# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_publication_text _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Li-Ya Wang' _publ_contact_author_address ;College of Chemistry and Chemical Engineering, Luoyang Normal University, Luoyang, Henan 471022, China. ; _publ_contact_author_email wlya@lynu.edu.cn _publ_contact_author_phone ' (+86) 379-65523593' _publ_contact_author_fax ' (+86) 379-65511205' loop_ _publ_author_name _publ_author_address 'Liu Guang-Zhen' ;College of Chemistry and Chemical Engineering, Luoyang Normal University, Luoyang, Henan 471022, China. ; 'Ling-Yun Xin' ;College of Chemistry and Chemical Engineering, Luoyang Normal University, Luoyang, Henan 471022, China. ; 'Li-Ya Wang' ;College of Chemistry and Chemical Engineering, Luoyang Normal University, Luoyang, Henan 471022, China. ; data_c1 _database_code_depnum_ccdc_archive 'CCDC 796993' #TrackingRef 'CIF-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H16 N2 O4 Zn' _chemical_formula_weight 425.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.660(3) _cell_length_b 10.260(4) _cell_length_c 12.880(5) _cell_angle_alpha 110.070(5) _cell_angle_beta 93.730(5) _cell_angle_gamma 105.240(5) _cell_volume 903.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1786 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5996 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6663 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3316 _reflns_number_gt 2759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.1846P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3316 _refine_ls_number_parameters 253 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.83483(6) 0.48313(5) 0.11059(3) 0.02706(18) Uani 1 1 d . . . N1 N 0.9967(5) 0.6472(4) 0.2645(3) 0.0335(8) Uani 1 1 d . . . N2 N 1.6888(4) 1.3053(4) 0.9573(3) 0.0325(8) Uani 1 1 d . . . O1 O 0.5975(4) 0.4627(3) 0.1733(2) 0.0427(7) Uani 1 1 d . . . O2 O 0.7059(4) 0.3193(4) 0.2303(3) 0.0611(8) Uani 1 1 d U . . O5 O 0.1778(4) 0.3633(3) -0.0505(2) 0.0367(7) Uani 1 1 d . . . O6 O 0.0439(4) 0.3981(3) 0.1017(2) 0.0367(7) Uani 1 1 d . . . C1 C 1.0822(6) 0.6143(5) 0.3406(3) 0.0419(11) Uani 1 1 d . . . H1 H 1.0691 0.5166 0.3260 0.050 Uiso 1 1 calc R . . C2 C 1.1211(7) 0.8926(5) 0.3839(4) 0.0464(11) Uani 1 1 d . . . H2 H 1.1315 0.9894 0.3965 0.056 Uiso 1 1 calc R . . C3 C 1.2112(5) 0.8601(4) 0.4643(3) 0.0335(9) Uani 1 1 d . . . C4 C 1.0190(6) 0.7878(5) 0.2880(3) 0.0436(11) Uani 1 1 d . . . H4 H 0.9619 0.8148 0.2363 0.052 Uiso 1 1 calc R . . C5 C 1.3164(6) 0.9756(5) 0.5679(3) 0.0387(10) Uani 1 1 d . . . H5A H 1.3373 1.0704 0.5710 0.046 Uiso 1 1 calc R . . C6 C 1.3858(6) 0.9606(5) 0.6585(3) 0.0389(10) Uani 1 1 d . . . H6A H 1.3692 0.8665 0.6562 0.047 Uiso 1 1 calc R . . C7 C 1.6820(6) 1.1688(5) 0.9370(4) 0.0448(11) Uani 1 1 d . . . H7 H 1.7481 1.1494 0.9901 0.054 Uiso 1 1 calc R . . C8 C 1.4855(6) 1.0802(5) 0.7608(3) 0.0358(9) Uani 1 1 d . . . C9 C 1.5851(7) 1.0567(5) 0.8441(4) 0.0457(11) Uani 1 1 d . . . H9 H 1.5840 0.9625 0.8350 0.055 Uiso 1 1 calc R . . C10 C 1.5902(6) 1.3286(4) 0.8808(3) 0.0364(10) Uani 1 1 d . . . H10 H 1.5893 1.4235 0.8945 0.044 Uiso 1 1 calc R . . C11 C 1.4901(6) 1.2216(5) 0.7832(4) 0.0398(10) Uani 1 1 d . . . H11 H 1.4252 1.2446 0.7319 0.048 Uiso 1 1 calc R . . C15 C 1.1884(6) 0.7157(5) 0.4394(3) 0.0435(11) Uani 1 1 d . . . H15 H 1.2451 0.6861 0.4895 0.052 Uiso 1 1 calc R . . C16 C 0.2395(5) 0.2569(4) 0.1879(3) 0.0288(8) Uani 1 1 d . . . C17 C 0.4079(5) 0.3242(4) 0.2603(3) 0.0297(8) Uani 1 1 d . . . C18 C 0.0961(7) 0.2379(6) 0.3461(4) 0.0540(13) Uani 1 1 d . . . H18 H -0.0102 0.2096 0.3743 0.065 Uiso 1 1 calc R . . C19 C 0.2615(8) 0.3037(6) 0.4169(4) 0.0537(13) Uani 1 1 d . . . H19 H 0.2690 0.3196 0.4928 0.064 Uiso 1 1 calc R . . C20 C 0.4162(6) 0.3458(5) 0.3738(3) 0.0401(10) Uani 1 1 d . . . H20 H 0.5294 0.3897 0.4213 0.048 Uiso 1 1 calc R . . C21 C 0.0854(6) 0.2133(5) 0.2332(4) 0.0433(11) Uani 1 1 d . . . H21 H -0.0280 0.1662 0.1863 0.052 Uiso 1 1 calc R . . C22 C 0.5836(6) 0.3713(5) 0.2192(5) 0.0503(9) Uani 1 1 d U . . C24 C 0.1405(5) 0.3414(4) 0.0373(3) 0.0264(8) Uani 1 1 d . . . C39 C 0.2205(5) 0.2363(4) 0.0660(3) 0.0319(9) Uani 1 1 d . . . H39A H 0.1432 0.1379 0.0221 0.038 Uiso 1 1 calc R . . H39B H 0.3407 0.2463 0.0442 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0269(3) 0.0291(3) 0.0212(3) 0.00523(19) 0.00050(18) 0.00864(19) N1 0.0359(19) 0.0340(19) 0.0248(17) 0.0058(14) -0.0018(14) 0.0101(15) N2 0.0300(18) 0.0326(19) 0.0273(17) 0.0031(14) -0.0027(14) 0.0103(15) O1 0.0401(17) 0.0461(19) 0.0438(17) 0.0215(15) 0.0123(14) 0.0086(14) O2 0.0369(16) 0.0624(19) 0.093(2) 0.0339(18) 0.0141(16) 0.0224(14) O5 0.0489(18) 0.0355(16) 0.0224(14) 0.0087(12) 0.0019(12) 0.0112(13) O6 0.0376(16) 0.0451(17) 0.0316(15) 0.0127(13) 0.0027(13) 0.0222(14) C1 0.055(3) 0.029(2) 0.030(2) 0.0023(18) -0.009(2) 0.010(2) C2 0.068(3) 0.029(2) 0.032(2) 0.0034(18) -0.006(2) 0.012(2) C3 0.032(2) 0.037(2) 0.024(2) 0.0055(17) 0.0015(16) 0.0058(18) C4 0.056(3) 0.037(2) 0.028(2) 0.0052(19) -0.008(2) 0.012(2) C5 0.043(2) 0.031(2) 0.027(2) 0.0023(17) -0.0019(18) 0.0005(19) C6 0.043(2) 0.030(2) 0.031(2) 0.0000(18) -0.0026(19) 0.0089(19) C7 0.050(3) 0.038(3) 0.039(2) 0.010(2) -0.013(2) 0.012(2) C8 0.033(2) 0.040(2) 0.029(2) 0.0063(18) -0.0001(17) 0.0119(18) C9 0.060(3) 0.025(2) 0.040(2) 0.0022(19) -0.013(2) 0.012(2) C10 0.035(2) 0.023(2) 0.038(2) 0.0012(17) -0.0085(18) 0.0033(17) C11 0.041(2) 0.039(2) 0.035(2) 0.0129(19) -0.0061(19) 0.011(2) C15 0.053(3) 0.039(3) 0.028(2) 0.0042(19) -0.014(2) 0.014(2) C16 0.029(2) 0.027(2) 0.032(2) 0.0125(17) 0.0031(16) 0.0120(16) C17 0.032(2) 0.029(2) 0.032(2) 0.0141(17) 0.0065(17) 0.0108(17) C18 0.049(3) 0.071(4) 0.056(3) 0.041(3) 0.022(3) 0.014(3) C19 0.072(4) 0.066(3) 0.039(3) 0.034(3) 0.019(3) 0.026(3) C20 0.047(3) 0.042(3) 0.031(2) 0.0140(19) 0.0012(19) 0.014(2) C21 0.035(2) 0.049(3) 0.052(3) 0.030(2) 0.007(2) 0.009(2) C22 0.0327(18) 0.053(2) 0.075(2) 0.0313(19) 0.0167(18) 0.0182(15) C24 0.0257(19) 0.0231(19) 0.0194(18) 0.0010(15) -0.0064(15) 0.0014(15) C39 0.032(2) 0.031(2) 0.031(2) 0.0088(17) 0.0014(17) 0.0113(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.000(3) 2_665 ? Zn1 O6 2.007(3) 1_655 ? Zn1 O1 2.027(3) . ? Zn1 N1 2.144(3) . ? Zn1 N2 2.155(3) 1_444 ? N1 C1 1.328(5) . ? N1 C4 1.329(5) . ? N2 C7 1.319(5) . ? N2 C10 1.327(5) . ? N2 Zn1 2.155(3) 1_666 ? O1 C22 1.255(5) . ? O2 C22 1.216(5) . ? O5 C24 1.262(4) . ? O5 Zn1 2.000(3) 2_665 ? O6 C24 1.244(4) . ? O6 Zn1 2.007(3) 1_455 ? C1 C15 1.369(6) . ? C1 H1 0.9300 . ? C2 C4 1.346(6) . ? C2 C3 1.388(6) . ? C2 H2 0.9300 . ? C3 C15 1.363(6) . ? C3 C5 1.452(6) . ? C4 H4 0.9300 . ? C5 C6 1.323(6) . ? C5 H5A 0.9300 . ? C6 C8 1.447(6) . ? C6 H6A 0.9300 . ? C7 C9 1.341(6) . ? C7 H7 0.9300 . ? C8 C11 1.369(6) . ? C8 C9 1.400(6) . ? C9 H9 0.9300 . ? C10 C11 1.364(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.387(6) . ? C16 C17 1.394(5) . ? C16 C39 1.503(5) . ? C17 C20 1.396(6) . ? C17 C22 1.501(6) . ? C18 C19 1.368(7) . ? C18 C21 1.381(6) . ? C18 H18 0.9300 . ? C19 C20 1.371(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C24 C39 1.505(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? 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_3 _geom_angle_publ_flag O5 Zn1 O6 123.52(12) 2_665 1_655 ? O5 Zn1 O1 98.67(12) 2_665 . ? O6 Zn1 O1 137.80(12) 1_655 . ? O5 Zn1 N1 90.34(12) 2_665 . ? O6 Zn1 N1 85.63(12) 1_655 . ? O1 Zn1 N1 93.79(13) . . ? O5 Zn1 N2 94.09(12) 2_665 1_444 ? O6 Zn1 N2 89.03(12) 1_655 1_444 ? O1 Zn1 N2 88.99(12) . 1_444 ? N1 Zn1 N2 174.37(12) . 1_444 ? C1 N1 C4 116.4(4) . . ? C1 N1 Zn1 122.0(3) . . ? C4 N1 Zn1 121.5(3) . . ? C7 N2 C10 116.5(3) . . ? C7 N2 Zn1 123.2(3) . 1_666 ? C10 N2 Zn1 120.2(3) . 1_666 ? C22 O1 Zn1 108.1(3) . . ? C24 O5 Zn1 134.5(2) . 2_665 ? C24 O6 Zn1 144.1(3) . 1_455 ? N1 C1 C15 123.8(4) . . ? N1 C1 H1 118.1 . . ? C15 C1 H1 118.1 . . ? C4 C2 C3 121.8(4) . . ? C4 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C15 C3 C2 115.4(4) . . ? C15 C3 C5 124.3(4) . . ? C2 C3 C5 120.3(4) . . ? N1 C4 C2 122.5(4) . . ? N1 C4 H4 118.8 . . ? C2 C4 H4 118.8 . . ? C6 C5 C3 127.1(4) . . ? C6 C5 H5A 116.5 . . ? C3 C5 H5A 116.5 . . ? C5 C6 C8 124.6(4) . . ? C5 C6 H6A 117.7 . . ? C8 C6 H6A 117.7 . . ? N2 C7 C9 123.6(4) . . ? N2 C7 H7 118.2 . . ? C9 C7 H7 118.2 . . ? C11 C8 C9 115.7(4) . . ? C11 C8 C6 123.4(4) . . ? C9 C8 C6 120.9(4) . . ? C7 C9 C8 120.5(4) . . ? C7 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N2 C10 C11 123.8(4) . . ? N2 C10 H10 118.1 . . ? C11 C10 H10 118.1 . . ? C10 C11 C8 119.8(4) . . ? C10 C11 H11 120.1 . . ? C8 C11 H11 120.1 . . ? C3 C15 C1 120.1(4) . . ? C3 C15 H15 120.0 . . ? C1 C15 H15 120.0 . . ? C21 C16 C17 117.6(4) . . ? C21 C16 C39 120.1(4) . . ? C17 C16 C39 122.3(4) . . ? C16 C17 C20 119.8(4) . . ? C16 C17 C22 121.8(4) . . ? C20 C17 C22 118.4(4) . . ? C19 C18 C21 120.6(4) . . ? C19 C18 H18 119.7 . . ? C21 C18 H18 119.7 . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C17 121.6(4) . . ? C19 C20 H20 119.2 . . ? C17 C20 H20 119.2 . . ? C18 C21 C16 121.7(4) . . ? C18 C21 H21 119.1 . . ? C16 C21 H21 119.1 . . ? O2 C22 O1 122.5(4) . . ? O2 C22 C17 119.4(4) . . ? O1 C22 C17 118.1(4) . . ? O6 C24 O5 126.1(4) . . ? O6 C24 C39 117.3(3) . . ? O5 C24 C39 116.6(3) . . ? C16 C39 C24 114.5(3) . . ? C16 C39 H39A 108.6 . . ? C24 C39 H39A 108.6 . . ? C16 C39 H39B 108.6 . . ? C24 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Zn1 N1 C1 -168.5(3) 2_665 . . . ? O6 Zn1 N1 C1 -44.9(3) 1_655 . . . ? O1 Zn1 N1 C1 92.8(3) . . . . ? N2 Zn1 N1 C1 -26.6(14) 1_444 . . . ? O5 Zn1 N1 C4 10.5(3) 2_665 . . . ? O6 Zn1 N1 C4 134.1(3) 1_655 . . . ? O1 Zn1 N1 C4 -88.2(3) . . . . ? N2 Zn1 N1 C4 152.4(11) 1_444 . . . ? O5 Zn1 O1 C22 -177.9(3) 2_665 . . . ? O6 Zn1 O1 C22 0.7(4) 1_655 . . . ? N1 Zn1 O1 C22 -87.0(3) . . . . ? N2 Zn1 O1 C22 88.1(3) 1_444 . . . ? C4 N1 C1 C15 0.2(7) . . . . ? Zn1 N1 C1 C15 179.3(4) . . . . ? C4 C2 C3 C15 -0.2(7) . . . . ? C4 C2 C3 C5 -178.5(4) . . . . ? C1 N1 C4 C2 -0.5(7) . . . . ? Zn1 N1 C4 C2 -179.5(4) . . . . ? C3 C2 C4 N1 0.5(8) . . . . ? C15 C3 C5 C6 -9.1(8) . . . . ? C2 C3 C5 C6 169.0(5) . . . . ? C3 C5 C6 C8 -178.2(4) . . . . ? C10 N2 C7 C9 1.2(7) . . . . ? Zn1 N2 C7 C9 177.0(4) 1_666 . . . ? C5 C6 C8 C11 12.6(7) . . . . ? C5 C6 C8 C9 -167.3(5) . . . . ? N2 C7 C9 C8 1.0(8) . . . . ? C11 C8 C9 C7 -2.1(7) . . . . ? C6 C8 C9 C7 177.8(4) . . . . ? C7 N2 C10 C11 -2.2(7) . . . . ? Zn1 N2 C10 C11 -178.2(3) 1_666 . . . ? N2 C10 C11 C8 1.1(7) . . . . ? C9 C8 C11 C10 1.1(7) . . . . ? C6 C8 C11 C10 -178.8(4) . . . . ? C2 C3 C15 C1 -0.1(7) . . . . ? C5 C3 C15 C1 178.1(4) . . . . ? N1 C1 C15 C3 0.1(8) . . . . ? C21 C16 C17 C20 -0.2(6) . . . . ? C39 C16 C17 C20 177.4(3) . . . . ? C21 C16 C17 C22 178.1(4) . . . . ? C39 C16 C17 C22 -4.4(6) . . . . ? C21 C18 C19 C20 0.6(8) . . . . ? C18 C19 C20 C17 0.6(7) . . . . ? C16 C17 C20 C19 -0.8(6) . . . . ? C22 C17 C20 C19 -179.1(4) . . . . ? C19 C18 C21 C16 -1.6(8) . . . . ? C17 C16 C21 C18 1.3(6) . . . . ? C39 C16 C21 C18 -176.2(4) . . . . ? Zn1 O1 C22 O2 6.3(6) . . . . ? Zn1 O1 C22 C17 -172.9(3) . . . . ? C16 C17 C22 O2 -119.1(5) . . . . ? C20 C17 C22 O2 59.1(6) . . . . ? C16 C17 C22 O1 60.1(6) . . . . ? C20 C17 C22 O1 -121.6(5) . . . . ? Zn1 O6 C24 O5 28.2(7) 1_455 . . . ? Zn1 O6 C24 C39 -151.6(3) 1_455 . . . ? Zn1 O5 C24 O6 17.4(6) 2_665 . . . ? Zn1 O5 C24 C39 -162.8(3) 2_665 . . . ? C21 C16 C39 C24 74.3(5) . . . . ? C17 C16 C39 C24 -103.2(4) . . . . ? O6 C24 C39 C16 -23.6(5) . . . . ? O5 C24 C39 C16 156.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.898 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.097 # Attachment 'CIF-2.cif' data_c2 _database_code_depnum_ccdc_archive 'CCDC 796994' #TrackingRef 'CIF-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H80 N8 O16 Zn4' _chemical_formula_weight 1767.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 35.298(3) _cell_length_b 11.5573(11) _cell_length_c 21.1145(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.5230(10) _cell_angle_gamma 90.00 _cell_volume 8557.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4952 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 17.55 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6835 _exptl_absorpt_correction_T_max 0.8250 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 63821 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.50 _reflns_number_total 15881 _reflns_number_gt 7756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15881 _refine_ls_number_parameters 1055 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.1378 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C37 C 0.25572(15) 0.8184(4) 0.2791(4) 0.0679(15) Uani 0.555(4) 1 d PDU A 1 H37A H 0.2517 0.8201 0.3238 0.082 Uiso 0.555(4) 1 calc PR A 1 H37B H 0.2312 0.8056 0.2544 0.082 Uiso 0.555(4) 1 calc PR A 1 C38 C 0.27144(14) 0.9337(3) 0.2609(4) 0.0773(17) Uani 0.555(4) 1 d PDU A 1 H38A H 0.2542 0.9936 0.2723 0.093 Uiso 0.555(4) 1 calc PR A 1 H38B H 0.2710 0.9353 0.2149 0.093 Uiso 0.555(4) 1 calc PR A 1 C39 C 0.31169(16) 0.9655(5) 0.2902(3) 0.0766(17) Uani 0.555(4) 1 d PDU A 1 H39A H 0.3291 0.9021 0.2853 0.092 Uiso 0.555(4) 1 calc PR A 1 H39B H 0.3119 0.9821 0.3352 0.092 Uiso 0.555(4) 1 calc PR A 1 C37' C 0.2630(2) 0.8153(4) 0.3009(4) 0.0679(15) Uani 0.445(4) 1 d PD A 2 H37C H 0.2373 0.8257 0.2800 0.082 Uiso 0.445(4) 1 calc PR A 2 H37D H 0.2611 0.7927 0.3447 0.082 Uiso 0.445(4) 1 calc PR A 2 C38' C 0.2840(2) 0.9288(4) 0.3006(3) 0.0773(17) Uani 0.445(4) 1 d PD A 2 H38C H 0.3068 0.9226 0.3308 0.093 Uiso 0.445(4) 1 calc PR A 2 H38D H 0.2680 0.9877 0.3167 0.093 Uiso 0.445(4) 1 calc PR A 2 C39' C 0.2960(2) 0.9720(6) 0.2376(3) 0.0766(17) Uani 0.445(4) 1 d PD A 2 H39C H 0.2739 0.9973 0.2095 0.092 Uiso 0.445(4) 1 calc PR A 2 H39D H 0.3086 0.9108 0.2165 0.092 Uiso 0.445(4) 1 calc PR A 2 Zn1 Zn 0.409658(13) 0.78550(4) 0.00224(2) 0.05766(14) Uani 1 1 d . . . Zn2 Zn 0.370198(14) 0.44224(4) 0.18991(2) 0.05516(14) Uani 1 1 d . . . Zn3 Zn 0.090707(15) 0.21404(4) 0.53653(2) 0.06433(15) Uani 1 1 d . . . Zn4 Zn 0.131374(14) -0.04530(4) 0.23264(2) 0.05566(14) Uani 1 1 d . . . O1 O 0.43875(10) 0.9747(3) -0.01695(14) 0.1064(12) Uani 1 1 d . . . O2 O 0.42958(8) 0.8305(2) -0.08085(14) 0.0813(9) Uani 1 1 d . . . O3 O 0.41416(8) 1.0333(2) -0.20593(14) 0.0815(10) Uani 1 1 d . . . O4 O 0.41951(7) 0.9788(2) -0.30350(12) 0.0678(9) Uani 1 1 d . . . O5 O 0.34759(8) 0.4589(2) 0.10098(12) 0.0729(9) Uani 1 1 d . . . O6 O 0.39034(10) 0.3446(3) 0.06570(14) 0.0940(11) Uani 1 1 d . . . O7 O 0.37443(8) 0.6502(2) -0.00917(13) 0.0740(9) Uani 1 1 d . . . O8 O 0.33899(9) 0.8001(2) -0.03093(16) 0.0970(12) Uani 1 1 d . . . O9 O 0.16359(10) 0.2017(3) 0.52991(19) 0.1158(13) Uani 1 1 d . . . O10 O 0.12568(8) 0.3493(3) 0.53759(14) 0.0801(10) Uani 1 1 d . . . O11 O 0.15299(8) 0.5349(2) 0.65184(11) 0.0698(9) Uani 1 1 d . . . O12 O 0.10894(9) 0.6521(3) 0.60516(15) 0.0940(11) Uani 1 1 d . . . O13 O 0.07108(10) 0.1708(3) 0.44606(14) 0.1029(4) Uani 1 1 d U . . O14 O 0.06169(10) 0.0253(3) 0.50292(15) 0.1088(4) Uani 1 1 d U . . O15 O 0.08124(8) 0.0269(2) 0.22316(12) 0.0661(8) Uani 1 1 d . . . O16 O 0.09062(9) -0.0119(3) 0.32471(14) 0.0848(10) Uani 1 1 d . . . N1 N 0.45802(9) 0.6877(3) 0.03664(13) 0.0561(9) Uani 1 1 d . . . N2 N 0.59970(9) 0.3430(3) 0.40797(15) 0.0587(10) Uani 1 1 d . . . N3 N 0.32970(9) 0.5481(2) 0.22622(15) 0.0553(9) Uani 1 1 d . A . N4 N 0.35689(10) 1.2811(3) 0.21848(16) 0.0658(10) Uani 1 1 d . . . N5 N 0.04248(9) 0.3107(3) 0.55196(14) 0.0607(10) Uani 1 1 d . . . N6 N -0.09947(9) 0.6510(3) 0.87190(15) 0.0636(10) Uani 1 1 d . . . N7 N 0.14621(9) -0.2026(2) 0.26984(15) 0.0565(10) Uani 1 1 d . . . N8 N 0.17207(9) -0.9310(3) 0.27875(15) 0.0615(10) Uani 1 1 d . . . C1 C 0.48322(10) 0.9042(3) -0.16030(17) 0.0473(10) Uani 1 1 d . . . C2 C 0.46571(10) 0.9048(3) -0.22272(16) 0.0451(10) Uani 1 1 d . . . C3 C 0.47933(11) 0.8325(3) -0.26764(18) 0.0605(12) Uani 1 1 d . . . H3 H 0.4676 0.8333 -0.3093 0.073 Uiso 1 1 calc R . . C4 C 0.51003(12) 0.7595(3) -0.2517(2) 0.0696(13) Uani 1 1 d . . . H4 H 0.5193 0.7128 -0.2823 0.084 Uiso 1 1 calc R . . C5 C 0.52651(11) 0.7576(3) -0.1893(2) 0.0684(13) Uani 1 1 d . . . H5 H 0.5466 0.7073 -0.1772 0.082 Uiso 1 1 calc R . . C6 C 0.51337(11) 0.8295(3) -0.14537(19) 0.0581(12) Uani 1 1 d . . . H6 H 0.5252 0.8280 -0.1037 0.070 Uiso 1 1 calc R . . C7 C 0.47189(11) 0.9789(3) -0.10721(18) 0.0611(12) Uani 1 1 d . . . H7A H 0.4947 0.9993 -0.0795 0.073 Uiso 1 1 calc R . . H7B H 0.4610 1.0501 -0.1256 0.073 Uiso 1 1 calc R . . C8 C 0.44413(12) 0.9264(4) -0.06745(18) 0.0648(13) Uani 1 1 d . . . C9 C 0.43105(11) 0.9789(3) -0.24318(19) 0.0562(12) Uani 1 1 d . . . C10 C 0.30814(12) 0.5003(3) -0.01688(17) 0.0579(12) Uani 1 1 d . . . C11 C 0.30759(12) 0.6194(4) -0.02175(18) 0.0624(13) Uani 1 1 d . . . C12 C 0.27288(13) 0.6776(4) -0.0264(2) 0.0823(16) Uani 1 1 d . . . H12 H 0.2723 0.7574 -0.0322 0.099 Uiso 1 1 calc R . . C13 C 0.23901(15) 0.6182(5) -0.0225(3) 0.107(2) Uani 1 1 d . . . H13 H 0.2162 0.6585 -0.0231 0.129 Uiso 1 1 calc R . . C14 C 0.23945(14) 0.5016(5) -0.0179(2) 0.0971(18) Uani 1 1 d . . . H14 H 0.2169 0.4609 -0.0158 0.116 Uiso 1 1 calc R . . C15 C 0.27308(13) 0.4442(4) -0.0164(2) 0.0803(15) Uani 1 1 d . . . H15 H 0.2728 0.3637 -0.0150 0.096 Uiso 1 1 calc R . . C16 C 0.34362(12) 0.4268(3) -0.01065(18) 0.0650(13) Uani 1 1 d . . . H16A H 0.3621 0.4627 -0.0351 0.078 Uiso 1 1 calc R . . H16B H 0.3372 0.3519 -0.0298 0.078 Uiso 1 1 calc R . . C17 C 0.36235(13) 0.4073(3) 0.05682(19) 0.0630(13) Uani 1 1 d . . . C18 C 0.34220(12) 0.6952(4) -0.02183(18) 0.0619(13) Uani 1 1 d . . . C19 C 0.49392(12) 0.7267(4) 0.03818(19) 0.0668(13) Uani 1 1 d . . . H19 H 0.4978 0.8011 0.0234 0.080 Uiso 1 1 calc R . . C20 C 0.52491(12) 0.6626(4) 0.06036(19) 0.0696(14) Uani 1 1 d . . . H20 H 0.5492 0.6942 0.0611 0.083 Uiso 1 1 calc R . . C21 C 0.52071(13) 0.5518(4) 0.08162(17) 0.0649(13) Uani 1 1 d . . . C22 C 0.48363(14) 0.5116(3) 0.08002(18) 0.0701(14) Uani 1 1 d . . . H22 H 0.4792 0.4370 0.0941 0.084 Uiso 1 1 calc R . . C23 C 0.45360(13) 0.5798(3) 0.05819(17) 0.0633(13) Uani 1 1 d . . . H23 H 0.4290 0.5506 0.0582 0.076 Uiso 1 1 calc R . . C24 C 0.55411(13) 0.4793(4) 0.10709(19) 0.0811(15) Uani 1 1 d . . . H24A H 0.5507 0.4012 0.0906 0.097 Uiso 1 1 calc R . . H24B H 0.5771 0.5106 0.0925 0.097 Uiso 1 1 calc R . . C25 C 0.55873(13) 0.4756(4) 0.17825(18) 0.0707(14) Uani 1 1 d . . . H25A H 0.5348 0.4520 0.1926 0.085 Uiso 1 1 calc R . . H25B H 0.5645 0.5529 0.1945 0.085 Uiso 1 1 calc R . . C26 C 0.58949(13) 0.3947(4) 0.20561(17) 0.0712(14) Uani 1 1 d . . . H26A H 0.5844 0.3189 0.1868 0.085 Uiso 1 1 calc R . . H26B H 0.6135 0.4212 0.1926 0.085 Uiso 1 1 calc R . . C27 C 0.61677(12) 0.2760(4) 0.36973(19) 0.0716(13) Uani 1 1 d . . . H27 H 0.6310 0.2140 0.3875 0.086 Uiso 1 1 calc R . . C28 C 0.61472(12) 0.2922(3) 0.30492(19) 0.0649(13) Uani 1 1 d . . . H28 H 0.6275 0.2416 0.2805 0.078 Uiso 1 1 calc R . . C29 C 0.59424(11) 0.3817(3) 0.27596(18) 0.0555(11) Uani 1 1 d . . . C30 C 0.57715(13) 0.4528(4) 0.31546(19) 0.0762(14) Uani 1 1 d . . . H30 H 0.5630 0.5158 0.2988 0.091 Uiso 1 1 calc R . . C31 C 0.58070(13) 0.4318(4) 0.3803(2) 0.0794(15) Uani 1 1 d . . . H31 H 0.5691 0.4831 0.4060 0.095 Uiso 1 1 calc R . . C32 C 0.30123(12) 0.5948(4) 0.1869(2) 0.0736(14) Uani 1 1 d . . . H32 H 0.2974 0.5702 0.1448 0.088 Uiso 1 1 calc R . . C33 C 0.27782(12) 0.6776(4) 0.2072(2) 0.0839(16) Uani 1 1 d . A . H33 H 0.2582 0.7067 0.1785 0.101 Uiso 1 1 calc R . . C34 C 0.28205(11) 0.7194(3) 0.2679(2) 0.0676(13) Uani 1 1 d D . . C35 C 0.31066(12) 0.6678(3) 0.3078(2) 0.0702(13) Uani 1 1 d . A . H35 H 0.3146 0.6899 0.3504 0.084 Uiso 1 1 calc R . . C36 C 0.33350(11) 0.5843(3) 0.28591(18) 0.0590(12) Uani 1 1 d . . . H36 H 0.3525 0.5516 0.3144 0.071 Uiso 1 1 calc R A . C40 C 0.34781(15) 1.1992(4) 0.1762(3) 0.0994(17) Uani 1 1 d U . . H40 H 0.3529 1.2097 0.1343 0.119 Uiso 1 1 calc R . . C41 C 0.33046(16) 1.0955(4) 0.1936(3) 0.1152(17) Uani 1 1 d U A . H41 H 0.3235 1.0401 0.1625 0.138 Uiso 1 1 calc R . . C42 C 0.32382(13) 1.0750(3) 0.2540(3) 0.1038(15) Uani 1 1 d DU . . C43 C 0.33501(15) 1.1557(4) 0.2972(3) 0.1060(16) Uani 1 1 d U A . H43 H 0.3317 1.1437 0.3398 0.127 Uiso 1 1 calc R . . C44 C 0.35170(14) 1.2585(4) 0.2788(2) 0.0934(16) Uani 1 1 d U . . H44 H 0.3595 1.3132 0.3100 0.112 Uiso 1 1 calc R A . C45 C 0.18944(12) 0.5101(4) 0.54459(18) 0.0634(13) Uani 1 1 d . . . C46 C 0.19254(12) 0.3885(4) 0.54225(19) 0.0692(14) Uani 1 1 d . . . C47 C 0.22798(14) 0.3365(5) 0.5444(3) 0.1041(19) Uani 1 1 d . . . H47 H 0.2294 0.2562 0.5423 0.125 Uiso 1 1 calc R . . C48 C 0.26168(16) 0.4008(6) 0.5496(3) 0.128(2) Uani 1 1 d . . . H48 H 0.2853 0.3644 0.5527 0.154 Uiso 1 1 calc R . . C49 C 0.25898(16) 0.5177(6) 0.5499(3) 0.121(2) Uani 1 1 d . . . H49 H 0.2809 0.5627 0.5518 0.146 Uiso 1 1 calc R . . C50 C 0.22453(15) 0.5693(5) 0.5475(2) 0.0993(19) Uani 1 1 d . . . H50 H 0.2239 0.6498 0.5478 0.119 Uiso 1 1 calc R . . C51 C 0.15391(14) 0.5757(4) 0.5407(2) 0.0807(16) Uani 1 1 d . . . H51A H 0.1353 0.5378 0.5103 0.097 Uiso 1 1 calc R . . H51B H 0.1585 0.6521 0.5241 0.097 Uiso 1 1 calc R . . C52 C 0.13683(13) 0.5892(4) 0.6038(2) 0.0654(13) Uani 1 1 d . . . C53 C 0.15761(14) 0.3066(4) 0.53571(19) 0.0740(14) Uani 1 1 d . . . C54 C 0.01904(11) 0.1020(3) 0.34360(17) 0.0514(11) Uani 1 1 d . . . C55 C 0.03671(10) 0.1037(3) 0.28799(17) 0.0483(11) Uani 1 1 d . . . C56 C 0.02227(12) 0.1771(3) 0.23797(19) 0.0637(13) Uani 1 1 d . . . H56 H 0.0336 0.1774 0.2003 0.076 Uiso 1 1 calc R . . C57 C -0.00820(13) 0.2481(4) 0.2437(2) 0.0733(14) Uani 1 1 d . . . H57 H -0.0174 0.2954 0.2098 0.088 Uiso 1 1 calc R . . C58 C -0.02533(12) 0.2504(4) 0.2987(2) 0.0718(14) Uani 1 1 d . . . H58 H -0.0455 0.3006 0.3028 0.086 Uiso 1 1 calc R . . C59 C -0.01216(11) 0.1771(3) 0.34782(19) 0.0628(12) Uani 1 1 d . . . H59 H -0.0241 0.1772 0.3848 0.075 Uiso 1 1 calc R . . C60 C 0.03026(12) 0.0242(4) 0.39946(18) 0.0657(13) Uani 1 1 d . . . H60A H 0.0073 0.0004 0.4172 0.079 Uiso 1 1 calc R . . H60B H 0.0420 -0.0448 0.3842 0.079 Uiso 1 1 calc R . . C61 C 0.05693(16) 0.0759(5) 0.4513(2) 0.1051(4) Uani 1 1 d U . . C62 C 0.07085(11) 0.0333(3) 0.28001(19) 0.0545(12) Uani 1 1 d . . . C63 C 0.00711(13) 0.2673(4) 0.5408(2) 0.0731(14) Uani 1 1 d . . . H63 H 0.0042 0.1917 0.5259 0.088 Uiso 1 1 calc R . . C64 C -0.02507(13) 0.3291(4) 0.5501(2) 0.0720(14) Uani 1 1 d . . . H64 H -0.0491 0.2965 0.5403 0.086 Uiso 1 1 calc R . . C65 C -0.02141(13) 0.4393(4) 0.57411(17) 0.0691(14) Uani 1 1 d . . . C66 C 0.01520(13) 0.4840(4) 0.58554(18) 0.0687(14) Uani 1 1 d . . . H66 H 0.0189 0.5592 0.6006 0.082 Uiso 1 1 calc R . . C67 C 0.04566(12) 0.4178(3) 0.57466(17) 0.0612(12) Uani 1 1 d . . . H67 H 0.0699 0.4491 0.5836 0.073 Uiso 1 1 calc R . . C68 C -0.05525(13) 0.5125(4) 0.58799(19) 0.0820(16) Uani 1 1 d . . . H68A H -0.0523 0.5904 0.5722 0.098 Uiso 1 1 calc R . . H68B H -0.0784 0.4802 0.5659 0.098 Uiso 1 1 calc R . . C69 C -0.05854(12) 0.5168(4) 0.65759(18) 0.0668(13) Uani 1 1 d . . . H69A H -0.0616 0.4387 0.6731 0.080 Uiso 1 1 calc R . . H69B H -0.0351 0.5480 0.6795 0.080 Uiso 1 1 calc R . . C70 C -0.09117(13) 0.5885(4) 0.67319(18) 0.0746(14) Uani 1 1 d . . . H70A H -0.1144 0.5536 0.6530 0.090 Uiso 1 1 calc R . . H70B H -0.0889 0.6642 0.6541 0.090 Uiso 1 1 calc R . . C71 C -0.08213(14) 0.5582(4) 0.8516(2) 0.0859(16) Uani 1 1 d . . . H71 H -0.0714 0.5058 0.8819 0.103 Uiso 1 1 calc R . . C72 C -0.07920(14) 0.5356(4) 0.7892(2) 0.0904(16) Uani 1 1 d . . . H72 H -0.0657 0.4706 0.7784 0.109 Uiso 1 1 calc R . . C73 C -0.09545(11) 0.6055(3) 0.74245(18) 0.0541(11) Uani 1 1 d . . . C74 C -0.11434(13) 0.6959(4) 0.7623(2) 0.0783(15) Uani 1 1 d . . . H74 H -0.1268 0.7457 0.7323 0.094 Uiso 1 1 calc R . . C75 C -0.11579(13) 0.7173(4) 0.82573(19) 0.0771(14) Uani 1 1 d . . . H75 H -0.1291 0.7823 0.8369 0.093 Uiso 1 1 calc R . . C76 C 0.15109(14) -0.2193(3) 0.3325(2) 0.0752(15) Uani 1 1 d . . . H76 H 0.1435 -0.1610 0.3586 0.090 Uiso 1 1 calc R . . C77 C 0.16689(15) -0.3189(3) 0.3610(2) 0.0841(16) Uani 1 1 d . . . H77 H 0.1695 -0.3266 0.4051 0.101 Uiso 1 1 calc R . . C78 C 0.17860(13) -0.4057(3) 0.3239(2) 0.0714(14) Uani 1 1 d . . . C79 C 0.17313(13) -0.3910(3) 0.2600(2) 0.0774(15) Uani 1 1 d . . . H79 H 0.1801 -0.4497 0.2335 0.093 Uiso 1 1 calc R . . C80 C 0.15698(12) -0.2882(3) 0.2328(2) 0.0707(14) Uani 1 1 d . . . H80 H 0.1538 -0.2797 0.1887 0.085 Uiso 1 1 calc R . . C81 C 0.19549(13) -0.5187(3) 0.3530(2) 0.0833(16) Uani 1 1 d . . . H81A H 0.1965 -0.5139 0.3990 0.100 Uiso 1 1 calc R . . H81B H 0.1785 -0.5820 0.3389 0.100 Uiso 1 1 calc R . . C82 C 0.23356(13) -0.5454(3) 0.3364(3) 0.0834(16) Uani 1 1 d . . . H82A H 0.2513 -0.4871 0.3548 0.100 Uiso 1 1 calc R . . H82B H 0.2333 -0.5421 0.2905 0.100 Uiso 1 1 calc R . . C83 C 0.24757(13) -0.6645(4) 0.3599(3) 0.0924(18) Uani 1 1 d . . . H83A H 0.2731 -0.6771 0.3483 0.111 Uiso 1 1 calc R . . H83B H 0.2490 -0.6667 0.4061 0.111 Uiso 1 1 calc R . . C84 C 0.19657(12) -0.8784(4) 0.2443(2) 0.0715(14) Uani 1 1 d . . . H84 H 0.1973 -0.9009 0.2022 0.086 Uiso 1 1 calc R . . C85 C 0.22091(12) -0.7915(4) 0.2691(2) 0.0782(15) Uani 1 1 d . . . H85 H 0.2367 -0.7541 0.2432 0.094 Uiso 1 1 calc R . . C86 C 0.22175(13) -0.7605(3) 0.3323(2) 0.0693(14) Uani 1 1 d . . . C87 C 0.19654(14) -0.8149(3) 0.3666(2) 0.0791(16) Uani 1 1 d . . . H87 H 0.1957 -0.7953 0.4092 0.095 Uiso 1 1 calc R . . C88 C 0.17206(13) -0.8993(3) 0.33880(19) 0.0681(14) Uani 1 1 d . . . H88 H 0.1551 -0.9347 0.3633 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C37 0.066(3) 0.052(2) 0.090(4) 0.004(2) 0.025(3) 0.002(2) C38 0.082(3) 0.053(3) 0.099(4) 0.013(3) 0.018(3) 0.009(3) C39 0.089(3) 0.055(3) 0.089(3) 0.006(3) 0.021(3) -0.005(3) C37' 0.066(3) 0.052(2) 0.090(4) 0.004(2) 0.025(3) 0.002(2) C38' 0.082(3) 0.053(3) 0.099(4) 0.013(3) 0.018(3) 0.009(3) C39' 0.089(3) 0.055(3) 0.089(3) 0.006(3) 0.021(3) -0.005(3) Zn1 0.0695(3) 0.0538(3) 0.0500(3) 0.0039(2) 0.0082(2) -0.0143(2) Zn2 0.0715(3) 0.0410(2) 0.0531(3) -0.0021(2) 0.0076(2) -0.0038(2) Zn3 0.0811(3) 0.0601(3) 0.0526(3) -0.0085(2) 0.0112(2) -0.0128(3) Zn4 0.0739(3) 0.0419(2) 0.0502(3) -0.0009(2) 0.0027(2) 0.0036(2) O1 0.124(3) 0.144(3) 0.0556(18) -0.0002(19) 0.0308(18) 0.042(2) O2 0.0884(19) 0.0737(18) 0.090(2) 0.0284(16) 0.0441(16) -0.0029(17) O3 0.081(2) 0.084(2) 0.081(2) -0.0157(17) 0.0176(16) 0.0249(17) O4 0.0671(18) 0.0756(18) 0.0597(17) 0.0108(15) 0.0028(14) 0.0143(15) O5 0.097(2) 0.0682(18) 0.0524(16) -0.0101(15) 0.0036(15) 0.0038(17) O6 0.115(3) 0.088(2) 0.076(2) -0.0048(18) -0.0008(19) 0.021(2) O7 0.0659(18) 0.0778(19) 0.0775(19) 0.0017(16) 0.0050(16) -0.0173(16) O8 0.113(2) 0.0614(19) 0.113(3) 0.0116(18) -0.002(2) -0.0299(18) O9 0.118(3) 0.074(2) 0.162(3) -0.023(2) 0.045(2) -0.013(2) O10 0.0687(18) 0.093(2) 0.081(2) -0.0138(17) 0.0206(16) -0.0165(17) O11 0.100(2) 0.0675(18) 0.0425(15) 0.0058(14) 0.0096(15) 0.0097(16) O12 0.102(2) 0.091(2) 0.089(2) 0.0077(19) 0.0118(19) 0.016(2) O13 0.1192(8) 0.1245(8) 0.0617(7) -0.0156(8) -0.0046(7) 0.0299(8) O14 0.1274(8) 0.1295(8) 0.0656(8) -0.0099(8) -0.0055(8) 0.0321(8) O15 0.0768(18) 0.0667(17) 0.0556(16) -0.0076(14) 0.0108(14) 0.0089(15) O16 0.091(2) 0.090(2) 0.0717(19) 0.0056(17) 0.0002(17) 0.0370(18) N1 0.076(2) 0.0528(19) 0.0391(17) 0.0044(15) 0.0048(16) -0.0065(17) N2 0.059(2) 0.0532(19) 0.064(2) 0.0027(17) 0.0092(17) 0.0216(17) N3 0.060(2) 0.0420(17) 0.064(2) 0.0014(16) 0.0064(17) -0.0075(16) N4 0.086(2) 0.0449(18) 0.066(2) -0.0069(17) 0.0073(19) -0.0085(18) N5 0.077(2) 0.061(2) 0.0467(18) -0.0038(16) 0.0165(17) -0.0104(18) N6 0.076(2) 0.0486(19) 0.069(2) 0.0083(17) 0.0207(18) 0.0217(17) N7 0.074(2) 0.0371(17) 0.058(2) -0.0060(16) 0.0038(17) 0.0067(16) N8 0.070(2) 0.0467(19) 0.065(2) -0.0024(17) -0.0031(18) 0.0063(17) C1 0.051(2) 0.0382(19) 0.055(2) 0.0049(18) 0.0173(18) -0.0096(18) C2 0.052(2) 0.0387(19) 0.046(2) 0.0104(17) 0.0116(18) -0.0054(18) C3 0.076(3) 0.061(2) 0.047(2) -0.003(2) 0.019(2) 0.001(2) C4 0.082(3) 0.049(2) 0.083(3) 0.003(2) 0.031(2) 0.018(2) C5 0.063(3) 0.059(2) 0.086(3) 0.029(2) 0.021(2) 0.010(2) C6 0.055(2) 0.062(2) 0.057(2) 0.011(2) 0.003(2) -0.004(2) C7 0.071(3) 0.057(2) 0.056(2) 0.001(2) 0.005(2) -0.002(2) C8 0.067(3) 0.081(3) 0.049(2) 0.024(2) 0.020(2) 0.028(2) C9 0.065(3) 0.048(2) 0.055(2) 0.009(2) 0.005(2) -0.009(2) C10 0.077(3) 0.056(2) 0.040(2) -0.0027(19) 0.005(2) -0.023(2) C11 0.066(3) 0.066(3) 0.053(2) 0.004(2) -0.004(2) -0.018(2) C12 0.080(3) 0.074(3) 0.091(3) -0.002(3) -0.003(3) -0.007(3) C13 0.065(3) 0.116(4) 0.140(5) -0.018(4) 0.007(3) 0.003(3) C14 0.073(3) 0.109(4) 0.108(4) -0.024(3) 0.004(3) -0.035(3) C15 0.088(3) 0.072(3) 0.080(3) -0.008(3) 0.007(3) -0.029(3) C16 0.094(3) 0.043(2) 0.057(2) -0.005(2) 0.005(2) -0.002(2) C17 0.083(3) 0.052(2) 0.055(3) -0.005(2) 0.012(2) -0.014(2) C18 0.057(3) 0.075(3) 0.050(2) 0.005(2) -0.008(2) -0.018(2) C19 0.073(3) 0.064(3) 0.065(3) 0.009(2) 0.011(2) -0.017(2) C20 0.067(3) 0.069(3) 0.073(3) 0.013(2) 0.008(2) -0.009(2) C21 0.091(3) 0.072(3) 0.032(2) 0.001(2) 0.011(2) 0.004(3) C22 0.115(4) 0.047(2) 0.050(2) 0.010(2) 0.015(2) -0.010(3) C23 0.086(3) 0.060(3) 0.045(2) 0.011(2) 0.015(2) -0.013(2) C24 0.106(3) 0.081(3) 0.062(3) 0.008(2) 0.029(2) 0.026(3) C25 0.093(3) 0.063(3) 0.057(3) 0.005(2) 0.012(2) 0.006(3) C26 0.097(3) 0.070(3) 0.048(2) -0.002(2) 0.017(2) 0.024(3) C27 0.092(3) 0.060(3) 0.065(3) 0.006(2) 0.018(2) 0.034(2) C28 0.090(3) 0.049(2) 0.060(2) -0.004(2) 0.023(2) 0.024(2) C29 0.064(2) 0.049(2) 0.056(2) -0.002(2) 0.017(2) 0.006(2) C30 0.105(3) 0.063(3) 0.062(3) 0.010(2) 0.022(2) 0.043(2) C31 0.102(3) 0.076(3) 0.063(3) -0.006(2) 0.024(3) 0.034(3) C32 0.065(3) 0.067(3) 0.086(3) -0.005(3) -0.003(3) 0.000(2) C33 0.058(3) 0.074(3) 0.118(4) 0.013(3) 0.003(3) 0.011(3) C34 0.065(2) 0.044(2) 0.101(3) 0.003(2) 0.040(2) -0.014(2) C35 0.096(3) 0.042(2) 0.081(3) -0.004(2) 0.047(2) -0.007(2) C36 0.074(3) 0.054(2) 0.052(2) 0.008(2) 0.017(2) -0.008(2) C40 0.127(3) 0.070(3) 0.098(3) 0.005(3) -0.001(3) -0.023(3) C41 0.133(3) 0.065(3) 0.140(3) -0.014(3) -0.012(3) -0.020(3) C42 0.112(3) 0.061(2) 0.142(3) 0.002(3) 0.034(3) -0.010(2) C43 0.132(3) 0.073(3) 0.121(3) 0.017(3) 0.048(3) -0.004(3) C44 0.126(3) 0.060(3) 0.098(3) 0.003(2) 0.028(3) -0.008(3) C45 0.069(3) 0.078(3) 0.043(2) -0.003(2) 0.005(2) -0.009(2) C46 0.065(3) 0.093(3) 0.051(2) -0.006(2) 0.015(2) -0.008(3) C47 0.080(3) 0.109(4) 0.126(4) -0.041(3) 0.020(3) -0.004(3) C48 0.071(4) 0.153(5) 0.162(6) -0.028(5) 0.020(4) -0.010(4) C49 0.084(4) 0.139(5) 0.144(5) -0.008(4) 0.024(4) -0.026(4) C50 0.107(4) 0.101(4) 0.091(4) 0.002(3) 0.018(3) -0.029(3) C51 0.107(4) 0.070(3) 0.062(3) 0.011(2) -0.004(3) -0.004(3) C52 0.079(3) 0.054(2) 0.064(3) -0.007(2) 0.013(2) -0.017(2) C53 0.094(3) 0.076(3) 0.056(2) -0.016(2) 0.029(2) -0.015(3) C54 0.054(2) 0.045(2) 0.052(2) -0.0083(19) -0.0069(19) -0.0111(19) C55 0.056(2) 0.039(2) 0.049(2) -0.0052(18) 0.0020(19) -0.0041(19) C56 0.086(3) 0.053(2) 0.049(2) -0.002(2) -0.004(2) 0.011(2) C57 0.083(3) 0.064(3) 0.067(3) 0.000(2) -0.017(3) 0.006(2) C58 0.062(3) 0.067(3) 0.083(3) -0.008(3) -0.005(2) 0.005(2) C59 0.062(3) 0.069(3) 0.058(2) -0.024(2) 0.012(2) -0.013(2) C60 0.077(3) 0.068(3) 0.053(2) 0.009(2) 0.011(2) -0.010(2) C61 0.1228(7) 0.1264(7) 0.0626(7) -0.0123(7) -0.0046(7) 0.0319(7) C62 0.055(2) 0.051(2) 0.056(2) -0.007(2) 0.004(2) 0.001(2) C63 0.091(3) 0.056(3) 0.076(3) -0.008(2) 0.025(3) -0.007(3) C64 0.074(3) 0.071(3) 0.070(3) -0.013(2) 0.007(2) -0.007(3) C65 0.090(3) 0.082(3) 0.033(2) 0.000(2) 0.001(2) 0.014(3) C66 0.098(3) 0.060(3) 0.047(2) -0.006(2) 0.003(2) 0.005(3) C67 0.077(3) 0.060(3) 0.046(2) -0.011(2) 0.004(2) -0.021(2) C68 0.095(3) 0.100(3) 0.048(3) -0.003(3) -0.007(2) 0.021(3) C69 0.077(3) 0.066(3) 0.057(3) 0.000(2) 0.006(2) 0.007(2) C70 0.083(3) 0.084(3) 0.055(3) -0.002(2) -0.001(2) 0.019(3) C71 0.120(4) 0.078(3) 0.057(3) 0.008(2) 0.001(3) 0.039(3) C72 0.121(4) 0.086(3) 0.064(3) 0.003(3) 0.010(3) 0.056(3) C73 0.054(2) 0.056(2) 0.050(2) 0.006(2) -0.001(2) 0.008(2) C74 0.108(4) 0.060(3) 0.066(3) 0.007(2) 0.001(3) 0.034(3) C75 0.117(3) 0.060(3) 0.055(3) 0.001(2) 0.012(3) 0.046(3) C76 0.121(4) 0.046(2) 0.059(3) 0.001(2) 0.013(3) 0.006(3) C77 0.141(4) 0.046(2) 0.061(3) 0.007(2) -0.008(3) 0.009(3) C78 0.088(3) 0.038(2) 0.086(3) 0.015(2) -0.001(3) -0.007(2) C79 0.104(3) 0.039(2) 0.091(3) -0.017(2) 0.019(3) 0.005(2) C80 0.085(3) 0.057(3) 0.069(3) 0.004(2) 0.006(2) 0.005(3) C81 0.090(3) 0.047(2) 0.114(4) 0.013(3) 0.016(3) 0.000(2) C82 0.075(3) 0.044(2) 0.128(4) -0.003(3) -0.003(3) -0.015(2) C83 0.070(3) 0.057(3) 0.142(5) -0.003(3) -0.027(3) 0.003(3) C84 0.067(3) 0.057(3) 0.090(3) -0.012(2) 0.008(3) 0.008(2) C85 0.070(3) 0.053(3) 0.110(4) 0.005(3) 0.003(3) 0.004(2) C86 0.080(3) 0.038(2) 0.081(3) 0.002(2) -0.024(3) 0.010(2) C87 0.125(4) 0.041(2) 0.062(3) 0.005(2) -0.032(3) 0.001(3) C88 0.105(3) 0.045(2) 0.050(2) 0.007(2) -0.009(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C37 C34 1.509(6) . ? C37 C38 1.510(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.528(6) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C42 1.562(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C37' C38' 1.507(6) . ? C37' C34 1.507(6) . ? C37' H37C 0.9700 . ? C37' H37D 0.9700 . ? C38' C39' 1.526(7) . ? C38' H38C 0.9700 . ? C38' H38D 0.9700 . ? C39' C42 1.557(6) . ? C39' H39C 0.9700 . ? C39' H39D 0.9700 . ? Zn1 O7 1.995(3) . ? Zn1 O2 2.031(3) . ? Zn1 N2 2.071(3) 2_655 ? Zn1 N1 2.107(3) . ? Zn1 O1 2.469(4) . ? Zn2 O4 1.956(3) 4_576 ? Zn2 O5 1.965(3) . ? Zn2 N4 2.029(3) 1_545 ? Zn2 N3 2.092(3) . ? Zn2 C9 2.598(4) 4_576 ? Zn3 O10 1.991(3) . ? Zn3 O13 2.019(3) . ? Zn3 N6 2.056(3) 2_546 ? Zn3 N5 2.092(3) . ? Zn3 O14 2.479(4) . ? Zn3 C61 2.593(5) . ? Zn4 O15 1.946(3) . ? Zn4 O11 1.950(3) 4_565 ? Zn4 N7 2.025(3) . ? Zn4 N8 2.106(3) 1_565 ? O1 C8 1.237(5) . ? O2 C8 1.241(5) . ? O3 C9 1.215(5) . ? O4 C9 1.292(4) . ? O4 Zn2 1.956(3) 4_575 ? O5 C17 1.268(5) . ? O6 C17 1.222(5) . ? O7 C18 1.252(5) . ? O8 C18 1.232(5) . ? O9 C53 1.239(5) . ? O10 C53 1.235(5) . ? O11 C52 1.272(5) . ? O11 Zn4 1.950(3) 4_566 ? O12 C52 1.227(5) . ? O13 C61 1.215(7) . ? O14 C61 1.232(6) . ? O15 C62 1.297(4) . ? O16 C62 1.225(4) . ? N1 C19 1.342(5) . ? N1 C23 1.342(5) . ? N2 C27 1.314(5) . ? N2 C31 1.325(5) . ? N2 Zn1 2.071(3) 2_645 ? N3 C36 1.320(5) . ? N3 C32 1.342(5) . ? N4 C40 1.316(6) . ? N4 C44 1.334(6) . ? N4 Zn2 2.029(3) 1_565 ? N5 C67 1.328(5) . ? N5 C63 1.341(5) . ? N6 C75 1.319(5) . ? N6 C71 1.329(5) . ? N6 Zn3 2.056(3) 2_556 ? N7 C76 1.328(5) . ? N7 C80 1.343(5) . ? N8 C88 1.320(5) . ? N8 C84 1.338(5) . ? N8 Zn4 2.106(3) 1_545 ? C1 C6 1.378(5) . ? C1 C2 1.391(5) . ? C1 C7 1.505(5) . ? C2 C3 1.390(5) . ? C2 C9 1.515(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9300 . ? C4 C5 1.377(6) . ? C4 H4 0.9300 . ? C5 C6 1.366(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.490(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 Zn2 2.598(4) 4_575 ? C10 C11 1.380(5) . ? C10 C15 1.398(6) . ? C10 C16 1.507(6) . ? C11 C12 1.391(6) . ? C11 C18 1.503(6) . ? C12 C13 1.389(6) . ? C12 H12 0.9300 . ? C13 C14 1.351(7) . ? C13 H13 0.9300 . ? C14 C15 1.357(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.518(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C19 C20 1.360(6) . ? C19 H19 0.9300 . ? C20 C21 1.370(6) . ? C20 H20 0.9300 . ? C21 C22 1.386(6) . ? C21 C24 1.496(6) . ? C22 C23 1.359(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.493(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.498(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C29 1.483(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.375(5) . ? C27 H27 0.9300 . ? C28 C29 1.365(5) . ? C28 H28 0.9300 . ? C29 C30 1.360(5) . ? C30 C31 1.381(6) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.365(6) . ? C32 H32 0.9300 . ? C33 C34 1.362(6) . ? C33 H33 0.9300 . ? C34 C35 1.375(5) . ? C35 C36 1.371(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C40 C41 1.414(7) . ? C40 H40 0.9300 . ? C41 C42 1.343(7) . ? C41 H41 0.9300 . ? C42 C43 1.333(7) . ? C43 C44 1.400(7) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C50 1.410(6) . ? C45 C46 1.412(6) . ? C45 C51 1.459(6) . ? C46 C47 1.384(6) . ? C46 C53 1.548(6) . ? C47 C48 1.396(7) . ? C47 H47 0.9300 . ? C48 C49 1.355(8) . ? C48 H48 0.9300 . ? C49 C50 1.350(7) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.532(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C54 C55 1.391(5) . ? C54 C59 1.414(5) . ? C54 C60 1.500(5) . ? C55 C56 1.404(5) . ? C55 C62 1.480(5) . ? C56 C57 1.369(6) . ? C56 H56 0.9300 . ? C57 C58 1.369(6) . ? C57 H57 0.9300 . ? C58 C59 1.379(6) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 C61 1.485(6) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C63 C64 1.375(6) . ? C63 H63 0.9300 . ? C64 C65 1.371(6) . ? C64 H64 0.9300 . ? C65 C66 1.387(6) . ? C65 C68 1.519(6) . ? C66 C67 1.361(6) . ? C66 H66 0.9300 . ? C67 H67 0.9300 . ? C68 C69 1.488(5) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.486(6) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C73 1.500(5) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.361(6) . ? C71 H71 0.9300 . ? C72 C73 1.351(5) . ? C72 H72 0.9300 . ? C73 C74 1.333(5) . ? C74 C75 1.369(6) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C76 C77 1.387(6) . ? C76 H76 0.9300 . ? C77 C78 1.365(6) . ? C77 H77 0.9300 . ? C78 C79 1.351(6) . ? C78 C81 1.535(6) . ? C79 C80 1.411(6) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? C81 C82 1.459(6) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C83 1.526(6) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C86 1.510(6) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 C85 1.385(6) . ? C84 H84 0.9300 . ? C85 C86 1.378(6) . ? C85 H85 0.9300 . ? C86 C87 1.363(6) . ? C87 C88 1.389(6) . ? C87 H87 0.9300 . ? C88 H88 0.9300 . ? 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_3 _geom_angle_publ_flag C34 C37 C38 112.2(4) . . ? C34 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? C34 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C37 C38 C39 117.5(5) . . ? C37 C38 H38A 107.9 . . ? C39 C38 H38A 107.9 . . ? C37 C38 H38B 107.9 . . ? C39 C38 H38B 107.9 . . ? H38A C38 H38B 107.2 . . ? C38 C39 C42 106.9(4) . . ? C38 C39 H39A 110.3 . . ? C42 C39 H39A 110.3 . . ? C38 C39 H39B 110.3 . . ? C42 C39 H39B 110.3 . . ? H39A C39 H39B 108.6 . . ? C38' C37' C34 113.1(5) . . ? C38' C37' H37C 109.0 . . ? C34 C37' H37C 108.9 . . ? C38' C37' H37D 108.9 . . ? C34 C37' H37D 108.9 . . ? H37C C37' H37D 107.8 . . ? C37' C38' C39' 118.2(5) . . ? C37' C38' H38C 107.8 . . ? C39' C38' H38C 107.8 . . ? C37' C38' H38D 107.8 . . ? C39' C38' H38D 107.8 . . ? H38C C38' H38D 107.1 . . ? C38' C39' C42 106.7(5) . . ? C38' C39' H39C 110.4 . . ? C42 C39' H39C 110.4 . . ? C38' C39' H39D 110.4 . . ? C42 C39' H39D 110.4 . . ? H39C C39' H39D 108.6 . . ? O7 Zn1 O2 111.63(12) . . ? O7 Zn1 N2 101.55(12) . 2_655 ? O2 Zn1 N2 144.66(12) . 2_655 ? O7 Zn1 N1 95.19(12) . . ? O2 Zn1 N1 95.09(12) . . ? N2 Zn1 N1 93.67(12) 2_655 . ? O7 Zn1 O1 159.96(11) . . ? O2 Zn1 O1 55.95(11) . . ? N2 Zn1 O1 88.76(11) 2_655 . ? N1 Zn1 O1 101.31(11) . . ? O4 Zn2 O5 106.48(12) 4_576 . ? O4 Zn2 N4 129.87(13) 4_576 1_545 ? O5 Zn2 N4 106.96(12) . 1_545 ? O4 Zn2 N3 109.94(11) 4_576 . ? O5 Zn2 N3 94.17(12) . . ? N4 Zn2 N3 103.68(13) 1_545 . ? O4 Zn2 C9 28.80(11) 4_576 4_576 ? O5 Zn2 C9 134.92(13) . 4_576 ? N4 Zn2 C9 111.43(13) 1_545 4_576 ? N3 Zn2 C9 98.79(12) . 4_576 ? O10 Zn3 O13 110.54(14) . . ? O10 Zn3 N6 103.92(12) . 2_546 ? O13 Zn3 N6 143.18(14) . 2_546 ? O10 Zn3 N5 95.38(12) . . ? O13 Zn3 N5 94.69(13) . . ? N6 Zn3 N5 94.62(12) 2_546 . ? O10 Zn3 O14 158.41(12) . . ? O13 Zn3 O14 54.91(13) . . ? N6 Zn3 O14 88.32(11) 2_546 . ? N5 Zn3 O14 101.37(12) . . ? O10 Zn3 C61 136.64(15) . . ? O13 Zn3 C61 27.07(15) . . ? N6 Zn3 C61 116.29(15) 2_546 . ? N5 Zn3 C61 96.82(15) . . ? O14 Zn3 C61 28.00(14) . . ? O15 Zn4 O11 108.97(11) . 4_565 ? O15 Zn4 N7 128.09(12) . . ? O11 Zn4 N7 106.55(12) 4_565 . ? O15 Zn4 N8 110.06(12) . 1_565 ? O11 Zn4 N8 92.97(12) 4_565 1_565 ? N7 Zn4 N8 104.52(12) . 1_565 ? C8 O1 Zn1 81.3(3) . . ? C8 O2 Zn1 101.9(3) . . ? C9 O4 Zn2 104.4(2) . 4_575 ? C17 O5 Zn2 120.0(3) . . ? C18 O7 Zn1 103.8(3) . . ? C53 O10 Zn3 104.6(3) . . ? C52 O11 Zn4 118.9(3) . 4_566 ? C61 O13 Zn3 103.8(3) . . ? C61 O14 Zn3 81.2(3) . . ? C62 O15 Zn4 106.2(2) . . ? C19 N1 C23 116.8(3) . . ? C19 N1 Zn1 123.6(3) . . ? C23 N1 Zn1 119.6(3) . . ? C27 N2 C31 115.5(3) . . ? C27 N2 Zn1 120.3(3) . 2_645 ? C31 N2 Zn1 121.8(3) . 2_645 ? C36 N3 C32 116.8(4) . . ? C36 N3 Zn2 122.4(3) . . ? C32 N3 Zn2 120.2(3) . . ? C40 N4 C44 117.3(4) . . ? C40 N4 Zn2 120.3(3) . 1_565 ? C44 N4 Zn2 121.7(3) . 1_565 ? C67 N5 C63 116.8(4) . . ? C67 N5 Zn3 121.1(3) . . ? C63 N5 Zn3 122.0(3) . . ? C75 N6 C71 114.1(4) . . ? C75 N6 Zn3 119.7(3) . 2_556 ? C71 N6 Zn3 124.2(3) . 2_556 ? C76 N7 C80 117.3(3) . . ? C76 N7 Zn4 121.0(3) . . ? C80 N7 Zn4 120.9(3) . . ? C88 N8 C84 117.8(4) . . ? C88 N8 Zn4 122.9(3) . 1_545 ? C84 N8 Zn4 118.9(3) . 1_545 ? C6 C1 C2 117.9(3) . . ? C6 C1 C7 116.9(3) . . ? C2 C1 C7 125.2(3) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 C9 118.4(3) . . ? C1 C2 C9 122.1(3) . . ? C4 C3 C2 121.5(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 118.4(4) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 122.6(4) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? C8 C7 C1 115.7(3) . . ? C8 C7 H7A 108.4 . . ? C1 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C1 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? O1 C8 O2 120.0(4) . . ? O1 C8 C7 118.5(4) . . ? O2 C8 C7 121.1(4) . . ? O3 C9 O4 121.0(4) . . ? O3 C9 C2 123.2(3) . . ? O4 C9 C2 115.8(3) . . ? O3 C9 Zn2 74.6(2) . 4_575 ? O4 C9 Zn2 46.82(18) . 4_575 ? C2 C9 Zn2 160.7(3) . 4_575 ? C11 C10 C15 117.3(4) . . ? C11 C10 C16 125.0(4) . . ? C15 C10 C16 117.7(4) . . ? C10 C11 C12 119.5(4) . . ? C10 C11 C18 125.2(4) . . ? C12 C11 C18 115.3(4) . . ? C13 C12 C11 120.9(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 119.6(5) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 119.5(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C10 123.1(4) . . ? C14 C15 H15 118.5 . . ? C10 C15 H15 118.5 . . ? C10 C16 C17 115.8(3) . . ? C10 C16 H16A 108.3 . . ? C17 C16 H16A 108.3 . . ? C10 C16 H16B 108.3 . . ? C17 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? O6 C17 O5 124.0(4) . . ? O6 C17 C16 119.4(4) . . ? O5 C17 C16 116.7(4) . . ? O8 C18 O7 120.5(4) . . ? O8 C18 C11 120.9(4) . . ? O7 C18 C11 118.5(4) . . ? N1 C19 C20 123.0(4) . . ? N1 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 116.3(4) . . ? C20 C21 C24 122.1(4) . . ? C22 C21 C24 121.6(4) . . ? C23 C22 C21 120.7(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N1 C23 C22 122.5(4) . . ? N1 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C25 C24 C21 111.7(4) . . ? C25 C24 H24A 109.3 . . ? C21 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C21 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 113.4(4) . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C29 C26 C25 116.3(3) . . ? C29 C26 H26A 108.2 . . ? C25 C26 H26A 108.2 . . ? C29 C26 H26B 108.2 . . ? C25 C26 H26B 108.2 . . ? H26A C26 H26B 107.4 . . ? N2 C27 C28 123.7(4) . . ? N2 C27 H27 118.1 . . ? C28 C27 H27 118.1 . . ? C29 C28 C27 121.0(4) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C30 C29 C28 115.6(4) . . ? C30 C29 C26 123.1(4) . . ? C28 C29 C26 121.3(4) . . ? C29 C30 C31 120.4(4) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? N2 C31 C30 123.9(4) . . ? N2 C31 H31 118.1 . . ? C30 C31 H31 118.1 . . ? N3 C32 C33 121.7(4) . . ? N3 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C34 C33 C32 122.6(4) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C33 C34 C35 114.6(4) . . ? C33 C34 C37' 133.5(5) . . ? C35 C34 C37' 111.8(5) . . ? C33 C34 C37 114.4(5) . . ? C35 C34 C37 130.9(5) . . ? C37' C34 C37 19.1(5) . . ? C36 C35 C34 121.2(4) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? N3 C36 C35 123.0(4) . . ? N3 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? N4 C40 C41 120.8(5) . . ? N4 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 121.6(5) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C43 C42 C41 117.1(4) . . ? C43 C42 C39' 144.9(5) . . ? C41 C42 C39' 95.6(5) . . ? C43 C42 C39 108.0(5) . . ? C41 C42 C39 133.9(5) . . ? C39' C42 C39 44.7(4) . . ? C42 C43 C44 120.4(5) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? N4 C44 C43 122.5(5) . . ? N4 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C50 C45 C46 114.4(4) . . ? C50 C45 C51 119.7(4) . . ? C46 C45 C51 125.8(4) . . ? C47 C46 C45 120.3(4) . . ? C47 C46 C53 116.4(4) . . ? C45 C46 C53 123.2(4) . . ? C46 C47 C48 122.0(5) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C49 C48 C47 118.1(5) . . ? C49 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? C50 C49 C48 120.3(6) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C45 124.8(5) . . ? C49 C50 H50 117.6 . . ? C45 C50 H50 117.6 . . ? C45 C51 C52 115.1(4) . . ? C45 C51 H51A 108.5 . . ? C52 C51 H51A 108.5 . . ? C45 C51 H51B 108.5 . . ? C52 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? O12 C52 O11 124.2(4) . . ? O12 C52 C51 118.5(4) . . ? O11 C52 C51 117.3(4) . . ? O10 C53 O9 124.1(4) . . ? O10 C53 C46 118.2(4) . . ? O9 C53 C46 117.7(4) . . ? C55 C54 C59 118.1(3) . . ? C55 C54 C60 124.7(3) . . ? C59 C54 C60 117.2(3) . . ? C54 C55 C56 119.0(4) . . ? C54 C55 C62 122.5(3) . . ? C56 C55 C62 118.5(3) . . ? C57 C56 C55 121.1(4) . . ? C57 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? C58 C57 C56 120.9(4) . . ? C58 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? C57 C58 C59 118.8(4) . . ? C57 C58 H58 120.6 . . ? C59 C58 H58 120.6 . . ? C58 C59 C54 121.9(4) . . ? C58 C59 H59 119.0 . . ? C54 C59 H59 119.0 . . ? C61 C60 C54 115.3(4) . . ? C61 C60 H60A 108.5 . . ? C54 C60 H60A 108.5 . . ? C61 C60 H60B 108.5 . . ? C54 C60 H60B 108.5 . . ? H60A C60 H60B 107.5 . . ? O13 C61 O14 119.5(5) . . ? O13 C61 C60 121.9(5) . . ? O14 C61 C60 118.2(5) . . ? O13 C61 Zn3 49.1(2) . . ? O14 C61 Zn3 70.8(3) . . ? C60 C61 Zn3 164.1(4) . . ? O16 C62 O15 119.5(4) . . ? O16 C62 C55 123.2(4) . . ? O15 C62 C55 117.2(3) . . ? N5 C63 C64 123.2(4) . . ? N5 C63 H63 118.4 . . ? C64 C63 H63 118.4 . . ? C65 C64 C63 119.4(4) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? C64 C65 C66 117.2(4) . . ? C64 C65 C68 123.0(4) . . ? C66 C65 C68 119.8(4) . . ? C67 C66 C65 120.0(4) . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? N5 C67 C66 123.3(4) . . ? N5 C67 H67 118.3 . . ? C66 C67 H67 118.3 . . ? C69 C68 C65 111.1(3) . . ? C69 C68 H68A 109.4 . . ? C65 C68 H68A 109.4 . . ? C69 C68 H68B 109.4 . . ? C65 C68 H68B 109.4 . . ? H68A C68 H68B 108.0 . . ? C70 C69 C68 112.8(3) . . ? C70 C69 H69A 109.0 . . ? C68 C69 H69A 109.0 . . ? C70 C69 H69B 109.0 . . ? C68 C69 H69B 109.0 . . ? H69A C69 H69B 107.8 . . ? C69 C70 C73 117.1(3) . . ? C69 C70 H70A 108.0 . . ? C73 C70 H70A 108.0 . . ? C69 C70 H70B 108.0 . . ? C73 C70 H70B 108.0 . . ? H70A C70 H70B 107.3 . . ? N6 C71 C72 123.8(4) . . ? N6 C71 H71 118.1 . . ? C72 C71 H71 118.1 . . ? C73 C72 C71 121.3(4) . . ? C73 C72 H72 119.3 . . ? C71 C72 H72 119.3 . . ? C74 C73 C72 115.2(4) . . ? C74 C73 C70 121.2(4) . . ? C72 C73 C70 123.5(4) . . ? C73 C74 C75 121.7(4) . . ? C73 C74 H74 119.2 . . ? C75 C74 H74 119.2 . . ? N6 C75 C74 123.8(4) . . ? N6 C75 H75 118.1 . . ? C74 C75 H75 118.1 . . ? N7 C76 C77 123.6(4) . . ? N7 C76 H76 118.2 . . ? C77 C76 H76 118.2 . . ? C78 C77 C76 119.6(4) . . ? C78 C77 H77 120.2 . . ? C76 C77 H77 120.2 . . ? C79 C78 C77 117.6(4) . . ? C79 C78 C81 120.7(4) . . ? C77 C78 C81 121.6(4) . . ? C78 C79 C80 121.2(4) . . ? C78 C79 H79 119.4 . . ? C80 C79 H79 119.4 . . ? N7 C80 C79 120.7(4) . . ? N7 C80 H80 119.6 . . ? C79 C80 H80 119.6 . . ? C82 C81 C78 114.2(4) . . ? C82 C81 H81A 108.7 . . ? C78 C81 H81A 108.7 . . ? C82 C81 H81B 108.7 . . ? C78 C81 H81B 108.7 . . ? H81A C81 H81B 107.6 . . ? C81 C82 C83 112.7(4) . . ? C81 C82 H82A 109.1 . . ? C83 C82 H82A 109.1 . . ? C81 C82 H82B 109.1 . . ? C83 C82 H82B 109.1 . . ? H82A C82 H82B 107.8 . . ? C86 C83 C82 112.2(4) . . ? C86 C83 H83A 109.2 . . ? C82 C83 H83A 109.2 . . ? C86 C83 H83B 109.2 . . ? C82 C83 H83B 109.2 . . ? H83A C83 H83B 107.9 . . ? N8 C84 C85 122.4(4) . . ? N8 C84 H84 118.8 . . ? C85 C84 H84 118.8 . . ? C86 C85 C84 119.9(4) . . ? C86 C85 H85 120.0 . . ? C84 C85 H85 120.0 . . ? C87 C86 C85 116.8(4) . . ? C87 C86 C83 122.4(4) . . ? C85 C86 C83 120.7(4) . . ? C86 C87 C88 120.8(4) . . ? C86 C87 H87 119.6 . . ? C88 C87 H87 119.6 . . ? N8 C88 C87 122.2(4) . . ? N8 C88 H88 118.9 . . ? C87 C88 H88 118.9 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C34 C37 C38 C39 -53.5(8) . . . . ? C37 C38 C39 C42 169.2(6) . . . . ? C34 C37' C38' C39' 49.1(9) . . . . ? C37' C38' C39' C42 -168.5(6) . . . . ? O7 Zn1 O1 C8 -61.5(4) . . . . ? O2 Zn1 O1 C8 -5.2(2) . . . . ? N2 Zn1 O1 C8 176.8(3) 2_655 . . . ? N1 Zn1 O1 C8 83.3(2) . . . . ? O7 Zn1 O2 C8 167.4(2) . . . . ? N2 Zn1 O2 C8 8.7(4) 2_655 . . . ? N1 Zn1 O2 C8 -95.0(3) . . . . ? O1 Zn1 O2 C8 5.3(2) . . . . ? O4 Zn2 O5 C17 68.3(3) 4_576 . . . ? N4 Zn2 O5 C17 -73.8(3) 1_545 . . . ? N3 Zn2 O5 C17 -179.5(3) . . . . ? C9 Zn2 O5 C17 73.7(3) 4_576 . . . ? O2 Zn1 O7 C18 -91.1(3) . . . . ? N2 Zn1 O7 C18 76.5(3) 2_655 . . . ? N1 Zn1 O7 C18 171.4(3) . . . . ? O1 Zn1 O7 C18 -43.2(5) . . . . ? O13 Zn3 O10 C53 -89.9(3) . . . . ? N6 Zn3 O10 C53 76.9(3) 2_546 . . . ? N5 Zn3 O10 C53 173.1(3) . . . . ? O14 Zn3 O10 C53 -46.1(5) . . . . ? C61 Zn3 O10 C53 -81.1(3) . . . . ? O10 Zn3 O13 C61 166.7(3) . . . . ? N6 Zn3 O13 C61 8.3(5) 2_546 . . . ? N5 Zn3 O13 C61 -95.8(4) . . . . ? O14 Zn3 O13 C61 4.8(3) . . . . ? O10 Zn3 O14 C61 -57.1(5) . . . . ? O13 Zn3 O14 C61 -4.6(3) . . . . ? N6 Zn3 O14 C61 177.5(3) 2_546 . . . ? N5 Zn3 O14 C61 83.1(3) . . . . ? O11 Zn4 O15 C62 -170.5(2) 4_565 . . . ? N7 Zn4 O15 C62 58.8(3) . . . . ? N8 Zn4 O15 C62 -69.9(3) 1_565 . . . ? O7 Zn1 N1 C19 162.3(3) . . . . ? O2 Zn1 N1 C19 50.0(3) . . . . ? N2 Zn1 N1 C19 -95.7(3) 2_655 . . . ? O1 Zn1 N1 C19 -6.2(3) . . . . ? O7 Zn1 N1 C23 -17.3(3) . . . . ? O2 Zn1 N1 C23 -129.6(3) . . . . ? N2 Zn1 N1 C23 84.7(3) 2_655 . . . ? O1 Zn1 N1 C23 174.1(3) . . . . ? O4 Zn2 N3 C36 -60.5(3) 4_576 . . . ? O5 Zn2 N3 C36 -169.7(3) . . . . ? N4 Zn2 N3 C36 81.7(3) 1_545 . . . ? C9 Zn2 N3 C36 -33.0(3) 4_576 . . . ? O4 Zn2 N3 C32 110.3(3) 4_576 . . . ? O5 Zn2 N3 C32 1.1(3) . . . . ? N4 Zn2 N3 C32 -107.5(3) 1_545 . . . ? C9 Zn2 N3 C32 137.8(3) 4_576 . . . ? O10 Zn3 N5 C67 -17.7(3) . . . . ? O13 Zn3 N5 C67 -128.9(3) . . . . ? N6 Zn3 N5 C67 86.7(3) 2_546 . . . ? O14 Zn3 N5 C67 176.0(3) . . . . ? C61 Zn3 N5 C67 -156.0(3) . . . . ? O10 Zn3 N5 C63 163.6(3) . . . . ? O13 Zn3 N5 C63 52.4(3) . . . . ? N6 Zn3 N5 C63 -91.9(3) 2_546 . . . ? O14 Zn3 N5 C63 -2.7(3) . . . . ? C61 Zn3 N5 C63 25.3(3) . . . . ? O15 Zn4 N7 C76 -78.1(3) . . . . ? O11 Zn4 N7 C76 150.4(3) 4_565 . . . ? N8 Zn4 N7 C76 52.7(3) 1_565 . . . ? O15 Zn4 N7 C80 112.0(3) . . . . ? O11 Zn4 N7 C80 -19.6(3) 4_565 . . . ? N8 Zn4 N7 C80 -117.2(3) 1_565 . . . ? C6 C1 C2 C3 -1.0(5) . . . . ? C7 C1 C2 C3 179.0(3) . . . . ? C6 C1 C2 C9 176.7(3) . . . . ? C7 C1 C2 C9 -3.3(5) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C9 C2 C3 C4 -177.7(3) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? C3 C4 C5 C6 -2.2(6) . . . . ? C4 C5 C6 C1 1.3(6) . . . . ? C2 C1 C6 C5 0.3(6) . . . . ? C7 C1 C6 C5 -179.7(4) . . . . ? C6 C1 C7 C8 -87.1(4) . . . . ? C2 C1 C7 C8 92.8(4) . . . . ? Zn1 O1 C8 O2 8.2(4) . . . . ? Zn1 O1 C8 C7 -164.6(3) . . . . ? Zn1 O2 C8 O1 -10.1(4) . . . . ? Zn1 O2 C8 C7 162.5(3) . . . . ? C1 C7 C8 O1 167.8(4) . . . . ? C1 C7 C8 O2 -4.9(5) . . . . ? Zn2 O4 C9 O3 -8.4(4) 4_575 . . . ? Zn2 O4 C9 C2 169.9(2) 4_575 . . . ? C3 C2 C9 O3 170.3(4) . . . . ? C1 C2 C9 O3 -7.4(6) . . . . ? C3 C2 C9 O4 -7.9(5) . . . . ? C1 C2 C9 O4 174.4(3) . . . . ? C3 C2 C9 Zn2 14.9(10) . . . 4_575 ? C1 C2 C9 Zn2 -162.8(6) . . . 4_575 ? C15 C10 C11 C12 -0.5(6) . . . . ? C16 C10 C11 C12 -179.1(4) . . . . ? C15 C10 C11 C18 178.8(4) . . . . ? C16 C10 C11 C18 0.2(6) . . . . ? C10 C11 C12 C13 3.8(7) . . . . ? C18 C11 C12 C13 -175.6(4) . . . . ? C11 C12 C13 C14 -3.9(8) . . . . ? C12 C13 C14 C15 0.8(8) . . . . ? C13 C14 C15 C10 2.6(8) . . . . ? C11 C10 C15 C14 -2.7(6) . . . . ? C16 C10 C15 C14 176.0(4) . . . . ? C11 C10 C16 C17 87.6(5) . . . . ? C15 C10 C16 C17 -91.0(4) . . . . ? Zn2 O5 C17 O6 0.9(6) . . . . ? Zn2 O5 C17 C16 -178.8(3) . . . . ? C10 C16 C17 O6 177.0(4) . . . . ? C10 C16 C17 O5 -3.3(5) . . . . ? Zn1 O7 C18 O8 7.4(5) . . . . ? Zn1 O7 C18 C11 -169.0(3) . . . . ? C10 C11 C18 O8 174.8(4) . . . . ? C12 C11 C18 O8 -5.9(6) . . . . ? C10 C11 C18 O7 -8.9(6) . . . . ? C12 C11 C18 O7 170.5(4) . . . . ? C23 N1 C19 C20 -0.2(6) . . . . ? Zn1 N1 C19 C20 -179.8(3) . . . . ? N1 C19 C20 C21 1.1(6) . . . . ? C19 C20 C21 C22 -1.1(6) . . . . ? C19 C20 C21 C24 -179.2(4) . . . . ? C20 C21 C22 C23 0.2(6) . . . . ? C24 C21 C22 C23 178.3(4) . . . . ? C19 N1 C23 C22 -0.7(5) . . . . ? Zn1 N1 C23 C22 178.9(3) . . . . ? C21 C22 C23 N1 0.8(6) . . . . ? C20 C21 C24 C25 101.5(5) . . . . ? C22 C21 C24 C25 -76.6(5) . . . . ? C21 C24 C25 C26 174.4(4) . . . . ? C24 C25 C26 C29 -176.7(4) . . . . ? C31 N2 C27 C28 -1.9(6) . . . . ? Zn1 N2 C27 C28 161.0(3) 2_645 . . . ? N2 C27 C28 C29 0.0(7) . . . . ? C27 C28 C29 C30 1.3(6) . . . . ? C27 C28 C29 C26 -175.4(4) . . . . ? C25 C26 C29 C30 -11.8(6) . . . . ? C25 C26 C29 C28 164.6(4) . . . . ? C28 C29 C30 C31 -0.7(6) . . . . ? C26 C29 C30 C31 175.9(4) . . . . ? C27 N2 C31 C30 2.5(6) . . . . ? Zn1 N2 C31 C30 -160.1(4) 2_645 . . . ? C29 C30 C31 N2 -1.3(7) . . . . ? C36 N3 C32 C33 1.4(6) . . . . ? Zn2 N3 C32 C33 -169.9(3) . . . . ? N3 C32 C33 C34 1.0(7) . . . . ? C32 C33 C34 C35 -2.8(6) . . . . ? C32 C33 C34 C37' 173.9(5) . . . . ? C32 C33 C34 C37 174.5(4) . . . . ? C38' C37' C34 C33 -93.1(7) . . . . ? C38' C37' C34 C35 83.7(6) . . . . ? C38' C37' C34 C37 -94.6(11) . . . . ? C38 C37 C34 C33 -84.6(6) . . . . ? C38 C37 C34 C35 92.1(7) . . . . ? C38 C37 C34 C37' 94.2(10) . . . . ? C33 C34 C35 C36 2.4(6) . . . . ? C37' C34 C35 C36 -175.1(4) . . . . ? C37 C34 C35 C36 -174.4(4) . . . . ? C32 N3 C36 C35 -1.8(6) . . . . ? Zn2 N3 C36 C35 169.3(3) . . . . ? C34 C35 C36 N3 -0.1(6) . . . . ? C44 N4 C40 C41 4.9(7) . . . . ? Zn2 N4 C40 C41 -165.8(4) 1_565 . . . ? N4 C40 C41 C42 -2.3(8) . . . . ? C40 C41 C42 C43 -1.4(8) . . . . ? C40 C41 C42 C39' 165.4(6) . . . . ? C40 C41 C42 C39 -168.5(5) . . . . ? C38' C39' C42 C43 -21.8(11) . . . . ? C38' C39' C42 C41 179.0(5) . . . . ? C38' C39' C42 C39 25.9(5) . . . . ? C38 C39 C42 C43 126.8(5) . . . . ? C38 C39 C42 C41 -65.2(8) . . . . ? C38 C39 C42 C39' -26.6(5) . . . . ? C41 C42 C43 C44 2.2(8) . . . . ? C39' C42 C43 C44 -154.4(8) . . . . ? C39 C42 C43 C44 172.5(5) . . . . ? C40 N4 C44 C43 -4.1(7) . . . . ? Zn2 N4 C44 C43 166.5(4) 1_565 . . . ? C42 C43 C44 N4 0.6(8) . . . . ? C50 C45 C46 C47 1.5(6) . . . . ? C51 C45 C46 C47 177.9(4) . . . . ? C50 C45 C46 C53 -177.1(4) . . . . ? C51 C45 C46 C53 -0.7(6) . . . . ? C45 C46 C47 C48 0.7(7) . . . . ? C53 C46 C47 C48 179.3(5) . . . . ? C46 C47 C48 C49 -2.6(9) . . . . ? C47 C48 C49 C50 2.2(9) . . . . ? C48 C49 C50 C45 0.0(9) . . . . ? C46 C45 C50 C49 -1.9(7) . . . . ? C51 C45 C50 C49 -178.6(5) . . . . ? C50 C45 C51 C52 -99.7(5) . . . . ? C46 C45 C51 C52 84.1(5) . . . . ? Zn4 O11 C52 O12 2.8(6) 4_566 . . . ? Zn4 O11 C52 C51 -178.1(3) 4_566 . . . ? C45 C51 C52 O12 173.4(4) . . . . ? C45 C51 C52 O11 -5.8(6) . . . . ? Zn3 O10 C53 O9 4.4(5) . . . . ? Zn3 O10 C53 C46 -174.4(3) . . . . ? C47 C46 C53 O10 175.6(4) . . . . ? C45 C46 C53 O10 -5.8(6) . . . . ? C47 C46 C53 O9 -3.3(6) . . . . ? C45 C46 C53 O9 175.3(4) . . . . ? C59 C54 C55 C56 -1.8(5) . . . . ? C60 C54 C55 C56 177.1(3) . . . . ? C59 C54 C55 C62 176.6(3) . . . . ? C60 C54 C55 C62 -4.5(6) . . . . ? C54 C55 C56 C57 1.5(6) . . . . ? C62 C55 C56 C57 -177.1(4) . . . . ? C55 C56 C57 C58 0.5(6) . . . . ? C56 C57 C58 C59 -2.0(6) . . . . ? C57 C58 C59 C54 1.6(6) . . . . ? C55 C54 C59 C58 0.4(6) . . . . ? C60 C54 C59 C58 -178.6(4) . . . . ? C55 C54 C60 C61 95.0(5) . . . . ? C59 C54 C60 C61 -86.1(5) . . . . ? Zn3 O13 C61 O14 -9.1(6) . . . . ? Zn3 O13 C61 C60 163.7(4) . . . . ? Zn3 O14 C61 O13 7.3(5) . . . . ? Zn3 O14 C61 C60 -165.7(5) . . . . ? C54 C60 C61 O13 -6.0(7) . . . . ? C54 C60 C61 O14 166.8(4) . . . . ? C54 C60 C61 Zn3 45.1(16) . . . . ? O10 Zn3 C61 O13 -18.4(5) . . . . ? N6 Zn3 C61 O13 -174.4(3) 2_546 . . . ? N5 Zn3 C61 O13 87.0(4) . . . . ? O14 Zn3 C61 O13 -171.6(6) . . . . ? O10 Zn3 C61 O14 153.3(3) . . . . ? O13 Zn3 C61 O14 171.6(6) . . . . ? N6 Zn3 C61 O14 -2.8(4) 2_546 . . . ? N5 Zn3 C61 O14 -101.4(3) . . . . ? O10 Zn3 C61 C60 -79.3(14) . . . . ? O13 Zn3 C61 C60 -60.9(13) . . . . ? N6 Zn3 C61 C60 124.6(14) 2_546 . . . ? N5 Zn3 C61 C60 26.0(14) . . . . ? O14 Zn3 C61 C60 127.5(16) . . . . ? Zn4 O15 C62 O16 -6.0(4) . . . . ? Zn4 O15 C62 C55 169.4(3) . . . . ? C54 C55 C62 O16 -15.8(6) . . . . ? C56 C55 C62 O16 162.7(4) . . . . ? C54 C55 C62 O15 169.0(3) . . . . ? C56 C55 C62 O15 -12.5(5) . . . . ? C67 N5 C63 C64 1.7(6) . . . . ? Zn3 N5 C63 C64 -179.6(3) . . . . ? N5 C63 C64 C65 -2.3(6) . . . . ? C63 C64 C65 C66 2.2(6) . . . . ? C63 C64 C65 C68 -178.0(4) . . . . ? C64 C65 C66 C67 -1.8(6) . . . . ? C68 C65 C66 C67 178.4(4) . . . . ? C63 N5 C67 C66 -1.2(6) . . . . ? Zn3 N5 C67 C66 -180.0(3) . . . . ? C65 C66 C67 N5 1.4(6) . . . . ? C64 C65 C68 C69 103.6(5) . . . . ? C66 C65 C68 C69 -76.6(5) . . . . ? C65 C68 C69 C70 179.5(4) . . . . ? C68 C69 C70 C73 -175.8(4) . . . . ? C75 N6 C71 C72 3.7(7) . . . . ? Zn3 N6 C71 C72 -160.4(4) 2_556 . . . ? N6 C71 C72 C73 -2.7(8) . . . . ? C71 C72 C73 C74 -0.4(7) . . . . ? C71 C72 C73 C70 176.2(4) . . . . ? C69 C70 C73 C74 156.7(4) . . . . ? C69 C70 C73 C72 -19.8(6) . . . . ? C72 C73 C74 C75 2.1(7) . . . . ? C70 C73 C74 C75 -174.6(4) . . . . ? C71 N6 C75 C74 -2.0(7) . . . . ? Zn3 N6 C75 C74 163.0(4) 2_556 . . . ? C73 C74 C75 N6 -1.0(7) . . . . ? C80 N7 C76 C77 0.7(7) . . . . ? Zn4 N7 C76 C77 -169.5(4) . . . . ? N7 C76 C77 C78 0.5(7) . . . . ? C76 C77 C78 C79 -1.8(7) . . . . ? C76 C77 C78 C81 -178.7(4) . . . . ? C77 C78 C79 C80 1.9(7) . . . . ? C81 C78 C79 C80 178.8(4) . . . . ? C76 N7 C80 C79 -0.6(6) . . . . ? Zn4 N7 C80 C79 169.7(3) . . . . ? C78 C79 C80 N7 -0.7(7) . . . . ? C79 C78 C81 C82 60.1(6) . . . . ? C77 C78 C81 C82 -123.1(5) . . . . ? C78 C81 C82 C83 -173.6(4) . . . . ? C81 C82 C83 C86 59.8(6) . . . . ? C88 N8 C84 C85 -1.3(6) . . . . ? Zn4 N8 C84 C85 171.7(3) 1_545 . . . ? N8 C84 C85 C86 3.2(6) . . . . ? C84 C85 C86 C87 -3.2(6) . . . . ? C84 C85 C86 C83 -178.9(4) . . . . ? C82 C83 C86 C87 -103.3(5) . . . . ? C82 C83 C86 C85 72.2(6) . . . . ? C85 C86 C87 C88 1.5(6) . . . . ? C83 C86 C87 C88 177.1(4) . . . . ? C84 N8 C88 C87 -0.5(6) . . . . ? Zn4 N8 C88 C87 -173.2(3) 1_545 . . . ? C86 C87 C88 N8 0.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.522 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.064 # Attachment 'CIF-3.cif' data_c3 _database_code_depnum_ccdc_archive 'CCDC 796995' #TrackingRef 'CIF-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H12 N6 O5 Zn2' _chemical_formula_weight 463.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 32.8723(16) _cell_length_b 32.8723(16) _cell_length_c 8.4085(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7868.8(9) _cell_formula_units_Z 18 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4254 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 2.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5432 _exptl_absorpt_correction_T_max 0.7496 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17107 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3240 _reflns_number_gt 2663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.9296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3240 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.880898(11) 0.168057(12) 1.02041(4) 0.02915(12) Uani 1 1 d . . . Zn2 Zn 0.962938(12) 0.224827(13) 0.68448(4) 0.03285(12) Uani 1 1 d . . . O1 O 1.13280(8) 0.25368(8) 1.1797(3) 0.0490(6) Uani 1 1 d . . . O2 O 1.08549(10) 0.23097(10) 0.9752(3) 0.0754(9) Uani 1 1 d . . . O3 O 0.98563(7) 0.18711(8) 0.7829(2) 0.0410(5) Uani 1 1 d . . . O4 O 0.95967(8) 0.18980(9) 1.0238(2) 0.0454(6) Uani 1 1 d . . . N1 N 0.93679(8) 0.25759(9) 0.8207(3) 0.0319(6) Uani 1 1 d . . . N2 N 0.90325(8) 0.23506(8) 0.9362(3) 0.0316(6) Uani 1 1 d . . . N3 N 0.92261(9) 0.30987(8) 0.9332(3) 0.0341(6) Uani 1 1 d . . . N4 N 0.88906(8) 0.17894(8) 0.2577(3) 0.0286(5) Uani 1 1 d . . . N5 N 0.85727(8) 0.18303(8) 0.3514(3) 0.0294(5) Uani 1 1 d . . . N6 N 0.91996(8) 0.20034(8) 0.4980(2) 0.0294(5) Uani 1 1 d . . . C1 C 1.05465(11) 0.19082(11) 1.2220(3) 0.0357(7) Uani 1 1 d . . . C2 C 1.01304(11) 0.15396(11) 1.1640(4) 0.0384(8) Uani 1 1 d . . . C3 C 0.98114(13) 0.12172(13) 1.2730(4) 0.0550(10) Uani 1 1 d . . . H3 H 0.9536 0.0960 1.2363 0.066 Uiso 1 1 calc R . . C4 C 0.99000(14) 0.12761(16) 1.4363(5) 0.0677(12) Uani 1 1 d . . . H4 H 0.9679 0.1064 1.5074 0.081 Uiso 1 1 calc R . . C5 C 1.03085(14) 0.16429(16) 1.4922(4) 0.0586(11) Uani 1 1 d . . . H5 H 1.0367 0.1680 1.6010 0.070 Uiso 1 1 calc R . . C6 C 1.06342(12) 0.19595(13) 1.3864(4) 0.0468(9) Uani 1 1 d . . . H6 H 1.0914 0.2209 1.4243 0.056 Uiso 1 1 calc R . . C7 C 1.09275(12) 0.22720(12) 1.1177(4) 0.0430(8) Uani 1 1 d . . . C8 C 0.99975(12) 0.14687(12) 0.9897(4) 0.0418(8) Uani 1 1 d . . . H8A H 1.0273 0.1536 0.9275 0.050 Uiso 1 1 calc R . . H8B H 0.9764 0.1142 0.9725 0.050 Uiso 1 1 calc R . . C9 C 0.98052(10) 0.17731(11) 0.9302(3) 0.0353(7) Uani 1 1 d . . . C10 C 0.89592(11) 0.26721(11) 0.9989(4) 0.0364(7) Uani 1 1 d . . . H10 H 0.8745 0.2612 1.0803 0.044 Uiso 1 1 calc R . . C11 C 0.94718(11) 0.30156(11) 0.8231(3) 0.0373(7) Uani 1 1 d . . . H11 H 0.9692 0.3245 0.7560 0.045 Uiso 1 1 calc R . . C12 C 0.87711(10) 0.19555(11) 0.4925(3) 0.0336(7) Uani 1 1 d . . . H12 H 0.8627 0.2006 0.5796 0.040 Uiso 1 1 calc R . . C13 C 0.92592(10) 0.18993(11) 0.3486(3) 0.0342(7) Uani 1 1 d . . . H13 H 0.9529 0.1904 0.3130 0.041 Uiso 1 1 calc R . . O5 O 1.02427(15) 0.28943(14) 1.0815(5) 0.1358(17) Uani 1 1 d . . . H2W H 1.0468 0.2839 1.0904 0.204 Uiso 1 1 d R . . H1W H 1.0055 0.2612 1.0544 0.204 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0309(2) 0.0311(2) 0.02073(17) -0.00266(13) -0.00047(13) 0.01204(16) Zn2 0.0277(2) 0.0458(2) 0.02290(18) -0.00424(14) -0.00323(13) 0.01678(17) O1 0.0351(14) 0.0436(14) 0.0680(16) 0.0149(12) 0.0117(12) 0.0195(12) O2 0.079(2) 0.0665(19) 0.0374(15) 0.0166(13) 0.0153(13) 0.0039(16) O3 0.0419(13) 0.0564(15) 0.0299(11) 0.0041(10) 0.0045(9) 0.0285(12) O4 0.0476(14) 0.0691(16) 0.0314(11) -0.0071(11) -0.0034(10) 0.0380(13) N1 0.0314(14) 0.0344(15) 0.0223(12) 0.0008(10) 0.0029(10) 0.0107(12) N2 0.0302(14) 0.0280(14) 0.0310(13) -0.0003(10) 0.0064(10) 0.0105(11) N3 0.0408(15) 0.0282(14) 0.0284(13) 0.0014(10) 0.0033(11) 0.0135(12) N4 0.0287(13) 0.0330(14) 0.0216(11) -0.0026(10) -0.0010(10) 0.0135(11) N5 0.0243(13) 0.0345(14) 0.0242(12) -0.0015(10) 0.0002(10) 0.0108(11) N6 0.0293(14) 0.0362(14) 0.0193(11) -0.0017(10) -0.0025(10) 0.0139(12) C1 0.0366(18) 0.0421(19) 0.0346(16) 0.0128(14) 0.0121(13) 0.0245(16) C2 0.0394(19) 0.0429(19) 0.0382(17) 0.0122(14) 0.0074(14) 0.0245(17) C3 0.043(2) 0.053(2) 0.057(2) 0.0218(18) 0.0075(17) 0.0150(18) C4 0.049(2) 0.094(3) 0.060(3) 0.045(2) 0.024(2) 0.036(3) C5 0.055(2) 0.102(3) 0.0358(19) 0.020(2) 0.0114(18) 0.051(3) C6 0.043(2) 0.065(2) 0.0386(18) 0.0074(16) 0.0071(15) 0.0309(19) C7 0.046(2) 0.039(2) 0.049(2) 0.0090(16) 0.0187(17) 0.0252(18) C8 0.045(2) 0.043(2) 0.0421(18) 0.0014(15) 0.0022(15) 0.0249(17) C9 0.0274(16) 0.0375(18) 0.0327(17) -0.0030(13) -0.0014(13) 0.0099(14) C10 0.0368(18) 0.0320(17) 0.0368(17) 0.0012(14) 0.0084(14) 0.0145(15) C11 0.0420(19) 0.0343(18) 0.0270(15) 0.0048(13) 0.0070(13) 0.0125(15) C12 0.0289(17) 0.0473(19) 0.0202(14) -0.0039(13) -0.0005(12) 0.0157(15) C13 0.0328(17) 0.0446(19) 0.0253(15) -0.0029(13) -0.0030(12) 0.0196(15) O5 0.128(4) 0.094(3) 0.190(5) -0.049(3) -0.053(3) 0.059(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N4 2.021(2) 1_556 ? Zn1 O1 2.027(2) 12_547 ? Zn1 N2 2.067(2) . ? Zn1 N5 2.144(2) 13_656 ? Zn1 O4 2.316(2) . ? Zn1 O2 2.401(3) 12_547 ? Zn1 C7 2.546(3) 12_547 ? Zn2 O3 1.925(2) . ? Zn2 N6 1.991(2) . ? Zn2 N3 2.028(2) 8_644 ? Zn2 N1 2.034(2) . ? O1 C7 1.271(4) . ? O1 Zn1 2.027(2) 11_667 ? O2 C7 1.240(4) . ? O2 Zn1 2.401(3) 11_667 ? O3 C9 1.269(3) . ? O4 C9 1.241(4) . ? O4 O5 2.918(5) . ? N1 C11 1.309(4) . ? N1 N2 1.375(3) . ? N2 C10 1.306(4) . ? N3 C11 1.343(4) . ? N3 C10 1.346(4) . ? N3 Zn2 2.028(2) 6_665 ? N4 C13 1.321(3) . ? N4 N5 1.368(3) . ? N4 Zn1 2.021(2) 1_554 ? N5 C12 1.316(3) . ? N5 Zn1 2.144(2) 13_656 ? N6 C12 1.338(4) . ? N6 C13 1.342(3) . ? C1 C2 1.385(4) . ? C1 C6 1.405(4) . ? C1 C7 1.506(4) . ? C2 C3 1.397(4) . ? C2 C8 1.514(4) . ? C3 C4 1.397(5) . ? C3 H3 0.9300 . ? C4 C5 1.363(6) . ? C4 H4 0.9300 . ? C5 C6 1.381(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 Zn1 2.546(3) 11_667 ? C8 C9 1.511(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? O5 H2W 0.8504 . ? O5 H1W 0.8501 . ? 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_3 _geom_angle_publ_flag N4 Zn1 O1 152.12(10) 1_556 12_547 ? N4 Zn1 N2 101.79(9) 1_556 . ? O1 Zn1 N2 102.60(9) 12_547 . ? N4 Zn1 N5 103.15(8) 1_556 13_656 ? O1 Zn1 N5 90.28(9) 12_547 13_656 ? N2 Zn1 N5 89.74(9) . 13_656 ? N4 Zn1 O4 84.50(8) 1_556 . ? O1 Zn1 O4 83.97(8) 12_547 . ? N2 Zn1 O4 85.91(9) . . ? N5 Zn1 O4 171.86(8) 13_656 . ? N4 Zn1 O2 97.23(9) 1_556 12_547 ? O1 Zn1 O2 58.39(9) 12_547 12_547 ? N2 Zn1 O2 160.84(9) . 12_547 ? N5 Zn1 O2 88.14(10) 13_656 12_547 ? O4 Zn1 O2 93.72(10) . 12_547 ? N4 Zn1 C7 124.52(11) 1_556 12_547 ? O1 Zn1 C7 29.60(10) 12_547 12_547 ? N2 Zn1 C7 132.20(11) . 12_547 ? N5 Zn1 C7 90.53(10) 13_656 12_547 ? O4 Zn1 C7 87.31(9) . 12_547 ? O2 Zn1 C7 28.85(10) 12_547 12_547 ? O3 Zn2 N6 120.22(10) . . ? O3 Zn2 N3 101.30(9) . 8_644 ? N6 Zn2 N3 105.39(9) . 8_644 ? O3 Zn2 N1 120.10(9) . . ? N6 Zn2 N1 104.79(10) . . ? N3 Zn2 N1 102.51(10) 8_644 . ? C7 O1 Zn1 98.4(2) . 11_667 ? C7 O2 Zn1 82.1(2) . 11_667 ? C9 O3 Zn2 122.6(2) . . ? C9 O4 Zn1 127.40(19) . . ? C9 O4 O5 105.3(2) . . ? Zn1 O4 O5 114.97(12) . . ? C11 N1 N2 106.3(2) . . ? C11 N1 Zn2 130.3(2) . . ? N2 N1 Zn2 123.37(19) . . ? C10 N2 N1 105.8(2) . . ? C10 N2 Zn1 127.8(2) . . ? N1 N2 Zn1 125.29(19) . . ? C11 N3 C10 102.5(2) . . ? C11 N3 Zn2 131.9(2) . 6_665 ? C10 N3 Zn2 124.8(2) . 6_665 ? C13 N4 N5 106.3(2) . . ? C13 N4 Zn1 129.93(19) . 1_554 ? N5 N4 Zn1 123.07(17) . 1_554 ? C12 N5 N4 105.4(2) . . ? C12 N5 Zn1 121.68(19) . 13_656 ? N4 N5 Zn1 132.35(17) . 13_656 ? C12 N6 C13 102.5(2) . . ? C12 N6 Zn2 124.60(18) . . ? C13 N6 Zn2 132.5(2) . . ? C2 C1 C6 120.3(3) . . ? C2 C1 C7 123.7(3) . . ? C6 C1 C7 116.0(3) . . ? C1 C2 C3 118.1(3) . . ? C1 C2 C8 123.9(3) . . ? C3 C2 C8 118.0(3) . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C1 120.6(3) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? O2 C7 O1 120.9(3) . . ? O2 C7 C1 121.1(3) . . ? O1 C7 C1 118.1(3) . . ? O2 C7 Zn1 69.09(19) . 11_667 ? O1 C7 Zn1 51.97(16) . 11_667 ? C1 C7 Zn1 168.7(3) . 11_667 ? C9 C8 C2 113.7(3) . . ? C9 C8 H8A 108.8 . . ? C2 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C2 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O4 C9 O3 124.1(3) . . ? O4 C9 C8 119.5(3) . . ? O3 C9 C8 116.4(3) . . ? N2 C10 N3 112.9(3) . . ? N2 C10 H10 123.5 . . ? N3 C10 H10 123.5 . . ? N1 C11 N3 112.6(3) . . ? N1 C11 H11 123.7 . . ? N3 C11 H11 123.7 . . ? N5 C12 N6 113.3(2) . . ? N5 C12 H12 123.3 . . ? N6 C12 H12 123.3 . . ? N4 C13 N6 112.4(3) . . ? N4 C13 H13 123.8 . . ? N6 C13 H13 123.8 . . ? O4 O5 H2W 89.9 . . ? O4 O5 H1W 6.1 . . ? H2W O5 H1W 91.4 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Zn2 O3 C9 -125.0(2) . . . . ? N3 Zn2 O3 C9 119.6(2) 8_644 . . . ? N1 Zn2 O3 C9 7.8(3) . . . . ? N4 Zn1 O4 C9 151.8(3) 1_556 . . . ? O1 Zn1 O4 C9 -2.8(3) 12_547 . . . ? N2 Zn1 O4 C9 -105.9(3) . . . . ? N5 Zn1 O4 C9 -48.1(8) 13_656 . . . ? O2 Zn1 O4 C9 54.9(3) 12_547 . . . ? C7 Zn1 O4 C9 26.7(3) 12_547 . . . ? N4 Zn1 O4 O5 -71.92(13) 1_556 . . . ? O1 Zn1 O4 O5 133.51(14) 12_547 . . . ? N2 Zn1 O4 O5 30.36(13) . . . . ? N5 Zn1 O4 O5 88.2(6) 13_656 . . . ? O2 Zn1 O4 O5 -168.84(13) 12_547 . . . ? C7 Zn1 O4 O5 163.01(15) 12_547 . . . ? O3 Zn2 N1 C11 128.3(3) . . . . ? N6 Zn2 N1 C11 -92.6(3) . . . . ? N3 Zn2 N1 C11 17.2(3) 8_644 . . . ? O3 Zn2 N1 N2 -50.3(2) . . . . ? N6 Zn2 N1 N2 88.7(2) . . . . ? N3 Zn2 N1 N2 -161.4(2) 8_644 . . . ? C11 N1 N2 C10 0.2(3) . . . . ? Zn2 N1 N2 C10 179.1(2) . . . . ? C11 N1 N2 Zn1 -168.2(2) . . . . ? Zn2 N1 N2 Zn1 10.7(3) . . . . ? N4 Zn1 N2 C10 -38.6(3) 1_556 . . . ? O1 Zn1 N2 C10 155.0(3) 12_547 . . . ? N5 Zn1 N2 C10 64.8(3) 13_656 . . . ? O4 Zn1 N2 C10 -122.1(3) . . . . ? O2 Zn1 N2 C10 148.4(3) 12_547 . . . ? C7 Zn1 N2 C10 155.3(2) 12_547 . . . ? N4 Zn1 N2 N1 127.3(2) 1_556 . . . ? O1 Zn1 N2 N1 -39.1(2) 12_547 . . . ? N5 Zn1 N2 N1 -129.3(2) 13_656 . . . ? O4 Zn1 N2 N1 43.8(2) . . . . ? O2 Zn1 N2 N1 -45.8(4) 12_547 . . . ? C7 Zn1 N2 N1 -38.8(3) 12_547 . . . ? C13 N4 N5 C12 -0.9(3) . . . . ? Zn1 N4 N5 C12 -172.39(19) 1_554 . . . ? C13 N4 N5 Zn1 -172.4(2) . . . 13_656 ? Zn1 N4 N5 Zn1 16.1(3) 1_554 . . 13_656 ? O3 Zn2 N6 C12 122.1(2) . . . . ? N3 Zn2 N6 C12 -124.6(2) 8_644 . . . ? N1 Zn2 N6 C12 -16.8(3) . . . . ? O3 Zn2 N6 C13 -66.4(3) . . . . ? N3 Zn2 N6 C13 46.9(3) 8_644 . . . ? N1 Zn2 N6 C13 154.6(3) . . . . ? C6 C1 C2 C3 -1.8(5) . . . . ? C7 C1 C2 C3 178.0(3) . . . . ? C6 C1 C2 C8 177.3(3) . . . . ? C7 C1 C2 C8 -2.8(5) . . . . ? C1 C2 C3 C4 2.8(5) . . . . ? C8 C2 C3 C4 -176.4(3) . . . . ? C2 C3 C4 C5 -2.1(6) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? C2 C1 C6 C5 0.3(5) . . . . ? C7 C1 C6 C5 -179.6(3) . . . . ? Zn1 O2 C7 O1 4.8(3) 11_667 . . . ? Zn1 O2 C7 C1 -174.5(3) 11_667 . . . ? Zn1 O1 C7 O2 -5.7(4) 11_667 . . . ? Zn1 O1 C7 C1 173.6(2) 11_667 . . . ? C2 C1 C7 O2 12.9(5) . . . . ? C6 C1 C7 O2 -167.2(3) . . . . ? C2 C1 C7 O1 -166.4(3) . . . . ? C6 C1 C7 O1 13.5(4) . . . . ? C2 C1 C7 Zn1 -140.0(11) . . . 11_667 ? C6 C1 C7 Zn1 39.9(13) . . . 11_667 ? C1 C2 C8 C9 -80.1(4) . . . . ? C3 C2 C8 C9 99.0(4) . . . . ? Zn1 O4 C9 O3 64.0(4) . . . . ? O5 O4 C9 O3 -75.5(3) . . . . ? Zn1 O4 C9 C8 -113.3(3) . . . . ? O5 O4 C9 C8 107.1(3) . . . . ? Zn2 O3 C9 O4 1.9(4) . . . . ? Zn2 O3 C9 C8 179.3(2) . . . . ? C2 C8 C9 O4 -28.7(4) . . . . ? C2 C8 C9 O3 153.7(3) . . . . ? N1 N2 C10 N3 -0.3(3) . . . . ? Zn1 N2 C10 N3 167.73(19) . . . . ? C11 N3 C10 N2 0.3(3) . . . . ? Zn2 N3 C10 N2 -170.7(2) 6_665 . . . ? N2 N1 C11 N3 0.0(3) . . . . ? Zn2 N1 C11 N3 -178.83(19) . . . . ? C10 N3 C11 N1 -0.2(3) . . . . ? Zn2 N3 C11 N1 169.9(2) 6_665 . . . ? N4 N5 C12 N6 0.5(3) . . . . ? Zn1 N5 C12 N6 173.10(19) 13_656 . . . ? C13 N6 C12 N5 0.1(3) . . . . ? Zn2 N6 C12 N5 173.69(19) . . . . ? N5 N4 C13 N6 1.0(3) . . . . ? Zn1 N4 C13 N6 171.75(19) 1_554 . . . ? C12 N6 C13 N4 -0.7(3) . . . . ? Zn2 N6 C13 N4 -173.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H1W O4 0.85 2.07 2.918(5) 171.5 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.303 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.069 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.006 286 24 ' ' 2 0.333 0.667 0.886 285 24 ' ' 3 0.667 0.333 0.552 285 24 ' ' _platon_squeeze_details ; ;