# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Daofeng Sun' _publ_contact_author_address ; Jinan Shandong China 250100 ; _publ_contact_author_email dfsun@sdu.edu.cn _publ_author_name 'Daofeng Sun' # Attachment '- 1.cif' data_test _database_code_depnum_ccdc_archive 'CCDC 775311' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H76 N6 O18 S4 Tm2' _chemical_formula_sum 'C64 H76 N6 O18 S4 Tm2' _chemical_formula_weight 1683.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0709(7) _cell_length_b 17.7102(13) _cell_length_c 21.7080(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.6210(10) _cell_angle_gamma 90.00 _cell_volume 3427.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5560 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.4 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6659 _exptl_absorpt_correction_T_max 0.8516 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19610 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.60 _reflns_number_total 7659 _reflns_number_gt 5100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT+ (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2007)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+1.2153P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7659 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.132 _refine_ls_shift/su_mean 0.002 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 Tm1 Tm -0.26819(2) -0.581896(10) 0.626768(9) 0.05372(8) Uani 1 1 d . . . S1 S -0.29616(12) -0.29485(5) 0.65398(5) 0.0471(2) Uani 1 1 d . . . S4 S 0.12280(12) -0.16792(5) 0.44765(4) 0.0454(2) Uani 1 1 d . . . O1 O -0.3027(3) -0.45116(15) 0.63928(13) 0.0603(8) Uani 1 1 d . . . O2 O -0.4049(4) -0.53008(16) 0.69564(16) 0.0779(10) Uani 1 1 d . . . O3 O 0.2041(3) -0.29545(14) 0.39718(13) 0.0600(8) Uani 1 1 d . . . O4 O 0.3426(3) -0.30880(15) 0.32599(13) 0.0605(8) Uani 1 1 d . . . O5 O -0.4944(5) -0.5949(2) 0.5667(2) 0.0961(12) Uani 1 1 d . . . O6 O -0.2204(4) -0.5582(2) 0.52795(15) 0.0785(10) Uani 1 1 d . . . O7 O -0.0884(6) -0.5850(2) 0.72307(19) 0.0930(12) Uani 1 1 d . . . O8 O -0.0089(5) -0.5581(3) 0.6385(2) 0.1024(13) Uani 1 1 d . . . O9 O 0.1345(9) -0.5638(4) 0.7257(4) 0.206(3) Uani 1 1 d . . . N1 N -0.7217(5) -0.6473(2) 0.5456(2) 0.0722(11) Uani 1 1 d . . . N2 N -0.2076(5) -0.6130(2) 0.43487(17) 0.0667(10) Uani 1 1 d . . . N3 N 0.0125(7) -0.5691(3) 0.6964(3) 0.0903(15) Uani 1 1 d . . . C1 C -0.3802(5) -0.4633(2) 0.68058(19) 0.0478(10) Uani 1 1 d . . . C2 C -0.4501(4) -0.4009(2) 0.71149(16) 0.0403(9) Uani 1 1 d . . . C3 C -0.5491(5) -0.4210(2) 0.75022(18) 0.0529(10) Uani 1 1 d . . . H3 H -0.5664 -0.4720 0.7563 0.063 Uiso 1 1 calc R . . C4 C -0.6224(5) -0.3686(3) 0.78002(18) 0.0566(11) Uani 1 1 d . . . H4 H -0.6906 -0.3835 0.8048 0.068 Uiso 1 1 calc R . . C5 C -0.5927(4) -0.2933(2) 0.77230(17) 0.0517(10) Uani 1 1 d . . . H5 H -0.6397 -0.2570 0.7929 0.062 Uiso 1 1 calc R . . C6 C -0.4947(4) -0.2711(2) 0.73475(16) 0.0433(9) Uani 1 1 d . . . H6 H -0.4769 -0.2199 0.7300 0.052 Uiso 1 1 calc R . . C7 C -0.4208(4) -0.32428(19) 0.70332(16) 0.0366(8) Uani 1 1 d . . . C8 C -0.2950(4) -0.19236(19) 0.66110(18) 0.0448(9) Uani 1 1 d . . . H8A H -0.3963 -0.1726 0.6508 0.054 Uiso 1 1 calc R . . H8B H -0.2518 -0.1773 0.7036 0.054 Uiso 1 1 calc R . . C9 C -0.2008(4) -0.16283(18) 0.61543(16) 0.0379(8) Uani 1 1 d . . . C10 C -0.2707(4) -0.1483(2) 0.55313(18) 0.0429(9) Uani 1 1 d . . . C11 C -0.4375(5) -0.1614(3) 0.5315(2) 0.0745(14) Uani 1 1 d . . . H11A H -0.4892 -0.1139 0.5289 0.112 Uiso 1 1 calc R . . H11B H -0.4743 -0.1935 0.5610 0.112 Uiso 1 1 calc R . . H11C H -0.4547 -0.1851 0.4911 0.112 Uiso 1 1 calc R . . C12 C -0.1842(4) -0.1211(2) 0.51039(17) 0.0437(9) Uani 1 1 d . . . C13 C -0.2597(6) -0.1047(3) 0.4440(2) 0.0695(13) Uani 1 1 d . . . H13A H -0.1853 -0.0919 0.4195 0.104 Uiso 1 1 calc R . . H13B H -0.3280 -0.0633 0.4437 0.104 Uiso 1 1 calc R . . H13C H -0.3139 -0.1486 0.4264 0.104 Uiso 1 1 calc R . . C14 C -0.0309(4) -0.11031(19) 0.52988(17) 0.0406(9) Uani 1 1 d . . . C15 C 0.0391(4) -0.12573(19) 0.59200(17) 0.0410(9) Uani 1 1 d . . . C16 C 0.2059(4) -0.1143(3) 0.6134(2) 0.0606(12) Uani 1 1 d . . . H16A H 0.2237 -0.0657 0.6331 0.091 Uiso 1 1 calc R . . H16B H 0.2550 -0.1167 0.5779 0.091 Uiso 1 1 calc R . . H16C H 0.2449 -0.1530 0.6428 0.091 Uiso 1 1 calc R . . C17 C -0.0469(4) -0.15169(19) 0.63515(16) 0.0387(8) Uani 1 1 d . . . C18 C 0.0269(5) -0.1694(3) 0.70186(17) 0.0589(11) Uani 1 1 d . . . H18A H -0.0483 -0.1836 0.7255 0.088 Uiso 1 1 calc R . . H18B H 0.0793 -0.1255 0.7205 0.088 Uiso 1 1 calc R . . H18C H 0.0966 -0.2102 0.7020 0.088 Uiso 1 1 calc R . . C19 C 0.0643(5) -0.08308(19) 0.48356(18) 0.0453(9) Uani 1 1 d . . . H19A H 0.1507 -0.0552 0.5050 0.054 Uiso 1 1 calc R . . H19B H 0.0062 -0.0506 0.4521 0.054 Uiso 1 1 calc R . . C20 C 0.2348(4) -0.13283(19) 0.39536(15) 0.0355(8) Uani 1 1 d . . . C21 C 0.2582(4) -0.0560(2) 0.38845(17) 0.0456(10) Uani 1 1 d . . . H21 H 0.2132 -0.0217 0.4116 0.055 Uiso 1 1 calc R . . C22 C 0.3470(5) -0.0297(2) 0.34784(18) 0.0510(10) Uani 1 1 d . . . H22 H 0.3613 0.0220 0.3442 0.061 Uiso 1 1 calc R . . C23 C 0.4147(5) -0.0789(2) 0.31271(19) 0.0494(10) Uani 1 1 d . . . H23 H 0.4740 -0.0609 0.2853 0.059 Uiso 1 1 calc R . . C24 C 0.3932(4) -0.1550(2) 0.31886(16) 0.0437(9) Uani 1 1 d . . . H24 H 0.4399 -0.1885 0.2957 0.052 Uiso 1 1 calc R . . C25 C 0.3031(4) -0.18319(19) 0.35902(16) 0.0359(8) Uani 1 1 d . . . C26 C 0.2831(4) -0.2662(2) 0.36097(17) 0.0443(9) Uani 1 1 d . . . C27A C -0.6130(8) -0.6101(4) 0.5264(3) 0.065(2) Uani 0.732(11) 1 d P . . H27A H -0.6219 -0.5951 0.4849 0.079 Uiso 0.732(11) 1 calc PR . . C28A C -0.7152(13) -0.6719(7) 0.6061(5) 0.131(5) Uani 0.732(11) 1 d P . . H28A H -0.8152 -0.6783 0.6140 0.196 Uiso 0.732(11) 1 calc PR . . H28B H -0.6631 -0.6353 0.6347 0.196 Uiso 0.732(11) 1 calc PR . . H28C H -0.6629 -0.7192 0.6118 0.196 Uiso 0.732(11) 1 calc PR . . C29A C -0.8564(10) -0.6622(6) 0.4973(5) 0.126(4) Uani 0.732(11) 1 d P . . H29A H -0.8513 -0.6332 0.4604 0.188 Uiso 0.732(11) 1 calc PR . . H29B H -0.9446 -0.6483 0.5132 0.188 Uiso 0.732(11) 1 calc PR . . H29C H -0.8609 -0.7150 0.4870 0.188 Uiso 0.732(11) 1 calc PR . . C30A C -0.1687(12) -0.5574(5) 0.4766(5) 0.074(3) Uani 0.531(8) 1 d P . . H30A H -0.1054 -0.5188 0.4686 0.089 Uiso 0.531(8) 1 calc PR . . C31A C -0.2958(14) -0.6735(6) 0.4463(5) 0.098(4) Uani 0.531(8) 1 d P . . H31A H -0.2398 -0.7195 0.4463 0.146 Uiso 0.531(8) 1 calc PR . . H31B H -0.3839 -0.6758 0.4141 0.146 Uiso 0.531(8) 1 calc PR . . H31C H -0.3248 -0.6671 0.4863 0.146 Uiso 0.531(8) 1 calc PR . . C32A C -0.1303(17) -0.6194(9) 0.3791(5) 0.124(6) Uani 0.531(8) 1 d P . . H32A H -0.0485 -0.5842 0.3837 0.187 Uiso 0.531(8) 1 calc PR . . H32B H -0.2006 -0.6083 0.3415 0.187 Uiso 0.531(8) 1 calc PR . . H32C H -0.0926 -0.6698 0.3769 0.187 Uiso 0.531(8) 1 calc PR . . C27B C -0.601(2) -0.6250(12) 0.5923(9) 0.076(7) Uani 0.268(11) 1 d P . . H27B H -0.5975 -0.6307 0.6352 0.091 Uiso 0.268(11) 1 calc PR . . C28B C -0.725(3) -0.6334(17) 0.4883(9) 0.115(11) Uani 0.268(11) 1 d P . . H28D H -0.6918 -0.5826 0.4837 0.172 Uiso 0.268(11) 1 calc PR . . H28E H -0.8261 -0.6390 0.4656 0.172 Uiso 0.268(11) 1 calc PR . . H28F H -0.6607 -0.6680 0.4719 0.172 Uiso 0.268(11) 1 calc PR . . C29B C -0.843(3) -0.6854(16) 0.5767(15) 0.115(11) Uani 0.268(11) 1 d P . . H29D H -0.9405 -0.6668 0.5575 0.172 Uiso 0.268(11) 1 calc PR . . H29E H -0.8251 -0.6738 0.6206 0.172 Uiso 0.268(11) 1 calc PR . . H29F H -0.8398 -0.7391 0.5711 0.172 Uiso 0.268(11) 1 calc PR . . C30B C -0.2339(12) -0.6194(6) 0.4916(5) 0.070(3) Uani 0.469(8) 1 d P . . H30B H -0.2615 -0.6656 0.5064 0.084 Uiso 0.469(8) 1 calc PR . . C31B C -0.193(2) -0.5404(7) 0.4078(6) 0.127(7) Uani 0.469(8) 1 d P . . H31D H -0.2865 -0.5261 0.3823 0.190 Uiso 0.469(8) 1 calc PR . . H31E H -0.1166 -0.5424 0.3825 0.190 Uiso 0.469(8) 1 calc PR . . H31F H -0.1651 -0.5039 0.4406 0.190 Uiso 0.469(8) 1 calc PR . . C32B C -0.2118(19) -0.6771(9) 0.3942(6) 0.112(6) Uani 0.469(8) 1 d P . . H32D H -0.2218 -0.6602 0.3516 0.168 Uiso 0.469(8) 1 calc PR . . H32E H -0.2957 -0.7085 0.3983 0.168 Uiso 0.469(8) 1 calc PR . . H32F H -0.1207 -0.7055 0.4055 0.168 Uiso 0.469(8) 1 calc PR . . 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 Tm1 0.07171(15) 0.02951(10) 0.06488(14) -0.00144(9) 0.02556(10) 0.00287(9) S1 0.0614(6) 0.0306(5) 0.0572(6) -0.0020(4) 0.0313(5) -0.0012(4) S4 0.0672(7) 0.0291(5) 0.0469(5) -0.0001(4) 0.0287(5) -0.0006(4) O1 0.090(2) 0.0314(14) 0.0714(19) -0.0015(13) 0.0465(18) 0.0003(14) O2 0.120(3) 0.0323(16) 0.099(2) 0.0038(16) 0.065(2) 0.0025(16) O3 0.092(2) 0.0281(14) 0.0714(19) 0.0005(13) 0.0452(18) 0.0037(14) O4 0.091(2) 0.0357(15) 0.0638(18) -0.0074(13) 0.0385(17) 0.0066(14) O5 0.071(3) 0.095(3) 0.117(3) 0.003(2) 0.004(3) -0.009(2) O6 0.107(3) 0.076(2) 0.055(2) -0.0035(17) 0.022(2) 0.012(2) O7 0.117(4) 0.085(3) 0.078(3) 0.003(2) 0.020(3) -0.008(2) O8 0.088(3) 0.139(4) 0.080(3) -0.001(3) 0.014(2) -0.012(2) O9 0.150(6) 0.249(9) 0.200(7) 0.007(6) -0.019(6) -0.006(5) N1 0.059(3) 0.061(3) 0.100(4) -0.008(2) 0.023(3) 0.002(2) N2 0.100(3) 0.054(2) 0.045(2) -0.0043(19) 0.011(2) -0.007(2) N3 0.074(4) 0.091(4) 0.096(4) -0.012(3) -0.010(3) 0.003(3) C1 0.059(3) 0.030(2) 0.057(2) 0.0006(18) 0.017(2) 0.0006(18) C2 0.050(2) 0.035(2) 0.038(2) 0.0006(15) 0.0128(17) 0.0005(16) C3 0.065(3) 0.045(2) 0.053(2) 0.0027(19) 0.021(2) -0.006(2) C4 0.065(3) 0.064(3) 0.047(2) -0.001(2) 0.028(2) -0.008(2) C5 0.057(3) 0.059(3) 0.045(2) -0.0098(19) 0.022(2) 0.004(2) C6 0.050(2) 0.039(2) 0.042(2) -0.0044(17) 0.0137(18) -0.0013(17) C7 0.042(2) 0.0346(19) 0.0340(19) 0.0001(15) 0.0100(16) 0.0004(16) C8 0.052(2) 0.032(2) 0.055(2) -0.0018(17) 0.021(2) -0.0009(17) C9 0.049(2) 0.0261(17) 0.043(2) -0.0020(15) 0.0197(18) -0.0010(16) C10 0.046(2) 0.035(2) 0.049(2) -0.0012(17) 0.0117(19) 0.0020(16) C11 0.054(3) 0.093(4) 0.076(3) 0.013(3) 0.009(3) -0.003(3) C12 0.054(3) 0.039(2) 0.039(2) 0.0005(17) 0.0103(19) 0.0046(18) C13 0.076(3) 0.080(3) 0.052(3) 0.009(2) 0.008(2) -0.005(3) C14 0.055(2) 0.0280(18) 0.044(2) -0.0027(16) 0.0216(19) 0.0008(16) C15 0.046(2) 0.0317(19) 0.048(2) -0.0041(16) 0.0172(19) 0.0002(16) C16 0.052(3) 0.071(3) 0.060(3) 0.000(2) 0.014(2) -0.009(2) C17 0.044(2) 0.0337(19) 0.039(2) -0.0007(15) 0.0118(17) 0.0012(16) C18 0.067(3) 0.068(3) 0.043(2) 0.007(2) 0.011(2) -0.004(2) C19 0.065(3) 0.0321(19) 0.045(2) 0.0009(17) 0.0255(19) 0.0022(18) C20 0.042(2) 0.0318(18) 0.0337(18) 0.0025(15) 0.0101(16) 0.0003(15) C21 0.067(3) 0.0264(18) 0.048(2) -0.0004(16) 0.023(2) 0.0034(17) C22 0.067(3) 0.032(2) 0.057(2) 0.0020(18) 0.020(2) -0.0044(19) C23 0.054(2) 0.048(2) 0.049(2) 0.0041(19) 0.019(2) -0.0059(19) C24 0.052(2) 0.043(2) 0.037(2) -0.0010(17) 0.0090(18) 0.0041(18) C25 0.043(2) 0.0317(19) 0.0343(18) -0.0018(15) 0.0092(16) 0.0009(15) C26 0.060(3) 0.035(2) 0.040(2) -0.0036(16) 0.0146(19) 0.0007(18) C27A 0.064(5) 0.074(5) 0.058(5) -0.001(4) 0.013(4) 0.010(4) C28A 0.125(11) 0.146(10) 0.141(9) 0.056(7) 0.078(8) 0.025(8) C29A 0.061(6) 0.141(9) 0.170(11) -0.051(8) 0.009(6) -0.014(5) C30A 0.103(8) 0.046(5) 0.077(7) 0.009(5) 0.029(6) -0.016(5) C31A 0.142(11) 0.080(8) 0.064(7) -0.011(6) 0.000(7) -0.049(7) C32A 0.169(14) 0.141(13) 0.073(8) -0.042(8) 0.047(8) -0.067(11) C27B 0.089(16) 0.090(15) 0.054(12) -0.006(10) 0.026(11) -0.011(12) C28B 0.13(3) 0.18(3) 0.029(11) -0.029(13) -0.001(13) 0.01(2) C29B 0.057(15) 0.13(2) 0.17(3) 0.028(19) 0.055(17) -0.026(14) C30B 0.094(8) 0.049(6) 0.067(7) 0.000(5) 0.018(6) -0.009(6) C31B 0.26(2) 0.070(9) 0.059(8) 0.008(7) 0.038(10) -0.027(11) C32B 0.166(16) 0.105(12) 0.055(8) -0.024(8) -0.003(9) 0.039(10) _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 Tm1 O5 2.231(4) . ? Tm1 O2 2.301(3) . ? Tm1 O6 2.304(3) . ? Tm1 O3 2.332(2) 3_546 ? Tm1 O4 2.347(3) 3_546 ? Tm1 O8 2.357(4) . ? Tm1 O1 2.359(3) . ? Tm1 O7 2.404(4) . ? Tm1 C26 2.709(4) 3_546 ? S1 C7 1.773(4) . ? S1 C8 1.822(4) . ? S4 C20 1.770(3) . ? S4 C19 1.817(4) . ? O1 C1 1.256(4) . ? O2 C1 1.258(4) . ? O3 C26 1.268(4) . ? O3 Tm1 2.332(2) 3_546 ? O4 C26 1.260(4) . ? O4 Tm1 2.347(3) 3_546 ? O5 C27A 1.283(8) . ? O5 C27B 1.32(2) . ? O6 C30A 1.286(10) . ? O6 C30B 1.334(10) . ? O7 N3 1.203(6) . ? O8 N3 1.251(6) . ? O9 N3 1.174(7) . ? N1 C28B 1.26(2) . ? N1 C27A 1.315(8) . ? N1 C28A 1.375(10) . ? N1 C27B 1.40(2) . ? N1 C29A 1.480(9) . ? N1 C29B 1.55(2) . ? N2 C30B 1.301(11) . ? N2 C30A 1.341(10) . ? N2 C31A 1.387(10) . ? N2 C31B 1.430(12) . ? N2 C32B 1.434(13) . ? N2 C32A 1.510(12) . ? C1 C2 1.493(5) . ? C2 C3 1.385(5) . ? C2 C7 1.400(5) . ? C3 C4 1.372(6) . ? C3 H3 0.9300 . ? C4 C5 1.376(6) . ? C4 H4 0.9300 . ? C5 C6 1.369(5) . ? C5 H5 0.9300 . ? C6 C7 1.404(5) . ? C6 H6 0.9300 . ? C8 C9 1.516(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C17 1.396(5) . ? C9 C10 1.408(5) . ? C10 C12 1.406(5) . ? C10 C11 1.517(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.390(5) . ? C12 C13 1.506(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.407(5) . ? C14 C19 1.519(5) . ? C15 C17 1.402(5) . ? C15 C16 1.513(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.512(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.389(5) . ? C20 C25 1.408(5) . ? C21 C22 1.380(5) . ? C21 H21 0.9300 . ? C22 C23 1.375(5) . ? C22 H22 0.9300 . ? C23 C24 1.372(5) . ? C23 H23 0.9300 . ? C24 C25 1.393(5) . ? C24 H24 0.9300 . ? C25 C26 1.483(5) . ? C26 Tm1 2.709(4) 3_546 ? C27A H27A 0.9300 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? C30A H30A 0.9300 . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C27B H27B 0.9300 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? C30B H30B 0.9300 . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Tm1 O2 82.74(15) . . ? O5 Tm1 O6 77.60(16) . . ? O2 Tm1 O6 138.46(12) . . ? O5 Tm1 O3 90.78(13) . 3_546 ? O2 Tm1 O3 134.63(10) . 3_546 ? O6 Tm1 O3 82.22(11) . 3_546 ? O5 Tm1 O4 82.10(13) . 3_546 ? O2 Tm1 O4 79.18(9) . 3_546 ? O6 Tm1 O4 132.51(11) . 3_546 ? O3 Tm1 O4 55.45(9) 3_546 3_546 ? O5 Tm1 O8 150.89(17) . . ? O2 Tm1 O8 120.30(14) . . ? O6 Tm1 O8 73.30(14) . . ? O3 Tm1 O8 84.61(13) 3_546 . ? O4 Tm1 O8 117.53(14) 3_546 . ? O5 Tm1 O1 92.38(13) . . ? O2 Tm1 O1 55.60(10) . . ? O6 Tm1 O1 88.86(11) . . ? O3 Tm1 O1 169.67(9) 3_546 . ? O4 Tm1 O1 134.77(9) 3_546 . ? O8 Tm1 O1 87.86(14) . . ? O5 Tm1 O7 155.47(17) . . ? O2 Tm1 O7 78.72(15) . . ? O6 Tm1 O7 126.86(15) . . ? O3 Tm1 O7 90.90(12) 3_546 . ? O4 Tm1 O7 78.77(13) 3_546 . ? O8 Tm1 O7 53.57(15) . . ? O1 Tm1 O7 90.30(12) . . ? O5 Tm1 C26 84.13(13) . 3_546 ? O2 Tm1 C26 106.83(10) . 3_546 ? O6 Tm1 C26 107.08(11) . 3_546 ? O3 Tm1 C26 27.86(10) 3_546 3_546 ? O4 Tm1 C26 27.71(9) 3_546 3_546 ? O8 Tm1 C26 103.54(14) . 3_546 ? O1 Tm1 C26 162.43(10) . 3_546 ? O7 Tm1 C26 86.00(12) . 3_546 ? C7 S1 C8 103.65(17) . . ? C20 S4 C19 103.45(17) . . ? C1 O1 Tm1 91.0(2) . . ? C1 O2 Tm1 93.6(2) . . ? C26 O3 Tm1 92.8(2) . 3_546 ? C26 O4 Tm1 92.3(2) . 3_546 ? C27A O5 C27B 67.2(9) . . ? C27A O5 Tm1 170.1(4) . . ? C27B O5 Tm1 117.7(10) . . ? C30A O6 C30B 60.3(6) . . ? C30A O6 Tm1 165.9(5) . . ? C30B O6 Tm1 113.0(5) . . ? N3 O7 Tm1 91.7(4) . . ? N3 O8 Tm1 92.7(4) . . ? C28B N1 C27A 58.4(14) . . ? C28B N1 C28A 172.6(15) . . ? C27A N1 C28A 123.9(8) . . ? C28B N1 C27B 122.2(17) . . ? C27A N1 C27B 63.8(9) . . ? C28A N1 C27B 60.5(9) . . ? C28B N1 C29A 58.0(13) . . ? C27A N1 C29A 115.8(7) . . ? C28A N1 C29A 120.2(7) . . ? C27B N1 C29A 173.5(10) . . ? C28B N1 C29B 128.5(18) . . ? C27A N1 C29B 172.2(13) . . ? C28A N1 C29B 49.8(12) . . ? C27B N1 C29B 109.3(15) . . ? C29A N1 C29B 70.6(12) . . ? C30B N2 C30A 59.7(6) . . ? C30B N2 C31A 63.3(6) . . ? C30A N2 C31A 122.4(7) . . ? C30B N2 C31B 120.9(8) . . ? C30A N2 C31B 65.4(6) . . ? C31A N2 C31B 150.4(9) . . ? C30B N2 C32B 121.6(9) . . ? C30A N2 C32B 166.3(9) . . ? C31A N2 C32B 63.1(8) . . ? C31B N2 C32B 116.9(9) . . ? C30B N2 C32A 160.8(9) . . ? C30A N2 C32A 119.6(7) . . ? C31A N2 C32A 117.0(8) . . ? C31B N2 C32A 69.3(8) . . ? C32B N2 C32A 53.9(7) . . ? O9 N3 O7 118.8(7) . . ? O9 N3 O8 119.2(8) . . ? O7 N3 O8 121.9(6) . . ? O2 C1 O1 119.7(4) . . ? O2 C1 C2 117.9(4) . . ? O1 C1 C2 122.3(3) . . ? C3 C2 C7 119.1(3) . . ? C3 C2 C1 117.3(3) . . ? C7 C2 C1 123.6(3) . . ? C4 C3 C2 122.5(4) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.4(4) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 121.2(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C2 C7 C6 118.0(3) . . ? C2 C7 S1 121.3(3) . . ? C6 C7 S1 120.8(3) . . ? C9 C8 S1 106.5(2) . . ? C9 C8 H8A 110.4 . . ? S1 C8 H8A 110.4 . . ? C9 C8 H8B 110.4 . . ? S1 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C17 C9 C10 121.1(3) . . ? C17 C9 C8 120.0(3) . . ? C10 C9 C8 118.9(3) . . ? C12 C10 C9 119.3(3) . . ? C12 C10 C11 119.6(4) . . ? C9 C10 C11 121.1(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C10 119.7(3) . . ? C14 C12 C13 121.2(4) . . ? C10 C12 C13 119.2(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 C15 120.9(3) . . ? C12 C14 C19 120.1(3) . . ? C15 C14 C19 119.0(3) . . ? C17 C15 C14 119.7(3) . . ? C17 C15 C16 119.2(3) . . ? C14 C15 C16 121.1(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9 C17 C15 119.3(3) . . ? C9 C17 C18 120.4(3) . . ? C15 C17 C18 120.3(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 S4 105.6(2) . . ? C14 C19 H19A 110.6 . . ? S4 C19 H19A 110.6 . . ? C14 C19 H19B 110.6 . . ? S4 C19 H19B 110.6 . . ? H19A C19 H19B 108.8 . . ? C21 C20 C25 117.9(3) . . ? C21 C20 S4 122.0(3) . . ? C25 C20 S4 120.1(3) . . ? C22 C21 C20 121.2(3) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 118.8(4) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 121.6(3) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C20 119.5(3) . . ? C24 C25 C26 117.6(3) . . ? C20 C25 C26 122.9(3) . . ? O4 C26 O3 118.9(3) . . ? O4 C26 C25 120.5(3) . . ? O3 C26 C25 120.6(3) . . ? O4 C26 Tm1 59.98(19) . 3_546 ? O3 C26 Tm1 59.30(18) . 3_546 ? C25 C26 Tm1 174.8(3) . 3_546 ? O5 C27A N1 118.2(6) . . ? O5 C27A H27A 120.9 . . ? N1 C27A H27A 120.9 . . ? N1 C28A H28A 109.5 . . ? N1 C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? N1 C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? N1 C29A H29A 109.5 . . ? N1 C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? N1 C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? O6 C30A N2 119.0(7) . . ? O6 C30A H30A 120.5 . . ? N2 C30A H30A 120.5 . . ? N2 C31A H31A 109.5 . . ? N2 C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? N2 C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? N2 C32A H32A 109.5 . . ? N2 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? N2 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? O5 C27B N1 110.1(14) . . ? O5 C27B H27B 124.9 . . ? N1 C27B H27B 124.9 . . ? N1 C28B H28D 109.5 . . ? N1 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? N1 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? N1 C29B H29D 109.5 . . ? N1 C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? N1 C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? N2 C30B O6 118.4(8) . . ? N2 C30B H30B 120.8 . . ? O6 C30B H30B 120.8 . . ? N2 C31B H31D 109.5 . . ? N2 C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? N2 C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? N2 C32B H32D 109.5 . . ? N2 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? N2 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Tm1 O1 C1 79.8(3) . . . . ? O2 Tm1 O1 C1 0.3(2) . . . . ? O6 Tm1 O1 C1 157.4(3) . . . . ? O3 Tm1 O1 C1 -172.5(5) 3_546 . . . ? O4 Tm1 O1 C1 -1.4(3) 3_546 . . . ? O8 Tm1 O1 C1 -129.3(3) . . . . ? O7 Tm1 O1 C1 -75.8(3) . . . . ? C26 Tm1 O1 C1 1.8(5) 3_546 . . . ? O5 Tm1 O2 C1 -98.2(3) . . . . ? O6 Tm1 O2 C1 -36.3(4) . . . . ? O3 Tm1 O2 C1 177.9(2) 3_546 . . . ? O4 Tm1 O2 C1 178.5(3) 3_546 . . . ? O8 Tm1 O2 C1 62.8(3) . . . . ? O1 Tm1 O2 C1 -0.3(2) . . . . ? O7 Tm1 O2 C1 97.9(3) . . . . ? C26 Tm1 O2 C1 -179.8(3) 3_546 . . . ? O2 Tm1 O5 C27A -166(3) . . . . ? O6 Tm1 O5 C27A 51(3) . . . . ? O3 Tm1 O5 C27A -31(3) 3_546 . . . ? O4 Tm1 O5 C27A -86(3) 3_546 . . . ? O8 Tm1 O5 C27A 49(3) . . . . ? O1 Tm1 O5 C27A 139(3) . . . . ? O7 Tm1 O5 C27A -125(3) . . . . ? C26 Tm1 O5 C27A -58(3) 3_546 . . . ? O2 Tm1 O5 C27B -48.6(10) . . . . ? O6 Tm1 O5 C27B 168.2(11) . . . . ? O3 Tm1 O5 C27B 86.4(10) 3_546 . . . ? O4 Tm1 O5 C27B 31.4(10) 3_546 . . . ? O8 Tm1 O5 C27B 166.7(10) . . . . ? O1 Tm1 O5 C27B -103.5(10) . . . . ? O7 Tm1 O5 C27B -7.5(12) . . . . ? C26 Tm1 O5 C27B 59.3(10) 3_546 . . . ? O5 Tm1 O6 C30A -128(2) . . . . ? O2 Tm1 O6 C30A 169(2) . . . . ? O3 Tm1 O6 C30A -35(2) 3_546 . . . ? O4 Tm1 O6 C30A -61(2) 3_546 . . . ? O8 Tm1 O6 C30A 52(2) . . . . ? O1 Tm1 O6 C30A 140(2) . . . . ? O7 Tm1 O6 C30A 50(2) . . . . ? C26 Tm1 O6 C30A -48(2) 3_546 . . . ? O5 Tm1 O6 C30B -69.1(6) . . . . ? O2 Tm1 O6 C30B -132.8(6) . . . . ? O3 Tm1 O6 C30B 23.4(6) 3_546 . . . ? O4 Tm1 O6 C30B -2.2(6) 3_546 . . . ? O8 Tm1 O6 C30B 110.1(6) . . . . ? O1 Tm1 O6 C30B -161.8(6) . . . . ? O7 Tm1 O6 C30B 108.7(6) . . . . ? C26 Tm1 O6 C30B 10.7(6) 3_546 . . . ? O5 Tm1 O7 N3 176.2(3) . . . . ? O2 Tm1 O7 N3 -142.2(3) . . . . ? O6 Tm1 O7 N3 1.4(4) . . . . ? O3 Tm1 O7 N3 82.3(3) 3_546 . . . ? O4 Tm1 O7 N3 136.8(3) 3_546 . . . ? O8 Tm1 O7 N3 -0.3(3) . . . . ? O1 Tm1 O7 N3 -87.4(3) . . . . ? C26 Tm1 O7 N3 109.8(3) 3_546 . . . ? O5 Tm1 O8 N3 -176.7(3) . . . . ? O2 Tm1 O8 N3 44.8(4) . . . . ? O6 Tm1 O8 N3 -178.3(4) . . . . ? O3 Tm1 O8 N3 -94.8(3) 3_546 . . . ? O4 Tm1 O8 N3 -48.6(4) 3_546 . . . ? O1 Tm1 O8 N3 92.2(3) . . . . ? O7 Tm1 O8 N3 0.3(3) . . . . ? C26 Tm1 O8 N3 -74.2(3) 3_546 . . . ? Tm1 O7 N3 O9 -179.5(6) . . . . ? Tm1 O7 N3 O8 0.5(6) . . . . ? Tm1 O8 N3 O9 179.5(6) . . . . ? Tm1 O8 N3 O7 -0.5(6) . . . . ? Tm1 O2 C1 O1 0.5(4) . . . . ? Tm1 O2 C1 C2 178.3(3) . . . . ? Tm1 O1 C1 O2 -0.5(4) . . . . ? Tm1 O1 C1 C2 -178.2(3) . . . . ? O2 C1 C2 C3 -6.0(6) . . . . ? O1 C1 C2 C3 171.7(4) . . . . ? O2 C1 C2 C7 173.9(4) . . . . ? O1 C1 C2 C7 -8.3(6) . . . . ? C7 C2 C3 C4 1.5(6) . . . . ? C1 C2 C3 C4 -178.6(4) . . . . ? C2 C3 C4 C5 -1.9(7) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? C4 C5 C6 C7 -0.5(6) . . . . ? C3 C2 C7 C6 -0.5(5) . . . . ? C1 C2 C7 C6 179.6(3) . . . . ? C3 C2 C7 S1 -179.6(3) . . . . ? C1 C2 C7 S1 0.5(5) . . . . ? C5 C6 C7 C2 0.0(5) . . . . ? C5 C6 C7 S1 179.1(3) . . . . ? C8 S1 C7 C2 -178.9(3) . . . . ? C8 S1 C7 C6 2.1(3) . . . . ? C7 S1 C8 C9 -175.1(3) . . . . ? S1 C8 C9 C17 -91.0(3) . . . . ? S1 C8 C9 C10 87.9(3) . . . . ? C17 C9 C10 C12 -1.0(5) . . . . ? C8 C9 C10 C12 -179.9(3) . . . . ? C17 C9 C10 C11 179.2(4) . . . . ? C8 C9 C10 C11 0.3(5) . . . . ? C9 C10 C12 C14 1.2(5) . . . . ? C11 C10 C12 C14 -178.9(4) . . . . ? C9 C10 C12 C13 -179.2(3) . . . . ? C11 C10 C12 C13 0.6(6) . . . . ? C10 C12 C14 C15 -0.5(5) . . . . ? C13 C12 C14 C15 180.0(4) . . . . ? C10 C12 C14 C19 178.2(3) . . . . ? C13 C12 C14 C19 -1.3(5) . . . . ? C12 C14 C15 C17 -0.6(5) . . . . ? C19 C14 C15 C17 -179.3(3) . . . . ? C12 C14 C15 C16 179.9(4) . . . . ? C19 C14 C15 C16 1.1(5) . . . . ? C10 C9 C17 C15 -0.1(5) . . . . ? C8 C9 C17 C15 178.8(3) . . . . ? C10 C9 C17 C18 -178.5(3) . . . . ? C8 C9 C17 C18 0.4(5) . . . . ? C14 C15 C17 C9 0.9(5) . . . . ? C16 C15 C17 C9 -179.6(3) . . . . ? C14 C15 C17 C18 179.3(3) . . . . ? C16 C15 C17 C18 -1.1(5) . . . . ? C12 C14 C19 S4 -88.4(4) . . . . ? C15 C14 C19 S4 90.3(3) . . . . ? C20 S4 C19 C14 -179.2(3) . . . . ? C19 S4 C20 C21 -1.1(3) . . . . ? C19 S4 C20 C25 179.1(3) . . . . ? C25 C20 C21 C22 -0.8(5) . . . . ? S4 C20 C21 C22 179.4(3) . . . . ? C20 C21 C22 C23 0.3(6) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C25 0.9(6) . . . . ? C23 C24 C25 C20 -1.4(6) . . . . ? C23 C24 C25 C26 178.2(3) . . . . ? C21 C20 C25 C24 1.3(5) . . . . ? S4 C20 C25 C24 -178.8(3) . . . . ? C21 C20 C25 C26 -178.3(3) . . . . ? S4 C20 C25 C26 1.6(5) . . . . ? Tm1 O4 C26 O3 -7.0(4) 3_546 . . . ? Tm1 O4 C26 C25 174.0(3) 3_546 . . . ? Tm1 O3 C26 O4 7.0(4) 3_546 . . . ? Tm1 O3 C26 C25 -173.9(3) 3_546 . . . ? C24 C25 C26 O4 -1.9(5) . . . . ? C20 C25 C26 O4 177.6(4) . . . . ? C24 C25 C26 O3 179.0(4) . . . . ? C20 C25 C26 O3 -1.4(6) . . . . ? C24 C25 C26 Tm1 92(3) . . . 3_546 ? C20 C25 C26 Tm1 -89(3) . . . 3_546 ? C27B O5 C27A N1 -6.8(11) . . . . ? Tm1 O5 C27A N1 115(3) . . . . ? C28B N1 C27A O5 -172.6(17) . . . . ? C28A N1 C27A O5 -0.9(10) . . . . ? C27B N1 C27A O5 6.5(11) . . . . ? C29A N1 C27A O5 179.2(6) . . . . ? C29B N1 C27A O5 34(9) . . . . ? C30B O6 C30A N2 12.7(8) . . . . ? Tm1 O6 C30A N2 77(2) . . . . ? C30B N2 C30A O6 -13.1(8) . . . . ? C31A N2 C30A O6 -3.2(13) . . . . ? C31B N2 C30A O6 144.1(13) . . . . ? C32B N2 C30A O6 -113(4) . . . . ? C32A N2 C30A O6 -170.9(10) . . . . ? C27A O5 C27B N1 5.9(10) . . . . ? Tm1 O5 C27B N1 -164.5(8) . . . . ? C28B N1 C27B O5 -5(2) . . . . ? C27A N1 C27B O5 -6.0(10) . . . . ? C28A N1 C27B O5 167.0(19) . . . . ? C29A N1 C27B O5 -94(9) . . . . ? C29B N1 C27B O5 177.8(15) . . . . ? C30A N2 C30B O6 12.5(8) . . . . ? C31A N2 C30B O6 -158.2(12) . . . . ? C31B N2 C30B O6 -11.8(15) . . . . ? C32B N2 C30B O6 176.5(9) . . . . ? C32A N2 C30B O6 106(2) . . . . ? C30A O6 C30B N2 -13.0(8) . . . . ? Tm1 O6 C30B N2 -179.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.818 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.081 # Attachment '- 2.cif' data_QQ _database_code_depnum_ccdc_archive 'CCDC 775312' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H24 N2 O4 S2 Zn,2(H~2~O)' _chemical_formula_sum 'C34 H28 N2 O6 S2 Zn' _chemical_formula_weight 694.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.8023(6) _cell_length_b 31.614(2) _cell_length_c 15.2690(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.204(2) _cell_angle_gamma 90.00 _cell_volume 3666.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2389 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 20.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8657 _exptl_absorpt_correction_T_max 0.9369 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; No H atom on H~2~O molecules can be located since the water molecules in the structure are heavily disordered. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15623 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 23.29 _reflns_number_total 5253 _reflns_number_gt 3543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT+ (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2007)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1342P)^2^+3.9679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5253 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.2053 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.24394(9) 0.38523(2) -0.01841(6) 0.0615(3) Uani 1 1 d . . . S1 S 0.44911(19) 0.31443(6) 0.29416(11) 0.0607(5) Uani 1 1 d . . . S2 S 0.03388(19) 0.30558(6) 0.70361(10) 0.0583(5) Uani 1 1 d . . . O1 O 0.3347(5) 0.35263(18) 0.1298(3) 0.0822(16) Uani 1 1 d . . . O2 O 0.4824(5) 0.36166(14) 0.0281(3) 0.0594(11) Uani 1 1 d . . . O3 O 0.1438(5) 0.34008(16) 0.8694(3) 0.0685(13) Uani 1 1 d . . . O4 O -0.0185(5) 0.36940(15) 0.9500(3) 0.0669(13) Uani 1 1 d . . . O5A O 0.211(10) 0.5696(18) 0.359(4) 0.58(6) Uani 0.55(5) 1 d P . . O5B O 0.263(8) 0.5916(12) 0.395(5) 0.42(4) Uani 0.45(5) 1 d P . . O6A O 0.125(6) 0.4298(8) 0.3643(16) 0.51(3) Uani 0.69(2) 1 d P . . O6B O 0.470(5) 0.4274(9) 0.339(2) 0.23(3) Uani 0.31(2) 1 d P . . N1 N 0.2244(7) 0.4452(2) 0.0411(5) 0.0848(19) Uani 1 1 d . . . N2 N 0.2880(8) 0.4292(2) -0.1213(4) 0.0794(18) Uani 1 1 d . . . C1 C 0.4747(8) 0.34933(19) 0.1052(4) 0.0488(15) Uani 1 1 d . . . C2 C 0.6374(7) 0.33194(19) 0.1653(4) 0.0454(14) Uani 1 1 d . . . C3 C 0.7929(8) 0.3331(2) 0.1347(4) 0.0550(16) Uani 1 1 d . . . H3 H 0.7899 0.3438 0.0776 0.066 Uiso 1 1 calc R . . C4 C 0.9488(8) 0.3190(2) 0.1860(4) 0.0628(18) Uani 1 1 d . . . H4 H 1.0508 0.3204 0.1644 0.075 Uiso 1 1 calc R . . C5 C 0.9538(8) 0.3027(2) 0.2690(5) 0.0657(19) Uani 1 1 d . . . H5 H 1.0589 0.2922 0.3036 0.079 Uiso 1 1 calc R . . C6 C 0.8037(8) 0.3018(2) 0.3019(4) 0.0654(19) Uani 1 1 d . . . H6 H 0.8100 0.2910 0.3592 0.078 Uiso 1 1 calc R . . C7 C 0.6427(7) 0.3165(2) 0.2520(4) 0.0516(15) Uani 1 1 d . . . C8 C 0.5323(8) 0.2945(2) 0.4067(4) 0.0631(18) Uani 1 1 d . . . H8A H 0.5823 0.2665 0.4042 0.076 Uiso 1 1 calc R . . H8B H 0.6240 0.3130 0.4394 0.076 Uiso 1 1 calc R . . C9 C 0.3824(8) 0.2923(2) 0.4543(4) 0.0549(16) Uani 1 1 d . . . C10 C 0.3132(9) 0.3291(2) 0.4804(5) 0.0692(19) Uani 1 1 d . . . H10 H 0.3591 0.3551 0.4688 0.083 Uiso 1 1 calc R . . C11 C 0.1741(9) 0.3275(2) 0.5245(5) 0.069(2) Uani 1 1 d . . . H11 H 0.1290 0.3525 0.5422 0.083 Uiso 1 1 calc R . . C12 C 0.1032(8) 0.2893(2) 0.5419(4) 0.0537(16) Uani 1 1 d . . . C13 C 0.1749(9) 0.2530(2) 0.5153(4) 0.0639(18) Uani 1 1 d . . . H13 H 0.1302 0.2270 0.5276 0.077 Uiso 1 1 calc R . . C14 C 0.3099(9) 0.2539(2) 0.4713(4) 0.0612(17) Uani 1 1 d . . . H14 H 0.3529 0.2287 0.4529 0.073 Uiso 1 1 calc R . . C15 C -0.0468(8) 0.2880(2) 0.5885(4) 0.0622(18) Uani 1 1 d . . . H15A H -0.0922 0.2594 0.5878 0.075 Uiso 1 1 calc R . . H15B H -0.1413 0.3063 0.5578 0.075 Uiso 1 1 calc R . . C16 C -0.1631(7) 0.3079(2) 0.7434(4) 0.0484(15) Uani 1 1 d . . . C17 C -0.3202(8) 0.2910(2) 0.6936(4) 0.0632(18) Uani 1 1 d . . . H17 H -0.3214 0.2776 0.6392 0.076 Uiso 1 1 calc R . . C18 C -0.4731(8) 0.2937(2) 0.7232(5) 0.0660(19) Uani 1 1 d . . . H18 H -0.5768 0.2825 0.6885 0.079 Uiso 1 1 calc R . . C19 C -0.4739(8) 0.3129(2) 0.8035(4) 0.0592(17) Uani 1 1 d . . . H19 H -0.5774 0.3145 0.8238 0.071 Uiso 1 1 calc R . . C20 C -0.3219(7) 0.3297(2) 0.8533(4) 0.0523(16) Uani 1 1 d . . . H20 H -0.3237 0.3430 0.9074 0.063 Uiso 1 1 calc R . . C21 C -0.1640(7) 0.32757(18) 0.8258(4) 0.0429(13) Uani 1 1 d . . . C22 C -0.0057(8) 0.34660(19) 0.8846(4) 0.0480(14) Uani 1 1 d . . . C23 C 0.1905(10) 0.4501(4) 0.1188(6) 0.102(3) Uani 1 1 d . . . H23 H 0.1737 0.4266 0.1525 0.122 Uiso 1 1 calc R . . C24 C 0.1782(13) 0.4931(4) 0.1548(8) 0.107(3) Uani 1 1 d . . . H24 H 0.1556 0.4970 0.2115 0.129 Uiso 1 1 calc R . . C25 C 0.2007(12) 0.5273(4) 0.1028(9) 0.116(4) Uani 1 1 d . . . H25 H 0.1889 0.5547 0.1227 0.139 Uiso 1 1 calc R . . C26 C 0.2431(9) 0.5200(3) 0.0169(8) 0.091(3) Uani 1 1 d . . . C27 C 0.2659(13) 0.5531(3) -0.0326(11) 0.126(4) Uani 1 1 d . . . H27 H 0.2553 0.5807 -0.0133 0.151 Uiso 1 1 calc R . . C28 C 0.3065(12) 0.5445(4) -0.1147(11) 0.119(4) Uani 1 1 d . . . H28 H 0.3305 0.5672 -0.1489 0.143 Uiso 1 1 calc R . . C29 C 0.3134(10) 0.5034(3) -0.1492(8) 0.090(3) Uani 1 1 d . . . C30 C 0.3431(15) 0.4938(4) -0.2324(10) 0.131(4) Uani 1 1 d . . . H30 H 0.3627 0.5156 -0.2698 0.158 Uiso 1 1 calc R . . C31 C 0.3444(15) 0.4534(5) -0.2612(7) 0.135(4) Uani 1 1 d . . . H31 H 0.3637 0.4471 -0.3176 0.163 Uiso 1 1 calc R . . C32 C 0.3145(13) 0.4200(3) -0.2006(7) 0.110(3) Uani 1 1 d . . . H32 H 0.3142 0.3919 -0.2185 0.132 Uiso 1 1 calc R . . C33 C 0.2855(9) 0.4692(3) -0.0955(6) 0.083(2) Uani 1 1 d . . . C34 C 0.2500(7) 0.4782(2) -0.0081(5) 0.0613(18) 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 Zn1 0.0401(5) 0.0620(5) 0.0772(6) -0.0016(4) 0.0028(4) -0.0004(3) S1 0.0323(8) 0.1065(14) 0.0460(9) 0.0170(9) 0.0144(7) 0.0037(8) S2 0.0320(8) 0.1022(13) 0.0432(9) -0.0164(8) 0.0137(7) -0.0028(8) O1 0.035(2) 0.139(5) 0.075(3) 0.037(3) 0.018(2) 0.008(3) O2 0.050(3) 0.081(3) 0.048(3) 0.009(2) 0.011(2) 0.008(2) O3 0.033(2) 0.106(4) 0.066(3) -0.028(3) 0.009(2) 0.000(2) O4 0.050(3) 0.092(3) 0.062(3) -0.031(3) 0.019(2) -0.013(2) O5A 1.09(14) 0.33(5) 0.55(7) -0.22(5) 0.64(10) -0.25(7) O5B 0.55(8) 0.12(3) 0.57(9) 0.03(4) 0.06(7) 0.15(4) O6A 0.94(9) 0.30(3) 0.28(3) 0.21(2) 0.12(3) 0.31(4) O6B 0.27(4) 0.15(3) 0.22(3) 0.14(2) -0.03(3) -0.08(2) N1 0.044(4) 0.101(5) 0.100(5) -0.003(4) -0.004(3) 0.007(3) N2 0.073(4) 0.089(5) 0.072(4) 0.006(4) 0.008(3) 0.005(4) C1 0.042(4) 0.060(4) 0.045(4) 0.000(3) 0.009(3) -0.009(3) C2 0.031(3) 0.067(4) 0.039(3) -0.002(3) 0.009(2) -0.003(3) C3 0.045(4) 0.077(4) 0.046(4) 0.001(3) 0.018(3) -0.005(3) C4 0.031(3) 0.102(5) 0.058(4) 0.007(4) 0.016(3) -0.002(3) C5 0.030(3) 0.107(6) 0.059(4) 0.007(4) 0.007(3) 0.003(3) C6 0.036(3) 0.111(6) 0.049(4) 0.016(4) 0.008(3) 0.006(4) C7 0.034(3) 0.078(4) 0.043(3) 0.010(3) 0.011(3) -0.002(3) C8 0.043(4) 0.108(5) 0.038(4) 0.015(3) 0.010(3) 0.003(4) C9 0.047(4) 0.086(5) 0.033(3) 0.003(3) 0.011(3) 0.009(3) C10 0.071(5) 0.079(5) 0.064(4) 0.010(4) 0.028(4) -0.006(4) C11 0.074(5) 0.081(5) 0.061(4) -0.004(4) 0.030(4) 0.016(4) C12 0.047(4) 0.086(5) 0.030(3) -0.007(3) 0.013(3) -0.002(3) C13 0.064(4) 0.077(5) 0.058(4) -0.010(4) 0.029(4) -0.012(4) C14 0.070(4) 0.068(5) 0.052(4) -0.005(3) 0.028(4) -0.001(4) C15 0.047(4) 0.097(5) 0.043(4) -0.011(3) 0.012(3) -0.002(4) C16 0.028(3) 0.074(4) 0.044(3) -0.003(3) 0.011(3) -0.001(3) C17 0.038(4) 0.097(5) 0.056(4) -0.021(4) 0.013(3) -0.004(3) C18 0.030(3) 0.102(5) 0.064(5) -0.001(4) 0.007(3) -0.004(3) C19 0.035(3) 0.088(5) 0.061(4) -0.001(4) 0.024(3) 0.001(3) C20 0.043(4) 0.077(4) 0.042(3) -0.004(3) 0.019(3) 0.001(3) C21 0.035(3) 0.060(4) 0.036(3) -0.001(3) 0.013(2) 0.001(3) C22 0.042(4) 0.060(4) 0.042(3) 0.001(3) 0.010(3) 0.005(3) C23 0.056(5) 0.177(10) 0.070(6) -0.031(6) 0.009(4) 0.004(5) C24 0.087(7) 0.108(8) 0.119(8) -0.030(7) 0.007(6) 0.022(6) C25 0.066(6) 0.142(11) 0.128(9) -0.051(8) -0.001(6) 0.019(6) C26 0.045(4) 0.054(5) 0.154(9) 0.006(5) -0.019(5) 0.004(4) C27 0.072(7) 0.071(7) 0.215(14) -0.007(9) -0.010(8) 0.008(5) C28 0.060(6) 0.093(9) 0.190(13) 0.022(8) 0.001(7) -0.008(5) C29 0.050(5) 0.103(8) 0.113(8) 0.041(6) 0.009(5) -0.004(4) C30 0.109(9) 0.120(10) 0.168(13) 0.046(9) 0.036(8) 0.004(7) C31 0.154(11) 0.174(12) 0.094(8) 0.044(8) 0.062(7) 0.011(9) C32 0.128(8) 0.122(8) 0.089(7) 0.018(6) 0.044(6) 0.016(6) C33 0.043(4) 0.087(6) 0.109(7) 0.019(5) -0.004(4) -0.005(4) C34 0.040(4) 0.066(5) 0.071(5) 0.011(4) -0.001(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.979(4) . ? Zn1 O4 2.056(4) 1_554 ? Zn1 N1 2.123(7) . ? Zn1 N2 2.183(7) . ? Zn1 O3 2.229(4) 1_554 ? Zn1 O1 2.440(5) . ? Zn1 C22 2.482(6) 1_554 ? Zn1 C1 2.557(6) . ? S1 C7 1.773(5) . ? S1 C8 1.806(6) . ? S2 C16 1.779(5) . ? S2 C15 1.814(6) . ? O1 C1 1.238(6) . ? O2 C1 1.255(7) . ? O3 C22 1.257(6) . ? O3 Zn1 2.229(4) 1_556 ? O4 C22 1.253(7) . ? O4 Zn1 2.056(4) 1_556 ? N1 C23 1.283(10) . ? N1 C34 1.327(9) . ? N2 C32 1.307(10) . ? N2 C33 1.326(10) . ? C1 C2 1.491(8) . ? C2 C3 1.396(7) . ? C2 C7 1.403(8) . ? C3 C4 1.363(8) . ? C3 H3 0.9300 . ? C4 C5 1.360(9) . ? C4 H4 0.9300 . ? C5 C6 1.376(8) . ? C5 H5 0.9300 . ? C6 C7 1.391(8) . ? C6 H6 0.9300 . ? C8 C9 1.512(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.379(9) . ? C9 C14 1.391(9) . ? C10 C11 1.403(9) . ? C10 H10 0.9300 . ? C11 C12 1.378(9) . ? C11 H11 0.9300 . ? C12 C13 1.378(9) . ? C12 C15 1.503(8) . ? C13 C14 1.373(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.394(8) . ? C16 C21 1.404(8) . ? C17 C18 1.371(8) . ? C17 H17 0.9300 . ? C18 C19 1.369(9) . ? C18 H18 0.9300 . ? C19 C20 1.363(8) . ? C19 H19 0.9300 . ? C20 C21 1.391(7) . ? C20 H20 0.9300 . ? C21 C22 1.479(8) . ? C22 Zn1 2.482(6) 1_556 ? C23 C24 1.478(13) . ? C23 H23 0.9300 . ? C24 C25 1.376(14) . ? C24 H24 0.9300 . ? C25 C26 1.442(13) . ? C25 H25 0.9300 . ? C26 C27 1.326(15) . ? C26 C34 1.382(11) . ? C27 C28 1.389(15) . ? C27 H27 0.9300 . ? C28 C29 1.407(14) . ? C28 H28 0.9300 . ? C29 C30 1.378(14) . ? C29 C33 1.403(11) . ? C30 C31 1.351(15) . ? C30 H30 0.9300 . ? C31 C32 1.456(13) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.451(11) . ? O5A O5B 0.92(7) . ? 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 Zn1 O4 142.8(2) . 1_554 ? O2 Zn1 N1 109.7(2) . . ? O4 Zn1 N1 98.8(2) 1_554 . ? O2 Zn1 N2 102.0(2) . . ? O4 Zn1 N2 107.4(2) 1_554 . ? N1 Zn1 N2 77.2(3) . . ? O2 Zn1 O3 99.80(17) . 1_554 ? O4 Zn1 O3 60.54(15) 1_554 1_554 ? N1 Zn1 O3 148.6(2) . 1_554 ? N2 Zn1 O3 86.6(2) . 1_554 ? O2 Zn1 O1 57.22(15) . . ? O4 Zn1 O1 100.22(17) 1_554 . ? N1 Zn1 O1 90.8(3) . . ? N2 Zn1 O1 151.2(2) . . ? O3 Zn1 O1 114.7(2) 1_554 . ? O2 Zn1 C22 125.03(19) . 1_554 ? O4 Zn1 C22 30.24(16) 1_554 1_554 ? N1 Zn1 C22 124.8(2) . 1_554 ? N2 Zn1 C22 96.6(2) . 1_554 ? O3 Zn1 C22 30.36(15) 1_554 1_554 ? O1 Zn1 C22 111.55(18) . 1_554 ? O2 Zn1 C1 28.66(16) . . ? O4 Zn1 C1 124.13(19) 1_554 . ? N1 Zn1 C1 100.8(2) . . ? N2 Zn1 C1 127.8(2) . . ? O3 Zn1 C1 110.29(18) 1_554 . ? O1 Zn1 C1 28.57(15) . . ? C22 Zn1 C1 123.1(2) 1_554 . ? C7 S1 C8 102.0(3) . . ? C16 S2 C15 102.0(3) . . ? C1 O1 Zn1 81.0(3) . . ? C1 O2 Zn1 102.2(4) . . ? C22 O3 Zn1 86.0(3) . 1_556 ? C22 O4 Zn1 94.1(3) . 1_556 ? C23 N1 C34 121.2(9) . . ? C23 N1 Zn1 123.7(7) . . ? C34 N1 Zn1 115.1(6) . . ? C32 N2 C33 120.3(8) . . ? C32 N2 Zn1 127.5(7) . . ? C33 N2 Zn1 112.2(6) . . ? O1 C1 O2 119.6(6) . . ? O1 C1 C2 122.0(5) . . ? O2 C1 C2 118.4(5) . . ? O1 C1 Zn1 70.4(3) . . ? O2 C1 Zn1 49.2(3) . . ? C2 C1 Zn1 167.1(4) . . ? C3 C2 C7 118.9(5) . . ? C3 C2 C1 117.8(5) . . ? C7 C2 C1 123.1(5) . . ? C4 C3 C2 121.9(6) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C5 C4 C3 119.4(6) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.2(6) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 122.0(6) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C2 117.5(5) . . ? C6 C7 S1 121.8(4) . . ? C2 C7 S1 120.7(4) . . ? C9 C8 S1 108.9(4) . . ? C9 C8 H8A 109.9 . . ? S1 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? S1 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C14 118.7(6) . . ? C10 C9 C8 119.9(6) . . ? C14 C9 C8 121.4(6) . . ? C9 C10 C11 120.3(6) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.9(6) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 117.7(6) . . ? C11 C12 C15 120.4(6) . . ? C13 C12 C15 121.9(6) . . ? C14 C13 C12 122.4(6) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C9 119.9(6) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? C12 C15 S2 108.4(4) . . ? C12 C15 H15A 110.0 . . ? S2 C15 H15A 110.0 . . ? C12 C15 H15B 110.0 . . ? S2 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? C17 C16 C21 118.4(5) . . ? C17 C16 S2 121.2(4) . . ? C21 C16 S2 120.4(4) . . ? C18 C17 C16 121.2(6) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C17 120.3(6) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 119.4(5) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 122.0(5) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 118.6(5) . . ? C20 C21 C22 118.1(5) . . ? C16 C21 C22 123.4(5) . . ? O4 C22 O3 119.1(5) . . ? O4 C22 C21 120.7(5) . . ? O3 C22 C21 120.2(5) . . ? O4 C22 Zn1 55.7(3) . 1_556 ? O3 C22 Zn1 63.6(3) . 1_556 ? C21 C22 Zn1 174.4(4) . 1_556 ? N1 C23 C24 120.0(11) . . ? N1 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 118.7(11) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 119.1(10) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C34 125.4(12) . . ? C27 C26 C25 118.7(12) . . ? C34 C26 C25 115.8(9) . . ? C26 C27 C28 116.5(11) . . ? C26 C27 H27 121.7 . . ? C28 C27 H27 121.7 . . ? C27 C28 C29 123.7(11) . . ? C27 C28 H28 118.1 . . ? C29 C28 H28 118.1 . . ? C30 C29 C33 116.7(11) . . ? C30 C29 C28 125.3(11) . . ? C33 C29 C28 117.9(11) . . ? C31 C30 C29 121.6(11) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C32 117.7(11) . . ? C30 C31 H31 121.2 . . ? C32 C31 H31 121.2 . . ? N2 C32 C31 120.6(10) . . ? N2 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? N2 C33 C29 123.1(10) . . ? N2 C33 C34 118.6(7) . . ? C29 C33 C34 118.3(9) . . ? N1 C34 C26 125.1(8) . . ? N1 C34 C33 116.9(7) . . ? C26 C34 C33 118.0(8) . . ? 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 O2 Zn1 O1 C1 1.5(4) . . . . ? O4 Zn1 O1 C1 149.4(4) 1_554 . . . ? N1 Zn1 O1 C1 -111.5(4) . . . . ? N2 Zn1 O1 C1 -47.3(7) . . . . ? O3 Zn1 O1 C1 87.3(4) 1_554 . . . ? C22 Zn1 O1 C1 120.2(4) 1_554 . . . ? O4 Zn1 O2 C1 -61.5(5) 1_554 . . . ? N1 Zn1 O2 C1 76.3(4) . . . . ? N2 Zn1 O2 C1 156.7(4) . . . . ? O3 Zn1 O2 C1 -114.7(4) 1_554 . . . ? O1 Zn1 O2 C1 -1.5(4) . . . . ? C22 Zn1 O2 C1 -96.2(4) 1_554 . . . ? O2 Zn1 N1 C23 -82.9(6) . . . . ? O4 Zn1 N1 C23 72.8(6) 1_554 . . . ? N2 Zn1 N1 C23 178.7(6) . . . . ? O3 Zn1 N1 C23 118.2(7) 1_554 . . . ? O1 Zn1 N1 C23 -27.7(6) . . . . ? C22 Zn1 N1 C23 89.6(6) 1_554 . . . ? C1 Zn1 N1 C23 -54.6(6) . . . . ? O2 Zn1 N1 C34 97.1(5) . . . . ? O4 Zn1 N1 C34 -107.2(5) 1_554 . . . ? N2 Zn1 N1 C34 -1.3(4) . . . . ? O3 Zn1 N1 C34 -61.8(7) 1_554 . . . ? O1 Zn1 N1 C34 152.3(5) . . . . ? C22 Zn1 N1 C34 -90.4(5) 1_554 . . . ? C1 Zn1 N1 C34 125.4(4) . . . . ? O2 Zn1 N2 C32 74.1(8) . . . . ? O4 Zn1 N2 C32 -82.9(8) 1_554 . . . ? N1 Zn1 N2 C32 -178.2(8) . . . . ? O3 Zn1 N2 C32 -25.2(7) 1_554 . . . ? O1 Zn1 N2 C32 114.4(8) . . . . ? C22 Zn1 N2 C32 -53.9(8) 1_554 . . . ? C1 Zn1 N2 C32 87.9(8) . . . . ? O2 Zn1 N2 C33 -106.1(5) . . . . ? O4 Zn1 N2 C33 97.0(5) 1_554 . . . ? N1 Zn1 N2 C33 1.6(5) . . . . ? O3 Zn1 N2 C33 154.6(5) 1_554 . . . ? O1 Zn1 N2 C33 -65.8(7) . . . . ? C22 Zn1 N2 C33 125.9(5) 1_554 . . . ? C1 Zn1 N2 C33 -92.2(5) . . . . ? Zn1 O1 C1 O2 -2.3(5) . . . . ? Zn1 O1 C1 C2 176.3(6) . . . . ? Zn1 O2 C1 O1 2.9(7) . . . . ? Zn1 O2 C1 C2 -175.8(4) . . . . ? O2 Zn1 C1 O1 -177.4(6) . . . . ? O4 Zn1 C1 O1 -37.2(4) 1_554 . . . ? N1 Zn1 C1 O1 71.3(4) . . . . ? N2 Zn1 C1 O1 153.4(4) . . . . ? O3 Zn1 C1 O1 -104.7(4) 1_554 . . . ? C22 Zn1 C1 O1 -73.7(4) 1_554 . . . ? O4 Zn1 C1 O2 140.1(4) 1_554 . . . ? N1 Zn1 C1 O2 -111.4(4) . . . . ? N2 Zn1 C1 O2 -29.3(5) . . . . ? O3 Zn1 C1 O2 72.6(4) 1_554 . . . ? O1 Zn1 C1 O2 177.4(6) . . . . ? C22 Zn1 C1 O2 103.6(4) 1_554 . . . ? O2 Zn1 C1 C2 16.9(17) . . . . ? O4 Zn1 C1 C2 157.0(18) 1_554 . . . ? N1 Zn1 C1 C2 -94.4(19) . . . . ? O3 Zn1 C1 C2 89.6(19) 1_554 . . . ? C22 Zn1 C1 C2 120.6(19) 1_554 . . . ? O1 C1 C2 C3 -174.2(6) . . . . ? O2 C1 C2 C3 4.4(8) . . . . ? Zn1 C1 C2 C3 -10(2) . . . . ? O1 C1 C2 C7 2.7(10) . . . . ? O2 C1 C2 C7 -178.7(6) . . . . ? Zn1 C1 C2 C7 166.8(16) . . . . ? C7 C2 C3 C4 1.1(10) . . . . ? C1 C2 C3 C4 178.2(6) . . . . ? C2 C3 C4 C5 0.9(11) . . . . ? C3 C4 C5 C6 -2.0(11) . . . . ? C4 C5 C6 C7 1.1(12) . . . . ? C5 C6 C7 C2 0.9(11) . . . . ? C5 C6 C7 S1 179.0(6) . . . . ? C3 C2 C7 C6 -2.0(9) . . . . ? C1 C2 C7 C6 -178.9(6) . . . . ? C3 C2 C7 S1 179.9(5) . . . . ? C1 C2 C7 S1 3.1(9) . . . . ? C8 S1 C7 C6 4.1(7) . . . . ? C8 S1 C7 C2 -177.9(5) . . . . ? C7 S1 C8 C9 177.8(5) . . . . ? S1 C8 C9 C10 -71.6(7) . . . . ? S1 C8 C9 C14 107.4(6) . . . . ? C14 C9 C10 C11 0.9(10) . . . . ? C8 C9 C10 C11 179.9(6) . . . . ? C9 C10 C11 C12 -0.4(11) . . . . ? C10 C11 C12 C13 0.6(10) . . . . ? C10 C11 C12 C15 -179.5(6) . . . . ? C11 C12 C13 C14 -1.3(10) . . . . ? C15 C12 C13 C14 178.9(6) . . . . ? C12 C13 C14 C9 1.7(11) . . . . ? C10 C9 C14 C13 -1.5(10) . . . . ? C8 C9 C14 C13 179.5(6) . . . . ? C11 C12 C15 S2 -68.0(7) . . . . ? C13 C12 C15 S2 111.9(6) . . . . ? C16 S2 C15 C12 173.4(5) . . . . ? C15 S2 C16 C17 10.6(6) . . . . ? C15 S2 C16 C21 -168.6(5) . . . . ? C21 C16 C17 C18 0.8(10) . . . . ? S2 C16 C17 C18 -178.4(6) . . . . ? C16 C17 C18 C19 -0.7(11) . . . . ? C17 C18 C19 C20 0.7(11) . . . . ? C18 C19 C20 C21 -0.9(10) . . . . ? C19 C20 C21 C16 0.9(9) . . . . ? C19 C20 C21 C22 -179.8(6) . . . . ? C17 C16 C21 C20 -0.8(9) . . . . ? S2 C16 C21 C20 178.3(5) . . . . ? C17 C16 C21 C22 179.9(6) . . . . ? S2 C16 C21 C22 -0.9(8) . . . . ? Zn1 O4 C22 O3 5.0(6) 1_556 . . . ? Zn1 O4 C22 C21 -174.9(5) 1_556 . . . ? Zn1 O3 C22 O4 -4.6(6) 1_556 . . . ? Zn1 O3 C22 C21 175.3(5) 1_556 . . . ? C20 C21 C22 O4 -10.5(9) . . . . ? C16 C21 C22 O4 168.7(6) . . . . ? C20 C21 C22 O3 169.6(6) . . . . ? C16 C21 C22 O3 -11.2(9) . . . . ? C34 N1 C23 C24 0.4(11) . . . . ? Zn1 N1 C23 C24 -179.6(6) . . . . ? N1 C23 C24 C25 1.1(13) . . . . ? C23 C24 C25 C26 -2.7(14) . . . . ? C24 C25 C26 C27 -179.5(9) . . . . ? C24 C25 C26 C34 2.7(12) . . . . ? C34 C26 C27 C28 -2.5(14) . . . . ? C25 C26 C27 C28 180.0(8) . . . . ? C26 C27 C28 C29 4.0(15) . . . . ? C27 C28 C29 C30 176.0(10) . . . . ? C27 C28 C29 C33 -3.0(14) . . . . ? C33 C29 C30 C31 0.3(16) . . . . ? C28 C29 C30 C31 -178.7(10) . . . . ? C29 C30 C31 C32 -0.5(18) . . . . ? C33 N2 C32 C31 1.0(14) . . . . ? Zn1 N2 C32 C31 -179.1(7) . . . . ? C30 C31 C32 N2 -0.2(17) . . . . ? C32 N2 C33 C29 -1.2(12) . . . . ? Zn1 N2 C33 C29 178.9(6) . . . . ? C32 N2 C33 C34 178.0(7) . . . . ? Zn1 N2 C33 C34 -1.9(8) . . . . ? C30 C29 C33 N2 0.5(12) . . . . ? C28 C29 C33 N2 179.6(7) . . . . ? C30 C29 C33 C34 -178.7(8) . . . . ? C28 C29 C33 C34 0.4(11) . . . . ? C23 N1 C34 C26 -0.2(10) . . . . ? Zn1 N1 C34 C26 179.7(5) . . . . ? C23 N1 C34 C33 -179.3(6) . . . . ? Zn1 N1 C34 C33 0.7(7) . . . . ? C27 C26 C34 N1 -178.9(8) . . . . ? C25 C26 C34 N1 -1.3(10) . . . . ? C27 C26 C34 C33 0.1(11) . . . . ? C25 C26 C34 C33 177.7(6) . . . . ? N2 C33 C34 N1 0.8(9) . . . . ? C29 C33 C34 N1 -179.9(6) . . . . ? N2 C33 C34 C26 -178.3(6) . . . . ? C29 C33 C34 C26 1.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.3 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.259 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.100 # Attachment '- 3.cif' data_test3 _database_code_depnum_ccdc_archive 'CCDC 775313' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H39 O11 Zn2, (H~2~O)' _chemical_formula_sum 'C39 H41 O12 Zn2' _chemical_formula_weight 832.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 12.2854(19) _cell_length_b 13.199(2) _cell_length_c 14.514(2) _cell_angle_alpha 66.739(2) _cell_angle_beta 65.433(3) _cell_angle_gamma 63.684(2) _cell_volume 1853.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1560 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 20.2 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 862 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8327 _exptl_absorpt_correction_T_max 0.9230 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11030 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.1037 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8032 _reflns_number_gt 4426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT+ (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2007)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints have been used to control the refinement of H atoms bonded to O7, O11 and O12. ; _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^)+(0.0440P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8032 _refine_ls_number_parameters 498 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.24375(5) 0.88489(4) 0.36732(4) 0.03952(16) Uani 1 1 d . . . Zn2 Zn 0.03303(5) 1.11348(4) 0.46933(4) 0.04031(16) Uani 1 1 d . . . O1 O -0.0812(3) 1.2442(3) 0.3891(2) 0.0570(9) Uani 1 1 d . . . O2 O -0.2651(3) 1.2540(3) 0.5159(3) 0.0584(9) Uani 1 1 d . . . O3 O -0.1507(3) 1.3717(3) 0.2057(2) 0.0532(9) Uani 1 1 d . . . O4 O 0.2740(3) 0.9303(3) 0.0224(2) 0.0599(10) Uani 1 1 d . . . O5 O 0.3204(3) 0.8450(3) 0.2360(2) 0.0581(9) Uani 1 1 d . . . O6 O 0.2010(5) 0.7434(5) 0.2721(4) 0.124(2) Uani 1 1 d . . . O7 O 0.0652(3) 0.9831(2) 0.4038(2) 0.0389(7) Uani 1 1 d D . . O8 O 0.3533(3) 0.9584(3) 0.3628(3) 0.0639(10) Uani 1 1 d . . . O9 O 0.2091(3) 1.1119(3) 0.4188(3) 0.0706(11) Uani 1 1 d . . . O10 O 0.2879(3) 1.2630(3) 0.4236(3) 0.0746(11) Uani 1 1 d . . . O11 O 0.0078(5) 1.2108(4) 0.5662(4) 0.0816(13) Uani 1 1 d D . . O12 O -0.0234(6) 1.0657(6) 0.2347(5) 0.1213(19) Uani 1 1 d D . . C1 C -0.1971(5) 1.2951(4) 0.4286(4) 0.0453(12) Uani 1 1 d . . . C2 C -0.2603(4) 1.4157(4) 0.3704(4) 0.0421(11) Uani 1 1 d . . . C3 C -0.3517(4) 1.4959(4) 0.4271(4) 0.0500(12) Uani 1 1 d . . . H3 H -0.3730 1.4715 0.4999 0.060 Uiso 1 1 calc R . . C4 C -0.4129(5) 1.6106(4) 0.3804(4) 0.0592(14) Uani 1 1 d . . . H4 H -0.4725 1.6624 0.4210 0.071 Uiso 1 1 calc R . . C5 C -0.3839(5) 1.6462(4) 0.2733(4) 0.0615(15) Uani 1 1 d . . . H5 H -0.4247 1.7225 0.2405 0.074 Uiso 1 1 calc R . . C6 C -0.2939(5) 1.5687(4) 0.2138(4) 0.0577(14) Uani 1 1 d . . . H6 H -0.2735 1.5941 0.1411 0.069 Uiso 1 1 calc R . . C7 C -0.2341(4) 1.4546(4) 0.2604(4) 0.0471(12) Uani 1 1 d . . . C8 C -0.1055(5) 1.4158(4) 0.0942(4) 0.0585(14) Uani 1 1 d . . . H8A H -0.0703 1.4757 0.0783 0.070 Uiso 1 1 calc R . . H8B H -0.1748 1.4501 0.0637 0.070 Uiso 1 1 calc R . . C9 C -0.0043(5) 1.3148(4) 0.0495(4) 0.0498(12) Uani 1 1 d . . . C10 C -0.0338(5) 1.2660(4) -0.0037(4) 0.0550(13) Uani 1 1 d . . . C11 C 0.0603(5) 1.1756(4) -0.0475(4) 0.0525(13) Uani 1 1 d . . . C12 C 0.1807(5) 1.1322(4) -0.0350(4) 0.0542(13) Uani 1 1 d . . . C13 C 0.2092(5) 1.1785(4) 0.0207(4) 0.0513(13) Uani 1 1 d . . . C14 C 0.1158(5) 1.2706(4) 0.0630(4) 0.0494(12) Uani 1 1 d . . . C15 C -0.1701(6) 1.3076(6) -0.0069(5) 0.098(2) Uani 1 1 d . . . H15A H -0.2219 1.3701 0.0269 0.146 Uiso 1 1 calc R . . H15B H -0.2029 1.2438 0.0289 0.146 Uiso 1 1 calc R . . H15C H -0.1712 1.3349 -0.0785 0.146 Uiso 1 1 calc R . . C16 C 0.0290(6) 1.1227(5) -0.1070(5) 0.087(2) Uani 1 1 d . . . H16A H 0.1034 1.0618 -0.1325 0.131 Uiso 1 1 calc R . . H16B H 0.0017 1.1826 -0.1650 0.131 Uiso 1 1 calc R . . H16C H -0.0374 1.0909 -0.0605 0.131 Uiso 1 1 calc R . . C17 C 0.3392(5) 1.1281(5) 0.0360(5) 0.0839(19) Uani 1 1 d . . . H17A H 0.3916 1.0659 0.0019 0.126 Uiso 1 1 calc R . . H17B H 0.3315 1.0982 0.1096 0.126 Uiso 1 1 calc R . . H17C H 0.3771 1.1882 0.0062 0.126 Uiso 1 1 calc R . . C18 C 0.1426(5) 1.3190(5) 0.1278(4) 0.0754(17) Uani 1 1 d . . . H18A H 0.0685 1.3816 0.1509 0.113 Uiso 1 1 calc R . . H18B H 0.2123 1.3480 0.0857 0.113 Uiso 1 1 calc R . . H18C H 0.1640 1.2580 0.1877 0.113 Uiso 1 1 calc R . . C19 C 0.2809(5) 1.0240(4) -0.0706(4) 0.0665(16) Uani 1 1 d . . . H19A H 0.2622 1.0116 -0.1233 0.080 Uiso 1 1 calc R . . H19B H 0.3645 1.0315 -0.0995 0.080 Uiso 1 1 calc R . . C20 C 0.3626(4) 0.8218(4) 0.0184(4) 0.0454(12) Uani 1 1 d . . . C21 C 0.4409(5) 0.7879(5) -0.0735(4) 0.0581(14) Uani 1 1 d . . . H21 H 0.4377 0.8414 -0.1382 0.070 Uiso 1 1 calc R . . C22 C 0.5225(5) 0.6758(5) -0.0686(5) 0.0663(16) Uani 1 1 d . . . H22 H 0.5738 0.6528 -0.1302 0.080 Uiso 1 1 calc R . . C23 C 0.5296(5) 0.5974(5) 0.0256(5) 0.0640(16) Uani 1 1 d . . . H23 H 0.5867 0.5216 0.0279 0.077 Uiso 1 1 calc R . . C24 C 0.4521(5) 0.6297(4) 0.1184(4) 0.0580(14) Uani 1 1 d . . . H24 H 0.4564 0.5754 0.1826 0.070 Uiso 1 1 calc R . . C25 C 0.3685(4) 0.7429(4) 0.1151(4) 0.0426(11) Uani 1 1 d . . . C26 C 0.2879(5) 0.7797(4) 0.2159(4) 0.0521(13) Uani 1 1 d . . . C27 C 0.3205(5) 1.0501(4) 0.3879(3) 0.0413(11) Uani 1 1 d . . . C28 C 0.4266(4) 1.0851(4) 0.3777(3) 0.0426(11) Uani 1 1 d . . . C29 C 0.5500(5) 1.0093(4) 0.3530(4) 0.0517(13) Uani 1 1 d . . . H29 H 0.5634 0.9392 0.3423 0.062 Uiso 1 1 calc R . . C30 C 0.6537(5) 1.0318(5) 0.3432(4) 0.0659(16) Uani 1 1 d . . . H30 H 0.7348 0.9774 0.3284 0.079 Uiso 1 1 calc R . . C31 C 0.6341(6) 1.1371(6) 0.3560(4) 0.0753(17) Uani 1 1 d . . . H31 H 0.7035 1.1551 0.3473 0.090 Uiso 1 1 calc R . . C32 C 0.5144(5) 1.2159(5) 0.3813(5) 0.0737(17) Uani 1 1 d . . . H32 H 0.5031 1.2866 0.3895 0.088 Uiso 1 1 calc R . . C33 C 0.4087(5) 1.1897(4) 0.3949(4) 0.0551(13) Uani 1 1 d . . . C34 C 0.2698(5) 1.3725(5) 0.4400(5) 0.0803(19) Uani 1 1 d . . . H34A H 0.3120 1.4193 0.3762 0.096 Uiso 1 1 calc R . . H34B H 0.3048 1.3566 0.4951 0.096 Uiso 1 1 calc R . . C35 C 0.1285(5) 1.4364(5) 0.4709(5) 0.0617(15) Uani 1 1 d . . . C36 C 0.0658(6) 1.5030(5) 0.3940(5) 0.0653(16) Uani 1 1 d . . . C37 C 0.0625(6) 1.4313(5) 0.5777(5) 0.0643(15) Uani 1 1 d . . . C38 C 0.1389(6) 1.5010(6) 0.2814(5) 0.099(2) Uani 1 1 d . . . H38A H 0.0804 1.5294 0.2417 0.148 Uiso 1 1 calc R . . H38B H 0.1924 1.4223 0.2780 0.148 Uiso 1 1 calc R . . H38C H 0.1902 1.5501 0.2526 0.148 Uiso 1 1 calc R . . C39 C 0.1267(7) 1.3516(6) 0.6622(5) 0.099(2) Uani 1 1 d . . . H39A H 0.1957 1.2870 0.6374 0.148 Uiso 1 1 calc R . . H39B H 0.0665 1.3226 0.7236 0.148 Uiso 1 1 calc R . . H39C H 0.1587 1.3944 0.6791 0.148 Uiso 1 1 calc R . . H11A H 0.046(5) 1.255(4) 0.555(4) 0.11(2) Uiso 1 1 d D . . H11B H -0.063(4) 1.224(6) 0.613(5) 0.15(4) Uiso 1 1 d D . . H7 H 0.047(4) 1.013(4) 0.348(2) 0.059(17) Uiso 1 1 d D . . H12B H -0.037(5) 1.134(3) 0.234(5) 0.088 Uiso 1 1 d D . . H12A H 0.054(3) 1.034(5) 0.204(5) 0.088 Uiso 1 1 d 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 Zn1 0.0403(3) 0.0393(3) 0.0391(3) -0.0128(2) -0.0086(3) -0.0139(3) Zn2 0.0335(3) 0.0368(3) 0.0482(3) -0.0110(2) -0.0105(3) -0.0111(2) O1 0.044(2) 0.050(2) 0.044(2) -0.0046(16) -0.0089(17) 0.0004(17) O2 0.047(2) 0.055(2) 0.047(2) 0.0014(17) -0.0077(18) -0.0132(18) O3 0.059(2) 0.0400(19) 0.0403(19) -0.0048(15) -0.0119(17) -0.0063(17) O4 0.067(2) 0.050(2) 0.043(2) -0.0152(17) -0.0060(18) -0.0096(19) O5 0.068(2) 0.064(2) 0.051(2) -0.0272(18) -0.0091(19) -0.027(2) O6 0.122(4) 0.191(5) 0.111(4) -0.102(4) 0.042(3) -0.111(4) O7 0.044(2) 0.0359(17) 0.0382(18) -0.0069(14) -0.0160(16) -0.0127(15) O8 0.046(2) 0.062(2) 0.099(3) -0.047(2) -0.014(2) -0.0162(18) O9 0.037(2) 0.064(2) 0.124(3) -0.055(2) -0.006(2) -0.0176(19) O10 0.051(2) 0.064(2) 0.124(3) -0.057(2) -0.010(2) -0.019(2) O11 0.085(3) 0.092(3) 0.092(3) -0.050(3) 0.009(3) -0.059(3) O12 0.129(4) 0.172(6) 0.084(4) 0.024(4) -0.058(4) -0.093(5) C1 0.047(3) 0.043(3) 0.045(3) -0.016(2) -0.010(3) -0.012(3) C2 0.035(3) 0.036(3) 0.047(3) -0.007(2) -0.011(2) -0.009(2) C3 0.041(3) 0.046(3) 0.051(3) -0.010(2) -0.008(2) -0.013(2) C4 0.044(3) 0.042(3) 0.074(4) -0.018(3) -0.014(3) -0.001(3) C5 0.057(4) 0.041(3) 0.072(4) -0.004(3) -0.027(3) -0.007(3) C6 0.057(3) 0.047(3) 0.057(3) -0.008(3) -0.022(3) -0.006(3) C7 0.037(3) 0.042(3) 0.051(3) -0.009(2) -0.015(2) -0.004(2) C8 0.060(4) 0.053(3) 0.038(3) -0.003(2) -0.008(3) -0.012(3) C9 0.048(3) 0.043(3) 0.047(3) -0.006(2) -0.009(3) -0.015(3) C10 0.056(4) 0.054(3) 0.048(3) -0.004(3) -0.016(3) -0.019(3) C11 0.063(4) 0.053(3) 0.040(3) -0.008(2) -0.008(3) -0.028(3) C12 0.053(3) 0.057(3) 0.042(3) -0.013(2) -0.001(3) -0.021(3) C13 0.042(3) 0.048(3) 0.056(3) -0.005(2) -0.015(3) -0.015(3) C14 0.054(3) 0.049(3) 0.044(3) -0.005(2) -0.012(3) -0.025(3) C15 0.063(4) 0.106(5) 0.127(6) -0.031(5) -0.045(4) -0.014(4) C16 0.117(6) 0.086(4) 0.080(4) -0.004(4) -0.051(4) -0.046(4) C17 0.057(4) 0.080(4) 0.115(5) -0.026(4) -0.034(4) -0.013(3) C18 0.076(4) 0.078(4) 0.088(4) -0.023(3) -0.032(4) -0.030(4) C19 0.068(4) 0.054(3) 0.054(3) -0.015(3) -0.004(3) -0.013(3) C20 0.039(3) 0.044(3) 0.056(3) -0.024(3) -0.010(3) -0.010(2) C21 0.058(3) 0.061(4) 0.058(3) -0.029(3) -0.007(3) -0.020(3) C22 0.055(4) 0.081(4) 0.076(4) -0.053(4) -0.003(3) -0.020(3) C23 0.053(4) 0.060(4) 0.091(5) -0.045(4) -0.019(3) -0.007(3) C24 0.055(3) 0.059(3) 0.067(4) -0.023(3) -0.024(3) -0.014(3) C25 0.038(3) 0.048(3) 0.051(3) -0.023(2) -0.014(2) -0.012(2) C26 0.049(3) 0.054(3) 0.053(3) -0.017(3) -0.012(3) -0.017(3) C27 0.046(3) 0.038(3) 0.037(3) -0.010(2) -0.007(2) -0.016(2) C28 0.038(3) 0.052(3) 0.043(3) -0.016(2) -0.006(2) -0.021(2) C29 0.042(3) 0.068(3) 0.048(3) -0.023(3) -0.011(3) -0.016(3) C30 0.039(3) 0.096(5) 0.064(4) -0.032(3) -0.010(3) -0.019(3) C31 0.057(4) 0.106(5) 0.084(4) -0.039(4) -0.008(3) -0.044(4) C32 0.055(4) 0.081(4) 0.104(5) -0.049(4) -0.010(4) -0.028(3) C33 0.042(3) 0.060(3) 0.073(4) -0.032(3) -0.009(3) -0.020(3) C34 0.068(4) 0.074(4) 0.112(5) -0.049(4) -0.002(4) -0.035(4) C35 0.055(4) 0.058(4) 0.084(4) -0.038(3) -0.004(3) -0.026(3) C36 0.075(4) 0.062(4) 0.066(4) -0.032(3) 0.005(4) -0.039(3) C37 0.072(4) 0.051(3) 0.082(4) -0.028(3) -0.016(4) -0.028(3) C38 0.107(6) 0.116(6) 0.084(5) -0.042(4) -0.004(4) -0.055(5) C39 0.110(6) 0.103(5) 0.101(5) -0.001(4) -0.038(5) -0.066(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.913(3) . ? Zn1 O2 1.947(3) 2_576 ? Zn1 O8 1.946(3) . ? Zn1 O7 1.956(3) . ? Zn2 O9 1.967(3) . ? Zn2 O1 1.982(3) . ? Zn2 O7 2.033(3) 2_576 ? Zn2 O7 2.098(3) . ? Zn2 O11 2.106(4) . ? Zn2 Zn2 3.1423(11) 2_576 ? O1 C1 1.259(5) . ? O2 C1 1.256(5) . ? O2 Zn1 1.947(3) 2_576 ? O3 C7 1.376(5) . ? O3 C8 1.435(5) . ? O4 C20 1.367(5) . ? O4 C19 1.428(6) . ? O5 C26 1.260(6) . ? O6 C26 1.205(6) . ? O7 Zn2 2.033(3) 2_576 ? O7 H7 0.825(19) . ? O8 C27 1.247(5) . ? O9 C27 1.237(5) . ? O10 C33 1.358(5) . ? O10 C34 1.463(6) . ? O11 H11A 0.835(19) . ? O11 H11B 0.849(19) . ? O12 H12B 0.837(19) . ? O12 H12A 0.845(19) . ? C1 C2 1.495(6) . ? C2 C3 1.387(6) . ? C2 C7 1.411(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9300 . ? C4 C5 1.369(7) . ? C4 H4 0.9300 . ? C5 C6 1.385(6) . ? C5 H5 0.9300 . ? C6 C7 1.375(6) . ? C6 H6 0.9300 . ? C8 C9 1.512(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.394(6) . ? C9 C10 1.405(6) . ? C10 C11 1.389(7) . ? C10 C15 1.529(7) . ? C11 C12 1.392(7) . ? C11 C16 1.539(7) . ? C12 C13 1.403(6) . ? C12 C19 1.522(7) . ? C13 C14 1.392(6) . ? C13 C17 1.509(7) . ? C14 C18 1.524(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.389(6) . ? C20 C25 1.387(6) . ? C21 C22 1.363(7) . ? C21 H21 0.9300 . ? C22 C23 1.359(7) . ? C22 H22 0.9300 . ? C23 C24 1.389(7) . ? C23 H23 0.9300 . ? C24 C25 1.383(6) . ? C24 H24 0.9300 . ? C25 C26 1.511(6) . ? C27 C28 1.502(6) . ? C28 C29 1.383(6) . ? C28 C33 1.405(6) . ? C29 C30 1.372(7) . ? C29 H29 0.9300 . ? C30 C31 1.377(7) . ? C30 H30 0.9300 . ? C31 C32 1.370(7) . ? C31 H31 0.9300 . ? C32 C33 1.406(7) . ? C32 H32 0.9300 . ? C34 C35 1.510(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.396(8) . ? C35 C37 1.409(7) . ? C36 C37 1.392(7) 2_586 ? C36 C38 1.508(7) . ? C37 C36 1.392(7) 2_586 ? C37 C39 1.511(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O2 111.45(14) . 2_576 ? O5 Zn1 O8 102.98(15) . . ? O2 Zn1 O8 103.43(15) 2_576 . ? O5 Zn1 O7 119.52(14) . . ? O2 Zn1 O7 107.15(13) 2_576 . ? O8 Zn1 O7 111.16(13) . . ? O9 Zn2 O1 115.16(15) . . ? O9 Zn2 O7 133.80(15) . 2_576 ? O1 Zn2 O7 110.78(13) . 2_576 ? O9 Zn2 O7 97.45(13) . . ? O1 Zn2 O7 97.43(13) . . ? O7 Zn2 O7 80.97(13) 2_576 . ? O9 Zn2 O11 83.32(17) . . ? O1 Zn2 O11 94.47(17) . . ? O7 Zn2 O11 88.70(16) 2_576 . ? O7 Zn2 O11 166.41(16) . . ? O9 Zn2 Zn2 122.30(10) . 2_576 ? O1 Zn2 Zn2 108.41(11) . 2_576 ? O7 Zn2 Zn2 41.26(8) 2_576 2_576 ? O7 Zn2 Zn2 39.72(9) . 2_576 ? O11 Zn2 Zn2 129.37(14) . 2_576 ? C1 O1 Zn2 124.6(3) . . ? C1 O2 Zn1 137.7(3) . 2_576 ? C7 O3 C8 115.7(3) . . ? C20 O4 C19 118.6(4) . . ? C26 O5 Zn1 122.1(3) . . ? Zn1 O7 Zn2 108.29(14) . 2_576 ? Zn1 O7 Zn2 112.83(14) . . ? Zn2 O7 Zn2 99.03(13) 2_576 . ? Zn1 O7 H7 105(3) . . ? Zn2 O7 H7 122(3) 2_576 . ? Zn2 O7 H7 110(3) . . ? C27 O8 Zn1 127.6(3) . . ? C27 O9 Zn2 142.5(3) . . ? C33 O10 C34 117.7(4) . . ? Zn2 O11 H11A 129(4) . . ? Zn2 O11 H11B 115(5) . . ? H11A O11 H11B 113(4) . . ? H12B O12 H12A 111(5) . . ? O2 C1 O1 125.1(4) . . ? O2 C1 C2 116.1(4) . . ? O1 C1 C2 118.7(4) . . ? C3 C2 C7 116.8(4) . . ? C3 C2 C1 118.8(4) . . ? C7 C2 C1 124.5(4) . . ? C2 C3 C4 123.1(5) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 121.2(5) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 O3 123.7(4) . . ? C6 C7 C2 120.2(4) . . ? O3 C7 C2 116.1(4) . . ? O3 C8 C9 108.1(4) . . ? O3 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? O3 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C14 C9 C10 121.1(5) . . ? C14 C9 C8 119.6(5) . . ? C10 C9 C8 119.3(5) . . ? C9 C10 C11 119.2(5) . . ? C9 C10 C15 119.9(5) . . ? C11 C10 C15 120.8(5) . . ? C12 C11 C10 119.7(5) . . ? C12 C11 C16 120.8(5) . . ? C10 C11 C16 119.5(5) . . ? C11 C12 C13 121.2(5) . . ? C11 C12 C19 120.8(5) . . ? C13 C12 C19 117.6(5) . . ? C12 C13 C14 119.3(5) . . ? C12 C13 C17 120.4(5) . . ? C14 C13 C17 120.3(5) . . ? C9 C14 C13 119.5(4) . . ? C9 C14 C18 120.1(5) . . ? C13 C14 C18 120.3(5) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C12 104.5(4) . . ? O4 C19 H19A 110.9 . . ? C12 C19 H19A 110.9 . . ? O4 C19 H19B 110.9 . . ? C12 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? O4 C20 C21 124.5(5) . . ? O4 C20 C25 115.1(4) . . ? C21 C20 C25 120.4(4) . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.6(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 119.9(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C20 118.9(4) . . ? C24 C25 C26 120.0(4) . . ? C20 C25 C26 121.1(4) . . ? O6 C26 O5 124.7(5) . . ? O6 C26 C25 119.4(5) . . ? O5 C26 C25 115.9(5) . . ? O9 C27 O8 124.4(5) . . ? O9 C27 C28 119.7(4) . . ? O8 C27 C28 115.9(4) . . ? C29 C28 C33 117.0(4) . . ? C29 C28 C27 118.9(4) . . ? C33 C28 C27 124.0(4) . . ? C30 C29 C28 123.7(5) . . ? C30 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? C29 C30 C31 118.1(5) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C32 C31 C30 121.2(5) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 120.0(5) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? O10 C33 C28 117.9(4) . . ? O10 C33 C32 122.2(4) . . ? C28 C33 C32 119.8(5) . . ? O10 C34 C35 106.8(4) . . ? O10 C34 H34A 110.4 . . ? C35 C34 H34A 110.4 . . ? O10 C34 H34B 110.4 . . ? C35 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? C36 C35 C37 120.9(5) . . ? C36 C35 C34 120.2(6) . . ? C37 C35 C34 118.9(6) . . ? C35 C36 C37 119.9(5) . 2_586 ? C35 C36 C38 119.0(6) . . ? C37 C36 C38 121.1(6) 2_586 . ? C36 C37 C35 119.2(5) 2_586 . ? C36 C37 C39 119.5(6) 2_586 . ? C35 C37 C39 121.3(6) . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Zn2 O1 C1 -144.9(4) . . . . ? O7 Zn2 O1 C1 30.2(4) 2_576 . . . ? O7 Zn2 O1 C1 113.3(4) . . . . ? O11 Zn2 O1 C1 -60.1(4) . . . . ? Zn2 Zn2 O1 C1 74.0(4) 2_576 . . . ? O2 Zn1 O5 C26 58.8(4) 2_576 . . . ? O8 Zn1 O5 C26 169.1(4) . . . . ? O7 Zn1 O5 C26 -67.2(4) . . . . ? O5 Zn1 O7 Zn2 115.25(16) . . . 2_576 ? O2 Zn1 O7 Zn2 -12.67(18) 2_576 . . 2_576 ? O8 Zn1 O7 Zn2 -125.02(16) . . . 2_576 ? O5 Zn1 O7 Zn2 -136.18(16) . . . . ? O2 Zn1 O7 Zn2 95.90(17) 2_576 . . . ? O8 Zn1 O7 Zn2 -16.4(2) . . . . ? O9 Zn2 O7 Zn1 19.01(19) . . . . ? O1 Zn2 O7 Zn1 135.72(16) . . . . ? O7 Zn2 O7 Zn1 -114.31(19) 2_576 . . . ? O11 Zn2 O7 Zn1 -73.4(7) . . . . ? Zn2 Zn2 O7 Zn1 -114.31(19) 2_576 . . . ? O9 Zn2 O7 Zn2 133.31(15) . . . 2_576 ? O1 Zn2 O7 Zn2 -109.97(14) . . . 2_576 ? O7 Zn2 O7 Zn2 0.0 2_576 . . 2_576 ? O11 Zn2 O7 Zn2 40.9(7) . . . 2_576 ? O5 Zn1 O8 C27 135.4(4) . . . . ? O2 Zn1 O8 C27 -108.5(4) 2_576 . . . ? O7 Zn1 O8 C27 6.2(4) . . . . ? O1 Zn2 O9 C27 -124.1(6) . . . . ? O7 Zn2 O9 C27 62.4(6) 2_576 . . . ? O7 Zn2 O9 C27 -22.2(6) . . . . ? O11 Zn2 O9 C27 144.1(6) . . . . ? Zn2 Zn2 O9 C27 11.1(7) 2_576 . . . ? Zn1 O2 C1 O1 3.6(8) 2_576 . . . ? Zn1 O2 C1 C2 -174.3(3) 2_576 . . . ? Zn2 O1 C1 O2 -19.6(7) . . . . ? Zn2 O1 C1 C2 158.3(3) . . . . ? O2 C1 C2 C3 34.6(6) . . . . ? O1 C1 C2 C3 -143.5(4) . . . . ? O2 C1 C2 C7 -145.0(5) . . . . ? O1 C1 C2 C7 36.9(7) . . . . ? C7 C2 C3 C4 -2.4(7) . . . . ? C1 C2 C3 C4 178.0(5) . . . . ? C2 C3 C4 C5 1.4(8) . . . . ? C3 C4 C5 C6 -0.8(8) . . . . ? C4 C5 C6 C7 1.4(8) . . . . ? C5 C6 C7 O3 175.3(5) . . . . ? C5 C6 C7 C2 -2.4(8) . . . . ? C8 O3 C7 C6 13.9(7) . . . . ? C8 O3 C7 C2 -168.3(4) . . . . ? C3 C2 C7 C6 2.8(7) . . . . ? C1 C2 C7 C6 -177.6(5) . . . . ? C3 C2 C7 O3 -175.0(4) . . . . ? C1 C2 C7 O3 4.6(7) . . . . ? C7 O3 C8 C9 173.4(4) . . . . ? O3 C8 C9 C14 -74.8(6) . . . . ? O3 C8 C9 C10 104.4(5) . . . . ? C14 C9 C10 C11 -2.8(7) . . . . ? C8 C9 C10 C11 178.1(4) . . . . ? C14 C9 C10 C15 173.4(5) . . . . ? C8 C9 C10 C15 -5.7(7) . . . . ? C9 C10 C11 C12 2.1(7) . . . . ? C15 C10 C11 C12 -174.1(5) . . . . ? C9 C10 C11 C16 -179.3(5) . . . . ? C15 C10 C11 C16 4.5(7) . . . . ? C10 C11 C12 C13 -0.3(7) . . . . ? C16 C11 C12 C13 -178.9(5) . . . . ? C10 C11 C12 C19 172.6(4) . . . . ? C16 C11 C12 C19 -5.9(7) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C19 C12 C13 C14 -174.0(4) . . . . ? C11 C12 C13 C17 178.3(5) . . . . ? C19 C12 C13 C17 5.1(7) . . . . ? C10 C9 C14 C13 1.7(7) . . . . ? C8 C9 C14 C13 -179.2(4) . . . . ? C10 C9 C14 C18 -175.5(5) . . . . ? C8 C9 C14 C18 3.6(7) . . . . ? C12 C13 C14 C9 0.2(7) . . . . ? C17 C13 C14 C9 -178.9(5) . . . . ? C12 C13 C14 C18 177.4(5) . . . . ? C17 C13 C14 C18 -1.7(7) . . . . ? C20 O4 C19 C12 -173.1(4) . . . . ? C11 C12 C19 O4 -97.4(5) . . . . ? C13 C12 C19 O4 75.8(6) . . . . ? C19 O4 C20 C21 -16.0(7) . . . . ? C19 O4 C20 C25 165.6(4) . . . . ? O4 C20 C21 C22 -177.2(5) . . . . ? C25 C20 C21 C22 1.1(7) . . . . ? C20 C21 C22 C23 -1.2(8) . . . . ? C21 C22 C23 C24 1.1(8) . . . . ? C22 C23 C24 C25 -1.0(8) . . . . ? C23 C24 C25 C20 0.9(7) . . . . ? C23 C24 C25 C26 -177.5(5) . . . . ? O4 C20 C25 C24 177.5(4) . . . . ? C21 C20 C25 C24 -0.9(7) . . . . ? O4 C20 C25 C26 -4.1(6) . . . . ? C21 C20 C25 C26 177.5(4) . . . . ? Zn1 O5 C26 O6 5.8(8) . . . . ? Zn1 O5 C26 C25 -172.1(3) . . . . ? C24 C25 C26 O6 -71.9(7) . . . . ? C20 C25 C26 O6 109.7(6) . . . . ? C24 C25 C26 O5 106.2(5) . . . . ? C20 C25 C26 O5 -72.2(6) . . . . ? Zn2 O9 C27 O8 13.1(9) . . . . ? Zn2 O9 C27 C28 -167.5(4) . . . . ? Zn1 O8 C27 O9 -1.5(7) . . . . ? Zn1 O8 C27 C28 179.1(3) . . . . ? O9 C27 C28 C29 173.8(4) . . . . ? O8 C27 C28 C29 -6.8(6) . . . . ? O9 C27 C28 C33 -4.3(7) . . . . ? O8 C27 C28 C33 175.1(5) . . . . ? C33 C28 C29 C30 -0.9(7) . . . . ? C27 C28 C29 C30 -179.1(5) . . . . ? C28 C29 C30 C31 -1.8(8) . . . . ? C29 C30 C31 C32 2.2(9) . . . . ? C30 C31 C32 C33 0.1(10) . . . . ? C34 O10 C33 C28 -179.3(5) . . . . ? C34 O10 C33 C32 0.2(8) . . . . ? C29 C28 C33 O10 -177.3(4) . . . . ? C27 C28 C33 O10 0.8(7) . . . . ? C29 C28 C33 C32 3.2(7) . . . . ? C27 C28 C33 C32 -178.7(5) . . . . ? C31 C32 C33 O10 177.6(5) . . . . ? C31 C32 C33 C28 -2.9(9) . . . . ? C33 O10 C34 C35 180.0(5) . . . . ? O10 C34 C35 C36 -82.2(6) . . . . ? O10 C34 C35 C37 100.2(6) . . . . ? C37 C35 C36 C37 2.3(8) . . . 2_586 ? C34 C35 C36 C37 -175.2(5) . . . 2_586 ? C37 C35 C36 C38 -176.9(5) . . . . ? C34 C35 C36 C38 5.6(7) . . . . ? C36 C35 C37 C36 -2.3(8) . . . 2_586 ? C34 C35 C37 C36 175.2(5) . . . 2_586 ? C36 C35 C37 C39 174.7(5) . . . . ? C34 C35 C37 C39 -7.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.432 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.080