diffrn_reflns_number 2293 _reflns_number_total 2069 _reflns_number_observed 1736 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.037 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.12298 _diffrn_orient_matrix_UB_12 -0.02493 _diffrn_orient_matrix_UB_13 -0.01206 _diffrn_orient_matrix_UB_21 -0.04472 _diffrn_orient_matrix_UB_22 -0.10193 _diffrn_orient_matrix_UB_23 -0.08269 _diffrn_orient_matrix_UB_31 -0.01138 _diffrn_orient_matrix_UB_32 0.01628 _diffrn_orient_matrix_UB_33 -0.19310 #------------------------------------------------------------------------------ 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 C 0 12 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 12 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 2 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 2 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 6 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cu 0 1 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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 Cu(1) 1.0000 0.0000 1.0000 0.0247(1) Uani d . 0.50 S S(1) 1.08044(7) -0.21003(6) 1.3452(1) 0.0238(1) Uani d . 1.00 . O(1) 1.1481(2) -0.0778(2) 1.2762(4) 0.0302(5) Uani d . 1.00 . O(2) 1.0907(3) -0.1882(2) 1.6483(4) 0.0314(5) Uani d . 1.00 . O(3) 1.1476(4) -0.3345(3) 1.2055(6) 0.0559(8) Uani d . 1.00 . N(1) 0.8082(3) -0.1332(2) 1.0442(4) 0.0228(5) Uani d . 1.00 . C(1) 0.8496(3) -0.2238(2) 1.2039(5) 0.0226(5) Uani d . 1.00 . C(2) 0.7272(3) -0.3205(3) 1.2561(5) 0.0260(6) Uani d . 1.00 . C(3) 0.5524(3) -0.3149(3) 1.1432(6) 0.0317(6) Uani d . 1.00 . C(4) 0.5084(3) -0.2217(3) 0.9798(6) 0.0332(7) Uani d . 1.00 . C(5) 0.6395(3) -0.1334(3) 0.9305(6) 0.0287(6) Uani d . 1.00 . C(6) 0.7761(4) -0.4280(3) 1.4202(6) 0.0347(7) Uani d . 1.00 . H(1) 0.4639 -0.3740 1.1958 0.029(8) Uiso calc . 1.00 S H(2) 0.3859 -0.2262 0.8779 0.06(1) Uiso calc . 1.00 S H(3) 0.6149 -0.0681 0.8153 0.040(9) Uiso calc . 1.00 S H(4) 0.8591 -0.3950 1.5721 0.05(1) Uiso calc . 1.00 S H(5) 0.8309 -0.4938 1.3164 0.044(10) Uiso calc . 1.00 S H(6) 0.6784 -0.4655 1.4872 0.07(1) Uiso calc . 1.00 S 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 Cu(1) 0.0190(2) 0.0313(2) 0.0269(2) -0.0011(2) -0.0002(2) 0.0161(2) S(1) 0.0212(3) 0.0293(3) 0.0228(3) 0.0033(2) 0.0020(2) 0.0109(2) O(1) 0.0222(9) 0.0381(10) 0.0326(9) -0.0035(7) -0.0026(7) 0.0190(8) O(2) 0.0321(10) 0.041(1) 0.0228(9) 0.0025(8) 0.0004(7) 0.0143(8) O(3) 0.049(1) 0.057(2) 0.067(2) 0.015(1) 0.015(1) 0.018(1) N(1) 0.0206(9) 0.0264(9) 0.0223(9) 0.0020(7) 0.0022(7) 0.0086(7) C(1) 0.021(1) 0.025(1) 0.022(1) 0.0027(8) 0.0025(8) 0.0062(8) C(2) 0.027(1) 0.025(1) 0.028(1) 0.0014(9) 0.0048(9) 0.0097(9) C(3) 0.024(1) 0.031(1) 0.041(1) -0.0014(10) 0.006(1) 0.012(1) C(4) 0.021(1) 0.036(1) 0.043(2) 0.0027(10) 0.001(1) 0.013(1) C(5) 0.022(1) 0.030(1) 0.035(1) 0.0039(9) 0.0004(10) 0.013(1) C(6) 0.035(1) 0.032(1) 0.041(1) 0.002(1) 0.004(1) 0.019(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[_s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1736 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0328 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0513 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.698 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.76 _refine_diff_density_max 0.28 #------------------------------------------------------------------------------ _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 Cu(1) O(1) 1.977(2) 1_555 1_555 yes Cu(1) O(1) 1.977(2) 1_555 2_757 yes Cu(1) N(1) 1.985(2) 1_555 1_555 yes Cu(1) N(1) 1.985(2) 1_555 2_757 yes S(1) O(1) 1.495(2) 1_555 1_555 yes S(1) O(2) 1.457(2) 1_555 1_555 yes S(1) O(3) 1.411(3) 1_555 1_555 yes S(1) C(1) 1.806(2) 1_555 1_555 yes N(1) C(1) 1.342(3) 1_555 1_555 yes N(1) C(5) 1.344(3) 1_555 1_555 yes C(1) C(2) 1.391(3) 1_555 1_555 yes C(2) C(3) 1.396(4) 1_555 1_555 yes C(2) C(6) 1.506(4) 1_555 1_555 yes C(3) C(4) 1.380(4) 1_555 1_555 yes C(4) C(5) 1.378(4) 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 O(1) Cu(1) O(1) 180.0 1_555 1_555 2_757 yes O(1) Cu(1) N(1) 85.26(7) 1_555 1_555 1_555 yes O(1) Cu(1) N(1) 94.74(7) 1_555 1_555 2_757 yes O(1) Cu(1) N(1) 94.74(7) 2_757 1_555 1_555 yes O(1) Cu(1) N(1) 85.26(7) 2_757 1_555 2_757 yes N(1) Cu(1) N(1) 180.0 1_555 1_555 2_757 yes O(1) S(1) O(2) 110.5(1) 1_555 1_555 1_555 yes O(1) S(1) O(3) 114.2(1) 1_555 1_555 1_555 yes O(1) S(1) C(1) 102.0(1) 1_555 1_555 1_555 yes O(2) S(1) O(3) 115.7(1) 1_555 1_555 1_555 yes O(2) S(1) C(1) 106.1(1) 1_555 1_555 1_555 yes O(3) S(1) C(1) 107.0(1) 1_555 1_555 1_555 yes Cu(1) O(1) S(1) 119.1(1) 1_555 1_555 1_555 yes Cu(1) N(1) C(1) 117.8(2) 1_555 1_555 1_555 yes Cu(1) N(1) C(5) 123.2(2) 1_555 1_555 1_555 yes C(1) N(1) C(5) 119.0(2) 1_555 1_555 1_555 yes S(1) C(1) N(1) 114.0(2) 1_555 1_555 1_555 yes S(1) C(1) C(2) 122.5(2) 1_555 1_555 1_555 yes N(1) C(1) C(2) 123.5(2) 1_555 1_555 1_555 yes C(1) C(2) C(3) 116.2(2) 1_555 1_555 1_555 yes C(1) C(2) C(6) 123.2(2) 1_555 1_555 1_555 yes C(3) C(2) C(6) 120.6(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.7(2) 1_555 1_555 1_555 yes C(2) C(3) H(1) 117.1(3) 1_555 1_555 1_555 no C(4) C(3) H(1) 122.1(3) 1_555 1_555 1_555 no C(3) C(4) C(5) 119.1(2) 1_555 1_555 1_555 yes C(3) C(4) H(2) 120.8(3) 1_555 1_555 1_555 no C(5) C(4) H(2) 119.7(3) 1_555 1_555 1_555 no N(1) C(5) C(4) 121.5(2) 1_555 1_555 1_555 yes N(1) C(5) H(3) 116.7(2) 1_555 1_555 1_555 no C(4) C(5) H(3) 121.8(3) 1_555 1_555 1_555 no C(2) C(6) H(4) 114.5(3) 1_555 1_555 1_555 no C(2) C(6) H(5) 108.6(3) 1_555 1_555 1_555 no C(2) C(6) H(6) 112.7(3) 1_555 1_555 1_555 no H(4) C(6) H(5) 100.9(3) 1_555 1_555 1_555 no H(4) C(6) H(6) 105.8(3) 1_555 1_555 1_555 no H(5) C(6) H(6) 113.9(3) 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 Cu(1) S(1) 3.5568(6) 1_555 1_554 ? Cu(1) S(1) 3.5568(6) 1_555 2_758 ? S(1) O(2) 3.524(2) 1_555 1_554 ? O(1) O(2) 3.000(3) 1_555 1_554 ? O(1) O(2) 3.244(3) 1_555 2_758 ? O(1) C(1) 3.411(3) 1_555 2_758 ? O(1) N(1) 3.462(3) 1_555 2_758 ? O(1) C(4) 3.532(3) 1_555 1_655 ? O(1) O(1) 3.561(4) 1_555 2_758 ? O(2) N(1) 3.121(3) 1_555 1_556 ? O(2) N(1) 3.137(3) 1_555 2_758 ? O(2) O(3) 3.386(3) 1_555 1_556 ? O(2) C(4) 3.478(3) 1_555 1_656 ? O(3) C(3) 3.185(4) 1_555 1_655 ? O(3) C(6) 3.323(4) 1_555 2_748 ? O(3) C(4) 3.369(4) 1_555 1_655 ? O(3) C(6) 3.544(4) 1_555 2_747 ? C(2) C(5) 3.581(4) 1_555 1_556 ? C(3) C(3) 3.546(5) 1_555 2_647 ? C(5) C(5) 3.474(5) 1_555 2_657 ? #------------------------------------------------------------------------------ _publ_requested_journal ' Chemical Communication ' _publ_contact_author ; Isamu Kinoshita Department of Molecular Materials Science, Graduate School of Science, Osaka City University, Sugimoto, Sumiyoshi-ku, Osaka 558-8585, JAPAN ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' +81-6-6605-3146 ' _publ_contact_author_fax ' +81-6-6690-2753 ' _publ_contact_author_email ' isamu@sci.osaka-cu.ac.jp ' loop_ _publ_author_name ' Kentaro Kimura ' ; _publ_author_address Department of Molecular Materials Science, Graduate School of Science, Osaka City University, Sugimoto, Sumiyoshi-ku, Osaka 558-8585, JAPAN ; _publ_section_title ; ENTER SECTION TITLE ; _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. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; # = END data_Zn(3mpSO3)2(H2O)2(2) #------------------------------------------------------------------------------ _audit_creation_date 'Thu Oct 22 10:12:14 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 445.77 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 N2 O8 S2 Zn ' _chemical_formula_moiety 'C12 H16 N2 O8 S2 Zn ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 19.058(1) _cell_length_b 7.381(1) _cell_length_c 14.321(1) _cell_angle_alpha 90 _cell_angle_beta 126.176(4) _cell_angle_gamma 90 _cell_volume 1626.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.620 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_min 0.280 _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 912.00 _exptl_absorpt_coefficient_mu 1.813 _exptl_absorpt_correction_type '_y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.768 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K_a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method ' _w-2_q ' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.39 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 0 -2 0 0 -2 2 -2 -2 _diffrn_reflns_number 2630 _reflns_number_total 2556 _reflns_number_observed 2056 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.031 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01455 _diffrn_orient_matrix_UB_12 -0.04838 _diffrn_orient_matrix_UB_13 -0.05189 _diffrn_orient_matrix_UB_21 -0.01489 _diffrn_orient_matrix_UB_22 -0.12514 _diffrn_orient_matrix_UB_23 0.00975 _diffrn_orient_matrix_UB_31 -0.06158 _diffrn_orient_matrix_UB_32 0.01882 _diffrn_orient_matrix_UB_33 -0.06852 #------------------------------------------------------------------------------ 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 C 0 48 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 32 0.011 0.006 ;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) ; Zn 0 4 0.284 1.430 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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 Zn(1) 1.0000 0.01962(4) 0.2500 0.02299(7) Uani d . 0.50 S S(1) 1.08092(3) -0.25552(6) 0.16920(3) 0.02362(10) Uani d . 1.00 . O(1) 0.99993(8) -0.1724(2) 0.1366(1) 0.0378(4) Uani d . 1.00 . O(2) 1.0868(1) -0.4453(2) 0.1971(1) 0.0441(4) Uani d . 1.00 . O(3) 1.10048(10) -0.2166(2) 0.0878(1) 0.0418(4) Uani d . 1.00 . O(4) 1.0079(1) 0.2313(2) 0.3533(1) 0.0398(4) Uani d . 1.00 . N(1) 1.13430(9) -0.0346(2) 0.3455(1) 0.0215(3) Uani d . 1.00 . C(1) 1.16409(10) -0.1466(2) 0.3024(1) 0.0201(3) Uani d . 1.00 . C(2) 1.2522(1) -0.1826(2) 0.3576(2) 0.0246(4) Uani d . 1.00 . C(3) 1.3100(1) -0.0998(3) 0.4647(2) 0.0294(4) Uani d . 1.00 . C(4) 1.2794(1) 0.0098(2) 0.5118(2) 0.0294(4) Uani d . 1.00 . C(5) 1.1915(1) 0.0409(2) 0.4497(2) 0.0262(4) Uani d . 1.00 . C(6) 1.2860(1) -0.3046(3) 0.3088(2) 0.0394(6) Uani d . 1.00 . H(1) 1.367(2) -0.124(3) 0.501(2) 0.041(6) Uiso calc . 1.00 . H(2) 1.317(1) 0.065(3) 0.586(2) 0.029(5) Uiso calc . 1.00 . H(3) 1.173(1) 0.109(3) 0.476(2) 0.031(6) Uiso calc . 1.00 . H(4) 1.277(3) -0.260(5) 0.241(3) 0.10(1) Uiso calc . 1.00 . H(5) 1.265(3) -0.413(6) 0.296(3) 0.10(1) Uiso calc . 1.00 . H(6) 1.340(3) -0.327(6) 0.367(4) 0.11(1) Uiso calc . 1.00 . H(7) 1.019(2) 0.212(4) 0.413(2) 0.044(7) Uiso calc . 1.00 . H(8) 0.983(2) 0.329(4) 0.333(2) 0.042(7) 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 Zn(1) 0.0184(1) 0.0249(2) 0.0229(1) 0.0000 0.0107(1) 0.0000 S(1) 0.0240(2) 0.0237(2) 0.0218(2) -0.0037(1) 0.0127(2) -0.0051(1) O(1) 0.0210(6) 0.0483(9) 0.0325(7) -0.0017(6) 0.0094(5) -0.0166(6) O(2) 0.0498(9) 0.0240(7) 0.0424(8) -0.0105(6) 0.0184(7) -0.0061(6) O(3) 0.0402(8) 0.062(1) 0.0246(6) -0.0091(7) 0.0199(6) -0.0072(7) O(4) 0.0522(9) 0.0367(8) 0.0228(6) 0.0192(7) 0.0179(6) 0.0020(6) N(1) 0.0201(6) 0.0211(6) 0.0212(6) -0.0015(5) 0.0109(5) -0.0017(5) C(1) 0.0207(7) 0.0180(7) 0.0199(6) -0.0016(5) 0.0111(6) -0.0003(5) C(2) 0.0232(7) 0.0210(8) 0.0306(8) 0.0022(6) 0.0164(7) 0.0031(6) C(3) 0.0192(7) 0.0277(9) 0.0332(9) 0.0011(6) 0.0110(7) 0.0042(7) C(4) 0.0247(8) 0.0264(8) 0.0234(8) -0.0034(6) 0.0067(7) -0.0015(6) C(5) 0.0263(8) 0.0245(8) 0.0236(7) -0.0010(6) 0.0124(7) -0.0047(6) C(6) 0.034(1) 0.039(1) 0.049(1) 0.0085(9) 0.0274(10) -0.0025(10) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[_s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2056 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0269 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0377 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.343 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.47 _refine_diff_density_max 0.30 #------------------------------------------------------------------------------ _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 Zn(1) O(1) 2.155(1) 1_555 1_555 yes Zn(1) O(1) 2.155(1) 1_555 2_755 yes Zn(1) O(4) 2.095(1) 1_555 1_555 yes Zn(1) O(4) 2.095(1) 1_555 2_755 yes Zn(1) N(1) 2.109(1) 1_555 1_555 yes Zn(1) N(1) 2.109(1) 1_555 2_755 yes S(1) O(1) 1.458(1) 1_555 1_555 yes S(1) O(2) 1.443(2) 1_555 1_555 yes S(1) O(3) 1.447(1) 1_555 1_555 yes S(1) C(1) 1.797(2) 1_555 1_555 yes N(1) C(1) 1.342(2) 1_555 1_555 yes N(1) C(5) 1.344(2) 1_555 1_555 yes C(1) C(2) 1.396(2) 1_555 1_555 yes C(2) C(3) 1.395(3) 1_555 1_555 yes C(2) C(6) 1.499(3) 1_555 1_555 yes C(3) C(4) 1.383(3) 1_555 1_555 yes C(4) C(5) 1.376(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 O(1) Zn(1) O(1) 97.76(9) 1_555 1_555 2_755 yes O(1) Zn(1) O(4) 172.05(7) 1_555 1_555 1_555 yes O(1) Zn(1) O(4) 89.47(6) 1_555 1_555 2_755 yes O(1) Zn(1) N(1) 79.90(5) 1_555 1_555 1_555 yes O(1) Zn(1) N(1) 85.75(5) 1_555 1_555 2_755 yes O(1) Zn(1) O(4) 89.47(6) 2_755 1_555 1_555 yes O(1) Zn(1) O(4) 172.05(7) 2_755 1_555 2_755 yes O(1) Zn(1) N(1) 85.75(5) 2_755 1_555 1_555 yes O(1) Zn(1) N(1) 79.90(5) 2_755 1_555 2_755 yes O(4) Zn(1) O(4) 83.51(9) 1_555 1_555 2_755 yes O(4) Zn(1) N(1) 97.45(6) 1_555 1_555 1_555 yes O(4) Zn(1) N(1) 98.83(6) 1_555 1_555 2_755 yes O(4) Zn(1) N(1) 98.83(6) 2_755 1_555 1_555 yes O(4) Zn(1) N(1) 97.45(6) 2_755 1_555 2_755 yes N(1) Zn(1) N(1) 158.12(8) 1_555 1_555 2_755 yes O(1) S(1) O(2) 113.07(10) 1_555 1_555 1_555 yes O(1) S(1) O(3) 112.69(10) 1_555 1_555 1_555 yes O(1) S(1) C(1) 104.82(8) 1_555 1_555 1_555 yes O(2) S(1) O(3) 113.7(1) 1_555 1_555 1_555 yes O(2) S(1) C(1) 105.33(8) 1_555 1_555 1_555 yes O(3) S(1) C(1) 106.33(8) 1_555 1_555 1_555 yes Zn(1) O(1) S(1) 120.37(7) 1_555 1_555 1_555 yes Zn(1) O(4) H(7) 120(2) 1_555 1_555 1_555 no Zn(1) O(4) H(8) 128(1) 1_555 1_555 1_555 no H(7) O(4) H(8) 106(2) 1_555 1_555 1_555 no Zn(1) N(1) C(1) 120.0(1) 1_555 1_555 1_555 yes Zn(1) N(1) C(5) 121.3(1) 1_555 1_555 1_555 yes C(1) N(1) C(5) 118.7(1) 1_555 1_555 1_555 yes S(1) C(1) N(1) 114.6(1) 1_555 1_555 1_555 yes S(1) C(1) C(2) 121.9(1) 1_555 1_555 1_555 yes N(1) C(1) C(2) 123.4(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 116.4(2) 1_555 1_555 1_555 yes C(1) C(2) C(6) 123.7(2) 1_555 1_555 1_555 yes C(3) C(2) C(6) 119.9(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.4(2) 1_555 1_555 1_555 yes C(2) C(3) H(1) 116(1) 1_555 1_555 1_555 no C(4) C(3) H(1) 123(1) 1_555 1_555 1_555 no C(3) C(4) C(5) 119.0(2) 1_555 1_555 1_555 yes C(3) C(4) H(2) 122(1) 1_555 1_555 1_555 no C(5) C(4) H(2) 118(1) 1_555 1_555 1_555 no N(1) C(5) C(4) 121.9(2) 1_555 1_555 1_555 yes N(1) C(5) H(3) 118(1) 1_555 1_555 1_555 no C(4) C(5) H(3) 119(1) 1_555 1_555 1_555 no C(2) C(6) H(4) 113(2) 1_555 1_555 1_555 no C(2) C(6) H(5) 112(2) 1_555 1_555 1_555 no C(2) C(6) H(6) 105(2) 1_555 1_555 1_555 no H(4) C(6) H(5) 108(3) 1_555 1_555 1_555 no H(4) C(6) H(6) 115(3) 1_555 1_555 1_555 no H(5) C(6) H(6) 99(3) 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 O(1) C(3) 3.386(2) 1_555 8_444 ? O(2) O(4) 2.818(2) 1_555 2_745 ? O(2) C(4) 3.399(3) 1_555 7_746 ? O(3) O(4) 2.723(2) 1_555 4_554 ? O(3) C(6) 3.513(3) 1_555 6_755 ? O(3) C(5) 3.557(2) 1_555 4_554 ? N(1) C(3) 3.520(2) 1_555 7_746 ? C(1) C(6) 3.405(3) 1_555 6_755 ? C(1) C(4) 3.471(2) 1_555 7_746 ? C(1) C(3) 3.595(2) 1_555 7_746 ? C(2) C(4) 3.320(3) 1_555 7_746 ? C(2) C(6) 3.456(3) 1_555 6_755 ? C(2) C(5) 3.502(3) 1_555 7_746 ? C(3) C(5) 3.485(3) 1_555 7_746 ? C(3) C(4) 3.585(3) 1_555 7_746 ? C(4) C(5) 3.354(3) 1_555 7_756 ? C(5) C(5) 3.576(4) 1_555 7_756 ? #------------------------------------------------------------------------------ _publ_requested_journal ' Chemical Communication ' _publ_contact_author ; Isamu Kinoshita Department of Molecular Materials Science, Graduate School of Science, Osaka City University, Sugimoto, Sumiyoshi-ku, Osaka 558-8585, JAPAN ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' +81-6-6605-3146 ' _publ_contact_author_fax ' +81-6-6690-2753 ' _publ_contact_author_email ' isamu@sci.osaka-cu.ac.jp ' loop_ _publ_author_name ' Kentaro Kimura ' ; _publ_author_address Department of Molecular Materials Science, Graduate School of Science, Osaka City University, Sugimoto, Sumiyoshi-ku, Osaka 558-8585, JAPAN ; _publ_section_title ; ENTER SECTION TITLE ; _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. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;