Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;A single entity comprising up to four phenoxyl radicals coordinated to two metal ions (CuII or ZnII) ; _publ_contact_author_name 'Thomas Fabrice' _publ_contact_author_email FABRICE.THOMAS@UJF-GRENOBLE.FR loop_ _publ_author_name 'Thomas Fabrice' 'Olivier Jarjayes' 'Christian Philouze' 'Jean-Louis Pierre' 'Olaf Rotthaus' ; E.Saint-Aman ; # Attachment 'CCDC-603806.cif' data_Olivier1_Moitie _database_code_depnum_ccdc_archive 'CCDC 603806' #------------------------------------------------------------------------------ _audit_creation_date 2006-12-05 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _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. ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-Enraf-Nonius kappaCCD' _computing_cell_refinement 'Bruker-Enraf-Nonius kappaCCD' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 11.8822(8) _cell_length_b 25.396(2) _cell_length_c 13.130(1) _cell_angle_alpha 90 _cell_angle_beta 92.2(3) _cell_angle_gamma 90 _cell_volume 3958.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293.0 _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/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 696.29 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H58 N2 O4 Zn1 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1496.00 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Bruker-Enraf-Nonius kappaCCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _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 23265 _reflns_number_total 6660 _reflns_number_gt 3442 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.07167 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 30.00 _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 Zn 0 4 0.222 1.431 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 160 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 232 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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 0.69389(4) 0.07741(2) 0.02652(4) 0.0386(1) 1.000 . Uani d ? O(1) 0.7074(3) 0.1259(1) -0.0863(3) 0.052(1) 1.000 . Uani d ? O(2) 0.6567(3) 0.1311(1) 0.1268(3) 0.048(1) 1.000 . Uani d ? O(3) 0.8694(3) 0.0646(2) 0.0688(3) 0.065(1) 1.000 . Uani d ? O(4) 0.0313(8) 0.0477(5) 0.9261(9) 0.142(4) 0.667 . Uani d ? O(4") -0.007(1) 0.0987(9) 0.902(2) 0.158(8) 0.333 . Uani d ? N(1) 0.6910(3) 0.0149(1) -0.0771(3) 0.035(1) 1.000 . Uani d ? N(2) 0.6179(3) 0.0203(1) 0.1098(3) 0.034(1) 1.000 . Uani d ? C(1) 0.7172(4) 0.0183(2) -0.1719(4) 0.041(1) 1.000 . Uani d ? C(2) 0.7474(4) 0.0668(2) -0.2215(4) 0.041(1) 1.000 . Uani d ? C(3) 0.7421(4) 0.1175(2) -0.1775(4) 0.039(1) 1.000 . Uani d ? C(4) 0.7756(4) 0.1619(2) -0.2376(4) 0.042(1) 1.000 . Uani d ? C(5) 0.8139(4) 0.1526(2) -0.3337(4) 0.045(1) 1.000 . Uani d ? C(6) 0.8206(4) 0.1027(2) -0.3791(4) 0.050(2) 1.000 . Uani d ? C(7) 0.7859(4) 0.0611(2) -0.3236(4) 0.048(1) 1.000 . Uani d ? C(8) 0.6593(3) -0.0336(2) -0.0338(3) 0.032(1) 1.000 . Uani d ? C(9) 0.6667(4) -0.0825(2) -0.0815(4) 0.045(1) 1.000 . Uani d ? C(10) 0.6280(4) -0.1274(2) -0.0340(4) 0.048(2) 1.000 . Uani d ? C(11) 0.5836(4) -0.1241(2) 0.0620(5) 0.058(2) 1.000 . Uani d ? C(12) 0.5791(4) -0.0766(2) 0.1106(4) 0.048(1) 1.000 . Uani d ? C(13) 0.6173(3) -0.0301(2) 0.0657(3) 0.034(1) 1.000 . Uani d ? C(14) 0.5713(4) 0.0289(2) 0.1966(3) 0.036(1) 1.000 . Uani d ? C(15) 0.5618(4) 0.0780(2) 0.2479(3) 0.037(1) 1.000 . Uani d ? C(16) 0.6005(4) 0.1274(2) 0.2093(3) 0.035(1) 1.000 . Uani d ? C(17) 0.5757(3) 0.1747(2) 0.2656(4) 0.036(1) 1.000 . Uani d ? C(18) 0.5160(4) 0.1696(2) 0.3519(4) 0.046(1) 1.000 . Uani d ? C(19) 0.4789(4) 0.1215(2) 0.3922(4) 0.044(1) 1.000 . Uani d ? C(20) 0.5034(4) 0.0770(2) 0.3384(4) 0.044(1) 1.000 . Uani d ? C(21) 0.7653(4) 0.2182(2) -0.1948(4) 0.053(2) 1.000 . Uani d ? C(22) 0.8386(6) 0.2237(3) -0.0954(5) 0.074(2) 1.000 . Uani d ? C(23) 0.6433(5) 0.2302(3) -0.1727(6) 0.077(2) 1.000 . Uani d ? C(24) 0.8043(6) 0.2605(3) -0.2690(6) 0.084(2) 1.000 . Uani d ? C(25) 0.8664(5) 0.0971(2) -0.4862(4) 0.056(2) 1.000 . Uani d ? C(26) 0.8094(7) 0.1357(4) -0.5581(5) 0.110(3) 1.000 . Uani d ? C(27) 0.9910(7) 0.1063(6) -0.4814(6) 0.149(4) 1.000 . Uani d ? C(28) 0.8411(9) 0.0448(4) -0.5322(6) 0.144(4) 1.000 . Uani d ? C(29) 0.6154(4) 0.2288(2) 0.2284(4) 0.044(1) 1.000 . Uani d ? C(30) 0.5812(5) 0.2734(2) 0.2999(5) 0.065(2) 1.000 . Uani d ? C(31) 0.7430(5) 0.2300(2) 0.2249(5) 0.063(2) 1.000 . Uani d ? C(32) 0.5615(5) 0.2406(2) 0.1214(5) 0.062(2) 1.000 . Uani d ? C(33) 0.4163(5) 0.1216(2) 0.4938(4) 0.060(2) 1.000 . Uani d ? C(34) 0.3102(6) 0.1543(4) 0.4814(6) 0.117(3) 1.000 . Uani d ? C(35) 0.4890(6) 0.1469(4) 0.5783(5) 0.103(3) 1.000 . Uani d ? C(36) 0.3853(9) 0.0660(4) 0.5234(7) 0.182(4) 1.000 . Uani d ? C(37) 0.9205(6) 0.0918(4) 0.1560(7) 0.131(3) 1.000 . Uani d ? C(38) 1.0275(7) 0.0751(4) 0.1882(8) 0.122(4) 1.000 . Uani d ? C(39) 0.112(1) 0.0878(9) 0.793(1) 0.163(8) 0.667 . Uani d ? C(39") 0.159(2) 0.075(2) 0.777(2) 0.16(1) 0.333 . Uani d ? C(40") 0.067(2) 0.070(1) 0.852(3) 0.15(1) 0.333 . Uani d ? C(40) 0.089(1) 0.0990(7) 0.885(2) 0.135(7) 0.667 . Uani d ? H(1) 0.9202 0.0809 0.0043 0.074 1.000 . Uiso c ? H(3) 0.7164 -0.0130 -0.2113 0.049 1.000 . Uiso c ? H(4) 0.8374 0.1820 -0.3720 0.054 1.000 . Uiso c ? H(5) 0.7872 0.0269 -0.3531 0.057 1.000 . Uiso c ? H(6) 0.6984 -0.0850 -0.1467 0.054 1.000 . Uiso c ? H(7) 0.6319 -0.1605 -0.0674 0.058 1.000 . Uiso c ? H(8) 0.5564 -0.1549 0.0939 0.070 1.000 . Uiso c ? H(9) 0.5492 -0.0751 0.1766 0.058 1.000 . Uiso c ? H(10) 0.5412 -0.0010 0.2296 0.043 1.000 . Uiso c ? H(11) 0.4982 0.2009 0.3875 0.055 1.000 . Uiso c ? H(12) 0.4797 0.0439 0.3637 0.053 1.000 . Uiso c ? H(13) 0.9155 0.2184 -0.1099 0.089 1.000 . Uiso c ? H(14) 0.8162 0.1981 -0.0475 0.089 1.000 . Uiso c ? H(15) 0.8293 0.2579 -0.0678 0.089 1.000 . Uiso c ? H(16) 0.6157 0.2041 -0.1282 0.092 1.000 . Uiso c ? H(17) 0.6388 0.2638 -0.1414 0.092 1.000 . Uiso c ? H(18) 0.5993 0.2301 -0.2346 0.092 1.000 . Uiso c ? H(19) 0.7969 0.2943 -0.2389 0.101 1.000 . Uiso c ? H(20) 0.8809 0.2545 -0.2837 0.101 1.000 . Uiso c ? H(21) 0.7592 0.2588 -0.3303 0.101 1.000 . Uiso c ? H(22) 0.8217 0.1705 -0.5335 0.132 1.000 . Uiso c ? H(23) 0.7308 0.1287 -0.5626 0.132 1.000 . Uiso c ? H(24) 0.8396 0.1323 -0.6237 0.132 1.000 . Uiso c ? H(25) 1.0061 0.1410 -0.4574 0.179 1.000 . Uiso c ? H(26) 1.0196 0.1022 -0.5475 0.179 1.000 . Uiso c ? H(27) 1.0262 0.0816 -0.4362 0.179 1.000 . Uiso c ? H(28) 0.8758 0.0180 -0.4913 0.173 1.000 . Uiso c ? H(29) 0.7620 0.0394 -0.5359 0.173 1.000 . Uiso c ? H(30) 0.8695 0.0434 -0.5988 0.173 1.000 . Uiso c ? H(31) 0.6154 0.2679 0.3657 0.078 1.000 . Uiso c ? H(32) 0.5016 0.2737 0.3046 0.078 1.000 . Uiso c ? H(33) 0.6054 0.3061 0.2737 0.078 1.000 . Uiso c ? H(34) 0.7751 0.2242 0.2913 0.075 1.000 . Uiso c ? H(35) 0.7674 0.2032 0.1803 0.075 1.000 . Uiso c ? H(36) 0.7663 0.2634 0.2007 0.075 1.000 . Uiso c ? H(37) 0.4821 0.2434 0.1259 0.075 1.000 . Uiso c ? H(38) 0.5787 0.2128 0.0760 0.075 1.000 . Uiso c ? H(39) 0.5906 0.2728 0.0966 0.075 1.000 . Uiso c ? H(40) 0.2727 0.1549 0.5440 0.140 1.000 . Uiso c ? H(41) 0.2620 0.1393 0.4298 0.140 1.000 . Uiso c ? H(42) 0.3294 0.1892 0.4627 0.140 1.000 . Uiso c ? H(43) 0.4501 0.1462 0.6401 0.124 1.000 . Uiso c ? H(44) 0.5577 0.1279 0.5869 0.124 1.000 . Uiso c ? H(45) 0.5047 0.1823 0.5606 0.124 1.000 . Uiso c ? H(46) 0.3456 0.0668 0.5848 0.219 1.000 . Uiso c ? H(47) 0.4519 0.0457 0.5334 0.219 1.000 . Uiso c ? H(48) 0.3390 0.0508 0.4707 0.219 1.000 . Uiso c ? H(49) 0.8722 0.0874 0.2114 0.157 1.000 . Uiso c ? H(50) 0.9252 0.1280 0.1391 0.157 1.000 . Uiso c ? H(51) 1.0545 0.0967 0.2429 0.146 1.000 . Uiso c ? H(52) 1.0241 0.0396 0.2105 0.146 1.000 . Uiso c ? H(53) 1.0769 0.0777 0.1333 0.146 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 0.0497(4) 0.0303(3) 0.0364(3) -0.0040(2) 0.0092(2) 0.0014(3) O(1) 0.084(3) 0.029(2) 0.045(2) -0.004(2) 0.024(2) 0.002(2) O(2) 0.060(2) 0.036(2) 0.047(2) -0.003(1) 0.018(2) -0.003(2) O(3) 0.045(2) 0.078(3) 0.072(3) -0.001(2) 0.004(2) -0.020(2) O(4) 0.113(6) 0.161(9) 0.155(8) -0.024(6) 0.059(6) -0.023(8) O(4") 0.09(1) 0.23(2) 0.16(2) 0.09(1) 0.05(1) 0.09(2) N(1) 0.044(2) 0.029(2) 0.033(2) 0.000(2) 0.009(1) 0.008(2) N(2) 0.037(2) 0.023(2) 0.041(2) -0.005(1) 0.003(2) 0.000(2) C(1) 0.052(3) 0.026(2) 0.045(3) -0.003(2) 0.003(2) -0.005(2) C(2) 0.040(3) 0.044(3) 0.040(3) 0.000(2) 0.005(2) 0.006(2) C(3) 0.046(3) 0.032(2) 0.039(2) -0.001(2) 0.004(2) 0.005(2) C(4) 0.041(3) 0.038(3) 0.045(3) -0.007(2) 0.003(2) 0.003(2) C(5) 0.046(3) 0.051(3) 0.038(3) -0.002(2) 0.004(2) 0.015(2) C(6) 0.045(3) 0.061(3) 0.043(3) 0.006(2) 0.010(2) 0.003(3) C(7) 0.055(3) 0.054(3) 0.035(3) 0.003(2) 0.007(2) 0.001(2) C(8) 0.035(3) 0.020(2) 0.042(2) 0.004(2) -0.004(2) 0.004(2) C(9) 0.046(3) 0.035(3) 0.053(3) 0.004(2) 0.000(2) 0.000(2) C(10) 0.052(3) 0.026(2) 0.067(3) 0.002(2) 0.002(2) -0.005(2) C(11) 0.062(4) 0.027(3) 0.085(4) -0.006(2) 0.008(3) 0.001(3) C(12) 0.062(3) 0.041(3) 0.043(3) 0.002(2) 0.010(2) 0.017(2) C(13) 0.033(3) 0.025(2) 0.042(2) -0.004(2) 0.000(2) 0.004(2) C(14) 0.042(3) 0.029(2) 0.037(2) -0.006(2) 0.006(2) 0.006(2) C(15) 0.045(3) 0.032(2) 0.036(2) 0.001(2) 0.004(2) 0.000(2) C(16) 0.040(3) 0.033(2) 0.034(2) 0.004(2) -0.001(2) 0.003(2) C(17) 0.033(3) 0.033(2) 0.042(2) 0.000(2) -0.004(2) -0.006(2) C(18) 0.041(3) 0.047(3) 0.051(3) 0.002(2) 0.005(2) -0.011(2) C(19) 0.046(3) 0.048(3) 0.037(2) 0.001(2) 0.008(2) -0.004(2) C(20) 0.043(3) 0.041(3) 0.048(3) -0.002(2) 0.010(2) 0.009(2) C(21) 0.065(4) 0.040(3) 0.055(3) -0.006(2) 0.008(2) 0.013(2) C(22) 0.103(5) 0.055(4) 0.064(4) -0.021(3) 0.004(3) 0.000(3) C(23) 0.073(4) 0.065(4) 0.094(5) 0.015(3) 0.025(3) 0.012(4) C(24) 0.110(5) 0.053(4) 0.091(5) -0.010(3) 0.029(4) 0.026(3) C(25) 0.063(4) 0.068(4) 0.039(3) 0.011(3) 0.015(2) 0.015(3) C(26) 0.144(7) 0.142(8) 0.045(4) 0.050(5) 0.016(4) 0.010(5) C(27) 0.074(5) 0.31(2) 0.064(5) 0.011(6) 0.033(4) 0.000(7) C(28) 0.260(9) 0.106(8) 0.072(5) -0.024(6) 0.087(5) -0.009(5) C(29) 0.047(3) 0.033(2) 0.052(3) -0.001(2) 0.007(2) 0.004(2) C(30) 0.076(4) 0.043(3) 0.077(4) 0.000(3) 0.008(3) -0.009(3) C(31) 0.065(4) 0.038(3) 0.086(4) -0.010(3) 0.002(3) -0.002(3) C(32) 0.077(4) 0.040(3) 0.070(4) 0.002(3) -0.001(3) 0.006(3) C(33) 0.063(4) 0.062(4) 0.056(3) -0.001(3) 0.024(3) -0.010(3) C(34) 0.079(5) 0.18(1) 0.096(6) 0.036(5) 0.039(4) 0.012(6) C(35) 0.119(6) 0.152(8) 0.040(4) 0.007(5) 0.011(3) -0.025(4) C(36) 0.32(1) 0.104(7) 0.136(5) -0.021(6) 0.172(5) -0.012(5) C(37) 0.083(5) 0.167(8) 0.138(6) 0.039(5) -0.041(4) -0.104(5) C(38) 0.099(6) 0.129(8) 0.134(7) 0.006(5) -0.045(5) -0.051(6) C(39) 0.048(8) 0.33(3) 0.12(1) 0.04(1) 0.034(8) 0.02(1) C(39") 0.10(2) 0.29(5) 0.10(2) 0.03(2) 0.07(1) 0.00(2) C(40") 0.10(2) 0.18(3) 0.18(2) -0.06(2) 0.11(1) -0.07(2) C(40) 0.061(9) 0.17(2) 0.18(2) -0.006(9) 0.018(9) -0.03(1) #------------------------------------------------------------------------------ _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) + 0.00106|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 3442 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_all 0.0860 _refine_ls_wR_factor_ref 0.0860 _refine_ls_goodness_of_fit_all 1.842 _refine_ls_goodness_of_fit_ref 1.842 _refine_ls_shift/su_max 0.0145 _refine_ls_shift/su_mean 0.0008 _refine_diff_density_min -0.29 _refine_diff_density_max 0.40 #------------------------------------------------------------------------------ _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 1.937(3) . . yes ZN O2 1.958(3) . . yes ZN O3 2.161(4) . . yes ZN N1 2.091(4) . . yes ZN N2 2.048(3) . . yes O1 C3 1.299(5) . . yes O2 C16 1.298(5) . . yes O3 C37 1.449(9) . . yes O3 H1 1.14 . . no O4 C40 1.58(2) . . yes O4" C40" 1.33(3) . . yes N1 C1 1.299(6) . . yes N1 C8 1.412(5) . . yes N2 C13 1.404(6) . . yes N2 C14 1.305(5) . . yes C1 C2 1.444(6) . . yes C1 H3 0.95 . . no C2 C3 1.414(7) . . yes C2 C7 1.441(7) . . yes C3 C4 1.442(6) . . yes C4 C5 1.379(7) . . yes C4 C21 1.541(7) . . yes C5 C6 1.404(7) . . yes C5 H4 0.95 . . no C6 C7 1.356(7) . . yes C6 C25 1.535(7) . . yes C7 H5 0.95 . . no C8 C9 1.395(6) . . yes C8 C13 1.419(6) . . yes C9 C10 1.388(7) . . yes C9 H6 0.95 . . no C10 C11 1.388(8) . . yes C10 H7 0.95 . . no C11 C12 1.367(7) . . yes C11 H8 0.95 . . no C12 C13 1.404(6) . . yes C12 H9 0.95 . . no C14 C15 1.423(6) . . yes C14 H10 0.95 . . no C15 C16 1.435(6) . . yes C15 C20 1.400(6) . . yes C16 C17 1.447(6) . . yes C17 C18 1.366(6) . . yes C17 C29 1.537(6) . . yes C18 C19 1.409(7) . . yes C18 H11 0.95 . . no C19 C20 1.370(7) . . yes C19 C33 1.553(7) . . yes C20 H12 0.95 . . no C21 C22 1.547(9) . . yes C21 C23 1.519(8) . . yes C21 C24 1.534(8) . . yes C22 H13 0.95 . . no C22 H14 0.95 . . no C22 H15 0.95 . . no C23 H16 0.95 . . no C23 H17 0.95 . . no C23 H18 0.95 . . no C24 H19 0.95 . . no C24 H20 0.95 . . no C24 H21 0.95 . . no C25 C26 1.50(1) . . yes C25 C27 1.497(9) . . yes C25 C28 1.49(1) . . yes C26 H22 0.95 . . no C26 H23 0.95 . . no C26 H24 0.95 . . no C27 H25 0.95 . . no C27 H26 0.95 . . no C27 H27 0.95 . . no C28 H28 0.95 . . no C28 H29 0.95 . . no C28 H30 0.95 . . no C29 C30 1.536(7) . . yes C29 C31 1.519(7) . . yes C29 C32 1.551(8) . . yes C30 H31 0.95 . . no C30 H32 0.95 . . no C30 H33 0.95 . . no C31 H34 0.95 . . no C31 H35 0.95 . . no C31 H36 0.95 . . no C32 H37 0.95 . . no C32 H38 0.95 . . no C32 H39 0.95 . . no C33 C34 1.51(1) . . yes C33 C35 1.521(9) . . yes C33 C36 1.51(1) . . yes C34 H40 0.95 . . no C34 H41 0.95 . . no C34 H42 0.95 . . no C35 H43 0.95 . . no C35 H44 0.95 . . no C35 H45 0.95 . . no C36 H46 0.95 . . no C36 H47 0.95 . . no C36 H48 0.95 . . no C37 C38 1.39(1) . . yes C37 H49 0.95 . . no C37 H50 0.95 . . no C38 H51 0.95 . . no C38 H52 0.95 . . no C38 H53 0.95 . . no C39 C40 1.29(2) . . yes C39" C40" 1.51(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 O1 ZN O2 95.8(1) . . . yes O1 ZN O3 100.6(2) . . . yes O1 ZN N1 89.1(1) . . . yes O1 ZN N2 155.5(1) . . . yes O2 ZN O3 100.0(1) . . . yes O2 ZN N1 165.5(1) . . . yes O2 ZN N2 91.0(1) . . . yes O3 ZN N1 92.5(1) . . . yes O3 ZN N2 101.4(2) . . . yes N1 ZN N2 79.2(1) . . . yes ZN O1 C3 129.8(3) . . . yes ZN O2 C16 130.4(3) . . . yes ZN O3 C37 120.1(4) . . . yes ZN O3 H1 106.8 . . . no C37 O3 H1 101.4 . . . no ZN N1 C1 125.0(3) . . . yes ZN N1 C8 113.4(3) . . . yes C1 N1 C8 121.5(4) . . . yes ZN N2 C13 114.9(3) . . . yes ZN N2 C14 123.9(3) . . . yes C13 N2 C14 121.2(4) . . . yes N1 C1 C2 124.3(4) . . . yes N1 C1 H3 117.8 . . . no C2 C1 H3 117.8 . . . no C1 C2 C3 125.2(4) . . . yes C1 C2 C7 115.3(4) . . . yes C3 C2 C7 119.6(4) . . . yes O1 C3 C2 123.1(4) . . . yes O1 C3 C4 118.7(4) . . . yes C2 C3 C4 118.1(4) . . . yes C3 C4 C5 118.3(4) . . . yes C3 C4 C21 119.9(4) . . . yes C5 C4 C21 121.8(4) . . . yes C4 C5 C6 124.8(5) . . . yes C4 C5 H4 117.6 . . . no C6 C5 H4 117.6 . . . no C5 C6 C7 116.9(5) . . . yes C5 C6 C25 120.0(5) . . . yes C7 C6 C25 123.1(5) . . . yes C2 C7 C6 122.4(5) . . . yes C2 C7 H5 118.8 . . . no C6 C7 H5 118.8 . . . no N1 C8 C9 124.9(4) . . . yes N1 C8 C13 115.2(4) . . . yes C9 C8 C13 119.9(4) . . . yes C8 C9 C10 120.2(5) . . . yes C8 C9 H6 119.9 . . . no C10 C9 H6 119.9 . . . no C9 C10 C11 120.2(5) . . . yes C9 C10 H7 119.9 . . . no C11 C10 H7 119.9 . . . no C10 C11 C12 120.0(5) . . . yes C10 C11 H8 120.0 . . . no C12 C11 H8 120.0 . . . no C11 C12 C13 121.8(5) . . . yes C11 C12 H9 119.1 . . . no C13 C12 H9 119.1 . . . no N2 C13 C8 116.1(4) . . . yes N2 C13 C12 126.2(4) . . . yes C8 C13 C12 117.8(4) . . . yes N2 C14 C15 127.2(4) . . . yes N2 C14 H10 116.3 . . . no C15 C14 H10 116.5 . . . no C14 C15 C16 124.5(4) . . . yes C14 C15 C20 115.9(4) . . . yes C16 C15 C20 119.5(4) . . . yes O2 C16 C15 122.7(4) . . . yes O2 C16 C17 119.2(4) . . . yes C15 C16 C17 118.1(4) . . . yes C16 C17 C18 117.9(4) . . . yes C16 C17 C29 120.6(4) . . . yes C18 C17 C29 121.5(4) . . . yes C17 C18 C19 125.0(5) . . . yes C17 C18 H11 117.5 . . . no C19 C18 H11 117.5 . . . no C18 C19 C20 116.5(4) . . . yes C18 C19 C33 119.3(4) . . . yes C20 C19 C33 124.2(5) . . . yes C15 C20 C19 123.0(4) . . . yes C15 C20 H12 118.5 . . . no C19 C20 H12 118.5 . . . no C4 C21 C22 109.9(5) . . . yes C4 C21 C23 110.2(4) . . . yes C4 C21 C24 112.7(5) . . . yes C22 C21 C23 109.3(5) . . . yes C22 C21 C24 107.4(5) . . . yes C23 C21 C24 107.2(5) . . . yes C21 C22 H13 109.5 . . . no C21 C22 H14 109.5 . . . no C21 C22 H15 109.5 . . . no H13 C22 H14 109.5 . . . no H13 C22 H15 109.5 . . . no H14 C22 H15 109.5 . . . no C21 C23 H16 109.5 . . . no C21 C23 H17 109.5 . . . no C21 C23 H18 109.5 . . . no H16 C23 H17 109.5 . . . no H16 C23 H18 109.5 . . . no H17 C23 H18 109.5 . . . no C21 C24 H19 109.5 . . . no C21 C24 H20 109.5 . . . no C21 C24 H21 109.5 . . . no H19 C24 H20 109.5 . . . no H19 C24 H21 109.5 . . . no H20 C24 H21 109.5 . . . no C6 C25 C26 110.4(5) . . . yes C6 C25 C27 109.4(5) . . . yes C6 C25 C28 112.5(5) . . . yes C26 C25 C27 110.2(6) . . . yes C26 C25 C28 104.4(6) . . . yes C27 C25 C28 109.9(7) . . . yes C25 C26 H22 109.5 . . . no C25 C26 H23 109.5 . . . no C25 C26 H24 109.5 . . . no H22 C26 H23 109.5 . . . no H22 C26 H24 109.5 . . . no H23 C26 H24 109.5 . . . no C25 C27 H25 109.5 . . . no C25 C27 H26 109.5 . . . no C25 C27 H27 109.5 . . . no H25 C27 H26 109.5 . . . no H25 C27 H27 109.5 . . . no H26 C27 H27 109.5 . . . no C25 C28 H28 109.5 . . . no C25 C28 H29 109.5 . . . no C25 C28 H30 109.5 . . . no H28 C28 H29 109.5 . . . no H28 C28 H30 109.5 . . . no H29 C28 H30 109.5 . . . no C17 C29 C30 111.9(4) . . . yes C17 C29 C31 110.3(4) . . . yes C17 C29 C32 109.8(4) . . . yes C30 C29 C31 106.9(4) . . . yes C30 C29 C32 107.5(4) . . . yes C31 C29 C32 110.2(4) . . . yes C29 C30 H31 109.5 . . . no C29 C30 H32 109.5 . . . no C29 C30 H33 109.5 . . . no H31 C30 H32 109.5 . . . no H31 C30 H33 109.5 . . . no H32 C30 H33 109.5 . . . no C29 C31 H34 109.5 . . . no C29 C31 H35 109.5 . . . no C29 C31 H36 109.5 . . . no H34 C31 H35 109.5 . . . no H34 C31 H36 109.5 . . . no H35 C31 H36 109.5 . . . no C29 C32 H37 109.5 . . . no C29 C32 H38 109.5 . . . no C29 C32 H39 109.5 . . . no H37 C32 H38 109.5 . . . no H37 C32 H39 109.5 . . . no H38 C32 H39 109.5 . . . no C19 C33 C34 109.4(5) . . . yes C19 C33 C35 110.5(5) . . . yes C19 C33 C36 110.4(5) . . . yes C34 C33 C35 107.1(6) . . . yes C34 C33 C36 109.3(7) . . . yes C35 C33 C36 110.1(7) . . . yes C33 C34 H40 109.5 . . . no C33 C34 H41 109.5 . . . no C33 C34 H42 109.5 . . . no H40 C34 H41 109.5 . . . no H40 C34 H42 109.5 . . . no H41 C34 H42 109.5 . . . no C33 C35 H43 109.5 . . . no C33 C35 H44 109.5 . . . no C33 C35 H45 109.5 . . . no H43 C35 H44 109.5 . . . no H43 C35 H45 109.5 . . . no H44 C35 H45 109.5 . . . no C33 C36 H46 109.5 . . . no C33 C36 H47 109.5 . . . no C33 C36 H48 109.5 . . . no H46 C36 H47 109.5 . . . no H46 C36 H48 109.5 . . . no H47 C36 H48 109.5 . . . no O3 C37 C38 116.5(6) . . . yes O3 C37 H49 107.7 . . . no O3 C37 H50 107.7 . . . no C38 C37 H49 107.7 . . . no C38 C37 H50 107.7 . . . no H49 C37 H50 109.5 . . . no C37 C38 H51 109.5 . . . no C37 C38 H52 109.5 . . . no C37 C38 H53 109.5 . . . no H51 C38 H52 109.5 . . . no H51 C38 H53 109.5 . . . no H52 C38 H53 109.5 . . . no O4" C40" C39" 142(3) . . . yes O4 C40 C39 104(2) . . . yes #------------------------------------------------------------------------------ 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 O4" 3.47(2) . 1_654 no O1 C11 3.485(6) . 3_655 no O2 C10 3.551(6) . 3_655 no O3 O4 2.77(1) . 1_654 no O3 O4" 2.82(2) . 1_654 no O3 O4 3.09(1) . 3_656 no O4 O4 3.21(2) . 3_557 no O4 C38 3.51(1) . 1_456 no O4 C38 3.52(1) . 3_656 no O4 C37 3.52(1) . 1_456 no O4" C3 3.15(2) . 1_456 no O4" C2 3.38(2) . 1_456 no O4" C37 3.48(2) . 1_456 no O4" C4 3.50(2) . 1_456 no N1 C12 3.584(6) . 3_655 no N2 C8 3.421(5) . 3_655 no N2 C13 3.561(5) . 3_655 no C8 C14 3.411(6) . 3_655 no C9 C15 3.420(7) . 3_655 no C9 C14 3.435(7) . 3_655 no C10 C16 3.489(7) . 3_655 no C12 C39" 3.39(3) . 3_656 no C13 C39" 3.49(3) . 3_656 no C13 C13 3.566(9) . 3_655 no O4 O4" 1.40(2) . . no O4 O3 2.77(1) . 1_456 no O4 O3 3.09(1) . 3_656 no O4 O4 3.21(2) . 3_557 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 ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A O3 H1 O4" 1.14 1.69 2.82(2) 173.6 1_654 O3 H1 O4 1.14 1.90 2.77(1) 129.9 1_654