# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Du, Hongbin' _publ_contact_author_email hbdu@nju.edu.cn _publ_section_title ; Two unprecedented NLO-active coordination polymers constructed by a semi-rigid tetrahedral linker ; _publ_author_name 'Hongbin Du' # Attachment '- 1-2.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 768477' #TrackingRef '- 1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H67 N O30 Zn4' _chemical_formula_sum 'C70 H67 N O30 Zn4' _chemical_formula_weight 1663.73 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 monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 24.602(4) _cell_length_b 19.992(3) _cell_length_c 18.972(3) _cell_angle_alpha 90.00 _cell_angle_beta 130.42 _cell_angle_gamma 90.00 _cell_volume 7104.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4045 _cell_measurement_theta_min 2.478 _cell_measurement_theta_max 21.391 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 1.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6913 _exptl_absorpt_correction_T_max 0.7448 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Apex 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 19190 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.99 _reflns_number_total 9935 _reflns_number_gt 7718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+1.9900P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.069(13) _refine_ls_number_reflns 9935 _refine_ls_number_parameters 853 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 C1 C -0.0037(4) 0.0899(4) 0.0840(5) 0.0466(17) Uani 1 1 d . . . C2 C 0.0600(4) 0.0950(4) 0.1885(4) 0.0477(18) Uani 1 1 d . . . H2A H 0.0640 0.1396 0.2115 0.057 Uiso 1 1 calc R . . H2B H 0.0558 0.0629 0.2231 0.057 Uiso 1 1 calc R . . C3 C 0.1826(2) 0.0518(2) 0.2708(2) 0.0413(16) Uani 1 1 d G . . C4 C 0.2039(2) 0.0539(2) 0.3588(3) 0.0490(18) Uani 1 1 d G . . H4 H 0.1731 0.0706 0.3671 0.059 Uiso 1 1 calc R . . C5 C 0.2712(3) 0.0310(2) 0.4345(2) 0.0501(19) Uani 1 1 d G . . H5 H 0.2855 0.0323 0.4935 0.060 Uiso 1 1 calc R . . C6 C 0.31728(19) 0.0060(2) 0.4222(3) 0.0519(19) Uani 1 1 d G . . C7 C 0.2960(2) 0.0039(2) 0.3341(3) 0.053(2) Uani 1 1 d G . . H7 H 0.3268 -0.0128 0.3258 0.064 Uiso 1 1 calc R . . C8 C 0.2286(2) 0.0269(3) 0.2584(2) 0.0519(18) Uani 1 1 d G . . H8 H 0.2144 0.0255 0.1995 0.062 Uiso 1 1 calc R . . C9 C 0.3904(4) -0.0194(3) 0.5018(5) 0.0387(15) Uani 1 1 d . . . C10 C -0.0032(4) 0.0166(4) 0.0586(5) 0.0524(19) Uani 1 1 d . . . H10A H -0.0433 0.0089 -0.0065 0.063 Uiso 1 1 calc R . . H10B H 0.0405 0.0075 0.0696 0.063 Uiso 1 1 calc R . . C11 C 0.0029(3) -0.09263(14) 0.1146(4) 0.0508(17) Uani 1 1 d G . . C12 C 0.0148(3) -0.1242(2) 0.0604(3) 0.062(2) Uani 1 1 d G . . H12 H 0.0190 -0.0990 0.0230 0.074 Uiso 1 1 calc R . . C13 C 0.0203(3) -0.1935(2) 0.0621(3) 0.0470(18) Uani 1 1 d G . . H13 H 0.0283 -0.2146 0.0258 0.056 Uiso 1 1 calc R . . C14 C 0.0140(3) -0.23118(14) 0.1180(4) 0.0495(18) Uani 1 1 d G . . C15 C 0.0021(3) -0.19958(19) 0.1722(3) 0.0518(19) Uani 1 1 d G . . H15 H -0.0022 -0.2248 0.2097 0.062 Uiso 1 1 calc R . . C16 C -0.0035(3) -0.1303(2) 0.1705(3) 0.0509(19) Uani 1 1 d G . . H16 H -0.0114 -0.1092 0.2068 0.061 Uiso 1 1 calc R . . C17 C 0.0250(4) -0.3066(3) 0.1258(5) 0.0484(18) Uani 1 1 d . . . C18 C -0.0703(4) 0.1051(4) 0.0651(5) 0.0463(17) Uani 1 1 d . . . H18A H -0.0845 0.0675 0.0822 0.056 Uiso 1 1 calc R . . H18B H -0.0642 0.1439 0.1003 0.056 Uiso 1 1 calc R . . C19 C -0.1887(2) 0.0886(3) -0.0832(3) 0.0517(19) Uani 1 1 d G . . C20 C -0.2225(2) 0.0652(2) -0.0512(2) 0.0457(17) Uani 1 1 d G . . H20 H -0.1994 0.0675 0.0115 0.055 Uiso 1 1 calc R . . C21 C -0.2909(2) 0.0384(2) -0.1130(3) 0.0502(19) Uani 1 1 d G . . H21 H -0.3135 0.0227 -0.0916 0.060 Uiso 1 1 calc R . . C22 C -0.3254(2) 0.0349(2) -0.2068(3) 0.054(2) Uani 1 1 d G . . C23 C -0.2916(3) 0.0583(3) -0.2388(2) 0.054(2) Uani 1 1 d G . . H23 H -0.3147 0.0560 -0.3016 0.064 Uiso 1 1 calc R . . C24 C -0.2233(3) 0.0851(3) -0.1770(3) 0.062(2) Uani 1 1 d G . . H24 H -0.2007 0.1008 -0.1984 0.074 Uiso 1 1 calc R . . C25 C -0.3955(4) -0.0014(4) -0.2731(6) 0.059(2) Uani 1 1 d . . . C26 C 0.0070(4) 0.1312(3) 0.0264(5) 0.0440(17) Uani 1 1 d . . . H26A H 0.0526 0.1211 0.0430 0.053 Uiso 1 1 calc R . . H26B H -0.0308 0.1225 -0.0391 0.053 Uiso 1 1 calc R . . C27 C 0.0002(3) 0.24888(17) -0.0053(3) 0.0457(17) Uani 1 1 d G . . C28 C -0.0070(3) 0.23609(16) -0.0830(3) 0.0473(17) Uani 1 1 d G . . H28 H -0.0058 0.1923 -0.0985 0.057 Uiso 1 1 calc R . . C29 C -0.0161(3) 0.2887(2) -0.1377(3) 0.0498(18) Uani 1 1 d G . . H29 H -0.0210 0.2802 -0.1897 0.060 Uiso 1 1 calc R . . C30 C -0.0180(3) 0.35419(18) -0.1146(3) 0.058(2) Uani 1 1 d G . . C31 C -0.0107(3) 0.36698(15) -0.0368(3) 0.053(2) Uani 1 1 d G . . H31 H -0.0119 0.4108 -0.0213 0.063 Uiso 1 1 calc R . . C32 C -0.0016(3) 0.3143(2) 0.0179(3) 0.056(2) Uani 1 1 d G . . H32 H 0.0033 0.3229 0.0699 0.068 Uiso 1 1 calc R . . C33 C -0.0268(4) 0.4091(3) -0.1755(5) 0.0479(18) Uani 1 1 d . . . C34 C 0.2303(4) 0.1669(3) 0.0666(5) 0.0396(15) Uani 1 1 d . . . C35 C 0.1682(4) 0.1187(3) 0.0188(4) 0.0373(14) Uani 1 1 d . . . H35A H 0.1373 0.1320 0.0312 0.045 Uiso 1 1 calc R . . H35B H 0.1408 0.1214 -0.0476 0.045 Uiso 1 1 calc R . . C36 C 0.1437(2) 0.00122(16) -0.0055(3) 0.0488(19) Uani 1 1 d G . . C37 C 0.1727(2) -0.0625(2) 0.0253(3) 0.058(2) Uani 1 1 d G . . H37 H 0.2200 -0.0677 0.0789 0.070 Uiso 1 1 calc R . . C38 C 0.1311(3) -0.11839(15) -0.0241(3) 0.060(2) Uani 1 1 d G . . H38 H 0.1505 -0.1610 -0.0035 0.072 Uiso 1 1 calc R . . C39 C 0.0604(2) -0.11063(16) -0.1042(3) 0.055(2) Uani 1 1 d G . . C40 C 0.03131(19) -0.0469(2) -0.1350(3) 0.0411(16) Uani 1 1 d G . . H40 H -0.0160 -0.0418 -0.1886 0.049 Uiso 1 1 calc R . . C41 C 0.0729(2) 0.00898(15) -0.0857(3) 0.050(2) Uani 1 1 d G . . H41 H 0.0535 0.0516 -0.1063 0.060 Uiso 1 1 calc R . . C42 C 0.0193(4) -0.1730(4) -0.1541(5) 0.057(2) Uani 1 1 d . . . C43 C 0.2669(4) 0.1640(4) 0.1697(4) 0.0419(16) Uani 1 1 d . . . H43A H 0.2830 0.1188 0.1932 0.050 Uiso 1 1 calc R . . H43B H 0.3079 0.1936 0.2051 0.050 Uiso 1 1 calc R . . C44 C 0.2345(2) 0.2095(2) 0.2575(2) 0.0445(17) Uani 1 1 d G . . C45 C 0.1792(2) 0.2367(2) 0.2504(2) 0.0507(19) Uani 1 1 d G . . H45 H 0.1340 0.2413 0.1927 0.061 Uiso 1 1 calc R . . C46 C 0.1914(2) 0.2572(2) 0.3297(3) 0.0447(17) Uani 1 1 d G . . H46 H 0.1543 0.2754 0.3249 0.054 Uiso 1 1 calc R . . C47 C 0.2589(3) 0.2504(2) 0.4160(2) 0.0473(17) Uani 1 1 d G . . C48 C 0.3142(2) 0.2231(3) 0.4230(2) 0.056(2) Uani 1 1 d G . . H48 H 0.3594 0.2186 0.4808 0.067 Uiso 1 1 calc R . . C49 C 0.3020(2) 0.2027(2) 0.3438(3) 0.055(2) Uani 1 1 d G . . H49 H 0.3391 0.1845 0.3485 0.066 Uiso 1 1 calc R . . C50 C 0.2769(4) 0.2720(4) 0.5040(5) 0.0478(18) Uani 1 1 d . . . C51 C 0.2023(4) 0.2352(3) 0.0303(5) 0.0463(17) Uani 1 1 d . . . H51A H 0.1808 0.2385 -0.0342 0.056 Uiso 1 1 calc R . . H51B H 0.1670 0.2473 0.0358 0.056 Uiso 1 1 calc R . . C52 C 0.2546(3) 0.34277(14) 0.0891(4) 0.059(2) Uani 1 1 d G . . C53 C 0.1880(2) 0.37277(19) 0.0259(4) 0.064(3) Uani 1 1 d G . . H53 H 0.1476 0.3465 -0.0150 0.077 Uiso 1 1 calc R . . C54 C 0.1818(2) 0.4420(2) 0.0237(3) 0.055(2) Uani 1 1 d G . . H54 H 0.1373 0.4621 -0.0186 0.066 Uiso 1 1 calc R . . C55 C 0.2422(3) 0.48122(14) 0.0849(4) 0.053(2) Uani 1 1 d G . . C56 C 0.3087(2) 0.4512(2) 0.1481(3) 0.0494(18) Uani 1 1 d G . . H56 H 0.3491 0.4775 0.1890 0.059 Uiso 1 1 calc R . . C57 C 0.3149(2) 0.3820(2) 0.1502(3) 0.056(2) Uani 1 1 d G . . H57 H 0.3594 0.3619 0.1925 0.067 Uiso 1 1 calc R . . C58 C 0.2264(5) 0.5551(3) 0.0775(6) 0.0495(19) Uani 1 1 d . . . C59 C 0.2822(4) 0.1474(4) 0.0564(5) 0.0485(18) Uani 1 1 d . . . H59A H 0.3073 0.1071 0.0915 0.058 Uiso 1 1 calc R . . H59B H 0.3168 0.1828 0.0781 0.058 Uiso 1 1 calc R . . C60 C 0.2656(3) 0.1549(2) -0.0859(3) 0.0462(18) Uani 1 1 d G . . C61 C 0.3338(2) 0.1791(2) -0.0422(2) 0.0507(18) Uani 1 1 d G . . H61 H 0.3673 0.1814 0.0220 0.061 Uiso 1 1 calc R . . C62 C 0.3519(2) 0.1997(2) -0.0946(3) 0.0476(18) Uani 1 1 d G . . H62 H 0.3975 0.2159 -0.0654 0.057 Uiso 1 1 calc R . . C63 C 0.3018(3) 0.1963(2) -0.1907(3) 0.0494(18) Uani 1 1 d G . . C64 C 0.2336(2) 0.1721(2) -0.2343(2) 0.0507(19) Uani 1 1 d G . . H64 H 0.2002 0.1698 -0.2986 0.061 Uiso 1 1 calc R . . C65 C 0.2155(2) 0.1514(2) -0.1820(3) 0.0511(19) Uani 1 1 d G . . H65 H 0.1699 0.1353 -0.2112 0.061 Uiso 1 1 calc R . . C66 C 0.3247(5) 0.2228(4) -0.2423(5) 0.053(2) Uani 1 1 d . . . C67 C 0.3124(5) 0.6238(4) 0.4561(5) 0.061(2) Uani 1 1 d . . . H67A H 0.3399 0.5875 0.4601 0.092 Uiso 1 1 calc R . . H67B H 0.2937 0.6110 0.4855 0.092 Uiso 1 1 calc R . . H67C H 0.3424 0.6624 0.4866 0.092 Uiso 1 1 calc R . . C68 C 0.1808(5) 0.6600(4) 0.3222(5) 0.052(2) Uani 1 1 d . . . H68A H 0.1644 0.6977 0.2816 0.078 Uiso 1 1 calc R . . H68B H 0.1835 0.6720 0.3734 0.078 Uiso 1 1 calc R . . H68C H 0.1481 0.6235 0.2890 0.078 Uiso 1 1 calc R . . C69 C 0.2705(5) 0.6346(4) 0.2991(5) 0.055(2) Uani 1 1 d . . . C70 C 0.3414(5) 0.6089(4) 0.3295(6) 0.066(3) Uani 1 1 d . . . H70A H 0.3739 0.6457 0.3513 0.099 Uiso 1 1 calc R . . H70B H 0.3335 0.5882 0.2779 0.099 Uiso 1 1 calc R . . H70C H 0.3614 0.5768 0.3783 0.099 Uiso 1 1 calc R . . N1 N 0.2526(4) 0.6397(3) 0.3573(5) 0.0577(19) Uani 1 1 d . . . O1 O 0.1210(3) 0.0794(2) 0.1943(4) 0.0580(15) Uani 1 1 d . . . O2 O 0.4272(3) -0.0366(2) 0.4829(3) 0.0417(11) Uani 1 1 d . . . O3 O 0.4036(3) -0.0291(2) 0.5758(3) 0.0412(11) Uani 1 1 d . . . O4 O -0.0080(3) -0.0254(2) 0.1126(4) 0.0521(13) Uani 1 1 d . . . O5 O 0.0530(3) -0.3291(2) 0.0937(4) 0.0481(12) Uani 1 1 d . . . O6 O 0.0010(3) -0.3370(2) 0.1567(4) 0.0496(13) Uani 1 1 d . . . O7 O -0.1242(3) 0.1183(2) -0.0337(3) 0.0557(15) Uani 1 1 d . . . O8 O -0.4212(3) -0.0179(3) -0.2339(4) 0.0548(14) Uani 1 1 d . . . O9 O -0.4170(3) -0.0154(2) -0.3479(4) 0.0541(14) Uani 1 1 d . . . O10 O 0.0047(3) 0.2003(2) 0.0486(3) 0.0442(12) Uani 1 1 d . . . O11 O -0.0384(3) 0.3915(2) -0.2476(3) 0.0370(10) Uani 1 1 d . . . O12 O -0.0238(3) 0.4686(2) -0.1545(4) 0.0504(13) Uani 1 1 d . . . O13 O 0.1894(3) 0.0540(2) 0.0468(3) 0.0515(14) Uani 1 1 d . . . O14 O -0.0401(3) -0.1614(3) -0.2324(3) 0.0543(14) Uani 1 1 d . . . O15 O 0.0362(3) -0.2272(2) -0.1284(4) 0.0556(15) Uani 1 1 d . . . O16 O 0.2145(3) 0.1848(3) 0.1772(3) 0.0464(12) Uani 1 1 d . . . O17 O 0.2228(3) 0.2895(3) 0.4960(4) 0.0573(15) Uani 1 1 d . . . O18 O 0.3377(3) 0.2764(2) 0.5804(4) 0.0513(13) Uani 1 1 d . . . O19 O 0.2654(3) 0.2777(2) 0.0887(4) 0.0487(12) Uani 1 1 d . . . O20 O 0.2849(3) 0.5850(2) 0.1342(4) 0.0532(14) Uani 1 1 d . . . O21 O 0.1778(3) 0.5929(3) 0.0404(4) 0.0509(13) Uani 1 1 d . . . O22 O 0.2405(3) 0.1355(3) -0.0433(4) 0.0552(14) Uani 1 1 d . . . O23 O 0.2780(3) 0.2328(2) -0.3244(4) 0.0575(15) Uani 1 1 d . . . O24 O 0.3923(3) 0.2317(3) -0.1942(4) 0.0565(14) Uani 1 1 d . . . O25 O 0.2294(3) 0.6514(3) 0.2163(4) 0.0589(16) Uani 1 1 d . . . O1W O 0.5372(3) -0.0640(3) 0.4627(4) 0.0625(16) Uani 1 1 d . . . H1W2 H 0.5363 -0.0174 0.4497 0.094 Uiso 1 1 d R . . H1W3 H 0.5015 -0.0874 0.4061 0.094 Uiso 1 1 d R . . O2W O -0.0521(3) -0.3244(2) -0.2856(4) 0.0508(13) Uani 1 1 d . . . H2W4 H -0.0033 -0.3142 -0.2556 0.076 Uiso 1 1 d R . . H2W6 H -0.0537 -0.3584 -0.2512 0.076 Uiso 1 1 d R . . O3W O 0.1264(3) 0.7190(3) 0.0403(4) 0.0528(13) Uani 1 1 d . . . H3W2 H 0.1046 0.6948 0.0600 0.079 Uiso 1 1 d R . . H3W3 H 0.0970 0.7154 -0.0257 0.079 Uiso 1 1 d R . . O4W O 0.5671(3) -0.1095(3) 0.3521(4) 0.0615(16) Uani 1 1 d . . . H4WA H 0.5705 -0.0763 0.3271 0.092 Uiso 1 1 d R . . H4WB H 0.6063 -0.1309 0.3852 0.092 Uiso 1 1 d R . . O5W O 0.8842(3) 0.5593(2) 0.6876(4) 0.0581(15) Uani 1 1 d . . . H5WA H 0.9089 0.5275 0.6913 0.087 Uiso 1 1 d R . . H5WB H 0.8803 0.5543 0.7287 0.087 Uiso 1 1 d R . . Zn1 Zn 0.51868(8) -0.07357(4) 0.54293(10) 0.0541(3) Uani 1 1 d . . . Zn2 Zn 0.48755(7) -0.07120(3) 0.68652(9) 0.03704(18) Uani 1 1 d . . . Zn3 Zn -0.10068(7) -0.24177(4) -0.29125(9) 0.0513(2) Uani 1 1 d . . . Zn4 Zn 0.22177(8) 0.68097(4) 0.10098(10) 0.0575(3) Uani 1 1 d . . . 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 C1 0.040(4) 0.044(3) 0.039(4) 0.004(3) 0.018(4) -0.005(3) C2 0.044(4) 0.057(4) 0.028(3) 0.025(3) 0.017(3) 0.022(3) C3 0.033(4) 0.047(4) 0.035(3) 0.021(3) 0.019(3) 0.014(3) C4 0.036(4) 0.073(5) 0.033(3) 0.025(3) 0.020(3) 0.026(4) C5 0.056(5) 0.045(4) 0.031(3) -0.007(3) 0.020(4) 0.009(3) C6 0.040(4) 0.039(3) 0.050(4) 0.010(3) 0.017(4) 0.001(3) C7 0.049(5) 0.044(4) 0.052(4) 0.018(3) 0.026(4) -0.008(3) C8 0.050(5) 0.055(4) 0.050(4) 0.011(3) 0.032(4) 0.014(4) C9 0.037(4) 0.040(3) 0.036(3) 0.002(3) 0.023(3) 0.000(3) C10 0.048(5) 0.044(4) 0.051(4) 0.009(3) 0.026(4) 0.014(3) C11 0.047(4) 0.034(3) 0.049(4) -0.007(3) 0.021(3) -0.005(3) C12 0.061(5) 0.053(4) 0.045(4) 0.003(4) 0.022(4) 0.015(4) C13 0.059(5) 0.042(3) 0.055(4) 0.023(3) 0.044(4) 0.022(3) C14 0.050(5) 0.036(3) 0.054(4) 0.004(3) 0.030(4) -0.001(3) C15 0.055(5) 0.038(3) 0.048(4) 0.010(3) 0.027(4) 0.021(3) C16 0.050(5) 0.040(4) 0.053(4) 0.015(3) 0.029(4) 0.011(3) C17 0.057(5) 0.042(3) 0.038(3) -0.017(3) 0.027(4) -0.009(3) C18 0.041(4) 0.042(3) 0.046(4) 0.013(3) 0.023(4) 0.003(3) C19 0.040(4) 0.055(4) 0.036(4) 0.004(3) 0.014(3) -0.002(3) C20 0.038(4) 0.047(4) 0.027(3) -0.008(3) 0.010(3) -0.014(3) C21 0.051(5) 0.037(3) 0.037(4) -0.014(3) 0.017(4) -0.015(3) C22 0.054(5) 0.038(3) 0.037(4) -0.009(3) 0.015(4) -0.004(3) C23 0.049(5) 0.057(4) 0.044(4) -0.021(3) 0.026(4) -0.009(4) C24 0.053(5) 0.075(5) 0.043(4) -0.010(4) 0.025(4) -0.018(4) C25 0.035(4) 0.057(4) 0.057(5) -0.012(4) 0.017(4) -0.004(3) C26 0.033(4) 0.043(3) 0.039(4) 0.018(3) 0.016(3) 0.015(3) C27 0.039(4) 0.040(3) 0.037(3) 0.011(3) 0.016(3) 0.001(3) C28 0.042(4) 0.042(4) 0.046(4) 0.005(3) 0.023(4) 0.012(3) C29 0.047(5) 0.045(4) 0.049(4) -0.002(3) 0.027(4) 0.010(3) C30 0.060(5) 0.037(3) 0.045(4) 0.005(3) 0.020(4) 0.000(3) C31 0.062(5) 0.041(4) 0.034(3) 0.004(3) 0.022(4) -0.008(3) C32 0.064(5) 0.031(3) 0.043(4) 0.010(3) 0.021(4) 0.001(3) C33 0.049(4) 0.036(3) 0.036(3) 0.006(3) 0.018(3) -0.012(3) C34 0.029(4) 0.050(4) 0.037(3) 0.000(3) 0.020(3) 0.007(3) C35 0.046(4) 0.034(3) 0.033(3) -0.001(2) 0.026(3) 0.003(3) C36 0.047(4) 0.033(3) 0.037(4) 0.003(3) 0.015(3) 0.008(3) C37 0.054(5) 0.035(3) 0.053(4) 0.010(3) 0.021(4) 0.013(3) C38 0.058(5) 0.048(4) 0.022(3) 0.000(3) 0.003(3) 0.008(4) C39 0.031(4) 0.051(4) 0.054(4) 0.002(3) 0.015(4) -0.004(3) C40 0.040(4) 0.042(3) 0.031(3) 0.005(3) 0.018(3) -0.002(3) C41 0.039(4) 0.021(3) 0.051(4) -0.003(3) 0.013(3) -0.004(3) C42 0.038(4) 0.044(4) 0.040(4) 0.005(3) 0.004(3) 0.001(3) C43 0.035(4) 0.057(4) 0.025(3) -0.008(3) 0.015(3) -0.013(3) C44 0.036(4) 0.031(3) 0.042(4) -0.004(3) 0.014(3) -0.005(3) C45 0.048(5) 0.046(4) 0.034(3) 0.007(3) 0.015(4) 0.006(3) C46 0.048(4) 0.044(4) 0.036(3) 0.005(3) 0.025(4) -0.004(3) C47 0.044(4) 0.042(4) 0.047(4) -0.001(3) 0.026(4) -0.004(3) C48 0.054(5) 0.062(5) 0.043(4) 0.007(3) 0.028(4) 0.004(4) C49 0.050(5) 0.043(4) 0.038(4) -0.009(3) 0.014(4) -0.008(3) C50 0.038(4) 0.047(4) 0.040(4) -0.009(3) 0.017(3) -0.002(3) C51 0.041(4) 0.038(4) 0.041(4) 0.007(3) 0.018(3) 0.000(3) C52 0.064(6) 0.040(4) 0.053(5) 0.015(3) 0.029(5) 0.002(4) C53 0.053(5) 0.035(4) 0.062(5) -0.003(3) 0.019(4) 0.009(3) C54 0.064(6) 0.026(3) 0.049(4) 0.002(3) 0.025(4) 0.001(3) C55 0.067(5) 0.040(4) 0.055(4) 0.013(3) 0.040(4) 0.004(4) C56 0.062(5) 0.041(4) 0.046(4) -0.002(3) 0.035(4) 0.001(3) C57 0.062(5) 0.033(3) 0.052(4) 0.002(3) 0.028(4) 0.022(3) C58 0.052(5) 0.034(3) 0.056(4) 0.014(3) 0.032(4) 0.012(3) C59 0.032(4) 0.054(4) 0.046(4) 0.000(3) 0.019(3) 0.014(3) C60 0.047(4) 0.040(4) 0.033(3) -0.009(3) 0.017(3) -0.005(3) C61 0.037(4) 0.051(4) 0.046(4) -0.004(3) 0.018(4) 0.000(3) C62 0.035(4) 0.045(4) 0.049(4) -0.003(3) 0.021(3) 0.014(3) C63 0.052(5) 0.038(3) 0.045(4) -0.013(3) 0.025(4) -0.011(3) C64 0.047(5) 0.051(4) 0.036(3) -0.016(3) 0.019(4) -0.013(3) C65 0.035(4) 0.049(4) 0.046(4) 0.010(3) 0.016(4) 0.007(3) C66 0.046(5) 0.045(4) 0.046(4) -0.015(3) 0.020(4) -0.011(3) C67 0.056(5) 0.061(5) 0.045(4) 0.001(4) 0.023(4) 0.007(4) C68 0.048(5) 0.048(4) 0.037(4) 0.002(3) 0.018(4) 0.008(3) C69 0.047(5) 0.044(4) 0.037(4) 0.005(3) 0.011(4) 0.004(3) C70 0.050(5) 0.044(4) 0.051(4) -0.013(4) 0.009(4) -0.014(4) N1 0.042(4) 0.044(3) 0.052(4) -0.007(3) 0.015(3) -0.006(3) O1 0.051(3) 0.046(3) 0.054(3) 0.025(2) 0.023(3) 0.022(2) O2 0.040(3) 0.034(2) 0.043(3) 0.0035(19) 0.023(2) 0.0034(19) O3 0.036(3) 0.037(2) 0.029(2) 0.0051(18) 0.011(2) 0.0021(19) O4 0.049(3) 0.043(2) 0.049(3) 0.011(2) 0.026(3) 0.009(2) O5 0.054(3) 0.044(3) 0.048(3) -0.016(2) 0.034(3) -0.014(2) O6 0.044(3) 0.039(2) 0.044(3) -0.004(2) 0.019(3) -0.005(2) O7 0.048(3) 0.040(3) 0.040(3) 0.010(2) 0.011(2) -0.022(2) O8 0.035(3) 0.049(3) 0.050(3) -0.014(2) 0.014(3) -0.004(2) O9 0.044(3) 0.035(2) 0.048(3) 0.006(2) 0.014(3) 0.006(2) O10 0.049(3) 0.027(2) 0.037(2) -0.0050(18) 0.019(2) -0.018(2) O11 0.037(3) 0.036(2) 0.032(2) 0.0031(17) 0.020(2) -0.0006(19) O12 0.047(3) 0.034(2) 0.048(3) 0.004(2) 0.021(3) 0.007(2) O13 0.050(3) 0.034(2) 0.040(3) 0.000(2) 0.016(3) 0.000(2) O14 0.050(3) 0.048(3) 0.039(3) -0.003(2) 0.017(3) 0.005(2) O15 0.046(3) 0.043(3) 0.043(3) -0.008(2) 0.013(3) 0.006(2) O16 0.040(3) 0.052(3) 0.034(2) 0.005(2) 0.018(2) -0.002(2) O17 0.052(3) 0.041(3) 0.050(3) 0.004(2) 0.021(3) 0.007(2) O18 0.044(3) 0.039(2) 0.043(3) 0.009(2) 0.016(2) 0.014(2) O19 0.043(3) 0.035(2) 0.048(3) -0.006(2) 0.021(3) 0.000(2) O20 0.052(3) 0.041(3) 0.044(3) -0.002(2) 0.021(3) 0.012(2) O21 0.043(3) 0.042(3) 0.052(3) -0.008(2) 0.024(3) -0.011(2) O22 0.047(3) 0.054(3) 0.041(3) 0.009(2) 0.018(3) 0.011(3) O23 0.047(3) 0.039(3) 0.055(3) 0.001(2) 0.019(3) 0.003(2) O24 0.042(3) 0.049(3) 0.052(3) 0.017(2) 0.019(3) 0.017(2) O25 0.049(3) 0.048(3) 0.041(3) 0.018(2) 0.012(3) 0.013(2) O1W 0.048(4) 0.053(3) 0.052(3) -0.005(2) 0.017(3) -0.013(3) O2W 0.047(3) 0.042(2) 0.047(3) 0.005(2) 0.023(3) 0.006(2) O3W 0.043(3) 0.052(3) 0.046(3) -0.008(2) 0.021(3) -0.014(2) O4W 0.049(3) 0.048(3) 0.049(3) 0.012(2) 0.015(3) 0.013(2) O5W 0.050(3) 0.035(2) 0.050(3) 0.004(2) 0.015(3) 0.005(2) Zn1 0.0444(5) 0.0347(4) 0.0481(5) 0.0057(4) 0.0143(4) 0.0056(4) Zn2 0.0373(4) 0.0360(4) 0.0321(3) 0.0031(3) 0.0199(3) 0.0006(3) Zn3 0.0435(5) 0.0393(4) 0.0429(4) 0.0086(4) 0.0155(4) 0.0138(4) Zn4 0.0473(5) 0.0393(4) 0.0546(5) 0.0009(4) 0.0190(5) 0.0028(4) _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 C1 C18 1.464(12) . ? C1 C26 1.521(10) . ? C1 C2 1.538(10) . ? C1 C10 1.546(10) . ? C2 O1 1.465(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O1 1.361(5) . ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 C9 1.500(7) . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O2 1.220(7) . ? C9 O3 1.233(7) . ? C10 O4 1.389(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O4 1.365(5) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 C17 1.523(7) . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O6 1.230(8) . ? C17 O5 1.260(8) . ? C18 O7 1.456(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O7 1.350(5) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 C25 1.507(9) . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.182(9) . ? C25 O8 1.293(10) . ? C26 O10 1.456(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O10 1.361(4) . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 C33 1.504(7) . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O12 1.242(7) . ? C33 O11 1.253(8) . ? C34 C59 1.464(8) . ? C34 C51 1.483(7) . ? C34 C35 1.511(10) . ? C34 C43 1.535(9) . ? C35 O13 1.368(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O13 1.384(5) . ? C36 C37 1.3900 . ? C36 C41 1.3900 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 C42 1.494(8) . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 O15 1.150(7) . ? C42 O14 1.258(7) . ? C43 O16 1.446(8) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O16 1.355(5) . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 H46 0.9300 . ? C47 C48 1.3900 . ? C47 C50 1.487(8) . ? C48 C49 1.3900 . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 O18 1.239(7) . ? C50 O17 1.288(8) . ? C51 O19 1.459(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O19 1.330(5) . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C53 H53 0.9300 . ? C54 C55 1.3900 . ? C54 H54 0.9300 . ? C55 C56 1.3900 . ? C55 C58 1.510(7) . ? C56 C57 1.3900 . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 O21 1.185(9) . ? C58 O20 1.257(10) . ? C58 Zn4 2.571(7) . ? C59 O22 1.473(9) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 O22 1.353(7) . ? C60 C61 1.3900 . ? C60 C65 1.3900 . ? C61 C62 1.3900 . ? C61 H61 0.9300 . ? C62 C63 1.3900 . ? C62 H62 0.9300 . ? C63 C64 1.3900 . ? C63 C66 1.506(10) . ? C64 C65 1.3900 . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 O23 1.211(9) . ? C66 O24 1.291(10) . ? C67 N1 1.486(10) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 N1 1.484(11) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 O25 1.243(9) . ? C69 N1 1.434(12) . ? C69 C70 1.527(13) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? O2 Zn1 1.893(5) . ? O3 Zn2 1.939(4) . ? O5 Zn1 2.090(5) 4_444 ? O6 Zn2 2.009(5) 4_444 ? O8 Zn2 2.015(5) 1_454 ? O9 Zn1 1.974(5) 1_454 ? O11 Zn2 1.886(5) 3_454 ? O14 Zn3 1.974(5) . ? O17 Zn4 2.093(6) 2_565 ? O18 Zn3 1.890(5) 3_556 ? O20 Zn4 2.285(5) . ? O21 Zn4 1.996(5) . ? O23 Zn4 2.086(5) 2_564 ? O24 Zn3 2.028(6) 3 ? O25 Zn4 2.153(6) . ? O1W Zn1 1.861(7) . ? O1W H1W2 0.9600 . ? O1W H1W3 0.9601 . ? O2W Zn3 2.001(5) . ? O2W H2W4 0.9601 . ? O2W H2W6 0.9601 . ? O3W Zn4 1.977(6) . ? O3W H3W2 0.9600 . ? O3W H3W3 0.9600 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8501 . ? Zn1 O9 1.974(5) 1_656 ? Zn1 O5 2.090(5) 4_545 ? Zn2 O11 1.886(5) 3_546 ? Zn2 O6 2.009(5) 4_545 ? Zn2 O8 2.015(5) 1_656 ? Zn3 O18 1.890(5) 3_444 ? Zn3 O24 2.028(6) 3_445 ? Zn4 O23 2.086(5) 2_565 ? Zn4 O17 2.093(6) 2_564 ? 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 C18 C1 C26 113.5(6) . . ? C18 C1 C2 110.2(7) . . ? C26 C1 C2 112.6(6) . . ? C18 C1 C10 110.7(6) . . ? C26 C1 C10 104.5(6) . . ? C2 C1 C10 104.9(6) . . ? O1 C2 C1 102.8(6) . . ? O1 C2 H2A 111.2 . . ? C1 C2 H2A 111.2 . . ? O1 C2 H2B 111.2 . . ? C1 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? O1 C3 C4 124.1(3) . . ? O1 C3 C8 115.6(3) . . ? C4 C3 C8 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 C9 121.8(4) . . ? C7 C6 C9 118.2(4) . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C3 120.0 . . ? C7 C8 H8 120.0 . . ? C3 C8 H8 120.0 . . ? O2 C9 O3 126.2(6) . . ? O2 C9 C6 115.7(5) . . ? O3 C9 C6 117.3(6) . . ? O4 C10 C1 108.8(6) . . ? O4 C10 H10A 109.9 . . ? C1 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C1 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O4 C11 C12 124.0(3) . . ? O4 C11 C16 115.9(3) . . ? C12 C11 C16 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 C17 119.3(4) . . ? C13 C14 C17 120.6(4) . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? O6 C17 O5 129.4(6) . . ? O6 C17 C14 115.1(6) . . ? O5 C17 C14 115.3(6) . . ? O7 C18 C1 107.0(6) . . ? O7 C18 H18A 110.3 . . ? C1 C18 H18A 110.3 . . ? O7 C18 H18B 110.3 . . ? C1 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? O7 C19 C20 127.7(3) . . ? O7 C19 C24 112.3(3) . . ? C20 C19 C24 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 C25 118.8(5) . . ? C21 C22 C25 120.7(5) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? O9 C25 O8 128.7(7) . . ? O9 C25 C22 119.7(8) . . ? O8 C25 C22 111.4(6) . . ? O10 C26 C1 104.5(6) . . ? O10 C26 H26A 110.8 . . ? C1 C26 H26A 110.8 . . ? O10 C26 H26B 110.8 . . ? C1 C26 H26B 110.8 . . ? H26A C26 H26B 108.9 . . ? O10 C27 C28 123.9(3) . . ? O10 C27 C32 116.0(3) . . ? C28 C27 C32 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 C33 122.5(4) . . ? C29 C30 C33 117.5(4) . . ? C30 C31 C32 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? O12 C33 O11 122.8(5) . . ? O12 C33 C30 120.2(6) . . ? O11 C33 C30 116.9(5) . . ? C59 C34 C51 111.5(5) . . ? C59 C34 C35 112.3(5) . . ? C51 C34 C35 108.9(5) . . ? C59 C34 C43 108.5(5) . . ? C51 C34 C43 109.8(5) . . ? C35 C34 C43 105.8(6) . . ? O13 C35 C34 112.8(5) . . ? O13 C35 H35A 109.0 . . ? C34 C35 H35A 109.0 . . ? O13 C35 H35B 109.0 . . ? C34 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? O13 C36 C37 116.0(3) . . ? O13 C36 C41 124.0(3) . . ? C37 C36 C41 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 C42 123.1(4) . . ? C38 C39 C42 116.9(4) . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C36 120.0 . . ? C40 C41 H41 120.0 . . ? C36 C41 H41 120.0 . . ? O15 C42 O14 119.9(6) . . ? O15 C42 C39 127.5(6) . . ? O14 C42 C39 112.6(5) . . ? O16 C43 C34 106.9(5) . . ? O16 C43 H43A 110.3 . . ? C34 C43 H43A 110.3 . . ? O16 C43 H43B 110.3 . . ? C34 C43 H43B 110.3 . . ? H43A C43 H43B 108.6 . . ? O16 C44 C45 114.6(3) . . ? O16 C44 C49 125.0(3) . . ? C45 C44 C49 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 C50 116.4(4) . . ? C46 C47 C50 123.6(4) . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 H49 120.0 . . ? C44 C49 H49 120.0 . . ? O18 C50 O17 119.4(6) . . ? O18 C50 C47 126.2(7) . . ? O17 C50 C47 114.4(5) . . ? O19 C51 C34 103.8(5) . . ? O19 C51 H51A 111.0 . . ? C34 C51 H51A 111.0 . . ? O19 C51 H51B 111.0 . . ? C34 C51 H51B 111.0 . . ? H51A C51 H51B 109.0 . . ? O19 C52 C53 123.1(4) . . ? O19 C52 C57 116.6(4) . . ? C53 C52 C57 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 120.0 . . ? C54 C55 C58 113.8(4) . . ? C56 C55 C58 126.2(4) . . ? C57 C56 C55 120.0 . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C52 120.0 . . ? C56 C57 H57 120.0 . . ? C52 C57 H57 120.0 . . ? O21 C58 O20 111.1(7) . . ? O21 C58 C55 141.1(8) . . ? O20 C58 C55 107.7(6) . . ? O21 C58 Zn4 48.5(4) . . ? O20 C58 Zn4 62.6(4) . . ? C55 C58 Zn4 168.1(5) . . ? C34 C59 O22 105.8(5) . . ? C34 C59 H59A 110.6 . . ? O22 C59 H59A 110.6 . . ? C34 C59 H59B 110.6 . . ? O22 C59 H59B 110.6 . . ? H59A C59 H59B 108.7 . . ? O22 C60 C61 125.8(4) . . ? O22 C60 C65 114.1(4) . . ? C61 C60 C65 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 C66 116.6(4) . . ? C64 C63 C66 123.3(4) . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C60 120.0 . . ? C64 C65 H65 120.0 . . ? C60 C65 H65 120.0 . . ? O23 C66 O24 126.8(9) . . ? O23 C66 C63 117.0(8) . . ? O24 C66 C63 116.3(6) . . ? N1 C67 H67A 109.5 . . ? N1 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N1 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N1 C68 H68A 109.5 . . ? N1 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N1 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O25 C69 N1 123.3(8) . . ? O25 C69 C70 111.2(9) . . ? N1 C69 C70 125.4(7) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 N1 C68 123.1(6) . . ? C69 N1 C67 114.1(7) . . ? C68 N1 C67 122.8(8) . . ? C3 O1 C2 123.0(4) . . ? C9 O2 Zn1 138.9(3) . . ? C9 O3 Zn2 127.7(4) . . ? C11 O4 C10 120.4(4) . . ? C17 O5 Zn1 111.8(3) . 4_444 ? C17 O6 Zn2 143.5(4) . 4_444 ? C19 O7 C18 119.6(4) . . ? C25 O8 Zn2 115.3(3) . 1_454 ? C25 O9 Zn1 146.1(4) . 1_454 ? C27 O10 C26 117.4(4) . . ? C33 O11 Zn2 132.6(3) . 3_454 ? C35 O13 C36 121.0(4) . . ? C42 O14 Zn3 113.0(3) . . ? C44 O16 C43 121.3(4) . . ? C50 O17 Zn4 127.9(4) . 2_565 ? C50 O18 Zn3 147.7(5) . 3_556 ? C52 O19 C51 117.1(5) . . ? C58 O20 Zn4 88.1(4) . . ? C58 O21 Zn4 105.0(5) . . ? C60 O22 C59 120.8(6) . . ? C66 O23 Zn4 131.9(5) . 2_564 ? C66 O24 Zn3 103.0(5) . 3 ? C69 O25 Zn4 145.3(7) . . ? Zn1 O1W H1W2 109.5 . . ? Zn1 O1W H1W3 109.4 . . ? H1W2 O1W H1W3 109.5 . . ? Zn3 O2W H2W4 109.3 . . ? Zn3 O2W H2W6 109.6 . . ? H2W4 O2W H2W6 109.5 . . ? Zn4 O3W H3W2 109.4 . . ? Zn4 O3W H3W3 109.6 . . ? H3W2 O3W H3W3 109.5 . . ? H4WA O4W H4WB 109.5 . . ? H5WA O5W H5WB 109.5 . . ? O1W Zn1 O2 107.1(2) . . ? O1W Zn1 O9 110.1(3) . 1_656 ? O2 Zn1 O9 103.5(2) . 1_656 ? O1W Zn1 O5 103.5(2) . 4_545 ? O2 Zn1 O5 127.4(2) . 4_545 ? O9 Zn1 O5 104.8(2) 1_656 4_545 ? O11 Zn2 O3 108.0(2) 3_546 . ? O11 Zn2 O6 90.8(2) 3_546 4_545 ? O3 Zn2 O6 110.2(2) . 4_545 ? O11 Zn2 O8 113.8(2) 3_546 1_656 ? O3 Zn2 O8 117.9(2) . 1_656 ? O6 Zn2 O8 112.7(2) 4_545 1_656 ? O18 Zn3 O14 104.7(2) 3_444 . ? O18 Zn3 O2W 100.3(2) 3_444 . ? O14 Zn3 O2W 115.9(2) . . ? O18 Zn3 O24 138.7(2) 3_444 3_445 ? O14 Zn3 O24 100.2(2) . 3_445 ? O2W Zn3 O24 97.7(2) . 3_445 ? O3W Zn4 O21 90.5(2) . . ? O3W Zn4 O23 95.3(2) . 2_565 ? O21 Zn4 O23 173.7(2) . 2_565 ? O3W Zn4 O17 94.6(2) . 2_564 ? O21 Zn4 O17 92.2(2) . 2_564 ? O23 Zn4 O17 90.0(2) 2_565 2_564 ? O3W Zn4 O25 89.2(2) . . ? O21 Zn4 O25 90.0(2) . . ? O23 Zn4 O25 87.4(2) 2_565 . ? O17 Zn4 O25 175.6(2) 2_564 . ? O3W Zn4 O20 145.2(2) . . ? O21 Zn4 O20 55.6(2) . . ? O23 Zn4 O20 118.3(2) 2_565 . ? O17 Zn4 O20 94.3(2) 2_564 . ? O25 Zn4 O20 83.9(2) . . ? O3W Zn4 C58 116.4(2) . . ? O21 Zn4 C58 26.4(2) . . ? O23 Zn4 C58 147.4(3) 2_565 . ? O17 Zn4 C58 94.7(2) 2_564 . ? O25 Zn4 C58 85.6(2) . . ? O20 Zn4 C58 29.2(2) . . ? 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 C18 C1 C2 O1 -179.3(5) . . . . ? C26 C1 C2 O1 -51.6(7) . . . . ? C10 C1 C2 O1 61.5(7) . . . . ? O1 C3 C4 C5 -172.9(5) . . . . ? C8 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C4 C5 C6 C9 -179.9(5) . . . . ? C5 C6 C7 C8 0.0 . . . . ? C9 C6 C7 C8 179.9(5) . . . . ? C6 C7 C8 C3 0.0 . . . . ? O1 C3 C8 C7 173.4(4) . . . . ? C4 C3 C8 C7 0.0 . . . . ? C5 C6 C9 O2 -176.1(4) . . . . ? C7 C6 C9 O2 4.0(7) . . . . ? C5 C6 C9 O3 13.3(7) . . . . ? C7 C6 C9 O3 -166.6(4) . . . . ? C18 C1 C10 O4 -61.3(8) . . . . ? C26 C1 C10 O4 176.2(5) . . . . ? C2 C1 C10 O4 57.5(8) . . . . ? O4 C11 C12 C13 -175.5(5) . . . . ? C16 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C12 C13 C14 C17 -175.8(6) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C17 C14 C15 C16 175.8(6) . . . . ? C14 C15 C16 C11 0.0 . . . . ? O4 C11 C16 C15 175.8(5) . . . . ? C12 C11 C16 C15 0.0 . . . . ? C15 C14 C17 O6 22.0(8) . . . . ? C13 C14 C17 O6 -162.3(4) . . . . ? C15 C14 C17 O5 -162.7(4) . . . . ? C13 C14 C17 O5 13.1(8) . . . . ? C26 C1 C18 O7 36.7(8) . . . . ? C2 C1 C18 O7 164.0(5) . . . . ? C10 C1 C18 O7 -80.4(7) . . . . ? O7 C19 C20 C21 177.2(5) . . . . ? C24 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C20 C21 C22 C25 172.5(6) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C25 C22 C23 C24 -172.6(6) . . . . ? C22 C23 C24 C19 0.0 . . . . ? O7 C19 C24 C23 -177.6(4) . . . . ? C20 C19 C24 C23 0.0 . . . . ? C23 C22 C25 O9 7.6(9) . . . . ? C21 C22 C25 O9 -165.0(5) . . . . ? C23 C22 C25 O8 -177.8(4) . . . . ? C21 C22 C25 O8 9.6(8) . . . . ? C18 C1 C26 O10 57.9(7) . . . . ? C2 C1 C26 O10 -68.1(7) . . . . ? C10 C1 C26 O10 178.6(5) . . . . ? O10 C27 C28 C29 175.6(5) . . . . ? C32 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C28 C29 C30 C33 179.0(6) . . . . ? C29 C30 C31 C32 0.0 . . . . ? C33 C30 C31 C32 -179.0(6) . . . . ? C30 C31 C32 C27 0.0 . . . . ? O10 C27 C32 C31 -175.9(5) . . . . ? C28 C27 C32 C31 0.0 . . . . ? C31 C30 C33 O12 4.0(9) . . . . ? C29 C30 C33 O12 -175.0(5) . . . . ? C31 C30 C33 O11 -174.6(5) . . . . ? C29 C30 C33 O11 6.4(8) . . . . ? C59 C34 C35 O13 54.7(7) . . . . ? C51 C34 C35 O13 178.6(5) . . . . ? C43 C34 C35 O13 -63.4(7) . . . . ? O13 C36 C37 C38 -178.7(5) . . . . ? C41 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C37 C38 C39 C42 179.2(6) . . . . ? C38 C39 C40 C41 0.0 . . . . ? C42 C39 C40 C41 -179.2(7) . . . . ? C39 C40 C41 C36 0.0 . . . . ? O13 C36 C41 C40 178.5(5) . . . . ? C37 C36 C41 C40 0.0 . . . . ? C40 C39 C42 O15 -170.3(7) . . . . ? C38 C39 C42 O15 10.5(12) . . . . ? C40 C39 C42 O14 9.3(10) . . . . ? C38 C39 C42 O14 -169.9(5) . . . . ? C59 C34 C43 O16 178.9(4) . . . . ? C51 C34 C43 O16 56.8(6) . . . . ? C35 C34 C43 O16 -60.5(6) . . . . ? O16 C44 C45 C46 173.1(4) . . . . ? C49 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C45 C46 C47 C50 178.9(5) . . . . ? C46 C47 C48 C49 0.0 . . . . ? C50 C47 C48 C49 -179.0(5) . . . . ? C47 C48 C49 C44 0.0 . . . . ? O16 C44 C49 C48 -172.4(4) . . . . ? C45 C44 C49 C48 0.0 . . . . ? C48 C47 C50 O18 10.4(9) . . . . ? C46 C47 C50 O18 -168.5(5) . . . . ? C48 C47 C50 O17 -172.2(4) . . . . ? C46 C47 C50 O17 8.9(8) . . . . ? C59 C34 C51 O19 -62.2(6) . . . . ? C35 C34 C51 O19 173.4(4) . . . . ? C43 C34 C51 O19 58.1(6) . . . . ? O19 C52 C53 C54 -172.9(6) . . . . ? C57 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C53 C54 C55 C58 -177.0(6) . . . . ? C54 C55 C56 C57 0.0 . . . . ? C58 C55 C56 C57 176.6(6) . . . . ? C55 C56 C57 C52 0.0 . . . . ? O19 C52 C57 C56 173.4(6) . . . . ? C53 C52 C57 C56 0.0 . . . . ? C54 C55 C58 O21 7.4(14) . . . . ? C56 C55 C58 O21 -169.4(10) . . . . ? C54 C55 C58 O20 -178.5(5) . . . . ? C56 C55 C58 O20 4.7(9) . . . . ? C54 C55 C58 Zn4 148(3) . . . . ? C56 C55 C58 Zn4 -29(3) . . . . ? C51 C34 C59 O22 -72.2(6) . . . . ? C35 C34 C59 O22 50.3(6) . . . . ? C43 C34 C59 O22 166.8(4) . . . . ? O22 C60 C61 C62 -177.6(5) . . . . ? C65 C60 C61 C62 0.0 . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C61 C62 C63 C66 177.1(5) . . . . ? C62 C63 C64 C65 0.0 . . . . ? C66 C63 C64 C65 -176.9(6) . . . . ? C63 C64 C65 C60 0.0 . . . . ? O22 C60 C65 C64 177.8(5) . . . . ? C61 C60 C65 C64 0.0 . . . . ? C62 C63 C66 O23 -165.3(5) . . . . ? C64 C63 C66 O23 11.7(9) . . . . ? C62 C63 C66 O24 15.6(8) . . . . ? C64 C63 C66 O24 -167.4(5) . . . . ? O25 C69 N1 C68 5.6(12) . . . . ? C70 C69 N1 C68 -175.1(7) . . . . ? O25 C69 N1 C67 -173.7(7) . . . . ? C70 C69 N1 C67 5.6(11) . . . . ? C4 C3 O1 C2 -20.4(6) . . . . ? C8 C3 O1 C2 166.5(4) . . . . ? C1 C2 O1 C3 -152.6(4) . . . . ? O3 C9 O2 Zn1 -8.4(10) . . . . ? C6 C9 O2 Zn1 -178.1(4) . . . . ? O2 C9 O3 Zn2 2.5(8) . . . . ? C6 C9 O3 Zn2 172.0(3) . . . . ? C12 C11 O4 C10 -4.1(6) . . . . ? C16 C11 O4 C10 -179.7(4) . . . . ? C1 C10 O4 C11 -169.4(5) . . . . ? O6 C17 O5 Zn1 24.8(9) . . . 4_444 ? C14 C17 O5 Zn1 -149.7(4) . . . 4_444 ? O5 C17 O6 Zn2 2.9(12) . . . 4_444 ? C14 C17 O6 Zn2 177.5(4) . . . 4_444 ? C20 C19 O7 C18 25.2(6) . . . . ? C24 C19 O7 C18 -157.4(4) . . . . ? C1 C18 O7 C19 132.3(5) . . . . ? O9 C25 O8 Zn2 -2.9(10) . . . 1_454 ? C22 C25 O8 Zn2 -176.9(4) . . . 1_454 ? O8 C25 O9 Zn1 -14.3(14) . . . 1_454 ? C22 C25 O9 Zn1 159.3(5) . . . 1_454 ? C28 C27 O10 C26 4.4(5) . . . . ? C32 C27 O10 C26 -179.8(4) . . . . ? C1 C26 O10 C27 -168.7(4) . . . . ? O12 C33 O11 Zn2 34.7(10) . . . 3_454 ? C30 C33 O11 Zn2 -146.8(4) . . . 3_454 ? C34 C35 O13 C36 -162.0(5) . . . . ? C37 C36 O13 C35 174.6(4) . . . . ? C41 C36 O13 C35 -4.0(6) . . . . ? O15 C42 O14 Zn3 8.1(11) . . . . ? C39 C42 O14 Zn3 -171.6(5) . . . . ? C45 C44 O16 C43 170.6(4) . . . . ? C49 C44 O16 C43 -16.6(5) . . . . ? C34 C43 O16 C44 -157.2(4) . . . . ? O18 C50 O17 Zn4 -5.4(9) . . . 2_565 ? C47 C50 O17 Zn4 177.0(3) . . . 2_565 ? O17 C50 O18 Zn3 48.9(10) . . . 3_556 ? C47 C50 O18 Zn3 -133.8(6) . . . 3_556 ? C53 C52 O19 C51 -11.6(8) . . . . ? C57 C52 O19 C51 175.3(5) . . . . ? C34 C51 O19 C52 -162.6(5) . . . . ? O21 C58 O20 Zn4 3.5(7) . . . . ? C55 C58 O20 Zn4 -172.6(5) . . . . ? O20 C58 O21 Zn4 -4.1(8) . . . . ? C55 C58 O21 Zn4 169.9(10) . . . . ? C61 C60 O22 C59 8.7(8) . . . . ? C65 C60 O22 C59 -169.0(5) . . . . ? C34 C59 O22 C60 140.6(6) . . . . ? O24 C66 O23 Zn4 -85.2(11) . . . 2_564 ? C63 C66 O23 Zn4 95.8(8) . . . 2_564 ? O23 C66 O24 Zn3 -4.4(9) . . . 3 ? C63 C66 O24 Zn3 174.7(5) . . . 3 ? N1 C69 O25 Zn4 158.6(6) . . . . ? C70 C69 O25 Zn4 -20.8(12) . . . . ? C9 O2 Zn1 O1W -166.8(5) . . . . ? C9 O2 Zn1 O9 -50.5(6) . . . 1_656 ? C9 O2 Zn1 O5 70.4(6) . . . 4_545 ? C9 O3 Zn2 O11 -153.6(4) . . . 3_546 ? C9 O3 Zn2 O6 -55.8(5) . . . 4_545 ? C9 O3 Zn2 O8 75.6(4) . . . 1_656 ? C42 O14 Zn3 O18 -154.7(5) . . . 3_444 ? C42 O14 Zn3 O2W -45.3(5) . . . . ? C42 O14 Zn3 O24 58.6(5) . . . 3_445 ? C58 O21 Zn4 O3W -169.2(6) . . . . ? C58 O21 Zn4 O23 -14(3) . . . 2_565 ? C58 O21 Zn4 O17 96.2(6) . . . 2_564 ? C58 O21 Zn4 O25 -80.0(6) . . . . ? C58 O21 Zn4 O20 2.6(5) . . . . ? C69 O25 Zn4 O3W -160.9(9) . . . . ? C69 O25 Zn4 O21 108.6(9) . . . . ? C69 O25 Zn4 O23 -65.6(9) . . . 2_565 ? C69 O25 Zn4 O17 -11(3) . . . 2_564 ? C69 O25 Zn4 O20 53.2(9) . . . . ? C69 O25 Zn4 C58 82.6(9) . . . . ? C58 O20 Zn4 O3W 12.3(7) . . . . ? C58 O20 Zn4 O21 -2.3(5) . . . . ? C58 O20 Zn4 O23 175.7(5) . . . 2_565 ? C58 O20 Zn4 O17 -92.0(5) . . . 2_564 ? C58 O20 Zn4 O25 91.9(5) . . . . ? O21 C58 Zn4 O3W 12.1(6) . . . . ? O20 C58 Zn4 O3W -172.2(4) . . . . ? C55 C58 Zn4 O3W -135(3) . . . . ? O20 C58 Zn4 O21 175.7(9) . . . . ? C55 C58 Zn4 O21 -148(3) . . . . ? O21 C58 Zn4 O23 177.2(5) . . . 2_565 ? O20 C58 Zn4 O23 -7.1(7) . . . 2_565 ? C55 C58 Zn4 O23 30(3) . . . 2_565 ? O21 C58 Zn4 O17 -85.4(6) . . . 2_564 ? O20 C58 Zn4 O17 90.3(5) . . . 2_564 ? C55 C58 Zn4 O17 127(3) . . . 2_564 ? O21 C58 Zn4 O25 99.0(6) . . . . ? O20 C58 Zn4 O25 -85.3(5) . . . . ? C55 C58 Zn4 O25 -49(3) . . . . ? O21 C58 Zn4 O20 -175.7(9) . . . . ? C55 C58 Zn4 O20 37(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.507 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.074 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 771904' #TrackingRef '- 1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H46 Cd2 N2 O16 ' _chemical_formula_sum 'C41 H46 Cd2 N2 O16' _chemical_formula_weight 1047.60 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 _symmetry_space_group_name_Hall I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 22.5854(10) _cell_length_b 22.5854(10) _cell_length_c 8.8962(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4538.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 7529 _cell_measurement_theta_min 2.461 _cell_measurement_theta_max 28.251 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7658 _exptl_absorpt_correction_T_max 0.8089 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Apex CCD' _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 12290 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4429 _reflns_number_gt 3747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0600P)^2^+1.9900P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 4429 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 C1 C 0.5000 0.0000 -0.7500 0.027(2) Uani 1 4 d S . . C2 C 0.5358(3) 0.0425(2) -0.6543(7) 0.0351(13) Uani 1 1 d . . . H2A H 0.5613 0.0664 -0.7176 0.042 Uiso 1 1 calc R . . H2B H 0.5095 0.0687 -0.5995 0.042 Uiso 1 1 calc R . . C3 C 0.5996(3) 0.0391(3) -0.4414(6) 0.0318(13) Uani 1 1 d . . . C4 C 0.6118(3) 0.0998(3) -0.4503(7) 0.0376(14) Uani 1 1 d . . . H4 H 0.6007 0.1214 -0.5346 0.045 Uiso 1 1 calc R . . C5 C 0.6407(3) 0.1271(3) -0.3320(8) 0.0392(13) Uani 1 1 d . . . H5 H 0.6488 0.1674 -0.3371 0.047 Uiso 1 1 calc R . . C6 C 0.6579(3) 0.0949(3) -0.2041(7) 0.0370(14) Uani 1 1 d . . . C7 C 0.6458(3) 0.0332(3) -0.2010(7) 0.0399(15) Uani 1 1 d . . . H7 H 0.6572 0.0109 -0.1180 0.048 Uiso 1 1 calc R . . C8 C 0.6177(3) 0.0063(2) -0.3179(8) 0.0359(13) Uani 1 1 d . . . H8 H 0.6107 -0.0342 -0.3150 0.043 Uiso 1 1 calc R . . C9 C 0.6836(3) 0.1245(3) -0.0702(6) 0.0388(15) Uani 1 1 d . . . C10 C 1.0000 0.0000 1.0000 0.026(2) Uani 1 4 d S . . C11 C 0.9464(3) 0.0152(3) 0.9035(7) 0.0349(13) Uani 1 1 d . . . H11A H 0.9324 -0.0199 0.8515 0.042 Uiso 1 1 calc R . . H11B H 0.9146 0.0301 0.9661 0.042 Uiso 1 1 calc R . . C12 C 0.9234(3) 0.0780(3) 0.6942(7) 0.0342(13) Uani 1 1 d . . . C13 C 0.8623(3) 0.0702(3) 0.7142(7) 0.0413(15) Uani 1 1 d . . . H13 H 0.8478 0.0507 0.7987 0.050 Uiso 1 1 calc R . . C14 C 0.8235(3) 0.0922(3) 0.6044(8) 0.0420(15) Uani 1 1 d . . . H14 H 0.7828 0.0884 0.6177 0.050 Uiso 1 1 calc R . . C15 C 0.8450(3) 0.1191(3) 0.4778(8) 0.0347(14) Uani 1 1 d . . . C16 C 0.9072(3) 0.1256(3) 0.4545(8) 0.0430(16) Uani 1 1 d . . . H16 H 0.9219 0.1433 0.3678 0.052 Uiso 1 1 calc R . . C17 C 0.9450(3) 0.1046(3) 0.5657(7) 0.0427(15) Uani 1 1 d . . . H17 H 0.9857 0.1086 0.5532 0.051 Uiso 1 1 calc R . . C18 C 0.8028(3) 0.1428(3) 0.3625(7) 0.0352(14) Uani 1 1 d . . . C19 C 0.6078(3) 0.2676(3) 0.4526(8) 0.0515(19) Uani 1 1 d . . . H19D H 0.6424 0.2487 0.4924 0.077 Uiso 1 1 calc R . . H19E H 0.5751 0.2616 0.5199 0.077 Uiso 1 1 calc R . . H19F H 0.6151 0.3093 0.4419 0.077 Uiso 1 1 calc R . . C20 C 0.5929(3) 0.2412(3) 0.2993(8) 0.0479(18) Uani 1 1 d . . . C21 C 0.4875(3) 0.2805(3) 0.3291(10) 0.0568(18) Uani 1 1 d . . . H21A H 0.5046 0.2948 0.4209 0.085 Uiso 1 1 calc R . . H21B H 0.4545 0.2552 0.3518 0.085 Uiso 1 1 calc R . . H21C H 0.4742 0.3133 0.2696 0.085 Uiso 1 1 calc R . . C22 C 0.5183(4) 0.2217(3) 0.0902(9) 0.056(2) Uani 1 1 d . . . H22A H 0.5481 0.2338 0.0198 0.084 Uiso 1 1 calc R . . H22B H 0.4804 0.2363 0.0583 0.084 Uiso 1 1 calc R . . H22C H 0.5172 0.1792 0.0951 0.084 Uiso 1 1 calc R . . Cd1 Cd 0.718996(19) 0.183051(19) 0.17374(5) 0.03509(12) Uani 1 1 d . . . N1 N 0.5327(3) 0.2463(2) 0.2437(7) 0.0419(13) Uani 1 1 d . . . O1 O 0.5706(2) 0.00874(19) -0.5516(5) 0.0403(10) Uani 1 1 d . . . O2 O 0.7043(2) 0.1766(2) -0.0858(5) 0.0456(12) Uani 1 1 d . . . O3 O 0.6836(2) 0.0997(2) 0.0523(5) 0.0460(12) Uani 1 1 d . . . O4 O 0.96415(18) 0.0596(2) 0.7965(5) 0.0424(11) Uani 1 1 d . . . O5 O 0.7514(2) 0.1579(2) 0.4069(5) 0.0440(11) Uani 1 1 d . . . O6 O 0.8183(2) 0.1465(2) 0.2273(5) 0.0464(11) Uani 1 1 d . . . O7 O 0.6269(2) 0.2070(2) 0.2440(6) 0.0516(12) Uani 1 1 d . . . O1W O 0.7496(2) 0.27501(19) 0.1625(6) 0.0479(11) Uani 1 1 d . . . H1X H 0.7456 0.2931 0.2595 0.057 Uiso 1 1 d R . . H1Y H 0.7261 0.2964 0.0906 0.057 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 C1 0.027(3) 0.027(3) 0.027(6) 0.000 0.000 0.000 C2 0.042(3) 0.031(3) 0.032(3) 0.001(3) -0.008(3) 0.000(2) C3 0.040(3) 0.038(3) 0.017(3) -0.006(2) -0.005(2) 0.006(3) C4 0.047(4) 0.041(3) 0.025(3) 0.008(3) -0.002(3) -0.009(3) C5 0.049(3) 0.038(3) 0.031(3) 0.003(3) -0.004(3) -0.009(2) C6 0.037(3) 0.039(3) 0.035(4) -0.005(3) -0.007(3) -0.003(2) C7 0.052(4) 0.033(3) 0.035(4) 0.004(2) -0.013(3) -0.005(3) C8 0.048(3) 0.026(3) 0.034(3) 0.004(3) -0.027(3) 0.001(2) C9 0.044(3) 0.050(4) 0.022(3) -0.008(3) -0.005(3) -0.017(3) C10 0.033(4) 0.033(4) 0.012(5) 0.000 0.000 0.000 C11 0.029(3) 0.046(3) 0.030(3) 0.013(3) -0.007(2) 0.000(3) C12 0.033(3) 0.041(3) 0.030(3) 0.007(3) -0.007(2) 0.001(2) C13 0.039(3) 0.054(4) 0.031(4) 0.018(3) 0.006(3) -0.001(3) C14 0.038(3) 0.043(4) 0.045(4) 0.011(3) 0.003(3) 0.003(3) C15 0.032(3) 0.040(3) 0.033(3) 0.006(3) -0.005(2) -0.002(2) C16 0.037(3) 0.054(4) 0.038(4) 0.017(3) -0.006(3) 0.004(3) C17 0.035(3) 0.054(4) 0.040(4) 0.010(3) -0.005(3) -0.004(3) C18 0.039(3) 0.031(3) 0.036(4) 0.003(2) -0.009(3) 0.001(2) C19 0.047(4) 0.059(4) 0.049(4) 0.027(4) -0.018(3) -0.012(3) C20 0.055(4) 0.048(4) 0.041(5) 0.008(3) -0.009(3) 0.008(3) C21 0.067(5) 0.052(4) 0.052(4) 0.001(4) 0.022(4) 0.015(3) C22 0.061(5) 0.052(4) 0.055(5) -0.005(3) -0.027(4) -0.019(4) Cd1 0.0399(3) 0.0365(2) 0.02885(19) -0.00016(19) -0.0096(2) -0.0018(2) N1 0.050(3) 0.039(3) 0.037(3) 0.010(2) -0.003(2) 0.004(2) O1 0.057(3) 0.034(2) 0.030(2) -0.0040(18) -0.019(2) 0.005(2) O2 0.057(3) 0.043(3) 0.036(2) 0.005(2) -0.011(2) -0.028(2) O3 0.054(3) 0.048(3) 0.037(3) 0.007(2) -0.026(2) -0.014(2) O4 0.032(2) 0.054(3) 0.041(3) 0.018(2) -0.0105(18) -0.0034(18) O5 0.038(3) 0.054(3) 0.040(3) 0.000(2) -0.009(2) -0.004(2) O6 0.060(3) 0.048(3) 0.032(2) 0.003(2) -0.005(2) 0.011(2) O7 0.048(3) 0.056(3) 0.051(3) 0.006(2) 0.022(2) 0.014(2) O1W 0.055(3) 0.041(2) 0.048(3) 0.000(2) -0.006(3) -0.0004(19) _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 C1 C2 1.517(6) . ? C1 C2 1.517(6) 7_553 ? C1 C2 1.517(6) 2_655 ? C1 C2 1.517(6) 8_543 ? C2 O1 1.427(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O1 1.363(7) . ? C3 C8 1.386(8) . ? C3 C4 1.401(9) . ? C4 C5 1.383(9) . ? C4 H4 0.9300 . ? C5 C6 1.406(9) . ? C5 H5 0.9300 . ? C6 C7 1.419(8) . ? C6 C9 1.485(8) . ? C7 C8 1.361(8) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 O3 1.226(8) . ? C9 O2 1.274(8) . ? C9 Cd1 2.664(6) . ? C10 C11 1.523(5) 2_755 ? C10 C11 1.523(5) 3_667 ? C10 C11 1.523(5) . ? C10 C11 1.523(5) 4_647 ? C11 O4 1.440(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O4 1.360(7) . ? C12 C17 1.381(9) . ? C12 C13 1.403(9) . ? C13 C14 1.404(9) . ? C13 H13 0.9300 . ? C14 C15 1.369(10) . ? C14 H14 0.9300 . ? C15 C16 1.427(9) . ? C15 C18 1.498(8) . ? C16 C17 1.390(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 O6 1.255(8) . ? C18 O5 1.273(8) . ? C18 Cd1 2.689(6) . ? C19 C20 1.526(11) . ? C19 H19D 0.9600 . ? C19 H19E 0.9600 . ? C19 H19F 0.9600 . ? C20 O7 1.194(8) . ? C20 N1 1.452(9) . ? C21 N1 1.489(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N1 1.510(9) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? Cd1 O1W 2.191(4) . ? Cd1 O7 2.238(4) . ? Cd1 O5 2.272(5) . ? Cd1 O3 2.313(4) . ? Cd1 O2 2.337(4) . ? Cd1 O6 2.438(5) . ? O1W H1X 0.9600 . ? O1W H1Y 0.9600 . ? 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 C2 C1 C2 108.4(2) . 7_553 ? C2 C1 C2 111.7(5) . 2_655 ? C2 C1 C2 108.4(2) 7_553 2_655 ? C2 C1 C2 108.4(2) . 8_543 ? C2 C1 C2 111.7(5) 7_553 8_543 ? C2 C1 C2 108.4(2) 2_655 8_543 ? O1 C2 C1 108.4(4) . . ? O1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? O1 C3 C8 116.3(5) . . ? O1 C3 C4 123.1(5) . . ? C8 C3 C4 120.6(5) . . ? C5 C4 C3 119.1(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 120.9(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 118.1(5) . . ? C5 C6 C9 121.6(6) . . ? C7 C6 C9 120.1(6) . . ? C8 C7 C6 120.8(5) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C3 120.3(5) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? O3 C9 O2 121.2(5) . . ? O3 C9 C6 120.5(6) . . ? O2 C9 C6 118.2(5) . . ? O3 C9 Cd1 60.1(3) . . ? O2 C9 Cd1 61.3(3) . . ? C6 C9 Cd1 174.0(5) . . ? C11 C10 C11 108.5(2) 2_755 3_667 ? C11 C10 C11 111.4(5) 2_755 . ? C11 C10 C11 108.5(2) 3_667 . ? C11 C10 C11 108.5(2) 2_755 4_647 ? C11 C10 C11 111.4(5) 3_667 4_647 ? C11 C10 C11 108.5(2) . 4_647 ? O4 C11 C10 107.9(4) . . ? O4 C11 H11A 110.1 . . ? C10 C11 H11A 110.1 . . ? O4 C11 H11B 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? O4 C12 C17 116.6(5) . . ? O4 C12 C13 122.8(5) . . ? C17 C12 C13 120.5(6) . . ? C12 C13 C14 118.7(6) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 120.6(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.9(6) . . ? C14 C15 C18 119.7(6) . . ? C16 C15 C18 119.3(6) . . ? C17 C16 C15 117.8(6) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? C12 C17 C16 121.3(6) . . ? C12 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? O6 C18 O5 122.2(6) . . ? O6 C18 C15 120.2(6) . . ? O5 C18 C15 117.5(6) . . ? O6 C18 Cd1 64.9(3) . . ? O5 C18 Cd1 57.4(3) . . ? C15 C18 Cd1 174.7(5) . . ? C20 C19 H19D 109.5 . . ? C20 C19 H19E 109.5 . . ? H19D C19 H19E 109.5 . . ? C20 C19 H19F 109.5 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? O7 C20 N1 120.9(7) . . ? O7 C20 C19 118.7(7) . . ? N1 C20 C19 118.6(6) . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1W Cd1 O7 94.36(18) . . ? O1W Cd1 O5 100.22(19) . . ? O7 Cd1 O5 96.03(18) . . ? O1W Cd1 O3 149.22(18) . . ? O7 Cd1 O3 90.38(19) . . ? O5 Cd1 O3 109.51(16) . . ? O1W Cd1 O2 93.35(19) . . ? O7 Cd1 O2 99.2(2) . . ? O5 Cd1 O2 158.77(19) . . ? O3 Cd1 O2 55.87(15) . . ? O1W Cd1 O6 92.27(17) . . ? O7 Cd1 O6 151.96(18) . . ? O5 Cd1 O6 55.96(16) . . ? O3 Cd1 O6 97.69(17) . . ? O2 Cd1 O6 107.62(18) . . ? O1W Cd1 C9 121.9(2) . . ? O7 Cd1 C9 94.0(2) . . ? O5 Cd1 C9 135.74(19) . . ? O3 Cd1 C9 27.37(18) . . ? O2 Cd1 C9 28.56(18) . . ? O6 Cd1 C9 105.50(19) . . ? O1W Cd1 C18 97.32(18) . . ? O7 Cd1 C18 124.18(19) . . ? O5 Cd1 C18 28.17(18) . . ? O3 Cd1 C18 105.03(16) . . ? O2 Cd1 C18 134.1(2) . . ? O6 Cd1 C18 27.79(18) . . ? C9 Cd1 C18 123.5(2) . . ? C20 N1 C21 120.7(6) . . ? C20 N1 C22 118.7(6) . . ? C21 N1 C22 120.3(6) . . ? C3 O1 C2 117.2(5) . . ? C9 O2 Cd1 90.1(3) . . ? C9 O3 Cd1 92.5(4) . . ? C12 O4 C11 117.9(4) . . ? C18 O5 Cd1 94.5(4) . . ? C18 O6 Cd1 87.3(4) . . ? C20 O7 Cd1 150.3(5) . . ? Cd1 O1W H1X 109.5 . . ? Cd1 O1W H1Y 109.5 . . ? H1X O1W H1Y 109.5 . . ? 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 C2 C1 C2 O1 -65.5(3) 7_553 . . . ? C2 C1 C2 O1 53.8(4) 2_655 . . . ? C2 C1 C2 O1 173.2(5) 8_543 . . . ? O1 C3 C4 C5 179.0(6) . . . . ? C8 C3 C4 C5 -2.0(10) . . . . ? C3 C4 C5 C6 0.1(10) . . . . ? C4 C5 C6 C7 1.2(10) . . . . ? C4 C5 C6 C9 -174.1(6) . . . . ? C5 C6 C7 C8 -0.7(10) . . . . ? C9 C6 C7 C8 174.6(6) . . . . ? C6 C7 C8 C3 -1.1(10) . . . . ? O1 C3 C8 C7 -178.5(6) . . . . ? C4 C3 C8 C7 2.4(10) . . . . ? C5 C6 C9 O3 160.3(6) . . . . ? C7 C6 C9 O3 -14.9(10) . . . . ? C5 C6 C9 O2 -18.1(10) . . . . ? C7 C6 C9 O2 166.8(6) . . . . ? C5 C6 C9 Cd1 66(5) . . . . ? C7 C6 C9 Cd1 -109(4) . . . . ? C11 C10 C11 O4 -51.6(4) 2_755 . . . ? C11 C10 C11 O4 67.8(3) 3_667 . . . ? C11 C10 C11 O4 -171.0(5) 4_647 . . . ? O4 C12 C13 C14 178.2(6) . . . . ? C17 C12 C13 C14 -2.8(10) . . . . ? C12 C13 C14 C15 2.1(11) . . . . ? C13 C14 C15 C16 -0.1(11) . . . . ? C13 C14 C15 C18 -179.5(6) . . . . ? C14 C15 C16 C17 -1.2(11) . . . . ? C18 C15 C16 C17 178.3(6) . . . . ? O4 C12 C17 C16 -179.4(6) . . . . ? C13 C12 C17 C16 1.6(11) . . . . ? C15 C16 C17 C12 0.4(11) . . . . ? C14 C15 C18 O6 -152.8(7) . . . . ? C16 C15 C18 O6 27.8(9) . . . . ? C14 C15 C18 O5 26.5(9) . . . . ? C16 C15 C18 O5 -153.0(6) . . . . ? C14 C15 C18 Cd1 9(5) . . . . ? C16 C15 C18 Cd1 -171(4) . . . . ? O3 C9 Cd1 O1W 179.2(4) . . . . ? O2 C9 Cd1 O1W 4.2(5) . . . . ? C6 C9 Cd1 O1W -83(5) . . . . ? O3 C9 Cd1 O7 -83.1(4) . . . . ? O2 C9 Cd1 O7 101.9(4) . . . . ? C6 C9 Cd1 O7 15(5) . . . . ? O3 C9 Cd1 O5 19.7(6) . . . . ? O2 C9 Cd1 O5 -155.3(4) . . . . ? C6 C9 Cd1 O5 117(4) . . . . ? O2 C9 Cd1 O3 -175.0(7) . . . . ? C6 C9 Cd1 O3 98(5) . . . . ? O3 C9 Cd1 O2 175.0(7) . . . . ? C6 C9 Cd1 O2 -87(5) . . . . ? O3 C9 Cd1 O6 76.5(4) . . . . ? O2 C9 Cd1 O6 -98.5(4) . . . . ? C6 C9 Cd1 O6 174(4) . . . . ? O3 C9 Cd1 C18 53.0(5) . . . . ? O2 C9 Cd1 C18 -122.0(4) . . . . ? C6 C9 Cd1 C18 151(4) . . . . ? O6 C18 Cd1 O1W -80.9(4) . . . . ? O5 C18 Cd1 O1W 98.0(4) . . . . ? C15 C18 Cd1 O1W 117(5) . . . . ? O6 C18 Cd1 O7 178.7(4) . . . . ? O5 C18 Cd1 O7 -2.4(4) . . . . ? C15 C18 Cd1 O7 17(5) . . . . ? O6 C18 Cd1 O5 -178.9(6) . . . . ? C15 C18 Cd1 O5 19(4) . . . . ? O6 C18 Cd1 O3 77.8(4) . . . . ? O5 C18 Cd1 O3 -103.4(4) . . . . ? C15 C18 Cd1 O3 -84(5) . . . . ? O6 C18 Cd1 O2 21.0(5) . . . . ? O5 C18 Cd1 O2 -160.1(3) . . . . ? C15 C18 Cd1 O2 -141(5) . . . . ? O5 C18 Cd1 O6 178.9(6) . . . . ? C15 C18 Cd1 O6 -162(5) . . . . ? O6 C18 Cd1 C9 55.4(4) . . . . ? O5 C18 Cd1 C9 -125.7(4) . . . . ? C15 C18 Cd1 C9 -107(5) . . . . ? O7 C20 N1 C21 168.9(7) . . . . ? C19 C20 N1 C21 4.4(9) . . . . ? O7 C20 N1 C22 -17.2(9) . . . . ? C19 C20 N1 C22 178.4(6) . . . . ? C8 C3 O1 C2 160.8(6) . . . . ? C4 C3 O1 C2 -20.1(9) . . . . ? C1 C2 O1 C3 -170.9(5) . . . . ? O3 C9 O2 Cd1 -5.1(7) . . . . ? C6 C9 O2 Cd1 173.2(6) . . . . ? O1W Cd1 O2 C9 -176.4(4) . . . . ? O7 Cd1 O2 C9 -81.4(4) . . . . ? O5 Cd1 O2 C9 53.7(7) . . . . ? O3 Cd1 O2 C9 2.8(4) . . . . ? O6 Cd1 O2 C9 90.2(4) . . . . ? C18 Cd1 O2 C9 80.0(5) . . . . ? O2 C9 O3 Cd1 5.1(7) . . . . ? C6 C9 O3 Cd1 -173.1(6) . . . . ? O1W Cd1 O3 C9 -1.2(6) . . . . ? O7 Cd1 O3 C9 97.9(4) . . . . ? O5 Cd1 O3 C9 -165.5(4) . . . . ? O2 Cd1 O3 C9 -2.9(4) . . . . ? O6 Cd1 O3 C9 -109.0(4) . . . . ? C18 Cd1 O3 C9 -136.4(4) . . . . ? C17 C12 O4 C11 -159.4(6) . . . . ? C13 C12 O4 C11 19.6(9) . . . . ? C10 C11 O4 C12 177.4(5) . . . . ? O6 C18 O5 Cd1 1.2(7) . . . . ? C15 C18 O5 Cd1 -178.0(5) . . . . ? O1W Cd1 O5 C18 -86.4(4) . . . . ? O7 Cd1 O5 C18 178.0(4) . . . . ? O3 Cd1 O5 C18 85.5(4) . . . . ? O2 Cd1 O5 C18 42.5(6) . . . . ? O6 Cd1 O5 C18 -0.6(3) . . . . ? C9 Cd1 O5 C18 76.0(4) . . . . ? O5 C18 O6 Cd1 -1.1(6) . . . . ? C15 C18 O6 Cd1 178.1(5) . . . . ? O1W Cd1 O6 C18 101.4(4) . . . . ? O7 Cd1 O6 C18 -2.2(6) . . . . ? O5 Cd1 O6 C18 0.6(4) . . . . ? O3 Cd1 O6 C18 -107.8(4) . . . . ? O2 Cd1 O6 C18 -164.3(4) . . . . ? C9 Cd1 O6 C18 -134.6(4) . . . . ? N1 C20 O7 Cd1 145.1(7) . . . . ? C19 C20 O7 Cd1 -50.4(13) . . . . ? O1W Cd1 O7 C20 -22.4(10) . . . . ? O5 Cd1 O7 C20 78.4(10) . . . . ? O3 Cd1 O7 C20 -171.9(10) . . . . ? O2 Cd1 O7 C20 -116.5(10) . . . . ? O6 Cd1 O7 C20 80.8(11) . . . . ? C9 Cd1 O7 C20 -144.8(10) . . . . ? C18 Cd1 O7 C20 79.5(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.366 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.088