#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_B008687H _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Buntine, Mark A.' 'Lincoln, S.' 'Tiekink, Edward R. T.' 'Wainwright, K.' 'Weeks, Jennifer M.' _publ_contact_author_name 'Prof S Lincoln' _publ_contact_author_address ; Prof S Lincoln Department of Chemistry University of Adelaide Adelaide SA 5005 AUSTRALIA ; _publ_contact_author_email 'STEPHEN.LINCOLN@ADELAIDE.EDU.AU' #============================================================================== _audit_creation_date '1999-09-02' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Dalton Trans ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr ERT Tiekink ' _publ_contact_author_address ; Department of Chemistry, The University of Adelaide, AUSTRALIA 5005 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 8 8303 5943 ' _publ_contact_author_fax ' 61 8 8303 4358 ' _publ_contact_author_email ' edward.tiekink@adelaide.edu.au ' #============================================================================== data__sthpc9 _database_code_CSD 164174 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 17.6183(6) _cell_length_b 10.4941(2) _cell_length_c 14.4786(5) _cell_angle_alpha 90 _cell_angle_beta 123.5040(10) _cell_angle_gamma 90 _cell_volume 2232.14(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _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 ' _symmetry_Int_Tables_number 5 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y, -z' '1/2+x,1/2+y, +z' '1/2-x,1/2+y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 535.73 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H33 Cl2 N3 O9 Zn ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.391 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_correction_T_min 0.729 _exptl_special_details ; ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method \w-2\q _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 17857 _reflns_number_total 7443 _reflns_number_gt 4797 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.099 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_theta_max 30.1 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 60 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 12 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 36 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Zn 0 4 0.222 1.431 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zn -0.96041(3) 0.0000 0.20049(4) 0.02360(12) 1.000 . Uani d ? Cl(1) -0.72030(10) -0.03506(10) -0.25538(10) 0.0388(4) 1.000 . Uani d ? Cl(2) 0.0000 0.4623(2) 0.5000 0.0619(7) 0.500 ST Uani d ? Cl(3) 0.0000 0.3231(4) 1.0000 0.133(2) 0.500 ST Uani d ? O(1) -0.8854(2) 0.0356(4) 0.1246(3) 0.0419(11) 1.000 . Uani d ? O(4) -1.0398(2) 0.1619(3) 0.1159(3) 0.0285(10) 1.000 . Uani d ? O(7) -1.0439(3) -0.1086(3) 0.0548(3) 0.0378(10) 1.000 . Uani d ? O(11) -0.7433(3) 0.0935(3) -0.2910(3) 0.0473(12) 1.000 . Uani d ? O(12) -0.6297(4) -0.0541(6) -0.2059(6) 0.109(2) 1.000 . Uani d ? O(13) -0.7397(4) -0.0566(4) -0.1703(4) 0.081(2) 1.000 . Uani d ? O(14) -0.7774(4) -0.1189(4) -0.3433(3) 0.083(2) 1.000 . Uani d ? O(15) -0.0739(4) 0.3859(5) 0.4303(6) 0.105(2) 1.000 . Uani d ? O(16) 0.0254(11) 0.542(1) 0.4512(11) 0.377(9) 1.000 . Uani d ? N(1) -0.8238(2) -0.0041(5) 0.3409(3) 0.0250(9) 1.000 . Uani d ? N(4) -0.9833(3) 0.0807(4) 0.3210(3) 0.0295(12) 1.000 . Uani d ? N(7) -0.9687(3) -0.1763(3) 0.2735(3) 0.0236(10) 1.000 . Uani d ? C(2) -0.8157(4) 0.0617(6) 0.4356(4) 0.046(2) 1.000 . Uani d ? C(3) -0.8950(4) 0.1471(5) 0.4000(4) 0.040(2) 1.000 . Uani d ? C(5) -1.0018(4) -0.0215(5) 0.3753(5) 0.043(2) 1.000 . Uani d ? C(6) -1.0293(4) -0.1437(6) 0.3135(4) 0.037(2) 1.000 . Uani d ? C(8) -0.8735(4) -0.2124(5) 0.3647(4) 0.039(1) 1.000 . Uani d ? C(9) -0.8052(3) -0.1431(5) 0.3603(4) 0.035(1) 1.000 . Uani d ? C(10) -0.7640(3) 0.0643(4) 0.3128(4) 0.0318(13) 1.000 . Uani d ? C(11) -0.7863(3) 0.0247(4) 0.2003(4) 0.0290(13) 1.000 . Uani d ? C(12) -0.7376(4) 0.1069(5) 0.1633(6) 0.047(2) 1.000 . Uani d ? C(13) -1.0610(4) 0.1658(5) 0.2632(5) 0.032(2) 1.000 . Uani d ? C(14) -1.0560(4) 0.2518(4) 0.1788(5) 0.035(2) 1.000 . Uani d ? C(15) -1.1403(4) 0.3233(5) 0.1059(5) 0.052(2) 1.000 . Uani d ? C(16) -1.0111(3) -0.2729(4) 0.1847(4) 0.0234(12) 1.000 . Uani d ? C(17) -1.0825(3) -0.2154(4) 0.0763(4) 0.0265(12) 1.000 . Uani d ? C(18) -1.1219(4) -0.3081(4) -0.0178(4) 0.034(1) 1.000 . Uani d ? H(11) -0.7690 -0.0617 0.2032 0.035 1.000 . Uiso c ? H(14) -1.0061 0.3089 0.2173 0.042 1.000 . Uiso c ? H(17) -1.1303 -0.1852 0.0825 0.032 1.000 . Uiso c ? H(21) -0.8125 -0.0001 0.4856 0.055 1.000 . Uiso c ? H(22) -0.7616 0.1113 0.4719 0.055 1.000 . Uiso c ? H(31) -0.8902 0.2200 0.3646 0.048 1.000 . Uiso c ? H(32) -0.8942 0.1729 0.4634 0.048 1.000 . Uiso c ? H(51) -0.9483 -0.0358 0.4465 0.052 1.000 . Uiso c ? H(52) -1.0495 0.0057 0.3830 0.052 1.000 . Uiso c ? H(61) -1.0904 -0.1367 0.2514 0.045 1.000 . Uiso c ? H(62) -1.0254 -0.2098 0.3608 0.045 1.000 . Uiso c ? H(81) -0.8658 -0.1957 0.4338 0.046 1.000 . Uiso c ? H(82) -0.8653 -0.3008 0.3589 0.046 1.000 . Uiso c ? H(91) -0.8018 -0.1771 0.3018 0.042 1.000 . Uiso c ? H(92) -0.7484 -0.1545 0.4287 0.042 1.000 . Uiso c ? H(101) -0.7731 0.1535 0.3126 0.038 1.000 . Uiso c ? H(102) -0.7021 0.0445 0.3669 0.038 1.000 . Uiso c ? H(121) -0.7021 0.1691 0.2184 0.057 1.000 . Uiso c ? H(122) -0.6989 0.0552 0.1523 0.057 1.000 . Uiso c ? H(123) -0.7810 0.1482 0.0958 0.057 1.000 . Uiso c ? H(131) -1.1152 0.1165 0.2245 0.038 1.000 . Uiso c ? H(132) -1.0620 0.2186 0.3159 0.038 1.000 . Uiso c ? H(151) -1.1307 0.4107 0.1267 0.062 1.000 . Uiso c ? H(152) -1.1575 0.3155 0.0314 0.062 1.000 . Uiso c ? H(153) -1.1873 0.2902 0.1125 0.062 1.000 . Uiso c ? H(161) -0.9654 -0.3101 0.1776 0.028 1.000 . Uiso c ? H(162) -1.0382 -0.3369 0.2038 0.028 1.000 . Uiso c ? H(181) -1.1515 -0.3749 -0.0053 0.040 1.000 . Uiso c ? H(182) -1.1646 -0.2655 -0.0849 0.040 1.000 . Uiso c ? H(183) -1.0745 -0.3426 -0.0230 0.040 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 Zn 0.0204(2) 0.0224(2) 0.0214(3) -0.0002(3) 0.0073(2) -0.0009(2) Cl(1) 0.0516(9) 0.0171(6) 0.0253(7) -0.0026(5) 0.0071(6) 0.0026(4) Cl(2) 0.0274(11) 0.0418(11) 0.078(2) 0.0000 0.0052(11) 0.0000 Cl(3) 0.136(4) 0.122(3) 0.129(3) 0.0000 0.066(3) 0.0000 O(1) 0.012(2) 0.084(3) 0.023(2) 0.004(2) 0.005(2) 0.001(2) O(4) 0.035(2) 0.031(2) 0.028(2) 0.005(2) 0.023(2) -0.003(1) O(7) 0.056(3) 0.020(2) 0.021(2) -0.006(2) 0.011(2) -0.0002(13) O(11) 0.077(3) 0.018(2) 0.040(3) -0.001(2) 0.027(2) -0.001(2) O(12) 0.097(5) 0.117(5) 0.123(5) 0.045(4) 0.068(4) 0.045(4) O(13) 0.136(5) 0.057(3) 0.044(3) -0.046(3) 0.046(3) -0.010(2) O(14) 0.148(6) 0.025(2) 0.021(2) -0.018(3) 0.012(3) -0.007(2) O(15) 0.067(4) 0.064(3) 0.135(6) -0.006(3) 0.026(4) -0.038(3) O(16) 0.28(2) 0.32(2) 0.27(2) -0.10(2) -0.021(13) 0.22(2) N(1) 0.013(2) 0.036(2) 0.014(2) 0.002(2) 0.000(1) 0.003(2) N(4) 0.039(3) 0.035(2) 0.020(2) 0.009(2) 0.019(2) 0.004(2) N(7) 0.027(2) 0.024(2) 0.013(2) -0.003(2) 0.006(2) 0.003(1) C(2) 0.024(3) 0.073(4) 0.018(3) -0.018(3) -0.002(2) -0.008(2) C(3) 0.053(4) 0.032(3) 0.024(3) -0.001(3) 0.014(3) -0.018(2) C(5) 0.056(3) 0.043(3) 0.044(3) 0.010(3) 0.036(3) 0.012(3) C(6) 0.047(4) 0.049(3) 0.013(3) -0.011(3) 0.014(3) 0.002(2) C(8) 0.035(3) 0.038(3) 0.017(3) 0.013(2) -0.002(2) 0.006(2) C(9) 0.017(3) 0.036(3) 0.033(3) 0.008(2) 0.002(2) 0.012(2) C(10) 0.021(3) 0.025(2) 0.030(3) -0.007(2) 0.002(2) -0.005(2) C(11) 0.014(2) 0.022(3) 0.048(3) 0.008(2) 0.016(2) 0.002(2) C(12) 0.048(4) 0.029(3) 0.081(5) -0.001(2) 0.045(4) 0.002(3) C(13) 0.035(3) 0.038(3) 0.036(3) -0.001(2) 0.029(3) -0.009(2) C(14) 0.029(3) 0.024(2) 0.053(4) 0.001(2) 0.023(3) -0.008(2) C(15) 0.061(4) 0.044(3) 0.059(4) 0.037(3) 0.038(4) 0.020(3) C(16) 0.022(3) 0.021(2) 0.020(3) -0.008(2) 0.007(2) -0.002(2) C(17) 0.020(3) 0.020(2) 0.023(2) 0.001(2) 0.002(2) -0.003(2) C(18) 0.032(3) 0.031(3) 0.031(3) -0.006(2) 0.013(3) -0.010(2) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _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 4797 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.065 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.075 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.13 _refine_ls_shift/su_max '<0.001' _refine_ls_shift/su_mean 0.000 _refine_diff_density_min -0.92 _refine_diff_density_max 0.97 #============================================================================== # MOLECULAR GEOMETRY _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 O1 2.167(5) . . ? ZN O4 2.110(5) . . ? ZN O7 2.118(5) . . ? ZN N1 2.128(4) . . ? ZN N4 2.168(6) . . ? ZN N7 2.175(5) . . ? CL1 O11 1.421(5) . . ? CL1 O12 1.356(9) . . ? CL1 O13 1.466(7) . . ? CL1 O14 1.411(6) . . ? CL2 O15 1.380(8) . . ? CL2 O15 1.380(8) . . ? CL2 O16 1.32(2) . . ? CL2 O16 1.32(2) . . ? O1 C11 1.467(8) . . ? O4 C14 1.445(9) . . ? O7 C17 1.431(8) . . ? N1 C2 1.470(10) . . ? N1 C9 1.488(10) . . ? N1 C10 1.505(9) . . ? N4 C3 1.500(10) . . ? N4 C5 1.469(9) . . ? N4 C13 1.451(10) . . ? N7 C6 1.507(10) . . ? N7 C8 1.503(9) . . ? N7 C16 1.477(8) . . ? C2 C3 1.492(12) . . ? C2 H21 0.95 . . no C2 H22 0.95 . . no C3 H31 0.95 . . no C3 H32 0.95 . . no C5 C6 1.485(12) . . ? C5 H51 0.95 . . no C5 H52 0.95 . . no C6 H61 0.95 . . no C6 H62 0.95 . . no C8 C9 1.437(11) . . ? C8 H81 0.95 . . no C8 H82 0.95 . . no C9 H91 0.95 . . no C9 H92 0.95 . . no C10 C11 1.507(10) . . ? C10 H101 0.95 . . no C10 H102 0.95 . . no C11 C12 1.510(10) . . ? C11 H11 0.95 . . no C12 H121 0.95 . . no C12 H122 0.95 . . no C12 H123 0.95 . . no C13 C14 1.560(11) . . ? C13 H131 0.95 . . no C13 H132 0.95 . . no C14 C15 1.467(11) . . ? C14 H14 0.95 . . no C15 H151 0.95 . . no C15 H152 0.95 . . no C15 H153 0.95 . . no C16 C17 1.493(9) . . ? C16 H161 0.95 . . no C16 H162 0.95 . . no C17 C18 1.497(9) . . ? C17 H17 0.95 . . no C18 H181 0.95 . . no C18 H182 0.95 . . no C18 H183 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 O1 ZN O4 87.8(2) . . . ? O1 ZN O7 82.6(2) . . . ? O1 ZN N1 78.6(2) . . . ? O1 ZN N4 141.0(2) . . . ? O1 ZN N7 128.1(2) . . . ? O4 ZN O7 89.0(2) . . . ? O4 ZN N1 127.5(2) . . . ? O4 ZN N4 78.1(2) . . . ? O4 ZN N7 140.0(2) . . . ? O7 ZN N1 137.6(2) . . . ? O7 ZN N4 132.5(2) . . . ? O7 ZN N7 80.2(2) . . . ? N1 ZN N4 81.6(2) . . . ? N1 ZN N7 82.1(2) . . . ? N4 ZN N7 81.3(2) . . . ? O11 CL1 O12 110.4(5) . . . ? O11 CL1 O13 107.4(4) . . . ? O11 CL1 O14 110.3(4) . . . ? O12 CL1 O13 106.6(5) . . . ? O12 CL1 O14 115.4(6) . . . ? O13 CL1 O14 106.3(4) . . . ? O15 CL2 O15 109.0(7) . . . ? O15 CL2 O16 116.0(10) . . . ? O15 CL2 O16 107.3(11) . . . ? O15 CL2 O16 107.3(11) 2_556 2_556 2_556 ? O15 CL2 O16 116.0(10) 2_556 2_556 2_556 ? O16 CL2 O16 101.5(25) . . . ? ZN O1 C11 114.5(4) . . . ? ZN O4 C14 117.2(4) . . . ? ZN O7 C17 110.9(4) . . . ? ZN N1 C2 111.0(4) . . . ? ZN N1 C9 102.4(4) . . . ? ZN N1 C10 108.9(4) . . . ? C2 N1 C9 112.8(6) . . . ? C2 N1 C10 107.9(6) . . . ? C9 N1 C10 113.8(5) . . . ? ZN N4 C3 102.7(4) . . . ? ZN N4 C5 109.9(4) . . . ? ZN N4 C13 108.2(4) . . . ? C3 N4 C5 111.9(6) . . . ? C3 N4 C13 113.9(6) . . . ? C5 N4 C13 109.9(6) . . . ? ZN N7 C6 104.2(4) . . . ? ZN N7 C8 107.4(4) . . . ? ZN N7 C16 107.3(4) . . . ? C6 N7 C8 113.8(5) . . . ? C6 N7 C16 111.4(5) . . . ? C8 N7 C16 112.0(5) . . . ? N1 C2 C3 111.7(6) . . . ? N1 C2 H21 108.9 . . . no N1 C2 H22 108.9 . . . no C3 C2 H21 108.9 . . . no C3 C2 H22 108.9 . . . no H21 C2 H22 109.5 . . . no N4 C3 C2 111.4(6) . . . ? N4 C3 H31 109.0 . . . no N4 C3 H32 109.0 . . . no C2 C3 H31 109.0 . . . no C2 C3 H32 109.0 . . . no H31 C3 H32 109.5 . . . no N4 C5 C6 113.8(6) . . . ? N4 C5 H51 108.4 . . . no N4 C5 H52 108.4 . . . no C6 C5 H51 108.4 . . . no C6 C5 H52 108.4 . . . no H51 C5 H52 109.5 . . . no N7 C6 C5 111.3(6) . . . ? N7 C6 H61 109.0 . . . no N7 C6 H62 109.0 . . . no C5 C6 H61 109.0 . . . no C5 C6 H62 109.0 . . . no H61 C6 H62 109.5 . . . no N7 C8 C9 112.9(6) . . . ? N7 C8 H81 108.6 . . . no N7 C8 H82 108.6 . . . no C9 C8 H81 108.6 . . . no C9 C8 H82 108.6 . . . no H81 C8 H82 109.5 . . . no N1 C9 C8 113.7(6) . . . ? N1 C9 H91 108.4 . . . no N1 C9 H92 108.4 . . . no C8 C9 H91 108.4 . . . no C8 C9 H92 108.4 . . . no H91 C9 H92 109.5 . . . no N1 C10 C11 110.9(5) . . . ? N1 C10 H101 109.1 . . . no N1 C10 H102 109.1 . . . no C11 C10 H101 109.1 . . . no C11 C10 H102 109.1 . . . no H101 C10 H102 109.5 . . . no O1 C11 C10 106.2(5) . . . ? O1 C11 C12 111.5(6) . . . ? O1 C11 H11 109.2 . . . no C10 C11 C12 111.5(6) . . . ? C10 C11 H11 109.2 . . . no C12 C11 H11 109.2 . . . no C11 C12 H121 109.5 . . . no C11 C12 H122 109.5 . . . no C11 C12 H123 109.5 . . . no H121 C12 H122 109.5 . . . no H121 C12 H123 109.5 . . . no H122 C12 H123 109.5 . . . no N4 C13 C14 111.4(6) . . . ? N4 C13 H131 109.0 . . . no N4 C13 H132 109.0 . . . no C14 C13 H131 109.0 . . . no C14 C13 H132 109.0 . . . no H131 C13 H132 109.5 . . . no O4 C14 C13 103.5(5) . . . ? O4 C14 C15 110.7(7) . . . ? O4 C14 H14 109.9 . . . no C13 C14 C15 112.7(7) . . . ? C13 C14 H14 109.9 . . . no C15 C14 H14 109.9 . . . no C14 C15 H151 109.5 . . . no C14 C15 H152 109.5 . . . no C14 C15 H153 109.5 . . . no H151 C15 H152 109.5 . . . no H151 C15 H153 109.5 . . . no H152 C15 H153 109.5 . . . no N7 C16 C17 111.4(5) . . . ? N7 C16 H161 109.0 . . . no N7 C16 H162 109.0 . . . no C17 C16 H161 109.0 . . . no C17 C16 H162 109.0 . . . no H161 C16 H162 109.5 . . . no O7 C17 C16 108.7(5) . . . ? O7 C17 C18 110.3(6) . . . ? O7 C17 H17 108.2 . . . no C16 C17 C18 113.1(5) . . . ? C16 C17 H17 108.2 . . . no C18 C17 H17 108.2 . . . no C17 C18 H181 109.5 . . . no C17 C18 H182 109.5 . . . no C17 C18 H183 109.5 . . . no H181 C18 H182 109.5 . . . no H181 C18 H183 109.5 . . . no H182 C18 H183 109.5 . . . 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 O1 O7 2.649(7) . 2_355 no O1 O4 3.248(7) . 2_355 no O7 O7 2.761(11) . 2_355 no O7 C11 3.514(9) . 2_355 no O11 C9 3.212(9) . 4_355 no O11 C2 3.439(10) . 1_554 no O11 C8 3.455(10) . 4_355 no O11 C18 3.456(9) . 3 no O13 C18 3.305(9) . 3 no O13 C6 3.519(11) . 2_355 no O13 C12 3.562(9) . 4_345 no O13 C15 3.594(10) . 3_545 no O14 C10 3.379(8) . 4_345 no O14 C2 3.451(10) . 1_554 no O15 C10 3.365(11) . 3 no O15 C13 3.442(11) . 1_655 no C5 C5 3.58(2) . 2_356 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 ZN O1 C11 C10 . . . . -31.2(6) no ZN O1 C11 C12 . . . . -152.7(5) no ZN O4 C14 C13 . . . . -33.5(6) no ZN O4 C14 C15 . . . . -154.6(5) no ZN O7 C17 C16 . . . . -41.6(6) no ZN O7 C17 C18 . . . . -166.1(4) no ZN N1 C2 C3 . . . . -18.2(8) no ZN N1 C9 C8 . . . . -50.7(7) no ZN N1 C10 C11 . . . . -45.0(6) no ZN N4 C3 C2 . . . . -49.4(7) no ZN N4 C5 C6 . . . . -18.4(8) no ZN N4 C13 C14 . . . . -44.2(7) no ZN N7 C6 C5 . . . . -46.8(6) no ZN N7 C8 C9 . . . . -14.4(7) no ZN N7 C16 C17 . . . . -35.9(7) no O1 ZN O4 C14 . . . . -133.6(5) no O1 ZN O7 C17 . . . . 148.2(4) no O1 ZN N1 C2 . . . . 138.9(5) no O1 ZN N1 C9 . . . . -100.5(4) no O1 ZN N1 C10 . . . . 20.3(4) no O1 ZN N4 C3 . . . . -30.3(6) no O1 ZN N4 C5 . . . . -149.6(4) no O1 ZN N4 C13 . . . . 90.4(6) no O1 ZN N7 C6 . . . . 179.5(4) no O1 ZN N7 C8 . . . . 58.4(5) no O1 ZN N7 C16 . . . . -62.2(5) no O1 C11 C10 N1 . . . . 49.5(7) no O4 ZN O1 C11 . . . . 135.4(4) no O4 ZN O7 C17 . . . . -123.9(4) no O4 ZN N1 C2 . . . . 60.7(5) no O4 ZN N1 C9 . . . . -178.7(4) no O4 ZN N1 C10 . . . . -57.9(5) no O4 ZN N4 C3 . . . . -101.5(4) no O4 ZN N4 C5 . . . . 139.2(5) no O4 ZN N4 C13 . . . . 19.2(5) no O4 ZN N7 C6 . . . . -31.6(5) no O4 ZN N7 C8 . . . . -152.7(4) no O4 ZN N7 C16 . . . . 86.7(5) no O4 C14 C13 N4 . . . . 50.6(8) no O7 ZN O1 C11 . . . . -135.3(4) no O7 ZN O4 C14 . . . . 143.8(5) no O7 ZN N1 C2 . . . . -155.6(5) no O7 ZN N1 C9 . . . . -35.0(5) no O7 ZN N1 C10 . . . . 85.8(5) no O7 ZN N4 C3 . . . . -178.9(4) no O7 ZN N4 C5 . . . . 61.8(6) no O7 ZN N4 C13 . . . . -58.2(6) no O7 ZN N7 C6 . . . . -108.1(4) no O7 ZN N7 C8 . . . . 130.8(4) no O7 ZN N7 C16 . . . . 10.2(4) no O7 C17 C16 N7 . . . . 52.5(7) no N1 ZN O1 C11 . . . . 6.4(4) no N1 ZN O4 C14 . . . . -59.8(5) no N1 ZN O7 C17 . . . . 84.1(5) no N1 ZN N4 C3 . . . . 29.8(4) no N1 ZN N4 C5 . . . . -89.5(5) no N1 ZN N4 C13 . . . . 150.5(5) no N1 ZN N7 C6 . . . . 110.7(4) no N1 ZN N7 C8 . . . . -10.4(4) no N1 ZN N7 C16 . . . . -131.1(4) no N1 C2 C3 N4 . . . . 47.1(9) no N1 C9 C8 N7 . . . . 45.4(8) no N1 C10 C11 C12 . . . . 171.1(6) no N4 ZN O1 C11 . . . . 67.5(5) no N4 ZN O4 C14 . . . . 9.8(5) no N4 ZN O7 C17 . . . . -51.1(5) no N4 ZN N1 C2 . . . . -7.3(5) no N4 ZN N1 C9 . . . . 113.3(4) no N4 ZN N1 C10 . . . . -125.8(5) no N4 ZN N7 C6 . . . . 28.0(4) no N4 ZN N7 C8 . . . . -93.1(4) no N4 ZN N7 C16 . . . . 146.3(5) no N4 C5 C6 N7 . . . . 45.3(9) no N4 C13 C14 C15 . . . . 170.3(7) no N7 ZN O1 C11 . . . . -64.0(5) no N7 ZN O4 C14 . . . . 70.4(5) no N7 ZN O7 C17 . . . . 17.4(4) no N7 ZN N1 C2 . . . . -89.6(5) no N7 ZN N1 C9 . . . . 31.0(4) no N7 ZN N1 C10 . . . . 151.9(5) no N7 ZN N4 C3 . . . . 113.0(4) no N7 ZN N4 C5 . . . . -6.2(5) no N7 ZN N4 C13 . . . . -126.3(5) no N7 C16 C17 C18 . . . . 175.3(6) no C2 N1 C9 C8 . . . . 68.7(8) no C2 N1 C10 C11 . . . . -165.5(6) no C2 C3 N4 C5 . . . . 68.4(8) no C2 C3 N4 C13 . . . . -166.1(6) no C3 N4 C5 C6 . . . . -131.9(7) no C3 N4 C13 C14 . . . . 69.2(8) no C3 C2 N1 C9 . . . . -132.4(6) no C3 C2 N1 C10 . . . . 101.0(7) no C5 N4 C13 C14 . . . . -164.2(6) no C5 C6 N7 C8 . . . . 69.9(7) no C5 C6 N7 C16 . . . . -162.3(6) no C6 N7 C8 C9 . . . . -129.2(7) no C6 N7 C16 C17 . . . . 77.6(7) no C6 C5 N4 C13 . . . . 100.5(8) no C8 N7 C16 C17 . . . . -153.5(6) no C8 C9 N1 C10 . . . . -168.0(6) no C9 N1 C10 C11 . . . . 68.5(6) no C9 C8 N7 C16 . . . . 103.2(7) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================