# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email 'jlzhang@chem.ecnu.edu.cn ' _publ_contact_author_name 'Junliang Zhang' loop_ _publ_author_name 'Junliang Zhang' 'Xingxing Wu' 'Lei Li' data_z _database_code_depnum_ccdc_archive 'CCDC 795474' #TrackingRef '- 4aa.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H31 N O10 S' _chemical_formula_weight 585.61 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 11.3456(4) _cell_length_b 11.9555(5) _cell_length_c 12.1699(5) _cell_angle_alpha 83.2260(10) _cell_angle_beta 64.7520(10) _cell_angle_gamma 78.1390(10) _cell_volume 1460.32(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9544 _exptl_absorpt_correction_T_max 0.9883 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 17083 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5115 _reflns_number_gt 4480 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.7044P] 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 5115 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.96902(4) 0.20619(3) 0.19968(3) 0.02242(11) Uani 1 1 d . . . O1 O 1.32910(11) 0.19765(9) 0.14375(10) 0.0246(2) Uani 1 1 d . . . O2 O 0.97947(12) 0.25340(10) 0.08297(10) 0.0315(3) Uani 1 1 d . . . O3 O 0.91740(11) 0.10261(9) 0.24572(11) 0.0288(3) Uani 1 1 d . . . O4 O 1.14251(12) 0.13675(10) 0.40559(10) 0.0310(3) Uani 1 1 d . . . O5 O 1.16502(15) -0.05244(10) 0.39967(12) 0.0429(3) Uani 1 1 d . . . O6 O 1.17191(12) 0.00192(10) 0.04905(10) 0.0310(3) Uani 1 1 d . . . O7 O 1.13103(14) -0.12107(10) 0.20898(12) 0.0388(3) Uani 1 1 d . . . O8 O 1.62490(12) 0.01114(10) 0.35767(11) 0.0345(3) Uani 1 1 d . . . O9 O 1.68292(12) -0.21046(10) 0.31039(11) 0.0351(3) Uani 1 1 d . . . O10 O 1.57609(13) -0.29766(10) 0.18816(12) 0.0368(3) Uani 1 1 d . . . N1 N 1.11647(13) 0.18075(10) 0.19941(12) 0.0209(3) Uani 1 1 d . . . C1 C 1.17464(18) 0.46304(15) 0.07744(19) 0.0382(4) Uani 1 1 d . . . H1A H 1.1901 0.4461 -0.0024 0.046 Uiso 1 1 calc R . . C2 C 1.1459(2) 0.57570(16) 0.1106(2) 0.0509(6) Uani 1 1 d . . . H2A H 1.1416 0.6359 0.0534 0.061 Uiso 1 1 calc R . . C3 C 1.1238(2) 0.60067(16) 0.2257(2) 0.0499(6) Uani 1 1 d . . . H3A H 1.1060 0.6781 0.2475 0.060 Uiso 1 1 calc R . . C4 C 1.1271(2) 0.51327(16) 0.3101(2) 0.0456(5) Uani 1 1 d . . . H4A H 1.1098 0.5306 0.3904 0.055 Uiso 1 1 calc R . . C5 C 1.15570(19) 0.40064(15) 0.27778(18) 0.0360(4) Uani 1 1 d . . . H5A H 1.1582 0.3407 0.3358 0.043 Uiso 1 1 calc R . . C6 C 1.18074(16) 0.37486(13) 0.16102(16) 0.0272(4) Uani 1 1 d . . . C7 C 1.21667(16) 0.25315(13) 0.12348(15) 0.0243(3) Uani 1 1 d . . . H7A H 1.2349 0.2502 0.0358 0.029 Uiso 1 1 calc R . . C8 C 1.18099(15) 0.06577(12) 0.21950(14) 0.0214(3) Uani 1 1 d . . . C9 C 1.33072(15) 0.07900(13) 0.14153(14) 0.0229(3) Uani 1 1 d . . . H9A H 1.3561 0.0591 0.0559 0.027 Uiso 1 1 calc R . . C10 C 1.56595(16) -0.02176(14) 0.29331(15) 0.0266(4) Uani 1 1 d . . . C11 C 1.47906(16) 0.05106(13) 0.25237(15) 0.0257(3) Uani 1 1 d . . . H11A H 1.4557 0.1300 0.2697 0.031 Uiso 1 1 calc R . . C12 C 1.42722(15) 0.00633(13) 0.18593(14) 0.0233(3) Uani 1 1 d . . . C13 C 1.45795(16) -0.10927(13) 0.16169(15) 0.0267(4) Uani 1 1 d . . . H13A H 1.4216 -0.1382 0.1157 0.032 Uiso 1 1 calc R . . C14 C 1.54201(16) -0.18224(13) 0.20498(15) 0.0276(4) Uani 1 1 d . . . C15 C 1.59832(16) -0.13822(14) 0.26875(15) 0.0272(4) Uani 1 1 d . . . C16 C 0.83254(18) 0.42073(14) 0.26540(17) 0.0341(4) Uani 1 1 d . . . H16A H 0.8632 0.4396 0.1809 0.041 Uiso 1 1 calc R . . C17 C 0.74742(19) 0.50090(16) 0.34999(19) 0.0413(5) Uani 1 1 d . . . H17A H 0.7198 0.5753 0.3228 0.050 Uiso 1 1 calc R . . C18 C 0.70194(18) 0.47474(16) 0.47315(18) 0.0392(4) Uani 1 1 d . . . C19 C 0.74404(19) 0.36564(16) 0.51090(17) 0.0381(4) Uani 1 1 d . . . H19A H 0.7139 0.3469 0.5954 0.046 Uiso 1 1 calc R . . C20 C 0.82850(17) 0.28395(14) 0.42860(15) 0.0298(4) Uani 1 1 d . . . H20A H 0.8560 0.2095 0.4557 0.036 Uiso 1 1 calc R . . C21 C 0.87237(15) 0.31249(13) 0.30577(15) 0.0239(3) Uani 1 1 d . . . C22 C 0.6079(2) 0.5634(2) 0.5639(2) 0.0613(6) Uani 1 1 d . . . H22A H 0.5895 0.6344 0.5205 0.092 Uiso 1 1 calc R . . H22B H 0.6483 0.5780 0.6166 0.092 Uiso 1 1 calc R . . H22C H 0.5251 0.5351 0.6135 0.092 Uiso 1 1 calc R . . C23 C 1.15855(15) 0.04062(13) 0.35305(14) 0.0236(3) Uani 1 1 d . . . C24 C 1.1411(2) 0.12489(18) 0.52610(16) 0.0414(5) Uani 1 1 d . . . H24A H 1.1287 0.2008 0.5563 0.062 Uiso 1 1 calc R . . H24B H 1.2252 0.0800 0.5224 0.062 Uiso 1 1 calc R . . H24C H 1.0683 0.0859 0.5811 0.062 Uiso 1 1 calc R . . C25 C 1.15431(16) -0.02975(13) 0.16338(15) 0.0252(3) Uani 1 1 d . . . C26 C 1.1591(2) -0.08318(17) -0.01831(18) 0.0428(5) Uani 1 1 d . . . H26A H 1.1734 -0.0527 -0.1005 0.064 Uiso 1 1 calc R . . H26B H 1.0702 -0.1026 0.0230 0.064 Uiso 1 1 calc R . . H26C H 1.2250 -0.1519 -0.0231 0.064 Uiso 1 1 calc R . . C27 C 1.58765(19) 0.12695(15) 0.39420(18) 0.0381(4) Uani 1 1 d . . . H27A H 1.6371 0.1394 0.4396 0.057 Uiso 1 1 calc R . . H27B H 1.4926 0.1426 0.4461 0.057 Uiso 1 1 calc R . . H27D H 1.6076 0.1784 0.3221 0.057 Uiso 1 1 calc R . . C28 C 1.81904(18) -0.21017(19) 0.23115(18) 0.0462(5) Uani 1 1 d . . . H28A H 1.8751 -0.2627 0.2646 0.069 Uiso 1 1 calc R . . H28D H 1.8383 -0.1327 0.2238 0.069 Uiso 1 1 calc R . . H28B H 1.8369 -0.2349 0.1508 0.069 Uiso 1 1 calc R . . C29 C 1.5057(2) -0.34651(15) 0.13787(18) 0.0405(5) Uani 1 1 d . . . H29D H 1.5385 -0.4290 0.1300 0.061 Uiso 1 1 calc R . . H29A H 1.5193 -0.3109 0.0576 0.061 Uiso 1 1 calc R . . H29B H 1.4111 -0.3331 0.1916 0.061 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 0.0250(2) 0.0220(2) 0.0247(2) -0.00019(15) -0.01482(17) -0.00348(15) O1 0.0243(6) 0.0194(5) 0.0323(6) 0.0048(4) -0.0148(5) -0.0042(4) O2 0.0358(7) 0.0363(7) 0.0282(6) 0.0016(5) -0.0209(5) -0.0032(5) O3 0.0285(6) 0.0249(6) 0.0365(7) -0.0020(5) -0.0153(5) -0.0072(5) O4 0.0451(7) 0.0289(6) 0.0237(6) 0.0012(5) -0.0188(5) -0.0073(5) O5 0.0683(10) 0.0276(7) 0.0342(7) 0.0122(5) -0.0254(7) -0.0096(6) O6 0.0418(7) 0.0287(6) 0.0281(6) -0.0038(5) -0.0173(5) -0.0098(5) O7 0.0549(8) 0.0214(6) 0.0449(8) 0.0034(5) -0.0231(7) -0.0135(6) O8 0.0326(7) 0.0330(7) 0.0447(7) -0.0042(5) -0.0242(6) -0.0002(5) O9 0.0307(7) 0.0331(7) 0.0377(7) 0.0036(5) -0.0168(6) 0.0055(5) O10 0.0436(7) 0.0209(6) 0.0449(7) -0.0037(5) -0.0206(6) 0.0030(5) N1 0.0236(7) 0.0161(6) 0.0252(7) 0.0032(5) -0.0126(6) -0.0045(5) C1 0.0362(10) 0.0277(9) 0.0497(11) 0.0133(8) -0.0206(9) -0.0054(8) C2 0.0454(12) 0.0257(10) 0.0789(16) 0.0190(10) -0.0288(12) -0.0054(8) C3 0.0396(11) 0.0199(9) 0.0942(18) -0.0034(10) -0.0319(12) -0.0035(8) C4 0.0493(12) 0.0303(10) 0.0675(14) -0.0101(9) -0.0324(11) -0.0055(9) C5 0.0453(11) 0.0237(9) 0.0480(11) 0.0023(8) -0.0280(9) -0.0075(8) C6 0.0233(8) 0.0204(8) 0.0403(10) 0.0064(7) -0.0162(7) -0.0066(6) C7 0.0254(8) 0.0227(8) 0.0273(8) 0.0063(6) -0.0144(7) -0.0057(6) C8 0.0248(8) 0.0166(7) 0.0237(8) 0.0027(6) -0.0120(7) -0.0028(6) C9 0.0251(8) 0.0197(7) 0.0228(8) 0.0015(6) -0.0094(7) -0.0042(6) C10 0.0223(8) 0.0293(9) 0.0272(8) 0.0015(7) -0.0099(7) -0.0044(7) C11 0.0234(8) 0.0215(8) 0.0298(8) 0.0005(6) -0.0098(7) -0.0026(6) C12 0.0203(8) 0.0230(8) 0.0231(8) 0.0015(6) -0.0068(7) -0.0022(6) C13 0.0270(9) 0.0257(8) 0.0257(8) -0.0021(7) -0.0099(7) -0.0028(7) C14 0.0279(9) 0.0206(8) 0.0268(8) -0.0003(6) -0.0064(7) 0.0005(6) C15 0.0232(8) 0.0260(8) 0.0277(8) 0.0036(7) -0.0096(7) 0.0014(6) C16 0.0353(10) 0.0270(9) 0.0375(10) 0.0041(7) -0.0162(8) -0.0001(7) C17 0.0404(11) 0.0253(9) 0.0566(13) -0.0008(8) -0.0230(10) 0.0042(8) C18 0.0327(10) 0.0354(10) 0.0498(12) -0.0138(9) -0.0173(9) 0.0009(8) C19 0.0402(11) 0.0398(10) 0.0319(9) -0.0051(8) -0.0129(8) -0.0044(8) C20 0.0350(10) 0.0255(8) 0.0311(9) 0.0015(7) -0.0165(8) -0.0047(7) C21 0.0235(8) 0.0221(8) 0.0287(8) -0.0002(6) -0.0135(7) -0.0038(6) C22 0.0544(14) 0.0533(14) 0.0691(16) -0.0282(12) -0.0224(12) 0.0135(11) C23 0.0208(8) 0.0240(8) 0.0246(8) 0.0029(6) -0.0091(7) -0.0036(6) C24 0.0547(12) 0.0523(12) 0.0240(9) 0.0012(8) -0.0206(9) -0.0153(10) C25 0.0245(8) 0.0205(8) 0.0303(9) -0.0021(7) -0.0117(7) -0.0019(6) C26 0.0519(12) 0.0427(11) 0.0421(11) -0.0151(9) -0.0227(10) -0.0107(9) C27 0.0382(10) 0.0363(10) 0.0462(11) -0.0076(8) -0.0224(9) -0.0055(8) C28 0.0293(10) 0.0636(14) 0.0397(11) -0.0053(10) -0.0159(9) 0.0104(9) C29 0.0462(11) 0.0257(9) 0.0453(11) -0.0040(8) -0.0139(9) -0.0068(8) _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 1.4300(12) . ? S1 O3 1.4300(12) . ? S1 N1 1.6363(13) . ? S1 C21 1.7581(16) . ? O1 C7 1.4178(18) . ? O1 C9 1.4181(18) . ? O4 C23 1.3233(19) . ? O4 C24 1.450(2) . ? O5 C23 1.1908(19) . ? O6 C25 1.338(2) . ? O6 C26 1.445(2) . ? O7 C25 1.1918(19) . ? O8 C10 1.358(2) . ? O8 C27 1.427(2) . ? O9 C15 1.3766(19) . ? O9 C28 1.430(2) . ? O10 C14 1.3694(19) . ? O10 C29 1.430(2) . ? N1 C8 1.4646(18) . ? N1 C7 1.488(2) . ? C1 C2 1.385(3) . ? C1 C6 1.389(2) . ? C1 H1A 0.9500 . ? C2 C3 1.372(3) . ? C2 H2A 0.9500 . ? C3 C4 1.383(3) . ? C3 H3A 0.9500 . ? C4 C5 1.382(2) . ? C4 H4A 0.9500 . ? C5 C6 1.385(3) . ? C5 H5A 0.9500 . ? C6 C7 1.499(2) . ? C7 H7A 1.0000 . ? C8 C23 1.536(2) . ? C8 C25 1.538(2) . ? C8 C9 1.585(2) . ? C9 C12 1.499(2) . ? C9 H9A 1.0000 . ? C10 C11 1.394(2) . ? C10 C15 1.399(2) . ? C11 C12 1.387(2) . ? C11 H11A 0.9500 . ? C12 C13 1.389(2) . ? C13 C14 1.388(2) . ? C13 H13A 0.9500 . ? C14 C15 1.395(2) . ? C16 C17 1.384(3) . ? C16 C21 1.385(2) . ? C16 H16A 0.9500 . ? C17 C18 1.381(3) . ? C17 H17A 0.9500 . ? C18 C19 1.389(3) . ? C18 C22 1.512(3) . ? C19 C20 1.379(2) . ? C19 H19A 0.9500 . ? C20 C21 1.383(2) . ? C20 H20A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27D 0.9800 . ? C28 H28A 0.9800 . ? C28 H28D 0.9800 . ? C28 H28B 0.9800 . ? C29 H29D 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 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 O2 S1 O3 120.39(7) . . ? O2 S1 N1 108.56(7) . . ? O3 S1 N1 105.19(6) . . ? O2 S1 C21 107.12(7) . . ? O3 S1 C21 107.87(7) . . ? N1 S1 C21 107.06(7) . . ? C7 O1 C9 105.34(11) . . ? C23 O4 C24 116.26(13) . . ? C25 O6 C26 115.11(14) . . ? C10 O8 C27 117.69(13) . . ? C15 O9 C28 112.54(13) . . ? C14 O10 C29 116.85(14) . . ? C8 N1 C7 110.68(12) . . ? C8 N1 S1 122.53(10) . . ? C7 N1 S1 120.61(10) . . ? C2 C1 C6 119.9(2) . . ? C2 C1 H1A 120.0 . . ? C6 C1 H1A 120.0 . . ? C3 C2 C1 120.32(19) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 120.05(18) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0(2) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.22(18) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 119.46(16) . . ? C5 C6 C7 120.73(15) . . ? C1 C6 C7 119.79(16) . . ? O1 C7 N1 101.87(11) . . ? O1 C7 C6 109.91(13) . . ? N1 C7 C6 114.12(13) . . ? O1 C7 H7A 110.2 . . ? N1 C7 H7A 110.2 . . ? C6 C7 H7A 110.2 . . ? N1 C8 C23 112.47(12) . . ? N1 C8 C25 114.33(12) . . ? C23 C8 C25 113.49(13) . . ? N1 C8 C9 99.35(11) . . ? C23 C8 C9 108.96(12) . . ? C25 C8 C9 107.01(12) . . ? O1 C9 C12 112.67(13) . . ? O1 C9 C8 103.67(11) . . ? C12 C9 C8 114.83(12) . . ? O1 C9 H9A 108.5 . . ? C12 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? O8 C10 C11 124.86(15) . . ? O8 C10 C15 115.01(14) . . ? C11 C10 C15 120.13(15) . . ? C12 C11 C10 118.90(15) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C13 121.48(14) . . ? C11 C12 C9 121.81(14) . . ? C13 C12 C9 116.66(14) . . ? C14 C13 C12 119.60(15) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? O10 C14 C13 124.04(15) . . ? O10 C14 C15 116.23(14) . . ? C13 C14 C15 119.73(14) . . ? O9 C15 C14 119.68(14) . . ? O9 C15 C10 120.17(15) . . ? C14 C15 C10 120.12(14) . . ? C17 C16 C21 119.04(17) . . ? C17 C16 H16A 120.5 . . ? C21 C16 H16A 120.5 . . ? C18 C17 C16 121.18(17) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 118.47(17) . . ? C17 C18 C22 120.27(19) . . ? C19 C18 C22 121.27(19) . . ? C20 C19 C18 121.58(18) . . ? C20 C19 H19A 119.2 . . ? C18 C19 H19A 119.2 . . ? C19 C20 C21 118.71(16) . . ? C19 C20 H20A 120.6 . . ? C21 C20 H20A 120.6 . . ? C20 C21 C16 121.02(15) . . ? C20 C21 S1 119.24(12) . . ? C16 C21 S1 119.53(13) . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 O4 124.89(15) . . ? O5 C23 C8 124.93(15) . . ? O4 C23 C8 109.93(12) . . ? O4 C24 H24A 109.5 . . ? O4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 O6 124.19(15) . . ? O7 C25 C8 126.73(15) . . ? O6 C25 C8 108.87(13) . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C27 H27A 109.5 . . ? O8 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O8 C27 H27D 109.5 . . ? H27A C27 H27D 109.5 . . ? H27B C27 H27D 109.5 . . ? O9 C28 H28A 109.5 . . ? O9 C28 H28D 109.5 . . ? H28A C28 H28D 109.5 . . ? O9 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? H28D C28 H28B 109.5 . . ? O10 C29 H29D 109.5 . . ? O10 C29 H29A 109.5 . . ? H29D C29 H29A 109.5 . . ? O10 C29 H29B 109.5 . . ? H29D C29 H29B 109.5 . . ? H29A C29 H29B 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 C8 -118.98(12) . . . . ? O3 S1 N1 C8 11.12(13) . . . . ? C21 S1 N1 C8 125.69(12) . . . . ? O2 S1 N1 C7 30.79(13) . . . . ? O3 S1 N1 C7 160.89(11) . . . . ? C21 S1 N1 C7 -84.54(13) . . . . ? C6 C1 C2 C3 0.1(3) . . . . ? C1 C2 C3 C4 -1.4(3) . . . . ? C2 C3 C4 C5 1.4(3) . . . . ? C3 C4 C5 C6 -0.1(3) . . . . ? C4 C5 C6 C1 -1.1(3) . . . . ? C4 C5 C6 C7 177.76(17) . . . . ? C2 C1 C6 C5 1.1(3) . . . . ? C2 C1 C6 C7 -177.77(17) . . . . ? C9 O1 C7 N1 41.43(14) . . . . ? C9 O1 C7 C6 162.78(13) . . . . ? C8 N1 C7 O1 -23.17(15) . . . . ? S1 N1 C7 O1 -176.19(9) . . . . ? C8 N1 C7 C6 -141.56(13) . . . . ? S1 N1 C7 C6 65.43(16) . . . . ? C5 C6 C7 O1 -56.1(2) . . . . ? C1 C6 C7 O1 122.81(16) . . . . ? C5 C6 C7 N1 57.6(2) . . . . ? C1 C6 C7 N1 -123.50(16) . . . . ? C7 N1 C8 C23 112.97(14) . . . . ? S1 N1 C8 C23 -94.62(14) . . . . ? C7 N1 C8 C25 -115.71(14) . . . . ? S1 N1 C8 C25 36.70(17) . . . . ? C7 N1 C8 C9 -2.14(15) . . . . ? S1 N1 C8 C9 150.26(10) . . . . ? C7 O1 C9 C12 -168.55(12) . . . . ? C7 O1 C9 C8 -43.81(14) . . . . ? N1 C8 C9 O1 26.96(14) . . . . ? C23 C8 C9 O1 -90.82(13) . . . . ? C25 C8 C9 O1 146.11(12) . . . . ? N1 C8 C9 C12 150.29(13) . . . . ? C23 C8 C9 C12 32.51(17) . . . . ? C25 C8 C9 C12 -90.56(15) . . . . ? C27 O8 C10 C11 5.0(2) . . . . ? C27 O8 C10 C15 -175.00(15) . . . . ? O8 C10 C11 C12 179.11(15) . . . . ? C15 C10 C11 C12 -0.9(2) . . . . ? C10 C11 C12 C13 1.3(2) . . . . ? C10 C11 C12 C9 178.52(14) . . . . ? O1 C9 C12 C11 16.8(2) . . . . ? C8 C9 C12 C11 -101.55(17) . . . . ? O1 C9 C12 C13 -165.82(13) . . . . ? C8 C9 C12 C13 75.80(17) . . . . ? C11 C12 C13 C14 0.2(2) . . . . ? C9 C12 C13 C14 -177.13(14) . . . . ? C29 O10 C14 C13 -9.0(2) . . . . ? C29 O10 C14 C15 171.70(15) . . . . ? C12 C13 C14 O10 178.58(15) . . . . ? C12 C13 C14 C15 -2.2(2) . . . . ? C28 O9 C15 C14 97.82(19) . . . . ? C28 O9 C15 C10 -84.02(19) . . . . ? O10 C14 C15 O9 0.1(2) . . . . ? C13 C14 C15 O9 -179.23(15) . . . . ? O10 C14 C15 C10 -178.09(15) . . . . ? C13 C14 C15 C10 2.6(2) . . . . ? O8 C10 C15 O9 0.8(2) . . . . ? C11 C10 C15 O9 -179.23(15) . . . . ? O8 C10 C15 C14 178.94(15) . . . . ? C11 C10 C15 C14 -1.1(2) . . . . ? C21 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C16 C17 C18 C22 -179.4(2) . . . . ? C17 C18 C19 C20 -0.5(3) . . . . ? C22 C18 C19 C20 179.21(19) . . . . ? C18 C19 C20 C21 0.4(3) . . . . ? C19 C20 C21 C16 -0.1(3) . . . . ? C19 C20 C21 S1 -174.84(14) . . . . ? C17 C16 C21 C20 -0.1(3) . . . . ? C17 C16 C21 S1 174.63(14) . . . . ? O2 S1 C21 C20 169.64(13) . . . . ? O3 S1 C21 C20 38.69(15) . . . . ? N1 S1 C21 C20 -74.08(14) . . . . ? O2 S1 C21 C16 -5.16(16) . . . . ? O3 S1 C21 C16 -136.11(14) . . . . ? N1 S1 C21 C16 111.13(14) . . . . ? C24 O4 C23 O5 3.9(2) . . . . ? C24 O4 C23 C8 -170.64(14) . . . . ? N1 C8 C23 O5 156.62(16) . . . . ? C25 C8 C23 O5 24.9(2) . . . . ? C9 C8 C23 O5 -94.23(19) . . . . ? N1 C8 C23 O4 -28.84(17) . . . . ? C25 C8 C23 O4 -160.59(13) . . . . ? C9 C8 C23 O4 80.31(15) . . . . ? C26 O6 C25 O7 0.8(2) . . . . ? C26 O6 C25 C8 175.91(14) . . . . ? N1 C8 C25 O7 -138.03(17) . . . . ? C23 C8 C25 O7 -7.2(2) . . . . ? C9 C8 C25 O7 113.02(18) . . . . ? N1 C8 C25 O6 46.98(17) . . . . ? C23 C8 C25 O6 177.81(12) . . . . ? C9 C8 C25 O6 -61.97(15) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.404 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.041