# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Trans.' _publ_contact_author ; Prof. Dr. Peter Roesky Freie Universitaet Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_requested_coeditor_name ? _publ_contact_author_phone +49/(0)3083854004 _publ_contact_author_fax +49/(0)3083852440 _publ_contact_author_email roesky@chemie.fu-berlin.de loop_ _publ_author_name 'Peter Roesky' 'Simmi Datta' 'Michael T. Gamer' _publ_section_title ; TADDOLate Complexes of Zinc ; data_1 _database_code_depnum_ccdc_archive 'CCDC 662788' _audit_creation_date 05-05-18 _audit_creation_method 'STOE X-RED' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H78 O10 Zn3, C7 H8' _chemical_formula_sum 'C79 H86 O10 Zn3' _chemical_formula_weight 1391.59 _chemical_absolute_configuration rmad 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' 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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.6229(8) _cell_length_b 22.6729(9) _cell_length_c 12.8913(8) _cell_angle_alpha 90.00 _cell_angle_beta 112.115(5) _cell_angle_gamma 90.00 _cell_volume 3418.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.254 _exptl_crystal_size_mid 0.193 _exptl_crystal_size_min 0.142 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7230 _exptl_absorpt_correction_T_max 0.7718 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24722 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 29.18 _reflns_number_total 17861 _reflns_number_gt 13860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0332P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(6) _refine_ls_number_reflns 17861 _refine_ls_number_parameters 836 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.001 _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 -0.2961(3) -0.13475(17) -0.2249(3) 0.0398(9) Uani 1 1 d . . . H1A H -0.2983 -0.1428 -0.1511 0.060 Uiso 1 1 calc R . . H1B H -0.3624 -0.1530 -0.2829 0.060 Uiso 1 1 calc R . . H1C H -0.2979 -0.0920 -0.2372 0.060 Uiso 1 1 calc R . . C2 C 0.4319(3) -0.30720(15) -0.1725(3) 0.0310(7) Uani 1 1 d . . . H2A H 0.4436 -0.3381 -0.1160 0.047 Uiso 1 1 calc R . . H2B H 0.4951 -0.2789 -0.1460 0.047 Uiso 1 1 calc R . . H2C H 0.4291 -0.3250 -0.2427 0.047 Uiso 1 1 calc R . . C3 C 0.0646(3) -0.10761(12) -0.0778(2) 0.0185(6) Uani 1 1 d . . . C4 C 0.1897(2) -0.12628(12) -0.0031(2) 0.0170(6) Uani 1 1 d . . . H4 H 0.2351 -0.1302 -0.0517 0.020 Uiso 1 1 calc R . . C5 C 0.1992(2) -0.18402(12) 0.0622(2) 0.0161(5) Uani 1 1 d . . . H5 H 0.1203 -0.1984 0.0489 0.019 Uiso 1 1 calc R . . C6 C 0.2658(2) -0.23451(14) 0.0309(2) 0.0177(5) Uani 1 1 d . . . C7 C 0.0651(3) -0.05338(12) -0.1499(2) 0.0174(5) Uani 1 1 d . . . C8 C -0.0404(3) -0.03070(13) -0.2215(2) 0.0223(6) Uani 1 1 d . . . H8 H -0.1091 -0.0469 -0.2196 0.027 Uiso 1 1 calc R . . C9 C -0.0463(3) 0.01496(14) -0.2952(2) 0.0267(7) Uani 1 1 d . . . H9 H -0.1187 0.0294 -0.3436 0.032 Uiso 1 1 calc R . . C10 C 0.0530(3) 0.03957(14) -0.2987(3) 0.0288(7) Uani 1 1 d . . . H10 H 0.0490 0.0705 -0.3499 0.035 Uiso 1 1 calc R . . C11 C 0.1575(3) 0.01861(13) -0.2271(3) 0.0270(7) Uani 1 1 d . . . H11 H 0.2258 0.0356 -0.2283 0.032 Uiso 1 1 calc R . . C12 C 0.1640(3) -0.02718(13) -0.1528(2) 0.0232(6) Uani 1 1 d . . . H12 H 0.2367 -0.0408 -0.1035 0.028 Uiso 1 1 calc R . . C13 C -0.0032(3) -0.09374(12) -0.0040(2) 0.0197(6) Uani 1 1 d . . . C14 C -0.0629(3) -0.13827(14) 0.0251(2) 0.0235(6) Uani 1 1 d . . . H14 H -0.0621 -0.1772 -0.0017 0.028 Uiso 1 1 calc R . . C15 C -0.1237(3) -0.12616(15) 0.0933(3) 0.0323(8) Uani 1 1 d . . . H15 H -0.1636 -0.1569 0.1131 0.039 Uiso 1 1 calc R . . C16 C -0.1262(3) -0.06952(17) 0.1322(3) 0.0399(9) Uani 1 1 d . . . H16 H -0.1676 -0.0613 0.1787 0.048 Uiso 1 1 calc R . . C17 C -0.0684(3) -0.02503(15) 0.1032(3) 0.0326(8) Uani 1 1 d . . . H17 H -0.0703 0.0140 0.1291 0.039 Uiso 1 1 calc R . . C18 C -0.0071(3) -0.03742(13) 0.0360(3) 0.0252(7) Uani 1 1 d . . . H18 H 0.0330 -0.0065 0.0169 0.030 Uiso 1 1 calc R . . C19 C 0.2432(3) -0.29389(13) 0.0759(2) 0.0214(6) Uani 1 1 d . . . C20 C 0.2718(3) -0.34576(13) 0.0343(2) 0.0248(6) Uani 1 1 d . . . H20 H 0.3055 -0.3436 -0.0202 0.030 Uiso 1 1 calc R . . C21 C 0.2517(3) -0.40027(15) 0.0712(3) 0.0334(8) Uani 1 1 d . . . H21 H 0.2693 -0.4352 0.0401 0.040 Uiso 1 1 calc R . . C22 C 0.2062(4) -0.40429(15) 0.1530(3) 0.0406(9) Uani 1 1 d . . . H22 H 0.1924 -0.4418 0.1785 0.049 Uiso 1 1 calc R . . C23 C 0.1811(4) -0.35347(16) 0.1971(3) 0.0417(9) Uani 1 1 d . . . H23 H 0.1511 -0.3561 0.2543 0.050 Uiso 1 1 calc R . . C24 C 0.1988(3) -0.29826(15) 0.1595(3) 0.0319(8) Uani 1 1 d . . . H24 H 0.1808 -0.2636 0.1908 0.038 Uiso 1 1 calc R . . C25 C 0.3947(3) -0.22237(12) 0.0746(2) 0.0194(6) Uani 1 1 d . . . C26 C 0.4681(3) -0.24656(13) 0.1750(2) 0.0260(7) Uani 1 1 d . . . H26 H 0.4378 -0.2712 0.2168 0.031 Uiso 1 1 calc R . . C27 C 0.5845(3) -0.23544(18) 0.2153(2) 0.0329(7) Uani 1 1 d . . . H27 H 0.6334 -0.2529 0.2835 0.040 Uiso 1 1 calc R . . C28 C 0.6299(3) -0.19879(16) 0.1561(3) 0.0326(7) Uani 1 1 d . . . H28 H 0.7095 -0.1904 0.1843 0.039 Uiso 1 1 calc R . . C29 C 0.5583(3) -0.17464(16) 0.0557(3) 0.0300(7) Uani 1 1 d . . . H29 H 0.5890 -0.1498 0.0146 0.036 Uiso 1 1 calc R . . C30 C 0.4421(3) -0.18642(13) 0.0147(2) 0.0227(6) Uani 1 1 d . . . H30 H 0.3939 -0.1699 -0.0549 0.027 Uiso 1 1 calc R . . C31 C 0.2824(3) -0.10670(13) 0.1897(2) 0.0250(6) Uani 1 1 d . . . C32 C 0.2232(3) -0.07799(15) 0.2597(3) 0.0329(8) Uani 1 1 d . . . H32A H 0.1419 -0.0884 0.2290 0.049 Uiso 1 1 calc R . . H32B H 0.2314 -0.0351 0.2580 0.049 Uiso 1 1 calc R . . H32C H 0.2581 -0.0920 0.3371 0.049 Uiso 1 1 calc R . . C33 C 0.4116(3) -0.09949(17) 0.2437(3) 0.0368(8) Uani 1 1 d . . . H33A H 0.4405 -0.1201 0.3158 0.055 Uiso 1 1 calc R . . H33B H 0.4307 -0.0575 0.2557 0.055 Uiso 1 1 calc R . . H33C H 0.4470 -0.1162 0.1944 0.055 Uiso 1 1 calc R . . C34 C 0.0715(3) -0.31388(12) -0.3815(2) 0.0191(6) Uani 1 1 d . . . C35 C -0.0536(2) -0.32871(12) -0.3934(2) 0.0174(6) Uani 1 1 d . . . H35 H -0.1033 -0.2937 -0.4258 0.021 Uiso 1 1 calc R . . C36 C -0.0724(3) -0.34867(12) -0.2868(2) 0.0192(6) Uani 1 1 d . . . H36 H 0.0036 -0.3513 -0.2235 0.023 Uiso 1 1 calc R . . C37 C -0.1504(3) -0.30609(12) -0.2527(2) 0.0171(6) Uani 1 1 d . . . C38 C 0.0677(3) -0.28379(12) -0.4909(2) 0.0214(6) Uani 1 1 d . . . C39 C 0.1698(3) -0.26211(15) -0.4936(2) 0.0285(7) Uani 1 1 d . . . H39 H 0.2392 -0.2682 -0.4313 0.034 Uiso 1 1 calc R . . C40 C 0.1712(3) -0.23150(17) -0.5869(3) 0.0365(8) Uani 1 1 d . . . H40 H 0.2413 -0.2167 -0.5876 0.044 Uiso 1 1 calc R . . C41 C 0.0703(4) -0.22265(15) -0.6787(3) 0.0378(9) Uani 1 1 d . . . H41 H 0.0705 -0.2006 -0.7413 0.045 Uiso 1 1 calc R . . C42 C -0.0298(3) -0.24612(15) -0.6781(3) 0.0356(8) Uani 1 1 d . . . H42 H -0.0985 -0.2414 -0.7419 0.043 Uiso 1 1 calc R . . C43 C -0.0318(3) -0.27684(14) -0.5849(2) 0.0271(7) Uani 1 1 d . . . H43 H -0.1016 -0.2930 -0.5859 0.033 Uiso 1 1 calc R . . C44 C 0.1465(3) -0.36886(13) -0.3564(2) 0.0214(6) Uani 1 1 d . . . C45 C 0.1910(3) -0.39209(13) -0.2476(3) 0.0256(6) Uani 1 1 d . . . H45 H 0.1712 -0.3740 -0.1908 0.031 Uiso 1 1 calc R . . C46 C 0.2632(3) -0.44078(15) -0.2204(3) 0.0336(8) Uani 1 1 d . . . H46 H 0.2908 -0.4560 -0.1463 0.040 Uiso 1 1 calc R . . C47 C 0.2946(3) -0.46683(15) -0.3005(3) 0.0427(9) Uani 1 1 d . . . H47 H 0.3459 -0.4993 -0.2816 0.051 Uiso 1 1 calc R . . C48 C 0.2505(3) -0.44540(16) -0.4097(3) 0.0427(9) Uani 1 1 d . . . H48 H 0.2711 -0.4638 -0.4657 0.051 Uiso 1 1 calc R . . C49 C 0.1770(3) -0.39750(14) -0.4373(3) 0.0310(7) Uani 1 1 d . . . H49 H 0.1467 -0.3838 -0.5125 0.037 Uiso 1 1 calc R . . C50 C -0.2737(3) -0.30634(13) -0.3382(2) 0.0207(6) Uani 1 1 d . . . C51 C -0.3525(3) -0.34755(15) -0.3302(3) 0.0295(7) Uani 1 1 d . . . H51 H -0.3294 -0.3755 -0.2709 0.035 Uiso 1 1 calc R . . C52 C -0.4641(3) -0.34814(18) -0.4080(3) 0.0394(9) Uani 1 1 d . . . H52 H -0.5167 -0.3765 -0.4016 0.047 Uiso 1 1 calc R . . C53 C -0.4995(3) -0.3076(2) -0.4953(3) 0.0438(10) Uani 1 1 d . . . H53 H -0.5760 -0.3080 -0.5484 0.053 Uiso 1 1 calc R . . C54 C -0.4222(3) -0.2665(2) -0.5041(3) 0.0390(8) Uani 1 1 d . . . H54 H -0.4459 -0.2384 -0.5630 0.047 Uiso 1 1 calc R . . C55 C -0.3096(3) -0.26624(16) -0.4269(2) 0.0283(6) Uani 1 1 d . . . H55 H -0.2568 -0.2384 -0.4348 0.034 Uiso 1 1 calc R . . C56 C -0.1505(2) -0.32191(12) -0.1364(2) 0.0189(6) Uani 1 1 d . . . C57 C -0.0926(3) -0.36916(13) -0.0723(2) 0.0260(7) Uani 1 1 d . . . H57 H -0.0504 -0.3949 -0.1006 0.031 Uiso 1 1 calc R . . C58 C -0.0952(3) -0.37969(15) 0.0331(3) 0.0329(8) Uani 1 1 d . . . H58 H -0.0538 -0.4120 0.0764 0.039 Uiso 1 1 calc R . . C59 C -0.1573(3) -0.34355(15) 0.0752(3) 0.0337(8) Uani 1 1 d . . . H59 H -0.1593 -0.3509 0.1471 0.040 Uiso 1 1 calc R . . C60 C -0.2171(3) -0.29628(15) 0.0112(3) 0.0328(8) Uani 1 1 d . . . H60 H -0.2603 -0.2711 0.0391 0.039 Uiso 1 1 calc R . . C61 C -0.2137(3) -0.28596(13) -0.0932(3) 0.0268(7) Uani 1 1 d . . . H61 H -0.2554 -0.2537 -0.1364 0.032 Uiso 1 1 calc R . . C62 C -0.1340(3) -0.42460(13) -0.4213(2) 0.0231(6) Uani 1 1 d . . . C63 C -0.2584(3) -0.43512(16) -0.4915(3) 0.0340(8) Uani 1 1 d . . . H63A H -0.3010 -0.3982 -0.4992 0.051 Uiso 1 1 calc R . . H63B H -0.2892 -0.4648 -0.4553 0.051 Uiso 1 1 calc R . . H63C H -0.2658 -0.4492 -0.5658 0.051 Uiso 1 1 calc R . . C64 C -0.0610(3) -0.47955(13) -0.4121(3) 0.0285(7) Uani 1 1 d . . . H64A H -0.0654 -0.4912 -0.4868 0.043 Uiso 1 1 calc R . . H64B H -0.0894 -0.5118 -0.3789 0.043 Uiso 1 1 calc R . . H64C H 0.0186 -0.4710 -0.3646 0.043 Uiso 1 1 calc R . . C65 C -0.0687(4) -0.13336(17) -0.4332(3) 0.0392(9) Uani 1 1 d . . . H65A H -0.0348 -0.1729 -0.4320 0.047 Uiso 1 1 calc R . . H65B H -0.0086 -0.1067 -0.3840 0.047 Uiso 1 1 calc R . . C66 C -0.1175(5) -0.1095(2) -0.5510(4) 0.0627(14) Uani 1 1 d . . . H66A H -0.1031 -0.0666 -0.5524 0.075 Uiso 1 1 calc R . . H66B H -0.0847 -0.1300 -0.5998 0.075 Uiso 1 1 calc R . . C67 C -0.2420(5) -0.1220(2) -0.5863(3) 0.0709(17) Uani 1 1 d . . . H67A H -0.2600 -0.1630 -0.6139 0.085 Uiso 1 1 calc R . . H67B H -0.2882 -0.0944 -0.6456 0.085 Uiso 1 1 calc R . . C68 C -0.2626(4) -0.11288(17) -0.4800(3) 0.0448(10) Uani 1 1 d . . . H68A H -0.2709 -0.0704 -0.4666 0.054 Uiso 1 1 calc R . . H68B H -0.3321 -0.1340 -0.4825 0.054 Uiso 1 1 calc R . . C69 C 0.2232(4) -0.13858(17) -0.3211(4) 0.0486(11) Uani 1 1 d . . . H69A H 0.1953 -0.1211 -0.2658 0.058 Uiso 1 1 calc R . . H69B H 0.1578 -0.1573 -0.3812 0.058 Uiso 1 1 calc R . . C70 C 0.2748(4) -0.0926(2) -0.3684(4) 0.0587(13) Uani 1 1 d . . . H70A H 0.2987 -0.0582 -0.3176 0.070 Uiso 1 1 calc R . . H70B H 0.2197 -0.0792 -0.4421 0.070 Uiso 1 1 calc R . . C71 C 0.3767(4) -0.12157(17) -0.3805(3) 0.0429(9) Uani 1 1 d . . . H71A H 0.4395 -0.0929 -0.3673 0.051 Uiso 1 1 calc R . . H71B H 0.3561 -0.1387 -0.4563 0.051 Uiso 1 1 calc R . . C72 C 0.4112(3) -0.16918(19) -0.2925(3) 0.0403(8) Uani 1 1 d . . . H72A H 0.4361 -0.2050 -0.3208 0.048 Uiso 1 1 calc R . . H72B H 0.4746 -0.1555 -0.2243 0.048 Uiso 1 1 calc R . . C73 C 0.3968(4) 0.0549(2) 0.0824(4) 0.0673(14) Uani 1 1 d . . . H73A H 0.3237 0.0346 0.0655 0.101 Uiso 1 1 calc R . . H73B H 0.3871 0.0971 0.0925 0.101 Uiso 1 1 calc R . . H73C H 0.4539 0.0386 0.1512 0.101 Uiso 1 1 calc R . . C74 C 0.4370(4) 0.0462(2) -0.0139(4) 0.0547(11) Uani 1 1 d . . . C75 C 0.4283(4) 0.0907(2) -0.0910(4) 0.0582(12) Uani 1 1 d . . . H75 H 0.4003 0.1282 -0.0808 0.070 Uiso 1 1 calc R . . C76 C 0.4591(5) 0.0819(3) -0.1821(5) 0.0741(15) Uani 1 1 d . . . H76 H 0.4522 0.1129 -0.2338 0.089 Uiso 1 1 calc R . . C77 C 0.5005(5) 0.0269(3) -0.1965(6) 0.087(2) Uani 1 1 d . . . H77 H 0.5202 0.0196 -0.2596 0.105 Uiso 1 1 calc R . . C78 C 0.5128(5) -0.0168(3) -0.1189(7) 0.089(2) Uani 1 1 d . . . H78 H 0.5439 -0.0538 -0.1269 0.107 Uiso 1 1 calc R . . C79 C 0.4801(5) -0.0071(2) -0.0291(6) 0.0767(17) Uani 1 1 d . . . H79 H 0.4877 -0.0380 0.0230 0.092 Uiso 1 1 calc R . . O1 O 0.01225(17) -0.15458(8) -0.15282(16) 0.0174(4) Uani 1 1 d . . . O2 O 0.24135(19) -0.08242(9) 0.07957(16) 0.0222(4) Uani 1 1 d . . . O3 O 0.25325(18) -0.16778(10) 0.17746(15) 0.0240(4) Uani 1 1 d . . . O4 O 0.22119(16) -0.23697(10) -0.08802(14) 0.0178(4) Uani 1 1 d . . . O5 O 0.11968(16) -0.27266(9) -0.29241(14) 0.0171(4) Uani 1 1 d . . . O6 O -0.0932(2) -0.37730(9) -0.46913(16) 0.0230(5) Uani 1 1 d . . . O7 O -0.1202(2) -0.40609(9) -0.31055(16) 0.0240(5) Uani 1 1 d . . . O8 O -0.10106(17) -0.24914(8) -0.24579(16) 0.0177(4) Uani 1 1 d . . . O9 O -0.1627(2) -0.13689(11) -0.39605(18) 0.0336(5) Uani 1 1 d . . . O10 O 0.31024(19) -0.18134(9) -0.26826(18) 0.0280(5) Uani 1 1 d . . . Zn1 Zn -0.15570(3) -0.167321(14) -0.23208(3) 0.02157(8) Uani 1 1 d . . . Zn2 Zn 0.06228(3) -0.232790(13) -0.18670(2) 0.01580(7) Uani 1 1 d . . . Zn3 Zn 0.28805(3) -0.266551(14) -0.19784(3) 0.01898(7) 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 0.0249(18) 0.042(2) 0.056(2) 0.0078(18) 0.0190(17) 0.0097(16) C2 0.0255(17) 0.0341(18) 0.0373(18) 0.0030(14) 0.0163(15) 0.0063(14) C3 0.0194(15) 0.0178(13) 0.0194(13) -0.0008(11) 0.0084(12) 0.0010(11) C4 0.0190(14) 0.0150(13) 0.0177(13) -0.0038(11) 0.0077(11) -0.0031(11) C5 0.0172(14) 0.0207(14) 0.0116(12) 0.0000(10) 0.0066(11) 0.0015(11) C6 0.0186(13) 0.0190(12) 0.0146(11) 0.0006(12) 0.0054(10) 0.0013(13) C7 0.0245(15) 0.0126(12) 0.0174(12) -0.0039(10) 0.0106(12) -0.0018(11) C8 0.0268(17) 0.0176(14) 0.0231(15) -0.0002(12) 0.0101(13) -0.0006(12) C9 0.0337(19) 0.0227(15) 0.0225(15) 0.0009(12) 0.0092(14) 0.0076(13) C10 0.046(2) 0.0212(15) 0.0235(15) 0.0021(12) 0.0181(15) -0.0001(14) C11 0.0334(18) 0.0238(15) 0.0289(15) 0.0031(13) 0.0175(14) -0.0052(13) C12 0.0296(17) 0.0200(14) 0.0215(14) 0.0000(12) 0.0113(13) -0.0017(12) C13 0.0225(15) 0.0186(14) 0.0215(14) 0.0018(11) 0.0125(12) 0.0030(11) C14 0.0246(16) 0.0210(14) 0.0269(15) 0.0031(12) 0.0119(13) 0.0017(12) C15 0.038(2) 0.0323(18) 0.0372(18) 0.0086(15) 0.0258(16) 0.0064(15) C16 0.045(2) 0.050(2) 0.0381(19) 0.0073(17) 0.0306(18) 0.0147(18) C17 0.049(2) 0.0274(17) 0.0311(17) 0.0003(14) 0.0259(17) 0.0109(15) C18 0.0350(19) 0.0170(14) 0.0277(15) -0.0014(12) 0.0164(14) 0.0043(13) C19 0.0197(15) 0.0222(14) 0.0200(14) 0.0028(12) 0.0048(12) -0.0011(12) C20 0.0251(17) 0.0234(15) 0.0242(15) 0.0015(12) 0.0074(13) 0.0031(13) C21 0.035(2) 0.0221(16) 0.042(2) 0.0010(14) 0.0122(16) 0.0020(14) C22 0.048(2) 0.0239(17) 0.053(2) 0.0137(16) 0.0230(19) -0.0015(16) C23 0.056(3) 0.0352(19) 0.048(2) 0.0111(17) 0.036(2) 0.0002(18) C24 0.038(2) 0.0278(17) 0.0355(17) 0.0068(14) 0.0204(16) 0.0030(15) C25 0.0205(14) 0.0222(16) 0.0156(12) -0.0045(11) 0.0071(11) -0.0004(11) C26 0.0232(15) 0.0323(17) 0.0211(14) 0.0037(11) 0.0066(12) -0.0007(12) C27 0.0230(15) 0.0464(19) 0.0225(14) 0.0048(16) 0.0006(12) 0.0052(17) C28 0.0196(16) 0.048(2) 0.0300(16) -0.0065(15) 0.0096(14) -0.0024(14) C29 0.0248(16) 0.0369(19) 0.0295(16) -0.0024(14) 0.0116(13) -0.0069(15) C30 0.0213(15) 0.0280(16) 0.0186(13) -0.0011(12) 0.0072(12) -0.0006(12) C31 0.0294(17) 0.0234(15) 0.0197(14) -0.0058(12) 0.0065(13) -0.0055(13) C32 0.045(2) 0.0309(17) 0.0243(15) -0.0068(13) 0.0145(15) 0.0022(15) C33 0.031(2) 0.041(2) 0.0315(18) -0.0080(15) 0.0047(15) -0.0048(16) C34 0.0227(15) 0.0196(14) 0.0155(13) 0.0003(11) 0.0076(11) -0.0011(12) C35 0.0173(14) 0.0176(13) 0.0165(13) -0.0029(11) 0.0055(11) -0.0032(11) C36 0.0202(15) 0.0185(13) 0.0200(13) 0.0000(11) 0.0090(12) -0.0034(11) C37 0.0202(14) 0.0151(13) 0.0175(13) -0.0012(10) 0.0088(11) -0.0034(11) C38 0.0311(17) 0.0173(14) 0.0195(13) -0.0016(11) 0.0139(13) 0.0008(12) C39 0.0312(17) 0.0366(17) 0.0205(13) -0.0043(14) 0.0130(12) -0.0070(15) C40 0.053(2) 0.0361(17) 0.0337(16) -0.0066(17) 0.0311(16) -0.0145(19) C41 0.062(2) 0.033(2) 0.0313(16) 0.0048(15) 0.0326(17) 0.0047(17) C42 0.045(2) 0.041(2) 0.0243(15) 0.0113(13) 0.0162(15) 0.0136(15) C43 0.0300(17) 0.0297(17) 0.0219(14) 0.0035(13) 0.0103(13) 0.0013(14) C44 0.0166(15) 0.0225(15) 0.0235(15) -0.0054(12) 0.0058(12) -0.0013(12) C45 0.0259(17) 0.0228(15) 0.0265(15) 0.0030(12) 0.0081(13) -0.0008(13) C46 0.032(2) 0.0246(16) 0.0376(19) 0.0075(14) 0.0057(15) 0.0032(14) C47 0.038(2) 0.0271(18) 0.055(2) -0.0064(17) 0.0091(18) 0.0105(16) C48 0.040(2) 0.036(2) 0.050(2) -0.0143(17) 0.0139(18) 0.0121(17) C49 0.035(2) 0.0274(16) 0.0300(17) -0.0073(14) 0.0118(15) 0.0012(14) C50 0.0180(14) 0.0244(14) 0.0208(13) -0.0053(12) 0.0086(12) -0.0039(12) C51 0.0267(17) 0.0359(18) 0.0295(16) -0.0045(14) 0.0148(14) -0.0108(14) C52 0.0265(19) 0.054(2) 0.0408(19) -0.0126(18) 0.0158(16) -0.0164(17) C53 0.0208(18) 0.072(3) 0.0345(19) -0.0072(19) 0.0055(15) -0.0024(18) C54 0.0313(19) 0.053(2) 0.0299(16) 0.0038(18) 0.0081(14) 0.0062(19) C55 0.0266(16) 0.0352(16) 0.0217(13) -0.0021(15) 0.0074(12) -0.0036(16) C56 0.0201(15) 0.0204(14) 0.0144(12) -0.0022(11) 0.0047(11) -0.0055(11) C57 0.0348(18) 0.0240(15) 0.0235(15) 0.0023(12) 0.0159(14) 0.0035(13) C58 0.044(2) 0.0287(17) 0.0274(16) 0.0059(13) 0.0156(16) 0.0031(15) C59 0.053(2) 0.0302(17) 0.0244(16) 0.0004(14) 0.0225(16) -0.0031(16) C60 0.048(2) 0.0281(17) 0.0334(17) -0.0027(14) 0.0283(17) -0.0007(15) C61 0.0353(18) 0.0247(15) 0.0270(15) 0.0008(12) 0.0192(14) 0.0019(13) C62 0.0285(17) 0.0223(14) 0.0224(14) -0.0048(12) 0.0142(13) -0.0080(12) C63 0.0322(19) 0.0364(19) 0.0355(18) -0.0110(15) 0.0150(16) -0.0094(15) C64 0.039(2) 0.0216(15) 0.0277(16) -0.0020(12) 0.0164(15) -0.0019(14) C65 0.045(2) 0.039(2) 0.038(2) 0.0032(17) 0.0203(18) 0.0085(18) C66 0.100(4) 0.054(3) 0.043(2) 0.007(2) 0.037(3) -0.001(3) C67 0.101(5) 0.053(3) 0.030(2) 0.011(2) -0.007(2) -0.016(3) C68 0.036(2) 0.036(2) 0.045(2) 0.0167(17) -0.0049(18) -0.0018(17) C69 0.054(3) 0.036(2) 0.071(3) 0.016(2) 0.040(2) 0.0182(19) C70 0.050(3) 0.045(2) 0.082(3) 0.035(2) 0.026(3) 0.009(2) C71 0.050(3) 0.041(2) 0.044(2) 0.0104(17) 0.026(2) -0.0079(19) C72 0.0287(18) 0.045(2) 0.053(2) 0.0137(19) 0.0219(16) -0.0062(18) C73 0.044(3) 0.059(3) 0.082(3) -0.005(3) 0.004(2) -0.009(2) C74 0.031(2) 0.046(2) 0.072(3) -0.016(2) 0.003(2) -0.0068(18) C75 0.039(2) 0.054(3) 0.079(3) -0.020(2) 0.018(2) -0.011(2) C76 0.051(3) 0.079(4) 0.088(4) -0.026(3) 0.021(3) -0.031(3) C77 0.060(4) 0.098(5) 0.109(5) -0.060(4) 0.037(3) -0.034(3) C78 0.064(4) 0.062(4) 0.135(6) -0.044(4) 0.029(4) -0.011(3) C79 0.051(3) 0.045(3) 0.113(5) -0.026(3) 0.007(3) -0.005(2) O1 0.0164(10) 0.0147(10) 0.0209(10) -0.0017(7) 0.0067(8) -0.0010(7) O2 0.0271(12) 0.0204(10) 0.0168(10) -0.0034(8) 0.0056(9) -0.0041(9) O3 0.0369(12) 0.0220(10) 0.0123(8) -0.0026(8) 0.0084(8) -0.0017(10) O4 0.0179(9) 0.0225(9) 0.0130(8) 0.0002(8) 0.0057(7) 0.0039(9) O5 0.0179(10) 0.0196(10) 0.0153(8) -0.0040(8) 0.0079(7) -0.0005(8) O6 0.0337(13) 0.0201(10) 0.0167(10) -0.0059(8) 0.0114(9) -0.0112(9) O7 0.0386(13) 0.0172(10) 0.0216(10) -0.0039(8) 0.0174(10) -0.0081(9) O8 0.0174(10) 0.0145(10) 0.0216(9) 0.0007(7) 0.0078(8) -0.0021(7) O9 0.0276(13) 0.0408(14) 0.0275(12) 0.0110(10) 0.0047(10) 0.0028(11) O10 0.0237(12) 0.0294(12) 0.0322(11) 0.0078(9) 0.0121(9) -0.0015(9) Zn1 0.01672(17) 0.02075(16) 0.02669(17) -0.00114(15) 0.00756(14) 0.00162(15) Zn2 0.01581(15) 0.01595(14) 0.01593(14) -0.00196(13) 0.00630(12) 0.00023(14) Zn3 0.01812(17) 0.02135(16) 0.01929(15) 0.00015(14) 0.00912(13) 0.00172(14) _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 Zn1 1.954(3) . ? C2 Zn3 1.951(3) . ? C3 O1 1.423(3) . ? C3 C13 1.534(4) . ? C3 C7 1.542(4) . ? C3 C4 1.566(4) . ? C4 O2 1.424(3) . ? C4 C5 1.536(4) . ? C5 O3 1.430(3) . ? C5 C6 1.561(4) . ? C6 O4 1.421(3) . ? C6 C25 1.533(4) . ? C6 C19 1.535(4) . ? C7 C12 1.395(4) . ? C7 C8 1.402(4) . ? C8 C9 1.388(4) . ? C9 C10 1.388(5) . ? C10 C11 1.379(5) . ? C11 C12 1.393(4) . ? C13 C18 1.385(4) . ? C13 C14 1.393(4) . ? C14 C15 1.395(4) . ? C15 C16 1.383(5) . ? C16 C17 1.377(5) . ? C17 C18 1.390(4) . ? C19 C24 1.391(4) . ? C19 C20 1.396(4) . ? C20 C21 1.382(4) . ? C21 C22 1.381(5) . ? C22 C23 1.373(5) . ? C23 C24 1.391(5) . ? C25 C26 1.390(4) . ? C25 C30 1.402(4) . ? C26 C27 1.386(4) . ? C27 C28 1.390(5) . ? C28 C29 1.382(5) . ? C29 C30 1.386(4) . ? C31 O3 1.426(4) . ? C31 O2 1.426(4) . ? C31 C32 1.517(4) . ? C31 C33 1.523(5) . ? C34 O5 1.427(3) . ? C34 C44 1.525(4) . ? C34 C38 1.551(4) . ? C34 C35 1.564(4) . ? C35 O6 1.432(3) . ? C35 C36 1.547(4) . ? C36 O7 1.419(3) . ? C36 C37 1.557(4) . ? C37 O8 1.422(3) . ? C37 C50 1.531(4) . ? C37 C56 1.541(4) . ? C38 C43 1.388(4) . ? C38 C39 1.392(4) . ? C39 C40 1.394(4) . ? C40 C41 1.389(5) . ? C41 C42 1.374(5) . ? C42 C43 1.398(4) . ? C44 C49 1.399(4) . ? C44 C45 1.403(4) . ? C45 C46 1.390(5) . ? C46 C47 1.370(5) . ? C47 C48 1.392(6) . ? C48 C49 1.385(5) . ? C50 C55 1.396(4) . ? C50 C51 1.396(4) . ? C51 C52 1.389(5) . ? C52 C53 1.390(6) . ? C53 C54 1.384(6) . ? C54 C55 1.394(5) . ? C56 C57 1.382(4) . ? C56 C61 1.395(4) . ? C57 C58 1.391(4) . ? C58 C59 1.380(5) . ? C59 C60 1.389(5) . ? C60 C61 1.382(4) . ? C62 O6 1.426(3) . ? C62 O7 1.435(3) . ? C62 C63 1.507(5) . ? C62 C64 1.527(4) . ? C65 O9 1.439(4) . ? C65 C66 1.509(5) . ? C66 C67 1.489(8) . ? C67 C68 1.503(7) . ? C68 O9 1.425(4) . ? C69 O10 1.431(4) . ? C69 C70 1.477(5) . ? C70 C71 1.504(6) . ? C71 C72 1.507(5) . ? C72 O10 1.448(4) . ? C73 C74 1.520(7) . ? C74 C79 1.369(7) . ? C74 C75 1.390(7) . ? C75 C76 1.383(7) . ? C76 C77 1.391(8) . ? C77 C78 1.375(9) . ? C78 C79 1.385(9) . ? O1 Zn2 1.9853(18) . ? O1 Zn1 1.998(2) . ? O4 Zn2 1.9312(19) . ? O4 Zn3 2.0165(18) . ? O5 Zn2 1.9855(17) . ? O5 Zn3 2.0179(19) . ? O8 Zn2 1.946(2) . ? O8 Zn1 2.0100(18) . ? O9 Zn1 2.194(2) . ? O10 Zn3 2.197(2) . ? Zn1 Zn2 2.9840(5) . ? Zn2 Zn3 3.0061(5) . ? 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 O1 C3 C13 110.5(2) . . ? O1 C3 C7 107.1(2) . . ? C13 C3 C7 109.9(2) . . ? O1 C3 C4 108.6(2) . . ? C13 C3 C4 110.0(2) . . ? C7 C3 C4 110.8(2) . . ? O2 C4 C5 105.4(2) . . ? O2 C4 C3 110.1(2) . . ? C5 C4 C3 114.9(2) . . ? O3 C5 C4 105.0(2) . . ? O3 C5 C6 111.4(2) . . ? C4 C5 C6 115.0(2) . . ? O4 C6 C25 109.8(2) . . ? O4 C6 C19 108.6(2) . . ? C25 C6 C19 110.0(2) . . ? O4 C6 C5 105.9(2) . . ? C25 C6 C5 111.9(2) . . ? C19 C6 C5 110.5(2) . . ? C12 C7 C8 117.6(3) . . ? C12 C7 C3 124.2(3) . . ? C8 C7 C3 118.1(3) . . ? C9 C8 C7 121.1(3) . . ? C10 C9 C8 120.4(3) . . ? C11 C10 C9 119.2(3) . . ? C10 C11 C12 120.7(3) . . ? C11 C12 C7 120.9(3) . . ? C18 C13 C14 118.0(3) . . ? C18 C13 C3 121.8(3) . . ? C14 C13 C3 120.2(3) . . ? C13 C14 C15 120.6(3) . . ? C16 C15 C14 120.2(3) . . ? C17 C16 C15 119.7(3) . . ? C16 C17 C18 119.8(3) . . ? C13 C18 C17 121.6(3) . . ? C24 C19 C20 118.4(3) . . ? C24 C19 C6 122.8(3) . . ? C20 C19 C6 118.8(3) . . ? C21 C20 C19 120.9(3) . . ? C22 C21 C20 120.4(3) . . ? C23 C22 C21 119.2(3) . . ? C22 C23 C24 121.2(3) . . ? C23 C24 C19 119.9(3) . . ? C26 C25 C30 118.0(3) . . ? C26 C25 C6 120.9(2) . . ? C30 C25 C6 121.0(2) . . ? C27 C26 C25 121.2(3) . . ? C26 C27 C28 120.1(3) . . ? C29 C28 C27 119.5(3) . . ? C28 C29 C30 120.4(3) . . ? C29 C30 C25 120.8(3) . . ? O3 C31 O2 106.4(2) . . ? O3 C31 C32 108.6(3) . . ? O2 C31 C32 110.5(3) . . ? O3 C31 C33 110.0(3) . . ? O2 C31 C33 109.8(3) . . ? C32 C31 C33 111.4(3) . . ? O5 C34 C44 108.8(2) . . ? O5 C34 C38 107.5(2) . . ? C44 C34 C38 110.9(2) . . ? O5 C34 C35 109.2(2) . . ? C44 C34 C35 111.6(2) . . ? C38 C34 C35 108.7(2) . . ? O6 C35 C36 104.4(2) . . ? O6 C35 C34 108.3(2) . . ? C36 C35 C34 117.5(2) . . ? O7 C36 C35 105.8(2) . . ? O7 C36 C37 111.5(2) . . ? C35 C36 C37 113.2(2) . . ? O8 C37 C50 110.5(2) . . ? O8 C37 C56 108.1(2) . . ? C50 C37 C56 109.1(2) . . ? O8 C37 C36 105.8(2) . . ? C50 C37 C36 111.9(2) . . ? C56 C37 C36 111.3(2) . . ? C43 C38 C39 118.7(3) . . ? C43 C38 C34 123.5(3) . . ? C39 C38 C34 117.8(3) . . ? C38 C39 C40 120.7(3) . . ? C41 C40 C39 120.1(3) . . ? C42 C41 C40 119.3(3) . . ? C41 C42 C43 120.8(3) . . ? C38 C43 C42 120.3(3) . . ? C49 C44 C45 116.9(3) . . ? C49 C44 C34 123.0(3) . . ? C45 C44 C34 120.1(3) . . ? C46 C45 C44 121.8(3) . . ? C47 C46 C45 120.1(3) . . ? C46 C47 C48 119.5(3) . . ? C49 C48 C47 120.5(3) . . ? C48 C49 C44 121.2(3) . . ? C55 C50 C51 118.4(3) . . ? C55 C50 C37 121.1(3) . . ? C51 C50 C37 120.5(3) . . ? C52 C51 C50 120.7(3) . . ? C51 C52 C53 120.5(3) . . ? C54 C53 C52 119.3(3) . . ? C53 C54 C55 120.4(4) . . ? C54 C55 C50 120.7(3) . . ? C57 C56 C61 117.8(3) . . ? C57 C56 C37 124.6(3) . . ? C61 C56 C37 117.5(2) . . ? C56 C57 C58 121.0(3) . . ? C59 C58 C57 120.5(3) . . ? C58 C59 C60 119.1(3) . . ? C61 C60 C59 120.0(3) . . ? C60 C61 C56 121.5(3) . . ? O6 C62 O7 106.4(2) . . ? O6 C62 C63 108.9(3) . . ? O7 C62 C63 110.7(2) . . ? O6 C62 C64 110.0(2) . . ? O7 C62 C64 108.5(2) . . ? C63 C62 C64 112.3(3) . . ? O9 C65 C66 106.2(3) . . ? C67 C66 C65 102.9(4) . . ? C66 C67 C68 102.7(3) . . ? O9 C68 C67 103.4(4) . . ? O10 C69 C70 107.2(3) . . ? C69 C70 C71 105.2(3) . . ? C70 C71 C72 104.5(3) . . ? O10 C72 C71 105.7(3) . . ? C79 C74 C75 117.8(5) . . ? C79 C74 C73 120.3(5) . . ? C75 C74 C73 121.9(4) . . ? C76 C75 C74 122.1(5) . . ? C75 C76 C77 118.8(6) . . ? C78 C77 C76 119.6(6) . . ? C77 C78 C79 120.4(6) . . ? C74 C79 C78 121.2(6) . . ? C3 O1 Zn2 135.47(17) . . ? C3 O1 Zn1 126.02(17) . . ? Zn2 O1 Zn1 97.04(8) . . ? C4 O2 C31 111.6(2) . . ? C31 O3 C5 111.6(2) . . ? C6 O4 Zn2 126.89(15) . . ? C6 O4 Zn3 132.03(16) . . ? Zn2 O4 Zn3 99.17(8) . . ? C34 O5 Zn2 134.06(17) . . ? C34 O5 Zn3 124.33(17) . . ? Zn2 O5 Zn3 97.33(8) . . ? C62 O6 C35 112.0(2) . . ? C36 O7 C62 111.4(2) . . ? C37 O8 Zn2 124.92(17) . . ? C37 O8 Zn1 133.37(17) . . ? Zn2 O8 Zn1 97.92(8) . . ? C68 O9 C65 109.3(3) . . ? C68 O9 Zn1 123.7(2) . . ? C65 O9 Zn1 126.8(2) . . ? C69 O10 C72 110.4(3) . . ? C69 O10 Zn3 126.7(2) . . ? C72 O10 Zn3 121.1(2) . . ? C1 Zn1 O1 136.71(14) . . ? C1 Zn1 O8 134.46(13) . . ? O1 Zn1 O8 81.10(8) . . ? C1 Zn1 O9 102.63(13) . . ? O1 Zn1 O9 95.58(8) . . ? O8 Zn1 O9 95.52(8) . . ? C1 Zn1 Zn2 164.69(12) . . ? O1 Zn1 Zn2 41.32(5) . . ? O8 Zn1 Zn2 40.23(6) . . ? O9 Zn1 Zn2 92.57(6) . . ? O4 Zn2 O8 158.95(8) . . ? O4 Zn2 O1 103.68(8) . . ? O8 Zn2 O1 83.01(8) . . ? O4 Zn2 O5 82.70(8) . . ? O8 Zn2 O5 104.55(8) . . ? O1 Zn2 O5 141.82(8) . . ? O4 Zn2 Zn1 143.70(6) . . ? O8 Zn2 Zn1 41.85(5) . . ? O1 Zn2 Zn1 41.64(6) . . ? O5 Zn2 Zn1 129.77(6) . . ? O4 Zn2 Zn3 41.47(5) . . ? O8 Zn2 Zn3 144.75(6) . . ? O1 Zn2 Zn3 128.59(6) . . ? O5 Zn2 Zn3 41.74(5) . . ? Zn1 Zn2 Zn3 159.731(14) . . ? C2 Zn3 O4 130.43(11) . . ? C2 Zn3 O5 140.44(12) . . ? O4 Zn3 O5 79.80(7) . . ? C2 Zn3 O10 103.26(12) . . ? O4 Zn3 O10 98.62(8) . . ? O5 Zn3 O10 94.58(8) . . ? C2 Zn3 Zn2 162.08(10) . . ? O4 Zn3 Zn2 39.36(5) . . ? O5 Zn3 Zn2 40.93(5) . . ? O10 Zn3 Zn2 93.81(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 O1 C3 C4 O2 -174.9(2) . . . . ? C13 C3 C4 O2 -53.9(3) . . . . ? C7 C3 C4 O2 67.8(3) . . . . ? O1 C3 C4 C5 -56.1(3) . . . . ? C13 C3 C4 C5 64.9(3) . . . . ? C7 C3 C4 C5 -173.5(2) . . . . ? O2 C4 C5 O3 1.5(3) . . . . ? C3 C4 C5 O3 -119.9(2) . . . . ? O2 C4 C5 C6 -121.3(2) . . . . ? C3 C4 C5 C6 117.3(3) . . . . ? O3 C5 C6 O4 -166.6(2) . . . . ? C4 C5 C6 O4 -47.3(3) . . . . ? O3 C5 C6 C25 -47.0(3) . . . . ? C4 C5 C6 C25 72.3(3) . . . . ? O3 C5 C6 C19 76.0(3) . . . . ? C4 C5 C6 C19 -164.8(2) . . . . ? O1 C3 C7 C12 -114.4(3) . . . . ? C13 C3 C7 C12 125.6(3) . . . . ? C4 C3 C7 C12 3.8(4) . . . . ? O1 C3 C7 C8 62.1(3) . . . . ? C13 C3 C7 C8 -57.9(3) . . . . ? C4 C3 C7 C8 -179.7(2) . . . . ? C12 C7 C8 C9 2.0(4) . . . . ? C3 C7 C8 C9 -174.7(3) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? C8 C9 C10 C11 -0.8(4) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C10 C11 C12 C7 0.7(5) . . . . ? C8 C7 C12 C11 -2.0(4) . . . . ? C3 C7 C12 C11 174.5(3) . . . . ? O1 C3 C13 C18 -149.5(3) . . . . ? C7 C3 C13 C18 -31.5(4) . . . . ? C4 C3 C13 C18 90.7(3) . . . . ? O1 C3 C13 C14 30.7(4) . . . . ? C7 C3 C13 C14 148.7(3) . . . . ? C4 C3 C13 C14 -89.1(3) . . . . ? C18 C13 C14 C15 -0.5(5) . . . . ? C3 C13 C14 C15 179.3(3) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? C14 C15 C16 C17 0.1(6) . . . . ? C15 C16 C17 C18 -0.6(6) . . . . ? C14 C13 C18 C17 0.0(5) . . . . ? C3 C13 C18 C17 -179.8(3) . . . . ? C16 C17 C18 C13 0.5(5) . . . . ? O4 C6 C19 C24 -133.4(3) . . . . ? C25 C6 C19 C24 106.4(3) . . . . ? C5 C6 C19 C24 -17.6(4) . . . . ? O4 C6 C19 C20 48.9(3) . . . . ? C25 C6 C19 C20 -71.3(3) . . . . ? C5 C6 C19 C20 164.6(3) . . . . ? C24 C19 C20 C21 3.0(5) . . . . ? C6 C19 C20 C21 -179.2(3) . . . . ? C19 C20 C21 C22 -2.1(5) . . . . ? C20 C21 C22 C23 0.0(6) . . . . ? C21 C22 C23 C24 1.1(6) . . . . ? C22 C23 C24 C19 -0.2(6) . . . . ? C20 C19 C24 C23 -1.8(5) . . . . ? C6 C19 C24 C23 -179.5(3) . . . . ? O4 C6 C25 C26 -146.1(3) . . . . ? C19 C6 C25 C26 -26.7(3) . . . . ? C5 C6 C25 C26 96.6(3) . . . . ? O4 C6 C25 C30 34.1(4) . . . . ? C19 C6 C25 C30 153.5(2) . . . . ? C5 C6 C25 C30 -83.2(3) . . . . ? C30 C25 C26 C27 0.2(4) . . . . ? C6 C25 C26 C27 -179.6(3) . . . . ? C25 C26 C27 C28 1.0(5) . . . . ? C26 C27 C28 C29 -1.4(5) . . . . ? C27 C28 C29 C30 0.5(5) . . . . ? C28 C29 C30 C25 0.7(5) . . . . ? C26 C25 C30 C29 -1.1(4) . . . . ? C6 C25 C30 C29 178.7(3) . . . . ? O5 C34 C35 O6 -170.1(2) . . . . ? C44 C34 C35 O6 -49.8(3) . . . . ? C38 C34 C35 O6 72.8(3) . . . . ? O5 C34 C35 C36 -52.2(3) . . . . ? C44 C34 C35 C36 68.2(3) . . . . ? C38 C34 C35 C36 -169.2(2) . . . . ? O6 C35 C36 O7 0.1(3) . . . . ? C34 C35 C36 O7 -119.8(3) . . . . ? O6 C35 C36 C37 -122.3(2) . . . . ? C34 C35 C36 C37 117.8(3) . . . . ? O7 C36 C37 O8 -172.5(2) . . . . ? C35 C36 C37 O8 -53.4(3) . . . . ? O7 C36 C37 C50 -52.1(3) . . . . ? C35 C36 C37 C50 67.1(3) . . . . ? O7 C36 C37 C56 70.3(3) . . . . ? C35 C36 C37 C56 -170.6(2) . . . . ? O5 C34 C38 C43 -123.0(3) . . . . ? C44 C34 C38 C43 118.1(3) . . . . ? C35 C34 C38 C43 -5.0(4) . . . . ? O5 C34 C38 C39 56.2(3) . . . . ? C44 C34 C38 C39 -62.7(3) . . . . ? C35 C34 C38 C39 174.3(3) . . . . ? C43 C38 C39 C40 3.1(5) . . . . ? C34 C38 C39 C40 -176.2(3) . . . . ? C38 C39 C40 C41 -0.4(5) . . . . ? C39 C40 C41 C42 -2.3(5) . . . . ? C40 C41 C42 C43 2.3(5) . . . . ? C39 C38 C43 C42 -3.0(4) . . . . ? C34 C38 C43 C42 176.2(3) . . . . ? C41 C42 C43 C38 0.4(5) . . . . ? O5 C34 C44 C49 -136.4(3) . . . . ? C38 C34 C44 C49 -18.3(4) . . . . ? C35 C34 C44 C49 103.1(3) . . . . ? O5 C34 C44 C45 41.9(4) . . . . ? C38 C34 C44 C45 160.0(3) . . . . ? C35 C34 C44 C45 -78.6(3) . . . . ? C49 C44 C45 C46 0.9(5) . . . . ? C34 C44 C45 C46 -177.5(3) . . . . ? C44 C45 C46 C47 1.2(5) . . . . ? C45 C46 C47 C48 -2.1(6) . . . . ? C46 C47 C48 C49 1.0(6) . . . . ? C47 C48 C49 C44 1.1(6) . . . . ? C45 C44 C49 C48 -2.0(5) . . . . ? C34 C44 C49 C48 176.4(3) . . . . ? O8 C37 C50 C55 25.8(4) . . . . ? C56 C37 C50 C55 144.6(3) . . . . ? C36 C37 C50 C55 -91.8(3) . . . . ? O8 C37 C50 C51 -155.2(3) . . . . ? C56 C37 C50 C51 -36.4(4) . . . . ? C36 C37 C50 C51 87.1(3) . . . . ? C55 C50 C51 C52 -0.7(5) . . . . ? C37 C50 C51 C52 -179.6(3) . . . . ? C50 C51 C52 C53 -0.1(5) . . . . ? C51 C52 C53 C54 0.1(6) . . . . ? C52 C53 C54 C55 0.6(6) . . . . ? C53 C54 C55 C50 -1.4(5) . . . . ? C51 C50 C55 C54 1.4(5) . . . . ? C37 C50 C55 C54 -179.6(3) . . . . ? O8 C37 C56 C57 -118.2(3) . . . . ? C50 C37 C56 C57 121.6(3) . . . . ? C36 C37 C56 C57 -2.4(4) . . . . ? O8 C37 C56 C61 62.0(3) . . . . ? C50 C37 C56 C61 -58.3(3) . . . . ? C36 C37 C56 C61 177.7(3) . . . . ? C61 C56 C57 C58 -1.5(5) . . . . ? C37 C56 C57 C58 178.6(3) . . . . ? C56 C57 C58 C59 1.0(5) . . . . ? C57 C58 C59 C60 -0.2(6) . . . . ? C58 C59 C60 C61 0.0(5) . . . . ? C59 C60 C61 C56 -0.4(5) . . . . ? C57 C56 C61 C60 1.2(5) . . . . ? C37 C56 C61 C60 -178.9(3) . . . . ? O9 C65 C66 C67 -20.2(5) . . . . ? C65 C66 C67 C68 35.7(5) . . . . ? C66 C67 C68 O9 -38.7(4) . . . . ? O10 C69 C70 C71 21.5(5) . . . . ? C69 C70 C71 C72 -26.6(5) . . . . ? C70 C71 C72 O10 22.1(4) . . . . ? C79 C74 C75 C76 1.5(7) . . . . ? C73 C74 C75 C76 -176.5(4) . . . . ? C74 C75 C76 C77 -0.2(7) . . . . ? C75 C76 C77 C78 -1.8(8) . . . . ? C76 C77 C78 C79 2.5(9) . . . . ? C75 C74 C79 C78 -0.7(7) . . . . ? C73 C74 C79 C78 177.3(5) . . . . ? C77 C78 C79 C74 -1.3(9) . . . . ? C13 C3 O1 Zn2 -124.1(2) . . . . ? C7 C3 O1 Zn2 116.2(2) . . . . ? C4 C3 O1 Zn2 -3.4(3) . . . . ? C13 C3 O1 Zn1 38.7(3) . . . . ? C7 C3 O1 Zn1 -81.0(2) . . . . ? C4 C3 O1 Zn1 159.39(16) . . . . ? C5 C4 O2 C31 0.1(3) . . . . ? C3 C4 O2 C31 124.5(2) . . . . ? O3 C31 O2 C4 -1.6(3) . . . . ? C32 C31 O2 C4 -119.3(3) . . . . ? C33 C31 O2 C4 117.4(3) . . . . ? O2 C31 O3 C5 2.6(3) . . . . ? C32 C31 O3 C5 121.6(3) . . . . ? C33 C31 O3 C5 -116.2(3) . . . . ? C4 C5 O3 C31 -2.5(3) . . . . ? C6 C5 O3 C31 122.5(3) . . . . ? C25 C6 O4 Zn2 -164.60(18) . . . . ? C19 C6 O4 Zn2 75.1(3) . . . . ? C5 C6 O4 Zn2 -43.6(3) . . . . ? C25 C6 O4 Zn3 34.6(3) . . . . ? C19 C6 O4 Zn3 -85.7(3) . . . . ? C5 C6 O4 Zn3 155.59(19) . . . . ? C44 C34 O5 Zn2 -122.0(2) . . . . ? C38 C34 O5 Zn2 117.8(2) . . . . ? C35 C34 O5 Zn2 0.0(3) . . . . ? C44 C34 O5 Zn3 29.1(3) . . . . ? C38 C34 O5 Zn3 -91.0(2) . . . . ? C35 C34 O5 Zn3 151.19(17) . . . . ? O7 C62 O6 C35 -0.1(3) . . . . ? C63 C62 O6 C35 119.2(3) . . . . ? C64 C62 O6 C35 -117.4(3) . . . . ? C36 C35 O6 C62 0.0(3) . . . . ? C34 C35 O6 C62 126.0(2) . . . . ? C35 C36 O7 C62 -0.2(3) . . . . ? C37 C36 O7 C62 123.3(2) . . . . ? O6 C62 O7 C36 0.1(3) . . . . ? C63 C62 O7 C36 -117.9(3) . . . . ? C64 C62 O7 C36 118.5(3) . . . . ? C50 C37 O8 Zn2 -159.95(17) . . . . ? C56 C37 O8 Zn2 80.7(2) . . . . ? C36 C37 O8 Zn2 -38.6(3) . . . . ? C50 C37 O8 Zn1 47.1(3) . . . . ? C56 C37 O8 Zn1 -72.3(3) . . . . ? C36 C37 O8 Zn1 168.46(17) . . . . ? C67 C68 O9 C65 26.7(4) . . . . ? C67 C68 O9 Zn1 -157.7(3) . . . . ? C66 C65 O9 C68 -4.2(4) . . . . ? C66 C65 O9 Zn1 -179.6(2) . . . . ? C70 C69 O10 C72 -7.7(5) . . . . ? C70 C69 O10 Zn3 -172.4(3) . . . . ? C71 C72 O10 C69 -9.2(4) . . . . ? C71 C72 O10 Zn3 156.4(2) . . . . ? C3 O1 Zn1 C1 -10.6(3) . . . . ? Zn2 O1 Zn1 C1 157.36(17) . . . . ? C3 O1 Zn1 O8 -160.8(2) . . . . ? Zn2 O1 Zn1 O8 7.19(8) . . . . ? C3 O1 Zn1 O9 104.5(2) . . . . ? Zn2 O1 Zn1 O9 -87.55(9) . . . . ? C3 O1 Zn1 Zn2 -167.9(2) . . . . ? C37 O8 Zn1 C1 -0.9(3) . . . . ? Zn2 O8 Zn1 C1 -158.81(17) . . . . ? C37 O8 Zn1 O1 150.5(2) . . . . ? Zn2 O8 Zn1 O1 -7.35(8) . . . . ? C37 O8 Zn1 O9 -114.7(2) . . . . ? Zn2 O8 Zn1 O9 87.45(9) . . . . ? C37 O8 Zn1 Zn2 157.9(3) . . . . ? C68 O9 Zn1 C1 -13.6(3) . . . . ? C65 O9 Zn1 C1 161.2(3) . . . . ? C68 O9 Zn1 O1 -154.1(3) . . . . ? C65 O9 Zn1 O1 20.7(3) . . . . ? C68 O9 Zn1 O8 124.4(3) . . . . ? C65 O9 Zn1 O8 -60.8(3) . . . . ? C68 O9 Zn1 Zn2 164.6(3) . . . . ? C65 O9 Zn1 Zn2 -20.6(3) . . . . ? C6 O4 Zn2 O8 -46.1(4) . . . . ? Zn3 O4 Zn2 O8 119.6(2) . . . . ? C6 O4 Zn2 O1 60.3(2) . . . . ? Zn3 O4 Zn2 O1 -133.95(9) . . . . ? C6 O4 Zn2 O5 -158.0(2) . . . . ? Zn3 O4 Zn2 O5 7.72(9) . . . . ? C6 O4 Zn2 Zn1 45.8(3) . . . . ? Zn3 O4 Zn2 Zn1 -148.48(4) . . . . ? C6 O4 Zn2 Zn3 -165.7(3) . . . . ? C37 O8 Zn2 O4 -43.0(3) . . . . ? Zn1 O8 Zn2 O4 117.5(2) . . . . ? C37 O8 Zn2 O1 -153.15(19) . . . . ? Zn1 O8 Zn2 O1 7.36(8) . . . . ? C37 O8 Zn2 O5 65.0(2) . . . . ? Zn1 O8 Zn2 O5 -134.49(8) . . . . ? C37 O8 Zn2 Zn1 -160.5(2) . . . . ? C37 O8 Zn2 Zn3 50.6(2) . . . . ? Zn1 O8 Zn2 Zn3 -148.91(5) . . . . ? C3 O1 Zn2 O4 -1.0(2) . . . . ? Zn1 O1 Zn2 O4 -167.08(7) . . . . ? C3 O1 Zn2 O8 158.7(2) . . . . ? Zn1 O1 Zn2 O8 -7.39(8) . . . . ? C3 O1 Zn2 O5 -96.6(3) . . . . ? Zn1 O1 Zn2 O5 97.30(13) . . . . ? C3 O1 Zn2 Zn1 166.1(3) . . . . ? C3 O1 Zn2 Zn3 -38.6(3) . . . . ? Zn1 O1 Zn2 Zn3 155.33(3) . . . . ? C34 O5 Zn2 O4 148.6(2) . . . . ? Zn3 O5 Zn2 O4 -7.68(9) . . . . ? C34 O5 Zn2 O8 -11.2(2) . . . . ? Zn3 O5 Zn2 O8 -167.53(8) . . . . ? C34 O5 Zn2 O1 -108.5(2) . . . . ? Zn3 O5 Zn2 O1 95.19(14) . . . . ? C34 O5 Zn2 Zn1 -49.5(3) . . . . ? Zn3 O5 Zn2 Zn1 154.21(3) . . . . ? C34 O5 Zn2 Zn3 156.3(3) . . . . ? C1 Zn1 Zn2 O4 -69.6(5) . . . . ? O1 Zn1 Zn2 O4 21.52(13) . . . . ? O8 Zn1 Zn2 O4 -147.44(13) . . . . ? O9 Zn1 Zn2 O4 117.05(12) . . . . ? C1 Zn1 Zn2 O8 77.8(5) . . . . ? O1 Zn1 Zn2 O8 168.97(12) . . . . ? O9 Zn1 Zn2 O8 -95.51(11) . . . . ? C1 Zn1 Zn2 O1 -91.1(5) . . . . ? O8 Zn1 Zn2 O1 -168.97(12) . . . . ? O9 Zn1 Zn2 O1 95.52(10) . . . . ? C1 Zn1 Zn2 O5 141.8(5) . . . . ? O1 Zn1 Zn2 O5 -127.09(11) . . . . ? O8 Zn1 Zn2 O5 63.94(11) . . . . ? O9 Zn1 Zn2 O5 -31.57(10) . . . . ? C1 Zn1 Zn2 Zn3 -161.5(5) . . . . ? O1 Zn1 Zn2 Zn3 -70.36(9) . . . . ? O8 Zn1 Zn2 Zn3 120.67(9) . . . . ? O9 Zn1 Zn2 Zn3 25.16(8) . . . . ? C6 O4 Zn3 C2 5.8(3) . . . . ? Zn2 O4 Zn3 C2 -158.80(14) . . . . ? C6 O4 Zn3 O5 156.9(2) . . . . ? Zn2 O4 Zn3 O5 -7.66(9) . . . . ? C6 O4 Zn3 O10 -109.9(2) . . . . ? Zn2 O4 Zn3 O10 85.48(10) . . . . ? C6 O4 Zn3 Zn2 164.6(3) . . . . ? C34 O5 Zn3 C2 -7.3(3) . . . . ? Zn2 O5 Zn3 C2 152.18(16) . . . . ? C34 O5 Zn3 O4 -152.1(2) . . . . ? Zn2 O5 Zn3 O4 7.41(9) . . . . ? C34 O5 Zn3 O10 109.93(19) . . . . ? Zn2 O5 Zn3 O10 -90.54(9) . . . . ? C34 O5 Zn3 Zn2 -159.5(2) . . . . ? C69 O10 Zn3 C2 167.7(3) . . . . ? C72 O10 Zn3 C2 4.5(3) . . . . ? C69 O10 Zn3 O4 -57.1(3) . . . . ? C72 O10 Zn3 O4 139.7(2) . . . . ? C69 O10 Zn3 O5 23.2(3) . . . . ? C72 O10 Zn3 O5 -140.0(2) . . . . ? C69 O10 Zn3 Zn2 -17.8(3) . . . . ? C72 O10 Zn3 Zn2 179.0(2) . . . . ? O4 Zn2 Zn3 C2 63.5(4) . . . . ? O8 Zn2 Zn3 C2 -83.7(4) . . . . ? O1 Zn2 Zn3 C2 127.0(4) . . . . ? O5 Zn2 Zn3 C2 -105.0(4) . . . . ? Zn1 Zn2 Zn3 C2 -179.8(3) . . . . ? O8 Zn2 Zn3 O4 -147.22(14) . . . . ? O1 Zn2 Zn3 O4 63.51(12) . . . . ? O5 Zn2 Zn3 O4 -168.45(14) . . . . ? Zn1 Zn2 Zn3 O4 116.69(10) . . . . ? O4 Zn2 Zn3 O5 168.45(14) . . . . ? O8 Zn2 Zn3 O5 21.24(13) . . . . ? O1 Zn2 Zn3 O5 -128.04(11) . . . . ? Zn1 Zn2 Zn3 O5 -74.85(10) . . . . ? O4 Zn2 Zn3 O10 -98.95(11) . . . . ? O8 Zn2 Zn3 O10 113.83(11) . . . . ? O1 Zn2 Zn3 O10 -35.44(9) . . . . ? O5 Zn2 Zn3 O10 92.60(11) . . . . ? Zn1 Zn2 Zn3 O10 17.75(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.444 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.060 #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 662789' _audit_creation_date 05-08-17 _audit_creation_method 'STOE X-RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H72 Li2 O10 Zn, C7 H8' _chemical_formula_sum 'C77 H80 Li2 O10 Zn' _chemical_formula_weight 1244.66 _chemical_absolute_configuration rmad 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6597(6) _cell_length_b 15.5812(7) _cell_length_c 19.3475(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.443(4) _cell_angle_gamma 90.00 _cell_volume 3388.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.571 _exptl_crystal_size_mid 0.427 _exptl_crystal_size_min 0.293 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7599 _exptl_absorpt_correction_T_max 0.8090 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37991 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15534 _reflns_number_gt 12590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0702P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(9) _refine_ls_number_reflns 15534 _refine_ls_number_parameters 719 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 -0.3926(3) -0.08482(19) -0.31143(16) 0.0325(6) Uani 1 1 d . . . C2 C -0.2832(3) -0.05159(18) -0.33562(17) 0.0329(6) Uani 1 1 d . . . H2 H -0.2790 -0.0844 -0.3793 0.039 Uiso 1 1 calc R . . C3 C -0.1597(3) -0.05519(18) -0.28098(18) 0.0323(6) Uani 1 1 d . . . H3 H -0.1714 -0.0479 -0.2319 0.039 Uiso 1 1 calc R . . C4 C -0.0694(2) -0.12989(17) -0.27776(16) 0.0306(6) Uani 1 1 d . . . C5 C -0.5094(3) -0.0792(2) -0.37166(17) 0.0381(7) Uani 1 1 d . . . C6 C -0.6079(3) -0.1223(2) -0.3598(2) 0.0447(8) Uani 1 1 d . . . H6 H -0.6004 -0.1505 -0.3152 0.054 Uiso 1 1 calc R . . C7 C -0.7160(3) -0.1248(3) -0.4116(2) 0.0558(10) Uani 1 1 d . . . H7 H -0.7819 -0.1537 -0.4019 0.067 Uiso 1 1 calc R . . C8 C -0.7281(3) -0.0861(3) -0.4763(2) 0.0695(12) Uani 1 1 d . . . H8 H -0.8014 -0.0889 -0.5124 0.083 Uiso 1 1 calc R . . C9 C -0.6304(4) -0.0419(4) -0.4886(2) 0.0825(16) Uani 1 1 d . . . H9 H -0.6386 -0.0135 -0.5331 0.099 Uiso 1 1 calc R . . C10 C -0.5221(3) -0.0390(3) -0.4369(2) 0.0559(9) Uani 1 1 d . . . H10 H -0.4567 -0.0094 -0.4464 0.067 Uiso 1 1 calc R . . C11 C -0.4072(3) -0.03468(19) -0.24608(17) 0.0338(6) Uani 1 1 d . . . C12 C -0.3596(3) -0.0643(2) -0.17670(18) 0.0387(8) Uani 1 1 d . . . H12 H -0.3150 -0.1161 -0.1696 0.046 Uiso 1 1 calc R . . C13 C -0.3752(3) -0.0206(3) -0.1175(2) 0.0508(9) Uani 1 1 d . . . H13 H -0.3423 -0.0430 -0.0707 0.061 Uiso 1 1 calc R . . C14 C -0.4376(4) 0.0542(3) -0.1261(2) 0.0585(10) Uani 1 1 d . . . H14 H -0.4482 0.0841 -0.0855 0.070 Uiso 1 1 calc R . . C15 C -0.4856(3) 0.0867(2) -0.1942(2) 0.0555(10) Uani 1 1 d . . . H15 H -0.5278 0.1395 -0.2004 0.067 Uiso 1 1 calc R . . C16 C -0.4718(3) 0.0416(2) -0.2542(2) 0.0438(7) Uani 1 1 d . . . H16 H -0.5069 0.0633 -0.3009 0.053 Uiso 1 1 calc R . . C17 C -0.0581(2) -0.1578(2) -0.35162(17) 0.0364(6) Uani 1 1 d . . . C18 C -0.0375(3) -0.2449(3) -0.36143(19) 0.0513(7) Uani 1 1 d . . . H18 H -0.0317 -0.2841 -0.3231 0.062 Uiso 1 1 calc R . . C19 C -0.0253(4) -0.2745(3) -0.4279(3) 0.0718(13) Uani 1 1 d . . . H19 H -0.0127 -0.3338 -0.4345 0.086 Uiso 1 1 calc R . . C20 C -0.0317(4) -0.2182(3) -0.4830(2) 0.0677(13) Uani 1 1 d . . . H20 H -0.0224 -0.2383 -0.5276 0.081 Uiso 1 1 calc R . . C21 C -0.0511(4) -0.1345(3) -0.4740(2) 0.0611(10) Uani 1 1 d . . . H21 H -0.0571 -0.0958 -0.5128 0.073 Uiso 1 1 calc R . . C22 C -0.0625(3) -0.1034(2) -0.40828(19) 0.0487(8) Uani 1 1 d . . . H22 H -0.0735 -0.0437 -0.4027 0.058 Uiso 1 1 calc R . . C23 C 0.0509(2) -0.09751(18) -0.22874(17) 0.0319(6) Uani 1 1 d . . . C24 C 0.0588(3) -0.0795(2) -0.15771(18) 0.0391(7) Uani 1 1 d . . . H24 H -0.0105 -0.0850 -0.1412 0.047 Uiso 1 1 calc R . . C25 C 0.1642(3) -0.0536(2) -0.10950(19) 0.0464(8) Uani 1 1 d . . . H25 H 0.1667 -0.0422 -0.0609 0.056 Uiso 1 1 calc R . . C26 C 0.2651(3) -0.0448(2) -0.1335(2) 0.0483(8) Uani 1 1 d . . . H26 H 0.3379 -0.0271 -0.1012 0.058 Uiso 1 1 calc R . . C27 C 0.2601(3) -0.0616(2) -0.2042(2) 0.0500(8) Uani 1 1 d . . . H27 H 0.3293 -0.0547 -0.2208 0.060 Uiso 1 1 calc R . . C28 C 0.1538(3) -0.0888(2) -0.25146(18) 0.0391(7) Uani 1 1 d . . . H28 H 0.1518 -0.1015 -0.2998 0.047 Uiso 1 1 calc R . . C29 C -0.1924(3) 0.0848(2) -0.3204(2) 0.0427(7) Uani 1 1 d . . . C30 C -0.2091(3) 0.1344(2) -0.2562(2) 0.0492(8) Uani 1 1 d . . . H30A H -0.2260 0.0943 -0.2212 0.074 Uiso 1 1 calc R . . H30B H -0.2758 0.1745 -0.2720 0.074 Uiso 1 1 calc R . . H30C H -0.1364 0.1666 -0.2341 0.074 Uiso 1 1 calc R . . C31 C -0.1574(4) 0.1422(2) -0.3747(2) 0.0523(9) Uani 1 1 d . . . H31A H -0.0814 0.1701 -0.3522 0.078 Uiso 1 1 calc R . . H31B H -0.2189 0.1860 -0.3915 0.078 Uiso 1 1 calc R . . H31C H -0.1495 0.1076 -0.4155 0.078 Uiso 1 1 calc R . . C32 C -0.2092(3) -0.3494(2) -0.10039(16) 0.0370(6) Uani 1 1 d . . . C33 C -0.2506(3) -0.4337(2) -0.14125(18) 0.0414(7) Uani 1 1 d . . . H33 H -0.1856 -0.4541 -0.1621 0.050 Uiso 1 1 calc R . . C34 C -0.3685(3) -0.4332(2) -0.2018(2) 0.0409(8) Uani 1 1 d . . . H34 H -0.4206 -0.3867 -0.1914 0.049 Uiso 1 1 calc R . . C35 C -0.3680(3) -0.4263(2) -0.28252(19) 0.0402(7) Uani 1 1 d . . . C36 C -0.0897(3) -0.3606(3) -0.04343(18) 0.0496(9) Uani 1 1 d . . . C37 C -0.0393(3) -0.2871(3) -0.0082(2) 0.0635(11) Uani 1 1 d . . . H37 H -0.0828 -0.2349 -0.0173 0.076 Uiso 1 1 calc R . . C38 C 0.0724(5) -0.2870(4) 0.0398(3) 0.0851(15) Uiso 1 1 d . . . H38 H 0.1078 -0.2356 0.0620 0.102 Uiso 1 1 calc R . . C39 C 0.1308(6) -0.3658(4) 0.0542(4) 0.0947(17) Uiso 1 1 d . . . H39 H 0.2064 -0.3677 0.0882 0.114 Uiso 1 1 calc R . . C40 C 0.0840(5) -0.4397(4) 0.0216(3) 0.0848(14) Uiso 1 1 d . . . H40 H 0.1270 -0.4920 0.0321 0.102 Uiso 1 1 calc R . . C41 C -0.0283(3) -0.4380(4) -0.0275(2) 0.0717(14) Uani 1 1 d . . . H41 H -0.0626 -0.4895 -0.0500 0.086 Uiso 1 1 calc R . . C42 C -0.3028(3) -0.3170(2) -0.06377(17) 0.0376(6) Uani 1 1 d . . . C43 C -0.3915(3) -0.2612(2) -0.0990(2) 0.0454(8) Uani 1 1 d . . . H43 H -0.3954 -0.2437 -0.1467 0.055 Uiso 1 1 calc R . . C44 C -0.4757(4) -0.2303(3) -0.0651(3) 0.0658(13) Uani 1 1 d . . . H44 H -0.5369 -0.1924 -0.0895 0.079 Uiso 1 1 calc R . . C45 C -0.4685(4) -0.2557(4) 0.0044(3) 0.0750(13) Uani 1 1 d . . . H45 H -0.5248 -0.2347 0.0279 0.090 Uiso 1 1 calc R . . C46 C -0.3806(4) -0.3110(3) 0.0399(2) 0.0668(12) Uani 1 1 d . . . H46 H -0.3761 -0.3282 0.0877 0.080 Uiso 1 1 calc R . . C47 C -0.2991(3) -0.3411(3) 0.0059(2) 0.0510(8) Uani 1 1 d . . . H47 H -0.2388 -0.3794 0.0306 0.061 Uiso 1 1 calc R . . C48 C -0.4959(3) -0.4451(2) -0.3277(2) 0.0482(8) Uani 1 1 d . . . C49 C -0.5834(4) -0.3853(3) -0.3257(2) 0.0553(9) Uani 1 1 d . . . H49 H -0.5639 -0.3386 -0.2932 0.066 Uiso 1 1 calc R . . C50 C -0.6981(4) -0.3919(4) -0.3697(3) 0.0793(14) Uani 1 1 d . . . H50 H -0.7547 -0.3485 -0.3683 0.095 Uiso 1 1 calc R . . C51 C -0.7306(5) -0.4591(5) -0.4146(3) 0.100(2) Uani 1 1 d . . . H51 H -0.8100 -0.4640 -0.4437 0.120 Uiso 1 1 calc R . . C52 C -0.6476(6) -0.5201(5) -0.4176(3) 0.108(2) Uani 1 1 d . . . H52 H -0.6699 -0.5673 -0.4495 0.129 Uiso 1 1 calc R . . C53 C -0.5295(4) -0.5143(3) -0.3742(3) 0.0759(14) Uani 1 1 d . . . H53 H -0.4731 -0.5574 -0.3768 0.091 Uiso 1 1 calc R . . C54 C -0.2738(3) -0.48589(19) -0.29906(19) 0.0439(7) Uani 1 1 d . . . C55 C -0.1879(3) -0.4528(2) -0.3284(2) 0.0504(9) Uani 1 1 d . . . H55 H -0.1904 -0.3935 -0.3399 0.061 Uiso 1 1 calc R . . C56 C -0.0973(4) -0.5029(3) -0.3419(3) 0.0633(10) Uiso 1 1 d . . . H56 H -0.0408 -0.4783 -0.3635 0.076 Uiso 1 1 calc R . . C57 C -0.0910(5) -0.5877(4) -0.3238(3) 0.0829(14) Uiso 1 1 d . . . H57 H -0.0272 -0.6222 -0.3299 0.099 Uiso 1 1 calc R . . C58 C -0.1779(6) -0.6228(4) -0.2965(4) 0.0939(17) Uiso 1 1 d . . . H58 H -0.1747 -0.6822 -0.2852 0.113 Uiso 1 1 calc R . . C59 C -0.2707(6) -0.5733(3) -0.2849(3) 0.0842(16) Uani 1 1 d . . . H59 H -0.3313 -0.5992 -0.2675 0.101 Uiso 1 1 calc R . . C60 C -0.3790(4) -0.5412(2) -0.1203(2) 0.0549(9) Uani 1 1 d . . . C61 C -0.4681(4) -0.5176(4) -0.0791(3) 0.0730(13) Uani 1 1 d . . . H61A H -0.4833 -0.4556 -0.0830 0.110 Uiso 1 1 calc R . . H61B H -0.4361 -0.5331 -0.0285 0.110 Uiso 1 1 calc R . . H61C H -0.5427 -0.5486 -0.0990 0.110 Uiso 1 1 calc R . . C62 C -0.3563(6) -0.6378(3) -0.1208(4) 0.0894(18) Uani 1 1 d . . . H62A H -0.4307 -0.6675 -0.1438 0.134 Uiso 1 1 calc R . . H62B H -0.3261 -0.6583 -0.0714 0.134 Uiso 1 1 calc R . . H62C H -0.2973 -0.6495 -0.1475 0.134 Uiso 1 1 calc R . . C63 C -0.5529(6) -0.2904(4) -0.5161(3) 0.0919(16) Uiso 1 1 d . . . H63A H -0.6215 -0.2528 -0.5163 0.110 Uiso 1 1 calc R . . H63B H -0.5774 -0.3509 -0.5138 0.110 Uiso 1 1 calc R . . C64 C -0.5098(6) -0.2750(4) -0.5821(3) 0.0996(18) Uiso 1 1 d . . . H64A H -0.5481 -0.3152 -0.6211 0.120 Uiso 1 1 calc R . . H64B H -0.5262 -0.2154 -0.5996 0.120 Uiso 1 1 calc R . . C65 C -0.3810(7) -0.2910(5) -0.5571(4) 0.112(2) Uiso 1 1 d . . . H65A H -0.3621 -0.3509 -0.5669 0.135 Uiso 1 1 calc R . . H65B H -0.3367 -0.2517 -0.5809 0.135 Uiso 1 1 calc R . . C66 C -0.3512(7) -0.2747(5) -0.4803(4) 0.115(2) Uiso 1 1 d . . . H66A H -0.2994 -0.3212 -0.4544 0.138 Uiso 1 1 calc R . . H66B H -0.3073 -0.2198 -0.4694 0.138 Uiso 1 1 calc R . . C67 C 0.1033(5) -0.4049(4) -0.1753(3) 0.0853(15) Uiso 1 1 d . . . H67A H 0.0223 -0.4185 -0.2051 0.102 Uiso 1 1 calc R A 1 H67B H 0.1267 -0.4485 -0.1369 0.102 Uiso 1 1 calc R A 1 C68A C 0.1884(9) -0.4045(6) -0.2198(6) 0.075(2) Uiso 0.60 1 d P B 1 H68A H 0.1460 -0.4003 -0.2713 0.090 Uiso 0.60 1 calc PR B 1 H68B H 0.2372 -0.4574 -0.2119 0.090 Uiso 0.60 1 calc PR B 1 C69A C 0.2669(7) -0.3243(5) -0.1949(5) 0.0645(18) Uiso 0.60 1 d P B 1 H69A H 0.2521 -0.2797 -0.2327 0.077 Uiso 0.60 1 calc PR B 1 H69B H 0.3525 -0.3393 -0.1812 0.077 Uiso 0.60 1 calc PR B 1 C68B C 0.2200(16) -0.4194(11) -0.1883(10) 0.092(5) Uiso 0.40 1 d P B 2 H68C H 0.2573 -0.4717 -0.1630 0.110 Uiso 0.40 1 calc PR B 2 H68D H 0.2119 -0.4265 -0.2402 0.110 Uiso 0.40 1 calc PR B 2 C69B C 0.2832(17) -0.3532(12) -0.1642(11) 0.103(5) Uiso 0.40 1 d P B 2 H69C H 0.3037 -0.3237 -0.2047 0.123 Uiso 0.40 1 calc PR B 2 H69D H 0.3585 -0.3722 -0.1303 0.123 Uiso 0.40 1 calc PR B 2 C70 C 0.2257(4) -0.2937(3) -0.1287(3) 0.0731(12) Uiso 1 1 d . . . H70A H 0.2736 -0.3208 -0.0840 0.088 Uiso 1 1 calc R B 1 H70B H 0.2316 -0.2305 -0.1234 0.088 Uiso 1 1 calc R B 1 C71 C -0.1649(12) -0.1395(9) 0.1215(7) 0.213(5) Uiso 1 1 d . . . H71A H -0.0843 -0.1156 0.1325 0.320 Uiso 1 1 calc R . . H71B H -0.2228 -0.0927 0.1155 0.320 Uiso 1 1 calc R . . H71C H -0.1802 -0.1730 0.0770 0.320 Uiso 1 1 calc R . . C72 C -0.1762(6) -0.1976(5) 0.1827(4) 0.1030(19) Uiso 1 1 d . . . C73 C -0.1306(5) -0.2777(4) 0.1867(3) 0.0904(16) Uiso 1 1 d . . . H73 H -0.0897 -0.2952 0.1528 0.109 Uiso 1 1 calc R . . C74 C -0.1416(5) -0.3319(4) 0.2365(3) 0.0866(15) Uiso 1 1 d . . . H74 H -0.1055 -0.3868 0.2384 0.104 Uiso 1 1 calc R . . C75 C -0.2014(7) -0.3130(5) 0.2845(4) 0.114(2) Uiso 1 1 d . . . H75 H -0.2117 -0.3546 0.3183 0.137 Uiso 1 1 calc R . . C76 C -0.2491(7) -0.2293(5) 0.2836(5) 0.126(2) Uiso 1 1 d . . . H76 H -0.2876 -0.2120 0.3189 0.151 Uiso 1 1 calc R . . C77 C -0.2382(7) -0.1724(5) 0.2293(4) 0.118(2) Uiso 1 1 d . . . H77 H -0.2738 -0.1171 0.2253 0.141 Uiso 1 1 calc R . . O1 O -0.37648(18) -0.17322(13) -0.29650(12) 0.0332(5) Uani 1 1 d . . . O2 O -0.10224(18) -0.19931(12) -0.24118(12) 0.0345(4) Uani 1 1 d . B . O3 O -0.29849(19) 0.03791(13) -0.35434(12) 0.0400(5) Uani 1 1 d . . . O4 O -0.10317(19) 0.02184(13) -0.29804(13) 0.0393(5) Uani 1 1 d . . . O5 O -0.18523(18) -0.28829(14) -0.14818(11) 0.0372(5) Uani 1 1 d . B . O6 O -0.3457(2) -0.34135(13) -0.29839(13) 0.0383(5) Uani 1 1 d . . . O7 O -0.2698(2) -0.49818(16) -0.09212(15) 0.0546(6) Uani 1 1 d . . . O8 O -0.4207(3) -0.51467(16) -0.19288(15) 0.0544(7) Uani 1 1 d . . . O9 O -0.4554(3) -0.2707(2) -0.45753(14) 0.0687(9) Uani 1 1 d . . . O10 O 0.1058(2) -0.32103(17) -0.14498(16) 0.0572(7) Uani 1 1 d . B . Li1 Li -0.4423(5) -0.2611(4) -0.3594(3) 0.0486(14) Uani 1 1 d . . . Li2 Li -0.0333(4) -0.2542(5) -0.1547(3) 0.0471(12) Uani 1 1 d . . . Zn Zn -0.25426(3) -0.24949(2) -0.244333(16) 0.02933(8) Uani 1 1 d . B . 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 0.0298(15) 0.0339(14) 0.0328(16) 0.0045(12) 0.0068(12) 0.0057(11) C2 0.0319(15) 0.0326(14) 0.0344(15) 0.0058(12) 0.0092(12) 0.0044(11) C3 0.0278(14) 0.0319(14) 0.0390(16) 0.0031(12) 0.0124(13) -0.0037(11) C4 0.0256(13) 0.0346(13) 0.0325(14) 0.0037(11) 0.0096(11) -0.0012(10) C5 0.0273(14) 0.0490(17) 0.0357(16) 0.0028(13) 0.0042(12) 0.0070(12) C6 0.0321(17) 0.064(2) 0.0365(18) -0.0034(16) 0.0073(14) 0.0000(15) C7 0.0307(17) 0.080(3) 0.055(2) -0.0102(19) 0.0070(16) 0.0015(16) C8 0.0339(19) 0.117(4) 0.048(2) -0.002(2) -0.0067(17) 0.004(2) C9 0.048(2) 0.148(5) 0.042(2) 0.034(3) -0.0057(18) 0.006(3) C10 0.0400(19) 0.078(2) 0.046(2) 0.0191(18) 0.0050(16) -0.0013(17) C11 0.0255(14) 0.0367(14) 0.0401(17) -0.0028(13) 0.0101(12) -0.0017(11) C12 0.0389(18) 0.0429(17) 0.0356(18) -0.0049(14) 0.0124(14) -0.0055(13) C13 0.046(2) 0.064(2) 0.0411(19) -0.0110(16) 0.0099(16) -0.0101(16) C14 0.047(2) 0.070(2) 0.061(3) -0.027(2) 0.0194(19) -0.0061(19) C15 0.047(2) 0.0474(18) 0.077(3) -0.0202(18) 0.026(2) 0.0001(15) C16 0.0346(16) 0.0406(16) 0.057(2) 0.0006(15) 0.0141(15) 0.0055(13) C17 0.0219(13) 0.0475(16) 0.0388(16) -0.0029(13) 0.0065(12) -0.0028(12) C18 0.0544(18) 0.0475(16) 0.0572(19) -0.006(2) 0.0239(15) -0.004(2) C19 0.078(3) 0.063(3) 0.085(3) -0.028(2) 0.040(3) -0.009(2) C20 0.048(2) 0.109(4) 0.048(2) -0.024(2) 0.0167(18) -0.006(2) C21 0.050(2) 0.092(3) 0.043(2) 0.012(2) 0.0166(17) 0.015(2) C22 0.047(2) 0.061(2) 0.0427(19) 0.0095(16) 0.0194(16) 0.0157(16) C23 0.0249(13) 0.0323(13) 0.0393(16) 0.0015(12) 0.0100(12) -0.0015(10) C24 0.0318(16) 0.0462(17) 0.0408(17) -0.0006(14) 0.0122(13) -0.0005(13) C25 0.0444(19) 0.0523(19) 0.0397(18) -0.0060(15) 0.0063(15) 0.0019(15) C26 0.0308(16) 0.057(2) 0.053(2) -0.0084(16) 0.0045(15) -0.0040(14) C27 0.0311(17) 0.068(2) 0.053(2) -0.0078(17) 0.0154(15) -0.0103(15) C28 0.0305(15) 0.0530(17) 0.0357(16) -0.0045(14) 0.0119(13) -0.0061(13) C29 0.0364(17) 0.0419(16) 0.0472(19) 0.0097(14) 0.0069(14) 0.0024(13) C30 0.0483(19) 0.0415(17) 0.057(2) -0.0014(15) 0.0135(17) 0.0011(14) C31 0.053(2) 0.0439(18) 0.060(2) 0.0152(17) 0.0162(18) -0.0024(16) C32 0.0298(14) 0.0529(17) 0.0288(14) 0.0119(13) 0.0088(12) 0.0011(12) C33 0.0408(17) 0.0432(16) 0.0421(18) 0.0117(14) 0.0141(15) 0.0060(13) C34 0.0442(19) 0.0394(17) 0.042(2) 0.0038(15) 0.0158(16) -0.0055(14) C35 0.0453(19) 0.0329(14) 0.0436(19) -0.0042(14) 0.0143(16) -0.0098(13) C36 0.0297(16) 0.084(3) 0.0363(17) 0.0173(17) 0.0105(14) 0.0043(16) C37 0.0386(19) 0.105(3) 0.043(2) 0.001(2) 0.0047(16) 0.0000(19) C41 0.039(2) 0.111(4) 0.066(3) 0.049(3) 0.0159(19) 0.020(2) C42 0.0317(15) 0.0456(16) 0.0374(16) 0.0020(13) 0.0124(13) -0.0053(12) C43 0.0352(15) 0.045(2) 0.0573(18) -0.0022(16) 0.0140(14) -0.0037(14) C44 0.043(2) 0.059(3) 0.102(3) -0.015(2) 0.031(2) -0.0001(17) C45 0.063(2) 0.086(3) 0.094(3) -0.029(3) 0.052(2) -0.013(3) C46 0.060(3) 0.098(3) 0.053(2) -0.013(2) 0.033(2) -0.021(2) C47 0.046(2) 0.068(2) 0.0428(19) 0.0030(16) 0.0179(16) -0.0092(16) C48 0.050(2) 0.0482(18) 0.044(2) -0.0080(15) 0.0097(16) -0.0146(16) C49 0.044(2) 0.063(2) 0.053(2) -0.0086(19) 0.0040(18) -0.0070(17) C50 0.043(2) 0.106(4) 0.079(3) 0.008(3) -0.002(2) -0.012(2) C51 0.064(3) 0.156(6) 0.071(3) -0.025(4) 0.004(3) -0.046(4) C52 0.095(4) 0.136(5) 0.090(4) -0.055(4) 0.022(3) -0.066(4) C53 0.068(3) 0.079(3) 0.085(3) -0.045(3) 0.028(2) -0.036(2) C54 0.055(2) 0.0334(15) 0.0446(19) -0.0030(13) 0.0149(16) -0.0001(14) C55 0.049(2) 0.0482(19) 0.051(2) -0.0144(16) 0.0091(17) -0.0059(16) C59 0.138(5) 0.045(2) 0.093(4) 0.011(2) 0.070(4) 0.021(3) C60 0.060(2) 0.051(2) 0.059(2) 0.0100(17) 0.024(2) -0.0058(17) C61 0.059(3) 0.105(4) 0.062(3) 0.005(3) 0.028(2) -0.016(2) C62 0.109(4) 0.053(2) 0.121(5) 0.032(3) 0.055(4) 0.004(3) O1 0.0277(11) 0.0319(10) 0.0376(12) 0.0030(9) 0.0043(9) -0.0011(8) O2 0.0284(10) 0.0334(10) 0.0416(12) 0.0099(9) 0.0095(9) -0.0028(8) O3 0.0348(11) 0.0371(10) 0.0459(13) 0.0138(9) 0.0071(10) 0.0034(9) O4 0.0323(11) 0.0297(10) 0.0559(14) 0.0084(9) 0.0119(10) -0.0016(8) O5 0.0302(10) 0.0488(11) 0.0316(11) 0.0111(9) 0.0063(9) -0.0048(9) O6 0.0459(13) 0.0288(10) 0.0369(12) 0.0020(9) 0.0052(10) -0.0022(9) O7 0.0502(15) 0.0547(14) 0.0579(16) 0.0267(12) 0.0129(12) -0.0004(11) O8 0.0627(17) 0.0497(14) 0.0531(15) 0.0025(12) 0.0193(13) -0.0185(12) O9 0.0582(16) 0.100(3) 0.0415(13) -0.0139(14) 0.0014(12) -0.0019(15) O10 0.0311(12) 0.0610(15) 0.0772(19) 0.0032(14) 0.0104(12) 0.0061(11) Li1 0.050(3) 0.050(4) 0.040(3) 0.002(3) 0.001(2) 0.001(3) Li2 0.026(2) 0.063(3) 0.049(3) 0.015(4) 0.006(2) -0.007(3) Zn 0.02685(13) 0.03194(12) 0.02832(15) 0.00206(17) 0.00579(10) -0.00246(15) _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 O1 1.410(4) . ? C1 C11 1.534(4) . ? C1 C5 1.541(4) . ? C1 C2 1.560(4) . ? C2 O3 1.440(3) . ? C2 C3 1.544(4) . ? C3 O4 1.449(3) . ? C3 C4 1.560(4) . ? C4 O2 1.401(3) . ? C4 C17 1.533(4) . ? C4 C23 1.553(4) . ? C5 C10 1.381(5) . ? C5 C6 1.401(5) . ? C6 C7 1.387(5) . ? C7 C8 1.363(6) . ? C8 C9 1.405(7) . ? C9 C10 1.387(5) . ? C11 C12 1.388(5) . ? C11 C16 1.393(4) . ? C12 C13 1.385(5) . ? C13 C14 1.361(6) . ? C14 C15 1.383(6) . ? C15 C16 1.401(5) . ? C17 C22 1.376(5) . ? C17 C18 1.399(5) . ? C18 C19 1.409(6) . ? C19 C20 1.367(7) . ? C20 C21 1.344(6) . ? C21 C22 1.399(5) . ? C23 C24 1.381(4) . ? C23 C28 1.390(4) . ? C24 C25 1.389(5) . ? C25 C26 1.382(5) . ? C26 C27 1.380(5) . ? C27 C28 1.396(5) . ? C29 O4 1.411(4) . ? C29 O3 1.436(4) . ? C29 C31 1.516(5) . ? C29 C30 1.519(5) . ? C32 O5 1.406(3) . ? C32 C42 1.536(4) . ? C32 C36 1.539(4) . ? C32 C33 1.542(5) . ? C33 O7 1.441(4) . ? C33 C34 1.551(5) . ? C34 O8 1.438(4) . ? C34 C35 1.567(5) . ? C35 O6 1.398(4) . ? C35 C54 1.535(5) . ? C35 C48 1.544(5) . ? C36 C37 1.381(6) . ? C36 C41 1.394(6) . ? C37 C38 1.384(7) . ? C38 C39 1.395(8) . ? C39 C40 1.355(8) . ? C40 C41 1.399(7) . ? C42 C43 1.384(5) . ? C42 C47 1.388(5) . ? C43 C44 1.405(5) . ? C44 C45 1.382(7) . ? C45 C46 1.375(7) . ? C46 C47 1.374(6) . ? C48 C49 1.389(6) . ? C48 C53 1.393(5) . ? C49 C50 1.385(6) . ? C49 Li1 2.729(8) . ? C50 C51 1.348(8) . ? C51 C52 1.370(10) . ? C52 C53 1.412(8) . ? C54 C55 1.377(5) . ? C54 C59 1.388(5) . ? C55 C56 1.392(6) . ? C56 C57 1.365(7) . ? C57 C58 1.375(8) . ? C58 C59 1.394(8) . ? C60 O7 1.414(5) . ? C60 O8 1.419(5) . ? C60 C61 1.515(6) . ? C60 C62 1.528(6) . ? C63 O9 1.409(7) . ? C63 C64 1.512(8) . ? C64 C65 1.470(9) . ? C65 C66 1.456(9) . ? C66 O9 1.399(7) . ? C67 O10 1.429(6) . ? C67 C68B 1.465(18) . ? C67 C68A 1.476(11) . ? C68A C69A 1.549(12) . ? C69A C70 1.557(9) . ? C68B C69B 1.28(2) . ? C69B C70 1.424(18) . ? C70 O10 1.415(5) . ? C71 C72 1.524(14) . ? C72 C73 1.351(9) . ? C72 C77 1.354(10) . ? C73 C74 1.312(8) . ? C74 C75 1.334(9) . ? C75 C76 1.417(10) . ? C76 C77 1.407(11) . ? O1 Li1 1.857(7) . ? O1 Zn 1.922(2) . ? O2 Li2 1.860(6) . ? O2 Zn 1.9234(19) . ? O5 Li2 1.886(5) . ? O5 Zn 1.918(2) . ? O6 Li1 1.875(6) . ? O6 Zn 1.920(2) . ? O9 Li1 1.870(6) . ? O10 Li2 1.894(7) . ? Li1 Zn 2.682(5) . ? Li2 Zn 2.696(5) . ? 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 O1 C1 C11 111.5(2) . . ? O1 C1 C5 104.7(2) . . ? C11 C1 C5 108.9(2) . . ? O1 C1 C2 108.1(2) . . ? C11 C1 C2 110.9(2) . . ? C5 C1 C2 112.5(3) . . ? O3 C2 C3 103.8(2) . . ? O3 C2 C1 109.9(2) . . ? C3 C2 C1 118.1(2) . . ? O4 C3 C2 102.2(2) . . ? O4 C3 C4 106.5(2) . . ? C2 C3 C4 123.5(3) . . ? O2 C4 C17 110.8(2) . . ? O2 C4 C23 105.4(2) . . ? C17 C4 C23 112.0(2) . . ? O2 C4 C3 108.9(2) . . ? C17 C4 C3 113.5(2) . . ? C23 C4 C3 105.8(2) . . ? C10 C5 C6 118.3(3) . . ? C10 C5 C1 125.1(3) . . ? C6 C5 C1 116.5(3) . . ? C7 C6 C5 121.5(4) . . ? C8 C7 C6 120.2(4) . . ? C7 C8 C9 118.9(4) . . ? C10 C9 C8 121.1(4) . . ? C5 C10 C9 120.0(4) . . ? C12 C11 C16 117.2(3) . . ? C12 C11 C1 121.6(3) . . ? C16 C11 C1 121.1(3) . . ? C13 C12 C11 122.0(3) . . ? C14 C13 C12 120.2(4) . . ? C13 C14 C15 119.8(4) . . ? C14 C15 C16 119.9(3) . . ? C11 C16 C15 120.8(3) . . ? C22 C17 C18 117.4(3) . . ? C22 C17 C4 125.0(3) . . ? C18 C17 C4 117.5(3) . . ? C17 C18 C19 120.3(4) . . ? C20 C19 C18 120.3(4) . . ? C21 C20 C19 119.8(4) . . ? C20 C21 C22 120.9(4) . . ? C17 C22 C21 121.3(4) . . ? C24 C23 C28 117.4(3) . . ? C24 C23 C4 118.9(3) . . ? C28 C23 C4 123.6(3) . . ? C23 C24 C25 122.7(3) . . ? C26 C25 C24 118.9(3) . . ? C27 C26 C25 120.0(3) . . ? C26 C27 C28 120.2(3) . . ? C23 C28 C27 120.9(3) . . ? O4 C29 O3 105.2(2) . . ? O4 C29 C31 108.1(3) . . ? O3 C29 C31 109.9(3) . . ? O4 C29 C30 110.4(3) . . ? O3 C29 C30 110.5(3) . . ? C31 C29 C30 112.5(3) . . ? O5 C32 C42 111.7(2) . . ? O5 C32 C36 104.3(2) . . ? C42 C32 C36 109.0(3) . . ? O5 C32 C33 109.2(2) . . ? C42 C32 C33 110.6(2) . . ? C36 C32 C33 111.8(3) . . ? O7 C33 C32 109.8(3) . . ? O7 C33 C34 103.8(3) . . ? C32 C33 C34 118.5(3) . . ? O8 C34 C33 102.9(3) . . ? O8 C34 C35 107.1(3) . . ? C33 C34 C35 121.0(3) . . ? O6 C35 C54 110.0(3) . . ? O6 C35 C48 105.3(3) . . ? C54 C35 C48 113.8(3) . . ? O6 C35 C34 109.5(3) . . ? C54 C35 C34 111.0(3) . . ? C48 C35 C34 106.9(3) . . ? C37 C36 C41 118.8(4) . . ? C37 C36 C32 116.3(3) . . ? C41 C36 C32 124.8(4) . . ? C36 C37 C38 122.2(5) . . ? C37 C38 C39 117.1(5) . . ? C40 C39 C38 122.7(6) . . ? C39 C40 C41 119.2(6) . . ? C36 C41 C40 120.0(5) . . ? C43 C42 C47 118.3(3) . . ? C43 C42 C32 120.6(3) . . ? C47 C42 C32 121.1(3) . . ? C42 C43 C44 120.6(4) . . ? C45 C44 C43 119.2(4) . . ? C46 C45 C44 120.6(4) . . ? C47 C46 C45 119.5(4) . . ? C46 C47 C42 121.8(4) . . ? C49 C48 C53 117.1(4) . . ? C49 C48 C35 117.6(3) . . ? C53 C48 C35 125.2(4) . . ? C50 C49 C48 122.0(4) . . ? C50 C49 Li1 116.8(4) . . ? C48 C49 Li1 88.6(3) . . ? C51 C50 C49 120.9(6) . . ? C50 C51 C52 119.1(5) . . ? C51 C52 C53 121.2(5) . . ? C48 C53 C52 119.7(5) . . ? C55 C54 C59 117.7(4) . . ? C55 C54 C35 119.9(3) . . ? C59 C54 C35 122.4(4) . . ? C54 C55 C56 122.7(4) . . ? C57 C56 C55 119.1(5) . . ? C56 C57 C58 119.3(6) . . ? C57 C58 C59 121.7(6) . . ? C54 C59 C58 119.4(5) . . ? O7 C60 O8 106.3(3) . . ? O7 C60 C61 110.8(4) . . ? O8 C60 C61 110.3(4) . . ? O7 C60 C62 109.2(4) . . ? O8 C60 C62 107.2(4) . . ? C61 C60 C62 112.8(4) . . ? O9 C63 C64 105.4(5) . . ? C65 C64 C63 103.6(5) . . ? C66 C65 C64 104.6(6) . . ? O9 C66 C65 109.8(6) . . ? O10 C67 C68B 107.1(8) . . ? O10 C67 C68A 107.0(5) . . ? C68B C67 C68A 26.1(7) . . ? C67 C68A C69A 104.8(7) . . ? C68A C69A C70 102.5(6) . . ? C69B C68B C67 106.5(14) . . ? C68B C69B C70 113.6(16) . . ? O10 C70 C69B 105.1(8) . . ? O10 C70 C69A 103.2(4) . . ? C69B C70 C69A 27.8(8) . . ? C73 C72 C77 120.1(7) . . ? C73 C72 C71 118.6(8) . . ? C77 C72 C71 121.2(8) . . ? C74 C73 C72 121.6(7) . . ? C73 C74 C75 122.7(7) . . ? C74 C75 C76 118.1(8) . . ? C77 C76 C75 118.4(8) . . ? C72 C77 C76 119.0(8) . . ? C1 O1 Li1 125.2(3) . . ? C1 O1 Zn 138.72(18) . . ? Li1 O1 Zn 90.4(2) . . ? C4 O2 Li2 134.3(3) . . ? C4 O2 Zn 132.20(17) . . ? Li2 O2 Zn 90.90(18) . . ? C29 O3 C2 110.1(2) . . ? C29 O4 C3 107.6(2) . . ? C32 O5 Li2 126.1(3) . . ? C32 O5 Zn 138.24(19) . . ? Li2 O5 Zn 90.29(18) . . ? C35 O6 Li1 130.8(3) . . ? C35 O6 Zn 134.0(2) . . ? Li1 O6 Zn 90.0(2) . . ? C60 O7 C33 111.0(3) . . ? C60 O8 C34 109.4(3) . . ? C66 O9 C63 108.7(5) . . ? C66 O9 Li1 118.7(4) . . ? C63 O9 Li1 131.6(4) . . ? C70 O10 C67 106.1(4) . . ? C70 O10 Li2 128.7(3) . . ? C67 O10 Li2 122.6(4) . . ? O1 Li1 O9 129.2(4) . . ? O1 Li1 O6 90.3(3) . . ? O9 Li1 O6 117.3(4) . . ? O1 Li1 Zn 45.78(14) . . ? O9 Li1 Zn 132.5(3) . . ? O6 Li1 Zn 45.70(14) . . ? O1 Li1 C49 122.5(3) . . ? O9 Li1 C49 107.1(3) . . ? O6 Li1 C49 71.1(2) . . ? Zn Li1 C49 105.1(2) . . ? O2 Li2 O5 90.1(2) . . ? O2 Li2 O10 119.7(3) . . ? O5 Li2 O10 129.3(4) . . ? O2 Li2 Zn 45.50(12) . . ? O5 Li2 Zn 45.33(12) . . ? O10 Li2 Zn 136.5(4) . . ? O5 Zn O6 108.80(9) . . ? O5 Zn O1 139.93(10) . . ? O6 Zn O1 87.04(9) . . ? O5 Zn O2 87.26(9) . . ? O6 Zn O2 133.94(10) . . ? O1 Zn O2 108.27(9) . . ? O5 Zn Li1 145.39(15) . . ? O6 Zn Li1 44.35(16) . . ? O1 Zn Li1 43.81(16) . . ? O2 Zn Li1 126.62(15) . . ? O5 Zn Li2 44.38(13) . . ? O6 Zn Li2 128.83(19) . . ? O1 Zn Li2 143.34(18) . . ? O2 Zn Li2 43.60(14) . . ? Li1 Zn Li2 164.06(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.653 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.054 #==============================================================================