# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1370 data_SB-9 # Complex 1 #------------------------------------------------------------------------------ _audit_creation_date '1999-01-24' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' ENTER CONTACT NAME HERE' _publ_contact_author_address ; 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_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). 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. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 8.103(1) _cell_length_b 13.576(2) _cell_length_c 13.987(2) _cell_angle_alpha 111.59(1) _cell_angle_beta 105.18(1) _cell_angle_gamma 95.82(1) _cell_volume 1346.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.7 _cell_measurement_theta_max 17.4 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1294.62 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H64 Br2 Cl2 N10 O10 S2 Zn2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 662.00 _exptl_absorpt_coefficient_mu 2.617 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.915 _exptl_special_details ; The scan width was (0.80+0.34tan\q)\% with an \w scan speed of 4\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.48 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 1 0 0 2 1 1 0 2 _diffrn_reflns_number 5143 _reflns_number_total 4774 _reflns_number_gt 3415 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01303 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01226 _diffrn_orient_matrix_UB_12 -0.07505 _diffrn_orient_matrix_UB_13 -0.05478 _diffrn_orient_matrix_UB_21 -0.00015 _diffrn_orient_matrix_UB_22 0.02905 _diffrn_orient_matrix_UB_23 -0.05615 _diffrn_orient_matrix_UB_31 0.13052 _diffrn_orient_matrix_UB_32 0.01095 _diffrn_orient_matrix_UB_33 0.02118 #------------------------------------------------------------------------------ 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 42 0.002 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) ; Br 0 2 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 2 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 10 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 10 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 2 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Zn 0 2 0.222 1.431 ;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_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Br(1) 0.91240(6) 0.02793(4) 0.69352(4) 0.0565(2) 1.000 . Uani d ? Zn(1) 0.70026(5) 0.13322(3) 0.76154(3) 0.0304(1) 1.000 . Uani d ? Cl(1) 0.7167(2) 0.4511(1) 0.2126(1) 0.0768(5) 1.000 . Uani d ? S(01) 0.2056(8) 0.3214(4) 0.3812(3) 0.115(1) 0.500 D Uani d ? S(01') 0.2649(7) 0.3534(4) 0.4404(5) 0.143(3) 0.500 D Uani d ? O(01) 0.3769(7) 0.3039(4) 0.4267(6) 0.161(3) 1.000 D Uani d ? O(11) 0.8061(6) 0.5611(3) 0.2596(4) 0.136(2) 1.000 D Uiso d ? O(12) 0.5417(7) 0.4576(6) 0.2296(7) 0.102(3) 0.500 D Uiso d ? O(12') 0.840(1) 0.3885(7) 0.1831(9) 0.199(6) 0.500 D Uiso d ? O(13) 0.704(2) 0.3974(8) 0.1186(5) 0.35(1) 0.500 D Uiso d ? O(13') 0.655(2) 0.4264(8) 0.2799(7) 0.222(7) 0.500 D Uiso d ? O(14) 0.8027(9) 0.4063(5) 0.2873(6) 0.088(2) 0.500 D Uiso d ? O(14') 0.589(1) 0.4352(7) 0.1164(5) 0.132(4) 0.500 D Uiso d ? N(1) 0.5821(4) 0.1466(3) 0.6039(2) 0.0377(8) 1.000 . Uani d ? N(2) 0.4719(4) 0.2052(2) 0.7932(3) 0.0368(8) 1.000 . Uani d ? N(3) 0.8065(4) 0.3079(2) 0.8133(3) 0.0398(8) 1.000 . Uani d ? N(4) 0.5429(4) 0.0105(2) 0.7815(2) 0.0325(8) 1.000 . Uani d ? N(5) 0.8927(4) 0.1885(3) 0.9262(2) 0.0374(8) 1.000 . Uani d ? C(1) 0.4134(5) 0.1816(3) 0.6028(3) 0.046(1) 1.000 . Uani d ? C(01) 0.238(1) 0.4740(5) 0.4351(6) 0.123(3) 1.000 D Uani d ? C(2) 0.3387(5) 0.1618(3) 0.6842(3) 0.042(1) 1.000 . Uani d ? C(02) 0.0624(9) 0.3004(6) 0.4504(6) 0.123(3) 1.000 D Uani d ? C(3) 0.5196(6) 0.3263(3) 0.8436(4) 0.048(1) 1.000 . Uani d ? C(4) 0.7169(6) 0.3675(3) 0.8898(3) 0.048(1) 1.000 . Uani d ? C(5) 0.7719(6) 0.3351(3) 0.7170(3) 0.050(1) 1.000 . Uani d ? C(6) 0.7228(6) 0.2323(3) 0.6111(3) 0.048(1) 1.000 . Uani d ? C(7) 0.4183(5) 0.1614(3) 0.8651(3) 0.044(1) 1.000 . Uani d ? C(8) 0.4246(5) 0.0424(3) 0.8304(3) 0.038(1) 1.000 . Uani d ? C(9) 0.3142(6) -0.0278(4) 0.8476(4) 0.051(1) 1.000 . Uani d ? C(10) 0.3234(6) -0.1335(4) 0.8128(4) 0.061(2) 1.000 . Uani d ? C(11) 0.4432(6) -0.1689(3) 0.7612(4) 0.051(1) 1.000 . Uani d ? C(12) 0.5508(5) -0.0947(3) 0.7464(3) 0.040(1) 1.000 . Uani d ? C(13) 0.9933(5) 0.3247(3) 0.8698(3) 0.044(1) 1.000 . Uani d ? C(14) 1.0199(5) 0.2724(3) 0.9486(3) 0.038(1) 1.000 . Uani d ? C(15) 1.1705(5) 0.3073(3) 1.0384(4) 0.049(1) 1.000 . Uani d ? C(16) 1.1883(6) 0.2538(4) 1.1049(4) 0.058(1) 1.000 . Uani d ? C(17) 1.0602(6) 0.1678(4) 1.0831(4) 0.056(1) 1.000 . Uani d ? C(18) 0.9157(6) 0.1371(3) 0.9934(3) 0.045(1) 1.000 . Uani d ? C(19) 0.5593(5) 0.0498(3) 0.5048(3) 0.042(1) 1.000 . Uani d ? H(1b) 0.3306 0.1424 0.5322 0.055 1.000 . Uiso c ? H(1a) 0.4327 0.2570 0.6193 0.055 1.000 . Uiso c ? H(2a) 0.2431 0.1964 0.6886 0.051 1.000 . Uiso c ? H(2b) 0.2986 0.0858 0.6606 0.051 1.000 . Uiso c ? H(3a) 0.4707 0.3524 0.9005 0.057 1.000 . Uiso c ? H(3b) 0.4736 0.3523 0.7900 0.057 1.000 . Uiso c ? H(4a) 0.7588 0.3587 0.9555 0.057 1.000 . Uiso c ? H(4b) 0.7436 0.4424 0.9042 0.057 1.000 . Uiso c ? H(5a) 0.6780 0.3718 0.7148 0.059 1.000 . Uiso c ? H(5b) 0.8743 0.3812 0.7235 0.059 1.000 . Uiso c ? H(6a) 0.6824 0.2513 0.5515 0.057 1.000 . Uiso c ? H(6b) 0.8242 0.2036 0.6074 0.057 1.000 . Uiso c ? H(7a) 0.3020 0.1688 0.8623 0.052 1.000 . Uiso c ? H(7b) 0.4952 0.2013 0.9373 0.052 1.000 . Uiso c ? H(9) 0.2324 -0.0027 0.8835 0.061 1.000 . Uiso c ? H(10) 0.2473 -0.1833 0.8238 0.073 1.000 . Uiso c ? H(11) 0.4512 -0.2429 0.7365 0.062 1.000 . Uiso c ? H(12) 0.6331 -0.1184 0.7104 0.048 1.000 . Uiso c ? H(13a) 1.0500 0.2937 0.8180 0.053 1.000 . Uiso c ? H(13b) 1.0426 0.4004 0.9082 0.053 1.000 . Uiso c ? H(15) 1.2593 0.3673 1.0533 0.059 1.000 . Uiso c ? H(16) 1.2903 0.2765 1.1667 0.069 1.000 . Uiso c ? H(17) 1.0712 0.1303 1.1291 0.067 1.000 . Uiso c ? H(18) 0.8272 0.0765 0.9774 0.054 1.000 . Uiso c ? H(19a) 0.6711 0.0343 0.5050 0.050 1.000 . Uiso c ? H(19b) 0.5098 0.0650 0.4436 0.050 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0404(3) 0.0623(3) 0.0563(3) 0.0083(2) 0.0162(2) 0.0133(3) Zn(1) 0.0289(3) 0.0293(2) 0.0289(2) 0.0012(2) 0.0074(2) 0.0101(2) Cl(1) 0.086(1) 0.0629(9) 0.073(1) 0.0062(7) 0.0106(8) 0.0319(8) S(01) 0.209(4) 0.098(2) 0.023(1) 0.056(3) 0.021(2) 0.013(2) S(01') 0.153(5) 0.124(4) 0.269(7) 0.093(4) 0.140(5) 0.144(5) O(01) 0.166(4) 0.101(4) 0.290(7) 0.072(3) 0.143(4) 0.101(5) N(1) 0.041(2) 0.038(2) 0.030(1) 0.000(1) 0.004(1) 0.016(1) N(2) 0.036(2) 0.034(2) 0.038(2) 0.012(1) 0.012(1) 0.012(1) N(3) 0.038(2) 0.033(1) 0.039(2) -0.004(1) 0.003(1) 0.013(1) N(4) 0.029(2) 0.034(1) 0.034(2) 0.003(1) 0.008(1) 0.017(1) N(5) 0.034(2) 0.039(2) 0.030(1) 0.001(1) 0.0050(9) 0.010(1) C(1) 0.038(2) 0.047(3) 0.044(2) 0.005(2) -0.001(2) 0.021(2) C(01) 0.134(6) 0.105(3) 0.149(7) 0.057(5) 0.040(5) 0.071(4) C(2) 0.033(2) 0.045(2) 0.046(2) 0.011(2) 0.005(1) 0.019(2) C(02) 0.134(5) 0.128(6) 0.114(6) 0.059(5) 0.036(4) 0.053(5) C(3) 0.058(2) 0.038(2) 0.049(3) 0.018(2) 0.020(2) 0.017(2) C(4) 0.062(2) 0.027(2) 0.040(3) 0.008(2) 0.010(2) 0.004(2) C(5) 0.053(3) 0.043(2) 0.048(2) -0.009(2) 0.003(2) 0.027(2) C(6) 0.050(3) 0.052(2) 0.038(2) -0.011(2) 0.008(2) 0.026(2) C(7) 0.046(3) 0.049(2) 0.042(2) 0.016(2) 0.026(2) 0.016(2) C(8) 0.035(2) 0.047(2) 0.028(2) 0.011(2) 0.008(2) 0.012(2) C(9) 0.046(3) 0.063(2) 0.065(3) 0.014(2) 0.033(2) 0.039(3) C(10) 0.057(3) 0.062(2) 0.087(4) 0.011(2) 0.034(3) 0.049(3) C(11) 0.049(3) 0.037(2) 0.070(3) 0.000(2) 0.011(2) 0.032(2) C(12) 0.036(2) 0.038(2) 0.042(2) 0.009(2) 0.008(2) 0.017(2) C(13) 0.040(2) 0.039(2) 0.036(2) -0.009(2) 0.001(2) 0.009(2) C(14) 0.033(2) 0.037(2) 0.036(2) 0.009(1) 0.009(2) 0.007(2) C(15) 0.034(2) 0.049(3) 0.043(2) 0.007(2) 0.002(2) 0.004(2) C(16) 0.045(3) 0.068(3) 0.045(3) 0.015(2) -0.005(2) 0.018(2) C(17) 0.058(3) 0.065(3) 0.046(3) 0.018(2) 0.006(2) 0.031(2) C(18) 0.050(2) 0.047(3) 0.042(2) 0.012(2) 0.015(2) 0.021(2) C(19) 0.045(3) 0.050(2) 0.022(2) -0.004(2) 0.007(2) 0.012(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00009|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3415 _refine_ls_number_parameters 317 _refine_ls_number_restraints 25 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_all 0.0723 _refine_ls_wR_factor_ref 0.0702 _refine_ls_goodness_of_fit_all 2.960 _refine_ls_goodness_of_fit_ref 3.449 _refine_ls_shift/esd_max 0.0060 _refine_ls_shift/esd_mean 0.2790 _refine_diff_density_min -0.79 _refine_diff_density_max 1.42 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Zn(1) 2.501(1) . . yes Zn(1) N(1) 2.244(5) . . yes Zn(1) N(2) 2.247(6) . . yes Zn(1) N(3) 2.211(6) . . yes Zn(1) N(4) 2.139(5) . . yes Zn(1) N(5) 2.216(6) . . yes Cl(1) O(11) 1.413(7) . . yes Cl(1) O(12) 1.504(9) . . yes Cl(1) O(12') 1.42(1) . . yes Cl(1) O(13) 1.215(9) . . yes Cl(1) O(13') 1.302(9) . . yes Cl(1) O(14) 1.456(9) . . yes Cl(1) O(14') 1.394(9) . . yes S(01) S(01') 0.77(1) . . yes S(01) O(01) 1.45(1) . . yes S(01) C(01) 1.89(1) . . yes S(01) C(02) 1.76(1) . . yes S(01') O(01) 1.20(1) . . yes S(01') C(01) 1.70(1) . . yes S(01') C(02) 1.79(1) . . yes O(12) O(13') 1.21(2) . . yes O(12) O(14') 1.65(2) . . yes O(12') O(13) 1.28(2) . . yes O(12') O(14) 1.50(2) . . yes O(13) O(14') 1.11(2) . . yes O(13') O(14) 1.24(2) . . yes N(1) C(1) 1.490(9) . . yes N(1) C(6) 1.499(9) . . yes N(1) C(19) 1.469(9) . . yes N(2) C(2) 1.478(9) . . yes N(2) C(3) 1.491(9) . . yes N(2) C(7) 1.473(9) . . yes N(3) C(4) 1.487(9) . . yes N(3) C(5) 1.490(9) . . yes N(3) C(13) 1.463(9) . . yes N(4) C(8) 1.336(9) . . yes N(4) C(12) 1.343(9) . . yes N(5) C(14) 1.337(9) . . yes N(5) C(18) 1.350(9) . . yes C(1) C(2) 1.51(1) . . yes C(1) H(1a) 0.95 . . no C(1) H(1b) 0.95 . . no C(2) H(2a) 0.95 . . no C(2) H(2b) 0.95 . . no C(3) C(4) 1.52(1) . . yes C(3) H(3a) 0.95 . . no C(3) H(3b) 0.95 . . no C(4) H(4a) 0.95 . . no C(4) H(4b) 0.95 . . no C(5) C(6) 1.54(1) . . yes C(5) H(5a) 0.95 . . no C(5) H(5b) 0.95 . . no C(6) H(6a) 0.95 . . no C(6) H(6b) 0.95 . . no C(7) C(8) 1.52(1) . . yes C(7) H(7a) 0.95 . . no C(7) H(7b) 0.95 . . no C(8) C(9) 1.37(1) . . yes C(9) C(10) 1.35(1) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.38(1) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.37(1) . . yes C(11) H(11) 0.96 . . no C(12) H(12) 0.95 . . no C(13) C(14) 1.50(1) . . yes C(13) H(13a) 0.95 . . no C(13) H(13b) 0.95 . . no C(14) C(15) 1.39(1) . . yes C(15) C(16) 1.37(1) . . yes C(15) H(15) 0.95 . . no C(16) C(17) 1.36(1) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.37(1) . . yes C(17) H(17) 0.95 . . no C(18) H(18) 0.95 . . no C(19) C(19) 1.52(1) . 2_656 yes C(19) H(19a) 0.95 . . no C(19) H(19b) 0.95 . . no #------------------------------------------------------------------------------ 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 Br(1) Zn(1) N(1) 93.3(2) . . . yes Br(1) Zn(1) N(2) 169.2(1) . . . yes Br(1) Zn(1) N(3) 108.9(2) . . . yes Br(1) Zn(1) N(4) 99.1(2) . . . yes Br(1) Zn(1) N(5) 86.5(2) . . . yes N(1) Zn(1) N(2) 79.6(2) . . . yes N(1) Zn(1) N(3) 81.0(2) . . . yes N(1) Zn(1) N(4) 112.9(2) . . . yes N(1) Zn(1) N(5) 153.7(2) . . . yes N(2) Zn(1) N(3) 78.3(2) . . . yes N(2) Zn(1) N(4) 76.5(2) . . . yes N(2) Zn(1) N(5) 103.5(2) . . . yes N(3) Zn(1) N(4) 148.1(2) . . . yes N(3) Zn(1) N(5) 74.3(2) . . . yes N(4) Zn(1) N(5) 93.0(2) . . . yes O(11) Cl(1) O(12) 103.2(6) . . . yes O(11) Cl(1) O(12') 106.3(8) . . . yes O(11) Cl(1) O(13) 118(1) . . . yes O(11) Cl(1) O(13') 111.4(9) . . . yes O(11) Cl(1) O(14) 104.7(6) . . . yes O(11) Cl(1) O(14') 106.5(7) . . . yes O(12) Cl(1) O(12') 149.9(9) . . . yes O(12) Cl(1) O(13) 113(1) . . . yes O(12) Cl(1) O(13') 51(1) . . . yes O(12) Cl(1) O(14) 103.8(6) . . . yes O(12) Cl(1) O(14') 69.4(8) . . . yes O(12') Cl(1) O(13) 57(1) . . . yes O(12') Cl(1) O(13') 111.3(9) . . . yes O(12') Cl(1) O(14) 63.0(9) . . . yes O(12') Cl(1) O(14') 107.0(8) . . . yes O(13) Cl(1) O(13') 131(1) . . . yes O(13) Cl(1) O(14) 113(1) . . . yes O(13) Cl(1) O(14') 50(1) . . . yes O(13') Cl(1) O(14) 53(1) . . . yes O(13') Cl(1) O(14') 113.8(9) . . . yes O(14) Cl(1) O(14') 148.8(8) . . . yes S(01') S(01) O(01) 55(1) . . . yes S(01') S(01) C(01) 64(1) . . . yes S(01') S(01) C(02) 79(1) . . . yes O(01) S(01) C(01) 104.1(8) . . . yes O(01) S(01) C(02) 111.2(8) . . . yes C(01) S(01) C(02) 97.1(8) . . . yes S(01) S(01') O(01) 93(2) . . . yes S(01) S(01') C(01) 92(1) . . . yes S(01) S(01') C(02) 76(1) . . . yes O(01) S(01') C(01) 131.5(9) . . . yes O(01) S(01') C(02) 124.5(9) . . . yes C(01) S(01') C(02) 103.4(8) . . . yes S(01) O(01) S(01') 31.9(7) . . . yes Cl(1) O(12) O(13') 56.0(6) . . . yes Cl(1) O(12) O(14') 52.2(5) . . . yes O(13') O(12) O(14') 103(1) . . . yes Cl(1) O(12') O(13) 53.1(6) . . . yes Cl(1) O(12') O(14) 59.6(6) . . . yes O(13) O(12') O(14) 107(1) . . . yes Cl(1) O(13) O(12') 70(1) . . . yes Cl(1) O(13) O(14') 74(1) . . . yes O(12') O(13) O(14') 143(1) . . . yes Cl(1) O(13') O(12) 73.3(9) . . . yes Cl(1) O(13') O(14) 69.8(8) . . . yes O(12) O(13') O(14) 143(1) . . . yes Cl(1) O(14) O(12') 57.5(6) . . . yes Cl(1) O(14) O(13') 57.1(6) . . . yes O(12') O(14) O(13') 110(1) . . . yes Cl(1) O(14') O(12) 58.4(6) . . . yes Cl(1) O(14') O(13) 56.7(7) . . . yes O(12) O(14') O(13) 109(1) . . . yes Zn(1) N(1) C(1) 109.1(4) . . . yes Zn(1) N(1) C(6) 100.4(4) . . . yes Zn(1) N(1) C(19) 116.0(4) . . . yes C(1) N(1) C(6) 113.0(6) . . . yes C(1) N(1) C(19) 111.0(6) . . . yes C(6) N(1) C(19) 107.0(5) . . . yes Zn(1) N(2) C(2) 103.5(4) . . . yes Zn(1) N(2) C(3) 111.9(4) . . . yes Zn(1) N(2) C(7) 105.3(4) . . . yes C(2) N(2) C(3) 112.1(6) . . . yes C(2) N(2) C(7) 111.8(6) . . . yes C(3) N(2) C(7) 111.8(6) . . . yes Zn(1) N(3) C(4) 106.3(4) . . . yes Zn(1) N(3) C(5) 110.0(4) . . . yes Zn(1) N(3) C(13) 104.6(4) . . . yes C(4) N(3) C(5) 111.4(6) . . . yes C(4) N(3) C(13) 110.9(6) . . . yes C(5) N(3) C(13) 113.1(6) . . . yes Zn(1) N(4) C(8) 116.1(5) . . . yes Zn(1) N(4) C(12) 125.4(5) . . . yes C(8) N(4) C(12) 118.4(6) . . . yes Zn(1) N(5) C(14) 112.3(5) . . . yes Zn(1) N(5) C(18) 128.5(5) . . . yes C(14) N(5) C(18) 117.7(6) . . . yes N(1) C(1) C(2) 113.0(6) . . . yes N(1) C(1) H(1a) 108.8 . . . no N(1) C(1) H(1b) 108.6 . . . no C(2) C(1) H(1a) 108.5 . . . no C(2) C(1) H(1b) 108.5 . . . no H(1a) C(1) H(1b) 109.5 . . . no S(01) C(01) S(01') 24.0(5) . . . yes N(2) C(2) C(1) 111.3(6) . . . yes N(2) C(2) H(2a) 109.2 . . . no N(2) C(2) H(2b) 108.9 . . . no C(1) C(2) H(2a) 109.1 . . . no C(1) C(2) H(2b) 108.9 . . . no H(2a) C(2) H(2b) 109.4 . . . no S(01) C(02) S(01') 25.0(5) . . . yes N(2) C(3) C(4) 111.0(6) . . . yes N(2) C(3) H(3a) 109.0 . . . no N(2) C(3) H(3b) 109.2 . . . no C(4) C(3) H(3a) 109.0 . . . no C(4) C(3) H(3b) 109.0 . . . no H(3a) C(3) H(3b) 109.6 . . . no N(3) C(4) C(3) 112.0(6) . . . yes N(3) C(4) H(4a) 109.1 . . . no N(3) C(4) H(4b) 109.2 . . . no C(3) C(4) H(4a) 108.7 . . . no C(3) C(4) H(4b) 108.6 . . . no H(4a) C(4) H(4b) 109.4 . . . no N(3) C(5) C(6) 111.2(6) . . . yes N(3) C(5) H(5a) 109.1 . . . no N(3) C(5) H(5b) 109.1 . . . no C(6) C(5) H(5a) 109.1 . . . no C(6) C(5) H(5b) 109.0 . . . no H(5a) C(5) H(5b) 109.2 . . . no N(1) C(6) C(5) 112.5(6) . . . yes N(1) C(6) H(6a) 108.6 . . . no N(1) C(6) H(6b) 108.8 . . . no C(5) C(6) H(6a) 108.6 . . . no C(5) C(6) H(6b) 108.7 . . . no H(6a) C(6) H(6b) 109.6 . . . no N(2) C(7) C(8) 111.1(6) . . . yes N(2) C(7) H(7a) 109.1 . . . no N(2) C(7) H(7b) 108.9 . . . no C(8) C(7) H(7a) 109.1 . . . no C(8) C(7) H(7b) 108.9 . . . no H(7a) C(7) H(7b) 109.6 . . . no N(4) C(8) C(7) 115.9(6) . . . yes N(4) C(8) C(9) 122.3(7) . . . yes C(7) C(8) C(9) 121.7(7) . . . yes C(8) C(9) C(10) 119.0(8) . . . yes C(8) C(9) H(9) 120.4 . . . no C(10) C(9) H(9) 120.6 . . . no C(9) C(10) C(11) 119.9(7) . . . yes C(9) C(10) H(10) 119.6 . . . no C(11) C(10) H(10) 120.5 . . . no C(10) C(11) C(12) 118.4(8) . . . yes C(10) C(11) H(11) 120.2 . . . no C(12) C(11) H(11) 121.4 . . . no N(4) C(12) C(11) 121.9(7) . . . yes N(4) C(12) H(12) 118.9 . . . no C(11) C(12) H(12) 119.2 . . . no N(3) C(13) C(14) 110.6(6) . . . yes N(3) C(13) H(13a) 109.3 . . . no N(3) C(13) H(13b) 109.5 . . . no C(14) C(13) H(13a) 109.1 . . . no C(14) C(13) H(13b) 109.2 . . . no H(13a) C(13) H(13b) 109.3 . . . no N(5) C(14) C(13) 116.3(6) . . . yes N(5) C(14) C(15) 121.8(7) . . . yes C(13) C(14) C(15) 121.8(7) . . . yes C(14) C(15) C(16) 118.7(8) . . . yes C(14) C(15) H(15) 120.7 . . . no C(16) C(15) H(15) 120.7 . . . no C(15) C(16) C(17) 120.2(8) . . . yes C(15) C(16) H(16) 119.8 . . . no C(17) C(16) H(16) 120.0 . . . no C(16) C(17) C(18) 118.3(8) . . . yes C(16) C(17) H(17) 121.1 . . . no C(18) C(17) H(17) 120.6 . . . no N(5) C(18) C(17) 123.2(7) . . . yes N(5) C(18) H(18) 118.3 . . . no C(17) C(18) H(18) 118.5 . . . no N(1) C(19) C(19) 113.1(7) . . 2_656 yes N(1) C(19) H(19a) 108.5 . . . no N(1) C(19) H(19b) 108.3 . . . no C(19) C(19) H(19a) 108.8 2_656 . . no C(19) C(19) H(19b) 108.7 2_656 . . no H(19a) C(19) H(19b) 109.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(01) C(16) 3.59(1) . 1_454 no O(01) C(12) 3.21(1) . 2_656 no O(01) C(11) 3.38(1) . 2_656 no O(01) C(1) 3.41(1) . . no O(11) C(13) 3.38(1) . 2_766 no O(11) C(3) 3.44(1) . 2_666 no O(11) C(5) 3.45(1) . 2_766 no O(11) C(02) 3.58(2) . 2_666 no O(12) C(15) 3.30(1) . 1_454 no O(12) C(16) 3.34(1) . 1_454 no O(12) C(3) 3.49(2) . 2_666 no O(13) C(4) 3.11(2) . 1_554 no O(13) C(3) 3.45(2) . 1_554 no O(13') C(11) 3.30(2) . 2_656 no O(13') C(01) 3.53(2) . 2_666 no O(14) C(11) 3.35(1) . 2_656 no O(14) C(10) 3.38(1) . 2_656 no O(14) C(01) 3.42(2) . 1_655 no O(14) C(02) 3.50(2) . 1_655 no O(14') C(3) 3.33(2) . 2_666 no O(14') C(15) 3.34(2) . 1_454 no O(14') C(3) 3.41(2) . 1_554 no O(14') C(4) 3.43(2) . 1_554 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Br(1) Zn(1) N(1) C(1) . . . . 165.2(4) no Br(1) Zn(1) N(1) C(6) . . . . -75.9(4) no Br(1) Zn(1) N(1) C(19) . . . . 39.0(5) no Br(1) Zn(1) N(2) C(2) . . . . -19(1) no Br(1) Zn(1) N(2) C(3) . . . . -139.8(7) no Br(1) Zn(1) N(2) C(7) . . . . 98.6(9) no Br(1) Zn(1) N(3) C(4) . . . . -158.6(4) no Br(1) Zn(1) N(3) C(5) . . . . 80.7(5) no Br(1) Zn(1) N(3) C(13) . . . . -41.2(5) no Br(1) Zn(1) N(4) C(8) . . . . 172.1(5) no Br(1) Zn(1) N(4) C(12) . . . . -9.8(6) no Br(1) Zn(1) N(5) C(14) . . . . 82.5(5) no Br(1) Zn(1) N(5) C(18) . . . . -83.0(6) no Zn(1) N(1) C(1) C(2) . . . . -19.4(7) no Zn(1) N(1) C(6) C(5) . . . . -53.3(7) no Zn(1) N(1) C(19) C(19) . . . 2_656 60.0(9) no Zn(1) N(2) C(2) C(1) . . . . -51.6(6) no Zn(1) N(2) C(3) C(4) . . . . -16.7(7) no Zn(1) N(2) C(7) C(8) . . . . -40.8(7) no Zn(1) N(3) C(4) C(3) . . . . -49.7(7) no Zn(1) N(3) C(5) C(6) . . . . -16.2(8) no Zn(1) N(3) C(13) C(14) . . . . -47.0(7) no Zn(1) N(4) C(8) C(7) . . . . 0.0(8) no Zn(1) N(4) C(8) C(9) . . . . 179.4(6) no Zn(1) N(4) C(12) C(11) . . . . -179.1(6) no Zn(1) N(5) C(14) C(13) . . . . 10.3(8) no Zn(1) N(5) C(14) C(15) . . . . -168.2(6) no Zn(1) N(5) C(18) C(17) . . . . 166.1(6) no Cl(1) O(12) O(13') O(14) . . . . -4(3) no Cl(1) O(12) O(14') O(13) . . . . 27(1) no Cl(1) O(12') O(13) O(14') . . . . -2(3) no Cl(1) O(12') O(14) O(13') . . . . 24(1) no Cl(1) O(13) O(12') O(14) . . . . 28(1) no Cl(1) O(13) O(14') O(12) . . . . -27(1) no Cl(1) O(13') O(12) O(14') . . . . 24(1) no Cl(1) O(13') O(14) O(12') . . . . -24(1) no Cl(1) O(14) O(12') O(13) . . . . -26(1) no Cl(1) O(14) O(13') O(12) . . . . 4(3) no Cl(1) O(14') O(12) O(13') . . . . -25(1) no Cl(1) O(14') O(13) O(12') . . . . 2(3) no S(01) O(01) S(01') C(01) . . . . -95(2) no S(01) O(01) S(01') C(02) . . . . 74(2) no S(01) C(01) S(01') O(01) . . . . 95(2) no S(01) C(01) S(01') C(02) . . . . -76(1) no S(01) C(02) S(01') O(01) . . . . -83(2) no S(01) C(02) S(01') C(01) . . . . 89(1) no S(01') O(01) S(01) C(01) . . . . 44(1) no S(01') O(01) S(01) C(02) . . . . -60(1) no S(01') C(01) S(01) O(01) . . . . -39(1) no S(01') C(01) S(01) C(02) . . . . 75(1) no S(01') C(02) S(01) O(01) . . . . 46(1) no S(01') C(02) S(01) C(01) . . . . -62(1) no O(01) S(01) S(01') C(01) . . . . 132(1) no O(01) S(01) S(01') C(02) . . . . -125.0(8) no O(01) S(01') S(01) C(01) . . . . -132(1) no O(01) S(01') S(01) C(02) . . . . 125.0(8) no O(11) Cl(1) O(12) O(13') . . . . -107(1) no O(11) Cl(1) O(12) O(14') . . . . 102.9(7) no O(11) Cl(1) O(12') O(13) . . . . -113(1) no O(11) Cl(1) O(12') O(14) . . . . 98.5(7) no O(11) Cl(1) O(13) O(12') . . . . 92(1) no O(11) Cl(1) O(13) O(14') . . . . -89(1) no O(11) Cl(1) O(13') O(12) . . . . 90(1) no O(11) Cl(1) O(13') O(14) . . . . -93(1) no O(11) Cl(1) O(14) O(12') . . . . -101.1(9) no O(11) Cl(1) O(14) O(13') . . . . 106(1) no O(11) Cl(1) O(14') O(12) . . . . -98.2(7) no O(11) Cl(1) O(14') O(13) . . . . 112(1) no O(12) Cl(1) O(12') O(13) . . . . 79(2) no O(12) Cl(1) O(12') O(14) . . . . -70(2) no O(12) Cl(1) O(13) O(12') . . . . -148(1) no O(12) Cl(1) O(13) O(14') . . . . 31(2) no O(12) Cl(1) O(13') O(14) . . . . 178(2) no O(12) Cl(1) O(14) O(12') . . . . 151(1) no O(12) Cl(1) O(14) O(13') . . . . -2(1) no O(12) Cl(1) O(14') O(13) . . . . -149(2) no O(12) O(13') Cl(1) O(12') . . . . -152(1) no O(12) O(13') Cl(1) O(13) . . . . -87(2) no O(12) O(13') Cl(1) O(14) . . . . -178(2) no O(12) O(13') Cl(1) O(14') . . . . -31(1) no O(12) O(13') O(14) O(12') . . . . -20(4) no O(12) O(14') Cl(1) O(12') . . . . 148(1) no O(12) O(14') Cl(1) O(13) . . . . 149(2) no O(12) O(14') Cl(1) O(13') . . . . 25(1) no O(12) O(14') Cl(1) O(14) . . . . 83(2) no O(12) O(14') O(13) O(12') . . . . -26(4) no O(12') Cl(1) O(12) O(13') . . . . 61(2) no O(12') Cl(1) O(12) O(14') . . . . -89(2) no O(12') Cl(1) O(13) O(14') . . . . 179(2) no O(12') Cl(1) O(13') O(14) . . . . 26(1) no O(12') Cl(1) O(14) O(13') . . . . -153(1) no O(12') Cl(1) O(14') O(13) . . . . -1(2) no O(12') O(13) Cl(1) O(13') . . . . -91(2) no O(12') O(13) Cl(1) O(14) . . . . -30(2) no O(12') O(13) Cl(1) O(14') . . . . -179(2) no O(12') O(14) Cl(1) O(13) . . . . 28(1) no O(12') O(14) Cl(1) O(13') . . . . 153(1) no O(12') O(14) Cl(1) O(14') . . . . 78(2) no O(13) Cl(1) O(12) O(13') . . . . 125(2) no O(13) Cl(1) O(12) O(14') . . . . -25(1) no O(13) Cl(1) O(12') O(14) . . . . -149(2) no O(13) Cl(1) O(13') O(14) . . . . 90(2) no O(13) Cl(1) O(14) O(13') . . . . -125(2) no O(13) O(12') Cl(1) O(13') . . . . 126(2) no O(13) O(12') Cl(1) O(14) . . . . 149(2) no O(13) O(12') Cl(1) O(14') . . . . 1(2) no O(13) O(12') O(14) O(13') . . . . -2(2) no O(13) O(14') Cl(1) O(13') . . . . -124(2) no O(13) O(14') Cl(1) O(14) . . . . -67(2) no O(13) O(14') O(12) O(13') . . . . 2(2) no O(13') Cl(1) O(12) O(14') . . . . -150(1) no O(13') Cl(1) O(12') O(14) . . . . -23(1) no O(13') Cl(1) O(13) O(14') . . . . 88(2) no O(13') O(12) Cl(1) O(14) . . . . 2(1) no O(13') O(12) Cl(1) O(14') . . . . 150(1) no O(13') O(14) Cl(1) O(14') . . . . -75(2) no O(14) Cl(1) O(12) O(14') . . . . -148.0(9) no O(14) Cl(1) O(13) O(14') . . . . 149(1) no O(14) O(12') Cl(1) O(14') . . . . -148.0(9) no O(14) O(12') O(13) O(14') . . . . 26(4) no O(14) O(13') Cl(1) O(14') . . . . 147(1) no O(14) O(13') O(12) O(14') . . . . 20(3) no N(1) Zn(1) N(2) C(2) . . . . 30.7(4) no N(1) Zn(1) N(2) C(3) . . . . -90.2(5) no N(1) Zn(1) N(2) C(7) . . . . 148.1(5) no N(1) Zn(1) N(3) C(4) . . . . 111.0(5) no N(1) Zn(1) N(3) C(5) . . . . -9.7(5) no N(1) Zn(1) N(3) C(13) . . . . -131.5(5) no N(1) Zn(1) N(4) C(8) . . . . -90.3(5) no N(1) Zn(1) N(4) C(12) . . . . 87.7(6) no N(1) Zn(1) N(5) C(14) . . . . -7.8(8) no N(1) Zn(1) N(5) C(18) . . . . -173.3(6) no N(1) C(1) C(2) N(2) . . . . 50.0(8) no N(1) C(6) C(5) N(3) . . . . 49.6(9) no N(1) C(19) C(19) N(1) . . 2_656 2_656 180.0000 no N(2) Zn(1) N(1) C(1) . . . . -6.5(4) no N(2) Zn(1) N(1) C(6) . . . . 112.4(5) no N(2) Zn(1) N(1) C(19) . . . . -132.7(5) no N(2) Zn(1) N(3) C(4) . . . . 29.8(4) no N(2) Zn(1) N(3) C(5) . . . . -90.9(5) no N(2) Zn(1) N(3) C(13) . . . . 147.3(5) no N(2) Zn(1) N(4) C(8) . . . . -18.0(5) no N(2) Zn(1) N(4) C(12) . . . . 160.1(6) no N(2) Zn(1) N(5) C(14) . . . . -101.7(5) no N(2) Zn(1) N(5) C(18) . . . . 92.8(6) no N(2) C(3) C(4) N(3) . . . . 45.0(8) no N(2) C(7) C(8) N(4) . . . . 29.3(9) no N(2) C(7) C(8) C(9) . . . . -150.1(7) no N(3) Zn(1) N(1) C(1) . . . . -86.1(4) no N(3) Zn(1) N(1) C(6) . . . . 32.8(5) no N(3) Zn(1) N(1) C(19) . . . . 147.7(5) no N(3) Zn(1) N(2) C(2) . . . . 113.5(5) no N(3) Zn(1) N(2) C(3) . . . . -7.4(5) no N(3) Zn(1) N(2) C(7) . . . . -129.0(5) no N(3) Zn(1) N(4) C(8) . . . . 20.6(7) no N(3) Zn(1) N(4) C(12) . . . . -161.3(5) no N(3) Zn(1) N(5) C(14) . . . . -28.2(5) no N(3) Zn(1) N(5) C(18) . . . . 166.3(7) no N(3) C(13) C(14) N(5) . . . . 25.7(9) no N(3) C(13) C(14) C(15) . . . . -155.8(7) no N(4) Zn(1) N(1) C(1) . . . . 63.9(5) no N(4) Zn(1) N(1) C(6) . . . . -177.2(4) no N(4) Zn(1) N(1) C(19) . . . . -62.3(5) no N(4) Zn(1) N(2) C(2) . . . . -86.2(4) no N(4) Zn(1) N(2) C(3) . . . . 152.9(5) no N(4) Zn(1) N(2) C(7) . . . . 31.3(4) no N(4) Zn(1) N(3) C(4) . . . . -8.4(7) no N(4) Zn(1) N(3) C(5) . . . . -129.2(5) no N(4) Zn(1) N(3) C(13) . . . . 109.0(5) no N(4) Zn(1) N(5) C(14) . . . . -178.5(5) no N(4) Zn(1) N(5) C(18) . . . . 16.0(6) no N(4) C(8) C(9) C(10) . . . . -1(1) no N(4) C(12) C(11) C(10) . . . . 1(1) no N(5) Zn(1) N(1) C(1) . . . . -106.0(6) no N(5) Zn(1) N(1) C(6) . . . . 12.9(8) no N(5) Zn(1) N(1) C(19) . . . . 127.8(6) no N(5) Zn(1) N(2) C(2) . . . . -176.0(4) no N(5) Zn(1) N(2) C(3) . . . . 63.1(5) no N(5) Zn(1) N(2) C(7) . . . . -58.5(5) no N(5) Zn(1) N(3) C(4) . . . . -77.9(5) no N(5) Zn(1) N(3) C(5) . . . . 161.3(5) no N(5) Zn(1) N(3) C(13) . . . . 39.5(4) no N(5) Zn(1) N(4) C(8) . . . . 85.2(5) no N(5) Zn(1) N(4) C(12) . . . . -96.7(6) no N(5) C(14) C(15) C(16) . . . . 0(1) no N(5) C(18) C(17) C(16) . . . . -1(1) no C(1) N(1) C(6) C(5) . . . . 62.7(8) no C(1) N(1) C(19) C(19) . . . 2_656 -65(1) no C(1) C(2) N(2) C(3) . . . . 69.2(8) no C(1) C(2) N(2) C(7) . . . . -164.4(6) no C(01) S(01) S(01') C(02) . . . . 103.3(8) no C(01) S(01') S(01) C(02) . . . . -103.3(8) no C(2) N(2) C(3) C(4) . . . . -132.4(7) no C(2) N(2) C(7) C(8) . . . . 70.9(7) no C(2) C(1) N(1) C(6) . . . . -130.2(6) no C(2) C(1) N(1) C(19) . . . . 109.6(7) no C(3) N(2) C(7) C(8) . . . . -162.4(6) no C(3) C(4) N(3) C(5) . . . . 70.2(7) no C(3) C(4) N(3) C(13) . . . . -162.9(6) no C(4) N(3) C(5) C(6) . . . . -133.8(7) no C(4) N(3) C(13) C(14) . . . . 67.2(8) no C(4) C(3) N(2) C(7) . . . . 101.1(7) no C(5) N(3) C(13) C(14) . . . . -166.8(6) no C(5) C(6) N(1) C(19) . . . . -174.8(6) no C(6) N(1) C(19) C(19) . . . 2_656 171.1(8) no C(6) C(5) N(3) C(13) . . . . 100.4(7) no C(7) C(8) N(4) C(12) . . . . -178.2(6) no C(7) C(8) C(9) C(10) . . . . 178.5(8) no C(8) N(4) C(12) C(11) . . . . -1(1) no C(8) C(9) C(10) C(11) . . . . 0(1) no C(9) C(8) N(4) C(12) . . . . 1(1) no C(9) C(10) C(11) C(12) . . . . 0(1) no C(13) C(14) N(5) C(18) . . . . 177.6(7) no C(13) C(14) C(15) C(16) . . . . -178.0(8) no C(14) N(5) C(18) C(17) . . . . 1(1) no C(14) C(15) C(16) C(17) . . . . 0(1) no C(15) C(14) N(5) C(18) . . . . -1(1) no C(15) C(16) C(17) C(18) . . . . 0(1) no #------------------------------------------------------------------------------ #=END data_[C39H54Cl3N10O13.5Zn2] # Complex 5 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Feb 10 16:03:15 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 18.863(9) _cell_length_b 19.011(5) _cell_length_c 12.663(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4540(2) _cell_formula_units_Z 4 _cell_measurement_temperature 220 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 32.3 _cell_measurement_theta_max 41.5 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'multifaceted' _exptl_crystal_colour 'pale-yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_meas ? _chemical_formula_weight 1116.03 _chemical_formula_analytical ? _chemical_formula_sum 'C39 H54 Cl3 N10 O13.50 Zn2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 2.623 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.383 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 220 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC6R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% -9.11 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -4 0 -2 -3 0 0 -2 2 _diffrn_reflns_number 5840 _reflns_number_total 5840 _reflns_number_observed 3195 _reflns_observed_criterion I>2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.03699 _diffrn_orient_matrix_UB_12 -0.03496 _diffrn_orient_matrix_UB_13 0.02111 _diffrn_orient_matrix_UB_21 -0.01907 _diffrn_orient_matrix_UB_22 0.00013 _diffrn_orient_matrix_UB_23 -0.07369 _diffrn_orient_matrix_UB_31 0.03284 _diffrn_orient_matrix_UB_32 -0.03931 _diffrn_orient_matrix_UB_33 -0.01901 #------------------------------------------------------------------------------ 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 0 156 0.003 0.002 'International Tables' H 0 216 0.000 0.000 'International Tables' Cl 0 12 0.148 0.159 'International Tables' N 0 40 0.006 0.003 'International Tables' O 0 54 0.011 0.006 'International Tables' Zn 0 8 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) 0.32808(8) 0.25812(8) 0.3068(1) 0.0270(4) Uij ? ? Zn(2) 0.17652(8) 0.18675(8) 0.1264(1) 0.0272(4) Uij ? ? Cl(1) 0.3107(3) 0.3430(3) 0.7863(4) 0.069(2) Uij ? ? Cl(2) 0.5315(2) 0.0783(2) 0.5726(3) 0.040(1) Uij ? ? Cl(3) 0.1157(2) 0.0452(2) 0.5715(4) 0.053(1) Uij ? ? O(1) 0.2485(4) 0.1930(5) 0.2528(8) 0.034(3) Uij ? ? O(2) 0.286(1) 0.410(1) 0.820(2) 0.26(1) Uij ? ? O(3) 0.359(1) 0.377(1) 0.722(2) 0.088(10) Uij ? ? O(3') 0.364(1) 0.299(1) 0.734(2) 0.05(1) Uij ? ? O(4) 0.249(1) 0.334(1) 0.731(2) 0.068(7) Uij ? ? O(4') 0.248(1) 0.296(2) 0.760(2) 0.048(9) Uij ? ? O(5') 0.337(2) 0.351(2) 0.900(3) 0.11(1) Uij ? ? O(5) 0.3249(10) 0.309(1) 0.883(2) 0.048(5) Uij ? ? O(6) 0.5679(6) 0.1430(6) 0.565(1) 0.069(4) Uij ? ? O(7) 0.5772(6) 0.0243(6) 0.618(1) 0.082(5) Uij ? ? O(8) 0.4733(5) 0.0866(6) 0.6437(9) 0.058(4) Uij ? ? O(9) 0.5055(6) 0.0585(6) 0.4695(9) 0.064(4) Uij ? ? O(10) 0.1694(7) 0.0093(7) 0.516(1) 0.092(4) Uij ? ? O(11) 0.1245(9) 0.1172(10) 0.562(1) 0.131(6) Uij ? ? O(12) 0.1181(8) 0.0237(9) 0.683(1) 0.127(6) Uij ? ? O(13) 0.0499(8) 0.0249(8) 0.533(1) 0.104(5) Uij ? ? O(14) 0.500(1) 0.454(1) 0.202(2) 0.066(7) Uij ? ? N(1) 0.3176(6) 0.1956(6) 0.4435(9) 0.034(3) Uij ? ? N(2) 0.4124(6) 0.3085(7) 0.411(1) 0.047(4) Uij ? ? N(3) 0.2630(6) 0.3319(6) 0.4050(9) 0.035(4) Uij ? ? N(4) 0.3178(6) 0.3434(5) 0.2032(10) 0.036(3) Uij ? ? N(5) 0.4329(5) 0.2078(6) 0.259(1) 0.038(4) Uij ? ? N(6) 0.1615(5) 0.0809(5) 0.187(1) 0.036(4) Uij ? ? N(7) 0.0611(5) 0.1925(7) 0.1875(9) 0.035(3) Uij ? ? N(8) 0.1162(5) 0.1408(6) -0.010(1) 0.034(4) Uij ? ? N(9) 0.2553(5) 0.1745(6) 0.0033(9) 0.028(3) Uij ? ? N(10) 0.1454(5) 0.2921(6) 0.0964(9) 0.031(3) Uij ? ? C(1) 0.3878(8) 0.1928(9) 0.495(1) 0.052(5) Uij ? ? C(2) 0.4219(8) 0.2650(8) 0.503(2) 0.049(5) Uij ? ? C(3) 0.3863(8) 0.3817(8) 0.430(1) 0.051(5) Uij ? ? C(4) 0.3084(8) 0.3751(9) 0.474(1) 0.050(6) Uij ? ? C(5) 0.2184(8) 0.2819(8) 0.465(1) 0.044(5) Uij ? ? C(6) 0.2643(9) 0.2275(9) 0.516(1) 0.051(6) Uij ? ? C(7) 0.2256(7) 0.3735(7) 0.326(1) 0.031(4) Uij ? ? C(8) 0.2734(7) 0.3959(8) 0.238(1) 0.031(4) Uij ? ? C(9) 0.2741(8) 0.4628(7) 0.198(1) 0.042(5) Uij ? ? C(10) 0.3217(9) 0.4759(8) 0.114(1) 0.059(6) Uij ? ? C(11) 0.3620(8) 0.4243(10) 0.078(2) 0.058(6) Uij ? ? C(12) 0.3600(7) 0.3565(8) 0.120(1) 0.033(4) Uij ? ? C(13) 0.4753(7) 0.3123(9) 0.339(1) 0.048(5) Uij ? ? C(14) 0.4895(7) 0.2410(8) 0.290(1) 0.037(4) Uij ? ? C(15) 0.5567(7) 0.2128(9) 0.287(1) 0.040(5) Uij ? ? C(16) 0.5681(8) 0.150(1) 0.241(1) 0.052(6) Uij ? ? C(17) 0.5081(9) 0.1130(8) 0.206(1) 0.054(6) Uij ? ? C(18) 0.4433(8) 0.1457(9) 0.213(1) 0.039(5) Uij ? ? C(19) 0.2950(7) 0.1265(7) 0.399(1) 0.036(5) Uij ? ? C(20) 0.2356(7) 0.1385(7) 0.321(1) 0.030(4) Uij ? ? C(21) 0.2229(7) 0.0703(8) 0.255(1) 0.046(5) Uij ? ? C(22) 0.0930(7) 0.0727(7) 0.248(1) 0.041(5) Uij ? ? C(23) 0.0583(7) 0.1432(9) 0.277(1) 0.041(5) Uij ? ? C(24) 0.0113(7) 0.1702(8) 0.100(1) 0.050(5) Uij ? ? C(25) 0.0446(7) 0.1755(9) -0.010(1) 0.049(5) Uij ? ? C(26) 0.1116(8) 0.0639(8) 0.006(1) 0.043(5) Uij ? ? C(27) 0.1641(7) 0.0393(7) 0.091(1) 0.040(5) Uij ? ? C(28) 0.1525(7) 0.1610(9) -0.110(1) 0.049(5) Uij ? ? C(29) 0.2322(7) 0.1537(8) -0.093(1) 0.032(4) Uij ? ? C(30) 0.2790(8) 0.1320(8) -0.174(1) 0.043(5) Uij ? ? C(31) 0.3500(7) 0.1343(8) -0.153(1) 0.041(5) Uij ? ? C(32) 0.3759(7) 0.1561(9) -0.054(1) 0.045(5) Uij ? ? C(33) 0.3252(7) 0.1749(7) 0.020(1) 0.032(4) Uij ? ? C(34) 0.0516(7) 0.2656(9) 0.216(1) 0.044(5) Uij ? ? C(35) 0.0865(6) 0.3152(7) 0.142(1) 0.028(4) Uij ? ? C(36) 0.0616(8) 0.3826(8) 0.125(1) 0.044(5) Uij ? ? C(37) 0.0984(9) 0.4252(8) 0.053(2) 0.058(6) Uij ? ? C(38) 0.1559(8) 0.4018(8) 0.011(1) 0.037(5) Uij ? ? C(39) 0.1796(7) 0.3351(8) 0.030(1) 0.037(4) Uij ? ? H(1a) 0.3821 0.1740 0.5658 0.0621 Uij ? ? H(1b) 0.4185 0.1621 0.4545 0.0621 Uij ? ? H(2a) 0.4724 0.2586 0.5138 0.0584 Uij ? ? H(2b) 0.4016 0.2893 0.5628 0.0584 Uij ? ? H(3a) 0.4161 0.4048 0.4821 0.0618 Uij ? ? H(3b) 0.3866 0.4085 0.3652 0.0618 Uij ? ? H(4a) 0.2880 0.4218 0.4788 0.0603 Uij ? ? H(4b) 0.3099 0.3537 0.5431 0.0603 Uij ? ? H(5a) 0.1923 0.3071 0.5188 0.0531 Uij ? ? H(5b) 0.1853 0.2592 0.4170 0.0531 Uij ? ? H(6a) 0.2340 0.1903 0.5421 0.0610 Uij ? ? H(6b) 0.2892 0.2493 0.5739 0.0610 Uij ? ? H(7a) 0.1872 0.3455 0.2975 0.0366 Uij ? ? H(7b) 0.2064 0.4151 0.3600 0.0366 Uij ? ? H(9) 0.2437 0.4994 0.2264 0.0503 Uij ? ? H(10) 0.3246 0.5224 0.0822 0.0713 Uij ? ? H(11) 0.3942 0.4338 0.0199 0.0694 Uij ? ? H(12) 0.3889 0.3194 0.0900 0.0400 Uij ? ? H(13a) 0.4661 0.3462 0.2831 0.0576 Uij ? ? H(13b) 0.5165 0.3269 0.3788 0.0576 Uij ? ? H(15) 0.5959 0.2382 0.3192 0.0484 Uij ? ? H(16) 0.6155 0.1305 0.2324 0.0626 Uij ? ? H(17) 0.5122 0.0659 0.1771 0.0647 Uij ? ? H(18) 0.4026 0.1220 0.1823 0.0467 Uij ? ? H(19a) 0.3348 0.1045 0.3631 0.0438 Uij ? ? H(19b) 0.2786 0.0961 0.4552 0.0438 Uij ? ? H(20) 0.1927 0.1489 0.3601 0.0362 Uij ? ? H(21b) 0.2643 0.0605 0.2119 0.0551 Uij ? ? H(21a) 0.2142 0.0310 0.3019 0.0551 Uij ? ? H(22b) 0.1028 0.0469 0.3121 0.0490 Uij ? ? H(22a) 0.0600 0.0462 0.2045 0.0490 Uij ? ? H(23b) 0.0092 0.1351 0.2966 0.0489 Uij ? ? H(23a) 0.0834 0.1635 0.3369 0.0489 Uij ? ? H(24b) -0.0303 0.2002 0.1018 0.0595 Uij ? ? H(24a) -0.0028 0.1218 0.1119 0.0595 Uij ? ? H(25b) 0.0142 0.1524 -0.0606 0.0585 Uij ? ? H(25a) 0.0499 0.2247 -0.0285 0.0585 Uij ? ? H(26b) 0.1226 0.0403 -0.0600 0.0518 Uij ? ? H(26a) 0.0637 0.0518 0.0276 0.0518 Uij ? ? H(27b) 0.1532 -0.0091 0.1095 0.0483 Uij ? ? H(27a) 0.2117 0.0419 0.0628 0.0483 Uij ? ? H(28b) 0.1411 0.2093 -0.1276 0.0590 Uij ? ? H(28a) 0.1375 0.1302 -0.1665 0.0590 Uij ? ? H(30) 0.2614 0.1162 -0.2415 0.0511 Uij ? ? H(31) 0.3834 0.1205 -0.2070 0.0486 Uij ? ? H(32) 0.4262 0.1578 -0.0382 0.0545 Uij ? ? H(33) 0.3418 0.1896 0.0891 0.0387 Uij ? ? H(34b) 0.0712 0.2729 0.2855 0.0526 Uij ? ? H(34a) 0.0013 0.2757 0.2163 0.0526 Uij ? ? H(36) 0.0202 0.4000 0.1622 0.0532 Uij ? ? H(37) 0.0808 0.4716 0.0351 0.0695 Uij ? ? H(38) 0.1828 0.4322 -0.0361 0.0449 Uij ? ? H(39) 0.2222 0.3186 -0.0050 0.0450 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) 0.0278(8) 0.0267(9) 0.0265(9) -0.0013(8) -0.0012(8) -0.0011(9) Zn(2) 0.0235(7) 0.0270(9) 0.0310(9) -0.0016(8) 0.0027(9) -0.0038(9) Cl(1) 0.077(3) 0.078(4) 0.052(3) -0.002(3) -0.020(3) 0.000(3) Cl(2) 0.039(2) 0.033(2) 0.046(3) -0.002(2) -0.008(2) -0.014(2) Cl(3) 0.044(2) 0.037(2) 0.078(4) 0.004(2) 0.011(2) 0.013(3) O(1) 0.040(5) 0.024(5) 0.037(6) -0.012(5) 0.008(5) 0.001(6) O(6) 0.067(8) 0.055(8) 0.08(1) -0.028(7) 0.007(7) -0.011(9) O(7) 0.074(8) 0.066(8) 0.10(1) 0.046(7) -0.017(8) -0.017(10) O(8) 0.047(6) 0.084(9) 0.044(8) 0.007(6) 0.002(6) 0.001(8) O(9) 0.086(8) 0.052(7) 0.055(9) -0.019(7) -0.023(7) -0.014(7) N(1) 0.031(6) 0.039(7) 0.031(7) 0.008(6) -0.006(6) -0.014(7) N(2) 0.038(7) 0.038(8) 0.07(1) -0.010(6) -0.018(7) -0.010(9) N(3) 0.037(7) 0.043(8) 0.024(8) 0.000(6) 0.003(5) -0.019(7) N(4) 0.030(6) 0.025(6) 0.052(8) -0.003(6) -0.003(7) -0.004(7) N(5) 0.029(6) 0.027(7) 0.060(10) -0.004(5) -0.006(6) -0.022(7) N(6) 0.031(7) 0.022(6) 0.056(9) -0.010(5) -0.004(6) -0.009(8) N(7) 0.031(6) 0.053(8) 0.021(7) 0.003(6) 0.006(6) -0.026(8) N(8) 0.017(6) 0.046(8) 0.039(8) -0.002(5) 0.014(6) -0.008(8) N(9) 0.027(6) 0.036(8) 0.020(7) 0.006(5) 0.001(5) -0.002(7) N(10) 0.032(6) 0.039(7) 0.020(7) 0.010(5) -0.013(5) -0.021(7) C(1) 0.050(9) 0.06(1) 0.04(1) 0.018(10) -0.004(8) 0.02(1) C(2) 0.07(1) 0.04(1) 0.04(1) 0.005(9) -0.031(9) 0.01(1) C(3) 0.05(1) 0.030(9) 0.07(1) 0.003(8) -0.03(1) 0.00(1) C(4) 0.05(1) 0.07(1) 0.04(1) 0.005(9) 0.001(8) -0.01(1) C(5) 0.056(10) 0.036(9) 0.04(1) 0.003(8) 0.030(8) 0.003(9) C(6) 0.06(1) 0.06(1) 0.025(10) 0.007(9) 0.007(8) 0.00(1) C(7) 0.037(8) 0.029(8) 0.025(9) 0.012(7) 0.001(7) -0.004(8) C(8) 0.026(7) 0.032(9) 0.034(10) 0.002(7) -0.009(7) -0.004(8) C(9) 0.055(9) 0.020(8) 0.05(1) 0.002(7) 0.001(9) 0.004(10) C(10) 0.06(1) 0.045(10) 0.08(1) -0.008(10) -0.02(1) 0.01(1) C(11) 0.047(10) 0.06(1) 0.07(1) -0.016(9) -0.016(9) 0.03(1) C(12) 0.044(9) 0.037(9) 0.019(8) 0.004(7) 0.006(7) -0.001(9) C(13) 0.035(8) 0.049(10) 0.06(1) -0.012(8) -0.004(7) 0.00(1) C(14) 0.029(8) 0.047(9) 0.034(10) 0.000(7) -0.004(7) -0.008(10) C(15) 0.027(8) 0.06(1) 0.04(1) -0.008(7) -0.002(7) -0.004(10) C(16) 0.033(9) 0.10(2) 0.03(1) 0.016(10) -0.003(7) -0.01(1) C(17) 0.06(1) 0.047(10) 0.06(1) 0.014(9) 0.00(1) -0.02(1) C(18) 0.046(9) 0.05(1) 0.023(10) 0.000(8) 0.001(7) -0.006(9) C(19) 0.041(8) 0.031(9) 0.04(1) 0.003(7) 0.002(7) 0.016(9) C(20) 0.038(8) 0.026(8) 0.026(9) -0.002(7) 0.008(7) 0.003(8) C(21) 0.037(8) 0.037(10) 0.06(1) 0.000(8) 0.006(9) 0.02(1) C(22) 0.042(9) 0.025(8) 0.06(1) -0.004(7) 0.016(8) -0.005(9) C(23) 0.023(7) 0.06(1) 0.04(1) -0.008(7) 0.011(7) -0.002(10) C(24) 0.023(8) 0.06(1) 0.07(1) -0.010(8) -0.008(8) 0.00(1) C(25) 0.033(8) 0.06(1) 0.05(1) -0.003(8) 0.008(8) -0.02(1) C(26) 0.053(10) 0.030(9) 0.05(1) -0.010(8) 0.022(9) -0.023(9) C(27) 0.026(8) 0.034(8) 0.06(1) -0.018(7) 0.013(8) -0.002(9) C(28) 0.033(8) 0.06(1) 0.06(1) -0.008(7) -0.008(8) -0.01(1) C(29) 0.035(8) 0.034(9) 0.028(10) -0.001(7) 0.004(7) -0.013(8) C(30) 0.040(9) 0.05(1) 0.04(1) -0.003(8) 0.003(8) -0.023(10) C(31) 0.037(8) 0.036(9) 0.05(1) 0.012(7) 0.024(7) 0.016(9) C(32) 0.025(8) 0.06(1) 0.06(1) 0.003(8) 0.000(8) -0.02(1) C(33) 0.025(6) 0.032(8) 0.040(9) 0.004(7) -0.012(8) -0.010(8) C(34) 0.033(8) 0.05(1) 0.05(1) 0.012(8) 0.011(7) 0.00(1) C(35) 0.037(7) 0.028(8) 0.018(8) -0.005(7) -0.009(6) -0.005(9) C(36) 0.048(9) 0.032(9) 0.05(1) 0.014(8) -0.011(9) -0.01(1) C(37) 0.07(1) 0.033(10) 0.07(1) -0.005(9) -0.02(1) 0.02(1) C(38) 0.05(1) 0.033(9) 0.031(9) 0.002(7) -0.012(8) 0.008(9) C(39) 0.031(7) 0.041(9) 0.040(10) 0.000(8) 0.002(8) 0.007(8) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment 'incl. in calc. positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; refinement of opp. hand gave sig. greater values of R and Rw, i.e. 0.078 and 0.073, resp. ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3195 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0715 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0665 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.107 _refine_ls_shift/esd_max 0.0315 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.65 _refine_diff_density_max 0.95 #------------------------------------------------------------------------------ _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) 2.062(9) ? ? yes Zn(1) N(1) 2.11(1) ? ? yes Zn(1) N(2) 2.27(1) ? ? yes Zn(1) N(3) 2.24(1) ? ? yes Zn(1) N(4) 2.09(1) ? ? yes Zn(1) N(5) 2.28(1) ? ? yes Zn(2) O(1) 2.103(10) ? ? yes Zn(2) N(6) 2.17(1) ? ? yes Zn(2) N(7) 2.313(10) ? ? yes Zn(2) N(8) 2.24(1) ? ? yes Zn(2) N(9) 2.17(1) ? ? yes Zn(2) N(10) 2.12(1) ? ? yes Cl(1) O(2) 1.41(3) ? ? yes Cl(1) O(3) 1.38(2) ? ? yes Cl(1) O(3') 1.47(3) ? ? yes Cl(1) O(4) 1.38(2) ? ? yes Cl(1) O(4') 1.52(3) ? ? yes Cl(1) O(5') 1.53(4) ? ? yes Cl(1) O(5) 1.41(2) ? ? yes Cl(2) O(6) 1.41(1) ? ? yes Cl(2) O(7) 1.46(1) ? ? yes Cl(2) O(8) 1.43(1) ? ? yes Cl(2) O(9) 1.44(1) ? ? yes Cl(3) O(10) 1.41(1) ? ? yes Cl(3) O(11) 1.38(2) ? ? yes Cl(3) O(12) 1.47(2) ? ? yes Cl(3) O(13) 1.39(1) ? ? yes O(1) C(20) 1.37(2) ? ? yes O(3) O(3') 1.51(3) ? ? yes O(4) O(4') 0.82(3) ? ? yes O(5') O(5) 0.86(4) ? ? yes N(1) C(1) 1.48(2) ? ? yes N(1) C(6) 1.49(2) ? ? yes N(1) C(19) 1.49(2) ? ? yes N(2) C(2) 1.44(2) ? ? yes N(2) C(3) 1.50(2) ? ? yes N(2) C(13) 1.50(2) ? ? yes N(3) C(4) 1.47(2) ? ? yes N(3) C(5) 1.48(2) ? ? yes N(3) C(7) 1.45(2) ? ? yes N(4) C(8) 1.37(2) ? ? yes N(4) C(12) 1.34(2) ? ? yes N(5) C(14) 1.30(2) ? ? yes N(5) C(18) 1.33(2) ? ? yes N(6) C(21) 1.46(2) ? ? yes N(6) C(22) 1.51(2) ? ? yes N(6) C(27) 1.45(2) ? ? yes N(7) C(23) 1.47(2) ? ? yes N(7) C(24) 1.51(2) ? ? yes N(7) C(34) 1.45(2) ? ? yes N(8) C(25) 1.50(2) ? ? yes N(8) C(26) 1.48(2) ? ? yes N(8) C(28) 1.49(2) ? ? yes N(9) C(29) 1.35(2) ? ? yes N(9) C(33) 1.34(2) ? ? yes N(10) C(35) 1.33(2) ? ? yes N(10) C(39) 1.34(2) ? ? yes C(1) C(2) 1.52(2) ? ? yes C(3) C(4) 1.57(2) ? ? yes C(5) C(6) 1.49(2) ? ? yes C(7) C(8) 1.50(2) ? ? yes C(8) C(9) 1.37(2) ? ? yes C(9) C(10) 1.42(2) ? ? yes C(10) C(11) 1.32(2) ? ? yes C(11) C(12) 1.40(2) ? ? yes C(13) C(14) 1.51(2) ? ? yes C(14) C(15) 1.38(2) ? ? yes C(15) C(16) 1.36(2) ? ? yes C(16) C(17) 1.40(2) ? ? yes C(17) C(18) 1.37(2) ? ? yes C(19) C(20) 1.51(2) ? ? yes C(20) C(21) 1.56(2) ? ? yes C(22) C(23) 1.54(2) ? ? yes C(24) C(25) 1.52(2) ? ? yes C(26) C(27) 1.54(2) ? ? yes C(28) C(29) 1.52(2) ? ? yes C(29) C(30) 1.41(2) ? ? yes C(30) C(31) 1.37(2) ? ? yes C(31) C(32) 1.40(2) ? ? yes C(32) C(33) 1.38(2) ? ? yes C(34) C(35) 1.48(2) ? ? yes C(35) C(36) 1.38(2) ? ? yes C(36) C(37) 1.41(2) ? ? yes C(37) C(38) 1.29(2) ? ? yes C(38) C(39) 1.37(2) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Zn(1) N(1) 82.3(4) ? ? ? yes O(1) Zn(1) N(2) 162.4(5) ? ? ? yes O(1) Zn(1) N(3) 99.3(4) ? ? ? yes O(1) Zn(1) N(4) 100.9(4) ? ? ? yes O(1) Zn(1) N(5) 106.9(4) ? ? ? yes N(1) Zn(1) N(2) 80.1(5) ? ? ? yes N(1) Zn(1) N(3) 81.1(4) ? ? ? yes N(1) Zn(1) N(4) 160.3(4) ? ? ? yes N(1) Zn(1) N(5) 93.6(5) ? ? ? yes N(2) Zn(1) N(3) 78.4(4) ? ? ? yes N(2) Zn(1) N(4) 95.8(5) ? ? ? yes N(2) Zn(1) N(5) 74.0(4) ? ? ? yes N(3) Zn(1) N(4) 79.2(5) ? ? ? yes N(3) Zn(1) N(5) 152.4(4) ? ? ? yes N(4) Zn(1) N(5) 103.8(5) ? ? ? yes O(1) Zn(2) N(6) 82.4(4) ? ? ? yes O(1) Zn(2) N(7) 110.5(4) ? ? ? yes O(1) Zn(2) N(8) 159.2(4) ? ? ? yes O(1) Zn(2) N(9) 96.3(4) ? ? ? yes O(1) Zn(2) N(10) 105.2(4) ? ? ? yes N(6) Zn(2) N(7) 78.6(4) ? ? ? yes N(6) Zn(2) N(8) 81.1(5) ? ? ? yes N(6) Zn(2) N(9) 104.1(4) ? ? ? yes N(6) Zn(2) N(10) 154.4(4) ? ? ? yes N(7) Zn(2) N(8) 78.4(4) ? ? ? yes N(7) Zn(2) N(9) 153.1(4) ? ? ? yes N(7) Zn(2) N(10) 75.8(5) ? ? ? yes N(8) Zn(2) N(9) 75.7(4) ? ? ? yes N(8) Zn(2) N(10) 95.1(4) ? ? ? yes N(9) Zn(2) N(10) 99.4(4) ? ? ? yes O(2) Cl(1) O(3) 88(1) ? ? ? yes O(2) Cl(1) O(3') 151(1) ? ? ? yes O(2) Cl(1) O(4) 89(1) ? ? ? yes O(2) Cl(1) O(4') 110(1) ? ? ? yes O(2) Cl(1) O(5') 74(1) ? ? ? yes O(2) Cl(1) O(5) 101(1) ? ? ? yes O(3) Cl(1) O(3') 63(1) ? ? ? yes O(3) Cl(1) O(4) 108(1) ? ? ? yes O(3) Cl(1) O(4') 131(1) ? ? ? yes O(3) Cl(1) O(5') 106(1) ? ? ? yes O(3) Cl(1) O(5) 126(1) ? ? ? yes O(3') Cl(1) O(4) 106(1) ? ? ? yes O(3') Cl(1) O(4') 94(1) ? ? ? yes O(3') Cl(1) O(5') 105(1) ? ? ? yes O(3') Cl(1) O(5) 90(1) ? ? ? yes O(4) Cl(1) O(4') 32(1) ? ? ? yes O(4) Cl(1) O(5') 140(1) ? ? ? yes O(4) Cl(1) O(5) 123(1) ? ? ? yes O(4') Cl(1) O(5') 121(2) ? ? ? yes O(4') Cl(1) O(5) 93(1) ? ? ? yes O(5') Cl(1) O(5) 33(1) ? ? ? yes O(6) Cl(2) O(7) 110.7(7) ? ? ? yes O(6) Cl(2) O(8) 108.6(7) ? ? ? yes O(6) Cl(2) O(9) 109.4(8) ? ? ? yes O(7) Cl(2) O(8) 106.4(8) ? ? ? yes O(7) Cl(2) O(9) 111.9(7) ? ? ? yes O(8) Cl(2) O(9) 109.7(7) ? ? ? yes O(10) Cl(3) O(11) 110.6(10) ? ? ? yes O(10) Cl(3) O(12) 108.7(9) ? ? ? yes O(10) Cl(3) O(13) 109.6(9) ? ? ? yes O(11) Cl(3) O(12) 110(1) ? ? ? yes O(11) Cl(3) O(13) 110(1) ? ? ? yes O(12) Cl(3) O(13) 106.7(9) ? ? ? yes Zn(1) O(1) Zn(2) 139.1(5) ? ? ? yes Zn(1) O(1) C(20) 112.1(8) ? ? ? yes Zn(2) O(1) C(20) 108.7(8) ? ? ? yes Cl(1) O(3) O(3') 60(1) ? ? ? yes Cl(1) O(3') O(3) 55(1) ? ? ? yes Cl(1) O(4) O(4') 83(3) ? ? ? yes Cl(1) O(4') O(4) 64(2) ? ? ? yes Cl(1) O(5') O(5) 65(3) ? ? ? yes Cl(1) O(5) O(5') 80(3) ? ? ? yes Zn(1) N(1) C(1) 107.4(9) ? ? ? yes Zn(1) N(1) C(6) 109.6(9) ? ? ? yes Zn(1) N(1) C(19) 102.2(8) ? ? ? yes C(1) N(1) C(6) 110(1) ? ? ? yes C(1) N(1) C(19) 113(1) ? ? ? yes C(6) N(1) C(19) 113(1) ? ? ? yes Zn(1) N(2) C(2) 108.2(9) ? ? ? yes Zn(1) N(2) C(3) 105.0(9) ? ? ? yes Zn(1) N(2) C(13) 102.9(9) ? ? ? yes C(2) N(2) C(3) 116(1) ? ? ? yes C(2) N(2) C(13) 114(1) ? ? ? yes C(3) N(2) C(13) 108(1) ? ? ? yes Zn(1) N(3) C(4) 111.0(8) ? ? ? yes Zn(1) N(3) C(5) 101.1(8) ? ? ? yes Zn(1) N(3) C(7) 103.0(8) ? ? ? yes C(4) N(3) C(5) 112(1) ? ? ? yes C(4) N(3) C(7) 112(1) ? ? ? yes C(5) N(3) C(7) 115(1) ? ? ? yes Zn(1) N(4) C(8) 114.8(10) ? ? ? yes Zn(1) N(4) C(12) 125.5(10) ? ? ? yes C(8) N(4) C(12) 118(1) ? ? ? yes Zn(1) N(5) C(14) 115.3(10) ? ? ? yes Zn(1) N(5) C(18) 128.2(9) ? ? ? yes C(14) N(5) C(18) 116(1) ? ? ? yes Zn(2) N(6) C(21) 103.5(8) ? ? ? yes Zn(2) N(6) C(22) 112.8(8) ? ? ? yes Zn(2) N(6) C(27) 102.0(9) ? ? ? yes C(21) N(6) C(22) 111(1) ? ? ? yes C(21) N(6) C(27) 112(1) ? ? ? yes C(22) N(6) C(27) 113(1) ? ? ? yes Zn(2) N(7) C(23) 105.2(8) ? ? ? yes Zn(2) N(7) C(24) 109.0(8) ? ? ? yes Zn(2) N(7) C(34) 104.1(8) ? ? ? yes C(23) N(7) C(24) 111(1) ? ? ? yes C(23) N(7) C(34) 114(1) ? ? ? yes C(24) N(7) C(34) 111(1) ? ? ? yes Zn(2) N(8) C(25) 106.4(9) ? ? ? yes Zn(2) N(8) C(26) 108(1) ? ? ? yes Zn(2) N(8) C(28) 108.7(8) ? ? ? yes C(25) N(8) C(26) 112(1) ? ? ? yes C(25) N(8) C(28) 107(1) ? ? ? yes C(26) N(8) C(28) 113(1) ? ? ? yes Zn(2) N(9) C(29) 117.2(8) ? ? ? yes Zn(2) N(9) C(33) 124.3(9) ? ? ? yes C(29) N(9) C(33) 117(1) ? ? ? yes Zn(2) N(10) C(35) 117.8(10) ? ? ? yes Zn(2) N(10) C(39) 123.8(9) ? ? ? yes C(35) N(10) C(39) 118(1) ? ? ? yes N(1) C(1) C(2) 112(1) ? ? ? yes N(2) C(2) C(1) 114(1) ? ? ? yes N(2) C(3) C(4) 106(1) ? ? ? yes N(3) C(4) C(3) 112(1) ? ? ? yes N(3) C(5) C(6) 109(1) ? ? ? yes N(1) C(6) C(5) 114(1) ? ? ? yes N(3) C(7) C(8) 112(1) ? ? ? yes N(4) C(8) C(7) 113(1) ? ? ? yes N(4) C(8) C(9) 123(1) ? ? ? yes C(7) C(8) C(9) 122(1) ? ? ? yes C(8) C(9) C(10) 116(1) ? ? ? yes C(9) C(10) C(11) 119(1) ? ? ? yes C(10) C(11) C(12) 122(1) ? ? ? yes N(4) C(12) C(11) 119(1) ? ? ? yes N(2) C(13) C(14) 110(1) ? ? ? yes N(5) C(14) C(13) 114(1) ? ? ? yes N(5) C(14) C(15) 124(1) ? ? ? yes C(13) C(14) C(15) 121(1) ? ? ? yes C(14) C(15) C(16) 120(1) ? ? ? yes C(15) C(16) C(17) 116(1) ? ? ? yes C(16) C(17) C(18) 118(1) ? ? ? yes N(5) C(18) C(17) 124(1) ? ? ? yes N(1) C(19) C(20) 109(1) ? ? ? yes O(1) C(20) C(19) 113(1) ? ? ? yes O(1) C(20) C(21) 108(1) ? ? ? yes C(19) C(20) C(21) 109(1) ? ? ? yes N(6) C(21) C(20) 108(1) ? ? ? yes N(6) C(22) C(23) 113(1) ? ? ? yes N(7) C(23) C(22) 110(1) ? ? ? yes N(7) C(24) C(25) 113(1) ? ? ? yes N(8) C(25) C(24) 110(1) ? ? ? yes N(8) C(26) C(27) 110(1) ? ? ? yes N(6) C(27) C(26) 113(1) ? ? ? yes N(8) C(28) C(29) 108(1) ? ? ? yes N(9) C(29) C(28) 114(1) ? ? ? yes N(9) C(29) C(30) 122(1) ? ? ? yes C(28) C(29) C(30) 122(1) ? ? ? yes C(29) C(30) C(31) 117(1) ? ? ? yes C(30) C(31) C(32) 121(1) ? ? ? yes C(31) C(32) C(33) 116(1) ? ? ? yes N(9) C(33) C(32) 124(1) ? ? ? yes N(7) C(34) C(35) 113(1) ? ? ? yes N(10) C(35) C(34) 115(1) ? ? ? yes N(10) C(35) C(36) 121(1) ? ? ? yes C(34) C(35) C(36) 122(1) ? ? ? yes C(35) C(36) C(37) 117(1) ? ? ? yes C(36) C(37) C(38) 119(1) ? ? ? yes C(37) C(38) C(39) 121(1) ? ? ? yes N(10) C(39) C(38) 121(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Trans ' _publ_contact_author ; Dr ERT TIEKINK, Department of Chemistry, The University of Adelaide, AUSTRALIA 5005 ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 8 8303 5943 ' _publ_contact_author_fax ' 61 8 8303 4358 ' _publ_contact_author_email ' etiekink@chemistry.adelaide.edu.au '