data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H25 N O7 S' _chemical_formula_weight 555.58 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' _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 10.0018(6) _cell_length_b 11.5034(6) _cell_length_c 12.0989(6) _cell_angle_alpha 88.001(2) _cell_angle_beta 75.075(2) _cell_angle_gamma 78.255(2) _cell_volume 1316.69(12) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9675 _exptl_absorpt_correction_T_max 0.9709 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 '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 29398 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4879 _reflns_number_gt 4018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1476P)^2^+1.3376P] 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 4879 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 0.725 _refine_ls_restrained_S_all 0.725 _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 S1 S 0.34380(6) 0.23498(5) 0.79782(5) 0.0482(2) Uani 1 1 d . . . O1 O 0.4605(2) 0.13730(19) 0.78519(18) 0.0702(6) Uani 1 1 d . . . O2 O 0.3655(2) 0.35351(16) 0.79572(16) 0.0594(5) Uani 1 1 d . . . O3 O 0.35602(18) 0.64638(16) 0.46479(17) 0.0609(5) Uani 1 1 d . . . O4 O 0.12966(18) 0.75200(15) 0.48542(16) 0.0560(5) Uani 1 1 d . . . O5 O -0.05899(15) 0.43133(13) 0.70314(13) 0.0411(4) Uani 1 1 d . . . O6 O -0.0264(2) 0.13159(15) 0.76694(17) 0.0623(5) Uani 1 1 d . . . O7 O -0.5565(2) 0.36423(17) 1.14827(15) 0.0608(5) Uani 1 1 d . . . N1 N 0.27059(19) 0.22174(15) 0.69289(15) 0.0404(4) Uani 1 1 d . . . C1 C -0.1256(4) 0.1883(4) 1.2149(3) 0.0857(10) Uani 1 1 d . . . H1A H -0.1860 0.1454 1.1903 0.129 Uiso 1 1 calc R . . H1B H -0.1776 0.2662 1.2415 0.129 Uiso 1 1 calc R . . H1C H -0.0922 0.1467 1.2758 0.129 Uiso 1 1 calc R . . C2 C -0.0024(3) 0.1987(3) 1.1167(2) 0.0613(7) Uani 1 1 d . . . C3 C 0.0267(3) 0.3095(3) 1.0818(2) 0.0633(7) Uani 1 1 d . . . H3 H -0.0267 0.3771 1.1236 0.076 Uiso 1 1 calc R . . C4 C 0.1334(3) 0.3206(2) 0.9863(2) 0.0571(6) Uani 1 1 d . . . H4 H 0.1499 0.3954 0.9628 0.068 Uiso 1 1 calc R . . C5 C 0.2160(3) 0.2204(2) 0.9255(2) 0.0473(5) Uani 1 1 d . . . C6 C 0.1932(3) 0.1090(2) 0.9615(2) 0.0621(7) Uani 1 1 d . . . H6 H 0.2504 0.0412 0.9223 0.075 Uiso 1 1 calc R . . C7 C 0.0850(4) 0.0997(3) 1.0559(2) 0.0687(8) Uani 1 1 d . . . H7 H 0.0700 0.0247 1.0797 0.082 Uiso 1 1 calc R . . C8 C 0.2852(3) 0.10223(19) 0.6429(2) 0.0465(5) Uani 1 1 d . . . H8A H 0.2061 0.0672 0.6830 0.056 Uiso 1 1 calc R . . H8B H 0.3712 0.0512 0.6525 0.056 Uiso 1 1 calc R . . C9 C 0.2894(2) 0.11006(18) 0.51789(19) 0.0417(5) Uani 1 1 d . . . C10 C 0.3963(3) 0.1522(2) 0.4410(2) 0.0598(7) Uani 1 1 d . . . H10 H 0.4641 0.1797 0.4673 0.072 Uiso 1 1 calc R . . C11 C 0.4032(4) 0.1537(3) 0.3252(3) 0.0783(10) Uani 1 1 d . . . H11 H 0.4760 0.1814 0.2738 0.094 Uiso 1 1 calc R . . C12 C 0.3029(5) 0.1144(3) 0.2865(3) 0.0830(11) Uani 1 1 d . . . H12 H 0.3071 0.1161 0.2087 0.100 Uiso 1 1 calc R . . C13 C 0.1977(4) 0.0732(3) 0.3606(3) 0.0792(10) Uani 1 1 d . . . H13 H 0.1303 0.0460 0.3336 0.095 Uiso 1 1 calc R . . C14 C 0.1896(3) 0.0711(2) 0.4768(2) 0.0587(6) Uani 1 1 d . . . H14 H 0.1164 0.0433 0.5273 0.070 Uiso 1 1 calc R . . C15 C 0.1567(2) 0.31547(17) 0.68405(17) 0.0359(4) Uani 1 1 d . . . C16 C 0.0154(2) 0.32250(18) 0.72732(17) 0.0379(5) Uani 1 1 d . . . C17 C 0.0392(2) 0.49290(18) 0.64278(17) 0.0374(5) Uani 1 1 d . . . C18 C 0.1746(2) 0.42580(17) 0.62971(17) 0.0355(4) Uani 1 1 d . . . C19 C 0.2934(2) 0.47063(19) 0.56930(19) 0.0424(5) Uani 1 1 d . . . H19 H 0.3855 0.4286 0.5600 0.051 Uiso 1 1 calc R . . C20 C 0.2621(2) 0.5803(2) 0.52585(19) 0.0429(5) Uani 1 1 d . . . C21 C 0.1244(2) 0.64514(19) 0.53880(19) 0.0419(5) Uani 1 1 d . . . C22 C 0.0073(2) 0.60586(19) 0.59832(19) 0.0424(5) Uani 1 1 d . . . H22 H -0.0842 0.6496 0.6083 0.051 Uiso 1 1 calc R . . C23 C 0.2740(3) 0.7476(3) 0.4293(3) 0.0645(7) Uani 1 1 d . . . H23A H 0.2875 0.7442 0.3470 0.077 Uiso 1 1 calc R . . H23B H 0.3027 0.8185 0.4482 0.077 Uiso 1 1 calc R . . C24 C -0.0692(2) 0.23733(19) 0.78931(19) 0.0417(5) Uani 1 1 d . . . C25 C -0.2010(2) 0.28014(19) 0.87772(18) 0.0407(5) Uani 1 1 d . . . C26 C -0.3004(3) 0.2078(2) 0.9082(2) 0.0458(5) Uani 1 1 d . . . H26 H -0.2864 0.1373 0.8675 0.055 Uiso 1 1 calc R . . C27 C -0.4181(3) 0.2388(2) 0.9968(2) 0.0503(6) Uani 1 1 d . . . H27 H -0.4848 0.1907 1.0146 0.060 Uiso 1 1 calc R . . C28 C -0.4383(2) 0.3427(2) 1.06048(19) 0.0458(5) Uani 1 1 d . . . C29 C -0.3417(3) 0.4160(2) 1.0317(2) 0.0499(6) Uani 1 1 d . . . H29 H -0.3546 0.4855 1.0736 0.060 Uiso 1 1 calc R . . C30 C -0.2257(3) 0.3850(2) 0.9398(2) 0.0478(5) Uani 1 1 d . . . H30 H -0.1623 0.4357 0.9190 0.057 Uiso 1 1 calc R . . C31 C -0.5683(3) 0.4548(3) 1.2308(2) 0.0672(8) Uani 1 1 d . . . H31A H -0.4874 0.4381 1.2619 0.101 Uiso 1 1 calc R . . H31B H -0.6525 0.4565 1.2912 0.101 Uiso 1 1 calc R . . H31C H -0.5729 0.5305 1.1944 0.101 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 0.0472(4) 0.0462(4) 0.0542(4) -0.0012(3) -0.0203(3) -0.0067(3) O1 0.0573(12) 0.0706(13) 0.0829(14) -0.0053(10) -0.0344(10) 0.0092(9) O2 0.0648(12) 0.0578(11) 0.0647(11) 0.0013(8) -0.0209(9) -0.0279(9) O3 0.0397(9) 0.0511(10) 0.0828(13) 0.0235(9) -0.0018(8) -0.0100(8) O4 0.0452(9) 0.0405(9) 0.0756(12) 0.0188(8) -0.0087(8) -0.0048(7) O5 0.0317(7) 0.0356(8) 0.0505(9) 0.0034(6) -0.0029(6) -0.0046(6) O6 0.0608(11) 0.0381(9) 0.0754(12) -0.0001(8) 0.0056(9) -0.0108(8) O7 0.0542(11) 0.0651(12) 0.0546(10) -0.0031(8) 0.0084(8) -0.0211(9) N1 0.0432(10) 0.0321(9) 0.0433(10) -0.0037(7) -0.0131(8) 0.0014(7) C1 0.101(3) 0.101(3) 0.0638(19) 0.0183(17) -0.0189(18) -0.045(2) C2 0.0814(19) 0.0700(18) 0.0449(13) 0.0123(12) -0.0268(13) -0.0315(15) C3 0.079(2) 0.0557(16) 0.0555(15) -0.0029(12) -0.0136(14) -0.0188(14) C4 0.0754(18) 0.0413(13) 0.0568(14) -0.0006(11) -0.0154(13) -0.0188(12) C5 0.0627(15) 0.0415(12) 0.0448(12) 0.0033(9) -0.0237(11) -0.0146(11) C6 0.093(2) 0.0426(14) 0.0553(15) 0.0073(11) -0.0275(14) -0.0144(13) C7 0.110(3) 0.0509(16) 0.0590(16) 0.0178(13) -0.0356(16) -0.0324(16) C8 0.0536(14) 0.0303(11) 0.0500(12) -0.0039(9) -0.0089(10) -0.0004(9) C9 0.0432(12) 0.0281(10) 0.0476(12) -0.0063(8) -0.0085(9) 0.0041(8) C10 0.0652(17) 0.0528(15) 0.0578(15) -0.0006(12) -0.0082(13) -0.0129(13) C11 0.100(3) 0.0635(18) 0.0547(16) 0.0052(13) 0.0015(16) -0.0073(17) C12 0.110(3) 0.073(2) 0.0558(17) -0.0113(15) -0.0300(19) 0.016(2) C13 0.084(2) 0.076(2) 0.083(2) -0.0232(17) -0.0420(19) 0.0028(17) C14 0.0534(15) 0.0521(15) 0.0691(17) -0.0114(12) -0.0181(13) -0.0020(12) C15 0.0378(11) 0.0314(10) 0.0364(10) -0.0037(8) -0.0077(8) -0.0039(8) C16 0.0391(11) 0.0320(10) 0.0402(11) -0.0023(8) -0.0072(9) -0.0050(8) C17 0.0321(10) 0.0354(10) 0.0410(11) -0.0029(8) -0.0033(8) -0.0061(8) C18 0.0336(10) 0.0311(10) 0.0382(10) -0.0031(8) -0.0057(8) -0.0026(8) C19 0.0312(11) 0.0382(11) 0.0514(12) 0.0016(9) -0.0040(9) -0.0008(8) C20 0.0360(11) 0.0405(12) 0.0475(12) 0.0030(9) -0.0031(9) -0.0070(9) C21 0.0421(12) 0.0329(11) 0.0477(12) 0.0030(9) -0.0094(9) -0.0035(9) C22 0.0343(11) 0.0347(11) 0.0537(13) 0.0009(9) -0.0082(9) -0.0003(8) C23 0.0506(15) 0.0538(15) 0.0828(19) 0.0250(14) -0.0083(13) -0.0112(12) C24 0.0436(12) 0.0360(11) 0.0448(12) 0.0015(9) -0.0090(9) -0.0094(9) C25 0.0407(12) 0.0394(11) 0.0424(11) 0.0030(9) -0.0090(9) -0.0117(9) C26 0.0497(13) 0.0406(12) 0.0481(12) -0.0005(9) -0.0101(10) -0.0146(10) C27 0.0483(13) 0.0506(14) 0.0548(13) 0.0051(10) -0.0076(11) -0.0242(11) C28 0.0426(12) 0.0498(13) 0.0421(11) 0.0039(9) -0.0041(9) -0.0116(10) C29 0.0528(14) 0.0435(13) 0.0501(13) -0.0048(10) -0.0015(10) -0.0159(11) C30 0.0467(13) 0.0453(13) 0.0506(13) -0.0017(10) -0.0026(10) -0.0196(10) C31 0.0629(17) 0.0709(18) 0.0558(15) -0.0100(13) 0.0066(13) -0.0125(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2 1.4219(18) . ? S1 O1 1.426(2) . ? S1 N1 1.6459(19) . ? S1 C5 1.761(3) . ? O3 C20 1.379(3) . ? O3 C23 1.404(3) . ? O4 C21 1.373(3) . ? O4 C23 1.420(3) . ? O5 C17 1.370(2) . ? O5 C16 1.384(2) . ? O6 C24 1.220(3) . ? O7 C28 1.356(3) . ? O7 C31 1.434(3) . ? N1 C15 1.423(3) . ? N1 C8 1.486(3) . ? C1 C2 1.497(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.387(5) . ? C2 C3 1.392(4) . ? C3 C4 1.379(4) . ? C3 H3 0.9300 . ? C4 C5 1.381(4) . ? C4 H4 0.9300 . ? C5 C6 1.384(3) . ? C6 C7 1.374(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.502(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.377(3) . ? C9 C10 1.383(4) . ? C10 C11 1.385(4) . ? C10 H10 0.9300 . ? C11 C12 1.369(5) . ? C11 H11 0.9300 . ? C12 C13 1.350(5) . ? C12 H12 0.9300 . ? C13 C14 1.386(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.361(3) . ? C15 C18 1.431(3) . ? C16 C24 1.483(3) . ? C17 C18 1.388(3) . ? C17 C22 1.397(3) . ? C18 C19 1.410(3) . ? C19 C20 1.357(3) . ? C19 H19 0.9300 . ? C20 C21 1.399(3) . ? C21 C22 1.361(3) . ? C22 H22 0.9300 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.473(3) . ? C25 C30 1.388(3) . ? C25 C26 1.394(3) . ? C26 C27 1.367(3) . ? C26 H26 0.9300 . ? C27 C28 1.396(3) . ? C27 H27 0.9300 . ? C28 C29 1.380(3) . ? C29 C30 1.379(3) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 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 O2 S1 O1 120.31(13) . . ? O2 S1 N1 106.64(10) . . ? O1 S1 N1 106.35(11) . . ? O2 S1 C5 107.15(11) . . ? O1 S1 C5 109.36(13) . . ? N1 S1 C5 106.21(11) . . ? C20 O3 C23 106.17(18) . . ? C21 O4 C23 105.97(18) . . ? C17 O5 C16 106.52(16) . . ? C28 O7 C31 118.0(2) . . ? C15 N1 C8 120.60(18) . . ? C15 N1 S1 115.97(13) . . ? C8 N1 S1 119.43(15) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 117.5(3) . . ? C7 C2 C1 121.8(3) . . ? C3 C2 C1 120.6(3) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 S1 119.95(19) . . ? C6 C5 S1 119.9(2) . . ? C7 C6 C5 119.2(3) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C2 122.2(3) . . ? C6 C7 H7 118.9 . . ? C2 C7 H7 118.9 . . ? N1 C8 C9 110.89(18) . . ? N1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C14 C9 C10 118.5(2) . . ? C14 C9 C8 120.6(2) . . ? C10 C9 C8 120.8(2) . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C9 C14 C13 120.5(3) . . ? C9 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 N1 128.90(19) . . ? C16 C15 C18 107.08(18) . . ? N1 C15 C18 123.95(18) . . ? C15 C16 O5 110.38(18) . . ? C15 C16 C24 132.9(2) . . ? O5 C16 C24 116.66(18) . . ? O5 C17 C18 110.33(17) . . ? O5 C17 C22 124.75(19) . . ? C18 C17 C22 124.90(19) . . ? C17 C18 C19 120.57(19) . . ? C17 C18 C15 105.68(18) . . ? C19 C18 C15 133.73(19) . . ? C20 C19 C18 114.43(19) . . ? C20 C19 H19 122.8 . . ? C18 C19 H19 122.8 . . ? C19 C20 O3 127.2(2) . . ? C19 C20 C21 123.8(2) . . ? O3 C20 C21 108.99(19) . . ? C22 C21 O4 127.4(2) . . ? C22 C21 C20 123.5(2) . . ? O4 C21 C20 109.10(19) . . ? C21 C22 C17 112.80(19) . . ? C21 C22 H22 123.6 . . ? C17 C22 H22 123.6 . . ? O3 C23 O4 108.82(19) . . ? O3 C23 H23A 109.9 . . ? O4 C23 H23A 109.9 . . ? O3 C23 H23B 109.9 . . ? O4 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O6 C24 C25 120.9(2) . . ? O6 C24 C16 118.7(2) . . ? C25 C24 C16 120.30(19) . . ? C30 C25 C26 117.9(2) . . ? C30 C25 C24 122.87(19) . . ? C26 C25 C24 119.0(2) . . ? C27 C26 C25 121.0(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.0(2) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? O7 C28 C29 124.4(2) . . ? O7 C28 C27 115.6(2) . . ? C29 C28 C27 120.0(2) . . ? C30 C29 C28 119.1(2) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C25 121.9(2) . . ? C29 C30 H30 119.1 . . ? C25 C30 H30 119.1 . . ? O7 C31 H31A 109.5 . . ? O7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 O2 S1 N1 C15 -46.20(18) . . . . ? O1 S1 N1 C15 -175.73(16) . . . . ? C5 S1 N1 C15 67.84(18) . . . . ? O2 S1 N1 C8 156.15(17) . . . . ? O1 S1 N1 C8 26.6(2) . . . . ? C5 S1 N1 C8 -89.81(18) . . . . ? C7 C2 C3 C4 3.7(4) . . . . ? C1 C2 C3 C4 -175.1(3) . . . . ? C2 C3 C4 C5 -1.8(4) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C3 C4 C5 S1 175.4(2) . . . . ? O2 S1 C5 C4 15.9(2) . . . . ? O1 S1 C5 C4 147.8(2) . . . . ? N1 S1 C5 C4 -97.8(2) . . . . ? O2 S1 C5 C6 -167.6(2) . . . . ? O1 S1 C5 C6 -35.7(2) . . . . ? N1 S1 C5 C6 78.7(2) . . . . ? C4 C5 C6 C7 2.1(4) . . . . ? S1 C5 C6 C7 -174.5(2) . . . . ? C5 C6 C7 C2 -0.1(4) . . . . ? C3 C2 C7 C6 -2.8(4) . . . . ? C1 C2 C7 C6 176.1(3) . . . . ? C15 N1 C8 C9 55.6(3) . . . . ? S1 N1 C8 C9 -147.85(17) . . . . ? N1 C8 C9 C14 -120.5(2) . . . . ? N1 C8 C9 C10 62.0(3) . . . . ? C14 C9 C10 C11 -0.7(4) . . . . ? C8 C9 C10 C11 176.9(2) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C10 C11 C12 C13 -0.6(5) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C10 C9 C14 C13 0.7(4) . . . . ? C8 C9 C14 C13 -176.9(2) . . . . ? C12 C13 C14 C9 -0.6(4) . . . . ? C8 N1 C15 C16 62.6(3) . . . . ? S1 N1 C15 C16 -94.8(2) . . . . ? C8 N1 C15 C18 -120.7(2) . . . . ? S1 N1 C15 C18 81.9(2) . . . . ? N1 C15 C16 O5 177.50(18) . . . . ? C18 C15 C16 O5 0.4(2) . . . . ? N1 C15 C16 C24 -4.8(4) . . . . ? C18 C15 C16 C24 178.1(2) . . . . ? C17 O5 C16 C15 0.3(2) . . . . ? C17 O5 C16 C24 -177.86(17) . . . . ? C16 O5 C17 C18 -0.9(2) . . . . ? C16 O5 C17 C22 177.6(2) . . . . ? O5 C17 C18 C19 179.43(18) . . . . ? C22 C17 C18 C19 0.9(3) . . . . ? O5 C17 C18 C15 1.1(2) . . . . ? C22 C17 C18 C15 -177.4(2) . . . . ? C16 C15 C18 C17 -0.9(2) . . . . ? N1 C15 C18 C17 -178.18(18) . . . . ? C16 C15 C18 C19 -178.9(2) . . . . ? N1 C15 C18 C19 3.8(4) . . . . ? C17 C18 C19 C20 -1.0(3) . . . . ? C15 C18 C19 C20 176.7(2) . . . . ? C18 C19 C20 O3 179.0(2) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? C23 O3 C20 C19 174.5(3) . . . . ? C23 O3 C20 C21 -6.4(3) . . . . ? C23 O4 C21 C22 -176.2(3) . . . . ? C23 O4 C21 C20 5.4(3) . . . . ? C19 C20 C21 C22 1.3(4) . . . . ? O3 C20 C21 C22 -177.9(2) . . . . ? C19 C20 C21 O4 179.7(2) . . . . ? O3 C20 C21 O4 0.6(3) . . . . ? O4 C21 C22 C17 -179.5(2) . . . . ? C20 C21 C22 C17 -1.4(3) . . . . ? O5 C17 C22 C21 -178.0(2) . . . . ? C18 C17 C22 C21 0.3(3) . . . . ? C20 O3 C23 O4 9.7(3) . . . . ? C21 O4 C23 O3 -9.4(3) . . . . ? C15 C16 C24 O6 -32.5(4) . . . . ? O5 C16 C24 O6 145.1(2) . . . . ? C15 C16 C24 C25 146.3(2) . . . . ? O5 C16 C24 C25 -36.1(3) . . . . ? O6 C24 C25 C30 152.4(2) . . . . ? C16 C24 C25 C30 -26.4(3) . . . . ? O6 C24 C25 C26 -21.6(3) . . . . ? C16 C24 C25 C26 159.6(2) . . . . ? C30 C25 C26 C27 -0.4(4) . . . . ? C24 C25 C26 C27 174.0(2) . . . . ? C25 C26 C27 C28 -1.8(4) . . . . ? C31 O7 C28 C29 -13.4(4) . . . . ? C31 O7 C28 C27 167.2(2) . . . . ? C26 C27 C28 O7 -178.5(2) . . . . ? C26 C27 C28 C29 2.1(4) . . . . ? O7 C28 C29 C30 -179.6(2) . . . . ? C27 C28 C29 C30 -0.2(4) . . . . ? C28 C29 C30 C25 -2.1(4) . . . . ? C26 C25 C30 C29 2.3(4) . . . . ? C24 C25 C30 C29 -171.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.411 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.157