# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Donald Craig' _publ_contact_author_email D.CRAIG@IMPERIAL.AC.UK _publ_section_title ; Highly regioselective ring-opening of trisubstituted aziridines by sulfur-stabilised carbanions ; loop_ _publ_author_name 'Donald Craig' 'Santiago Carballares' 'Christopher Hyland' 'Pengfei Lu.' 'Tanya Mathie' 'Andrew J. P. White' # Attachment 'D_Craig_combined_CIF.cif' data_Compound_5c _database_code_depnum_ccdc_archive 'CCDC 698819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H35 N O5 S2' _chemical_formula_sum 'C34 H35 N O5 S2' _chemical_formula_weight 601.75 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.4954(2) _cell_length_b 13.9284(3) _cell_length_c 26.6078(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6113.26(19) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27281 _cell_measurement_theta_min 3.7013 _cell_measurement_theta_max 28.3807 _exptl_crystal_description tablets _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82041 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57080 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 28.43 _reflns_number_total 7155 _reflns_number_gt 5780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0179P)^2^+12.2429P] 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 7155 _refine_ls_number_parameters 394 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.233 _refine_ls_restrained_S_all 1.234 _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 C1 C 0.1271(9) 0.7795(8) 0.3905(3) 0.052(3) Uani 0.79(4) 1 d PDU A 1 H1A H 0.1724 0.8208 0.3947 0.063 Uiso 0.79(4) 1 calc PR A 1 H1B H 0.0796 0.8023 0.3742 0.063 Uiso 0.79(4) 1 calc PR A 1 C2 C 0.1302(4) 0.6899(7) 0.4072(3) 0.0387(14) Uani 0.79(4) 1 d PDU A 1 H2A H 0.0843 0.6499 0.4026 0.046 Uiso 0.79(4) 1 calc PR A 1 C1' C 0.1020(17) 0.751(2) 0.3859(9) 0.048(6) Uiso 0.21(4) 1 d PDU A 2 H1'A H 0.1360 0.8064 0.3882 0.058 Uiso 0.21(4) 1 calc PR A 2 H1'B H 0.0511 0.7559 0.3693 0.058 Uiso 0.21(4) 1 calc PR A 2 C2' C 0.1255(13) 0.669(2) 0.4058(16) 0.039(4) Uiso 0.21(4) 1 d PDU A 2 H2'A H 0.0891 0.6165 0.4024 0.047 Uiso 0.21(4) 1 calc PR A 2 C3 C 0.20324(17) 0.6492(2) 0.43317(11) 0.0272(6) Uani 1 1 d D . . H3A H 0.2448 0.7014 0.4340 0.033 Uiso 0.79(4) 1 calc PR A 1 H3B H 0.2396 0.7029 0.4324 0.033 Uiso 0.21(4) 1 d PR A 2 C4 C 0.18365(16) 0.62429(19) 0.48845(11) 0.0240(5) Uani 1 1 d . A . H4A H 0.2331 0.5965 0.5046 0.029 Uiso 1 1 calc R . . C5 C 0.15933(18) 0.7147(2) 0.51660(11) 0.0301(6) Uani 1 1 d . . . H5A H 0.1998 0.7652 0.5089 0.036 Uiso 1 1 calc R A . H5B H 0.1066 0.7367 0.5030 0.036 Uiso 1 1 calc R . . C6 C 0.24206(16) 0.5639(2) 0.40412(11) 0.0264(6) Uani 1 1 d . A . H6A H 0.2329 0.5041 0.4241 0.032 Uiso 1 1 calc R . . S7 S 0.35068(4) 0.58182(6) 0.39828(3) 0.03024(17) Uani 1 1 d . . . O8 O 0.38425(14) 0.49964(18) 0.37367(9) 0.0432(6) Uani 1 1 d . A . O9 O 0.36531(14) 0.67503(17) 0.37691(9) 0.0399(5) Uani 1 1 d . A . C10 C 0.38306(16) 0.5822(2) 0.46141(11) 0.0281(6) Uani 1 1 d . A . C11 C 0.40234(17) 0.6678(2) 0.48502(12) 0.0315(6) Uani 1 1 d . . . H11A H 0.3996 0.7267 0.4671 0.038 Uiso 1 1 calc R A . C12 C 0.42560(19) 0.6665(2) 0.53498(13) 0.0385(7) Uani 1 1 d . A . H12A H 0.4397 0.7246 0.5515 0.046 Uiso 1 1 calc R . . C13 C 0.4282(2) 0.5805(3) 0.56072(13) 0.0414(8) Uani 1 1 d . . . H13A H 0.4439 0.5799 0.5951 0.050 Uiso 1 1 calc R A . C14 C 0.40815(18) 0.4949(2) 0.53711(13) 0.0380(7) Uani 1 1 d . A . H14A H 0.4094 0.4363 0.5554 0.046 Uiso 1 1 calc R . . C15 C 0.38644(17) 0.4951(2) 0.48702(12) 0.0318(6) Uani 1 1 d . . . H15A H 0.3740 0.4367 0.4703 0.038 Uiso 1 1 calc R A . C16 C 0.20867(18) 0.5480(2) 0.35269(11) 0.0325(6) Uani 1 1 d . . . H16A H 0.2133 0.5982 0.3287 0.039 Uiso 1 1 calc R A . C17 C 0.17268(18) 0.4667(2) 0.33898(12) 0.0321(7) Uani 1 1 d . A . H17A H 0.1742 0.4153 0.3624 0.039 Uiso 1 1 calc R . . C18 C 0.13076(19) 0.4483(2) 0.29126(12) 0.0359(7) Uani 1 1 d . . . C19 C 0.0980(2) 0.3570(3) 0.28294(14) 0.0454(8) Uani 1 1 d . A . H19A H 0.1067 0.3074 0.3068 0.054 Uiso 1 1 calc R . . C20 C 0.0529(2) 0.3384(3) 0.24000(15) 0.0563(11) Uani 1 1 d . . . H20A H 0.0314 0.2761 0.2343 0.068 Uiso 1 1 calc R A . C21 C 0.0394(3) 0.4111(4) 0.20532(15) 0.0662(13) Uani 1 1 d . A . H21A H 0.0065 0.3994 0.1766 0.079 Uiso 1 1 calc R . . C22 C 0.0733(3) 0.4994(4) 0.21252(15) 0.0643(12) Uani 1 1 d . . . H22A H 0.0665 0.5477 0.1877 0.077 Uiso 1 1 calc R A . C23 C 0.1172(2) 0.5195(3) 0.25517(14) 0.0499(9) Uani 1 1 d . A . H23A H 0.1384 0.5822 0.2602 0.060 Uiso 1 1 calc R . . C24 C 0.15158(17) 0.70767(19) 0.57314(11) 0.0263(6) Uani 1 1 d . A . C25 C 0.21496(17) 0.6762(2) 0.60301(12) 0.0319(6) Uani 1 1 d . . . H25A H 0.2626 0.6523 0.5873 0.038 Uiso 1 1 calc R A . C26 C 0.21124(19) 0.6782(2) 0.65502(12) 0.0349(7) Uani 1 1 d . A . H26A H 0.2553 0.6550 0.6746 0.042 Uiso 1 1 calc R . . C27 C 0.1422(2) 0.7145(2) 0.67821(12) 0.0355(7) Uani 1 1 d . . . C28 C 0.07715(19) 0.7443(2) 0.64891(13) 0.0376(7) Uani 1 1 d . A . H28A H 0.0291 0.7672 0.6645 0.045 Uiso 1 1 calc R . . C29 C 0.08205(17) 0.7406(2) 0.59726(12) 0.0316(6) Uani 1 1 d . . . H29A H 0.0370 0.7610 0.5777 0.038 Uiso 1 1 calc R A . O30 O 0.13344(17) 0.7253(2) 0.72901(9) 0.0562(7) Uani 1 1 d . A . C31 C 0.2006(3) 0.6987(4) 0.75983(15) 0.0667(13) Uani 1 1 d . . . H31A H 0.2485 0.7356 0.7498 0.100 Uiso 1 1 calc R A . H31B H 0.2115 0.6300 0.7557 0.100 Uiso 1 1 calc R . . H31C H 0.1878 0.7122 0.7951 0.100 Uiso 1 1 calc R . . N32 N 0.11774(13) 0.55267(16) 0.49040(9) 0.0234(5) Uani 1 1 d D . . H32 H 0.0674(8) 0.578(2) 0.4914(12) 0.033(9) Uiso 1 1 d D . . S33 S 0.12735(4) 0.44469(5) 0.51146(3) 0.02437(15) Uani 1 1 d . A . O34 O 0.05235(11) 0.39787(14) 0.49843(8) 0.0304(5) Uani 1 1 d . . . O35 O 0.20203(12) 0.40591(14) 0.49263(8) 0.0317(5) Uani 1 1 d . . . C36 C 0.13349(17) 0.44605(19) 0.57723(11) 0.0261(6) Uani 1 1 d . . . C37 C 0.20280(19) 0.4128(2) 0.60143(13) 0.0378(7) Uani 1 1 d . A . H37A H 0.2483 0.3920 0.5825 0.045 Uiso 1 1 calc R . . C38 C 0.2047(2) 0.4105(3) 0.65330(14) 0.0473(9) Uani 1 1 d . . . H38A H 0.2518 0.3871 0.6698 0.057 Uiso 1 1 calc R A . C39 C 0.1401(2) 0.4411(2) 0.68164(13) 0.0442(8) Uani 1 1 d . A . C40 C 0.0717(2) 0.4765(3) 0.65706(13) 0.0408(8) Uani 1 1 d . . . H40A H 0.0270 0.4986 0.6763 0.049 Uiso 1 1 calc R A . C41 C 0.06791(18) 0.4802(2) 0.60528(12) 0.0343(7) Uani 1 1 d . A . H41A H 0.0214 0.5056 0.5889 0.041 Uiso 1 1 calc R . . C42 C 0.1427(3) 0.4369(3) 0.73840(15) 0.0666(12) Uani 1 1 d . . . H42A H 0.1992 0.4384 0.7497 0.100 Uiso 1 1 calc R A . H42B H 0.1169 0.3774 0.7499 0.100 Uiso 1 1 calc R . . H42C H 0.1135 0.4922 0.7523 0.100 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 C1 0.073(5) 0.041(4) 0.043(3) 0.010(2) 0.011(3) 0.029(4) C2 0.044(3) 0.039(3) 0.033(2) 0.011(3) 0.0056(19) 0.021(2) C3 0.0274(14) 0.0207(13) 0.0336(15) 0.0015(11) 0.0048(12) 0.0017(11) C4 0.0208(12) 0.0215(13) 0.0296(14) 0.0003(11) 0.0007(11) -0.0015(10) C5 0.0318(15) 0.0225(14) 0.0361(16) -0.0010(12) 0.0025(13) 0.0000(12) C6 0.0256(13) 0.0253(14) 0.0282(14) 0.0002(11) 0.0028(11) 0.0000(11) S7 0.0269(3) 0.0321(4) 0.0317(4) 0.0004(3) 0.0066(3) 0.0005(3) O8 0.0385(12) 0.0478(14) 0.0432(13) -0.0114(11) 0.0107(10) 0.0099(11) O9 0.0377(12) 0.0417(13) 0.0403(13) 0.0121(10) 0.0074(10) -0.0068(10) C10 0.0193(12) 0.0307(15) 0.0344(15) 0.0013(12) 0.0041(11) 0.0002(11) C11 0.0241(14) 0.0278(15) 0.0426(17) 0.0026(13) 0.0037(13) -0.0010(11) C12 0.0321(16) 0.0378(18) 0.0455(19) -0.0057(15) -0.0053(14) -0.0025(14) C13 0.0322(16) 0.054(2) 0.0381(18) 0.0031(16) -0.0054(14) 0.0046(15) C14 0.0276(15) 0.0393(18) 0.0471(19) 0.0126(15) 0.0003(14) 0.0030(13) C15 0.0221(14) 0.0266(14) 0.0466(18) 0.0033(13) 0.0027(13) -0.0015(11) C16 0.0329(15) 0.0346(16) 0.0299(15) 0.0024(13) 0.0009(12) -0.0011(13) C17 0.0315(15) 0.0318(16) 0.0331(16) 0.0035(13) -0.0012(12) -0.0033(12) C18 0.0321(16) 0.0421(18) 0.0334(16) 0.0016(14) -0.0007(13) -0.0064(14) C19 0.0428(19) 0.049(2) 0.045(2) -0.0006(16) -0.0020(16) -0.0114(16) C20 0.057(2) 0.065(3) 0.047(2) -0.0032(19) -0.0075(18) -0.026(2) C21 0.063(3) 0.098(4) 0.038(2) 0.004(2) -0.0137(19) -0.031(3) C22 0.063(3) 0.087(3) 0.043(2) 0.020(2) -0.0163(19) -0.022(2) C23 0.054(2) 0.054(2) 0.042(2) 0.0081(17) -0.0062(17) -0.0151(18) C24 0.0262(13) 0.0176(12) 0.0350(15) -0.0038(11) 0.0017(12) -0.0048(11) C25 0.0235(13) 0.0323(15) 0.0398(17) -0.0079(13) 0.0021(12) 0.0010(12) C26 0.0301(15) 0.0353(17) 0.0393(18) -0.0040(14) -0.0039(13) 0.0024(13) C27 0.0385(17) 0.0334(16) 0.0346(16) -0.0025(13) 0.0062(13) 0.0006(14) C28 0.0309(15) 0.0340(17) 0.0479(19) -0.0007(14) 0.0118(14) 0.0041(14) C29 0.0249(14) 0.0262(15) 0.0438(18) 0.0018(13) 0.0017(13) 0.0007(11) O30 0.0594(17) 0.073(2) 0.0364(13) -0.0032(13) 0.0066(12) 0.0138(15) C31 0.082(3) 0.080(3) 0.038(2) -0.005(2) -0.009(2) 0.016(3) N32 0.0182(10) 0.0198(11) 0.0323(12) 0.0028(10) -0.0001(9) 0.0002(9) S33 0.0199(3) 0.0192(3) 0.0340(4) 0.0011(3) 0.0019(3) 0.0007(2) O34 0.0226(9) 0.0229(10) 0.0457(12) -0.0024(9) 0.0002(9) -0.0029(8) O35 0.0241(10) 0.0271(10) 0.0439(12) 0.0024(9) 0.0065(9) 0.0049(8) C36 0.0244(13) 0.0178(12) 0.0360(15) 0.0055(11) 0.0011(11) 0.0012(11) C37 0.0334(16) 0.0346(17) 0.0453(18) 0.0000(15) -0.0015(14) 0.0128(13) C38 0.054(2) 0.0405(19) 0.048(2) 0.0024(16) -0.0145(17) 0.0152(17) C39 0.059(2) 0.0353(18) 0.0379(18) 0.0037(14) -0.0050(16) -0.0007(17) C40 0.0417(18) 0.0425(19) 0.0381(18) 0.0007(15) 0.0092(15) -0.0021(15) C41 0.0245(14) 0.0346(16) 0.0438(18) 0.0023(14) 0.0034(13) 0.0002(12) C42 0.090(3) 0.066(3) 0.044(2) 0.005(2) -0.006(2) 0.005(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 C1 C2 1.325(6) . ? C2 C3 1.500(4) . ? C1' C2' 1.324(8) . ? C2' C3 1.500(6) . ? C3 C4 1.545(4) . ? C3 C6 1.555(4) . ? C4 N32 1.476(3) . ? C4 C5 1.519(4) . ? C5 C24 1.513(4) . ? C6 C16 1.491(4) . ? C6 S7 1.816(3) . ? S7 O8 1.430(2) . ? S7 O9 1.438(2) . ? S7 C10 1.763(3) . ? C10 C11 1.385(4) . ? C10 C15 1.392(4) . ? C11 C12 1.384(5) . ? C12 C13 1.380(5) . ? C13 C14 1.387(5) . ? C14 C15 1.380(5) . ? C16 C17 1.330(4) . ? C17 C18 1.468(4) . ? C18 C23 1.399(5) . ? C18 C19 1.399(5) . ? C19 C20 1.387(5) . ? C20 C21 1.388(6) . ? C21 C22 1.365(6) . ? C22 C23 1.375(5) . ? C24 C25 1.385(4) . ? C24 C29 1.392(4) . ? C25 C26 1.386(4) . ? C26 C27 1.390(4) . ? C27 O30 1.368(4) . ? C27 C28 1.390(5) . ? C28 C29 1.378(5) . ? O30 C31 1.427(5) . ? N32 S33 1.613(2) . ? S33 O35 1.435(2) . ? S33 O34 1.441(2) . ? S33 C36 1.753(3) . ? C36 C37 1.391(4) . ? C36 C41 1.398(4) . ? C37 C38 1.381(5) . ? C38 C39 1.373(5) . ? C39 C40 1.394(5) . ? C39 C42 1.512(5) . ? C40 C41 1.380(5) . ? 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 C1 C2 C3 122.8(6) . . ? C1' C2' C3 127.1(15) . . ? C2 C3 C4 110.8(4) . . ? C2' C3 C4 108.9(17) . . ? C2 C3 C6 113.0(5) . . ? C2' C3 C6 104.5(17) . . ? C4 C3 C6 112.8(2) . . ? N32 C4 C5 110.4(2) . . ? N32 C4 C3 109.8(2) . . ? C5 C4 C3 109.8(2) . . ? C24 C5 C4 117.3(2) . . ? C16 C6 C3 114.6(2) . . ? C16 C6 S7 107.83(19) . . ? C3 C6 S7 110.11(19) . . ? O8 S7 O9 118.47(14) . . ? O8 S7 C10 108.73(14) . . ? O9 S7 C10 108.88(14) . . ? O8 S7 C6 108.12(14) . . ? O9 S7 C6 108.89(14) . . ? C10 S7 C6 102.58(13) . . ? C11 C10 C15 121.3(3) . . ? C11 C10 S7 120.3(2) . . ? C15 C10 S7 118.4(2) . . ? C12 C11 C10 119.2(3) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C14 120.9(3) . . ? C15 C14 C13 119.8(3) . . ? C14 C15 C10 119.0(3) . . ? C17 C16 C6 122.8(3) . . ? C16 C17 C18 126.6(3) . . ? C23 C18 C19 118.3(3) . . ? C23 C18 C17 123.1(3) . . ? C19 C18 C17 118.5(3) . . ? C20 C19 C18 120.4(4) . . ? C19 C20 C21 119.9(4) . . ? C22 C21 C20 119.8(4) . . ? C21 C22 C23 121.0(4) . . ? C22 C23 C18 120.5(4) . . ? C25 C24 C29 117.5(3) . . ? C25 C24 C5 121.8(3) . . ? C29 C24 C5 120.4(3) . . ? C24 C25 C26 122.2(3) . . ? C25 C26 C27 119.1(3) . . ? O30 C27 C28 116.1(3) . . ? O30 C27 C26 124.4(3) . . ? C28 C27 C26 119.5(3) . . ? C29 C28 C27 120.2(3) . . ? C28 C29 C24 121.4(3) . . ? C27 O30 C31 117.2(3) . . ? C4 N32 S33 124.74(18) . . ? O35 S33 O34 118.86(12) . . ? O35 S33 N32 108.31(12) . . ? O34 S33 N32 104.72(12) . . ? O35 S33 C36 107.63(13) . . ? O34 S33 C36 107.14(13) . . ? N32 S33 C36 110.02(13) . . ? C37 C36 C41 120.1(3) . . ? C37 C36 S33 120.4(2) . . ? C41 C36 S33 119.5(2) . . ? C38 C37 C36 119.3(3) . . ? C39 C38 C37 121.6(3) . . ? C38 C39 C40 118.7(3) . . ? C38 C39 C42 121.0(4) . . ? C40 C39 C42 120.3(4) . . ? C41 C40 C39 121.2(3) . . ? C40 C41 C36 119.0(3) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.713 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.063 #===END data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 698820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H33 N O3 S2' _chemical_formula_sum 'C29 H33 N O3 S2' _chemical_formula_weight 507.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.6552(2) _cell_length_b 12.3842(2) _cell_length_c 28.0436(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5437.01(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4261 _cell_measurement_theta_min 3.1491 _cell_measurement_theta_max 52.1864 _exptl_crystal_description needles _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 2.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.61918 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10559 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 52.24 _reflns_number_total 3002 _reflns_number_gt 1958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0427P)^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 3002 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _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 C1 C 0.7314(2) 0.4958(3) 0.55809(13) 0.0713(11) Uani 1 1 d . . . H1A H 0.7659 0.5427 0.5767 0.086 Uiso 1 1 calc R . . H1B H 0.7162 0.5153 0.5264 0.086 Uiso 1 1 calc R . . C2 C 0.7046(2) 0.4041(3) 0.57613(11) 0.0575(10) Uani 1 1 d . . . H2A H 0.6702 0.3592 0.5565 0.069 Uiso 1 1 calc R . . C3 C 0.72425(17) 0.3652(2) 0.62521(10) 0.0456(9) Uani 1 1 d . . . H3A H 0.7492 0.4263 0.6439 0.055 Uiso 1 1 calc R . . C4 C 0.64359(19) 0.3237(2) 0.65165(10) 0.0436(9) Uani 1 1 d . . . H4A H 0.6047 0.3872 0.6557 0.052 Uiso 1 1 calc R . . C5 C 0.5949(2) 0.2405(3) 0.62341(10) 0.0478(9) Uani 1 1 d . . . H5A H 0.6221 0.1733 0.6174 0.057 Uiso 1 1 calc R . . C6 C 0.5177(2) 0.2548(3) 0.60669(11) 0.0608(10) Uani 1 1 d . . . H6A H 0.4888 0.3211 0.6121 0.073 Uiso 1 1 calc R . . H6B H 0.4906 0.1989 0.5891 0.073 Uiso 1 1 calc R . . S7 S 0.80384(5) 0.25558(8) 0.62193(3) 0.0708(3) Uani 1 1 d . . . C8 C 0.89147(18) 0.3233(3) 0.59571(12) 0.0435(9) Uani 1 1 d . . . C9 C 0.9207(2) 0.2927(3) 0.55203(14) 0.0684(11) Uani 1 1 d . . . H9A H 0.8926 0.2362 0.5352 0.082 Uiso 1 1 calc R . . C10 C 0.9914(3) 0.3435(5) 0.53167(14) 0.0854(15) Uani 1 1 d . . . H10A H 1.0122 0.3211 0.5014 0.102 Uiso 1 1 calc R . . C11 C 1.0306(3) 0.4258(4) 0.5557(2) 0.0874(16) Uani 1 1 d . . . H11A H 1.0776 0.4623 0.5417 0.105 Uiso 1 1 calc R . . C12 C 1.0025(3) 0.4558(3) 0.59964(18) 0.0735(12) Uani 1 1 d . . . H12A H 1.0307 0.5123 0.6163 0.088 Uiso 1 1 calc R . . C13 C 0.9336(2) 0.4049(3) 0.62016(12) 0.0591(10) Uani 1 1 d . . . H13A H 0.9149 0.4256 0.6511 0.071 Uiso 1 1 calc R . . C14 C 0.66356(18) 0.2803(3) 0.70255(10) 0.0429(9) Uani 1 1 d . . . H14A H 0.7033 0.2176 0.6991 0.052 Uiso 1 1 calc R . . N15 N 0.58484(14) 0.24083(19) 0.72527(8) 0.0382(7) Uani 1 1 d . . . S16 S 0.56543(5) 0.11334(7) 0.73194(3) 0.0440(3) Uani 1 1 d . . . O17 O 0.63620(12) 0.05514(16) 0.71174(6) 0.0492(6) Uani 1 1 d . . . O18 O 0.48035(12) 0.09094(16) 0.71559(7) 0.0525(6) Uani 1 1 d . . . C19 C 0.5642(2) 0.0886(2) 0.79361(10) 0.0375(8) Uani 1 1 d . . . C20 C 0.6371(2) 0.0527(2) 0.81641(12) 0.0489(9) Uani 1 1 d . . . H20A H 0.6885 0.0433 0.7988 0.059 Uiso 1 1 calc R . . C21 C 0.6355(2) 0.0302(3) 0.86476(12) 0.0554(10) Uani 1 1 d . . . H21A H 0.6860 0.0054 0.8800 0.066 Uiso 1 1 calc R . . C22 C 0.5618(3) 0.0433(3) 0.89121(11) 0.0514(10) Uani 1 1 d . . . C23 C 0.4895(2) 0.0791(3) 0.86786(13) 0.0562(10) Uani 1 1 d . . . H23A H 0.4382 0.0889 0.8855 0.067 Uiso 1 1 calc R . . C24 C 0.4898(2) 0.1010(2) 0.81984(12) 0.0485(9) Uani 1 1 d . . . H24A H 0.4389 0.1245 0.8046 0.058 Uiso 1 1 calc R . . C25 C 0.5594(2) 0.0190(3) 0.94399(10) 0.0781(12) Uani 1 1 d . . . H25A H 0.5569 0.0868 0.9619 0.117 Uiso 1 1 calc R . . H25B H 0.6109 -0.0210 0.9530 0.117 Uiso 1 1 calc R . . H25C H 0.5088 -0.0247 0.9512 0.117 Uiso 1 1 calc R . . C26 C 0.51533(18) 0.3160(2) 0.73545(10) 0.0492(9) Uani 1 1 d . . . H26A H 0.5384 0.3892 0.7387 0.074 Uiso 1 1 calc R . . H26B H 0.4870 0.2949 0.7652 0.074 Uiso 1 1 calc R . . H26C H 0.4739 0.3144 0.7093 0.074 Uiso 1 1 calc R . . C27 C 0.70763(18) 0.3649(3) 0.73415(10) 0.0497(9) Uani 1 1 d . . . H27A H 0.7611 0.3887 0.7185 0.060 Uiso 1 1 calc R . . H27B H 0.6699 0.4286 0.7373 0.060 Uiso 1 1 calc R . . C28 C 0.7284(2) 0.3225(3) 0.78308(11) 0.0450(9) Uani 1 1 d . . . C29 C 0.79495(19) 0.2501(3) 0.79005(12) 0.0525(10) Uani 1 1 d . . . H29A H 0.8272 0.2267 0.7633 0.063 Uiso 1 1 calc R . . C30 C 0.81550(19) 0.2111(3) 0.83431(13) 0.0560(10) Uani 1 1 d . . . H30A H 0.8617 0.1622 0.8381 0.067 Uiso 1 1 calc R . . C31 C 0.7685(2) 0.2436(3) 0.87325(13) 0.0590(10) Uani 1 1 d . . . C32 C 0.7014(2) 0.3143(3) 0.86799(13) 0.0603(10) Uani 1 1 d . . . H32A H 0.6687 0.3361 0.8949 0.072 Uiso 1 1 calc R . . C33 C 0.68217(19) 0.3533(3) 0.82284(13) 0.0540(10) Uani 1 1 d . . . H33A H 0.6360 0.4024 0.8192 0.065 Uiso 1 1 calc R . . O34 O 0.79377(14) 0.1986(2) 0.91618(9) 0.0815(8) Uani 1 1 d . . . C35 C 0.7482(2) 0.2318(3) 0.95712(12) 0.0981(15) Uani 1 1 d . . . H35A H 0.7712 0.1948 0.9852 0.147 Uiso 1 1 calc R . . H35B H 0.6877 0.2135 0.9534 0.147 Uiso 1 1 calc R . . H35C H 0.7542 0.3100 0.9612 0.147 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 C1 0.086(3) 0.061(3) 0.067(2) 0.013(2) -0.003(2) 0.002(3) C2 0.064(2) 0.055(3) 0.054(2) -0.001(2) 0.0053(19) -0.004(2) C3 0.051(2) 0.039(2) 0.047(2) -0.002(2) 0.0047(17) 0.0012(19) C4 0.047(2) 0.037(2) 0.047(2) 0.000(2) -0.0004(18) 0.0014(19) C5 0.058(2) 0.043(2) 0.043(2) -0.002(2) -0.0013(18) 0.001(2) C6 0.073(3) 0.052(3) 0.058(2) -0.001(2) -0.013(2) -0.009(2) S7 0.0630(6) 0.0478(6) 0.1015(7) 0.0057(6) 0.0226(6) 0.0090(6) C8 0.048(2) 0.039(2) 0.044(2) 0.002(2) 0.0047(19) 0.009(2) C9 0.063(3) 0.084(3) 0.058(3) -0.003(3) -0.010(2) 0.012(3) C10 0.077(4) 0.122(5) 0.058(3) 0.014(3) 0.006(3) 0.029(3) C11 0.062(3) 0.102(5) 0.098(4) 0.057(4) 0.011(3) 0.020(3) C12 0.058(3) 0.056(3) 0.107(4) 0.018(3) -0.012(3) -0.001(2) C13 0.066(3) 0.052(3) 0.058(2) -0.007(2) -0.001(2) 0.012(2) C14 0.0389(19) 0.040(2) 0.050(2) -0.0044(19) -0.0009(18) 0.0013(18) N15 0.0368(15) 0.0256(17) 0.0522(17) -0.0006(14) 0.0013(13) 0.0036(14) S16 0.0496(5) 0.0322(6) 0.0501(5) -0.0006(5) -0.0050(5) -0.0001(5) O17 0.0605(14) 0.0337(13) 0.0532(13) -0.0034(12) 0.0052(11) 0.0131(12) O18 0.0490(13) 0.0438(16) 0.0647(14) 0.0046(12) -0.0164(11) -0.0113(12) C19 0.0430(19) 0.023(2) 0.047(2) -0.0005(17) 0.001(2) -0.0033(18) C20 0.049(2) 0.041(2) 0.057(3) -0.003(2) -0.0030(19) 0.0022(19) C21 0.062(3) 0.051(3) 0.053(3) 0.004(2) -0.010(2) 0.004(2) C22 0.069(3) 0.041(2) 0.044(2) -0.001(2) -0.003(2) -0.003(2) C23 0.068(3) 0.045(3) 0.056(3) -0.006(2) 0.012(2) -0.003(2) C24 0.050(2) 0.038(2) 0.058(2) 0.001(2) -0.0016(19) 0.005(2) C25 0.105(3) 0.079(3) 0.051(2) 0.004(2) 0.000(2) -0.014(3) C26 0.046(2) 0.037(2) 0.065(2) 0.002(2) 0.0029(18) 0.0016(19) C27 0.048(2) 0.050(2) 0.051(2) -0.006(2) 0.0056(18) -0.0074(19) C28 0.038(2) 0.051(2) 0.045(2) -0.006(2) 0.0030(19) -0.018(2) C29 0.034(2) 0.071(3) 0.052(2) -0.009(2) 0.0061(19) -0.001(2) C30 0.044(2) 0.075(3) 0.049(2) 0.005(2) -0.007(2) 0.002(2) C31 0.056(2) 0.082(3) 0.039(2) 0.001(2) -0.001(2) -0.022(2) C32 0.052(2) 0.076(3) 0.054(3) -0.016(2) 0.009(2) -0.004(2) C33 0.043(2) 0.061(3) 0.058(2) -0.011(2) -0.001(2) -0.002(2) O34 0.0713(17) 0.125(3) 0.0481(16) 0.0081(18) -0.0042(14) -0.0088(17) C35 0.097(3) 0.149(4) 0.049(2) 0.008(3) -0.003(3) -0.036(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 C1 C2 1.312(4) . ? C2 C3 1.490(4) . ? C3 C4 1.552(4) . ? C3 S7 1.845(3) . ? C4 C5 1.507(4) . ? C4 C14 1.557(4) . ? C5 C6 1.308(4) . ? S7 C8 1.768(3) . ? C8 C9 1.361(4) . ? C8 C13 1.388(4) . ? C9 C10 1.396(5) . ? C10 C11 1.368(5) . ? C11 C12 1.359(5) . ? C12 C13 1.375(4) . ? C14 N15 1.471(3) . ? C14 C27 1.536(4) . ? N15 C26 1.460(3) . ? N15 S16 1.619(2) . ? S16 O18 1.4357(18) . ? S16 O17 1.4380(19) . ? S16 C19 1.756(3) . ? C19 C20 1.382(4) . ? C19 C24 1.387(4) . ? C20 C21 1.384(4) . ? C21 C22 1.381(4) . ? C22 C23 1.382(4) . ? C22 C25 1.511(4) . ? C23 C24 1.374(4) . ? C27 C28 1.505(4) . ? C28 C33 1.383(4) . ? C28 C29 1.388(4) . ? C29 C30 1.370(4) . ? C30 C31 1.377(4) . ? C31 C32 1.376(4) . ? C31 O34 1.384(4) . ? C32 C33 1.388(4) . ? O34 C35 1.413(4) . ? 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 C1 C2 C3 124.7(3) . . ? C2 C3 C4 112.3(3) . . ? C2 C3 S7 109.3(2) . . ? C4 C3 S7 109.3(2) . . ? C5 C4 C3 112.8(2) . . ? C5 C4 C14 110.3(2) . . ? C3 C4 C14 112.9(2) . . ? C6 C5 C4 124.3(3) . . ? C8 S7 C3 101.29(14) . . ? C9 C8 C13 119.2(3) . . ? C9 C8 S7 120.2(3) . . ? C13 C8 S7 120.6(3) . . ? C8 C9 C10 120.6(4) . . ? C11 C10 C9 119.3(4) . . ? C12 C11 C10 120.4(4) . . ? C11 C12 C13 120.5(4) . . ? C12 C13 C8 120.0(3) . . ? N15 C14 C27 110.7(2) . . ? N15 C14 C4 110.1(2) . . ? C27 C14 C4 112.6(3) . . ? C26 N15 C14 119.8(2) . . ? C26 N15 S16 117.36(18) . . ? C14 N15 S16 122.1(2) . . ? O18 S16 O17 119.48(12) . . ? O18 S16 N15 109.01(12) . . ? O17 S16 N15 107.38(12) . . ? O18 S16 C19 105.71(14) . . ? O17 S16 C19 107.99(14) . . ? N15 S16 C19 106.60(13) . . ? C20 C19 C24 119.0(3) . . ? C20 C19 S16 120.2(3) . . ? C24 C19 S16 120.8(3) . . ? C19 C20 C21 120.2(3) . . ? C22 C21 C20 121.2(3) . . ? C21 C22 C23 117.9(3) . . ? C21 C22 C25 121.6(3) . . ? C23 C22 C25 120.5(3) . . ? C24 C23 C22 121.7(3) . . ? C23 C24 C19 120.1(3) . . ? C28 C27 C14 112.7(3) . . ? C33 C28 C29 117.2(3) . . ? C33 C28 C27 121.7(3) . . ? C29 C28 C27 121.1(3) . . ? C30 C29 C28 122.1(3) . . ? C29 C30 C31 119.4(3) . . ? C32 C31 C30 120.6(3) . . ? C32 C31 O34 124.6(3) . . ? C30 C31 O34 114.8(4) . . ? C31 C32 C33 119.0(3) . . ? C28 C33 C32 121.7(3) . . ? C31 O34 C35 116.5(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 52.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.157 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.035 #===END data_Compound_15 _database_code_depnum_ccdc_archive 'CCDC 698821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H35 N O6 S2' _chemical_formula_sum 'C34 H35 N O6 S2' _chemical_formula_weight 617.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 15.99842(7) _cell_length_b 30.52231(13) _cell_length_c 12.73593(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6219.07(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 59266 _cell_measurement_theta_min 2.7596 _cell_measurement_theta_max 70.8247 _exptl_crystal_description tablets _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 1.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76604 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 165242 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 71.03 _reflns_number_total 6002 _reflns_number_gt 4796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0697P)^2^+0.8753P] 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 6002 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _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 N1 N -0.18193(9) 0.39883(5) 0.59559(11) 0.0330(3) Uani 1 1 d . . . C2 C -0.13497(10) 0.35946(5) 0.56341(13) 0.0298(3) Uani 1 1 d . . . H2A H -0.1059 0.3479 0.6272 0.036 Uiso 1 1 calc R . . C3 C -0.06658(10) 0.37196(5) 0.48258(13) 0.0292(3) Uani 1 1 d . . . H3A H -0.0522 0.3447 0.4428 0.035 Uiso 1 1 calc R . . C4 C -0.10173(11) 0.40467(5) 0.40349(13) 0.0331(4) Uani 1 1 d . . . H4A H -0.0570 0.4137 0.3543 0.040 Uiso 1 1 calc R . . H4B H -0.1466 0.3905 0.3621 0.040 Uiso 1 1 calc R . . O5 O -0.13457(8) 0.44260(4) 0.45533(9) 0.0363(3) Uani 1 1 d . . . C6 C -0.20512(11) 0.43026(6) 0.51386(14) 0.0382(4) Uani 1 1 d . . . H6A H -0.2472 0.4169 0.4667 0.046 Uiso 1 1 calc R . . H6B H -0.2304 0.4565 0.5466 0.046 Uiso 1 1 calc R . . S7 S -0.19843(3) 0.408200(13) 0.71894(3) 0.03272(12) Uani 1 1 d . . . O8 O -0.26192(8) 0.44131(4) 0.72400(10) 0.0424(3) Uani 1 1 d . . . O9 O -0.21250(8) 0.36690(4) 0.76958(10) 0.0401(3) Uani 1 1 d . . . C10 C -0.10599(11) 0.43036(5) 0.77326(13) 0.0318(4) Uani 1 1 d . . . C11 C -0.07016(12) 0.46737(6) 0.72795(14) 0.0373(4) Uani 1 1 d . . . H11A H -0.0946 0.4804 0.6676 0.045 Uiso 1 1 calc R . . C12 C 0.00132(13) 0.48484(6) 0.77176(15) 0.0409(4) Uani 1 1 d . . . H12A H 0.0262 0.5099 0.7403 0.049 Uiso 1 1 calc R . . C13 C 0.03778(12) 0.46669(6) 0.86079(15) 0.0405(4) Uani 1 1 d . . . C14 C 0.00036(12) 0.43004(6) 0.90475(15) 0.0422(4) Uani 1 1 d . . . H14A H 0.0243 0.4173 0.9658 0.051 Uiso 1 1 calc R . . C15 C -0.07099(12) 0.41151(6) 0.86187(14) 0.0375(4) Uani 1 1 d . . . H15A H -0.0955 0.3863 0.8928 0.045 Uiso 1 1 calc R . . C16 C 0.11581(15) 0.48581(8) 0.90829(19) 0.0575(6) Uani 1 1 d . . . H16A H 0.1053 0.4933 0.9820 0.086 Uiso 1 1 calc R . . H16B H 0.1317 0.5123 0.8696 0.086 Uiso 1 1 calc R . . H16C H 0.1612 0.4643 0.9042 0.086 Uiso 1 1 calc R . . C17 C -0.19383(11) 0.32299(6) 0.52348(15) 0.0367(4) Uani 1 1 d . . . H17A H -0.2461 0.3232 0.5652 0.044 Uiso 1 1 calc R . . H17B H -0.2086 0.3286 0.4492 0.044 Uiso 1 1 calc R . . C18 C -0.15256(11) 0.27883(5) 0.53257(14) 0.0347(4) Uani 1 1 d . . . C19 C -0.13948(13) 0.26040(6) 0.63058(15) 0.0426(4) Uani 1 1 d . . . H19A H -0.1571 0.2760 0.6913 0.051 Uiso 1 1 calc R . . C20 C -0.10113(13) 0.21962(6) 0.64280(15) 0.0431(4) Uani 1 1 d . . . H20A H -0.0928 0.2077 0.7110 0.052 Uiso 1 1 calc R . . C21 C -0.07558(12) 0.19678(6) 0.55556(15) 0.0382(4) Uani 1 1 d . . . C22 C -0.08766(15) 0.21442(6) 0.45665(15) 0.0483(5) Uani 1 1 d . . . H22A H -0.0698 0.1989 0.3961 0.058 Uiso 1 1 calc R . . C23 C -0.12598(14) 0.25494(6) 0.44655(15) 0.0445(5) Uani 1 1 d . . . H23A H -0.1343 0.2667 0.3783 0.053 Uiso 1 1 calc R . . O24 O -0.03829(10) 0.15609(4) 0.55952(11) 0.0504(4) Uani 1 1 d . . . C25 C -0.04261(16) 0.13324(7) 0.65696(17) 0.0526(5) Uani 1 1 d . . . H25A H -0.0078 0.1482 0.7091 0.079 Uiso 1 1 calc R . . H25B H -0.0223 0.1032 0.6474 0.079 Uiso 1 1 calc R . . H25C H -0.1007 0.1325 0.6814 0.079 Uiso 1 1 calc R . . C26 C 0.01317(10) 0.38641(5) 0.54162(13) 0.0295(3) Uani 1 1 d . . . H26A H -0.0005 0.4111 0.5903 0.035 Uiso 1 1 calc R . . S27 S 0.09460(2) 0.403421(12) 0.45091(3) 0.02993(12) Uani 1 1 d . . . O28 O 0.11226(8) 0.36686(4) 0.38326(10) 0.0419(3) Uani 1 1 d . . . O29 O 0.07170(8) 0.44449(4) 0.40360(11) 0.0428(3) Uani 1 1 d . . . C30 C 0.18140(11) 0.41331(5) 0.53286(13) 0.0311(4) Uani 1 1 d . . . C31 C 0.24129(12) 0.38110(6) 0.54605(17) 0.0432(5) Uani 1 1 d . . . H31A H 0.2372 0.3541 0.5093 0.052 Uiso 1 1 calc R . . C32 C 0.30716(14) 0.38888(7) 0.6137(2) 0.0566(6) Uani 1 1 d . . . H32A H 0.3490 0.3672 0.6235 0.068 Uiso 1 1 calc R . . C33 C 0.31221(14) 0.42834(8) 0.66744(17) 0.0558(6) Uani 1 1 d . . . H33A H 0.3571 0.4333 0.7148 0.067 Uiso 1 1 calc R . . C34 C 0.25287(14) 0.46014(7) 0.65267(17) 0.0509(5) Uani 1 1 d . . . H34A H 0.2573 0.4872 0.6891 0.061 Uiso 1 1 calc R . . C35 C 0.18631(12) 0.45307(6) 0.58493(15) 0.0392(4) Uani 1 1 d . . . H35A H 0.1450 0.4750 0.5745 0.047 Uiso 1 1 calc R . . C36 C 0.04594(11) 0.34767(6) 0.60435(15) 0.0378(4) Uani 1 1 d . . . H36A H 0.0480 0.3200 0.5702 0.045 Uiso 1 1 calc R . . C37 C 0.07145(12) 0.34950(6) 0.70158(15) 0.0401(4) Uani 1 1 d . . . H37A H 0.0734 0.3776 0.7334 0.048 Uiso 1 1 calc R . . C38 C 0.09767(12) 0.31184(6) 0.76705(17) 0.0432(5) Uani 1 1 d . . . C39 C 0.09881(16) 0.26898(8) 0.72952(19) 0.0599(6) Uani 1 1 d . . . H39A H 0.0846 0.2632 0.6584 0.072 Uiso 1 1 calc R . . C40 C 0.12079(17) 0.23427(7) 0.7961(2) 0.0632(6) Uani 1 1 d . . . H40A H 0.1219 0.2051 0.7703 0.076 Uiso 1 1 calc R . . C41 C 0.14072(14) 0.24281(7) 0.89872(19) 0.0545(6) Uani 1 1 d . . . H41A H 0.1557 0.2195 0.9444 0.065 Uiso 1 1 calc R . . C42 C 0.13907(16) 0.28497(8) 0.9354(2) 0.0609(6) Uani 1 1 d . . . H42A H 0.1526 0.2907 1.0068 0.073 Uiso 1 1 calc R . . C43 C 0.11802(15) 0.31923(7) 0.87002(18) 0.0554(5) Uani 1 1 d . . . H43A H 0.1176 0.3483 0.8967 0.066 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 N1 0.0334(7) 0.0358(7) 0.0299(8) 0.0007(6) 0.0016(6) 0.0079(6) C2 0.0283(8) 0.0295(8) 0.0317(9) -0.0009(6) -0.0010(7) 0.0026(6) C3 0.0295(8) 0.0288(8) 0.0293(8) -0.0006(6) -0.0008(7) 0.0015(6) C4 0.0325(9) 0.0393(9) 0.0275(9) 0.0006(7) -0.0020(7) 0.0038(7) O5 0.0416(7) 0.0346(6) 0.0327(6) 0.0044(5) -0.0005(5) 0.0080(5) C6 0.0361(10) 0.0438(10) 0.0347(9) 0.0025(8) -0.0014(7) 0.0119(7) S7 0.0307(2) 0.0362(2) 0.0313(2) -0.00081(16) 0.00541(16) 0.00176(16) O8 0.0353(7) 0.0481(7) 0.0438(7) -0.0055(6) 0.0056(6) 0.0094(5) O9 0.0434(7) 0.0393(7) 0.0378(7) 0.0017(5) 0.0094(5) -0.0075(5) C10 0.0342(9) 0.0313(8) 0.0297(9) -0.0020(6) 0.0046(7) 0.0017(7) C11 0.0447(10) 0.0320(8) 0.0353(9) 0.0054(7) 0.0011(8) 0.0003(7) C12 0.0484(11) 0.0339(9) 0.0405(10) 0.0037(7) 0.0040(8) -0.0051(8) C13 0.0412(10) 0.0434(10) 0.0369(10) -0.0032(8) 0.0017(8) -0.0022(8) C14 0.0439(11) 0.0480(11) 0.0348(9) 0.0064(8) -0.0020(8) -0.0003(8) C15 0.0412(10) 0.0374(9) 0.0338(9) 0.0081(7) 0.0040(8) -0.0004(7) C16 0.0529(13) 0.0652(14) 0.0543(13) 0.0004(11) -0.0066(10) -0.0167(11) C17 0.0287(9) 0.0404(9) 0.0409(10) 0.0000(8) -0.0017(7) -0.0042(7) C18 0.0323(9) 0.0343(9) 0.0375(9) -0.0017(7) 0.0008(7) -0.0090(7) C19 0.0528(12) 0.0423(10) 0.0327(9) -0.0062(8) 0.0044(8) 0.0018(8) C20 0.0581(12) 0.0410(10) 0.0302(9) -0.0014(7) 0.0023(8) 0.0017(8) C21 0.0449(10) 0.0331(9) 0.0365(10) -0.0023(7) 0.0071(8) -0.0054(7) C22 0.0725(15) 0.0383(10) 0.0341(10) -0.0035(8) 0.0157(9) 0.0003(9) C23 0.0616(13) 0.0404(10) 0.0313(9) 0.0021(7) 0.0049(9) -0.0046(9) O24 0.0757(10) 0.0351(7) 0.0404(8) 0.0012(6) 0.0146(7) 0.0070(6) C25 0.0717(15) 0.0417(10) 0.0444(12) 0.0070(9) 0.0099(10) 0.0076(10) C26 0.0274(8) 0.0326(8) 0.0286(8) 0.0014(6) 0.0014(6) 0.0007(6) S27 0.0296(2) 0.0309(2) 0.0293(2) 0.00233(15) 0.00109(15) -0.00112(15) O28 0.0420(7) 0.0453(7) 0.0383(7) -0.0113(6) 0.0059(6) -0.0043(5) O29 0.0422(7) 0.0401(7) 0.0461(8) 0.0178(6) -0.0027(6) -0.0025(5) C30 0.0292(8) 0.0309(8) 0.0331(9) 0.0018(7) 0.0021(7) -0.0037(6) C31 0.0355(10) 0.0317(9) 0.0625(13) 0.0000(8) -0.0069(9) 0.0008(7) C32 0.0416(11) 0.0512(12) 0.0769(16) 0.0135(11) -0.0176(11) -0.0016(9) C33 0.0503(12) 0.0709(15) 0.0462(12) 0.0088(10) -0.0146(10) -0.0184(11) C34 0.0564(13) 0.0518(11) 0.0444(11) -0.0126(9) 0.0022(10) -0.0160(10) C35 0.0393(10) 0.0339(9) 0.0444(10) -0.0052(8) 0.0063(8) -0.0032(7) C36 0.0301(9) 0.0434(10) 0.0401(10) 0.0041(8) 0.0025(7) 0.0004(7) C37 0.0391(10) 0.0390(9) 0.0423(10) 0.0017(8) -0.0008(8) 0.0005(8) C38 0.0346(10) 0.0388(10) 0.0563(12) 0.0148(8) 0.0027(8) 0.0027(7) C39 0.0737(16) 0.0579(13) 0.0481(13) 0.0112(10) -0.0097(11) 0.0035(11) C40 0.0809(17) 0.0414(11) 0.0673(15) 0.0121(11) -0.0133(13) 0.0032(11) C41 0.0510(12) 0.0459(11) 0.0665(15) 0.0262(10) -0.0140(10) -0.0034(9) C42 0.0666(15) 0.0564(13) 0.0596(14) 0.0147(11) -0.0166(12) -0.0032(11) C43 0.0638(14) 0.0466(11) 0.0558(13) 0.0092(10) -0.0102(11) 0.0003(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 N1 C6 1.463(2) . ? N1 C2 1.475(2) . ? N1 S7 1.6185(15) . ? C2 C17 1.544(2) . ? C2 C3 1.550(2) . ? C3 C4 1.526(2) . ? C3 C26 1.545(2) . ? C4 O5 1.4327(19) . ? O5 C6 1.404(2) . ? S7 O9 1.4339(13) . ? S7 O8 1.4343(13) . ? S7 C10 1.7673(18) . ? C10 C15 1.385(2) . ? C10 C11 1.392(2) . ? C11 C12 1.380(3) . ? C12 C13 1.390(3) . ? C13 C14 1.387(3) . ? C13 C16 1.505(3) . ? C14 C15 1.386(3) . ? C17 C18 1.505(2) . ? C18 C23 1.383(3) . ? C18 C19 1.385(3) . ? C19 C20 1.397(3) . ? C20 C21 1.374(3) . ? C21 O24 1.379(2) . ? C21 C22 1.384(3) . ? C22 C23 1.386(3) . ? O24 C25 1.425(2) . ? C26 C36 1.520(2) . ? C26 S27 1.8169(16) . ? S27 O28 1.4378(12) . ? S27 O29 1.4382(12) . ? S27 C30 1.7632(18) . ? C30 C31 1.383(3) . ? C30 C35 1.385(2) . ? C31 C32 1.382(3) . ? C32 C33 1.387(3) . ? C33 C34 1.371(3) . ? C34 C35 1.387(3) . ? C36 C37 1.305(3) . ? C37 C38 1.480(2) . ? C38 C43 1.370(3) . ? C38 C39 1.393(3) . ? C39 C40 1.402(3) . ? C40 C41 1.370(3) . ? C41 C42 1.369(3) . ? C42 C43 1.379(3) . ? 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 C6 N1 C2 117.75(14) . . ? C6 N1 S7 122.22(11) . . ? C2 N1 S7 119.78(11) . . ? N1 C2 C17 111.60(14) . . ? N1 C2 C3 110.08(13) . . ? C17 C2 C3 112.90(14) . . ? C4 C3 C26 116.02(13) . . ? C4 C3 C2 109.84(13) . . ? C26 C3 C2 109.26(13) . . ? O5 C4 C3 111.08(13) . . ? C6 O5 C4 108.82(13) . . ? O5 C6 N1 110.46(13) . . ? O9 S7 O8 119.22(8) . . ? O9 S7 N1 107.87(7) . . ? O8 S7 N1 106.48(8) . . ? O9 S7 C10 106.96(8) . . ? O8 S7 C10 107.78(8) . . ? N1 S7 C10 108.13(8) . . ? C15 C10 C11 120.55(17) . . ? C15 C10 S7 119.90(13) . . ? C11 C10 S7 119.53(14) . . ? C12 C11 C10 119.17(17) . . ? C11 C12 C13 121.57(17) . . ? C14 C13 C12 118.01(18) . . ? C14 C13 C16 120.57(18) . . ? C12 C13 C16 121.42(18) . . ? C15 C14 C13 121.71(18) . . ? C10 C15 C14 118.99(16) . . ? C18 C17 C2 110.65(14) . . ? C23 C18 C19 116.96(17) . . ? C23 C18 C17 123.10(17) . . ? C19 C18 C17 119.94(16) . . ? C18 C19 C20 121.92(17) . . ? C21 C20 C19 119.53(18) . . ? C20 C21 O24 123.80(17) . . ? C20 C21 C22 119.82(18) . . ? O24 C21 C22 116.38(16) . . ? C21 C22 C23 119.57(17) . . ? C18 C23 C22 122.20(18) . . ? C21 O24 C25 116.85(15) . . ? C36 C26 C3 108.57(13) . . ? C36 C26 S27 108.01(11) . . ? C3 C26 S27 111.35(11) . . ? O28 S27 O29 118.38(8) . . ? O28 S27 C30 109.43(8) . . ? O29 S27 C30 107.42(8) . . ? O28 S27 C26 107.47(8) . . ? O29 S27 C26 109.44(8) . . ? C30 S27 C26 103.72(8) . . ? C31 C30 C35 121.69(17) . . ? C31 C30 S27 119.73(13) . . ? C35 C30 S27 118.56(14) . . ? C32 C31 C30 118.82(18) . . ? C31 C32 C33 120.1(2) . . ? C34 C33 C32 120.45(19) . . ? C33 C34 C35 120.44(19) . . ? C30 C35 C34 118.53(18) . . ? C37 C36 C26 124.98(17) . . ? C36 C37 C38 126.15(18) . . ? C43 C38 C39 118.67(19) . . ? C43 C38 C37 118.61(18) . . ? C39 C38 C37 122.7(2) . . ? C38 C39 C40 120.4(2) . . ? C41 C40 C39 119.5(2) . . ? C42 C41 C40 120.0(2) . . ? C41 C42 C43 120.7(2) . . ? C38 C43 C42 120.8(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 71.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.631 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.046 #===END data_Compound_17 _database_code_depnum_ccdc_archive 'CCDC 699430' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H36 N2 O6 S2' _chemical_formula_sum 'C31 H36 N2 O6 S2' _chemical_formula_weight 596.74 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 Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 15.217(9) _cell_length_b 15.731(3) _cell_length_c 26.981(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.78(3) _cell_angle_gamma 90.00 _cell_volume 6323(4) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.66 _cell_measurement_theta_max 12.50 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4274 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.1254 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 22.51 _reflns_number_total 4093 _reflns_number_gt 2042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0642P)^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 4093 _refine_ls_number_parameters 383 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1677 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _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 N1 N 0.5769(4) 0.3306(4) 0.6238(2) 0.0599(17) Uani 1 1 d . . . C2 C 0.6077(5) 0.3629(5) 0.5838(3) 0.0518(18) Uani 1 1 d . . . H2A H 0.6677 0.3783 0.5847 0.062 Uiso 1 1 calc R . . C3 C 0.5395(4) 0.3701(4) 0.5419(2) 0.0446(17) Uani 1 1 d . . . C4 C 0.4603(5) 0.3413(4) 0.5576(2) 0.0470(18) Uani 1 1 d . . . C5 C 0.3697(5) 0.3334(5) 0.5328(3) 0.057(2) Uani 1 1 d . . . H5A H 0.3506 0.3493 0.4987 0.069 Uiso 1 1 calc R . . C6 C 0.3095(5) 0.3010(5) 0.5608(3) 0.062(2) Uani 1 1 d . . . H6A H 0.2485 0.2966 0.5453 0.075 Uiso 1 1 calc R . . C7 C 0.3368(5) 0.2751(5) 0.6109(3) 0.066(2) Uani 1 1 d . . . H7A H 0.2941 0.2525 0.6280 0.079 Uiso 1 1 calc R . . C8 C 0.4259(5) 0.2819(5) 0.6363(3) 0.0579(19) Uani 1 1 d . . . H8A H 0.4447 0.2651 0.6703 0.070 Uiso 1 1 calc R . . C9 C 0.4856(5) 0.3151(4) 0.6084(2) 0.0494(18) Uani 1 1 d . . . C10 C 0.6298(5) 0.3110(7) 0.6740(3) 0.087(3) Uani 1 1 d . . . H10A H 0.6447 0.2510 0.6760 0.130 Uiso 1 1 calc R . . H10B H 0.5953 0.3248 0.6995 0.130 Uiso 1 1 calc R . . H10C H 0.6847 0.3443 0.6800 0.130 Uiso 1 1 calc R . . C11 C 0.5473(5) 0.4027(4) 0.4905(2) 0.0477(17) Uani 1 1 d . . . H11A H 0.6019 0.4373 0.4942 0.057 Uiso 1 1 calc R . . H11B H 0.4960 0.4399 0.4777 0.057 Uiso 1 1 calc R . . C12 C 0.5506(4) 0.3330(4) 0.4511(2) 0.0432(16) Uani 1 1 d . . . H12A H 0.4935 0.3009 0.4464 0.052 Uiso 1 1 calc R . . N13 N 0.6243(3) 0.2729(3) 0.4695(2) 0.0413(13) Uani 1 1 d D A . H13 H 0.664(4) 0.289(5) 0.4974(16) 0.07(2) Uiso 1 1 d D . . S14 S 0.61430(11) 0.17231(11) 0.46353(6) 0.0461(5) Uani 1 1 d D . . O15 O 0.7035(3) 0.1382(3) 0.48099(18) 0.0558(13) Uani 1 1 d . A . O16 O 0.5673(3) 0.1556(3) 0.41259(17) 0.0591(13) Uani 1 1 d . A . C17 C 0.5474(5) 0.1355(3) 0.5065(4) 0.047(3) Uani 0.74(3) 1 d PGDU A 1 C18 C 0.5843(7) 0.1285(6) 0.5579(4) 0.070(3) Uani 0.74(3) 1 d PGDU A 1 H18A H 0.6450 0.1420 0.5701 0.084 Uiso 0.74(3) 1 calc PR A 1 C19 C 0.5313(10) 0.1016(6) 0.5912(4) 0.069(4) Uani 0.74(3) 1 d PGDU A 1 H19A H 0.5562 0.0969 0.6260 0.083 Uiso 0.74(3) 1 calc PR A 1 C20 C 0.4415(8) 0.0816(5) 0.5731(6) 0.064(4) Uani 0.74(3) 1 d PGDU A 1 C21 C 0.4046(5) 0.0886(6) 0.5217(6) 0.062(4) Uani 0.74(3) 1 d PGDU A 1 H21A H 0.3439 0.0751 0.5095 0.075 Uiso 0.74(3) 1 calc PR A 1 C22 C 0.4576(5) 0.1155(6) 0.4884(5) 0.062(3) Uani 0.74(3) 1 d PGDU A 1 H22A H 0.4327 0.1202 0.4537 0.074 Uiso 0.74(3) 1 calc PR A 1 C23 C 0.3840(12) 0.0511(7) 0.6101(8) 0.081(5) Uani 0.74(3) 1 d PDU A 1 H23A H 0.3642 -0.0067 0.6017 0.121 Uiso 0.74(3) 1 calc PR A 1 H23B H 0.3321 0.0879 0.6076 0.121 Uiso 0.74(3) 1 calc PR A 1 H23C H 0.4193 0.0528 0.6444 0.121 Uiso 0.74(3) 1 calc PR A 1 C17' C 0.5360(15) 0.1346(7) 0.4966(12) 0.048(8) Uiso 0.26(3) 1 d PGDU A 2 C18' C 0.5578(16) 0.1351(17) 0.5492(12) 0.064(8) Uiso 0.26(3) 1 d PGDU A 2 H18B H 0.6142 0.1554 0.5660 0.077 Uiso 0.26(3) 1 calc PR A 2 C19' C 0.496(2) 0.1058(19) 0.5769(10) 0.073(9) Uiso 0.26(3) 1 d PGDU A 2 H19B H 0.5111 0.1062 0.6125 0.087 Uiso 0.26(3) 1 calc PR A 2 C20' C 0.4131(17) 0.0758(13) 0.5520(12) 0.049(8) Uiso 0.26(3) 1 d PGDU A 2 C21' C 0.3912(14) 0.0753(18) 0.4994(12) 0.062(8) Uiso 0.26(3) 1 d PGDU A 2 H21B H 0.3349 0.0550 0.4825 0.075 Uiso 0.26(3) 1 calc PR A 2 C22' C 0.4527(18) 0.1046(17) 0.4717(10) 0.055(7) Uiso 0.26(3) 1 d PGDU A 2 H22B H 0.4379 0.1042 0.4361 0.065 Uiso 0.26(3) 1 calc PR A 2 C23' C 0.346(2) 0.0438(18) 0.5830(16) 0.074(9) Uiso 0.26(3) 1 d PDU A 2 H23D H 0.3057 0.0896 0.5876 0.112 Uiso 0.26(3) 1 calc PR A 2 H23E H 0.3781 0.0243 0.6158 0.112 Uiso 0.26(3) 1 calc PR A 2 H23F H 0.3114 -0.0029 0.5653 0.112 Uiso 0.26(3) 1 calc PR A 2 C24 C 0.5595(4) 0.3674(4) 0.3992(2) 0.0406(16) Uani 1 1 d . . . H24A H 0.5559 0.3179 0.3763 0.049 Uiso 1 1 calc R . . C25 C 0.6541(4) 0.4067(5) 0.4032(3) 0.0543(19) Uani 1 1 d . . . H25A H 0.6600 0.4566 0.4254 0.065 Uiso 1 1 calc R . . H25B H 0.6996 0.3652 0.4186 0.065 Uiso 1 1 calc R . . O26 O 0.6701(3) 0.4311(3) 0.35545(17) 0.0534(13) Uani 1 1 d . . . C27 C 0.6110(5) 0.5002(5) 0.3353(3) 0.0525(18) Uani 1 1 d . . . H27A H 0.6184 0.5489 0.3590 0.063 Uiso 1 1 calc R . . C28 C 0.5147(4) 0.4678(5) 0.3248(2) 0.0463(17) Uani 1 1 d . . . H28A H 0.5079 0.4230 0.2990 0.056 Uiso 1 1 calc R . . H28B H 0.4738 0.5143 0.3114 0.056 Uiso 1 1 calc R . . C29 C 0.4899(4) 0.4328(4) 0.3728(2) 0.0397(16) Uani 1 1 d . . . H29A H 0.4918 0.4812 0.3964 0.048 Uiso 1 1 calc R . . O30 O 0.6311(3) 0.5235(3) 0.28952(17) 0.0594(14) Uani 1 1 d . . . C31 C 0.7166(6) 0.5622(6) 0.2957(3) 0.083(3) Uani 1 1 d . . . H31A H 0.7280 0.5778 0.2628 0.125 Uiso 1 1 calc R . . H31B H 0.7623 0.5225 0.3120 0.125 Uiso 1 1 calc R . . H31C H 0.7182 0.6127 0.3165 0.125 Uiso 1 1 calc R . . S32 S 0.37595(11) 0.39589(12) 0.35831(7) 0.0471(5) Uani 1 1 d . . . O33 O 0.3540(3) 0.3629(3) 0.40403(17) 0.0549(13) Uani 1 1 d . . . O34 O 0.3221(3) 0.4637(3) 0.33258(18) 0.0567(13) Uani 1 1 d . . . C35 C 0.3751(4) 0.3112(5) 0.3153(3) 0.0475(18) Uani 1 1 d . . . C36 C 0.3953(4) 0.2308(5) 0.3324(3) 0.0548(19) Uani 1 1 d . . . H36A H 0.4073 0.2198 0.3674 0.066 Uiso 1 1 calc R . . C37 C 0.3983(5) 0.1648(5) 0.2986(3) 0.061(2) Uani 1 1 d . . . H37A H 0.4140 0.1098 0.3110 0.073 Uiso 1 1 calc R . . C38 C 0.3785(5) 0.1788(6) 0.2465(3) 0.062(2) Uani 1 1 d . . . C39 C 0.3597(5) 0.2605(6) 0.2301(3) 0.061(2) Uani 1 1 d . . . H39A H 0.3482 0.2718 0.1951 0.073 Uiso 1 1 calc R . . C40 C 0.3570(4) 0.3273(5) 0.2637(3) 0.0540(18) Uani 1 1 d . . . H40A H 0.3431 0.3827 0.2515 0.065 Uiso 1 1 calc R . . C41 C 0.3790(5) 0.1079(6) 0.2095(4) 0.083(3) Uani 1 1 d . . . H41A H 0.3235 0.0761 0.2055 0.124 Uiso 1 1 calc R . . H41B H 0.4294 0.0705 0.2219 0.124 Uiso 1 1 calc R . . H41C H 0.3847 0.1314 0.1770 0.124 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 N1 0.048(4) 0.078(4) 0.044(3) -0.001(3) -0.012(3) -0.008(3) C2 0.036(4) 0.068(5) 0.053(4) -0.008(4) 0.010(3) -0.001(3) C3 0.054(4) 0.041(4) 0.039(4) -0.007(3) 0.011(3) -0.004(3) C4 0.057(5) 0.045(4) 0.036(4) -0.012(3) 0.004(3) -0.012(3) C5 0.059(5) 0.062(5) 0.045(4) -0.018(4) -0.003(4) 0.000(4) C6 0.053(5) 0.078(6) 0.057(5) -0.012(4) 0.013(4) -0.006(4) C7 0.068(6) 0.067(5) 0.073(6) -0.016(5) 0.036(5) -0.009(5) C8 0.067(5) 0.051(4) 0.057(4) -0.006(4) 0.015(4) -0.001(4) C9 0.058(5) 0.047(4) 0.039(4) -0.007(3) 0.000(3) 0.001(4) C10 0.061(5) 0.121(8) 0.071(6) 0.004(6) -0.004(4) 0.004(5) C11 0.053(4) 0.040(4) 0.051(4) -0.007(3) 0.012(3) -0.002(3) C12 0.036(4) 0.043(4) 0.051(4) -0.009(3) 0.009(3) 0.002(3) N13 0.034(3) 0.045(3) 0.044(3) -0.002(3) 0.006(2) 0.003(3) S14 0.0406(10) 0.0467(10) 0.0491(10) -0.0038(9) 0.0044(8) 0.0043(9) O15 0.042(3) 0.055(3) 0.070(3) 0.000(2) 0.011(2) 0.015(2) O16 0.065(3) 0.056(3) 0.051(3) -0.012(2) 0.000(2) 0.001(3) C17 0.039(6) 0.043(6) 0.059(8) 0.009(5) 0.013(5) 0.001(4) C18 0.059(7) 0.089(8) 0.065(7) 0.004(6) 0.019(6) -0.004(7) C19 0.080(9) 0.075(7) 0.058(7) 0.014(6) 0.027(7) 0.007(7) C20 0.069(8) 0.046(6) 0.084(9) 0.001(6) 0.028(8) 0.007(6) C21 0.047(6) 0.052(7) 0.086(11) 0.014(7) 0.011(6) 0.003(5) C22 0.043(6) 0.066(7) 0.073(8) 0.021(7) 0.003(6) 0.004(5) C23 0.097(10) 0.059(8) 0.106(11) 0.007(7) 0.066(9) -0.004(7) C24 0.030(3) 0.051(4) 0.040(4) 0.000(3) 0.006(3) -0.010(3) C25 0.039(4) 0.074(5) 0.051(4) 0.007(4) 0.010(3) -0.008(4) O26 0.036(3) 0.076(3) 0.051(3) 0.005(3) 0.017(2) 0.000(2) C27 0.057(5) 0.059(5) 0.041(4) -0.001(4) 0.008(3) -0.013(4) C28 0.037(4) 0.057(4) 0.045(4) 0.004(3) 0.007(3) -0.006(3) C29 0.029(4) 0.043(4) 0.046(4) -0.003(3) 0.004(3) -0.003(3) O30 0.055(3) 0.080(4) 0.043(3) 0.006(3) 0.008(2) -0.024(3) C31 0.073(6) 0.107(7) 0.072(6) 0.003(5) 0.021(5) -0.033(6) S32 0.0329(9) 0.0597(12) 0.0475(10) -0.0012(9) 0.0057(7) -0.0026(9) O33 0.031(2) 0.088(4) 0.049(3) 0.000(3) 0.015(2) -0.006(2) O34 0.040(3) 0.065(3) 0.062(3) 0.007(3) 0.004(2) 0.008(2) C35 0.030(4) 0.059(5) 0.051(4) 0.001(4) 0.002(3) -0.013(3) C36 0.038(4) 0.072(6) 0.053(4) 0.002(4) 0.005(3) -0.013(4) C37 0.040(4) 0.058(5) 0.081(6) -0.009(5) 0.006(4) -0.005(4) C38 0.038(4) 0.083(6) 0.065(5) -0.010(5) 0.012(4) -0.027(4) C39 0.046(4) 0.091(7) 0.049(4) -0.006(5) 0.015(3) -0.022(4) C40 0.044(4) 0.063(5) 0.053(5) 0.002(4) 0.006(3) -0.006(4) C41 0.048(5) 0.091(7) 0.112(7) -0.050(6) 0.021(5) -0.012(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 N1 C2 1.359(9) . ? N1 C9 1.387(9) . ? N1 C10 1.462(9) . ? C2 C3 1.374(9) . ? C3 C4 1.429(9) . ? C3 C11 1.508(9) . ? C4 C9 1.408(9) . ? C4 C5 1.409(9) . ? C5 C6 1.398(10) . ? C6 C7 1.390(11) . ? C7 C8 1.394(11) . ? C8 C9 1.393(10) . ? C11 C12 1.534(9) . ? C12 N13 1.473(8) . ? C12 C24 1.533(9) . ? N13 S14 1.594(6) . ? S14 O16 1.438(5) . ? S14 O15 1.447(5) . ? S14 C17' 1.732(12) . ? S14 C17 1.789(5) . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C20 C23 1.532(10) . ? C21 C22 1.3900 . ? C17' C18' 1.3900 . ? C17' C22' 1.3900 . ? C18' C19' 1.3900 . ? C19' C20' 1.3900 . ? C20' C21' 1.3900 . ? C20' C23' 1.533(19) . ? C21' C22' 1.3900 . ? C24 C29 1.543(9) . ? C24 C25 1.550(9) . ? C25 O26 1.412(8) . ? O26 C27 1.446(9) . ? C27 O30 1.380(8) . ? C27 C28 1.522(9) . ? C28 C29 1.524(9) . ? C29 S32 1.795(6) . ? O30 C31 1.416(9) . ? S32 O34 1.435(5) . ? S32 O33 1.439(5) . ? S32 C35 1.765(7) . ? C35 C36 1.358(10) . ? C35 C40 1.388(9) . ? C36 C37 1.390(10) . ? C37 C38 1.393(11) . ? C38 C39 1.371(11) . ? C38 C41 1.499(11) . ? C39 C40 1.394(10) . ? 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 C2 N1 C9 108.4(5) . . ? C2 N1 C10 126.9(6) . . ? C9 N1 C10 124.7(7) . . ? N1 C2 C3 111.0(6) . . ? C2 C3 C4 105.8(6) . . ? C2 C3 C11 126.6(6) . . ? C4 C3 C11 127.6(6) . . ? C9 C4 C5 118.9(7) . . ? C9 C4 C3 107.5(6) . . ? C5 C4 C3 133.6(6) . . ? C6 C5 C4 117.5(7) . . ? C7 C6 C5 122.2(7) . . ? C6 C7 C8 121.6(7) . . ? C9 C8 C7 116.0(7) . . ? N1 C9 C8 128.9(6) . . ? N1 C9 C4 107.3(6) . . ? C8 C9 C4 123.8(6) . . ? C3 C11 C12 114.4(6) . . ? N13 C12 C24 109.3(5) . . ? N13 C12 C11 110.9(5) . . ? C24 C12 C11 113.6(6) . . ? C12 N13 S14 123.6(4) . . ? O16 S14 O15 119.6(3) . . ? O16 S14 N13 107.3(3) . . ? O15 S14 N13 105.8(3) . . ? O16 S14 C17' 99.8(12) . . ? O15 S14 C17' 113.8(9) . . ? N13 S14 C17' 110.4(5) . . ? O16 S14 C17 108.8(4) . . ? O15 S14 C17 106.8(4) . . ? N13 S14 C17 108.1(3) . . ? C18 C17 C22 120.0 . . ? C18 C17 S14 120.3(5) . . ? C22 C17 S14 119.6(5) . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 C23 119.6(8) . . ? C21 C20 C23 120.4(8) . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? C18' C17' C22' 120.0 . . ? C18' C17' S14 118.5(19) . . ? C22' C17' S14 121.5(19) . . ? C19' C18' C17' 120.0 . . ? C18' C19' C20' 120.0 . . ? C21' C20' C19' 120.0 . . ? C21' C20' C23' 121(2) . . ? C19' C20' C23' 119(2) . . ? C20' C21' C22' 120.0 . . ? C21' C22' C17' 120.0 . . ? C12 C24 C29 118.5(5) . . ? C12 C24 C25 109.4(5) . . ? C29 C24 C25 107.8(5) . . ? O26 C25 C24 112.1(5) . . ? C25 O26 C27 109.7(5) . . ? O30 C27 O26 107.6(6) . . ? O30 C27 C28 107.6(5) . . ? O26 C27 C28 108.6(6) . . ? C27 C28 C29 111.0(5) . . ? C28 C29 C24 111.6(5) . . ? C28 C29 S32 109.2(4) . . ? C24 C29 S32 115.2(4) . . ? C27 O30 C31 112.0(6) . . ? O34 S32 O33 118.2(3) . . ? O34 S32 C35 108.4(3) . . ? O33 S32 C35 108.6(3) . . ? O34 S32 C29 107.2(3) . . ? O33 S32 C29 108.3(3) . . ? C35 S32 C29 105.3(3) . . ? C36 C35 C40 119.7(7) . . ? C36 C35 S32 120.6(6) . . ? C40 C35 S32 119.7(6) . . ? C35 C36 C37 120.6(7) . . ? C36 C37 C38 120.9(8) . . ? C39 C38 C37 117.6(8) . . ? C39 C38 C41 120.7(8) . . ? C37 C38 C41 121.7(9) . . ? C38 C39 C40 121.9(7) . . ? C35 C40 C39 119.3(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.267 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.067 #===END