# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_3 _database_code_depnum_ccdc_archive 'CCDC 830650' #TrackingRef '- comp3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H77 O16 Zn4' _chemical_formula_weight 1820.12 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.302(3) _cell_length_b 14.733(3) _cell_length_c 23.048(5) _cell_angle_alpha 103.534(14) _cell_angle_beta 98.096(8) _cell_angle_gamma 105.510(16) _cell_volume 4441.1(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6855 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description block-shaped _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1874 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15230 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 21.97 _reflns_number_total 9746 _reflns_number_gt 6049 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _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^)+(0.0958P)^2^+4.8510P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9746 _refine_ls_number_parameters 1099 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1631 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.4844(9) 0.3855(7) 0.7208(4) 0.072(3) Uani 1 1 d . . . C2 C 0.4928(8) 0.4372(7) 0.6690(4) 0.073(3) Uani 1 1 d . . . C3 C 0.4137(8) 0.4137(7) 0.6198(4) 0.070(3) Uani 1 1 d . . . C4 C 0.3260(8) 0.3362(8) 0.6105(5) 0.083(3) Uani 1 1 d . . . H4 H 0.3200 0.2975 0.6383 0.100 Uiso 1 1 calc R . . C5 C 0.2505(8) 0.3160(8) 0.5629(5) 0.093(3) Uani 1 1 d . . . H5 H 0.1911 0.2643 0.5583 0.112 Uiso 1 1 calc R . . C6 C 0.2575(9) 0.3700(9) 0.5196(5) 0.093(3) Uani 1 1 d . . . H6 H 0.2040 0.3544 0.4857 0.112 Uiso 1 1 calc R . . C7 C 0.3420(9) 0.4444(8) 0.5274(4) 0.082(3) Uani 1 1 d . . . H7 H 0.3468 0.4800 0.4979 0.098 Uiso 1 1 calc R . . C8 C 0.4227(8) 0.4716(7) 0.5770(4) 0.077(3) Uani 1 1 d . . . C9 C 0.5085(8) 0.5455(7) 0.5863(4) 0.075(3) Uani 1 1 d . . . H9 H 0.5133 0.5833 0.5579 0.090 Uiso 1 1 calc R . . C10 C 0.5882(8) 0.5697(7) 0.6334(4) 0.073(3) Uani 1 1 d . . . C11 C 0.6765(9) 0.6445(7) 0.6406(4) 0.089(3) Uani 1 1 d . . . H11 H 0.6810 0.6809 0.6115 0.107 Uiso 1 1 calc R . . C12 C 0.7557(9) 0.6677(8) 0.6869(5) 0.102(4) Uani 1 1 d . . . H12 H 0.8143 0.7197 0.6907 0.122 Uiso 1 1 calc R . . C13 C 0.7488(9) 0.6116(7) 0.7303(4) 0.088(3) Uani 1 1 d . . . H13 H 0.8042 0.6262 0.7629 0.105 Uiso 1 1 calc R . . C14 C 0.6659(9) 0.5391(7) 0.7257(4) 0.083(3) Uani 1 1 d . . . H14 H 0.6631 0.5033 0.7550 0.099 Uiso 1 1 calc R . . C15 C 0.5815(8) 0.5149(7) 0.6771(4) 0.073(3) Uani 1 1 d . . . C16 C 0.1796(8) 0.2015(8) 0.7032(6) 0.074(3) Uani 1 1 d . . . C17 C 0.0707(8) 0.1852(7) 0.6792(4) 0.073(3) Uani 1 1 d . . . C18 C 0.0018(7) 0.0899(7) 0.6692(4) 0.071(3) Uani 1 1 d . . . C19 C 0.0302(7) 0.0122(7) 0.6834(4) 0.073(3) Uani 1 1 d . . . H19 H 0.0977 0.0221 0.7009 0.087 Uiso 1 1 calc R . . C20 C -0.0398(9) -0.0787(8) 0.6720(5) 0.088(3) Uani 1 1 d . . . H20 H -0.0198 -0.1310 0.6814 0.105 Uiso 1 1 calc R . . C21 C -0.1393(9) -0.0945(8) 0.6469(5) 0.095(3) Uani 1 1 d . . . H21 H -0.1862 -0.1579 0.6383 0.114 Uiso 1 1 calc R . . C22 C -0.1696(8) -0.0202(7) 0.6346(4) 0.080(3) Uani 1 1 d . . . H22 H -0.2378 -0.0317 0.6182 0.095 Uiso 1 1 calc R . . C23 C -0.1014(8) 0.0738(8) 0.6457(4) 0.073(3) Uani 1 1 d . . . C24 C -0.1315(8) 0.1497(8) 0.6317(4) 0.080(3) Uani 1 1 d . . . H24 H -0.1996 0.1377 0.6146 0.096 Uiso 1 1 calc R . . C25 C -0.0649(8) 0.2422(7) 0.6422(4) 0.074(3) Uani 1 1 d . . . C26 C -0.0977(9) 0.3198(9) 0.6292(5) 0.097(3) Uani 1 1 d . . . H26 H -0.1657 0.3070 0.6115 0.116 Uiso 1 1 calc R . . C27 C -0.0333(10) 0.4115(10) 0.6419(6) 0.110(4) Uani 1 1 d . . . H27 H -0.0565 0.4631 0.6340 0.132 Uiso 1 1 calc R . . C28 C 0.0688(9) 0.4304(8) 0.6670(6) 0.100(3) Uani 1 1 d . . . H28 H 0.1142 0.4944 0.6751 0.120 Uiso 1 1 calc R . . C29 C 0.1023(8) 0.3569(8) 0.6797(5) 0.086(3) Uani 1 1 d . . . H29 H 0.1707 0.3712 0.6974 0.103 Uiso 1 1 calc R . . C30 C 0.0389(8) 0.2620(7) 0.6674(4) 0.070(3) Uani 1 1 d . . . C31 C 0.2634(7) 0.2010(10) 0.8890(4) 0.075(3) Uani 1 1 d . . . C32 C 0.1932(10) 0.2152(8) 0.9316(5) 0.092(3) Uani 1 1 d . . . C33 C 0.0957(9) 0.2123(8) 0.9086(5) 0.094(3) Uani 1 1 d . . . C34 C 0.0587(11) 0.1941(9) 0.8455(6) 0.113(4) Uani 1 1 d . . . H34 H 0.0992 0.1811 0.8173 0.135 Uiso 1 1 calc R . . C35 C -0.0354(12) 0.1952(11) 0.8249(7) 0.135(5) Uani 1 1 d . . . H35 H -0.0572 0.1889 0.7828 0.162 Uiso 1 1 calc R . . C36 C -0.0987(12) 0.2051(13) 0.8634(7) 0.161(6) Uani 1 1 d . . . H36 H -0.1653 0.2007 0.8476 0.193 Uiso 1 1 calc R . . C37 C -0.0652(12) 0.2217(13) 0.9267(8) 0.153(6) Uani 1 1 d . . . H37 H -0.1095 0.2295 0.9532 0.184 Uiso 1 1 calc R . . C38 C 0.0316(11) 0.2268(10) 0.9513(6) 0.116(4) Uani 1 1 d . . . C39 C 0.0710(11) 0.2475(10) 1.0134(6) 0.114(4) Uani 1 1 d . . . H39 H 0.0307 0.2617 1.0416 0.136 Uiso 1 1 calc R . . C40 C 0.1634(11) 0.2481(8) 1.0353(5) 0.093(3) Uani 1 1 d . . . C41 C 0.2021(11) 0.2693(9) 1.0981(5) 0.115(4) Uani 1 1 d . . . H41 H 0.1609 0.2821 1.1258 0.138 Uiso 1 1 calc R . . C42 C 0.2958(13) 0.2723(11) 1.1207(6) 0.130(5) Uani 1 1 d . . . H42 H 0.3198 0.2885 1.1636 0.156 Uiso 1 1 calc R . . C43 C 0.3591(11) 0.2507(9) 1.0793(6) 0.118(4) Uani 1 1 d . . . H43 H 0.4235 0.2481 1.0943 0.141 Uiso 1 1 calc R . . C44 C 0.3249(10) 0.2342(8) 1.0187(5) 0.101(4) Uani 1 1 d . . . H44 H 0.3678 0.2236 0.9917 0.121 Uiso 1 1 calc R . . C45 C 0.2299(10) 0.2323(7) 0.9947(5) 0.088(3) Uani 1 1 d . . . C46 C 0.5244(8) 0.1363(6) 0.6542(5) 0.065(2) Uani 1 1 d . . . C47 C 0.5744(7) 0.1092(7) 0.6040(4) 0.068(2) Uani 1 1 d . . . C48 C 0.5778(7) 0.0114(7) 0.5857(4) 0.073(3) Uani 1 1 d . . . C49 C 0.5436(7) -0.0603(7) 0.6176(4) 0.072(3) Uani 1 1 d . . . H49 H 0.5182 -0.0423 0.6530 0.086 Uiso 1 1 calc R . . C50 C 0.5476(7) -0.1516(8) 0.5977(5) 0.082(3) Uani 1 1 d . . . H50 H 0.5257 -0.1971 0.6199 0.099 Uiso 1 1 calc R . . C51 C 0.5841(7) -0.1833(7) 0.5434(4) 0.077(3) Uani 1 1 d . . . H51 H 0.5861 -0.2487 0.5299 0.092 Uiso 1 1 calc R . . C52 C 0.6149(7) -0.1179(7) 0.5128(4) 0.075(3) Uani 1 1 d . . . H52 H 0.6376 -0.1387 0.4767 0.090 Uiso 1 1 calc R . . C53 C 0.6153(7) -0.0203(7) 0.5319(4) 0.069(2) Uani 1 1 d . . . C54 C 0.6505(7) 0.0509(8) 0.5022(4) 0.078(3) Uani 1 1 d . . . H54 H 0.6761 0.0317 0.4670 0.094 Uiso 1 1 calc R . . C55 C 0.6503(8) 0.1461(7) 0.5206(4) 0.076(3) Uani 1 1 d . . . C56 C 0.6884(7) 0.2171(8) 0.4888(4) 0.079(3) Uani 1 1 d . . . H56 H 0.7146 0.1984 0.4538 0.095 Uiso 1 1 calc R . . C57 C 0.6863(7) 0.3092(8) 0.5089(4) 0.080(3) Uani 1 1 d . . . H57 H 0.7102 0.3546 0.4871 0.095 Uiso 1 1 calc R . . C58 C 0.6498(8) 0.3418(7) 0.5617(4) 0.081(3) Uani 1 1 d . . . H58 H 0.6512 0.4082 0.5759 0.098 Uiso 1 1 calc R . . C59 C 0.6126(7) 0.2746(7) 0.5913(4) 0.075(3) Uani 1 1 d . . . H59 H 0.5866 0.2952 0.6260 0.090 Uiso 1 1 calc R . . C60 C 0.6111(7) 0.1763(7) 0.5725(4) 0.069(3) Uani 1 1 d . . . C61 C 0.5656(10) 0.1216(8) 0.8703(4) 0.080(3) Uani 1 1 d . . . C62 C 0.6394(8) 0.0806(7) 0.9002(4) 0.080(3) Uani 1 1 d . . . C63 C 0.6971(9) 0.0379(9) 0.8670(5) 0.096(3) Uani 1 1 d . . . C64 C 0.6864(10) 0.0246(9) 0.8021(5) 0.107(4) Uani 1 1 d . . . H64 H 0.6408 0.0493 0.7817 0.129 Uiso 1 1 calc R . . C65 C 0.7408(12) -0.0231(12) 0.7694(6) 0.148(6) Uani 1 1 d . . . H65 H 0.7311 -0.0336 0.7265 0.178 Uiso 1 1 calc R . . C66 C 0.8105(12) -0.0561(12) 0.7997(7) 0.150(6) Uani 1 1 d . . . H66 H 0.8526 -0.0833 0.7776 0.180 Uiso 1 1 calc R . . C67 C 0.8200(12) -0.0504(12) 0.8609(8) 0.148(6) Uani 1 1 d . . . H67 H 0.8647 -0.0777 0.8799 0.177 Uiso 1 1 calc R . . C68 C 0.7624(10) -0.0033(10) 0.8957(6) 0.110(4) Uani 1 1 d . . . C69 C 0.7707(10) 0.0026(9) 0.9567(6) 0.107(4) Uani 1 1 d . . . H69 H 0.8171 -0.0229 0.9758 0.128 Uiso 1 1 calc R . . C70 C 0.7130(9) 0.0448(8) 0.9911(5) 0.091(3) Uani 1 1 d . . . C71 C 0.7172(10) 0.0501(9) 1.0552(5) 0.098(4) Uani 1 1 d . . . H71 H 0.7628 0.0252 1.0755 0.118 Uiso 1 1 calc R . . C72 C 0.6587(10) 0.0891(9) 1.0860(5) 0.100(4) Uani 1 1 d . . . H72 H 0.6630 0.0905 1.1278 0.120 Uiso 1 1 calc R . . C73 C 0.5920(9) 0.1275(8) 1.0591(5) 0.092(3) Uani 1 1 d . . . H73 H 0.5517 0.1554 1.0825 0.111 Uiso 1 1 calc R . . C74 C 0.5833(8) 0.1259(7) 0.9986(4) 0.081(3) Uani 1 1 d . . . H74 H 0.5375 0.1533 0.9809 0.097 Uiso 1 1 calc R . . C75 C 0.6415(7) 0.0840(7) 0.9624(5) 0.076(3) Uani 1 1 d . . . C76 C 0.2975(7) -0.0653(7) 0.7110(5) 0.075(3) Uani 1 1 d . . . C77 C 0.2820(9) -0.1719(8) 0.6873(5) 0.082(3) Uani 1 1 d . . . C78 C 0.2005(9) -0.2295(9) 0.6404(5) 0.086(3) Uani 1 1 d . . . C79 C 0.1300(9) -0.1928(9) 0.6133(5) 0.099(3) Uani 1 1 d . . . H79 H 0.1392 -0.1243 0.6272 0.119 Uiso 1 1 calc R . . C80 C 0.0495(11) -0.2495(10) 0.5684(6) 0.133(5) Uani 1 1 d . . . H80 H 0.0025 -0.2214 0.5528 0.160 Uiso 1 1 calc R . . C81 C 0.0356(12) -0.3538(11) 0.5444(7) 0.157(6) Uani 1 1 d . . . H81 H -0.0193 -0.3955 0.5124 0.188 Uiso 1 1 calc R . . C82 C 0.1046(12) -0.3886(10) 0.5696(7) 0.119(4) Uani 1 1 d . . . H82 H 0.0963 -0.4566 0.5539 0.143 Uiso 1 1 calc R . . C83 C 0.1856(9) -0.3341(9) 0.6160(5) 0.087(3) Uani 1 1 d . . . C84 C 0.2555(10) -0.3707(8) 0.6429(6) 0.093(3) Uani 1 1 d . . . H84 H 0.2455 -0.4393 0.6286 0.112 Uiso 1 1 calc R . . C85 C 0.3376(10) -0.3155(9) 0.6883(5) 0.093(3) Uani 1 1 d . . . C86 C 0.4072(11) -0.3565(10) 0.7118(6) 0.112(4) Uani 1 1 d . . . H86 H 0.3973 -0.4250 0.6970 0.135 Uiso 1 1 calc R . . C87 C 0.4856(12) -0.3004(11) 0.7539(7) 0.121(4) Uani 1 1 d . . . H87 H 0.5342 -0.3281 0.7677 0.145 Uiso 1 1 calc R . . C88 C 0.4993(10) -0.2020(10) 0.7787(5) 0.113(4) Uani 1 1 d . . . H88 H 0.5551 -0.1641 0.8110 0.135 Uiso 1 1 calc R . . C89 C 0.4341(10) -0.1576(8) 0.7579(5) 0.090(3) Uani 1 1 d . . . H89 H 0.4459 -0.0891 0.7744 0.108 Uiso 1 1 calc R . . C90 C 0.3486(9) -0.2149(8) 0.7113(5) 0.082(3) Uani 1 1 d . . . C91 C 0.2362(12) 0.4396(10) 0.8661(6) 0.130(5) Uani 1 1 d . . . H91A H 0.1826 0.3824 0.8377 0.156 Uiso 1 1 calc R . . H91B H 0.2442 0.4297 0.9073 0.156 Uiso 1 1 calc R . . C92 C 0.2111(15) 0.5312(14) 0.8678(10) 0.195(8) Uani 1 1 d . . . H92A H 0.1448 0.5169 0.8416 0.234 Uiso 1 1 calc R . . H92B H 0.2113 0.5663 0.9101 0.234 Uiso 1 1 calc R . . C93 C 0.2881(18) 0.5888(14) 0.8448(11) 0.209(8) Uani 1 1 d U . . H93A H 0.3273 0.6497 0.8774 0.251 Uiso 1 1 calc R . . H93B H 0.2572 0.6079 0.8103 0.251 Uiso 1 1 calc R . . C94 C 0.3552(13) 0.5323(10) 0.8239(7) 0.149(6) Uani 1 1 d U . . H94A H 0.3442 0.5133 0.7788 0.179 Uiso 1 1 calc R . . H94B H 0.4257 0.5723 0.8413 0.179 Uiso 1 1 calc R . . C95 C 0.5300(11) 0.3560(10) 0.9295(5) 0.132(5) Uani 1 1 d U . . H95A H 0.4682 0.3584 0.9436 0.158 Uiso 1 1 calc R . . H95B H 0.5347 0.2889 0.9246 0.158 Uiso 1 1 calc R . . C96 C 0.6058(17) 0.4189(13) 0.9693(7) 0.235(9) Uani 1 1 d U . . H96A H 0.6612 0.3909 0.9734 0.282 Uiso 1 1 calc R . . H96B H 0.5882 0.4357 1.0097 0.282 Uiso 1 1 calc R . . C97 C 0.6364(14) 0.5096(12) 0.9480(7) 0.201(8) Uani 1 1 d U . . H97A H 0.6203 0.5646 0.9740 0.242 Uiso 1 1 calc R . . H97B H 0.7087 0.5300 0.9495 0.242 Uiso 1 1 calc R . . C98 C 0.5781(11) 0.4809(9) 0.8834(6) 0.135(5) Uani 1 1 d U . . H98A H 0.5307 0.5185 0.8799 0.162 Uiso 1 1 calc R . . H98B H 0.6230 0.4928 0.8550 0.162 Uiso 1 1 calc R . . C99 C 0.7730(13) 0.3841(14) 0.8528(9) 0.194(8) Uani 1 1 d U . . H99A H 0.7839 0.3441 0.8806 0.233 Uiso 1 1 calc R . . H99B H 0.7420 0.4320 0.8728 0.233 Uiso 1 1 calc R . . C100 C 0.8711(13) 0.4385(13) 0.8427(9) 0.177(7) Uani 1 1 d U . . H10A H 0.9263 0.4255 0.8670 0.213 Uiso 1 1 calc R . . H10B H 0.8817 0.5102 0.8543 0.213 Uiso 1 1 calc R . . C101 C 0.8641(12) 0.3993(12) 0.7756(9) 0.151(6) Uani 1 1 d . . . H10C H 0.8691 0.4526 0.7557 0.181 Uiso 1 1 calc R . . H10D H 0.9186 0.3713 0.7687 0.181 Uiso 1 1 calc R . . C102 C 0.7656(10) 0.3214(10) 0.7499(6) 0.115(4) Uani 1 1 d . . . H10E H 0.7292 0.3342 0.7144 0.138 Uiso 1 1 calc R . . H10F H 0.7749 0.2561 0.7362 0.138 Uiso 1 1 calc R . . O1 O 0.4085(4) 0.1998(4) 0.7767(2) 0.0707(17) Uani 1 1 d . . . O2 O 0.4112(5) 0.3870(5) 0.7442(3) 0.0773(18) Uani 1 1 d . . . O3 O 0.5492(5) 0.3457(5) 0.7330(3) 0.0745(17) Uani 1 1 d . . . O4 O 0.2189(5) 0.2591(5) 0.7553(3) 0.0823(19) Uani 1 1 d . . . O5 O 0.2215(5) 0.1519(5) 0.6686(3) 0.0763(18) Uani 1 1 d . . . O6 O 0.3097(5) 0.2813(5) 0.8789(3) 0.0865(19) Uani 1 1 d . . . O7 O 0.2675(6) 0.1200(5) 0.8683(3) 0.087(2) Uani 1 1 d . . . O8 O 0.5658(5) 0.1486(4) 0.7088(3) 0.0781(18) Uani 1 1 d . . . O9 O 0.4396(5) 0.1447(4) 0.6387(2) 0.0690(16) Uani 1 1 d . . . O10 O 0.6020(5) 0.1920(5) 0.8499(3) 0.0807(18) Uani 1 1 d . . . O11 O 0.4763(6) 0.0839(5) 0.8674(3) 0.085(2) Uani 1 1 d . . . O12 O 0.3114(5) -0.0134(4) 0.6742(3) 0.0809(18) Uani 1 1 d . . . O13 O 0.2984(5) -0.0323(4) 0.7652(3) 0.0780(18) Uani 1 1 d . . . O14 O 0.3323(6) 0.4504(5) 0.8444(3) 0.098(2) Uani 1 1 d . . . O15 O 0.5266(6) 0.3784(5) 0.8702(3) 0.101(2) Uani 1 1 d . . . O16 O 0.7096(6) 0.3240(6) 0.7990(3) 0.101(2) Uani 1 1 d . . . Zn1 Zn 0.36156(9) 0.31555(8) 0.80454(5) 0.0743(4) Uani 1 1 d . . . Zn2 Zn 0.55413(9) 0.24858(8) 0.78277(5) 0.0739(4) Uani 1 1 d . . . Zn3 Zn 0.34709(8) 0.13109(8) 0.69264(5) 0.0706(4) Uani 1 1 d . . . Zn4 Zn 0.36477(9) 0.10390(8) 0.81924(5) 0.0743(4) 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 0.095(9) 0.073(7) 0.049(6) 0.022(5) 0.025(6) 0.020(6) C2 0.095(8) 0.069(6) 0.062(6) 0.028(5) 0.018(6) 0.028(6) C3 0.085(8) 0.068(6) 0.064(6) 0.030(5) 0.024(6) 0.021(6) C4 0.081(8) 0.107(8) 0.073(7) 0.050(6) 0.018(6) 0.026(7) C5 0.082(8) 0.096(8) 0.108(9) 0.057(7) 0.032(7) 0.009(6) C6 0.080(8) 0.112(9) 0.086(8) 0.042(7) 0.009(6) 0.020(7) C7 0.105(9) 0.091(8) 0.069(7) 0.043(6) 0.026(7) 0.042(7) C8 0.090(8) 0.088(7) 0.059(6) 0.039(5) 0.009(6) 0.028(6) C9 0.086(8) 0.072(7) 0.063(6) 0.029(5) 0.011(6) 0.013(6) C10 0.096(8) 0.060(6) 0.064(6) 0.024(5) 0.015(6) 0.022(6) C11 0.106(9) 0.078(7) 0.064(6) 0.037(5) -0.002(6) -0.005(7) C12 0.112(10) 0.094(8) 0.088(8) 0.043(7) 0.006(7) 0.006(7) C13 0.112(9) 0.077(7) 0.066(6) 0.031(5) 0.003(6) 0.018(7) C14 0.103(9) 0.074(7) 0.069(7) 0.031(5) 0.019(6) 0.014(6) C15 0.094(8) 0.070(6) 0.058(6) 0.025(5) 0.013(6) 0.024(6) C16 0.071(8) 0.083(8) 0.086(8) 0.056(7) 0.022(7) 0.024(6) C17 0.087(8) 0.069(7) 0.067(6) 0.031(5) 0.028(6) 0.014(6) C18 0.070(8) 0.094(8) 0.064(6) 0.037(5) 0.026(5) 0.032(6) C19 0.076(7) 0.073(7) 0.064(6) 0.029(5) -0.002(5) 0.015(6) C20 0.094(9) 0.085(8) 0.083(7) 0.038(6) 0.006(7) 0.020(7) C21 0.092(10) 0.094(8) 0.090(8) 0.042(6) 0.009(7) 0.004(7) C22 0.092(8) 0.081(7) 0.064(6) 0.030(5) 0.014(5) 0.017(7) C23 0.070(8) 0.093(8) 0.065(6) 0.035(5) 0.022(5) 0.024(6) C24 0.082(8) 0.092(8) 0.073(6) 0.034(6) 0.014(6) 0.028(7) C25 0.072(8) 0.066(7) 0.088(7) 0.031(5) 0.022(6) 0.019(6) C26 0.074(8) 0.089(8) 0.124(10) 0.035(7) 0.014(7) 0.021(7) C27 0.086(10) 0.104(10) 0.155(12) 0.058(8) 0.023(8) 0.037(8) C28 0.091(10) 0.073(7) 0.134(10) 0.035(7) 0.027(8) 0.012(6) C29 0.069(7) 0.085(8) 0.120(9) 0.046(6) 0.032(6) 0.029(6) C30 0.080(8) 0.059(6) 0.065(6) 0.026(5) 0.017(5) 0.007(5) C31 0.073(7) 0.107(9) 0.049(6) 0.035(6) 0.024(5) 0.018(7) C32 0.113(10) 0.095(8) 0.078(8) 0.044(6) 0.028(8) 0.031(7) C33 0.080(9) 0.118(9) 0.085(9) 0.038(7) 0.035(7) 0.018(7) C34 0.105(11) 0.148(11) 0.076(9) 0.031(7) 0.029(8) 0.021(9) C35 0.110(12) 0.195(15) 0.111(11) 0.072(10) 0.033(10) 0.032(11) C36 0.126(13) 0.245(19) 0.109(12) 0.069(12) 0.050(11) 0.027(12) C37 0.103(12) 0.253(19) 0.128(13) 0.087(13) 0.049(10) 0.055(12) C38 0.110(11) 0.155(12) 0.096(10) 0.058(8) 0.028(9) 0.038(9) C39 0.122(12) 0.164(12) 0.082(9) 0.054(8) 0.042(8) 0.063(10) C40 0.122(11) 0.098(8) 0.074(8) 0.038(6) 0.037(8) 0.038(7) C41 0.143(13) 0.161(12) 0.067(8) 0.052(8) 0.033(8) 0.070(10) C42 0.168(15) 0.189(14) 0.070(8) 0.046(8) 0.046(10) 0.098(12) C43 0.158(13) 0.130(11) 0.095(10) 0.043(8) 0.030(9) 0.083(9) C44 0.138(12) 0.126(10) 0.051(7) 0.030(6) 0.022(7) 0.057(8) C45 0.108(10) 0.078(7) 0.084(8) 0.031(6) 0.025(8) 0.031(6) C46 0.074(7) 0.058(6) 0.081(8) 0.036(5) 0.032(6) 0.026(5) C47 0.073(7) 0.076(7) 0.064(6) 0.030(5) 0.011(5) 0.030(5) C48 0.069(7) 0.098(8) 0.068(6) 0.044(6) 0.015(5) 0.035(6) C49 0.093(8) 0.065(6) 0.068(6) 0.030(5) 0.011(5) 0.036(5) C50 0.089(8) 0.083(8) 0.073(7) 0.040(6) -0.003(6) 0.018(6) C51 0.095(8) 0.070(6) 0.064(6) 0.021(5) -0.006(6) 0.033(6) C52 0.099(8) 0.078(7) 0.059(6) 0.027(5) 0.011(5) 0.040(6) C53 0.070(7) 0.080(7) 0.066(6) 0.033(5) 0.015(5) 0.025(5) C54 0.076(7) 0.108(9) 0.055(6) 0.037(6) 0.014(5) 0.023(6) C55 0.105(8) 0.067(7) 0.065(6) 0.038(5) 0.006(6) 0.033(6) C56 0.093(8) 0.093(8) 0.076(7) 0.046(6) 0.032(6) 0.045(6) C57 0.093(8) 0.088(8) 0.075(7) 0.048(6) 0.026(6) 0.032(6) C58 0.112(9) 0.085(7) 0.065(6) 0.037(5) 0.027(6) 0.044(6) C59 0.093(8) 0.078(7) 0.064(6) 0.038(5) 0.010(5) 0.029(5) C60 0.098(8) 0.064(6) 0.055(6) 0.033(5) 0.013(5) 0.027(5) C61 0.098(9) 0.102(8) 0.050(6) 0.043(6) 0.023(6) 0.024(7) C62 0.088(8) 0.100(8) 0.069(7) 0.054(6) 0.015(6) 0.033(6) C63 0.105(9) 0.139(10) 0.085(8) 0.060(7) 0.042(7) 0.071(8) C64 0.128(11) 0.142(11) 0.076(8) 0.051(7) 0.031(7) 0.059(9) C65 0.196(16) 0.215(16) 0.097(10) 0.076(11) 0.059(11) 0.126(14) C66 0.187(16) 0.200(16) 0.140(13) 0.094(12) 0.077(12) 0.126(13) C67 0.166(15) 0.191(15) 0.148(13) 0.115(12) 0.037(12) 0.096(12) C68 0.120(11) 0.146(11) 0.105(10) 0.061(8) 0.049(8) 0.074(9) C69 0.127(11) 0.119(10) 0.093(9) 0.060(8) 0.014(8) 0.047(8) C70 0.109(9) 0.090(8) 0.087(8) 0.052(6) 0.018(7) 0.032(7) C71 0.111(10) 0.119(9) 0.077(8) 0.063(7) 0.015(7) 0.027(8) C72 0.109(10) 0.104(9) 0.078(8) 0.051(7) 0.007(8) 0.004(7) C73 0.112(9) 0.098(8) 0.072(7) 0.043(6) 0.022(6) 0.025(7) C74 0.100(8) 0.078(7) 0.065(7) 0.041(5) 0.008(6) 0.017(6) C75 0.076(7) 0.078(7) 0.081(7) 0.039(6) 0.015(6) 0.021(6) C76 0.096(8) 0.077(7) 0.053(6) 0.025(6) 0.017(6) 0.022(6) C77 0.105(9) 0.085(8) 0.062(6) 0.032(6) 0.029(7) 0.025(7) C78 0.091(9) 0.094(9) 0.079(7) 0.026(7) 0.028(7) 0.029(7) C79 0.093(9) 0.097(8) 0.080(8) 0.010(6) -0.011(7) 0.012(7) C80 0.120(12) 0.111(11) 0.129(11) -0.006(9) -0.017(9) 0.029(9) C81 0.129(14) 0.106(12) 0.159(14) -0.033(10) -0.038(11) 0.012(10) C82 0.110(11) 0.095(9) 0.128(12) 0.004(8) 0.020(10) 0.018(9) C83 0.086(9) 0.093(9) 0.070(7) 0.015(6) 0.017(7) 0.015(7) C84 0.106(10) 0.084(8) 0.099(9) 0.032(7) 0.040(8) 0.030(8) C85 0.101(10) 0.095(9) 0.081(8) 0.030(7) 0.032(7) 0.021(8) C86 0.128(12) 0.103(10) 0.108(10) 0.030(8) 0.004(9) 0.051(9) C87 0.148(14) 0.127(12) 0.103(10) 0.036(9) 0.021(10) 0.068(10) C88 0.163(13) 0.099(10) 0.086(8) 0.024(7) 0.026(8) 0.059(9) C89 0.144(11) 0.076(7) 0.068(7) 0.034(6) 0.034(8) 0.044(8) C90 0.122(10) 0.075(8) 0.068(7) 0.035(6) 0.038(7) 0.042(7) C91 0.156(14) 0.117(11) 0.122(11) 0.025(8) 0.030(10) 0.055(10) C92 0.19(2) 0.144(16) 0.28(2) 0.073(15) 0.121(18) 0.057(14) C93 0.25(2) 0.134(15) 0.27(2) 0.077(15) 0.055(18) 0.081(15) C94 0.227(17) 0.086(10) 0.159(13) 0.057(9) 0.054(12) 0.064(10) C95 0.161(12) 0.122(10) 0.078(8) 0.062(8) -0.012(8) -0.019(9) C96 0.31(2) 0.167(13) 0.101(11) 0.052(10) -0.017(13) -0.104(14) C97 0.249(17) 0.157(13) 0.121(11) 0.061(10) 0.010(12) -0.067(12) C98 0.163(13) 0.110(10) 0.114(10) 0.058(8) -0.014(9) 0.011(9) C99 0.132(14) 0.209(18) 0.160(15) -0.018(13) 0.005(13) -0.006(13) C100 0.113(13) 0.181(16) 0.185(17) 0.030(13) 0.017(13) -0.012(11) C101 0.114(13) 0.155(14) 0.193(18) 0.082(13) 0.034(12) 0.028(11) C102 0.104(10) 0.146(11) 0.102(9) 0.057(8) 0.033(8) 0.027(9) O1 0.091(5) 0.069(4) 0.055(3) 0.034(3) 0.004(3) 0.021(3) O2 0.084(5) 0.094(5) 0.071(4) 0.044(4) 0.028(4) 0.033(4) O3 0.086(5) 0.086(5) 0.062(4) 0.037(3) 0.022(3) 0.027(4) O4 0.091(5) 0.091(5) 0.065(4) 0.023(4) 0.018(4) 0.027(4) O5 0.072(5) 0.092(5) 0.064(4) 0.032(4) 0.012(4) 0.016(4) O6 0.113(6) 0.087(5) 0.066(4) 0.030(4) 0.030(4) 0.029(4) O7 0.124(6) 0.073(5) 0.080(5) 0.028(4) 0.043(4) 0.041(4) O8 0.103(5) 0.095(5) 0.047(4) 0.038(3) 0.010(3) 0.036(4) O9 0.088(5) 0.084(4) 0.051(4) 0.033(3) 0.027(3) 0.035(4) O10 0.093(5) 0.099(5) 0.058(4) 0.043(4) 0.016(4) 0.025(4) O11 0.097(6) 0.094(5) 0.075(4) 0.054(4) 0.017(4) 0.025(4) O12 0.106(5) 0.084(4) 0.061(4) 0.029(4) 0.018(4) 0.035(4) O13 0.092(5) 0.073(4) 0.072(5) 0.030(3) 0.023(4) 0.019(4) O14 0.107(6) 0.105(6) 0.096(5) 0.042(4) 0.034(5) 0.037(5) O15 0.130(6) 0.083(5) 0.078(5) 0.041(4) 0.002(4) 0.010(4) O16 0.098(6) 0.137(6) 0.074(5) 0.062(5) 0.012(5) 0.021(5) Zn1 0.0892(9) 0.0795(8) 0.0590(7) 0.0323(6) 0.0173(6) 0.0225(6) Zn2 0.0855(9) 0.0845(8) 0.0581(7) 0.0386(6) 0.0144(6) 0.0218(6) Zn3 0.0813(8) 0.0787(7) 0.0565(6) 0.0315(5) 0.0132(6) 0.0228(6) Zn4 0.0905(9) 0.0782(8) 0.0601(7) 0.0350(6) 0.0182(6) 0.0214(6) _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 O2 1.246(11) . ? C1 O3 1.255(11) . ? C1 C2 1.562(12) . ? C2 C3 1.390(13) . ? C2 C15 1.418(13) . ? C3 C4 1.402(13) . ? C3 C8 1.445(12) . ? C4 C5 1.341(13) . ? C4 H4 0.9500 . ? C5 C6 1.414(13) . ? C5 H5 0.9500 . ? C6 C7 1.354(13) . ? C6 H6 0.9500 . ? C7 C8 1.403(13) . ? C7 H7 0.9500 . ? C8 C9 1.356(13) . ? C9 C10 1.364(12) . ? C9 H9 0.9500 . ? C10 C11 1.396(13) . ? C10 C15 1.427(12) . ? C11 C12 1.348(13) . ? C11 H11 0.9500 . ? C12 C13 1.439(13) . ? C12 H12 0.9500 . ? C13 C14 1.338(13) . ? C13 H13 0.9500 . ? C14 C15 1.429(13) . ? C14 H14 0.9500 . ? C16 O4 1.247(12) . ? C16 O5 1.274(12) . ? C16 C17 1.512(13) . ? C17 C30 1.396(12) . ? C17 C18 1.428(13) . ? C18 C19 1.404(12) . ? C18 C23 1.434(12) . ? C19 C20 1.381(13) . ? C19 H19 0.9500 . ? C20 C21 1.394(14) . ? C20 H20 0.9500 . ? C21 C22 1.354(13) . ? C21 H21 0.9500 . ? C22 C23 1.405(13) . ? C22 H22 0.9500 . ? C23 C24 1.387(12) . ? C24 C25 1.383(13) . ? C24 H24 0.9500 . ? C25 C26 1.421(13) . ? C25 C30 1.439(13) . ? C26 C27 1.355(14) . ? C26 H26 0.9500 . ? C27 C28 1.420(15) . ? C27 H27 0.9500 . ? C28 C29 1.370(13) . ? C28 H28 0.9500 . ? C29 C30 1.386(13) . ? C29 H29 0.9500 . ? C31 O7 1.198(12) . ? C31 O6 1.283(11) . ? C31 C32 1.520(14) . ? C32 C33 1.406(15) . ? C32 C45 1.413(14) . ? C33 C34 1.412(15) . ? C33 C38 1.454(16) . ? C34 C35 1.368(16) . ? C34 H34 0.9500 . ? C35 C36 1.367(18) . ? C35 H35 0.9500 . ? C36 C37 1.411(19) . ? C36 H36 0.9500 . ? C37 C38 1.395(17) . ? C37 H37 0.9500 . ? C38 C39 1.392(16) . ? C39 C40 1.343(15) . ? C39 H39 0.9500 . ? C40 C41 1.402(15) . ? C40 C45 1.451(14) . ? C41 C42 1.353(16) . ? C41 H41 0.9500 . ? C42 C43 1.445(16) . ? C42 H42 0.9500 . ? C43 C44 1.355(14) . ? C43 H43 0.9500 . ? C44 C45 1.383(15) . ? C44 H44 0.9500 . ? C46 O8 1.262(11) . ? C46 O9 1.263(10) . ? C46 C47 1.476(12) . ? C47 C60 1.395(12) . ? C47 C48 1.419(12) . ? C48 C49 1.443(12) . ? C48 C53 1.446(12) . ? C49 C50 1.335(12) . ? C49 H49 0.9500 . ? C50 C51 1.448(13) . ? C50 H50 0.9500 . ? C51 C52 1.341(12) . ? C51 H51 0.9500 . ? C52 C53 1.401(12) . ? C52 H52 0.9500 . ? C53 C54 1.405(12) . ? C54 C55 1.368(12) . ? C54 H54 0.9500 . ? C55 C60 1.419(12) . ? C55 C56 1.448(12) . ? C56 C57 1.336(12) . ? C56 H56 0.9500 . ? C57 C58 1.422(13) . ? C57 H57 0.9500 . ? C58 C59 1.366(12) . ? C58 H58 0.9500 . ? C59 C60 1.405(12) . ? C59 H59 0.9500 . ? C61 O11 1.234(11) . ? C61 O10 1.255(11) . ? C61 C62 1.512(13) . ? C62 C63 1.377(13) . ? C62 C75 1.418(13) . ? C63 C68 1.410(14) . ? C63 C64 1.443(14) . ? C64 C65 1.369(16) . ? C64 H64 0.9500 . ? C65 C66 1.392(17) . ? C65 H65 0.9500 . ? C66 C67 1.379(18) . ? C66 H66 0.9500 . ? C67 C68 1.426(17) . ? C67 H67 0.9500 . ? C68 C69 1.376(15) . ? C69 C70 1.388(15) . ? C69 H69 0.9500 . ? C70 C71 1.451(14) . ? C70 C75 1.456(13) . ? C71 C72 1.330(15) . ? C71 H71 0.9500 . ? C72 C73 1.379(14) . ? C72 H72 0.9500 . ? C73 C74 1.376(13) . ? C73 H73 0.9500 . ? C74 C75 1.415(13) . ? C74 H74 0.9500 . ? C76 O13 1.227(10) . ? C76 O12 1.270(10) . ? C76 C77 1.480(13) . ? C77 C78 1.389(14) . ? C77 C90 1.397(14) . ? C78 C79 1.405(14) . ? C78 C83 1.457(14) . ? C79 C80 1.357(15) . ? C79 H79 0.9500 . ? C80 C81 1.454(17) . ? C80 H80 0.9500 . ? C81 C82 1.350(17) . ? C81 H81 0.9500 . ? C82 C83 1.372(16) . ? C82 H82 0.9500 . ? C83 C84 1.394(15) . ? C84 C85 1.372(15) . ? C84 H84 0.9500 . ? C85 C86 1.404(15) . ? C85 C90 1.409(14) . ? C86 C87 1.305(17) . ? C86 H86 0.9500 . ? C87 C88 1.377(16) . ? C87 H87 0.9500 . ? C88 C89 1.370(14) . ? C88 H88 0.9500 . ? C89 C90 1.420(15) . ? C89 H89 0.9500 . ? C91 C92 1.480(19) . ? C91 O14 1.510(14) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C93 1.44(2) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.49(2) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 O14 1.373(13) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.289(17) . ? C95 O15 1.475(11) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.508(19) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.504(17) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 O15 1.429(13) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 O16 1.373(16) . ? C99 C100 1.50(2) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 C101 1.50(2) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.495(17) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 O16 1.475(13) . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? O1 Zn3 1.917(6) . ? O1 Zn4 1.923(5) . ? O1 Zn2 1.986(6) . ? O1 Zn1 1.999(6) . ? O2 Zn1 2.028(6) . ? O3 Zn2 2.042(6) . ? O4 Zn1 2.035(7) . ? O5 Zn3 1.929(7) . ? O6 Zn1 2.075(6) . ? O7 Zn4 1.939(7) . ? O8 Zn2 2.035(6) . ? O9 Zn3 1.942(6) . ? O10 Zn2 2.042(6) . ? O11 Zn4 1.941(7) . ? O12 Zn3 1.977(6) . ? O13 Zn4 1.989(6) . ? O14 Zn1 2.160(7) . ? O15 Zn1 2.427(7) . ? O15 Zn2 2.588(8) . ? O16 Zn2 2.137(8) . ? Zn2 Zn3 3.1501(18) . ? Zn3 Zn4 3.0219(15) . ? 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 O2 C1 O3 127.8(8) . . ? O2 C1 C2 114.7(10) . . ? O3 C1 C2 117.4(9) . . ? C3 C2 C15 121.5(8) . . ? C3 C2 C1 121.4(9) . . ? C15 C2 C1 116.9(9) . . ? C2 C3 C4 122.3(8) . . ? C2 C3 C8 118.4(9) . . ? C4 C3 C8 119.3(9) . . ? C5 C4 C3 120.9(9) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.4(10) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 118.6(10) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C8 123.2(9) . . ? C6 C7 H7 118.4 . . ? C8 C7 H7 118.4 . . ? C9 C8 C7 124.8(9) . . ? C9 C8 C3 118.5(9) . . ? C7 C8 C3 116.7(10) . . ? C8 C9 C10 124.7(9) . . ? C8 C9 H9 117.7 . . ? C10 C9 H9 117.7 . . ? C9 C10 C11 123.2(9) . . ? C9 C10 C15 118.4(9) . . ? C11 C10 C15 118.4(9) . . ? C12 C11 C10 123.2(9) . . ? C12 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? C11 C12 C13 118.2(10) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C14 C13 C12 121.1(10) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 120.9(9) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C2 C15 C10 118.5(9) . . ? C2 C15 C14 123.2(8) . . ? C10 C15 C14 118.2(9) . . ? O4 C16 O5 126.3(10) . . ? O4 C16 C17 117.5(10) . . ? O5 C16 C17 116.2(10) . . ? C30 C17 C18 121.1(10) . . ? C30 C17 C16 120.3(9) . . ? C18 C17 C16 118.5(8) . . ? C19 C18 C17 122.8(9) . . ? C19 C18 C23 118.5(9) . . ? C17 C18 C23 118.7(9) . . ? C20 C19 C18 120.1(10) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.9(10) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 120.4(10) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.9(10) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 121.2(10) . . ? C24 C23 C18 119.6(9) . . ? C22 C23 C18 119.1(9) . . ? C25 C24 C23 121.7(10) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 120.8(10) . . ? C24 C25 C30 120.3(9) . . ? C26 C25 C30 118.9(9) . . ? C27 C26 C25 120.9(11) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 119.8(11) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 120.5(10) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 121.5(10) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C29 C30 C17 123.0(10) . . ? C29 C30 C25 118.5(9) . . ? C17 C30 C25 118.5(8) . . ? O7 C31 O6 128.5(9) . . ? O7 C31 C32 118.9(10) . . ? O6 C31 C32 112.6(11) . . ? C33 C32 C45 121.6(11) . . ? C33 C32 C31 120.7(9) . . ? C45 C32 C31 117.7(11) . . ? C32 C33 C34 121.7(11) . . ? C32 C33 C38 118.6(11) . . ? C34 C33 C38 119.7(12) . . ? C35 C34 C33 120.1(12) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 121.5(14) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 120.0(15) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 121.5(14) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C39 C38 C37 124.5(14) . . ? C39 C38 C33 118.5(13) . . ? C37 C38 C33 117.0(12) . . ? C40 C39 C38 122.9(12) . . ? C40 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? C39 C40 C41 122.2(12) . . ? C39 C40 C45 120.8(11) . . ? C41 C40 C45 116.8(12) . . ? C42 C41 C40 122.8(12) . . ? C42 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? C41 C42 C43 119.6(12) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 118.6(12) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? C43 C44 C45 122.5(12) . . ? C43 C44 H44 118.7 . . ? C45 C44 H44 118.7 . . ? C44 C45 C32 123.1(11) . . ? C44 C45 C40 119.4(11) . . ? C32 C45 C40 117.4(11) . . ? O8 C46 O9 123.5(8) . . ? O8 C46 C47 120.3(9) . . ? O9 C46 C47 116.2(9) . . ? C60 C47 C48 120.8(9) . . ? C60 C47 C46 120.5(9) . . ? C48 C47 C46 118.5(8) . . ? C47 C48 C49 123.2(9) . . ? C47 C48 C53 119.5(8) . . ? C49 C48 C53 117.3(9) . . ? C50 C49 C48 120.5(9) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 122.1(9) . . ? C49 C50 H50 119.0 . . ? C51 C50 H50 119.0 . . ? C52 C51 C50 118.2(9) . . ? C52 C51 H51 120.9 . . ? C50 C51 H51 120.9 . . ? C51 C52 C53 122.8(9) . . ? C51 C52 H52 118.6 . . ? C53 C52 H52 118.6 . . ? C52 C53 C54 124.2(9) . . ? C52 C53 C48 119.2(8) . . ? C54 C53 C48 116.6(9) . . ? C55 C54 C53 124.2(9) . . ? C55 C54 H54 117.9 . . ? C53 C54 H54 117.9 . . ? C54 C55 C60 119.0(8) . . ? C54 C55 C56 122.2(10) . . ? C60 C55 C56 118.8(9) . . ? C57 C56 C55 119.5(9) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C58 122.7(9) . . ? C56 C57 H57 118.7 . . ? C58 C57 H57 118.7 . . ? C59 C58 C57 117.8(9) . . ? C59 C58 H58 121.1 . . ? C57 C58 H58 121.1 . . ? C58 C59 C60 122.8(9) . . ? C58 C59 H59 118.6 . . ? C60 C59 H59 118.6 . . ? C47 C60 C59 121.9(9) . . ? C47 C60 C55 119.8(9) . . ? C59 C60 C55 118.3(8) . . ? O11 C61 O10 125.6(10) . . ? O11 C61 C62 118.6(9) . . ? O10 C61 C62 115.7(10) . . ? C63 C62 C75 122.6(9) . . ? C63 C62 C61 120.7(8) . . ? C75 C62 C61 116.6(9) . . ? C62 C63 C68 119.3(10) . . ? C62 C63 C64 122.3(10) . . ? C68 C63 C64 118.1(11) . . ? C65 C64 C63 121.2(11) . . ? C65 C64 H64 119.4 . . ? C63 C64 H64 119.4 . . ? C64 C65 C66 119.5(13) . . ? C64 C65 H65 120.3 . . ? C66 C65 H65 120.3 . . ? C67 C66 C65 121.8(13) . . ? C67 C66 H66 119.1 . . ? C65 C66 H66 119.1 . . ? C66 C67 C68 119.6(12) . . ? C66 C67 H67 120.2 . . ? C68 C67 H67 120.2 . . ? C69 C68 C63 120.3(12) . . ? C69 C68 C67 120.3(12) . . ? C63 C68 C67 119.5(11) . . ? C68 C69 C70 121.5(11) . . ? C68 C69 H69 119.2 . . ? C70 C69 H69 119.2 . . ? C69 C70 C71 123.5(10) . . ? C69 C70 C75 119.7(10) . . ? C71 C70 C75 116.7(11) . . ? C72 C71 C70 121.5(11) . . ? C72 C71 H71 119.2 . . ? C70 C71 H71 119.2 . . ? C71 C72 C73 121.8(11) . . ? C71 C72 H72 119.1 . . ? C73 C72 H72 119.1 . . ? C74 C73 C72 120.6(11) . . ? C74 C73 H73 119.7 . . ? C72 C73 H73 119.7 . . ? C73 C74 C75 121.0(10) . . ? C73 C74 H74 119.5 . . ? C75 C74 H74 119.5 . . ? C74 C75 C62 125.2(9) . . ? C74 C75 C70 118.3(9) . . ? C62 C75 C70 116.4(10) . . ? O13 C76 O12 124.1(9) . . ? O13 C76 C77 118.1(8) . . ? O12 C76 C77 117.8(9) . . ? C78 C77 C90 119.8(10) . . ? C78 C77 C76 119.5(10) . . ? C90 C77 C76 120.7(10) . . ? C77 C78 C79 123.9(11) . . ? C77 C78 C83 119.9(10) . . ? C79 C78 C83 116.2(11) . . ? C80 C79 C78 123.7(12) . . ? C80 C79 H79 118.1 . . ? C78 C79 H79 118.1 . . ? C79 C80 C81 119.4(13) . . ? C79 C80 H80 120.3 . . ? C81 C80 H80 120.3 . . ? C82 C81 C80 116.8(13) . . ? C82 C81 H81 121.6 . . ? C80 C81 H81 121.6 . . ? C81 C82 C83 125.5(13) . . ? C81 C82 H82 117.2 . . ? C83 C82 H82 117.2 . . ? C82 C83 C84 125.4(12) . . ? C82 C83 C78 118.3(12) . . ? C84 C83 C78 116.3(11) . . ? C85 C84 C83 125.1(11) . . ? C85 C84 H84 117.4 . . ? C83 C84 H84 117.4 . . ? C84 C85 C86 122.2(12) . . ? C84 C85 C90 116.7(12) . . ? C86 C85 C90 121.1(12) . . ? C87 C86 C85 119.9(13) . . ? C87 C86 H86 120.1 . . ? C85 C86 H86 120.1 . . ? C86 C87 C88 121.5(13) . . ? C86 C87 H87 119.2 . . ? C88 C87 H87 119.2 . . ? C89 C88 C87 121.3(13) . . ? C89 C88 H88 119.3 . . ? C87 C88 H88 119.3 . . ? C88 C89 C90 119.4(10) . . ? C88 C89 H89 120.3 . . ? C90 C89 H89 120.3 . . ? C77 C90 C85 122.0(12) . . ? C77 C90 C89 121.2(10) . . ? C85 C90 C89 116.7(10) . . ? C92 C91 O14 107.1(12) . . ? C92 C91 H91A 110.3 . . ? O14 C91 H91A 110.3 . . ? C92 C91 H91B 110.3 . . ? O14 C91 H91B 110.3 . . ? H91A C91 H91B 108.6 . . ? C93 C92 C91 104.6(15) . . ? C93 C92 H92A 110.8 . . ? C91 C92 H92A 110.8 . . ? C93 C92 H92B 110.8 . . ? C91 C92 H92B 110.8 . . ? H92A C92 H92B 108.9 . . ? C92 C93 C94 111.0(15) . . ? C92 C93 H93A 109.4 . . ? C94 C93 H93A 109.4 . . ? C92 C93 H93B 109.4 . . ? C94 C93 H93B 109.4 . . ? H93A C93 H93B 108.0 . . ? O14 C94 C93 106.2(14) . . ? O14 C94 H94A 110.5 . . ? C93 C94 H94A 110.5 . . ? O14 C94 H94B 110.5 . . ? C93 C94 H94B 110.5 . . ? H94A C94 H94B 108.7 . . ? C96 C95 O15 109.8(11) . . ? C96 C95 H95A 109.7 . . ? O15 C95 H95A 109.7 . . ? C96 C95 H95B 109.7 . . ? O15 C95 H95B 109.7 . . ? H95A C95 H95B 108.2 . . ? C95 C96 C97 108.1(15) . . ? C95 C96 H96A 110.1 . . ? C97 C96 H96A 110.1 . . ? C95 C96 H96B 110.1 . . ? C97 C96 H96B 110.1 . . ? H96A C96 H96B 108.4 . . ? C98 C97 C96 105.3(12) . . ? C98 C97 H97A 110.7 . . ? C96 C97 H97A 110.7 . . ? C98 C97 H97B 110.7 . . ? C96 C97 H97B 110.7 . . ? H97A C97 H97B 108.8 . . ? O15 C98 C97 104.5(9) . . ? O15 C98 H98A 110.9 . . ? C97 C98 H98A 110.9 . . ? O15 C98 H98B 110.9 . . ? C97 C98 H98B 110.9 . . ? H98A C98 H98B 108.9 . . ? O16 C99 C100 112.0(15) . . ? O16 C99 H99A 109.2 . . ? C100 C99 H99A 109.2 . . ? O16 C99 H99B 109.2 . . ? C100 C99 H99B 109.2 . . ? H99A C99 H99B 107.9 . . ? C99 C100 C101 104.3(14) . . ? C99 C100 H10A 110.9 . . ? C101 C100 H10A 110.9 . . ? C99 C100 H10B 110.9 . . ? C101 C100 H10B 110.9 . . ? H10A C100 H10B 108.9 . . ? C102 C101 C100 107.2(13) . . ? C102 C101 H10C 110.3 . . ? C100 C101 H10C 110.3 . . ? C102 C101 H10D 110.3 . . ? C100 C101 H10D 110.3 . . ? H10C C101 H10D 108.5 . . ? O16 C102 C101 107.1(11) . . ? O16 C102 H10E 110.3 . . ? C101 C102 H10E 110.3 . . ? O16 C102 H10F 110.3 . . ? C101 C102 H10F 110.3 . . ? H10E C102 H10F 108.5 . . ? Zn3 O1 Zn4 103.8(3) . . ? Zn3 O1 Zn2 107.6(3) . . ? Zn4 O1 Zn2 115.9(3) . . ? Zn3 O1 Zn1 110.4(3) . . ? Zn4 O1 Zn1 110.7(3) . . ? Zn2 O1 Zn1 108.2(3) . . ? C1 O2 Zn1 128.2(6) . . ? C1 O3 Zn2 131.3(6) . . ? C16 O4 Zn1 133.1(7) . . ? C16 O5 Zn3 126.2(6) . . ? C31 O6 Zn1 134.0(6) . . ? C31 O7 Zn4 118.6(6) . . ? C46 O8 Zn2 125.0(6) . . ? C46 O9 Zn3 119.6(5) . . ? C61 O10 Zn2 136.1(7) . . ? C61 O11 Zn4 127.4(6) . . ? C76 O12 Zn3 128.1(6) . . ? C76 O13 Zn4 128.4(6) . . ? C94 O14 C91 109.5(10) . . ? C94 O14 Zn1 124.5(8) . . ? C91 O14 Zn1 116.2(7) . . ? C98 O15 C95 106.8(8) . . ? C98 O15 Zn1 117.5(7) . . ? C95 O15 Zn1 113.5(7) . . ? C98 O15 Zn2 121.8(8) . . ? C95 O15 Zn2 115.6(7) . . ? Zn1 O15 Zn2 80.1(2) . . ? C99 O16 C102 108.4(11) . . ? C99 O16 Zn2 128.7(10) . . ? C102 O16 Zn2 122.8(7) . . ? O1 Zn1 O2 97.0(2) . . ? O1 Zn1 O4 99.3(3) . . ? O2 Zn1 O4 94.0(3) . . ? O1 Zn1 O6 98.4(2) . . ? O2 Zn1 O6 163.8(3) . . ? O4 Zn1 O6 88.4(3) . . ? O1 Zn1 O14 171.3(3) . . ? O2 Zn1 O14 83.4(3) . . ? O4 Zn1 O14 89.3(3) . . ? O6 Zn1 O14 80.7(3) . . ? O1 Zn1 O15 81.0(2) . . ? O2 Zn1 O15 90.7(2) . . ? O4 Zn1 O15 175.2(2) . . ? O6 Zn1 O15 86.9(3) . . ? O14 Zn1 O15 90.3(3) . . ? O1 Zn2 O8 99.5(3) . . ? O1 Zn2 O10 99.6(2) . . ? O8 Zn2 O10 99.2(2) . . ? O1 Zn2 O3 96.0(2) . . ? O8 Zn2 O3 90.9(2) . . ? O10 Zn2 O3 159.7(3) . . ? O1 Zn2 O16 170.2(3) . . ? O8 Zn2 O16 89.7(3) . . ? O10 Zn2 O16 81.9(3) . . ? O3 Zn2 O16 80.6(3) . . ? O1 Zn2 O15 77.2(2) . . ? O8 Zn2 O15 174.7(2) . . ? O10 Zn2 O15 85.6(2) . . ? O3 Zn2 O15 85.3(2) . . ? O16 Zn2 O15 93.3(3) . . ? O1 Zn2 Zn3 35.46(16) . . ? O8 Zn2 Zn3 67.62(19) . . ? O10 Zn2 Zn3 118.55(19) . . ? O3 Zn2 Zn3 81.52(19) . . ? O16 Zn2 Zn3 150.8(2) . . ? O15 Zn2 Zn3 108.08(17) . . ? O1 Zn3 O5 111.8(3) . . ? O1 Zn3 O9 112.9(3) . . ? O5 Zn3 O9 117.6(3) . . ? O1 Zn3 O12 113.8(2) . . ? O5 Zn3 O12 103.3(3) . . ? O9 Zn3 O12 96.1(3) . . ? O1 Zn3 Zn4 38.16(16) . . ? O5 Zn3 Zn4 109.11(19) . . ? O9 Zn3 Zn4 132.91(19) . . ? O12 Zn3 Zn4 78.27(17) . . ? O1 Zn3 Zn2 36.92(19) . . ? O5 Zn3 Zn2 138.0(2) . . ? O9 Zn3 Zn2 76.29(19) . . ? O12 Zn3 Zn2 114.91(19) . . ? Zn4 Zn3 Zn2 64.89(4) . . ? O1 Zn4 O7 118.3(3) . . ? O1 Zn4 O11 111.6(3) . . ? O7 Zn4 O11 109.6(3) . . ? O1 Zn4 O13 114.5(2) . . ? O7 Zn4 O13 101.1(3) . . ? O11 Zn4 O13 99.8(3) . . ? O1 Zn4 Zn3 38.03(17) . . ? O7 Zn4 Zn3 122.7(2) . . ? O11 Zn4 Zn3 127.4(2) . . ? O13 Zn4 Zn3 77.05(18) . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 0.510 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.069 data_4 _database_code_depnum_ccdc_archive 'CCDC 830651' #TrackingRef '- comp4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H56 O17 Zn4' _chemical_formula_weight 1238.55 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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.1389(9) _cell_length_b 11.6701(5) _cell_length_c 24.0951(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.427(2) _cell_angle_gamma 90.00 _cell_volume 5775.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4885 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 1.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13573 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 21.97 _reflns_number_total 7042 _reflns_number_gt 5152 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _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^)+(0.0265P)^2^+34.5402P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7042 _refine_ls_number_parameters 692 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.008 _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 0.3442(3) 0.7169(6) 0.3030(3) 0.0210(16) Uani 1 1 d . . . C2 C 0.3841(3) 0.6142(6) 0.3399(3) 0.0226(17) Uani 1 1 d . . . C3 C 0.4505(3) 0.6269(6) 0.3779(3) 0.0243(17) Uani 1 1 d . . . H3 H 0.4713 0.6974 0.3786 0.029 Uiso 1 1 calc R . . C4 C 0.4860(4) 0.5366(7) 0.4146(3) 0.0308(19) Uani 1 1 d . . . H4 H 0.5313 0.5455 0.4412 0.037 Uiso 1 1 calc R . . C5 C 0.4564(4) 0.4336(7) 0.4130(3) 0.0309(18) Uani 1 1 d . . . H5 H 0.4814 0.3717 0.4383 0.037 Uiso 1 1 calc R . . C6 C 0.3898(4) 0.4195(7) 0.3745(3) 0.0326(19) Uani 1 1 d . . . H6 H 0.3691 0.3482 0.3728 0.039 Uiso 1 1 calc R . . C7 C 0.3545(4) 0.5113(6) 0.3390(3) 0.0280(18) Uani 1 1 d . . . H7 H 0.3089 0.5034 0.3134 0.034 Uiso 1 1 calc R . . C8 C 0.2913(4) 1.1110(6) 0.1200(3) 0.0239(18) Uani 1 1 d . . . C9 C 0.3048(3) 1.1617(6) 0.0698(3) 0.0237(17) Uani 1 1 d . . . C10 C 0.3662(4) 1.1912(6) 0.0817(3) 0.0272(18) Uani 1 1 d . . . H10 H 0.4012 1.1766 0.1220 0.033 Uiso 1 1 calc R . . C11 C 0.3790(4) 1.2421(7) 0.0365(4) 0.039(2) Uani 1 1 d . . . H11 H 0.4222 1.2631 0.0459 0.046 Uiso 1 1 calc R . . C12 C 0.3285(4) 1.2617(7) -0.0223(4) 0.041(2) Uani 1 1 d . . . H12 H 0.3366 1.2974 -0.0534 0.049 Uiso 1 1 calc R . . C13 C 0.2656(4) 1.2292(6) -0.0360(3) 0.036(2) Uani 1 1 d . . . H13 H 0.2309 1.2402 -0.0769 0.043 Uiso 1 1 calc R . . C14 C 0.2535(4) 1.1804(6) 0.0105(3) 0.0333(19) Uani 1 1 d . . . H14 H 0.2104 1.1600 0.0017 0.040 Uiso 1 1 calc R . . C15 C 0.4185(3) 1.0748(5) 0.3600(3) 0.0211(16) Uani 1 1 d . . . C16 C 0.4858(3) 1.0844(6) 0.4126(3) 0.0208(17) Uani 1 1 d . . . C17 C 0.5376(3) 1.0383(6) 0.4076(3) 0.0296(18) Uani 1 1 d . . . H17 H 0.5312 1.0045 0.3693 0.035 Uiso 1 1 calc R . . C18 C 0.5991(4) 1.0406(7) 0.4578(3) 0.037(2) Uani 1 1 d . . . H18 H 0.6346 1.0086 0.4536 0.044 Uiso 1 1 calc R . . C19 C 0.6099(4) 1.0882(6) 0.5136(3) 0.0312(19) Uani 1 1 d . . . H19 H 0.6523 1.0878 0.5481 0.037 Uiso 1 1 calc R . . C20 C 0.5583(4) 1.1371(6) 0.5193(3) 0.0314(19) Uani 1 1 d . . . H20 H 0.5655 1.1717 0.5576 0.038 Uiso 1 1 calc R . . C21 C 0.4960(4) 1.1355(6) 0.4690(3) 0.0263(18) Uani 1 1 d . . . H21 H 0.4606 1.1689 0.4728 0.032 Uiso 1 1 calc R . . C22 C 0.1172(3) 0.8514(7) 0.1199(3) 0.0248(17) Uani 1 1 d . . . C23 C 0.0599(3) 0.7965(6) 0.0682(3) 0.0243(17) Uani 1 1 d . . . C24 C 0.0394(4) 0.6875(7) 0.0762(3) 0.0316(19) Uani 1 1 d . . . H24 H 0.0636 0.6466 0.1141 0.038 Uiso 1 1 calc R . . C25 C -0.0159(4) 0.6397(6) 0.0288(3) 0.0306(19) Uani 1 1 d . . . H25 H -0.0301 0.5660 0.0341 0.037 Uiso 1 1 calc R . . C26 C -0.0506(4) 0.6995(8) -0.0263(4) 0.045(2) Uani 1 1 d . . . H26 H -0.0893 0.6673 -0.0584 0.054 Uiso 1 1 calc R . . C27 C -0.0298(4) 0.8055(7) -0.0353(3) 0.037(2) Uani 1 1 d . . . H27 H -0.0530 0.8448 -0.0739 0.045 Uiso 1 1 calc R . . C28 C 0.0245(3) 0.8534(6) 0.0120(3) 0.0270(18) Uani 1 1 d . . . H28 H 0.0384 0.9271 0.0062 0.032 Uiso 1 1 calc R . . C29 C 0.2003(3) 0.9211(7) 0.3471(3) 0.0247(17) Uani 1 1 d . . . C30 C 0.1659(3) 0.9006(6) 0.3858(3) 0.0246(17) Uani 1 1 d . . . C31 C 0.1219(4) 0.8142(6) 0.3735(3) 0.0311(19) Uani 1 1 d . . . H31 H 0.1114 0.7671 0.3379 0.037 Uiso 1 1 calc R . . C32 C 0.0921(4) 0.7922(7) 0.4105(3) 0.0341(19) Uani 1 1 d . . . H32 H 0.0631 0.7294 0.4018 0.041 Uiso 1 1 calc R . . C33 C 0.1057(4) 0.8642(7) 0.4606(3) 0.032(2) Uani 1 1 d . . . H33 H 0.0843 0.8530 0.4857 0.039 Uiso 1 1 calc R . . C34 C 0.1499(4) 0.9519(8) 0.4744(3) 0.047(2) Uani 1 1 d . . . H34 H 0.1595 0.9993 0.5097 0.057 Uiso 1 1 calc R . . C35 C 0.1806(4) 0.9723(8) 0.4376(3) 0.041(2) Uani 1 1 d . . . H35 H 0.2109 1.0333 0.4472 0.049 Uiso 1 1 calc R . . C36 C 0.1851(4) 1.2417(6) 0.2397(3) 0.0280(18) Uani 1 1 d . . . C37 C 0.1492(4) 1.3483(6) 0.2388(3) 0.0288(18) Uani 1 1 d . . . C38 C 0.0868(4) 1.3668(6) 0.1904(3) 0.0325(19) Uani 1 1 d . . . H38 H 0.0667 1.3103 0.1588 0.039 Uiso 1 1 calc R . . C39 C 0.0542(4) 1.4676(7) 0.1883(3) 0.044(2) Uani 1 1 d . . . H39 H 0.0110 1.4786 0.1562 0.053 Uiso 1 1 calc R . . C40 C 0.0837(4) 1.5513(7) 0.2322(3) 0.039(2) Uani 1 1 d . . . H40 H 0.0614 1.6209 0.2298 0.047 Uiso 1 1 calc R . . C41 C 0.1467(4) 1.5343(7) 0.2806(3) 0.038(2) Uani 1 1 d . . . H41 H 0.1679 1.5930 0.3105 0.046 Uiso 1 1 calc R . . C42 C 0.1779(4) 1.4307(7) 0.2844(3) 0.0336(19) Uani 1 1 d . . . H42 H 0.2194 1.4165 0.3187 0.040 Uiso 1 1 calc R . . C43 C 0.2211(5) 0.5363(7) 0.1563(4) 0.052(2) Uani 1 1 d . . . H43A H 0.2076 0.5489 0.1894 0.062 Uiso 1 1 calc R A 1 H43B H 0.1848 0.5561 0.1150 0.062 Uiso 1 1 calc R A 1 C44 C 0.2462(4) 0.4164(7) 0.1578(4) 0.046(2) Uani 1 1 d . C . H44A H 0.2099 0.3615 0.1369 0.055 Uiso 1 1 calc R . . H44B H 0.2740 0.3908 0.2013 0.055 Uiso 1 1 calc R . . C45 C 0.2857(4) 0.4280(7) 0.1220(4) 0.044(2) Uani 1 1 d . . . H45A H 0.2591 0.4084 0.0773 0.053 Uiso 1 1 calc R C . H45B H 0.3246 0.3780 0.1401 0.053 Uiso 1 1 calc R . . C46 C 0.3052(4) 0.5554(7) 0.1300(5) 0.055(2) Uani 1 1 d . C . H46A H 0.3529 0.5626 0.1464 0.066 Uiso 1 1 calc R B 1 H46B H 0.2836 0.5948 0.0891 0.066 Uiso 1 1 calc R B 1 C47 C 0.2537(4) 0.8471(9) -0.0061(4) 0.058(3) Uani 1 1 d . . . H47A H 0.2232 0.9105 -0.0116 0.069 Uiso 1 1 calc R . . H47B H 0.2298 0.7737 -0.0139 0.069 Uiso 1 1 calc R . . C48 C 0.2822(4) 0.8606(8) -0.0504(4) 0.049(2) Uani 1 1 d . . . H48A H 0.2547 0.9116 -0.0856 0.059 Uiso 1 1 calc R . . H48B H 0.2861 0.7854 -0.0673 0.059 Uiso 1 1 calc R . . C49 C 0.3482(4) 0.9129(7) -0.0117(3) 0.035(2) Uani 1 1 d . . . H49A H 0.3460 0.9976 -0.0136 0.042 Uiso 1 1 calc R . . H49B H 0.3798 0.8865 -0.0260 0.042 Uiso 1 1 calc R . . C50 C 0.3665(4) 0.8700(6) 0.0537(3) 0.0305(19) Uani 1 1 d . . . H50A H 0.3925 0.7988 0.0625 0.037 Uiso 1 1 calc R . . H50B H 0.3922 0.9284 0.0852 0.037 Uiso 1 1 calc R . . C51 C 0.4792(3) 0.9755(6) 0.2245(3) 0.0260(18) Uani 1 1 d . . . H51A H 0.4834 1.0375 0.2541 0.031 Uiso 1 1 calc R . . H51B H 0.4667 1.0096 0.1829 0.031 Uiso 1 1 calc R . . C52 C 0.5427(3) 0.9099(6) 0.2472(3) 0.0295(18) Uani 1 1 d . . . H52A H 0.5661 0.9056 0.2934 0.035 Uiso 1 1 calc R . . H52B H 0.5715 0.9444 0.2316 0.035 Uiso 1 1 calc R . . C53 C 0.5179(4) 0.7925(6) 0.2181(4) 0.0354(19) Uani 1 1 d . . . H53A H 0.5086 0.7911 0.1736 0.042 Uiso 1 1 calc R . . H53B H 0.5500 0.7317 0.2410 0.042 Uiso 1 1 calc R . . C54 C 0.4564(4) 0.7777(6) 0.2244(4) 0.0331(19) Uani 1 1 d . . . H54A H 0.4245 0.7296 0.1900 0.040 Uiso 1 1 calc R . . H54B H 0.4660 0.7414 0.2648 0.040 Uiso 1 1 calc R . . O1 O 0.2659(2) 0.9773(4) 0.24179(19) 0.0231(11) Uani 1 1 d . . . O2 O 0.3740(2) 0.8006(4) 0.29634(19) 0.0256(11) Uani 1 1 d . . . O3 O 0.2833(2) 0.7070(4) 0.2810(2) 0.0287(12) Uani 1 1 d . . . O4 O 0.3380(2) 1.0700(4) 0.16854(19) 0.0238(11) Uani 1 1 d . . . O5 O 0.2319(2) 1.1111(4) 0.1094(2) 0.0274(12) Uani 1 1 d . . . O6 O 0.4119(2) 1.0396(4) 0.30807(19) 0.0233(11) Uani 1 1 d . . . O7 O 0.3715(2) 1.1026(4) 0.37130(19) 0.0235(11) Uani 1 1 d . . . O8 O 0.1514(2) 0.7883(4) 0.1671(2) 0.0270(12) Uani 1 1 d . . . O9 O 0.1288(2) 0.9537(4) 0.1138(2) 0.0275(12) Uani 1 1 d . . . O10 O 0.1837(2) 0.8543(4) 0.3008(2) 0.0323(13) Uani 1 1 d . . . O11 O 0.2413(2) 1.0008(4) 0.3619(2) 0.0304(12) Uani 1 1 d . . . O12 O 0.1621(2) 1.1798(4) 0.1911(2) 0.0281(12) Uani 1 1 d . . . O13 O 0.2361(2) 1.2207(4) 0.2895(2) 0.0295(12) Uani 1 1 d . . . O14 O 0.2902(3) 0.8356(4) 0.1575(2) 0.0271(13) Uani 1 1 d . . . O16 O 0.3061(3) 0.8488(6) 0.0548(2) 0.0585(18) Uani 1 1 d . . . O17 O 0.4316(2) 0.8927(4) 0.2210(2) 0.0251(12) Uani 1 1 d . . . Zn1 Zn 0.34752(4) 0.94133(7) 0.23394(3) 0.0200(2) Uani 1 1 d . . . Zn2 Zn 0.22489(4) 0.83593(7) 0.24538(3) 0.0225(2) Uani 1 1 d . . . Zn3 Zn 0.20265(4) 1.05194(7) 0.16673(3) 0.0218(2) Uani 1 1 d . . . Zn4 Zn 0.28126(4) 1.07100(7) 0.31280(3) 0.0218(2) Uani 1 1 d . . . O15 O 0.2869(8) 0.6038(15) 0.1702(6) 0.039(5) Uani 0.50 1 d P C 1 O15A O 0.2537(8) 0.6106(14) 0.1407(7) 0.039(4) Uani 0.50 1 d P C 2 H14A H 0.295(4) 0.838(7) 0.127(4) 0.047 Uiso 1 1 d . . . H14B H 0.281(4) 0.773(7) 0.160(4) 0.047 Uiso 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 0.018(5) 0.023(5) 0.021(4) 0.004(3) 0.008(3) 0.007(4) C2 0.026(5) 0.023(4) 0.024(4) -0.005(3) 0.016(3) -0.008(4) C3 0.024(4) 0.024(4) 0.029(4) 0.003(3) 0.016(4) 0.005(4) C4 0.027(4) 0.044(5) 0.022(4) 0.007(4) 0.012(3) 0.003(4) C5 0.033(5) 0.023(5) 0.043(5) 0.006(4) 0.023(4) 0.007(4) C6 0.048(6) 0.024(5) 0.032(4) 0.002(4) 0.024(4) 0.004(4) C7 0.034(5) 0.021(4) 0.030(4) 0.000(3) 0.017(4) -0.001(4) C8 0.041(5) 0.015(4) 0.016(4) -0.004(3) 0.015(4) -0.003(4) C9 0.032(5) 0.014(4) 0.032(4) 0.005(3) 0.021(4) 0.001(4) C10 0.033(5) 0.022(4) 0.030(4) 0.004(3) 0.018(4) 0.004(4) C11 0.044(5) 0.043(5) 0.043(5) 0.013(4) 0.032(4) 0.008(4) C12 0.052(6) 0.041(5) 0.048(5) 0.023(4) 0.039(5) 0.011(5) C13 0.049(6) 0.025(5) 0.033(4) 0.009(4) 0.017(4) 0.012(4) C14 0.033(5) 0.033(5) 0.037(5) 0.004(4) 0.018(4) 0.000(4) C15 0.026(4) 0.006(4) 0.030(4) 0.003(3) 0.011(4) -0.001(3) C16 0.024(4) 0.024(4) 0.019(4) 0.010(3) 0.013(3) 0.002(3) C17 0.031(5) 0.029(5) 0.030(4) -0.004(4) 0.016(4) 0.001(4) C18 0.030(5) 0.052(6) 0.035(5) 0.010(4) 0.020(4) 0.008(4) C19 0.023(4) 0.033(5) 0.022(4) 0.007(3) -0.002(3) -0.006(4) C20 0.034(5) 0.033(5) 0.027(4) 0.002(3) 0.014(4) -0.003(4) C21 0.033(5) 0.021(4) 0.023(4) 0.004(3) 0.011(4) -0.007(4) C22 0.023(4) 0.028(5) 0.027(4) -0.007(4) 0.015(4) -0.001(4) C23 0.027(4) 0.020(4) 0.027(4) -0.011(3) 0.014(4) -0.006(4) C24 0.034(5) 0.035(5) 0.031(4) -0.005(4) 0.019(4) -0.006(4) C25 0.039(5) 0.024(5) 0.034(4) -0.008(4) 0.022(4) -0.014(4) C26 0.028(5) 0.065(7) 0.038(5) -0.018(5) 0.012(4) -0.013(5) C27 0.036(5) 0.037(5) 0.032(4) -0.003(4) 0.010(4) 0.001(4) C28 0.020(4) 0.027(5) 0.030(4) 0.000(4) 0.009(4) 0.001(4) C29 0.027(4) 0.030(5) 0.019(4) 0.004(4) 0.012(3) 0.006(4) C30 0.019(4) 0.036(5) 0.022(4) 0.006(3) 0.012(3) 0.003(4) C31 0.036(5) 0.025(5) 0.033(4) 0.002(4) 0.017(4) 0.010(4) C32 0.029(5) 0.033(5) 0.052(5) 0.004(4) 0.028(4) 0.001(4) C33 0.036(5) 0.034(5) 0.036(5) 0.014(4) 0.025(4) 0.012(4) C34 0.058(6) 0.061(6) 0.033(5) -0.007(4) 0.030(4) -0.010(5) C35 0.039(5) 0.052(6) 0.038(5) 0.002(4) 0.023(4) -0.008(4) C36 0.028(5) 0.030(5) 0.027(4) -0.007(4) 0.014(4) -0.004(4) C37 0.039(5) 0.026(5) 0.021(4) 0.001(3) 0.013(4) 0.008(4) C38 0.040(5) 0.022(5) 0.030(4) -0.001(3) 0.011(4) 0.001(4) C39 0.047(5) 0.038(6) 0.033(5) -0.006(4) 0.006(4) 0.012(5) C40 0.043(5) 0.031(5) 0.038(5) 0.005(4) 0.015(4) 0.014(4) C41 0.047(6) 0.033(5) 0.040(5) -0.010(4) 0.026(4) 0.000(4) C42 0.041(5) 0.029(5) 0.031(4) 0.006(4) 0.017(4) 0.007(4) C43 0.085(7) 0.037(6) 0.053(5) 0.002(4) 0.049(5) -0.009(5) C44 0.062(6) 0.028(5) 0.048(5) 0.000(4) 0.026(5) -0.002(5) C45 0.049(6) 0.026(5) 0.049(5) -0.005(4) 0.016(4) 0.006(4) C46 0.044(6) 0.035(6) 0.088(7) -0.002(5) 0.033(5) 0.007(5) C47 0.041(6) 0.082(8) 0.045(5) -0.007(5) 0.014(5) -0.016(5) C48 0.054(6) 0.056(6) 0.034(5) 0.003(4) 0.017(4) -0.005(5) C49 0.038(5) 0.034(5) 0.035(4) -0.001(4) 0.019(4) -0.009(4) C50 0.033(5) 0.026(5) 0.036(4) -0.001(3) 0.019(4) -0.007(4) C51 0.027(4) 0.025(4) 0.034(4) 0.000(3) 0.021(3) -0.003(4) C52 0.030(5) 0.021(4) 0.043(4) -0.001(3) 0.021(4) -0.002(4) C53 0.044(5) 0.019(4) 0.052(5) 0.009(4) 0.030(4) 0.010(4) C54 0.043(5) 0.010(4) 0.057(5) 0.001(4) 0.032(4) 0.009(4) O1 0.025(3) 0.023(3) 0.023(2) 0.002(2) 0.012(2) 0.008(2) O2 0.027(3) 0.023(3) 0.026(3) 0.007(2) 0.011(2) -0.003(3) O3 0.019(3) 0.026(3) 0.039(3) 0.000(2) 0.012(2) -0.002(2) O4 0.032(3) 0.018(3) 0.022(3) 0.004(2) 0.013(2) 0.001(2) O5 0.027(3) 0.031(3) 0.028(3) 0.005(2) 0.016(2) 0.001(2) O6 0.021(3) 0.027(3) 0.023(3) -0.008(2) 0.010(2) -0.005(2) O7 0.023(3) 0.024(3) 0.025(3) 0.000(2) 0.012(2) 0.006(2) O8 0.026(3) 0.026(3) 0.029(3) -0.003(2) 0.012(2) -0.008(2) O9 0.032(3) 0.017(3) 0.030(3) -0.001(2) 0.011(2) -0.001(2) O10 0.035(3) 0.035(3) 0.035(3) -0.005(3) 0.023(3) -0.009(3) O11 0.031(3) 0.037(3) 0.026(3) -0.006(2) 0.015(2) -0.011(3) O12 0.025(3) 0.024(3) 0.030(3) -0.006(2) 0.008(2) 0.004(2) O13 0.026(3) 0.028(3) 0.028(3) -0.004(2) 0.007(3) 0.005(2) O14 0.037(3) 0.018(3) 0.034(3) -0.008(3) 0.023(3) -0.009(3) O16 0.048(4) 0.100(5) 0.027(3) -0.012(3) 0.017(3) -0.035(4) O17 0.024(3) 0.021(3) 0.037(3) 0.002(2) 0.020(2) 0.002(2) Zn1 0.0234(5) 0.0182(5) 0.0207(4) 0.0010(4) 0.0121(3) 0.0004(4) Zn2 0.0246(5) 0.0207(5) 0.0232(4) 0.0011(4) 0.0119(4) -0.0009(4) Zn3 0.0228(5) 0.0208(5) 0.0219(4) 0.0002(4) 0.0104(4) -0.0001(4) Zn4 0.0226(5) 0.0219(5) 0.0214(4) -0.0013(4) 0.0106(4) -0.0007(4) O15 0.068(12) 0.021(7) 0.022(8) -0.010(7) 0.015(7) -0.021(8) O15A 0.063(12) 0.028(8) 0.056(11) -0.018(9) 0.052(9) -0.009(9) _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 O2 1.247(8) . ? C1 O3 1.262(8) . ? C1 C2 1.524(9) . ? C2 C7 1.378(9) . ? C2 C3 1.386(9) . ? C3 C4 1.378(10) . ? C3 H3 0.9500 . ? C4 C5 1.376(10) . ? C4 H4 0.9500 . ? C5 C6 1.395(10) . ? C5 H5 0.9500 . ? C6 C7 1.379(10) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O4 1.265(8) . ? C8 O5 1.276(8) . ? C8 C9 1.505(9) . ? C9 C10 1.357(9) . ? C9 C14 1.392(10) . ? C10 C11 1.389(9) . ? C10 H10 0.9500 . ? C11 C12 1.378(11) . ? C11 H11 0.9500 . ? C12 C13 1.389(11) . ? C12 H12 0.9500 . ? C13 C14 1.394(10) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O6 1.258(8) . ? C15 O7 1.278(8) . ? C15 C16 1.493(9) . ? C16 C17 1.370(9) . ? C16 C21 1.399(9) . ? C17 C18 1.379(10) . ? C17 H17 0.9500 . ? C18 C19 1.367(10) . ? C18 H18 0.9500 . ? C19 C20 1.384(10) . ? C19 H19 0.9500 . ? C20 C21 1.393(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O9 1.246(8) . ? C22 O8 1.278(8) . ? C22 C23 1.484(9) . ? C23 C28 1.387(9) . ? C23 C24 1.401(10) . ? C24 C25 1.381(10) . ? C24 H24 0.9500 . ? C25 C26 1.384(11) . ? C25 H25 0.9500 . ? C26 C27 1.380(11) . ? C26 H26 0.9500 . ? C27 C28 1.368(10) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 O11 1.258(8) . ? C29 O10 1.267(8) . ? C29 C30 1.498(9) . ? C30 C31 1.365(10) . ? C30 C35 1.407(10) . ? C31 C32 1.379(10) . ? C31 H31 0.9500 . ? C32 C33 1.384(10) . ? C32 H32 0.9500 . ? C33 C34 1.374(11) . ? C33 H33 0.9500 . ? C34 C35 1.390(10) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 O13 1.260(8) . ? C36 O12 1.266(8) . ? C36 C37 1.491(10) . ? C37 C42 1.379(10) . ? C37 C38 1.392(10) . ? C38 C39 1.387(10) . ? C38 H38 0.9500 . ? C39 C40 1.368(11) . ? C39 H39 0.9500 . ? C40 C41 1.400(10) . ? C40 H40 0.9500 . ? C41 C42 1.389(10) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 O15A 1.314(17) . ? C43 C44 1.509(11) . ? C43 O15 1.607(19) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.525(11) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.539(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 O15 1.346(18) . ? C46 O15A 1.475(18) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 O16 1.409(9) . ? C47 C48 1.496(11) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.504(10) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.515(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O16 1.432(8) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O17 1.438(8) . ? C51 C52 1.517(10) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.525(10) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.510(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O17 1.447(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? O1 Zn4 1.921(4) . ? O1 Zn2 1.925(5) . ? O1 Zn3 1.932(4) . ? O1 Zn1 2.027(4) . ? O2 Zn1 2.118(4) . ? O3 Zn2 1.939(5) . ? O4 Zn1 2.114(4) . ? O5 Zn3 1.925(4) . ? O6 Zn1 2.067(4) . ? O7 Zn4 1.942(4) . ? O8 Zn2 1.950(4) . ? O9 Zn3 1.962(5) . ? O10 Zn2 1.977(5) . ? O11 Zn4 1.984(5) . ? O12 Zn3 1.989(5) . ? O13 Zn4 1.980(5) . ? O14 Zn1 2.102(5) . ? O14 H14A 0.80(8) . ? O14 H14B 0.77(8) . ? O17 Zn1 2.183(4) . ? Zn2 Zn3 3.0517(11) . ? Zn2 Zn4 3.1486(11) . ? Zn3 Zn4 3.1383(10) . ? 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 O2 C1 O3 126.5(6) . . ? O2 C1 C2 117.9(6) . . ? O3 C1 C2 115.6(6) . . ? C7 C2 C3 119.6(7) . . ? C7 C2 C1 120.9(6) . . ? C3 C2 C1 119.4(6) . . ? C4 C3 C2 119.6(7) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.5(7) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.4(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 118.5(7) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C2 C7 C6 121.3(7) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? O4 C8 O5 124.8(6) . . ? O4 C8 C9 119.0(7) . . ? O5 C8 C9 116.2(6) . . ? C10 C9 C14 119.5(6) . . ? C10 C9 C8 121.0(6) . . ? C14 C9 C8 119.5(7) . . ? C9 C10 C11 121.5(7) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C12 C11 C10 119.4(8) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.0(7) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 119.7(7) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C9 C14 C13 119.8(7) . . ? C9 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? O6 C15 O7 124.7(6) . . ? O6 C15 C16 118.1(6) . . ? O7 C15 C16 117.2(6) . . ? C17 C16 C21 119.4(6) . . ? C17 C16 C15 120.6(6) . . ? C21 C16 C15 120.0(6) . . ? C16 C17 C18 120.3(7) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 121.3(7) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 119.3(7) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C21 120.2(7) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 119.6(7) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? O9 C22 O8 125.3(6) . . ? O9 C22 C23 118.2(7) . . ? O8 C22 C23 116.5(7) . . ? C28 C23 C24 119.0(6) . . ? C28 C23 C22 120.7(7) . . ? C24 C23 C22 120.3(7) . . ? C25 C24 C23 119.7(7) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 119.8(7) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 120.9(7) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 119.2(7) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C23 121.3(7) . . ? C27 C28 H28 119.3 . . ? C23 C28 H28 119.3 . . ? O11 C29 O10 126.0(6) . . ? O11 C29 C30 119.3(6) . . ? O10 C29 C30 114.7(7) . . ? C31 C30 C35 118.9(6) . . ? C31 C30 C29 122.6(7) . . ? C35 C30 C29 118.4(7) . . ? C30 C31 C32 122.8(7) . . ? C30 C31 H31 118.6 . . ? C32 C31 H31 118.6 . . ? C31 C32 C33 118.1(7) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C34 C33 C32 120.5(7) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 121.0(8) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C30 118.6(8) . . ? C34 C35 H35 120.7 . . ? C30 C35 H35 120.7 . . ? O13 C36 O12 125.5(7) . . ? O13 C36 C37 116.5(6) . . ? O12 C36 C37 118.0(6) . . ? C42 C37 C38 119.5(7) . . ? C42 C37 C36 120.7(7) . . ? C38 C37 C36 119.8(6) . . ? C39 C38 C37 119.9(7) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C40 C39 C38 120.5(7) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 120.0(8) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 119.2(7) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C37 C42 C41 120.7(7) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? O15A C43 C44 110.6(10) . . ? O15A C43 O15 28.5(7) . . ? C44 C43 O15 97.6(9) . . ? O15A C43 H43A 124.6 . . ? C44 C43 H43A 112.2 . . ? O15 C43 H43A 112.2 . . ? O15A C43 H43B 83.7 . . ? C44 C43 H43B 112.2 . . ? O15 C43 H43B 112.2 . . ? H43A C43 H43B 109.8 . . ? C43 C44 C45 103.2(7) . . ? C43 C44 H44A 111.1 . . ? C45 C44 H44A 111.1 . . ? C43 C44 H44B 111.1 . . ? C45 C44 H44B 111.1 . . ? H44A C44 H44B 109.1 . . ? C44 C45 C46 103.4(7) . . ? C44 C45 H45A 111.1 . . ? C46 C45 H45A 111.1 . . ? C44 C45 H45B 111.1 . . ? C46 C45 H45B 111.1 . . ? H45A C45 H45B 109.0 . . ? O15 C46 O15A 31.4(6) . . ? O15 C46 C45 109.0(10) . . ? O15A C46 C45 103.4(9) . . ? O15 C46 H46A 109.9 . . ? O15A C46 H46A 137.2 . . ? C45 C46 H46A 109.9 . . ? O15 C46 H46B 109.9 . . ? O15A C46 H46B 83.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? O16 C47 C48 106.9(7) . . ? O16 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? O16 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.6 . . ? C47 C48 C49 104.9(6) . . ? C47 C48 H48A 110.8 . . ? C49 C48 H48A 110.8 . . ? C47 C48 H48B 110.8 . . ? C49 C48 H48B 110.8 . . ? H48A C48 H48B 108.9 . . ? C48 C49 C50 103.1(6) . . ? C48 C49 H49A 111.1 . . ? C50 C49 H49A 111.1 . . ? C48 C49 H49B 111.1 . . ? C50 C49 H49B 111.1 . . ? H49A C49 H49B 109.1 . . ? O16 C50 C49 105.6(6) . . ? O16 C50 H50A 110.6 . . ? C49 C50 H50A 110.6 . . ? O16 C50 H50B 110.6 . . ? C49 C50 H50B 110.6 . . ? H50A C50 H50B 108.7 . . ? O17 C51 C52 105.7(5) . . ? O17 C51 H51A 110.6 . . ? C52 C51 H51A 110.6 . . ? O17 C51 H51B 110.6 . . ? C52 C51 H51B 110.6 . . ? H51A C51 H51B 108.7 . . ? C51 C52 C53 101.0(6) . . ? C51 C52 H52A 111.6 . . ? C53 C52 H52A 111.6 . . ? C51 C52 H52B 111.6 . . ? C53 C52 H52B 111.6 . . ? H52A C52 H52B 109.4 . . ? C54 C53 C52 103.2(6) . . ? C54 C53 H53A 111.1 . . ? C52 C53 H53A 111.1 . . ? C54 C53 H53B 111.1 . . ? C52 C53 H53B 111.1 . . ? H53A C53 H53B 109.1 . . ? O17 C54 C53 104.9(6) . . ? O17 C54 H54A 110.8 . . ? C53 C54 H54A 110.8 . . ? O17 C54 H54B 110.8 . . ? C53 C54 H54B 110.8 . . ? H54A C54 H54B 108.9 . . ? Zn4 O1 Zn2 109.9(2) . . ? Zn4 O1 Zn3 109.1(2) . . ? Zn2 O1 Zn3 104.6(2) . . ? Zn4 O1 Zn1 113.7(2) . . ? Zn2 O1 Zn1 109.1(2) . . ? Zn3 O1 Zn1 110.0(2) . . ? C1 O2 Zn1 134.5(4) . . ? C1 O3 Zn2 122.1(5) . . ? C8 O4 Zn1 135.1(4) . . ? C8 O5 Zn3 123.8(4) . . ? C15 O6 Zn1 138.6(4) . . ? C15 O7 Zn4 122.2(4) . . ? C22 O8 Zn2 127.1(5) . . ? C22 O9 Zn3 130.8(5) . . ? C29 O10 Zn2 128.1(5) . . ? C29 O11 Zn4 129.3(4) . . ? C36 O12 Zn3 130.3(5) . . ? C36 O13 Zn4 125.5(5) . . ? Zn1 O14 H14A 120(6) . . ? Zn1 O14 H14B 125(6) . . ? H14A O14 H14B 105(8) . . ? C47 O16 C50 111.2(6) . . ? C51 O17 C54 110.3(5) . . ? C51 O17 Zn1 121.7(4) . . ? C54 O17 Zn1 126.1(4) . . ? O1 Zn1 O6 97.82(17) . . ? O1 Zn1 O14 87.94(19) . . ? O6 Zn1 O14 174.22(19) . . ? O1 Zn1 O4 98.11(17) . . ? O6 Zn1 O4 92.08(17) . . ? O14 Zn1 O4 87.53(19) . . ? O1 Zn1 O2 94.13(17) . . ? O6 Zn1 O2 87.64(18) . . ? O14 Zn1 O2 91.51(19) . . ? O4 Zn1 O2 167.68(18) . . ? O1 Zn1 O17 175.91(18) . . ? O6 Zn1 O17 86.16(17) . . ? O14 Zn1 O17 88.07(19) . . ? O4 Zn1 O17 82.63(17) . . ? O2 Zn1 O17 85.06(17) . . ? O1 Zn2 O3 115.29(19) . . ? O1 Zn2 O8 115.38(19) . . ? O3 Zn2 O8 109.0(2) . . ? O1 Zn2 O10 109.78(19) . . ? O3 Zn2 O10 103.9(2) . . ? O8 Zn2 O10 101.99(19) . . ? O1 Zn2 Zn3 37.78(13) . . ? O3 Zn2 Zn3 143.07(14) . . ? O8 Zn2 Zn3 79.16(14) . . ? O10 Zn2 Zn3 109.52(15) . . ? O1 Zn2 Zn4 34.99(12) . . ? O3 Zn2 Zn4 114.15(14) . . ? O8 Zn2 Zn4 135.78(15) . . ? O10 Zn2 Zn4 76.78(14) . . ? Zn3 Zn2 Zn4 60.79(2) . . ? O5 Zn3 O1 118.0(2) . . ? O5 Zn3 O9 103.41(19) . . ? O1 Zn3 O9 113.7(2) . . ? O5 Zn3 O12 108.2(2) . . ? O1 Zn3 O12 108.58(18) . . ? O9 Zn3 O12 104.02(19) . . ? O5 Zn3 Zn2 136.70(15) . . ? O1 Zn3 Zn2 37.61(14) . . ? O9 Zn3 Zn2 76.58(14) . . ? O12 Zn3 Zn2 113.82(14) . . ? O5 Zn3 Zn4 124.47(14) . . ? O1 Zn3 Zn4 35.34(13) . . ? O9 Zn3 Zn4 130.63(14) . . ? O12 Zn3 Zn4 74.00(13) . . ? Zn2 Zn3 Zn4 61.13(2) . . ? O1 Zn4 O7 116.79(19) . . ? O1 Zn4 O13 113.16(18) . . ? O7 Zn4 O13 106.79(19) . . ? O1 Zn4 O11 110.5(2) . . ? O7 Zn4 O11 106.64(19) . . ? O13 Zn4 O11 101.7(2) . . ? O1 Zn4 Zn3 35.58(13) . . ? O7 Zn4 Zn3 134.54(13) . . ? O13 Zn4 Zn3 77.72(13) . . ? O11 Zn4 Zn3 116.83(14) . . ? O1 Zn4 Zn2 35.07(13) . . ? O7 Zn4 Zn2 126.26(14) . . ? O13 Zn4 Zn2 125.70(14) . . ? O11 Zn4 Zn2 75.65(14) . . ? Zn3 Zn4 Zn2 58.08(2) . . ? C46 O15 C43 103.0(10) . . ? C43 O15A C46 112.2(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.473 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.097