# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1387 data_(Cpd_1a) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 15 10:30:58 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ' DIRDIF92 (PATTY) ' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.310(2) _cell_length_b 8.339(2) _cell_length_c 17.935(3) _cell_angle_alpha 90 _cell_angle_beta 102.43(2) _cell_angle_gamma 90 _cell_volume 1505.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _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 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 354.67 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H15 N3 O4 Zn ' _chemical_formula_moiety 'C14 H15 N3 O4 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 728.00 _exptl_absorpt_coefficient_mu 1.652 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector IPDS _diffrn_measurement_device 'MAR IPDS' _diffrn_measurement_method 'omega scans with profile analysis' _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 2929 _reflns_number_total 2929 _reflns_number_observed 2326 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.56 _diffrn_reflns_reduction_process ? _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 C 0 56 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' N 0 12 0.006 0.003 'International Tables' O 0 16 0.011 0.006 'International Tables' Zn 0 4 0.284 1.430 'International Tables' #------------------------------------------------------------------------------ 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 Zn(1) 0.18644(3) 0.09947(4) 0.09443(2) 0.0376 Uij ? ? O(1) 0.0622(3) 0.0229(3) 0.1710(2) 0.0684 Uij ? ? O(2) 0.0168(3) 0.2397(3) 0.1056(1) 0.0749 Uij ? ? O(3) 0.3185(2) 0.2131(3) 0.1712(1) 0.0505 Uij ? ? O(4) 0.4799(3) 0.1375(3) 0.1173(2) 0.0696 Uij ? ? N(1) 0.1896(2) 0.1741(3) -0.0144(1) 0.0383 Uij ? ? N(2) 0.3337(2) -0.0369(3) -0.0330(1) 0.0421 Uij ? ? N(3) 0.2364(2) -0.1264(3) 0.0673(1) 0.0376 Uij ? ? C(1) -0.0048(3) 0.1469(4) 0.1557(2) 0.0497 Uij ? ? C(2) -0.1090(3) 0.1886(5) 0.1993(2) 0.0602 Uij ? ? C(3) 0.4392(3) 0.2129(3) 0.1664(2) 0.0418 Uij ? ? C(4) 0.5311(4) 0.3146(5) 0.2229(2) 0.0748 Uij ? ? C(5) 0.1234(3) 0.3090(4) -0.0422(2) 0.0477 Uij ? ? C(6) 0.1355(4) 0.3816(4) -0.1080(2) 0.0575 Uij ? ? C(7) 0.2218(4) 0.3150(4) -0.1494(2) 0.0576 Uij ? ? C(8) 0.2893(3) 0.1776(4) -0.1231(2) 0.0525 Uij ? ? C(9) 0.2691(3) 0.1069(3) -0.0556(2) 0.0395 Uij ? ? C(10) 0.3100(3) -0.1542(3) 0.0156(2) 0.0386 Uij ? ? C(11) 0.3657(3) -0.3068(4) 0.0089(2) 0.0516 Uij ? ? C(12) 0.3400(4) -0.4290(4) 0.0541(2) 0.0597 Uij ? ? C(13) 0.2585(4) -0.4020(3) 0.1054(2) 0.0543 Uij ? ? C(14) 0.2101(3) -0.2523(4) 0.1100(2) 0.0447 Uij ? ? H(1) 0.391(4) -0.068(4) -0.060(2) 0.0623 Uij ? ? H(2) -0.0864 0.2875 0.2253 0.0730 Uij ? ? H(3) -0.1924 0.1990 0.1648 0.0730 Uij ? ? H(4) -0.1135 0.1066 0.2352 0.0730 Uij ? ? H(5) 0.5298 0.2809 0.2732 0.0898 Uij ? ? H(6) 0.6187 0.3062 0.2145 0.0898 Uij ? ? H(7) 0.5031 0.4239 0.2166 0.0898 Uij ? ? H(8) 0.0649 0.3552 -0.0142 0.0576 Uij ? ? H(9) 0.0866 0.4759 -0.1251 0.0690 Uij ? ? H(10) 0.2338 0.3643 -0.1952 0.0700 Uij ? ? H(11) 0.3487 0.1307 -0.1505 0.0633 Uij ? ? H(12) 0.4201 -0.3241 -0.0268 0.0620 Uij ? ? H(13) 0.3779 -0.5320 0.0508 0.0715 Uij ? ? H(14) 0.2380 -0.4863 0.1368 0.0646 Uij ? ? H(15) 0.1543 -0.2341 0.1447 0.0533 Uij ? ? 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) 0.0413(2) 0.0392(3) 0.0369(2) 0.0050(1) 0.0182(2) -0.0007(1) O(1) 0.066(2) 0.053(1) 0.099(2) 0.005(1) 0.047(1) -0.008(1) O(2) 0.064(2) 0.108(2) 0.063(2) 0.030(1) 0.036(1) 0.028(1) O(3) 0.041(1) 0.063(1) 0.051(1) 0.0012(10) 0.0190(9) -0.0139(10) O(4) 0.059(2) 0.091(2) 0.070(2) -0.002(1) 0.038(1) -0.026(1) N(1) 0.038(1) 0.042(1) 0.037(1) 0.0042(10) 0.0134(10) 0.0013(9) N(2) 0.046(1) 0.045(1) 0.042(1) 0.006(1) 0.025(1) -0.002(1) N(3) 0.039(1) 0.039(1) 0.037(1) 0.0016(9) 0.014(1) -0.0028(9) C(1) 0.041(2) 0.066(2) 0.045(2) -0.004(1) 0.016(1) -0.020(2) C(2) 0.052(2) 0.076(2) 0.062(2) 0.000(2) 0.031(2) -0.013(2) C(3) 0.045(2) 0.045(2) 0.039(1) 0.007(1) 0.017(1) 0.005(1) C(4) 0.052(2) 0.102(3) 0.070(2) -0.007(2) 0.013(2) -0.026(2) C(5) 0.049(2) 0.048(2) 0.047(2) 0.006(1) 0.010(1) 0.001(1) C(6) 0.062(2) 0.056(2) 0.052(2) 0.003(1) 0.007(2) 0.011(1) C(7) 0.068(2) 0.062(2) 0.044(2) -0.011(2) 0.013(2) 0.012(1) C(8) 0.055(2) 0.066(2) 0.043(2) -0.009(2) 0.025(1) -0.002(2) C(9) 0.038(2) 0.047(2) 0.035(2) -0.005(1) 0.012(1) -0.002(1) C(10) 0.034(1) 0.045(2) 0.039(1) 0.004(1) 0.012(1) -0.005(1) C(11) 0.053(2) 0.049(2) 0.058(2) 0.012(1) 0.023(2) -0.006(1) C(12) 0.062(2) 0.044(2) 0.074(2) 0.015(1) 0.016(2) -0.004(2) C(13) 0.061(2) 0.041(2) 0.063(2) 0.001(1) 0.017(2) 0.006(1) C(14) 0.049(2) 0.045(2) 0.044(2) 0.003(1) 0.020(1) 0.006(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2326 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0557 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.935 _refine_ls_shift/esd_max 0.0220 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.73 _refine_diff_density_max 0.38 #------------------------------------------------------------------------------ _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) 2.166(2) ? ? yes Zn(1) O(2) 2.149(2) ? ? yes Zn(1) O(3) 1.960(2) ? ? yes Zn(1) N(1) 2.055(2) ? ? yes Zn(1) N(3) 2.039(2) ? ? yes O(1) C(1) 1.241(4) ? ? yes O(2) C(1) 1.242(4) ? ? yes O(3) C(3) 1.266(3) ? ? yes O(4) C(3) 1.228(3) ? ? yes N(1) C(5) 1.354(4) ? ? yes N(1) C(9) 1.339(4) ? ? yes N(2) C(9) 1.389(4) ? ? yes N(2) C(10) 1.368(4) ? ? yes N(3) C(10) 1.338(3) ? ? yes N(3) C(14) 1.362(4) ? ? yes C(1) C(2) 1.500(4) ? ? yes C(3) C(4) 1.493(5) ? ? yes C(5) C(6) 1.356(4) ? ? yes C(6) C(7) 1.390(5) ? ? yes C(7) C(8) 1.370(5) ? ? yes C(8) C(9) 1.401(4) ? ? yes C(10) C(11) 1.411(4) ? ? yes C(11) C(12) 1.363(5) ? ? yes C(12) C(13) 1.390(5) ? ? yes C(13) C(14) 1.353(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 O(1) Zn(1) O(2) 59.81(9) ? ? ? yes O(1) Zn(1) O(3) 96.51(10) ? ? ? yes O(1) Zn(1) N(1) 145.5(1) ? ? ? yes O(1) Zn(1) N(3) 95.36(9) ? ? ? yes O(2) Zn(1) O(3) 97.3(1) ? ? ? yes O(2) Zn(1) N(1) 95.93(9) ? ? ? yes O(2) Zn(1) N(3) 141.0(1) ? ? ? yes O(3) Zn(1) N(1) 111.72(9) ? ? ? yes O(3) Zn(1) N(3) 116.21(9) ? ? ? yes N(1) Zn(1) N(3) 89.78(9) ? ? ? yes Zn(1) O(1) C(1) 89.5(2) ? ? ? yes Zn(1) O(2) C(1) 90.2(2) ? ? ? yes Zn(1) O(3) C(3) 119.7(2) ? ? ? yes Zn(1) N(1) C(5) 119.4(2) ? ? ? yes Zn(1) N(1) C(9) 122.3(2) ? ? ? yes C(5) N(1) C(9) 117.6(2) ? ? ? yes C(9) N(2) C(10) 131.5(2) ? ? ? yes Zn(1) N(3) C(10) 122.4(2) ? ? ? yes Zn(1) N(3) C(14) 119.1(2) ? ? ? yes C(10) N(3) C(14) 117.8(2) ? ? ? yes O(1) C(1) O(2) 120.1(3) ? ? ? yes O(1) C(1) C(2) 120.3(3) ? ? ? yes O(2) C(1) C(2) 119.5(3) ? ? ? yes O(3) C(3) O(4) 122.8(3) ? ? ? yes O(3) C(3) C(4) 116.3(3) ? ? ? yes O(4) C(3) C(4) 120.8(3) ? ? ? yes N(1) C(5) C(6) 123.9(3) ? ? ? yes C(5) C(6) C(7) 118.4(3) ? ? ? yes C(6) C(7) C(8) 119.1(3) ? ? ? yes C(7) C(8) C(9) 119.4(3) ? ? ? yes N(1) C(9) N(2) 120.8(2) ? ? ? yes N(1) C(9) C(8) 121.5(3) ? ? ? yes N(2) C(9) C(8) 117.7(3) ? ? ? yes N(2) C(10) N(3) 121.6(2) ? ? ? yes N(2) C(10) C(11) 117.3(3) ? ? ? yes N(3) C(10) C(11) 121.1(3) ? ? ? yes C(10) C(11) C(12) 119.2(3) ? ? ? yes C(11) C(12) C(13) 119.7(3) ? ? ? yes C(12) C(13) C(14) 118.2(3) ? ? ? yes N(3) C(14) C(13) 123.8(3) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(Cpd_1b) #----------------------------------------------------------------------- _audit_creation_date 'Fri Jan 15 11:40:17 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ' DIRDIF92 (PATTY) ' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 7.439(2) _cell_length_b 8.669(2) _cell_length_c 9.409(2) _cell_angle_alpha 75.28(2) _cell_angle_beta 89.32(2) _cell_angle_gamma 86.11(2) _cell_volume 585.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 301.2 _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 'prism' _exptl_crystal_colour 'colourlessprism' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 307.49 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H9 Cl2 N3 Zn ' _chemical_formula_moiety 'C10 H9 Cl2 N3 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 308.00 _exptl_absorpt_coefficient_mu 2.526 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _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 2512 _reflns_number_total 2512 _reflns_number_observed 2291 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.92 _diffrn_reflns_reduction_process ? _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 C 0 20 0.003 0.002 'International Tables' H 0 18 0.000 0.000 'International Tables' N 0 6 0.006 0.003 'International Tables' Cl 0 4 0.148 0.159 'International Tables' Zn 0 2 0.284 1.430 'International Tables' #----------------------------------------------------------------------- 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 Zn(1) 0.25139(4) 0.19005(4) 0.15868(3) 0.0394 Uij ? ? Cl(1) 0.4769(1) 0.2822(1) 0.25466(10) 0.0551 Uij ? ? Cl(2) -0.0170(1) 0.30977(10) 0.19187(9) 0.0501 Uij ? ? N(1) 0.2906(3) 0.1878(3) -0.0540(2) 0.0382 Uij ? ? N(2) 0.2131(4) -0.0810(3) -0.0187(3) 0.0428 Uij ? ? N(3) 0.2286(4) -0.0488(3) 0.2238(2) 0.0394 Uij ? ? C(1) 0.3388(5) 0.3242(4) -0.1475(3) 0.0451 Uij ? ? C(2) 0.3541(5) 0.3429(4) -0.2965(4) 0.0526 Uij ? ? C(3) 0.3149(5) 0.2157(4) -0.3520(3) 0.0525 Uij ? ? C(4) 0.2677(5) 0.0752(4) -0.2591(3) 0.0462 Uij ? ? C(5) 0.2576(4) 0.0630(3) -0.1082(3) 0.0352 Uij ? ? C(6) 0.2051(4) -0.1415(3) 0.1318(3) 0.0350 Uij ? ? C(7) 0.1666(5) -0.3026(4) 0.1837(3) 0.0441 Uij ? ? C(8) 0.1562(5) -0.3673(4) 0.3331(4) 0.0500 Uij ? ? C(9) 0.1829(5) -0.2724(4) 0.4288(3) 0.0539 Uij ? ? C(10) 0.2200(5) -0.1184(4) 0.3714(3) 0.0511 Uij ? ? H(1) 0.124(6) -0.133(5) -0.087(4) 0.0641 Uij ? ? H(2) 0.3632 0.4115 -0.1085 0.0541 Uij ? ? H(3) 0.3905 0.4398 -0.3592 0.0630 Uij ? ? H(4) 0.3204 0.2258 -0.4549 0.0629 Uij ? ? H(5) 0.2420 -0.0128 -0.2969 0.0554 Uij ? ? H(6) 0.1482 -0.3658 0.1168 0.0528 Uij ? ? H(7) 0.1308 -0.4761 0.3704 0.0600 Uij ? ? H(8) 0.1753 -0.3146 0.5321 0.0645 Uij ? ? H(9) 0.2410 -0.0547 0.4373 0.0612 Uij ? ? 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) 0.0480(3) 0.0367(2) 0.0388(2) -0.0105(2) 0.0025(2) -0.0174(2) Cl(1) 0.0541(5) 0.0546(5) 0.0654(5) -0.0145(4) -0.0063(4) -0.0280(4) Cl(2) 0.0495(5) 0.0516(5) 0.0584(5) -0.0074(3) 0.0065(3) -0.0299(4) N(1) 0.043(1) 0.036(1) 0.038(1) -0.0083(9) 0.0043(9) -0.0124(9) N(2) 0.061(2) 0.036(1) 0.035(1) -0.011(1) 0.0005(10) -0.0130(9) N(3) 0.049(1) 0.036(1) 0.035(1) -0.0075(10) -0.0019(9) -0.0108(9) C(1) 0.055(2) 0.036(1) 0.045(1) -0.011(1) 0.003(1) -0.009(1) C(2) 0.062(2) 0.044(2) 0.048(2) -0.008(1) 0.011(1) -0.004(1) C(3) 0.068(2) 0.052(2) 0.037(1) -0.005(2) 0.007(1) -0.009(1) C(4) 0.063(2) 0.044(2) 0.036(1) -0.005(1) 0.006(1) -0.016(1) C(5) 0.037(1) 0.035(1) 0.036(1) -0.0041(10) 0.0013(9) -0.0127(10) C(6) 0.038(1) 0.033(1) 0.036(1) -0.0046(10) -0.0038(9) -0.011(1) C(7) 0.057(2) 0.033(1) 0.044(1) -0.009(1) -0.002(1) -0.010(1) C(8) 0.060(2) 0.037(2) 0.051(2) -0.010(1) 0.000(1) -0.005(1) C(9) 0.070(2) 0.051(2) 0.037(1) -0.008(2) 0.001(1) -0.003(1) C(10) 0.074(2) 0.046(2) 0.036(1) -0.011(1) 0.002(1) -0.015(1) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2291 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0492 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0659 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.946 _refine_ls_shift/esd_max 0.0300 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.45 _refine_diff_density_max 0.53 #----------------------------------------------------------------------- _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) Cl(1) 2.2029(9) ? ? yes Zn(1) Cl(2) 2.243(1) ? ? yes Zn(1) N(1) 2.023(2) ? ? yes Zn(1) N(3) 2.023(2) ? ? yes N(1) C(1) 1.350(4) ? ? yes N(1) C(5) 1.346(3) ? ? yes N(2) C(5) 1.375(4) ? ? yes N(2) C(6) 1.382(3) ? ? yes N(3) C(6) 1.342(3) ? ? yes N(3) C(10) 1.369(4) ? ? yes C(1) C(2) 1.373(4) ? ? yes C(2) C(3) 1.383(5) ? ? yes C(3) C(4) 1.372(4) ? ? yes C(4) C(5) 1.399(4) ? ? yes C(6) C(7) 1.406(4) ? ? yes C(7) C(8) 1.378(4) ? ? yes C(8) C(9) 1.390(5) ? ? yes C(9) C(10) 1.353(5) ? ? 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 Cl(1) Zn(1) Cl(2) 113.14(4) ? ? ? yes Cl(1) Zn(1) N(1) 113.36(7) ? ? ? yes Cl(1) Zn(1) N(3) 116.26(8) ? ? ? yes Cl(2) Zn(1) N(1) 111.79(7) ? ? ? yes Cl(2) Zn(1) N(3) 107.56(8) ? ? ? yes N(1) Zn(1) N(3) 93.08(9) ? ? ? yes Zn(1) N(1) C(1) 117.4(2) ? ? ? yes Zn(1) N(1) C(5) 123.6(2) ? ? ? yes C(1) N(1) C(5) 118.8(2) ? ? ? yes C(5) N(2) C(6) 133.8(2) ? ? ? yes Zn(1) N(3) C(6) 124.2(2) ? ? ? yes Zn(1) N(3) C(10) 118.0(2) ? ? ? yes C(6) N(3) C(10) 117.5(2) ? ? ? yes N(1) C(1) C(2) 123.2(3) ? ? ? yes C(1) C(2) C(3) 117.7(3) ? ? ? yes C(2) C(3) C(4) 120.2(3) ? ? ? yes C(3) C(4) C(5) 119.2(3) ? ? ? yes N(1) C(5) N(2) 121.9(2) ? ? ? yes N(1) C(5) C(4) 120.8(3) ? ? ? yes N(2) C(5) C(4) 117.3(3) ? ? ? yes N(2) C(6) N(3) 121.2(2) ? ? ? yes N(2) C(6) C(7) 117.1(2) ? ? ? yes N(3) C(6) C(7) 121.7(2) ? ? ? yes C(6) C(7) C(8) 118.9(3) ? ? ? yes C(7) C(8) C(9) 119.6(3) ? ? ? yes C(8) C(9) C(10) 118.4(3) ? ? ? yes N(3) C(10) C(9) 123.9(3) ? ? ? yes #----------------------------------------------------------------------- _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(Cpd_1d) #----------------------------------------------------------------------- _audit_creation_date 'Fri Jan 15 11:43:12 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ' DIRDIF92 (PATTY) ' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 8.637(2) _cell_length_b 11.018(2) _cell_length_c 12.138(2) _cell_angle_alpha 86.55(2) _cell_angle_beta 86.59(2) _cell_angle_gamma 80.74(2) _cell_volume 1136.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 301.2 _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 'prism' _exptl_crystal_colour 'colourlessprism' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 482.97 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H23 N3 S2 Zn ' _chemical_formula_moiety 'C24 H23 N3 S2 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 500.00 _exptl_absorpt_coefficient_mu 1.280 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _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 4950 _reflns_number_total 4950 _reflns_number_observed 4108 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 28.01 _diffrn_reflns_reduction_process ? _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 C 0 48 0.003 0.002 'International Tables' H 0 46 0.000 0.000 'International Tables' N 0 6 0.006 0.003 'International Tables' S 0 4 0.125 0.123 'International Tables' Zn 0 2 0.284 1.430 'International Tables' #----------------------------------------------------------------------- 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 Zn(1) 0.13978(3) 0.08808(3) 0.28686(2) 0.0377 Uij ? ? S(1) -0.07261(7) 0.00700(6) 0.24106(7) 0.0456 Uij ? ? S(2) 0.10386(8) 0.25760(7) 0.38943(7) 0.0531 Uij ? ? N(1) 0.3089(2) -0.0369(2) 0.3613(2) 0.0364 Uij ? ? N(2) 0.5210(2) 0.0289(2) 0.2528(2) 0.0426 Uij ? ? N(3) 0.2964(2) 0.1056(2) 0.1527(2) 0.0385 Uij ? ? C(1) 0.2611(3) -0.1060(3) 0.4489(2) 0.0443 Uij ? ? C(2) 0.3617(3) -0.1789(3) 0.5167(3) 0.0494 Uij ? ? C(3) 0.5223(3) -0.1823(2) 0.4940(3) 0.0459 Uij ? ? C(4) 0.5741(3) -0.1156(2) 0.4058(2) 0.0417 Uij ? ? C(5) 0.4642(3) -0.0417(2) 0.3394(2) 0.0342 Uij ? ? C(6) 0.4534(3) 0.0876(2) 0.1593(2) 0.0367 Uij ? ? C(7) 0.5508(3) 0.1263(3) 0.0747(3) 0.0476 Uij ? ? C(8) 0.4877(4) 0.1810(3) -0.0212(3) 0.0523 Uij ? ? C(9) 0.3262(4) 0.1974(3) -0.0294(3) 0.0539 Uij ? ? C(10) 0.2366(3) 0.1592(3) 0.0574(2) 0.0472 Uij ? ? C(11) 0.0102(3) -0.1437(2) 0.2008(2) 0.0386 Uij ? ? C(12) -0.0071(3) -0.2469(3) 0.2713(2) 0.0490 Uij ? ? C(13) 0.0472(4) -0.3640(3) 0.2360(3) 0.0553 Uij ? ? C(14) 0.1213(3) -0.3847(3) 0.1339(3) 0.0487 Uij ? ? C(15) 0.1413(3) -0.2809(3) 0.0648(2) 0.0479 Uij ? ? C(16) 0.0860(3) -0.1637(3) 0.0991(2) 0.0441 Uij ? ? C(17) 0.1786(5) -0.5133(3) 0.0966(3) 0.0725 Uij ? ? C(18) -0.0793(3) 0.3452(2) 0.3562(2) 0.0382 Uij ? ? C(19) -0.1561(3) 0.4265(2) 0.4330(2) 0.0439 Uij ? ? C(20) -0.2978(4) 0.4991(3) 0.4111(3) 0.0506 Uij ? ? C(21) -0.3688(4) 0.4944(3) 0.3128(3) 0.0531 Uij ? ? C(22) -0.2928(4) 0.4121(3) 0.2370(2) 0.0542 Uij ? ? C(23) -0.1498(3) 0.3404(3) 0.2579(2) 0.0463 Uij ? ? C(24) -0.5248(5) 0.5720(4) 0.2896(4) 0.0919 Uij ? ? H(1) 0.622(4) 0.023(3) 0.251(3) 0.0663 Uij ? ? H(2) 0.1514 -0.1034 0.4641 0.0532 Uij ? ? H(3) 0.3235 -0.2260 0.5774 0.0593 Uij ? ? H(4) 0.5956 -0.2312 0.5403 0.0551 Uij ? ? H(5) 0.6835 -0.1187 0.3891 0.0501 Uij ? ? H(6) 0.6610 0.1151 0.0825 0.0571 Uij ? ? H(7) 0.5536 0.2071 -0.0804 0.0628 Uij ? ? H(8) 0.2792 0.2345 -0.0945 0.0647 Uij ? ? H(9) 0.1261 0.1706 0.0512 0.0567 Uij ? ? H(10) -0.0560 -0.2363 0.3430 0.0588 Uij ? ? H(11) 0.0328 -0.4328 0.2843 0.0664 Uij ? ? H(12) 0.1933 -0.2913 -0.0061 0.0575 Uij ? ? H(13) 0.1009 -0.0948 0.0510 0.0530 Uij ? ? H(14) 0.0923 -0.5569 0.0963 0.0869 Uij ? ? H(15) 0.2263 -0.5088 0.0243 0.0869 Uij ? ? H(16) 0.2533 -0.5550 0.1459 0.0869 Uij ? ? H(17) -0.1103 0.4319 0.5014 0.0527 Uij ? ? H(18) -0.3476 0.5536 0.4649 0.0607 Uij ? ? H(19) -0.3401 0.4050 0.1695 0.0650 Uij ? ? H(20) -0.0992 0.2868 0.2036 0.0556 Uij ? ? H(21) -0.5159 0.6567 0.2918 0.1103 Uij ? ? H(22) -0.5550 0.5561 0.2186 0.1103 Uij ? ? H(23) -0.6019 0.5523 0.3439 0.1103 Uij ? ? 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) 0.0235(2) 0.0428(2) 0.0455(2) -0.0013(1) -0.0011(1) -0.0046(1) S(1) 0.0226(3) 0.0456(4) 0.0685(5) -0.0029(2) -0.0033(3) -0.0080(3) S(2) 0.0367(4) 0.0586(5) 0.0636(5) 0.0047(3) -0.0124(3) -0.0220(3) N(1) 0.0242(9) 0.039(1) 0.046(1) -0.0048(8) -0.0028(8) -0.0006(8) N(2) 0.0239(9) 0.059(1) 0.044(1) -0.0079(9) -0.0019(9) 0.0030(10) N(3) 0.0283(10) 0.045(1) 0.042(1) -0.0033(8) -0.0017(9) -0.0026(9) C(1) 0.033(1) 0.050(1) 0.051(2) -0.012(1) 0.001(1) 0.001(1) C(2) 0.048(2) 0.046(1) 0.055(2) -0.013(1) -0.006(1) 0.007(1) C(3) 0.039(1) 0.039(1) 0.059(2) -0.003(1) -0.012(1) 0.002(1) C(4) 0.027(1) 0.044(1) 0.053(1) 0.0005(10) -0.004(1) -0.007(1) C(5) 0.025(1) 0.037(1) 0.040(1) -0.0026(9) -0.0014(9) -0.0059(9) C(6) 0.029(1) 0.040(1) 0.041(1) -0.0041(9) 0.000(1) -0.0054(10) C(7) 0.035(1) 0.058(2) 0.050(2) -0.011(1) 0.000(1) 0.001(1) C(8) 0.050(2) 0.060(2) 0.047(2) -0.013(1) 0.005(1) 0.008(1) C(9) 0.055(2) 0.057(2) 0.048(2) -0.004(1) -0.010(1) 0.005(1) C(10) 0.036(1) 0.057(2) 0.047(1) 0.001(1) -0.006(1) -0.003(1) C(11) 0.024(1) 0.043(1) 0.048(1) -0.0062(9) -0.004(1) -0.001(1) C(12) 0.049(2) 0.050(2) 0.046(1) -0.006(1) 0.008(1) 0.005(1) C(13) 0.063(2) 0.046(2) 0.056(2) -0.010(1) 0.004(2) 0.006(1) C(14) 0.044(1) 0.044(1) 0.059(2) -0.008(1) -0.005(1) -0.007(1) C(15) 0.045(1) 0.057(2) 0.043(1) -0.013(1) 0.002(1) -0.006(1) C(16) 0.041(1) 0.047(1) 0.044(1) -0.011(1) -0.001(1) 0.005(1) C(17) 0.083(3) 0.055(2) 0.080(2) -0.006(2) -0.004(2) -0.018(2) C(18) 0.034(1) 0.035(1) 0.046(1) -0.0058(10) 0.000(1) -0.0038(10) C(19) 0.045(1) 0.041(1) 0.046(1) -0.005(1) -0.002(1) -0.012(1) C(20) 0.051(2) 0.044(1) 0.054(2) 0.004(1) -0.001(1) -0.014(1) C(21) 0.048(2) 0.053(2) 0.054(2) 0.007(1) -0.003(1) -0.007(1) C(22) 0.056(2) 0.060(2) 0.043(1) 0.005(1) -0.010(1) -0.007(1) C(23) 0.048(2) 0.048(1) 0.040(1) 0.002(1) 0.000(1) -0.009(1) C(24) 0.083(3) 0.097(3) 0.082(3) 0.043(2) -0.025(2) -0.023(2) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4108 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0423 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0642 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.634 _refine_ls_shift/esd_max 0.0390 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.65 _refine_diff_density_max 0.41 #----------------------------------------------------------------------- _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) S(1) 2.2761(8) ? ? yes Zn(1) S(2) 2.2764(8) ? ? yes Zn(1) N(1) 2.051(2) ? ? yes Zn(1) N(3) 2.074(2) ? ? yes S(1) C(11) 1.784(3) ? ? yes S(2) C(18) 1.770(3) ? ? yes N(1) C(1) 1.353(3) ? ? yes N(1) C(5) 1.345(3) ? ? yes N(2) C(5) 1.384(3) ? ? yes N(2) C(6) 1.384(3) ? ? yes N(3) C(6) 1.344(3) ? ? yes N(3) C(10) 1.358(3) ? ? yes C(1) C(2) 1.363(4) ? ? yes C(2) C(3) 1.393(4) ? ? yes C(3) C(4) 1.356(4) ? ? yes C(4) C(5) 1.406(3) ? ? yes C(6) C(7) 1.380(4) ? ? yes C(7) C(8) 1.378(4) ? ? yes C(8) C(9) 1.386(4) ? ? yes C(9) C(10) 1.357(4) ? ? yes C(11) C(12) 1.403(4) ? ? yes C(11) C(16) 1.375(4) ? ? yes C(12) C(13) 1.384(4) ? ? yes C(13) C(14) 1.375(4) ? ? yes C(14) C(15) 1.404(4) ? ? yes C(14) C(17) 1.510(4) ? ? yes C(15) C(16) 1.383(4) ? ? yes C(18) C(19) 1.395(4) ? ? yes C(18) C(23) 1.380(4) ? ? yes C(19) C(20) 1.381(4) ? ? yes C(20) C(21) 1.380(4) ? ? yes C(21) C(22) 1.391(4) ? ? yes C(21) C(24) 1.508(4) ? ? yes C(22) C(23) 1.383(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) Zn(1) S(2) 119.52(3) ? ? ? yes S(1) Zn(1) N(1) 114.08(6) ? ? ? yes S(1) Zn(1) N(3) 112.25(7) ? ? ? yes S(2) Zn(1) N(1) 106.19(7) ? ? ? yes S(2) Zn(1) N(3) 111.45(7) ? ? ? yes N(1) Zn(1) N(3) 89.18(8) ? ? ? yes Zn(1) S(1) C(11) 103.43(8) ? ? ? yes Zn(1) S(2) C(18) 107.12(9) ? ? ? yes Zn(1) N(1) C(1) 117.0(2) ? ? ? yes Zn(1) N(1) C(5) 124.2(2) ? ? ? yes C(1) N(1) C(5) 118.1(2) ? ? ? yes C(5) N(2) C(6) 132.6(2) ? ? ? yes Zn(1) N(3) C(6) 124.0(2) ? ? ? yes Zn(1) N(3) C(10) 117.4(2) ? ? ? yes C(6) N(3) C(10) 117.5(2) ? ? ? yes N(1) C(1) C(2) 123.6(2) ? ? ? yes C(1) C(2) C(3) 117.9(3) ? ? ? yes C(2) C(3) C(4) 120.0(2) ? ? ? yes C(3) C(4) C(5) 119.3(2) ? ? ? yes N(1) C(5) N(2) 121.1(2) ? ? ? yes N(1) C(5) C(4) 121.1(2) ? ? ? yes N(2) C(5) C(4) 117.8(2) ? ? ? yes N(2) C(6) N(3) 119.9(2) ? ? ? yes N(2) C(6) C(7) 118.3(2) ? ? ? yes N(3) C(6) C(7) 121.7(2) ? ? ? yes C(6) C(7) C(8) 119.8(3) ? ? ? yes C(7) C(8) C(9) 118.7(3) ? ? ? yes C(8) C(9) C(10) 118.6(3) ? ? ? yes N(3) C(10) C(9) 123.6(3) ? ? ? yes S(1) C(11) C(12) 120.2(2) ? ? ? yes S(1) C(11) C(16) 121.9(2) ? ? ? yes C(12) C(11) C(16) 117.9(3) ? ? ? yes C(11) C(12) C(13) 119.8(3) ? ? ? yes C(12) C(13) C(14) 122.7(3) ? ? ? yes C(13) C(14) C(15) 117.2(3) ? ? ? yes C(13) C(14) C(17) 121.8(3) ? ? ? yes C(15) C(14) C(17) 121.0(3) ? ? ? yes C(14) C(15) C(16) 120.5(3) ? ? ? yes C(11) C(16) C(15) 122.0(2) ? ? ? yes S(2) C(18) C(19) 118.2(2) ? ? ? yes S(2) C(18) C(23) 124.1(2) ? ? ? yes C(19) C(18) C(23) 117.6(2) ? ? ? yes C(18) C(19) C(20) 121.0(3) ? ? ? yes C(19) C(20) C(21) 121.5(3) ? ? ? yes C(20) C(21) C(22) 117.3(3) ? ? ? yes C(20) C(21) C(24) 121.5(3) ? ? ? yes C(22) C(21) C(24) 121.1(3) ? ? ? yes C(21) C(22) C(23) 121.4(3) ? ? ? yes C(18) C(23) C(22) 121.1(2) ? ? ? yes #----------------------------------------------------------------------- _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(Cpd_2) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 15 10:29:26 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 16.393(3) _cell_length_b 8.897(2) _cell_length_c 19.610(3) _cell_angle_alpha 90 _cell_angle_beta 103.05(2) _cell_angle_gamma 90 _cell_volume 2786.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _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 2/c' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourlessprism' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 705.91 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H18 F6 N6 O6 S2 Zn ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1424.00 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector IPDS _diffrn_measurement_device 'MAR IPDS' _diffrn_measurement_method 'omega scans with profile analysis' _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 2573 _reflns_number_total 2573 _reflns_number_observed 2097 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.58 _diffrn_reflns_reduction_process ? _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 Zn 0 4 0.284 1.430 'International Tables' O 0 24 0.011 0.006 'International Tables' N 0 24 0.006 0.003 'International Tables' C 0 88 0.003 0.002 'International Tables' H 0 72 0.000 0.000 'International Tables' F 0 24 0.017 0.010 'International Tables' S 0 8 0.125 0.123 'International Tables' #------------------------------------------------------------------------------ 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 Zn(1) 0.5000 -0.00090(6) 0.2500 0.0500 Uij ? ? S(1) 0.34190(6) -0.1575(1) 0.38185(5) 0.0488 Uij ? ? F(1) 0.2457(2) -0.3884(3) 0.3404(2) 0.1053 Uij ? ? F(2) 0.1918(2) -0.2205(4) 0.3958(2) 0.0986 Uij ? ? F(3) 0.2879(2) -0.3701(4) 0.4515(2) 0.1072 Uij ? ? O(1) 0.4144(2) -0.2493(4) 0.3835(2) 0.0664 Uij ? ? O(2) 0.3485(2) -0.0588(4) 0.4411(2) 0.0697 Uij ? ? O(3) 0.3065(2) -0.0890(4) 0.3166(2) 0.0822 Uij ? ? N(1) 0.5763(2) -0.1268(3) 0.3191(1) 0.0442 Uij ? ? N(2) 0.5634(2) 0.0246(3) 0.4159(2) 0.0479 Uij ? ? N(3) 0.4695(2) 0.1392(3) 0.3201(2) 0.0548 Uij ? ? C(1) 0.6079(3) -0.2540(5) 0.2960(2) 0.0607 Uij ? ? C(2) 0.6553(3) -0.3540(6) 0.3389(2) 0.0763 Uij ? ? C(3) 0.6722(3) -0.3260(5) 0.4112(3) 0.0719 Uij ? ? C(4) 0.6409(3) -0.2002(5) 0.4353(2) 0.0593 Uij ? ? C(5) 0.5924(2) -0.1025(4) 0.3891(2) 0.0433 Uij ? ? C(6) 0.5077(2) 0.1351(4) 0.3886(2) 0.0449 Uij ? ? C(7) 0.4931(3) 0.2481(5) 0.4355(2) 0.0649 Uij ? ? C(8) 0.4391(4) 0.3637(6) 0.4069(3) 0.0881 Uij ? ? C(9) 0.3947(4) 0.3570(7) 0.3388(3) 0.1035 Uij ? ? C(10) 0.4140(3) 0.2475(6) 0.2983(3) 0.0851 Uij ? ? C(11) 0.2632(3) -0.2910(5) 0.3935(3) 0.0649 Uij ? ? H(1) 0.581(3) 0.040(5) 0.456(3) 0.0794 Uij ? ? H(2) 0.5950 -0.2738 0.2472 0.0717 Uij ? ? H(3) 0.6768 -0.4413 0.3211 0.0930 Uij ? ? H(4) 0.7050 -0.3946 0.4429 0.0863 Uij ? ? H(5) 0.6536 -0.1804 0.4842 0.0716 Uij ? ? H(6) 0.5196 0.2443 0.4841 0.0737 Uij ? ? H(7) 0.4307 0.4457 0.4357 0.0936 Uij ? ? H(8) 0.3529 0.4296 0.3202 0.1046 Uij ? ? H(9) 0.3867 0.2477 0.2501 0.0896 Uij ? ? 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) 0.0648(5) 0.0364(4) 0.0435(5) 0.0000 0.0013(3) 0.0000 S(1) 0.0506(6) 0.0475(6) 0.0487(6) 0.0011(4) 0.0119(4) -0.0067(4) F(1) 0.086(2) 0.079(2) 0.143(3) -0.014(2) 0.007(2) -0.051(2) F(2) 0.053(2) 0.092(2) 0.159(3) 0.001(1) 0.040(2) -0.010(2) F(3) 0.122(3) 0.083(2) 0.130(3) 0.005(2) 0.058(2) 0.035(2) O(1) 0.050(2) 0.073(2) 0.076(2) 0.011(1) 0.013(1) -0.011(1) O(2) 0.071(2) 0.065(2) 0.069(2) -0.001(2) 0.007(1) -0.023(2) O(3) 0.115(3) 0.072(2) 0.059(2) 0.027(2) 0.018(2) 0.013(1) N(1) 0.050(2) 0.036(2) 0.047(2) 0.001(1) 0.012(1) 0.000(1) N(2) 0.054(2) 0.042(2) 0.043(2) 0.002(1) -0.001(1) -0.008(1) N(3) 0.060(2) 0.044(2) 0.056(2) 0.008(1) 0.005(1) 0.003(1) C(1) 0.069(3) 0.058(3) 0.058(3) 0.012(2) 0.020(2) -0.004(2) C(2) 0.101(4) 0.066(3) 0.062(3) 0.042(3) 0.019(2) 0.003(2) C(3) 0.080(3) 0.061(3) 0.066(3) 0.030(2) -0.002(2) -0.005(2) C(4) 0.061(3) 0.055(2) 0.054(2) 0.009(2) -0.002(2) 0.001(2) C(5) 0.040(2) 0.041(2) 0.048(2) -0.002(1) 0.007(1) 0.001(1) C(6) 0.046(2) 0.036(2) 0.053(2) 0.000(1) 0.011(2) -0.004(1) C(7) 0.074(3) 0.052(2) 0.066(3) 0.011(2) 0.011(2) -0.011(2) C(8) 0.111(4) 0.069(3) 0.080(4) 0.040(3) 0.011(3) -0.017(2) C(9) 0.127(5) 0.082(4) 0.099(4) 0.058(3) 0.023(3) 0.010(3) C(10) 0.104(4) 0.081(3) 0.062(3) 0.041(3) 0.001(2) -0.001(2) C(11) 0.057(3) 0.058(3) 0.083(3) 0.002(2) 0.021(2) 0.000(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2097 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0543 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0824 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.900 _refine_ls_shift/esd_max 3.1960 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.76 _refine_diff_density_max 0.47 #------------------------------------------------------------------------------ _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) N(1) 1.972(3) ? ? yes Zn(1) N(1) 1.972(3) ? ? yes Zn(1) N(3) 2.001(3) ? ? yes Zn(1) N(3) 2.001(3) ? ? yes S(1) O(1) 1.436(3) ? ? yes S(1) O(2) 1.441(3) ? ? yes S(1) O(3) 1.417(3) ? ? yes S(1) C(11) 1.805(4) ? ? yes F(1) C(11) 1.335(5) ? ? yes F(2) C(11) 1.339(5) ? ? yes F(3) C(11) 1.320(5) ? ? yes N(1) C(1) 1.363(5) ? ? yes N(1) C(5) 1.356(4) ? ? yes N(2) C(5) 1.376(4) ? ? yes N(2) C(6) 1.366(4) ? ? yes N(3) C(6) 1.349(4) ? ? yes N(3) C(10) 1.328(5) ? ? yes C(1) C(2) 1.344(6) ? ? yes C(2) C(3) 1.403(7) ? ? yes C(3) C(4) 1.360(6) ? ? yes C(4) C(5) 1.373(5) ? ? yes C(6) C(7) 1.418(5) ? ? yes C(7) C(8) 1.390(6) ? ? yes C(8) C(9) 1.369(8) ? ? yes C(9) C(10) 1.339(7) ? ? 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 N(1) Zn(1) N(1) 110.8(2) ? ? ? yes N(1) Zn(1) N(3) 95.8(1) ? ? ? yes N(1) Zn(1) N(3) 127.4(1) ? ? ? yes N(1) Zn(1) N(3) 127.4(1) ? ? ? yes N(1) Zn(1) N(3) 95.8(1) ? ? ? yes N(3) Zn(1) N(3) 102.9(2) ? ? ? yes O(1) S(1) O(2) 114.7(2) ? ? ? yes O(1) S(1) O(3) 115.6(2) ? ? ? yes O(1) S(1) C(11) 103.5(2) ? ? ? yes O(2) S(1) O(3) 114.0(2) ? ? ? yes O(2) S(1) C(11) 103.0(2) ? ? ? yes O(3) S(1) C(11) 103.8(2) ? ? ? yes Zn(1) N(1) C(1) 118.3(3) ? ? ? yes Zn(1) N(1) C(5) 123.6(2) ? ? ? yes C(1) N(1) C(5) 117.8(3) ? ? ? yes C(5) N(2) C(6) 134.4(3) ? ? ? yes Zn(1) N(3) C(6) 122.4(2) ? ? ? yes Zn(1) N(3) C(10) 119.4(3) ? ? ? yes C(6) N(3) C(10) 118.1(3) ? ? ? yes N(1) C(1) C(2) 123.5(4) ? ? ? yes C(1) C(2) C(3) 118.0(4) ? ? ? yes C(2) C(3) C(4) 119.5(4) ? ? ? yes C(3) C(4) C(5) 120.0(4) ? ? ? yes N(1) C(5) N(2) 120.9(3) ? ? ? yes N(1) C(5) C(4) 121.2(3) ? ? ? yes N(2) C(5) C(4) 117.9(3) ? ? ? yes N(2) C(6) N(3) 121.9(3) ? ? ? yes N(2) C(6) C(7) 116.9(3) ? ? ? yes N(3) C(6) C(7) 121.2(3) ? ? ? yes C(6) C(7) C(8) 116.6(4) ? ? ? yes C(7) C(8) C(9) 120.7(4) ? ? ? yes C(8) C(9) C(10) 117.7(5) ? ? ? yes N(3) C(10) C(9) 124.9(5) ? ? ? yes S(1) C(11) F(1) 111.3(3) ? ? ? yes S(1) C(11) F(2) 110.6(3) ? ? ? yes S(1) C(11) F(3) 111.8(3) ? ? ? yes F(1) C(11) F(2) 107.1(4) ? ? ? yes F(1) C(11) F(3) 107.2(4) ? ? ? yes F(2) C(11) F(3) 108.7(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(Cpd_3a) #----------------------------------------------------------------------- _audit_creation_date 'Fri Jan 15 10:33:25 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ' DIRDIF92 (PATTY) ' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 9.662(2) _cell_length_b 8.016(2) _cell_length_c 24.566(4) _cell_angle_alpha 90 _cell_angle_beta 92.16(2) _cell_angle_gamma 90 _cell_volume 1901.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _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 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 446.77 _chemical_formula_analytical ? _chemical_formula_sum 'C19 H19 N5 O4 Zn ' _chemical_formula_moiety 'C19 H19 N5 O4 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 920.00 _exptl_absorpt_coefficient_mu 1.330 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _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 3749 _reflns_number_total 3749 _reflns_number_observed 2791 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.57 _diffrn_reflns_reduction_process ? _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 C 0 76 0.003 0.002 'International Tables' H 0 76 0.000 0.000 'International Tables' N 0 20 0.006 0.003 'International Tables' O 0 16 0.011 0.006 'International Tables' Zn 0 4 0.284 1.430 'International Tables' #----------------------------------------------------------------------- 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 Zn(1) 0.21155(3) 0.21385(4) 0.37929(1) 0.0380 Uij ? ? O(1) 0.3733(2) 0.0721(3) 0.40986(8) 0.0487 Uij ? ? O(2) 0.2231(3) -0.0696(3) 0.45719(9) 0.0576 Uij ? ? O(3) 0.3125(3) 0.4454(3) 0.36250(8) 0.0529 Uij ? ? O(4) 0.1002(3) 0.4579(3) 0.32732(10) 0.0571 Uij ? ? N(1) 0.1651(3) 0.3105(3) 0.45520(9) 0.0389 Uij ? ? N(2) -0.0454(3) 0.1642(3) 0.46058(9) 0.0423 Uij ? ? N(3) 0.0088(2) 0.1134(3) 0.36720(8) 0.0348 Uij ? ? N(4) 0.0394(3) 0.0563(3) 0.27228(10) 0.0460 Uij ? ? N(5) 0.2653(3) 0.1270(3) 0.30206(9) 0.0420 Uij ? ? C(1) 0.3411(3) -0.0478(4) 0.4407(1) 0.0402 Uij ? ? C(2) 0.4542(4) -0.1713(5) 0.4557(1) 0.0580 Uij ? ? C(3) 0.2131(3) 0.5261(4) 0.3400(1) 0.0419 Uij ? ? C(4) 0.2306(5) 0.7078(4) 0.3292(1) 0.0586 Uij ? ? C(5) 0.2611(4) 0.4089(4) 0.4805(1) 0.0487 Uij ? ? C(6) 0.2529(4) 0.4616(5) 0.5335(1) 0.0591 Uij ? ? C(7) 0.1404(4) 0.4106(5) 0.5622(1) 0.0614 Uij ? ? C(8) 0.0432(4) 0.3097(4) 0.5383(1) 0.0517 Uij ? ? C(9) 0.0571(3) 0.2624(4) 0.4835(1) 0.0398 Uij ? ? C(10) -0.0816(3) 0.1106(3) 0.4084(1) 0.0391 Uij ? ? C(11) -0.2162(4) 0.0513(5) 0.4018(1) 0.0553 Uij ? ? C(12) -0.2610(4) -0.0112(5) 0.3523(1) 0.0611 Uij ? ? C(13) -0.1718(4) -0.0107(5) 0.3102(1) 0.0538 Uij ? ? C(14) -0.0399(3) 0.0545(3) 0.3182(1) 0.0377 Uij ? ? C(15) 0.1784(3) 0.0676(4) 0.2639(1) 0.0403 Uij ? ? C(16) 0.2249(4) 0.0118(5) 0.2131(1) 0.0581 Uij ? ? C(17) 0.3613(4) 0.0228(6) 0.2035(1) 0.0701 Uij ? ? C(18) 0.4536(4) 0.0850(6) 0.2435(2) 0.0731 Uij ? ? C(19) 0.4004(4) 0.1352(5) 0.2911(1) 0.0571 Uij ? ? H(1) -0.104(4) 0.140(5) 0.483(1) 0.0651 Uij ? ? H(2) -0.023(4) 0.030(5) 0.242(1) 0.0651 Uij ? ? H(3) 0.4187 -0.2546 0.4789 0.0697 Uij ? ? H(4) 0.4863 -0.2222 0.4236 0.0697 Uij ? ? H(5) 0.5287 -0.1150 0.4741 0.0697 Uij ? ? H(6) 0.3210 0.7416 0.3410 0.0704 Uij ? ? H(7) 0.2180 0.7283 0.2912 0.0704 Uij ? ? H(8) 0.1639 0.7691 0.3484 0.0704 Uij ? ? H(9) 0.3383 0.4437 0.4606 0.0586 Uij ? ? H(10) 0.3226 0.5308 0.5498 0.0711 Uij ? ? H(11) 0.1311 0.4464 0.5988 0.0737 Uij ? ? H(12) -0.0330 0.2714 0.5582 0.0620 Uij ? ? H(13) -0.2767 0.0539 0.4314 0.0664 Uij ? ? H(14) -0.3523 -0.0542 0.3472 0.0733 Uij ? ? H(15) -0.2003 -0.0548 0.2757 0.0647 Uij ? ? H(16) 0.1615 -0.0324 0.1864 0.0697 Uij ? ? H(17) 0.3944 -0.0121 0.1694 0.0843 Uij ? ? H(18) 0.5501 0.0922 0.2377 0.0879 Uij ? ? H(19) 0.4625 0.1788 0.3185 0.0685 Uij ? ? 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) 0.0378(2) 0.0385(2) 0.0380(2) -0.0028(1) 0.0068(1) 0.0016(1) O(1) 0.047(1) 0.051(1) 0.049(1) 0.004(1) 0.0095(10) 0.0163(10) O(2) 0.047(1) 0.064(1) 0.063(1) -0.001(1) 0.017(1) 0.012(1) O(3) 0.059(2) 0.050(1) 0.049(1) 0.001(1) 0.001(1) 0.0086(10) O(4) 0.059(2) 0.052(1) 0.060(1) -0.003(1) 0.000(1) 0.009(1) N(1) 0.041(1) 0.039(1) 0.036(1) 0.000(1) 0.004(1) 0.0028(10) N(2) 0.043(2) 0.049(1) 0.036(1) -0.007(1) 0.011(1) 0.000(1) N(3) 0.036(1) 0.035(1) 0.034(1) -0.0009(10) 0.0025(9) 0.0049(9) N(4) 0.044(2) 0.060(2) 0.034(1) -0.002(1) 0.003(1) 0.000(1) N(5) 0.042(1) 0.044(1) 0.041(1) 0.000(1) 0.008(1) 0.000(1) C(1) 0.044(2) 0.043(2) 0.034(1) -0.002(1) 0.003(1) 0.001(1) C(2) 0.054(2) 0.055(2) 0.065(2) 0.001(2) -0.004(2) 0.017(2) C(3) 0.056(2) 0.040(2) 0.031(1) 0.002(1) 0.010(1) 0.004(1) C(4) 0.084(3) 0.041(2) 0.052(2) 0.001(2) 0.006(2) 0.004(1) C(5) 0.052(2) 0.049(2) 0.045(2) -0.006(1) 0.000(1) 0.001(1) C(6) 0.064(3) 0.060(2) 0.052(2) -0.009(2) -0.005(2) -0.011(2) C(7) 0.078(3) 0.072(2) 0.034(2) -0.003(2) -0.001(2) -0.007(2) C(8) 0.059(2) 0.060(2) 0.037(2) 0.003(2) 0.009(1) 0.001(1) C(9) 0.046(2) 0.038(1) 0.036(1) 0.005(1) 0.006(1) 0.003(1) C(10) 0.038(2) 0.040(1) 0.040(1) 0.000(1) 0.007(1) 0.004(1) C(11) 0.045(2) 0.073(2) 0.049(2) -0.013(2) 0.012(1) 0.002(2) C(12) 0.041(2) 0.084(3) 0.059(2) -0.019(2) 0.003(1) 0.003(2) C(13) 0.052(2) 0.064(2) 0.045(2) -0.012(2) -0.002(1) 0.000(2) C(14) 0.040(2) 0.038(1) 0.036(1) 0.001(1) 0.003(1) 0.007(1) C(15) 0.044(2) 0.041(1) 0.035(1) 0.006(1) 0.006(1) 0.010(1) C(16) 0.065(2) 0.073(2) 0.036(2) 0.010(2) 0.007(1) 0.002(2) C(17) 0.069(3) 0.099(3) 0.043(2) 0.018(2) 0.021(2) 0.004(2) C(18) 0.047(2) 0.109(3) 0.065(2) 0.007(2) 0.019(2) 0.006(2) C(19) 0.042(2) 0.076(2) 0.054(2) 0.001(2) 0.013(1) 0.001(2) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2791 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0395 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0541 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.530 _refine_ls_shift/esd_max 1.2850 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.63 _refine_diff_density_max 0.46 #----------------------------------------------------------------------- _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) 2.052(2) ? ? yes Zn(1) O(3) 2.144(2) ? ? yes Zn(1) N(1) 2.083(2) ? ? yes Zn(1) N(3) 2.129(2) ? ? yes Zn(1) N(5) 2.104(2) ? ? yes O(1) C(1) 1.269(4) ? ? yes O(2) C(1) 1.237(4) ? ? yes O(3) C(3) 1.267(4) ? ? yes O(4) C(3) 1.250(4) ? ? yes N(1) C(5) 1.352(4) ? ? yes N(1) C(9) 1.332(4) ? ? yes N(2) C(9) 1.369(4) ? ? yes N(2) C(10) 1.384(4) ? ? yes N(3) C(10) 1.362(4) ? ? yes N(3) C(14) 1.360(4) ? ? yes N(4) C(14) 1.388(4) ? ? yes N(4) C(15) 1.369(4) ? ? yes N(5) C(15) 1.323(4) ? ? yes N(5) C(19) 1.344(4) ? ? yes C(1) C(2) 1.510(4) ? ? yes C(3) C(4) 1.491(4) ? ? yes C(5) C(6) 1.372(5) ? ? yes C(6) C(7) 1.380(5) ? ? yes C(7) C(8) 1.357(5) ? ? yes C(8) C(9) 1.411(4) ? ? yes C(10) C(11) 1.389(4) ? ? yes C(11) C(12) 1.370(5) ? ? yes C(12) C(13) 1.371(5) ? ? yes C(13) C(14) 1.385(4) ? ? yes C(15) C(16) 1.416(4) ? ? yes C(16) C(17) 1.350(5) ? ? yes C(17) C(18) 1.396(6) ? ? yes C(18) C(19) 1.356(5) ? ? 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(3) 101.77(9) ? ? ? yes O(1) Zn(1) N(1) 93.73(9) ? ? ? yes O(1) Zn(1) N(3) 121.73(9) ? ? ? yes O(1) Zn(1) N(5) 86.34(9) ? ? ? yes O(3) Zn(1) N(1) 88.01(9) ? ? ? yes O(3) Zn(1) N(3) 136.36(9) ? ? ? yes O(3) Zn(1) N(5) 89.04(9) ? ? ? yes N(1) Zn(1) N(3) 92.14(9) ? ? ? yes N(1) Zn(1) N(5) 177.00(9) ? ? ? yes N(3) Zn(1) N(5) 90.37(9) ? ? ? yes Zn(1) O(1) C(1) 115.9(2) ? ? ? yes Zn(1) O(3) C(3) 100.6(2) ? ? ? yes Zn(1) N(1) C(5) 117.6(2) ? ? ? yes Zn(1) N(1) C(9) 123.9(2) ? ? ? yes C(5) N(1) C(9) 117.8(3) ? ? ? yes C(9) N(2) C(10) 135.4(2) ? ? ? yes Zn(1) N(3) C(10) 121.0(2) ? ? ? yes Zn(1) N(3) C(14) 122.7(2) ? ? ? yes C(10) N(3) C(14) 116.2(2) ? ? ? yes C(14) N(4) C(15) 134.2(3) ? ? ? yes Zn(1) N(5) C(15) 125.8(2) ? ? ? yes Zn(1) N(5) C(19) 116.0(2) ? ? ? yes C(15) N(5) C(19) 118.2(3) ? ? ? yes O(1) C(1) O(2) 123.5(3) ? ? ? yes O(1) C(1) C(2) 116.8(3) ? ? ? yes O(2) C(1) C(2) 119.6(3) ? ? ? yes O(3) C(3) O(4) 121.7(3) ? ? ? yes O(3) C(3) C(4) 119.2(3) ? ? ? yes O(4) C(3) C(4) 119.1(3) ? ? ? yes N(1) C(5) C(6) 123.6(3) ? ? ? yes C(5) C(6) C(7) 117.9(3) ? ? ? yes C(6) C(7) C(8) 120.0(3) ? ? ? yes C(7) C(8) C(9) 119.0(3) ? ? ? yes N(1) C(9) N(2) 121.4(2) ? ? ? yes N(1) C(9) C(8) 121.7(3) ? ? ? yes N(2) C(9) C(8) 117.0(3) ? ? ? yes N(2) C(10) N(3) 122.5(3) ? ? ? yes N(2) C(10) C(11) 114.7(3) ? ? ? yes N(3) C(10) C(11) 122.8(3) ? ? ? yes C(10) C(11) C(12) 119.5(3) ? ? ? yes C(11) C(12) C(13) 118.8(3) ? ? ? yes C(12) C(13) C(14) 119.7(3) ? ? ? yes N(3) C(14) N(4) 122.2(3) ? ? ? yes N(3) C(14) C(13) 122.9(3) ? ? ? yes N(4) C(14) C(13) 114.9(3) ? ? ? yes N(4) C(15) N(5) 121.2(3) ? ? ? yes N(4) C(15) C(16) 117.2(3) ? ? ? yes N(5) C(15) C(16) 121.6(3) ? ? ? yes C(15) C(16) C(17) 118.6(3) ? ? ? yes C(16) C(17) C(18) 120.1(3) ? ? ? yes C(17) C(18) C(19) 117.5(4) ? ? ? yes N(5) C(19) C(18) 124.1(3) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_(Cpd_3b) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 15 11:38:32 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ' DIRDIF92 (PATTY) ' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 7.519(2) _cell_length_b 17.202(2) _cell_length_c 12.869(2) _cell_angle_alpha 90 _cell_angle_beta 103.96(1) _cell_angle_gamma 90 _cell_volume 1615.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 41.5 _cell_measurement_theta_max 47.0 #------------------------------------------------------------------------------ _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' ' 1/2+x,1/2+y, +z' ' -x, +y,1/2-z' ' 1/2-x,1/2+y,1/2-z' ' -x, -y, -z' ' 1/2-x,1/2-y, -z' ' +x, -y,1/2+z' ' 1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 399.59 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H13 Cl2 N5 Zn ' _chemical_formula_moiety 'C15 H13 Cl2 N5 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 808.00 _exptl_absorpt_coefficient_mu 1.856 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.755 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -1.85 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 1787 _reflns_number_total 1656 _reflns_number_observed 1367 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 26.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.13019 _diffrn_orient_matrix_UB_12 0.01815 _diffrn_orient_matrix_UB_13 0.01901 _diffrn_orient_matrix_UB_21 -0.04278 _diffrn_orient_matrix_UB_22 0.05522 _diffrn_orient_matrix_UB_23 -0.00678 _diffrn_orient_matrix_UB_31 -0.00151 _diffrn_orient_matrix_UB_32 0.00038 _diffrn_orient_matrix_UB_33 0.07748 #------------------------------------------------------------------------------ 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 60 0.003 0.002 'International Tables' H 0 52 0.000 0.000 'International Tables' N 0 20 0.006 0.003 'International Tables' Cl 0 8 0.148 0.159 'International Tables' Zn 0 4 0.284 1.430 'International Tables' #------------------------------------------------------------------------------ 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 Zn(1) 0.0000 0.08794(2) 0.2500 0.0378 Uij ? ? Cl(1) 0.17365(8) 0.15160(3) 0.14753(4) 0.0519 Uij ? ? N(1) 0.0000 -0.0341(1) 0.2500 0.0341 Uij ? ? N(2) 0.2225(2) 0.08467(10) 0.3880(1) 0.0440 Uij ? ? N(3) 0.1377(3) -0.0382(1) 0.4377(1) 0.0443 Uij ? ? C(1) 0.0000 -0.1964(2) 0.2500 0.0494 Uij ? ? C(2) 0.0686(3) -0.1563(1) 0.3432(2) 0.0456 Uij ? ? C(3) 0.0682(3) -0.0756(1) 0.3406(2) 0.0369 Uij ? ? C(4) 0.2347(3) 0.0305(1) 0.4624(2) 0.0398 Uij ? ? C(5) 0.3416(3) 0.0397(1) 0.5672(2) 0.0510 Uij ? ? C(6) 0.4378(4) 0.1074(2) 0.5925(2) 0.0609 Uij ? ? C(7) 0.4277(4) 0.1644(2) 0.5159(2) 0.0640 Uij ? ? C(8) 0.3198(4) 0.1511(1) 0.4156(2) 0.0577 Uij ? ? H(1) 0.152(4) -0.067(2) 0.484(2) 0.0692 Uij ? ? H(2) 0.0000 -0.2519 0.2500 0.0593 Uij ? ? H(3) 0.1162 -0.1833 0.4084 0.0550 Uij ? ? H(4) 0.3467 0.0000 0.6189 0.0610 Uij ? ? H(5) 0.5120 0.1149 0.6626 0.0729 Uij ? ? H(6) 0.4938 0.2116 0.5325 0.0770 Uij ? ? H(7) 0.3132 0.1902 0.3627 0.0692 Uij ? ? 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) 0.0460(2) 0.0318(2) 0.0323(2) 0.0000 0.0028(1) 0.0000 Cl(1) 0.0663(4) 0.0503(3) 0.0384(3) -0.0143(3) 0.0113(3) -0.0027(2) N(1) 0.036(1) 0.032(1) 0.033(1) 0.0000 0.0053(9) 0.0000 N(2) 0.048(1) 0.042(1) 0.0378(10) -0.0058(8) 0.0016(8) 0.0004(8) N(3) 0.058(1) 0.0385(10) 0.0317(9) 0.0004(8) 0.0024(8) 0.0041(7) C(1) 0.055(2) 0.033(2) 0.057(2) 0.0000 0.009(2) 0.0000 C(2) 0.054(1) 0.037(1) 0.043(1) 0.0024(10) 0.0063(10) 0.0074(9) C(3) 0.037(1) 0.036(1) 0.036(1) 0.0020(8) 0.0062(8) 0.0015(8) C(4) 0.039(1) 0.043(1) 0.036(1) 0.0045(9) 0.0055(8) -0.0034(9) C(5) 0.054(1) 0.062(2) 0.033(1) -0.001(1) 0.0030(10) -0.001(1) C(6) 0.056(1) 0.083(2) 0.039(1) -0.013(1) 0.002(1) -0.014(1) C(7) 0.063(2) 0.069(2) 0.054(1) -0.023(1) 0.003(1) -0.012(1) C(8) 0.066(2) 0.053(1) 0.049(1) -0.016(1) 0.003(1) -0.003(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1367 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0220 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0300 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.605 _refine_ls_shift/esd_max 0.0240 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.20 _refine_diff_density_max 0.32 #------------------------------------------------------------------------------ _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) Cl(1) 2.3397(6) ? ? yes Zn(1) Cl(1) 2.3397(6) ? ? yes Zn(1) N(1) 2.099(2) ? ? yes Zn(1) N(2) 2.126(2) ? ? yes Zn(1) N(2) 2.126(2) ? ? yes N(1) C(3) 1.358(2) ? ? yes N(1) C(3) 1.358(2) ? ? yes N(2) C(4) 1.324(3) ? ? yes N(2) C(8) 1.357(3) ? ? yes N(3) C(3) 1.391(3) ? ? yes N(3) C(4) 1.385(3) ? ? yes C(1) C(2) 1.371(3) ? ? yes C(1) C(2) 1.371(3) ? ? yes C(2) C(3) 1.388(3) ? ? yes C(4) C(5) 1.403(3) ? ? yes C(5) C(6) 1.369(3) ? ? yes C(6) C(7) 1.379(4) ? ? yes C(7) C(8) 1.368(3) ? ? 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 Cl(1) Zn(1) Cl(1) 124.18(3) ? ? ? yes Cl(1) Zn(1) N(1) 117.91(2) ? ? ? yes Cl(1) Zn(1) N(2) 92.84(5) ? ? ? yes Cl(1) Zn(1) N(2) 88.57(5) ? ? ? yes Cl(1) Zn(1) N(1) 117.91(2) ? ? ? yes Cl(1) Zn(1) N(2) 88.57(5) ? ? ? yes Cl(1) Zn(1) N(2) 92.84(5) ? ? ? yes N(1) Zn(1) N(2) 88.49(5) ? ? ? yes N(1) Zn(1) N(2) 88.49(5) ? ? ? yes N(2) Zn(1) N(2) 176.98(9) ? ? ? yes Zn(1) N(1) C(3) 121.7(1) ? ? ? yes Zn(1) N(1) C(3) 121.7(1) ? ? ? yes C(3) N(1) C(3) 116.5(2) ? ? ? yes Zn(1) N(2) C(4) 121.7(1) ? ? ? yes Zn(1) N(2) C(8) 117.5(1) ? ? ? yes C(4) N(2) C(8) 117.7(2) ? ? ? yes C(3) N(3) C(4) 131.6(2) ? ? ? yes C(2) C(1) C(2) 119.6(3) ? ? ? yes C(1) C(2) C(3) 118.9(2) ? ? ? yes N(1) C(3) N(3) 120.7(2) ? ? ? yes N(1) C(3) C(2) 123.0(2) ? ? ? yes N(3) C(3) C(2) 116.3(2) ? ? ? yes N(2) C(4) N(3) 119.6(2) ? ? ? yes N(2) C(4) C(5) 122.7(2) ? ? ? yes N(3) C(4) C(5) 117.7(2) ? ? ? yes C(4) C(5) C(6) 118.2(2) ? ? ? yes C(5) C(6) C(7) 120.0(2) ? ? ? yes C(6) C(7) C(8) 118.2(2) ? ? ? yes N(2) C(8) C(7) 123.2(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _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 (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;