# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/110 data_wong544_HLKWONG025_Zn_4_Au #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 24 17:10:21 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 'SIR88' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 14.646(2) _cell_length_b 8.597(2) _cell_length_c 10.128(2) _cell_angle_alpha 90 _cell_angle_beta 105.45(1) _cell_angle_gamma 90 _cell_volume 1229.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.0 _cell_measurement_theta_max 16.6 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2 ' _symmetry_Int_Tables_number 5 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y, -z' ' -x, +y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_meas ? _chemical_formula_weight 492.79 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H32 Cl2 N2 O2 Zn ' _chemical_formula_moiety 'C22 H32 Cl2 N2 O2 Zn ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 516.00 _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.943 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _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/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_decay_% -0.95 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -2 -2 -3 -1 -2 4 -2 -2 _diffrn_reflns_number 1822 _reflns_number_total 870 _reflns_number_observed 1546 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 3.83 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 22.49 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.01322 _diffrn_orient_matrix_UB_12 0.00912 _diffrn_orient_matrix_UB_13 -0.09160 _diffrn_orient_matrix_UB_21 0.06355 _diffrn_orient_matrix_UB_22 -0.04883 _diffrn_orient_matrix_UB_23 0.03804 _diffrn_orient_matrix_UB_31 -0.02836 _diffrn_orient_matrix_UB_32 -0.10518 _diffrn_orient_matrix_UB_33 -0.02560 #------------------------------------------------------------------------------ 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 2 0.284 1.430 'International Tables' Cl 0 4 0.148 0.159 'International Tables' O 0 4 0.011 0.006 'International Tables' N 0 4 0.006 0.003 'International Tables' C 0 44 0.003 0.002 'International Tables' H 0 64 0.000 0.000 '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 -0.0148 0.0000 0.0650(2) Uij ? ? Cl(1) 0.0639(1) -0.1520(2) -0.1341(2) 0.1622(8) Uij ? ? O(1) -0.1953(2) -0.0171(5) -0.4206(2) 0.0539(7) Uij ? ? N(1) -0.0752(2) 0.1677(4) -0.1123(3) 0.0310(9) Uij ? ? C(1) -0.0367(3) 0.3072(4) -0.0658(3) 0.0357(10) Uij ? ? C(2) -0.0660(3) 0.4424(4) -0.1399(4) 0.044(1) Uij ? ? C(3) -0.1360(3) 0.4314(5) -0.2630(4) 0.054(1) Uij ? ? C(4) -0.1730(3) 0.2902(5) -0.3092(4) 0.051(1) Uij ? ? C(5) -0.1438(3) 0.1578(5) -0.2318(4) 0.0380(10) Uij ? ? C(6) -0.1853(2) 0.0014(6) -0.2760(3) 0.0410(9) Uij ? ? C(7) -0.1068(3) -0.0337(8) -0.4547(4) 0.067(1) Uij ? ? C(8) -0.2836(3) -0.0331(7) -0.2506(4) 0.052(1) Uij ? ? C(9) -0.2803(3) 0.0121(8) -0.1027(3) 0.064(2) Uij ? ? C(10) -0.3630(3) 0.0573(7) -0.3491(4) 0.073(2) Uij ? ? C(11) -0.3010(4) -0.2127(6) -0.2688(6) 0.085(2) Uij ? ? H(1) -0.0385 0.5395 -0.1062 0.0552 Uij ? ? H(2) -0.1574 0.5215 -0.3153 0.0670 Uij ? ? H(3) -0.2199 0.2820 -0.3940 0.0597 Uij ? ? H(4) -0.1418 -0.0755 -0.2294 0.0490 Uij ? ? H(5) -0.1183 -0.0427 -0.5513 0.0822 Uij ? ? H(6) -0.0755 -0.1249 -0.4122 0.0822 Uij ? ? H(7) -0.0683 0.0544 -0.4235 0.0822 Uij ? ? H(8) -0.2655 0.1199 -0.0894 0.0767 Uij ? ? H(9) -0.2333 -0.0472 -0.0406 0.0767 Uij ? ? H(10) -0.3404 -0.0069 -0.0867 0.0767 Uij ? ? H(11) -0.3522 0.1659 -0.3350 0.0890 Uij ? ? H(12) -0.4221 0.0307 -0.3334 0.0890 Uij ? ? H(13) -0.3641 0.0324 -0.4412 0.0890 Uij ? ? H(14) -0.3613 -0.2365 -0.2548 0.1001 Uij ? ? H(15) -0.2531 -0.2669 -0.2052 0.1001 Uij ? ? H(16) -0.3011 -0.2413 -0.3597 0.1001 Uij ? ? Cl(1*) -0.0639(1) -0.1520(2) 0.1341(2) 0.1622(8) Uij ? ? N(1*) 0.0752(2) 0.1677(4) 0.1123(3) 0.0310(9) Uij ? ? C(1*) 0.0367(3) 0.3072(4) 0.0658(3) 0.0357(10) Uij ? ? C(5*) 0.1438(3) 0.1578(5) 0.2319(4) 0.0380(10) Uij ? ? C(2*) 0.0660(3) 0.4424(4) 0.1399(4) 0.044(1) Uij ? ? C(4*) 0.1730(3) 0.2902(5) 0.3092(4) 0.051(1) Uij ? ? C(6*) 0.1853(2) 0.0014(6) 0.2760(3) 0.0410(9) Uij ? ? C(3*) 0.1360(3) 0.4314(5) 0.2630(4) 0.054(1) Uij ? ? H(1*) 0.0385 0.5395 0.1062 0.0552 Uij ? ? H(3*) 0.2199 0.2820 0.3940 0.0597 Uij ? ? O(1*) 0.1953(2) -0.0171(5) 0.4206(2) 0.0539(7) Uij ? ? C(8*) 0.2836(3) -0.0331(7) 0.2506(4) 0.052(1) Uij ? ? H(4*) 0.1418 -0.0755 0.2294 0.0490 Uij ? ? H(2*) 0.1574 0.5215 0.3153 0.0670 Uij ? ? C(7*) 0.1068(3) -0.0337(8) 0.4547(4) 0.067(1) Uij ? ? C(9*) 0.2803(3) 0.0121(8) 0.1027(3) 0.064(2) Uij ? ? C(10*) 0.3630(3) 0.0573(7) 0.3491(4) 0.073(2) Uij ? ? C(11*) 0.3010(4) -0.2127(6) 0.2688(6) 0.085(2) Uij ? ? H(5*) 0.1183 -0.0427 0.5513 0.0822 Uij ? ? H(6*) 0.0755 -0.1249 0.4122 0.0822 Uij ? ? H(7*) 0.0683 0.0544 0.4235 0.0822 Uij ? ? H(8*) 0.2655 0.1199 0.0894 0.0767 Uij ? ? H(9*) 0.2333 -0.0472 0.0407 0.0767 Uij ? ? H(10*) 0.3404 -0.0069 0.0867 0.0767 Uij ? ? H(11*) 0.3522 0.1659 0.3350 0.0890 Uij ? ? H(12*) 0.4221 0.0307 0.3334 0.0890 Uij ? ? H(13*) 0.3641 0.0324 0.4412 0.0890 Uij ? ? H(14*) 0.3613 -0.2365 0.2548 0.1001 Uij ? ? H(15*) 0.2531 -0.2669 0.2052 0.1001 Uij ? ? H(16*) 0.3011 -0.2413 0.3597 0.1001 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) 0.0741(5) 0.0306(3) 0.0649(4) 0.0000 -0.0257(4) 0.0000 Cl(1) 0.116(1) 0.156(2) 0.164(2) 0.086(1) -0.051(1) -0.116(2) O(1) 0.048(1) 0.076(2) 0.035(1) -0.006(2) 0.007(1) -0.020(2) N(1) 0.046(2) 0.023(2) 0.027(2) 0.000(1) 0.014(1) -0.008(1) C(1) 0.042(2) 0.030(2) 0.034(2) 0.004(2) 0.008(2) -0.005(1) C(2) 0.055(3) 0.033(2) 0.047(2) 0.006(2) 0.017(2) 0.003(2) C(3) 0.060(3) 0.054(2) 0.047(2) 0.022(2) 0.012(2) 0.016(2) C(4) 0.060(3) 0.059(2) 0.030(2) 0.015(2) 0.005(2) 0.008(2) C(5) 0.041(2) 0.045(2) 0.029(2) 0.002(2) 0.011(1) -0.005(2) C(6) 0.043(2) 0.041(2) 0.033(1) 0.011(2) 0.001(2) -0.002(2) C(7) 0.056(2) 0.093(4) 0.058(2) -0.007(4) 0.025(2) -0.024(3) C(8) 0.044(2) 0.066(2) 0.048(2) 0.002(2) 0.016(2) -0.010(2) C(9) 0.052(2) 0.103(5) 0.043(2) -0.001(3) 0.020(2) 0.003(3) C(10) 0.041(3) 0.120(5) 0.054(3) 0.008(3) 0.006(2) 0.007(3) C(11) 0.081(4) 0.070(3) 0.114(4) -0.022(3) 0.044(3) -0.020(4) Cl(1*) 0.116(1) 0.156(2) 0.164(2) -0.086(1) -0.051(1) 0.116(2) N(1*) 0.046(2) 0.023(2) 0.027(2) 0.000(1) 0.014(1) 0.008(1) C(1*) 0.042(2) 0.030(2) 0.034(2) -0.004(2) 0.008(2) 0.005(1) C(5*) 0.041(2) 0.045(2) 0.029(2) -0.002(2) 0.011(1) 0.005(2) C(2*) 0.055(3) 0.033(2) 0.047(2) -0.006(2) 0.017(2) -0.003(2) C(4*) 0.060(3) 0.059(2) 0.030(2) -0.015(2) 0.005(2) -0.008(2) C(6*) 0.043(2) 0.041(2) 0.033(1) -0.011(2) 0.001(2) 0.002(2) C(3*) 0.060(3) 0.054(2) 0.047(2) -0.022(2) 0.012(2) -0.016(2) O(1*) 0.048(1) 0.076(2) 0.035(1) 0.006(2) 0.007(1) 0.020(2) C(8*) 0.044(2) 0.066(2) 0.048(2) -0.002(2) 0.016(2) 0.010(2) C(7*) 0.056(2) 0.093(4) 0.058(2) 0.007(4) 0.025(2) 0.024(3) C(9*) 0.052(2) 0.103(5) 0.043(2) 0.001(3) 0.020(2) -0.003(3) C(10*) 0.041(3) 0.120(5) 0.054(3) -0.008(3) 0.006(2) -0.007(3) C(11*) 0.081(4) 0.070(3) 0.114(4) 0.022(3) 0.044(3) 0.020(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1546 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0505 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0508 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.550 _refine_ls_shift/esd_max 8.1083 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.44 _refine_diff_density_max 0.54 #------------------------------------------------------------------------------ _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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(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 ; #===================End of data============================