# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 1145/164 data_ttpc _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42 O20 S12' _chemical_formula_weight 1323.54 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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.017(10) _cell_length_b 14.307(12) _cell_length_c 25.091(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.11(3) _cell_angle_gamma 90.00 _cell_volume 5746(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Black _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.559 _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method Floatation _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 0.530 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5029 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5029 _reflns_number_gt 2562 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+62.8727P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(18) _refine_ls_number_reflns 5029 _refine_ls_number_parameters 490 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 0.768 _refine_ls_restrained_S_all 0.768 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.3792 0.6210(2) 0.16007(14) 0.0440(8) Uani 1 d . . . S2 S 0.4831(3) 0.7516(3) 0.22112(15) 0.0482(9) Uani 1 d . . . S3 S 0.3594(3) 0.4960(2) 0.26774(14) 0.0445(8) Uani 1 d . . . S4 S 0.4700(3) 0.6250(3) 0.32523(13) 0.0474(9) Uani 1 d . . . S5 S 0.5357(3) 0.4347(3) 0.17238(14) 0.0498(9) Uani 1 d . . . S6 S 0.6436(3) 0.5664(3) 0.23360(17) 0.0534(10) Uani 1 d . . . S7 S 0.5234(3) 0.3033(3) 0.27559(14) 0.0465(8) Uani 1 d . . . S8 S 0.6315(3) 0.4326(3) 0.33811(15) 0.0518(9) Uani 1 d . . . S9 S 0.2011(3) 0.7400(3) 0.18939(16) 0.0540(10) Uani 1 d . . . S10 S 0.3083(3) 0.8762(3) 0.24349(14) 0.0475(9) Uani 1 d . . . S11 S 0.1913(3) 0.6208(3) 0.29672(16) 0.0509(9) Uani 1 d . . . S12 S 0.2973(3) 0.7561(3) 0.35266(14) 0.0465(9) Uani 1 d . . . C13 C 0.4254(8) 0.6502(8) 0.2211(5) 0.038(3) Uiso 1 d . . . C14 C 0.4197(8) 0.5940(9) 0.2660(5) 0.039(3) Uiso 1 d . . . C15 C 0.5880(9) 0.4604(10) 0.2333(5) 0.042(3) Uiso 1 d . . . C16 C 0.5823(8) 0.4075(9) 0.2773(5) 0.040(3) Uiso 1 d . . . C17 C 0.2544(9) 0.7734(10) 0.2475(6) 0.041(3) Uiso 1 d . . . C18 C 0.2490(9) 0.7224(10) 0.2942(5) 0.044(3) Uiso 1 d . . . C19 C 0.4210(9) 0.7145(10) 0.1261(6) 0.053(4) Uiso 1 d . . . H19 H 0.4101 0.7233 0.0898 0.064 Uiso 1 calc R . . C20 C 0.4695(9) 0.7734(11) 0.1546(6) 0.052(4) Uiso 1 d . . . H20 H 0.4949 0.8242 0.1387 0.062 Uiso 1 calc R . . C21 C 0.3849(8) 0.4701(10) 0.3333(5) 0.047(3) Uiso 1 d . . . H21 H 0.3631 0.4176 0.3497 0.056 Uiso 1 calc R . . C22 C 0.4367(9) 0.5277(10) 0.3597(6) 0.049(3) Uiso 1 d . . . H22 H 0.4542 0.5164 0.3949 0.059 Uiso 1 calc R . . C23 C 0.5792(10) 0.5267(11) 0.1393(6) 0.057(4) Uiso 1 d . . . H23 H 0.5695 0.5346 0.1028 0.068 Uiso 1 calc R . . C24 C 0.6258(11) 0.5849(12) 0.1666(7) 0.063(4) Uiso 1 d . . . H24 H 0.6493 0.6362 0.1500 0.075 Uiso 1 calc R . . C25 C 0.5441(9) 0.2764(11) 0.3416(6) 0.053(4) Uiso 1 d . . . H25 H 0.5223 0.2231 0.3571 0.064 Uiso 1 calc R . . C26 C 0.5926(10) 0.3351(12) 0.3691(7) 0.060(4) Uiso 1 d . . . H26 H 0.6056 0.3240 0.4050 0.072 Uiso 1 calc R . . C27 C 0.2314(10) 0.8334(12) 0.1528(7) 0.059(4) Uiso 1 d . . . H27 H 0.2142 0.8405 0.1172 0.071 Uiso 1 calc R . . C28 C 0.2807(10) 0.8959(12) 0.1776(7) 0.064(4) Uiso 1 d . . . H28 H 0.2996 0.9484 0.1598 0.077 Uiso 1 calc R . . C29 C 0.2125(10) 0.6018(12) 0.3642(6) 0.057(4) Uiso 1 d . . . H29 H 0.1915 0.5501 0.3818 0.068 Uiso 1 calc R . . C30 C 0.2607(9) 0.6657(11) 0.3896(6) 0.053(4) Uiso 1 d . . . H30 H 0.2737 0.6609 0.4259 0.063 Uiso 1 calc R . . C31 C 0.5359(8) 0.0340(8) -0.2062(5) 0.036(3) Uiso 1 d . . . C32 C 0.6051(8) 0.0869(8) -0.2201(5) 0.037(3) Uiso 1 d . . . C33 C 0.6188(8) 0.0724(9) -0.2746(5) 0.037(3) Uiso 1 d . . . C34 C 0.5568(8) 0.0100(9) -0.2948(5) 0.041(3) Uiso 1 d . . . C35 C 0.5059(8) -0.0129(9) -0.2528(5) 0.043(3) Uiso 1 d . . . C36 C 0.5891(7) 0.4684(8) 0.0009(4) 0.033(2) Uiso 1 d . . . C37 C 0.5031(8) 0.4542(9) 0.0006(5) 0.042(3) Uiso 1 d . . . C38 C 0.4645(8) 0.5416(9) 0.0015(5) 0.040(3) Uiso 1 d . . . C39 C 0.5287(8) 0.6111(8) 0.0019(5) 0.035(3) Uiso 1 d . . . C40 C 0.6059(7) 0.5637(8) 0.0018(4) 0.031(2) Uiso 1 d . . . C41 C 0.5017(9) 0.0245(10) -0.1533(5) 0.047(3) Uiso 1 d . . . C42 C 0.6582(9) 0.1437(9) -0.1850(5) 0.045(3) Uiso 1 d . . . C43 C 0.6816(8) 0.1226(9) -0.3060(5) 0.044(3) Uiso 1 d . . . C44 C 0.5482(9) -0.0239(11) -0.3504(6) 0.053(4) Uiso 1 d . . . C45 C 0.4305(9) -0.0752(10) -0.2603(6) 0.049(3) Uiso 1 d . . . C46 C 0.6546(8) 0.3945(9) 0.0088(5) 0.040(3) Uiso 1 d . . . C47 C 0.4600(9) 0.3666(10) -0.0035(6) 0.047(3) Uiso 1 d . . . C48 C 0.3719(9) 0.5553(10) -0..0028(6) 0.053(3) Uiso 1 d . . . C49 C 0.5142(8) 0.7103(9) -0.0003(5) 0.044(3) Uiso 1 d . . . C50 C 0.6919(8) 0.6073(9) 0.0055(5) 0.041(3) Uiso 1 d . . . O51 O 0.5429(7) 0.0095(9) -0.1134(4) 0.073(3) Uani 1 d . . . O52 O 0.7321(7) 0.1485(8) -0.1850(5) 0.065(3) Uani 1 d . . . O53 O 0.6973(8) 0.2043(7) -0.3020(5) 0.075(4) Uani 1 d . . . O54 O 0.5413(12) 0.0246(9) -0.3889(4) 0.110(6) Uani 1 d . . . O55 O 0.3865(7) -0.0775(9) -0.2987(4) 0.072(3) Uani 1 d . . . O56 O 0.6457(7) 0.3202(6) 0.0286(4) 0.059(3) Uani 1 d . . . O57 O 0.3976(11) 0.3453(11) 0.0175(8) 0.156(9) Uani 1 d . . . O58 O 0.3321(9) 0.544(2) -0.0421(7) 0.211(14) Uani 1 d . . . O59 O 0.4455(8) 0.7473(9) -0.0044(6) 0.089(4) Uani 1 d . . . O60 O 0.7277(7) 0.6409(8) -0.0312(4) 0.062(3) Uani 1 d . . . O61 O 0.4197(6) 0.0355(7) -0.1528(4) 0.050(2) Uani 1 d . . . O62 O 0.6146(7) 0.1949(8) -0.1515(4) 0.072(3) Uani 1 d . . . O63 O 0.7203(8) 0.0681(7) -0.3397(5) 0.071(3) Uani 1 d . . . O64 O 0.5476(7) -0.1166(8) -0.3522(4) 0.063(3) Uani 1 d . . . O65 O 0.4199(6) -0.1259(7) -0.2166(4) 0.058(3) Uani 1 d . . . O66 O 0.7277(6) 0.4237(7) -0.0097(5) 0.066(3) Uani 1 d . . . O67 O 0.4924(6) 0.3089(7) -0.0396(4) 0.058(3) Uani 1 d . . . O68 O 0.3377(6) 0.5844(9) 0.0395(4) 0.067(3) Uani 1 d . . . O69 O 0.5835(7) 0.7586(7) 0.0027(5) 0.069(3) Uani 1 d . . . O70 O 0.7214(6) 0.6035(9) 0.0543(4) 0.062(3) Uani 1 d . . . C71 C 0.3780(11) 0.0062(13) -0.1061(7) 0.067(5) Uiso 1 d . . . H71A H 0.3770 -0.0609 -0.1046 0.100 Uiso 1 calc R . . H71B H 0.3218 0.0297 -0.1074 0.100 Uiso 1 calc R . . H71C H 0.4073 0.0301 -0.0749 0.100 Uiso 1 calc R . . C72 C 0.6612(14) 0.2523(16) -0.1147(9) 0.098(7) Uiso 1 d . . . H72A H 0.7026 0.2150 -0.0959 0.147 Uiso 1 calc R . . H72B H 0.6242 0.2791 -0.0896 0.147 Uiso 1 calc R . . H72C H 0.6882 0.3013 -0.1336 0.147 Uiso 1 calc R . . C73 C 0.7775(13) 0.1160(15) -0.3739(9) 0.090(6) Uiso 1 d . . . H73A H 0.7477 0.1630 -0.3942 0.135 Uiso 1 calc R . . H73B H 0.8014 0.0718 -0.3978 0.135 Uiso 1 calc R . . H73C H 0.8211 0.1448 -0.3525 0.135 Uiso 1 calc R . . C74 C 0.5301(12) -0.1586(13) -0.4032(7) 0.077(5) Uiso 1 d . . . H74A H 0.5746 -0.1447 -0.4266 0.116 Uiso 1 calc R . . H74B H 0.4785 -0.1341 -0.4181 0.116 Uiso 1 calc R . . H74C H 0.5254 -0.2251 -0.3991 0.116 Uiso 1 calc R . . C75 C 0.3434(12) -0.1819(14) -0.2169(8) 0.081(5) Uiso 1 d . . . H75A H 0.2969 -0.1427 -0.2089 0.122 Uiso 1 calc R . . H75B H 0.3491 -0.2305 -0.1906 0.122 Uiso 1 calc R . . H75C H 0.3340 -0.2094 -0.2515 0.122 Uiso 1 calc R . . C76 C 0.7988(11) 0.3623(12) 0.0017(7) 0.072(5) Uiso 1 d . . . H76A H 0.8016 0.3473 0.0390 0.108 Uiso 1 calc R . . H76B H 0.8494 0.3933 -0.0077 0.108 Uiso 1 calc R . . H76C H 0.7924 0.3058 -0.0187 0.108 Uiso 1 calc R . . C77 C 0.4610(10) 0.2175(11) -0.0448(6) 0.058(4) Uiso 1 d . . . H77A H 0.4844 0.1792 -0.0167 0.087 Uiso 1 calc R . . H77B H 0.4758 0.1923 -0.0787 0.087 Uiso 1 calc R . . H77C H 0.4012 0.2187 -0.0428 0.087 Uiso 1 calc R . . C78 C 0.2470(13) 0.5956(15) 0.0345(9) 0.091(6) Uiso 1 d . . . H78A H 0.2336 0.6437 0.0089 0.136 Uiso 1 calc R . . H78B H 0.2258 0.6126 0.0684 0.136 Uiso 1 calc R . . H78C H 0.2221 0.5378 0.0227 0.136 Uiso 1 calc R . . C79 C 0.5770(13) 0.8589(14) -0.0031(8) 0.085(6) Uiso 1 d . . . H79A H 0.5524 0.8736 -0.0375 0.128 Uiso 1 calc R . . H79B H 0.6317 0.8862 0.0003 0.128 Uiso 1 calc R . . H79C H 0.5427 0.8836 0.0241 0.128 Uiso 1 calc R . . C80 C 0.8073(12) 0.6346(14) 0.0639(8) 0.079(5) Uiso 1 d . . . H80A H 0.8439 0.5979 0.0429 0.118 Uiso 1 calc R . . H80B H 0.8227 0.6271 0.1010 0.118 Uiso 1 calc R . . H80C H 0.8119 0.6993 0.0543 0.118 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0431(18) 0.0462(19) 0.0422(19) -0.0062(16) -0.0032(15) -0.0031(16) S2 0.0448(19) 0.046(2) 0.053(2) -0.0080(17) 0.0022(15) -0.0095(16) S3 0.0388(17) 0.0449(18) 0.050(2) -0.0021(15) 0.0006(14) -0.0045(14) S4 0.047(2) 0.056(2) 0.0390(19) -0.0060(16) -0.0011(15) -0.0086(17) S5 0.051(2) 0.055(2) 0.043(2) -0.0024(17) -0.0042(16) 0.0009(17) S6 0.044(2) 0.049(2) 0.068(3) -0.0020(18) 0.0079(18) -0.0095(17) S7 0.0421(18) 0.051(2) 0.0463(19) 0.0010(16) 0.0010(15) -0.0070(16) S8 0.043(2) 0.063(2) 0.048(2) -0.0128(19) -0.0038(16) 0.0009(18) S9 0.043(2) 0.068(3) 0.049(2) -0.015(2) -0.0080(17) -0.0048(19) S10 0.047(2) 0.043(2) 0.052(2) -0.0073(17) 0.0034(17) -0.0063(16) S11 0.0409(19) 0.044(2) 0.068(2) -0.0021(18) 0.0051(17) -0.0074(16) S12 0.047(2) 0.047(2) 0.045(2) -0.0057(16) -0.0056(15) -0.0038(16) O51 0.046(6) 0.123(10) 0.051(6) 0.018(7) 0.004(5) 0.014(7) O52 0.040(6) 0.062(7) 0.092(9) -0.022(6) 0.004(6) -0.006(5) O53 0.080(8) 0.042(6) 0.104(10) -0.004(6) 0.043(8) -0.008(6) O54 0.232(18) 0.057(8) 0.039(6) 0.001(6) -0.005(8) 0.006(10) O55 0.060(7) 0.091(8) 0.064(7) 0.002(6) -0.021(6) -0.014(6) O56 0.059(6) 0.042(5) 0.076(7) 0.019(5) 0.006(5) 0.005(5) O57 0.151(14) 0.110(11) 0.217(19) -0.093(12) 0.138(14) -0.084(11) O58 0.051(8) 0.47(4) 0.111(12) -0.183(19) -0.017(8) 0.053(14) O59 0.057(7) 0.072(8) 0.138(13) 0.021(8) 0.023(7) 0.021(6) O60 0.047(6) 0.084(7) 0.055(6) 0.023(5) 0.011(5) -0.013(5) O61 0.030(4) 0.064(6) 0.057(6) 0.010(5) 0.017(4) 0.009(4) O62 0.049(6) 0.096(8) 0.073(7) -0.044(6) 0.010(5) -0.001(6) O63 0.095(8) 0.053(6) 0.068(7) -0.001(5) 0.051(6) -0.009(6) O64 0.076(7) 0.061(7) 0.052(6) -0.018(5) -0.019(5) 0.017(6) O65 0.039(5) 0.050(6) 0.084(7) 0.010(5) 0.003(5) -0.012(4) O66 0.043(5) 0.057(6) 0.098(8) 0.027(6) 0.022(5) 0.025(5) O67 0.057(6) 0.044(6) 0.073(7) -0.016(5) 0.019(5) -0.015(5) O68 0.029(5) 0.107(9) 0.066(7) -0.030(7) 0.006(5) 0.000(6) O69 0.063(7) 0.037(5) 0.107(9) -0.001(6) -0.004(6) 0.004(5) O70 0.034(5) 0.101(9) 0.051(6) 0.009(6) -0.001(4) -0.018(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 S1 C13 1.728(12) . ? S1 C19 1.733(15) . ? S2 C20 1.704(15) . ? S2 C13 1.721(12) . ? S3 C14 1.704(14) . ? S3 C21 1.721(14) . ? S4 C14 1.723(13) . ? S4 C22 1.734(15) . ? S5 C23 1.717(16) . ? S5 C15 1.755(14) . ? S6 C24 1.716(17) . ? S6 C15 1.758(14) . ? S7 C25 1.721(15) . ? S7 C16 1.764(14) . ? S8 C16 1.728(14) . ? S8 C26 1.725(17) . ? S9 C27 1.702(17) . ? S9 C17 1.730(14) . ? S10 C17 1.709(15) . ? S10 C28 1.720(17) . ? S11 C18 1.725(14) . ? S11 C29 1.735(17) . ? S12 C30 1.707(15) . ? S12 C18 1.703(14) . ? C13 C14 1.389(17) . ? C15 C16 1.345(17) . ? C17 C18 1.385(18) . ? C19 C20 1.34(2) . ? C21 C22 1.329(19) . ? C23 C24 1.30(2) . ? C25 C26 1.32(2) . ? C27 C28 1.33(2) . ? C29 C30 1.34(2) . ? C31 C32 1.397(17) . ? C31 C35 1.417(17) . ? C31 C41 1.460(18) . ? C32 C33 1.406(17) . ? C32 C42 1.452(18) . ? C33 C34 1.416(17) . ? C33 C43 1.488(18) . ? C34 C35 1.396(18) . ? C34 C44 1.477(19) . ? C35 C45 1.508(19) . ? C36 C40 1.390(16) . ? C36 C37 1.391(16) . ? C36 C46 1.498(16) . ? C37 C38 1.395(18) . ? C37 C47 1.434(19) . ? C38 C39 1.431(17) . ? C38 C48 1.497(19) . ? C39 C40 1.411(16) . ? C39 C49 1.438(17) . ? C40 C50 1.512(16) . ? C41 O51 1.198(16) . ? C41 O61 1.324(16) . ? C42 O52 1.186(16) . ? C42 O62 1.332(16) . ? C43 O53 1.198(16) . ? C43 O63 1.321(16) . ? C44 O54 1.192(18) . ? C44 O64 1.328(18) . ? C45 O55 1.175(17) . ? C45 O65 1.331(17) . ? C46 O56 1.185(15) . ? C46 O66 1.342(15) . ? C47 O57 1.187(18) . ? C47 O67 1.343(16) . ? C48 O58 1.164(19) . ? C48 O68 1.283(17) . ? C49 O59 1.222(17) . ? C49 O69 1.306(16) . ? C50 O60 1.203(15) . ? C50 O70 1.298(15) . ? O61 C71 1.432(18) . ? O62 C72 1.43(2) . ? O63 C73 1.45(2) . ? O64 C74 1.432(19) . ? O65 C75 1.46(2) . ? O66 C76 1.459(19) . ? O67 C77 1.405(17) . ? O68 C78 1.46(2) . ? O69 C79 1.45(2) . ? O70 C80 1.46(2) . ? 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 C13 S1 C19 95.1(7) . . ? C20 S2 C13 96.0(7) . . ? C14 S3 C21 95.0(6) . . ? C14 S4 C22 94.7(7) . . ? C23 S5 C15 94.1(7) . . ? C24 S6 C15 93.6(8) . . ? C25 S7 C16 94.7(7) . . ? C16 S8 C26 94.0(7) . . ? C27 S9 C17 95.5(8) . . ? C17 S10 C28 94.9(8) . . ? C18 S11 C29 94.8(7) . . ? C30 S12 C18 95.7(7) . . ? C14 C13 S2 122.7(9) . . ? C14 C13 S1 122.6(9) . . ? S2 C13 S1 114.6(7) . . ? C13 C14 S3 123.5(10) . . ? C13 C14 S4 120.4(10) . . ? S3 C14 S4 115.9(7) . . ? C16 C15 S5 123.5(10) . . ? C16 C15 S6 122.2(10) . . ? S5 C15 S6 114.2(8) . . ? C15 C16 S8 124.4(10) . . ? C15 C16 S7 120.6(10) . . ? S8 C16 S7 115.0(8) . . ? C18 C17 S10 123.4(11) . . ? C18 C17 S9 121.5(11) . . ? S10 C17 S9 115.0(8) . . ? C17 C18 S12 122.6(11) . . ? C17 C18 S11 121.7(10) . . ? S12 C18 S11 115.7(8) . . ? C20 C19 S1 116.8(12) . . ? C19 C20 S2 117.4(12) . . ? C22 C21 S3 117.7(12) . . ? C21 C22 S4 116.5(12) . . ? C24 C23 S5 118.2(14) . . ? C23 C24 S6 119.4(14) . . ? C26 C25 S7 116.7(13) . . ? C25 C26 S8 119.6(13) . . ? C28 C27 S9 116.8(14) . . ? C27 C28 S10 117.8(14) . . ? C30 C29 S11 116.4(13) . . ? C29 C30 S12 117.5(13) . . ? C32 C31 C35 107.3(11) . . ? C32 C31 C41 127.3(11) . . ? C35 C31 C41 125.4(12) . . ? C33 C32 C31 108.5(11) . . ? C33 C32 C42 124.3(11) . . ? C31 C32 C42 127.1(11) . . ? C32 C33 C34 108.0(11) . . ? C32 C33 C43 125.3(11) . . ? C34 C33 C43 126.4(11) . . ? C35 C34 C33 107.3(11) . . ? C35 C34 C44 126.8(12) . . ? C33 C34 C44 125.9(12) . . ? C34 C35 C31 108.9(11) . . ? C34 C35 C45 122.2(12) . . ? C31 C35 C45 128.9(12) . . ? C40 C36 C37 109.5(10) . . ? C40 C36 C46 123.8(10) . . ? C37 C36 C46 125.9(11) . . ? C38 C37 C36 108.0(11) . . ? C38 C37 C47 124.9(12) . . ? C36 C37 C47 127.0(12) . . ? C37 C38 C39 107.7(11) . . ? C37 C38 C48 123.7(12) . . ? C39 C38 C48 128.3(12) . . ? C40 C39 C38 107.1(11) . . ? C40 C39 C49 128.0(11) . . ? C38 C39 C49 124.8(11) . . ? C36 C40 C39 107.6(10) . . ? C36 C40 C50 125.6(10) . . ? C39 C40 C50 126.7(10) . . ? O51 C41 O61 122.0(13) . . ? O51 C41 C31 124.3(13) . . ? O61 C41 C31 113.7(11) . . ? O52 C42 O62 120.9(13) . . ? O52 C42 C32 126.5(13) . . ? O62 C42 C32 112.5(11) . . ? O53 C43 O63 121.9(13) . . ? O53 C43 C33 124.8(13) . . ? O63 C43 C33 113.3(11) . . ? O54 C44 O64 123.6(15) . . ? O54 C44 C34 125.2(14) . . ? O64 C44 C34 111.1(13) . . ? O55 C45 O65 124.9(14) . . ? O55 C45 C35 124.9(14) . . ? O65 C45 C35 110.2(12) . . ? O56 C46 O66 123.0(12) . . ? O56 C46 C36 126.5(12) . . ? O66 C46 C36 110.5(10) . . ? O57 C47 O67 119.7(14) . . ? O57 C47 C37 127.1(14) . . ? O67 C47 C37 112.9(12) . . ? O58 C48 O68 120.6(14) . . ? O58 C48 C38 123.6(14) . . ? O68 C48 C38 115.7(12) . . ? O59 C49 O69 122.4(13) . . ? O59 C49 C39 125.0(13) . . ? O69 C49 C39 112.6(11) . . ? O60 C50 O70 124.9(12) . . ? O60 C50 C40 125.3(12) . . ? O70 C50 C40 109.8(11) . . ? C41 O61 C71 117.7(12) . . ? C42 O62 C72 116.9(13) . . ? C43 O63 C73 114.9(13) . . ? C44 O64 C74 116.8(13) . . ? C45 O65 C75 115.2(13) . . ? C46 O66 C76 115.4(11) . . ? C47 O67 C77 119.2(11) . . ? C48 O68 C78 114.6(13) . . ? C49 O69 C79 117.5(13) . . ? C50 O70 C80 116.8(12) . . ? _diffrn_measured_fraction_theta_max 0.499 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.499 _refine_diff_density_max 0.39 _refine_diff_density_min -0.26 _refine_diff_density_rms 0.07