data_qq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H18 O2 S' _chemical_formula_weight 298.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 9.917(18) _cell_length_b 10.332(18) _cell_length_c 17.37(4) _cell_angle_alpha 89.13(7) _cell_angle_beta 88.64(7) _cell_angle_gamma 67.30(5) _cell_volume 1642(5) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 2788 _cell_measurement_theta_min 3.1630 _cell_measurement_theta_max 25.3426 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.199 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9901 _exptl_absorpt_correction_T_max 0.9960 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn70 CCD (4x4 bin mode) with MicroMax-007 ; _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 15111 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_av_sigmaI/netI 0.1192 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5638 _reflns_number_gt 3305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RIGAKU CrystalClear' _computing_cell_refinement 'RIGAKU CrystalClear' _computing_data_reduction 'RIGAKU CrystalClear' _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5638 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1788 _refine_ls_R_factor_gt 0.1153 _refine_ls_wR_factor_ref 0.3115 _refine_ls_wR_factor_gt 0.2623 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.94069(16) 0.20405(16) 0.81667(9) 0.0429(5) Uani 1 1 d . . . C1 C 0.7994(6) 0.3225(6) 0.8782(4) 0.0407(15) Uani 1 1 d . . . C2 C 0.7376(6) 0.4549(6) 0.8400(3) 0.0385(15) Uani 1 1 d . . . H1 H 0.6622 0.5341 0.8623 0.046 Uiso 1 1 calc R . . C3 C 0.8014(6) 0.4578(6) 0.7626(4) 0.0397(15) Uani 1 1 d . . . C4 C 0.7336(6) 0.5894(6) 0.7144(4) 0.0428(16) Uani 1 1 d . . . H2 H 0.6624 0.6666 0.7406 0.051 Uiso 1 1 calc R . . C5 C 0.7596(7) 0.6153(6) 0.6368(4) 0.0440(16) Uani 1 1 d . . . C6 C 0.8783(7) 0.5133(6) 0.5813(4) 0.0480(17) Uani 1 1 d . . . H3 H 0.8418 0.5360 0.5282 0.058 Uiso 1 1 calc R . . H4 H 0.9666 0.5356 0.5842 0.058 Uiso 1 1 calc R . . C7 C 0.9277(7) 0.3514(7) 0.5927(4) 0.0498(17) Uani 1 1 d . . . H5 H 0.8399 0.3280 0.5920 0.060 Uiso 1 1 calc R . . H6 H 0.9908 0.3041 0.5482 0.060 Uiso 1 1 calc R . . C8 C 1.0120(7) 0.2899(7) 0.6679(3) 0.0483(17) Uani 1 1 d . . . H7 H 1.0558 0.1863 0.6641 0.058 Uiso 1 1 calc R . . H8 H 1.0929 0.3229 0.6721 0.058 Uiso 1 1 calc R . . C9 C 0.9157(6) 0.3306(6) 0.7423(4) 0.0420(15) Uani 1 1 d . . . C10 C 0.7669(6) 0.2761(6) 0.9578(3) 0.0341(14) Uani 1 1 d . . . C11 C 0.6922(6) 0.3789(6) 1.0155(4) 0.0422(15) Uani 1 1 d . . . H9 H 0.6595 0.4758 1.0029 0.051 Uiso 1 1 calc R . . C12 C 0.6663(6) 0.3372(6) 1.0916(4) 0.0428(16) Uani 1 1 d . . . H10 H 0.6159 0.4067 1.1287 0.051 Uiso 1 1 calc R . . C13 C 0.7154(6) 0.1931(6) 1.1121(4) 0.0422(16) Uani 1 1 d . . . C14 C 0.7886(6) 0.0890(7) 1.0543(3) 0.0401(15) Uani 1 1 d . . . H11 H 0.8198 -0.0078 1.0669 0.048 Uiso 1 1 calc R . . C15 C 0.8142(6) 0.1309(6) 0.9784(4) 0.0399(15) Uani 1 1 d . . . H12 H 0.8634 0.0613 0.9412 0.048 Uiso 1 1 calc R . . C16 C 0.6987(7) 0.1448(7) 1.1966(4) 0.0502(17) Uani 1 1 d . . . H13 H 0.6813 0.0577 1.1954 0.075 Uiso 1 1 calc R . . H14 H 0.6159 0.2178 1.2225 0.075 Uiso 1 1 calc R . . H15 H 0.7883 0.1287 1.2247 0.075 Uiso 1 1 calc R . . C17 C 0.6695(7) 0.7568(7) 0.5992(4) 0.0475(17) Uani 1 1 d . . . O1 O 0.6858(5) 0.7905(5) 0.5315(3) 0.0574(13) Uani 1 1 d . . . O2 O 0.5633(5) 0.8472(5) 0.6492(3) 0.0577(13) Uani 1 1 d . . . C18 C 0.4617(7) 0.9817(7) 0.6134(4) 0.062(2) Uani 1 1 d . . . H16 H 0.3901 0.9630 0.5823 0.093 Uiso 1 1 calc R . . H17 H 0.5180 1.0212 0.5804 0.093 Uiso 1 1 calc R . . H18 H 0.4106 1.0487 0.6540 0.093 Uiso 1 1 calc R . . S2 S 0.46932(16) 0.22819(17) 0.83361(10) 0.0433(5) Uani 1 1 d . . . C19 C 0.2929(6) 0.3153(6) 0.8790(3) 0.0349(14) Uani 1 1 d . . . C20 C 0.2029(6) 0.4214(6) 0.8304(3) 0.0410(15) Uani 1 1 d . . . H19 H 0.1043 0.4784 0.8433 0.049 Uiso 1 1 calc R . . C21 C 0.2758(6) 0.4369(6) 0.7570(3) 0.0396(15) Uani 1 1 d . . . C22 C 0.1954(6) 0.5609(6) 0.7034(3) 0.0426(15) Uani 1 1 d . . . H20 H 0.0973 0.6164 0.7181 0.051 Uiso 1 1 calc R . . C23 C 0.2456(6) 0.6034(6) 0.6364(4) 0.0416(15) Uani 1 1 d . . . C24 C 0.3940(7) 0.5261(7) 0.5934(4) 0.060(2) Uani 1 1 d . . . H21 H 0.4641 0.5661 0.6108 0.072 Uiso 1 1 calc R . . H22 H 0.3791 0.5471 0.5378 0.072 Uiso 1 1 calc R . . C25 C 0.4668(7) 0.3623(7) 0.6037(4) 0.0485(17) Uani 1 1 d . . . H23 H 0.3917 0.3228 0.5960 0.058 Uiso 1 1 calc R . . H24 H 0.5433 0.3236 0.5632 0.058 Uiso 1 1 calc R . . C26 C 0.5371(6) 0.3128(7) 0.6841(4) 0.0479(17) Uani 1 1 d . . . H25 H 0.6000 0.2117 0.6818 0.058 Uiso 1 1 calc R . . H26 H 0.5999 0.3644 0.6961 0.058 Uiso 1 1 calc R . . C27 C 0.4204(6) 0.3373(7) 0.7498(4) 0.0430(16) Uani 1 1 d . . . C28 C 0.2641(6) 0.2723(6) 0.9595(3) 0.0375(15) Uani 1 1 d . . . C29 C 0.1154(6) 0.3069(6) 0.9892(4) 0.0414(15) Uani 1 1 d . . . H27 H 0.0348 0.3595 0.9582 0.050 Uiso 1 1 calc R . . C30 C 0.0901(7) 0.2633(6) 1.0633(4) 0.0421(15) Uani 1 1 d . . . H28 H -0.0079 0.2887 1.0813 0.051 Uiso 1 1 calc R . . C31 C 0.2076(6) 0.1814(6) 1.1129(3) 0.0388(15) Uani 1 1 d . . . C32 C 0.3539(6) 0.1514(6) 1.0840(4) 0.0444(16) Uani 1 1 d . . . H29 H 0.4340 0.1008 1.1159 0.053 Uiso 1 1 calc R . . C33 C 0.3824(6) 0.1943(6) 1.0102(3) 0.0409(15) Uani 1 1 d . . . H30 H 0.4806 0.1718 0.9934 0.049 Uiso 1 1 calc R . . C34 C 0.1769(7) 0.1313(7) 1.1940(4) 0.0487(17) Uani 1 1 d . . . H31 H 0.1787 0.1982 1.2329 0.073 Uiso 1 1 calc R . . H32 H 0.2520 0.0386 1.2052 0.073 Uiso 1 1 calc R . . H33 H 0.0805 0.1254 1.1948 0.073 Uiso 1 1 calc R . . C35 C 0.1527(7) 0.7462(7) 0.6002(4) 0.0463(16) Uani 1 1 d . . . O3 O 0.2016(5) 0.8072(5) 0.5509(3) 0.0601(13) Uani 1 1 d . . . O4 O 0.0104(4) 0.8047(4) 0.6303(2) 0.0539(12) Uani 1 1 d . . . C36 C -0.0821(7) 0.9465(6) 0.5989(4) 0.0563(19) Uani 1 1 d . . . H34 H -0.0347 1.0122 0.6081 0.084 Uiso 1 1 calc R . . H35 H -0.1783 0.9803 0.6246 0.084 Uiso 1 1 calc R . . H36 H -0.0936 0.9397 0.5434 0.084 Uiso 1 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 0.0392(9) 0.0402(9) 0.0432(10) 0.0049(8) -0.0001(7) -0.0085(7) C1 0.031(3) 0.045(4) 0.048(4) 0.002(3) -0.008(3) -0.017(3) C2 0.033(3) 0.036(3) 0.042(4) 0.002(3) 0.001(3) -0.008(3) C3 0.037(3) 0.034(3) 0.045(4) 0.012(3) -0.008(3) -0.011(3) C4 0.035(3) 0.046(4) 0.045(4) -0.001(3) 0.007(3) -0.013(3) C5 0.041(4) 0.043(4) 0.049(4) -0.002(3) -0.001(3) -0.017(3) C6 0.051(4) 0.052(4) 0.038(4) 0.011(3) -0.002(3) -0.017(3) C7 0.045(4) 0.055(4) 0.047(4) 0.005(3) 0.003(3) -0.018(3) C8 0.047(4) 0.055(4) 0.042(4) -0.003(3) 0.001(3) -0.018(3) C9 0.032(3) 0.038(3) 0.051(4) 0.008(3) -0.006(3) -0.008(3) C10 0.024(3) 0.040(3) 0.037(4) -0.002(3) -0.004(3) -0.011(3) C11 0.031(3) 0.038(3) 0.055(4) 0.005(3) -0.005(3) -0.011(3) C12 0.038(3) 0.041(4) 0.047(4) 0.006(3) -0.005(3) -0.012(3) C13 0.030(3) 0.051(4) 0.048(4) 0.012(3) -0.007(3) -0.017(3) C14 0.033(3) 0.046(4) 0.042(4) 0.009(3) -0.003(3) -0.016(3) C15 0.029(3) 0.034(3) 0.051(4) -0.001(3) -0.006(3) -0.006(3) C16 0.040(4) 0.062(4) 0.047(4) 0.011(3) -0.003(3) -0.019(3) C17 0.042(4) 0.049(4) 0.052(5) 0.001(4) -0.004(3) -0.017(3) O1 0.070(3) 0.064(3) 0.040(3) 0.012(2) -0.001(2) -0.027(3) O2 0.057(3) 0.048(3) 0.053(3) 0.016(2) -0.002(2) -0.004(2) C18 0.062(5) 0.051(4) 0.055(5) 0.015(4) -0.014(4) -0.003(4) S2 0.0312(9) 0.0464(10) 0.0482(11) 0.0094(8) -0.0024(7) -0.0105(7) C19 0.027(3) 0.044(4) 0.037(4) 0.005(3) -0.003(3) -0.017(3) C20 0.029(3) 0.042(4) 0.045(4) -0.002(3) 0.004(3) -0.005(3) C21 0.037(3) 0.044(4) 0.040(4) 0.000(3) -0.001(3) -0.019(3) C22 0.033(3) 0.047(4) 0.042(4) 0.006(3) -0.009(3) -0.008(3) C23 0.042(4) 0.036(3) 0.045(4) 0.004(3) -0.002(3) -0.012(3) C24 0.046(4) 0.073(5) 0.053(5) 0.020(4) 0.004(3) -0.015(4) C25 0.044(4) 0.052(4) 0.045(4) 0.011(3) -0.002(3) -0.015(3) C26 0.038(4) 0.050(4) 0.057(5) 0.007(3) 0.001(3) -0.018(3) C27 0.032(3) 0.057(4) 0.040(4) 0.001(3) 0.001(3) -0.017(3) C28 0.034(3) 0.032(3) 0.046(4) 0.006(3) -0.004(3) -0.012(3) C29 0.032(3) 0.040(3) 0.052(4) 0.006(3) -0.006(3) -0.014(3) C30 0.037(3) 0.042(4) 0.046(4) -0.005(3) 0.004(3) -0.013(3) C31 0.039(4) 0.035(3) 0.039(4) 0.001(3) 0.004(3) -0.011(3) C32 0.035(3) 0.037(4) 0.053(4) 0.005(3) 0.000(3) -0.006(3) C33 0.030(3) 0.047(4) 0.044(4) 0.009(3) 0.000(3) -0.013(3) C34 0.049(4) 0.047(4) 0.054(4) 0.001(3) 0.003(3) -0.022(3) C35 0.047(4) 0.047(4) 0.043(4) 0.000(3) 0.005(3) -0.017(3) O3 0.051(3) 0.067(3) 0.065(3) 0.028(3) -0.001(2) -0.027(3) O4 0.044(3) 0.050(3) 0.052(3) 0.007(2) 0.010(2) -0.002(2) C36 0.048(4) 0.041(4) 0.066(5) 0.013(3) -0.001(4) -0.002(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 S1 C9 1.777(7) . ? S1 C1 1.803(7) . ? C1 C2 1.426(8) . ? C1 C10 1.524(9) . ? C2 C3 1.477(8) . ? C2 H1 0.9500 . ? C3 C9 1.408(8) . ? C3 C4 1.513(8) . ? C4 C5 1.408(8) . ? C4 H2 0.9500 . ? C5 C17 1.533(9) . ? C5 C6 1.565(9) . ? C6 C7 1.562(9) . ? C6 H3 0.9900 . ? C6 H4 0.9900 . ? C7 C8 1.558(9) . ? C7 H5 0.9900 . ? C7 H6 0.9900 . ? C8 C9 1.551(9) . ? C8 H7 0.9900 . ? C8 H8 0.9900 . ? C10 C15 1.431(8) . ? C10 C11 1.440(8) . ? C11 C12 1.432(9) . ? C11 H9 0.9500 . ? C12 C13 1.419(8) . ? C12 H10 0.9500 . ? C13 C14 1.444(9) . ? C13 C16 1.569(9) . ? C14 C15 1.429(8) . ? C14 H11 0.9500 . ? C15 H12 0.9500 . ? C16 H13 0.9800 . ? C16 H14 0.9800 . ? C16 H15 0.9800 . ? C17 O1 1.247(8) . ? C17 O2 1.399(8) . ? O2 C18 1.503(7) . ? C18 H16 0.9800 . ? C18 H17 0.9800 . ? C18 H18 0.9800 . ? S2 C27 1.785(7) . ? S2 C19 1.798(6) . ? C19 C20 1.400(8) . ? C19 C28 1.515(8) . ? C20 C21 1.488(8) . ? C20 H19 0.9500 . ? C21 C27 1.410(8) . ? C21 C22 1.535(8) . ? C22 C23 1.385(8) . ? C22 H20 0.9500 . ? C23 C35 1.539(9) . ? C23 C24 1.556(9) . ? C24 C25 1.572(9) . ? C24 H21 0.9900 . ? C24 H22 0.9900 . ? C25 C26 1.564(9) . ? C25 H23 0.9900 . ? C25 H24 0.9900 . ? C26 C27 1.558(8) . ? C26 H25 0.9900 . ? C26 H26 0.9900 . ? C28 C33 1.448(8) . ? C28 C29 1.460(8) . ? C29 C30 1.405(8) . ? C29 H27 0.9500 . ? C30 C31 1.443(8) . ? C30 H28 0.9500 . ? C31 C32 1.441(8) . ? C31 C34 1.557(9) . ? C32 C33 1.408(8) . ? C32 H29 0.9500 . ? C33 H30 0.9500 . ? C34 H31 0.9800 . ? C34 H32 0.9800 . ? C34 H33 0.9800 . ? C35 O3 1.252(7) . ? C35 O4 1.395(7) . ? O4 C36 1.499(7) . ? C36 H34 0.9800 . ? C36 H35 0.9800 . ? C36 H36 0.9800 . ? 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 C9 S1 C1 94.0(3) . . ? C2 C1 C10 130.6(6) . . ? C2 C1 S1 108.4(5) . . ? C10 C1 S1 121.0(4) . . ? C1 C2 C3 113.9(5) . . ? C1 C2 H1 123.0 . . ? C3 C2 H1 123.0 . . ? C9 C3 C2 113.5(5) . . ? C9 C3 C4 128.5(6) . . ? C2 C3 C4 117.9(5) . . ? C5 C4 C3 130.0(6) . . ? C5 C4 H2 115.0 . . ? C3 C4 H2 115.0 . . ? C4 C5 C17 120.2(6) . . ? C4 C5 C6 126.6(6) . . ? C17 C5 C6 113.2(6) . . ? C7 C6 C5 119.6(5) . . ? C7 C6 H3 107.4 . . ? C5 C6 H3 107.4 . . ? C7 C6 H4 107.4 . . ? C5 C6 H4 107.4 . . ? H3 C6 H4 107.0 . . ? C8 C7 C6 115.7(6) . . ? C8 C7 H5 108.4 . . ? C6 C7 H5 108.4 . . ? C8 C7 H6 108.4 . . ? C6 C7 H6 108.4 . . ? H5 C7 H6 107.4 . . ? C9 C8 C7 114.0(5) . . ? C9 C8 H7 108.7 . . ? C7 C8 H7 108.7 . . ? C9 C8 H8 108.7 . . ? C7 C8 H8 108.7 . . ? H7 C8 H8 107.6 . . ? C3 C9 C8 130.2(6) . . ? C3 C9 S1 110.1(5) . . ? C8 C9 S1 119.7(5) . . ? C15 C10 C11 118.2(6) . . ? C15 C10 C1 121.6(5) . . ? C11 C10 C1 120.2(5) . . ? C12 C11 C10 121.0(6) . . ? C12 C11 H9 119.5 . . ? C10 C11 H9 119.5 . . ? C13 C12 C11 120.6(6) . . ? C13 C12 H10 119.7 . . ? C11 C12 H10 119.7 . . ? C12 C13 C14 118.9(6) . . ? C12 C13 C16 121.6(6) . . ? C14 C13 C16 119.4(6) . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H11 119.8 . . ? C13 C14 H11 119.8 . . ? C14 C15 C10 120.9(6) . . ? C14 C15 H12 119.5 . . ? C10 C15 H12 119.5 . . ? C13 C16 H13 109.5 . . ? C13 C16 H14 109.5 . . ? H13 C16 H14 109.5 . . ? C13 C16 H15 109.5 . . ? H13 C16 H15 109.5 . . ? H14 C16 H15 109.5 . . ? O1 C17 O2 122.2(6) . . ? O1 C17 C5 125.0(6) . . ? O2 C17 C5 112.8(6) . . ? C17 O2 C18 115.2(5) . . ? O2 C18 H16 109.5 . . ? O2 C18 H17 109.5 . . ? H16 C18 H17 109.5 . . ? O2 C18 H18 109.5 . . ? H16 C18 H18 109.5 . . ? H17 C18 H18 109.5 . . ? C27 S2 C19 93.0(3) . . ? C20 C19 C28 130.4(5) . . ? C20 C19 S2 109.8(4) . . ? C28 C19 S2 119.8(4) . . ? C19 C20 C21 114.0(5) . . ? C19 C20 H19 123.0 . . ? C21 C20 H19 123.0 . . ? C27 C21 C20 112.6(5) . . ? C27 C21 C22 128.2(5) . . ? C20 C21 C22 119.0(5) . . ? C23 C22 C21 129.1(6) . . ? C23 C22 H20 115.4 . . ? C21 C22 H20 115.4 . . ? C22 C23 C35 119.0(5) . . ? C22 C23 C24 127.3(5) . . ? C35 C23 C24 113.6(5) . . ? C23 C24 C25 116.9(5) . . ? C23 C24 H21 108.1 . . ? C25 C24 H21 108.1 . . ? C23 C24 H22 108.1 . . ? C25 C24 H22 108.1 . . ? H21 C24 H22 107.3 . . ? C26 C25 C24 114.2(6) . . ? C26 C25 H23 108.7 . . ? C24 C25 H23 108.7 . . ? C26 C25 H24 108.7 . . ? C24 C25 H24 108.7 . . ? H23 C25 H24 107.6 . . ? C27 C26 C25 112.5(5) . . ? C27 C26 H25 109.1 . . ? C25 C26 H25 109.1 . . ? C27 C26 H26 109.1 . . ? C25 C26 H26 109.1 . . ? H25 C26 H26 107.8 . . ? C21 C27 C26 130.9(6) . . ? C21 C27 S2 110.6(5) . . ? C26 C27 S2 118.5(5) . . ? C33 C28 C29 117.0(5) . . ? C33 C28 C19 121.7(5) . . ? C29 C28 C19 121.3(5) . . ? C30 C29 C28 120.8(6) . . ? C30 C29 H27 119.6 . . ? C28 C29 H27 119.6 . . ? C29 C30 C31 122.3(5) . . ? C29 C30 H28 118.8 . . ? C31 C30 H28 118.8 . . ? C32 C31 C30 116.4(6) . . ? C32 C31 C34 122.1(5) . . ? C30 C31 C34 121.5(5) . . ? C33 C32 C31 122.3(6) . . ? C33 C32 H29 118.8 . . ? C31 C32 H29 118.8 . . ? C32 C33 C28 121.0(5) . . ? C32 C33 H30 119.5 . . ? C28 C33 H30 119.5 . . ? C31 C34 H31 109.5 . . ? C31 C34 H32 109.5 . . ? H31 C34 H32 109.5 . . ? C31 C34 H33 109.5 . . ? H31 C34 H33 109.5 . . ? H32 C34 H33 109.5 . . ? O3 C35 O4 122.9(6) . . ? O3 C35 C23 123.4(6) . . ? O4 C35 C23 113.7(5) . . ? C35 O4 C36 115.4(5) . . ? O4 C36 H34 109.5 . . ? O4 C36 H35 109.5 . . ? H34 C36 H35 109.5 . . ? O4 C36 H36 109.5 . . ? H34 C36 H36 109.5 . . ? H35 C36 H36 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 C9 S1 C1 C2 0.0(4) . . . . ? C9 S1 C1 C10 -178.0(4) . . . . ? C10 C1 C2 C3 179.1(5) . . . . ? S1 C1 C2 C3 1.3(6) . . . . ? C1 C2 C3 C9 -2.5(7) . . . . ? C1 C2 C3 C4 174.4(5) . . . . ? C9 C3 C4 C5 4.8(11) . . . . ? C2 C3 C4 C5 -171.5(6) . . . . ? C3 C4 C5 C17 176.5(5) . . . . ? C3 C4 C5 C6 -5.2(10) . . . . ? C4 C5 C6 C7 30.0(9) . . . . ? C17 C5 C6 C7 -151.6(5) . . . . ? C5 C6 C7 C8 -66.8(8) . . . . ? C6 C7 C8 C9 70.4(7) . . . . ? C2 C3 C9 C8 -179.3(6) . . . . ? C4 C3 C9 C8 4.3(11) . . . . ? C2 C3 C9 S1 2.4(6) . . . . ? C4 C3 C9 S1 -174.1(5) . . . . ? C7 C8 C9 C3 -38.3(9) . . . . ? C7 C8 C9 S1 140.0(5) . . . . ? C1 S1 C9 C3 -1.4(5) . . . . ? C1 S1 C9 C8 -180.0(5) . . . . ? C2 C1 C10 C15 164.3(6) . . . . ? S1 C1 C10 C15 -18.2(7) . . . . ? C2 C1 C10 C11 -18.3(9) . . . . ? S1 C1 C10 C11 159.2(4) . . . . ? C15 C10 C11 C12 0.2(8) . . . . ? C1 C10 C11 C12 -177.2(5) . . . . ? C10 C11 C12 C13 0.7(8) . . . . ? C11 C12 C13 C14 -1.5(8) . . . . ? C11 C12 C13 C16 175.5(5) . . . . ? C12 C13 C14 C15 1.5(8) . . . . ? C16 C13 C14 C15 -175.5(5) . . . . ? C13 C14 C15 C10 -0.7(8) . . . . ? C11 C10 C15 C14 -0.2(8) . . . . ? C1 C10 C15 C14 177.2(5) . . . . ? C4 C5 C17 O1 178.7(6) . . . . ? C6 C5 C17 O1 0.2(9) . . . . ? C4 C5 C17 O2 -1.6(8) . . . . ? C6 C5 C17 O2 179.8(5) . . . . ? O1 C17 O2 C18 5.5(9) . . . . ? C5 C17 O2 C18 -174.1(5) . . . . ? C27 S2 C19 C20 0.6(5) . . . . ? C27 S2 C19 C28 -177.2(4) . . . . ? C28 C19 C20 C21 175.9(5) . . . . ? S2 C19 C20 C21 -1.6(6) . . . . ? C19 C20 C21 C27 2.2(7) . . . . ? C19 C20 C21 C22 -172.5(5) . . . . ? C27 C21 C22 C23 -0.2(10) . . . . ? C20 C21 C22 C23 173.6(6) . . . . ? C21 C22 C23 C35 -169.6(6) . . . . ? C21 C22 C23 C24 6.8(10) . . . . ? C22 C23 C24 C25 26.7(10) . . . . ? C35 C23 C24 C25 -156.7(6) . . . . ? C23 C24 C25 C26 -74.2(7) . . . . ? C24 C25 C26 C27 72.2(7) . . . . ? C20 C21 C27 C26 179.8(6) . . . . ? C22 C21 C27 C26 -6.1(11) . . . . ? C20 C21 C27 S2 -1.7(6) . . . . ? C22 C21 C27 S2 172.5(5) . . . . ? C25 C26 C27 C21 -27.2(9) . . . . ? C25 C26 C27 S2 154.3(5) . . . . ? C19 S2 C27 C21 0.6(5) . . . . ? C19 S2 C27 C26 179.4(5) . . . . ? C20 C19 C28 C33 -158.7(6) . . . . ? S2 C19 C28 C33 18.6(7) . . . . ? C20 C19 C28 C29 21.7(9) . . . . ? S2 C19 C28 C29 -161.0(4) . . . . ? C33 C28 C29 C30 -1.3(8) . . . . ? C19 C28 C29 C30 178.3(5) . . . . ? C28 C29 C30 C31 -0.9(9) . . . . ? C29 C30 C31 C32 2.7(8) . . . . ? C29 C30 C31 C34 -178.5(6) . . . . ? C30 C31 C32 C33 -2.4(8) . . . . ? C34 C31 C32 C33 178.9(5) . . . . ? C31 C32 C33 C28 0.3(9) . . . . ? C29 C28 C33 C32 1.5(8) . . . . ? C19 C28 C33 C32 -178.0(5) . . . . ? C22 C23 C35 O3 163.7(6) . . . . ? C24 C23 C35 O3 -13.1(9) . . . . ? C22 C23 C35 O4 -13.3(8) . . . . ? C24 C23 C35 O4 169.8(5) . . . . ? O3 C35 O4 C36 0.6(9) . . . . ? C23 C35 O4 C36 177.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.678 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.091