Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'John Ripmeester' 'Gary D. Enright' 'Paul S. Sidhu' 'Konstantin A. Udachin' _publ_contact_author_name 'Prof John Ripmeester' _publ_contact_author_address ; Steacie Inst Mol Sci, National Res Council Canada 100 Sussex Dr Ottawa Ontario K1A 0R6 CANADA ; _publ_contact_author_email JOHN.RIPMEESTER@NRC-CNRC.GC.CA _publ_requested_journal 'Chemical Communications' _publ_section_title ; The first example of a crystalline guest-free form of the tris(5-acetyl-3-thienyl) methane (TATM) host material. ; data_Guest-free_TATM _database_code_depnum_ccdc_archive 'CCDC 255669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TATM _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 O6 S6' _chemical_formula_weight 777.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5004(12) _cell_length_b 12.5300(15) _cell_length_c 14.8353(17) _cell_angle_alpha 82.316(2) _cell_angle_beta 72.311(2) _cell_angle_gamma 88.529(2) _cell_volume 1842.7(4) _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 plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _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 16789 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6508 _reflns_number_gt 4116 _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^)+(0.1114P)^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 6508 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1793 _refine_ls_wR_factor_gt 0.1626 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _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 S2 S -0.13704(11) 0.90019(10) 0.07168(9) 0.0386(3) Uani 1 1 d . . . S1 S -0.16670(11) 0.97359(10) 0.48336(8) 0.0369(3) Uani 1 1 d . . . S3 S 0.46119(11) 1.01388(11) 0.11564(8) 0.0426(3) Uani 1 1 d . . . S3' S 0.02596(11) 0.47794(10) 0.88327(8) 0.0398(3) Uani 1 1 d . . . S2' S 0.61330(11) 0.38814(10) 0.96689(8) 0.0385(3) Uani 1 1 d . . . S1' S 0.66124(11) 0.45010(10) 0.54065(8) 0.0375(3) Uani 1 1 d . . . O2 O -0.0576(3) 0.7966(3) -0.1048(2) 0.0486(9) Uani 1 1 d . . . O1 O -0.2224(3) 1.2043(3) 0.4963(2) 0.0468(9) Uani 1 1 d . . . O3 O 0.6456(3) 1.0401(3) 0.2248(2) 0.0479(9) Uani 1 1 d . . . O3' O -0.1496(3) 0.4970(3) 0.7618(3) 0.0512(9) Uani 1 1 d . . . O2' O 0.5237(3) 0.3104(3) 1.1717(2) 0.0479(9) Uani 1 1 d . . . O1' O 0.7023(3) 0.6862(3) 0.4775(2) 0.0559(10) Uani 1 1 d . . . C17 C 0.3131(4) 0.9215(4) 0.2773(3) 0.0282(10) Uani 1 1 d . . . C8 C 0.0302(4) 0.8753(3) 0.1675(3) 0.0283(10) Uani 1 1 d . . . C17' C 0.1773(4) 0.3836(4) 0.7463(3) 0.0278(10) Uani 1 1 d . . . C2 C 0.0062(4) 0.9365(4) 0.3271(3) 0.0304(10) Uani 1 1 d . . . C11 C 0.0856(5) 0.8229(4) 0.0861(3) 0.0317(10) Uani 1 1 d . . . C2' C 0.4811(4) 0.4036(4) 0.7023(3) 0.0287(10) Uani 1 1 d . . . C16 C 0.4383(4) 0.9694(4) 0.2346(3) 0.0300(10) Uani 1 1 d . . . C14 C 0.2361(4) 0.9243(4) 0.2139(3) 0.0303(10) Uani 1 1 d . . . C5 C -0.0056(4) 1.0498(4) 0.3212(3) 0.0323(10) Uani 1 1 d . . . C5' C 0.4828(4) 0.5173(4) 0.6807(3) 0.0307(10) Uani 1 1 d . . . C4 C -0.0954(4) 1.0832(4) 0.4002(3) 0.0305(10) Uani 1 1 d . . . C18' C -0.0462(4) 0.4528(4) 0.7244(3) 0.0367(11) Uani 1 1 d . . . C8' C 0.4500(4) 0.3490(3) 0.8760(3) 0.0297(10) Uani 1 1 d . . . C1 C 0.0934(4) 0.8780(4) 0.2472(3) 0.0303(10) Uani 1 1 d . . . C1' C 0.3908(4) 0.3423(4) 0.7953(3) 0.0307(10) Uani 1 1 d . . . C14' C 0.2500(4) 0.3858(3) 0.8140(3) 0.0298(10) Uani 1 1 d . . . C3 C -0.0747(5) 0.8866(5) 0.4104(4) 0.0370(12) Uani 1 1 d . . . C10' C 0.4652(4) 0.3224(3) 1.0306(3) 0.0315(10) Uani 1 1 d . . . C18 C 0.5472(4) 0.9873(4) 0.2737(3) 0.0335(10) Uani 1 1 d . . . C15' C 0.1780(4) 0.4335(4) 0.8903(3) 0.0337(11) Uani 1 1 d . . . C12' C 0.4370(4) 0.2973(4) 1.1354(3) 0.0356(11) Uani 1 1 d . . . C10 C 0.0056(4) 0.8297(3) 0.0271(3) 0.0327(10) Uani 1 1 d . . . C15 C 0.3036(4) 0.9697(4) 0.1246(3) 0.0364(11) Uani 1 1 d . . . C9 C -0.0881(4) 0.9218(4) 0.1679(3) 0.0328(10) Uani 1 1 d . . . C3' C 0.5728(4) 0.3588(4) 0.6328(3) 0.0345(11) Uani 1 1 d . . . C9' C 0.5713(4) 0.3957(4) 0.8639(3) 0.0337(11) Uani 1 1 d . . . C16' C 0.0553(4) 0.4325(3) 0.7744(3) 0.0318(10) Uani 1 1 d . . . C4' C 0.5748(4) 0.5548(4) 0.5952(3) 0.0340(11) Uani 1 1 d . . . C11' C 0.3887(4) 0.3062(4) 0.9734(3) 0.0321(10) Uani 1 1 d . . . C6' C 0.6069(5) 0.6678(4) 0.5504(3) 0.0406(12) Uani 1 1 d . . . C12 C 0.0312(4) 0.7894(4) -0.0657(3) 0.0348(11) Uani 1 1 d . . . C19 C 0.5347(5) 0.9392(5) 0.3740(3) 0.0481(13) Uani 1 1 d . . . H19A H 0.5722 0.9895 0.4049 0.072 Uiso 1 1 calc R . . H19B H 0.5836 0.8715 0.3734 0.072 Uiso 1 1 calc R . . H19C H 0.4402 0.9251 0.4095 0.072 Uiso 1 1 calc R . . C13' C 0.2994(5) 0.2580(4) 1.1937(3) 0.0447(12) Uani 1 1 d . . . H13D H 0.3038 0.2134 1.2522 0.067 Uiso 1 1 calc R . . H13E H 0.2622 0.2152 1.1568 0.067 Uiso 1 1 calc R . . H13F H 0.2421 0.3198 1.2105 0.067 Uiso 1 1 calc R . . C19' C -0.0151(5) 0.4225(4) 0.6252(4) 0.0485(13) Uani 1 1 d . . . H19D H -0.0856 0.3743 0.6227 0.073 Uiso 1 1 calc R . . H19E H 0.0709 0.3858 0.6087 0.073 Uiso 1 1 calc R . . H19F H -0.0102 0.4877 0.5796 0.073 Uiso 1 1 calc R . . C13 C 0.1631(4) 0.7447(4) -0.1088(4) 0.0440(12) Uani 1 1 d . . . H13A H 0.1624 0.7133 -0.1658 0.066 Uiso 1 1 calc R . . H13B H 0.1837 0.6887 -0.0627 0.066 Uiso 1 1 calc R . . H13C H 0.2312 0.8022 -0.1268 0.066 Uiso 1 1 calc R . . C6 C -0.1361(4) 1.1902(4) 0.4225(3) 0.0384(11) Uani 1 1 d . . . C7' C 0.5174(5) 0.7532(4) 0.5925(3) 0.0471(13) Uani 1 1 d . . . H7D H 0.5579 0.8239 0.5631 0.071 Uiso 1 1 calc R . . H7E H 0.5041 0.7453 0.6614 0.071 Uiso 1 1 calc R . . H7F H 0.4310 0.7468 0.5810 0.071 Uiso 1 1 calc R . . C7 C -0.0652(6) 1.2852(4) 0.3526(4) 0.0596(16) Uani 1 1 d . . . H7A H -0.1213 1.3490 0.3620 0.089 Uiso 1 1 calc R . . H7B H -0.0487 1.2690 0.2872 0.089 Uiso 1 1 calc R . . H7C H 0.0201 1.2991 0.3633 0.089 Uiso 1 1 calc R . . H3' H 0.594(4) 0.284(4) 0.631(3) 0.029(12) Uiso 1 1 d . . . H5 H 0.034(4) 1.096(3) 0.267(3) 0.016(10) Uiso 1 1 d . . . H11 H 0.156(4) 0.787(3) 0.075(3) 0.011(10) Uiso 1 1 d . . . H5' H 0.423(4) 0.559(3) 0.716(3) 0.020(11) Uiso 1 1 d . . . H1 H 0.099(4) 0.806(4) 0.276(3) 0.031(12) Uiso 1 1 d . . . H9 H -0.145(3) 0.959(3) 0.212(3) 0.013(10) Uiso 1 1 d . . . H9' H 0.636(4) 0.428(3) 0.807(3) 0.031(11) Uiso 1 1 d . . . H17' H 0.208(5) 0.363(4) 0.699(3) 0.039(16) Uiso 1 1 d . . . H1' H 0.390(4) 0.258(4) 0.781(3) 0.034(12) Uiso 1 1 d . . . H17 H 0.280(4) 0.894(4) 0.335(3) 0.034(13) Uiso 1 1 d . . . H3 H -0.081(4) 0.829(4) 0.430(3) 0.026(14) Uiso 1 1 d . . . H15 H 0.269(5) 0.982(4) 0.070(4) 0.059(15) Uiso 1 1 d . . . H11' H 0.307(5) 0.275(4) 0.991(3) 0.037(13) Uiso 1 1 d . . . H15' H 0.196(5) 0.449(5) 0.940(4) 0.063(18) Uiso 1 1 d . . . 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 S2 0.0351(6) 0.0399(7) 0.0471(7) -0.0102(6) -0.0193(5) -0.0098(5) S1 0.0338(6) 0.0414(7) 0.0310(6) -0.0042(5) -0.0026(5) -0.0112(5) S3 0.0349(6) 0.0647(9) 0.0277(6) -0.0021(6) -0.0088(5) -0.0176(6) S3' 0.0361(6) 0.0480(8) 0.0359(7) -0.0123(6) -0.0085(5) -0.0049(5) S2' 0.0324(6) 0.0491(8) 0.0374(7) -0.0031(6) -0.0159(5) -0.0124(5) S1' 0.0319(6) 0.0491(8) 0.0307(6) -0.0123(5) -0.0048(5) -0.0102(5) O2 0.052(2) 0.062(2) 0.041(2) -0.0108(17) -0.0260(16) -0.0121(17) O1 0.053(2) 0.044(2) 0.037(2) -0.0121(16) -0.0018(16) 0.0006(16) O3 0.0300(17) 0.058(2) 0.054(2) -0.0026(18) -0.0116(15) -0.0130(16) O3' 0.0317(18) 0.057(2) 0.064(2) -0.0054(19) -0.0135(16) -0.0101(17) O2' 0.050(2) 0.065(2) 0.0360(19) -0.0110(17) -0.0221(16) -0.0121(18) O1' 0.060(2) 0.059(2) 0.038(2) -0.0024(18) 0.0008(17) -0.0299(18) C17 0.031(2) 0.032(3) 0.020(2) -0.0089(19) -0.0044(18) -0.0038(19) C8 0.026(2) 0.028(2) 0.030(2) -0.0064(19) -0.0066(17) -0.0094(18) C17' 0.029(2) 0.028(2) 0.027(3) -0.003(2) -0.0083(19) -0.0132(19) C2 0.027(2) 0.039(3) 0.029(2) -0.006(2) -0.0116(18) -0.0064(19) C11 0.033(2) 0.032(3) 0.034(3) -0.008(2) -0.013(2) -0.010(2) C2' 0.030(2) 0.034(3) 0.026(2) -0.0081(19) -0.0123(18) -0.0063(19) C16 0.027(2) 0.036(3) 0.030(2) -0.012(2) -0.0113(18) -0.0009(19) C14 0.033(2) 0.034(3) 0.027(2) -0.0112(19) -0.0098(18) -0.0050(19) C5 0.034(2) 0.038(3) 0.027(2) -0.004(2) -0.0112(19) -0.012(2) C5' 0.029(2) 0.040(3) 0.024(2) -0.010(2) -0.0075(18) -0.006(2) C4 0.025(2) 0.037(3) 0.028(2) -0.003(2) -0.0055(18) -0.0086(18) C18' 0.032(2) 0.033(3) 0.045(3) 0.001(2) -0.012(2) -0.019(2) C8' 0.032(2) 0.029(2) 0.030(2) -0.0041(19) -0.0123(18) -0.0086(19) C1 0.033(2) 0.033(3) 0.028(2) -0.008(2) -0.0115(18) -0.009(2) C1' 0.034(2) 0.031(3) 0.027(2) -0.0048(19) -0.0083(18) -0.0060(19) C14' 0.032(2) 0.032(2) 0.027(2) -0.0012(19) -0.0099(18) -0.0170(19) C3 0.036(3) 0.034(3) 0.038(3) 0.000(2) -0.008(2) -0.013(2) C10' 0.032(2) 0.031(2) 0.035(3) -0.0052(19) -0.0129(19) -0.0082(19) C18 0.029(2) 0.040(3) 0.034(3) -0.014(2) -0.0097(19) 0.000(2) C15' 0.035(2) 0.037(3) 0.028(3) -0.009(2) -0.006(2) -0.005(2) C12' 0.042(3) 0.040(3) 0.030(2) -0.007(2) -0.016(2) -0.005(2) C10 0.037(2) 0.030(2) 0.036(3) -0.003(2) -0.0175(19) -0.0126(19) C15 0.036(2) 0.051(3) 0.026(2) -0.006(2) -0.013(2) -0.014(2) C9 0.032(2) 0.034(3) 0.037(3) -0.011(2) -0.013(2) -0.010(2) C3' 0.036(2) 0.031(3) 0.039(3) -0.011(2) -0.011(2) -0.005(2) C9' 0.028(2) 0.048(3) 0.027(2) -0.003(2) -0.0111(19) -0.009(2) C16' 0.034(2) 0.027(2) 0.032(2) -0.0004(19) -0.0079(19) -0.0119(19) C4' 0.032(2) 0.047(3) 0.025(2) -0.004(2) -0.0115(18) -0.013(2) C11' 0.030(2) 0.036(3) 0.031(3) -0.004(2) -0.0100(19) -0.007(2) C6' 0.045(3) 0.050(3) 0.029(3) -0.003(2) -0.015(2) -0.020(2) C12 0.043(3) 0.031(3) 0.032(2) 0.003(2) -0.015(2) -0.018(2) C19 0.044(3) 0.066(4) 0.045(3) -0.015(3) -0.024(2) -0.012(3) C13' 0.044(3) 0.057(3) 0.032(3) -0.004(2) -0.010(2) -0.008(2) C19' 0.051(3) 0.058(3) 0.043(3) -0.006(3) -0.023(2) -0.012(3) C13 0.044(3) 0.049(3) 0.043(3) -0.018(2) -0.014(2) -0.010(2) C6 0.040(3) 0.042(3) 0.032(3) -0.010(2) -0.007(2) -0.007(2) C7' 0.062(3) 0.043(3) 0.037(3) 0.004(2) -0.018(2) -0.012(3) C7 0.074(4) 0.040(3) 0.050(3) -0.008(3) 0.006(3) -0.015(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 S2 C9 1.712(5) . ? S2 C10 1.717(5) . ? S1 C3 1.709(5) . ? S1 C4 1.734(4) . ? S3 C15 1.719(4) . ? S3 C16 1.724(4) . ? S3' C15' 1.706(5) . ? S3' C16' 1.721(5) . ? S2' C9' 1.705(5) . ? S2' C10' 1.718(4) . ? S1' C3' 1.704(5) . ? S1' C4' 1.726(5) . ? O2 C12 1.234(5) . ? O1 C6 1.221(5) . ? O3 C18 1.218(5) . ? O3' C18' 1.216(5) . ? O2' C12' 1.215(5) . ? O1' C6' 1.230(5) . ? C17 C16 1.386(6) . ? C17 C14 1.411(6) . ? C8 C9 1.358(6) . ? C8 C11 1.412(6) . ? C8 C1 1.526(6) . ? C17' C16' 1.376(6) . ? C17' C14' 1.437(6) . ? C2 C3 1.350(6) . ? C2 C5 1.415(6) . ? C2 C1 1.523(6) . ? C11 C10 1.379(6) . ? C2' C3' 1.353(6) . ? C2' C5' 1.416(6) . ? C2' C1' 1.534(6) . ? C16 C18 1.465(6) . ? C14 C15 1.353(6) . ? C14 C1 1.531(6) . ? C5 C4 1.370(6) . ? C5' C4' 1.373(6) . ? C4 C6 1.447(6) . ? C18' C16' 1.471(6) . ? C18' C19' 1.506(7) . ? C8' C9' 1.368(6) . ? C8' C11' 1.426(6) . ? C8' C1' 1.520(6) . ? C1' C14' 1.519(6) . ? C14' C15' 1.360(6) . ? C10' C11' 1.370(6) . ? C10' C12' 1.482(6) . ? C18 C19 1.497(6) . ? C12' C13' 1.497(6) . ? C10 C12 1.475(6) . ? C4' C6' 1.482(7) . ? C6' C7' 1.479(7) . ? C12 C13 1.470(6) . ? C6 C7 1.514(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 S2 C10 91.2(2) . . ? C3 S1 C4 91.0(2) . . ? C15 S3 C16 91.3(2) . . ? C15' S3' C16' 90.9(2) . . ? C9' S2' C10' 91.1(2) . . ? C3' S1' C4' 90.9(2) . . ? C16 C17 C14 112.8(4) . . ? C9 C8 C11 112.1(4) . . ? C9 C8 C1 123.5(4) . . ? C11 C8 C1 124.5(4) . . ? C16' C17' C14' 112.1(4) . . ? C3 C2 C5 111.6(4) . . ? C3 C2 C1 124.1(4) . . ? C5 C2 C1 124.2(4) . . ? C10 C11 C8 112.5(4) . . ? C3' C2' C5' 111.1(4) . . ? C3' C2' C1' 125.5(4) . . ? C5' C2' C1' 123.3(4) . . ? C17 C16 C18 131.1(4) . . ? C17 C16 S3 110.8(3) . . ? C18 C16 S3 118.0(3) . . ? C15 C14 C17 112.3(4) . . ? C15 C14 C1 126.4(4) . . ? C17 C14 C1 121.2(4) . . ? C4 C5 C2 113.4(4) . . ? C4' C5' C2' 113.2(4) . . ? C5 C4 C6 130.8(4) . . ? C5 C4 S1 110.7(3) . . ? C6 C4 S1 118.6(3) . . ? O3' C18' C16' 119.9(4) . . ? O3' C18' C19' 121.7(4) . . ? C16' C18' C19' 118.3(4) . . ? C9' C8' C11' 111.0(4) . . ? C9' C8' C1' 123.9(4) . . ? C11' C8' C1' 125.0(4) . . ? C2 C1 C8 111.7(3) . . ? C2 C1 C14 110.0(3) . . ? C8 C1 C14 114.5(3) . . ? C14' C1' C8' 113.7(3) . . ? C14' C1' C2' 108.9(3) . . ? C8' C1' C2' 109.9(3) . . ? C15' C14' C17' 111.0(4) . . ? C15' C14' C1' 127.5(4) . . ? C17' C14' C1' 121.4(4) . . ? C2 C3 S1 113.3(4) . . ? C11' C10' C12' 130.5(4) . . ? C11' C10' S2' 111.9(3) . . ? C12' C10' S2' 117.5(3) . . ? O3 C18 C16 120.1(4) . . ? O3 C18 C19 121.3(4) . . ? C16 C18 C19 118.6(4) . . ? C14' C15' S3' 113.9(4) . . ? O2' C12' C10' 120.0(4) . . ? O2' C12' C13' 121.9(4) . . ? C10' C12' C13' 118.1(4) . . ? C11 C10 C12 128.7(4) . . ? C11 C10 S2 111.4(4) . . ? C12 C10 S2 119.8(3) . . ? C14 C15 S3 112.7(3) . . ? C8 C9 S2 112.8(4) . . ? C2' C3' S1' 113.8(4) . . ? C8' C9' S2' 113.4(3) . . ? C17' C16' C18' 129.7(4) . . ? C17' C16' S3' 112.0(3) . . ? C18' C16' S3' 118.2(3) . . ? C5' C4' C6' 128.6(4) . . ? C5' C4' S1' 111.0(4) . . ? C6' C4' S1' 120.4(3) . . ? C10' C11' C8' 112.6(4) . . ? O1' C6' C7' 122.8(4) . . ? O1' C6' C4' 119.0(5) . . ? C7' C6' C4' 118.1(4) . . ? O2 C12 C13 122.7(4) . . ? O2 C12 C10 118.9(4) . . ? C13 C12 C10 118.3(4) . . ? O1 C6 C4 121.6(4) . . ? O1 C6 C7 120.5(4) . . ? C4 C6 C7 117.9(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.863 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.109 #===END data_Depleted_MeOH/TATM _database_code_depnum_ccdc_archive 'CCDC 255670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TATM _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19.05 H16.20 O3.05 S3' _chemical_formula_weight 388.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9681(8) _cell_length_b 10.7633(11) _cell_length_c 11.9587(12) _cell_angle_alpha 95.793(2) _cell_angle_beta 106.221(2) _cell_angle_gamma 95.522(2) _cell_volume 971.41(17) _cell_formula_units_Z 2 _cell_measurement_temperature 125(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 398(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 9563 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 29.58 _reflns_number_total 5279 _reflns_number_gt 3844 _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^)+(0.0709P)^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 5279 _refine_ls_number_parameters 271 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 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 -0.41087(6) 0.80633(4) -0.00282(4) 0.03319(11) Uani 1 1 d . . . S2 S -0.24324(5) 0.54190(3) 0.49291(4) 0.02481(9) Uani 1 1 d . . . S3 S 0.42250(5) 0.82784(4) 0.34162(4) 0.02630(9) Uani 1 1 d . . . O1 O -0.47566(19) 0.57393(12) -0.17151(11) 0.0443(4) Uani 1 1 d . . . O2 O -0.05957(16) 0.53856(11) 0.74682(11) 0.0345(3) Uani 1 1 d . . . O3 O 0.64730(15) 1.06595(11) 0.35190(11) 0.0331(3) Uani 1 1 d . . . C1 C -0.09108(19) 0.82537(14) 0.32795(13) 0.0215(3) Uani 1 1 d . . . C2 C -0.19995(19) 0.79096(14) 0.20078(13) 0.0229(3) Uani 1 1 d . . . C3 C -0.3072(2) 0.86903(16) 0.14022(14) 0.0274(4) Uani 1 1 d . . . C4 C -0.3117(2) 0.67096(15) 0.01569(14) 0.0259(4) Uani 1 1 d . . . C5 C -0.2019(2) 0.67692(15) 0.12826(14) 0.0244(3) Uani 1 1 d . . . C6 C -0.3606(2) 0.56622(16) -0.08126(14) 0.0308(4) Uani 1 1 d . . . C7 C -0.2688(2) 0.45260(16) -0.06595(15) 0.0340(4) Uani 1 1 d . . . H7A H -0.3454 0.3804 -0.1129 0.051 Uiso 1 1 calc R . . H7B H -0.2377 0.4400 0.0153 0.051 Uiso 1 1 calc R . . H7C H -0.1639 0.4641 -0.0903 0.051 Uiso 1 1 calc R . . C8 C -0.12054(19) 0.72841(14) 0.40725(13) 0.0214(3) Uani 1 1 d . . . C9 C -0.2454(2) 0.62393(14) 0.37723(14) 0.0235(3) Uani 1 1 d . . . C10 C -0.07275(19) 0.64808(13) 0.58593(13) 0.0218(3) Uani 1 1 d . . . C11 C -0.02145(19) 0.74124(13) 0.52736(13) 0.0212(3) Uani 1 1 d . . . C12 C -0.0038(2) 0.63025(15) 0.70898(14) 0.0269(4) Uani 1 1 d . . . C13 C 0.1381(3) 0.7285(2) 0.78867(17) 0.0456(5) Uani 1 1 d . . . H13A H 0.1225 0.7381 0.8657 0.068 Uiso 1 1 calc R . . H13C H 0.1307 0.8073 0.7577 0.068 Uiso 1 1 calc R . . H13B H 0.2516 0.7026 0.7934 0.068 Uiso 1 1 calc R . . C14 C 0.10325(19) 0.85350(13) 0.33620(13) 0.0203(3) Uani 1 1 d . . . C15 C 0.2149(2) 0.76460(14) 0.33716(14) 0.0245(3) Uani 1 1 d . . . C16 C 0.3633(2) 0.97737(13) 0.34315(13) 0.0221(3) Uani 1 1 d . . . C17 C 0.1897(2) 0.97628(14) 0.34041(13) 0.0220(3) Uani 1 1 d . . . C18 C 0.4966(2) 1.08393(14) 0.34870(14) 0.0254(3) Uani 1 1 d . . . C19 C 0.4413(2) 1.21320(15) 0.34752(18) 0.0366(4) Uani 1 1 d . . . H19A H 0.5437 1.2748 0.3650 0.055 Uiso 1 1 calc R . . H19C H 0.3805 1.2278 0.4056 0.055 Uiso 1 1 calc R . . H19B H 0.3644 1.2197 0.2713 0.055 Uiso 1 1 calc R . . H1 H -0.127(2) 0.9041(16) 0.3572(14) 0.023(4) Uiso 1 1 d . . . H3 H -0.325(2) 0.9460(18) 0.1667(16) 0.031(5) Uiso 1 1 d . . . H5 H -0.138(2) 0.6145(16) 0.1510(14) 0.016(4) Uiso 1 1 d . . . H9 H -0.323(2) 0.5945(17) 0.3073(15) 0.028(5) Uiso 1 1 d . . . H11 H 0.074(2) 0.8073(16) 0.5617(15) 0.025(4) Uiso 1 1 d . . . H15 H 0.193(2) 0.6750(17) 0.3331(15) 0.027(5) Uiso 1 1 d . . . H17 H 0.135(2) 1.0400(15) 0.3422(13) 0.013(4) Uiso 1 1 d . . . C001 C 0.162(2) 0.915(3) 0.066(12) 0.100 Uiso 0.025(3) 1 d PD A -1 O001 O 0.028(6) 0.991(5) 0.035(8) 0.100 Uiso 0.025(3) 1 d PD A -1 O002 O -0.025(3) 0.855(6) -0.052(5) 0.100 Uiso 0.027(4) 1 d PD B -2 C002 C 0.133(7) 0.906(12) 0.033(8) 0.100 Uiso 0.027(4) 1 d PD B -2 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 0.0335(2) 0.0318(2) 0.0254(2) 0.00436(16) -0.00443(16) -0.00044(17) S2 0.02360(17) 0.01932(16) 0.02879(19) -0.00108(14) 0.00721(14) -0.00454(14) S3 0.02063(17) 0.02138(17) 0.0362(2) 0.00175(15) 0.00852(15) 0.00078(14) O1 0.0525(8) 0.0372(7) 0.0266(7) 0.0005(5) -0.0083(6) -0.0105(6) O2 0.0402(7) 0.0284(6) 0.0346(6) 0.0089(5) 0.0111(5) -0.0022(5) O3 0.0256(6) 0.0305(6) 0.0402(7) -0.0037(5) 0.0108(5) -0.0060(5) C1 0.0194(7) 0.0205(6) 0.0218(7) 0.0006(5) 0.0030(5) 0.0002(5) C2 0.0176(6) 0.0259(7) 0.0228(7) 0.0016(6) 0.0044(5) -0.0022(6) C3 0.0256(7) 0.0286(7) 0.0237(8) 0.0024(6) 0.0017(6) 0.0013(6) C4 0.0246(7) 0.0261(7) 0.0236(7) 0.0031(6) 0.0044(6) -0.0046(6) C5 0.0214(7) 0.0262(7) 0.0222(7) 0.0025(6) 0.0027(6) -0.0026(6) C6 0.0362(8) 0.0291(8) 0.0225(8) 0.0028(6) 0.0065(7) -0.0117(7) C7 0.0405(9) 0.0337(8) 0.0250(8) -0.0023(7) 0.0107(7) -0.0051(7) C8 0.0179(6) 0.0208(6) 0.0236(7) -0.0001(5) 0.0049(5) -0.0002(5) C9 0.0212(7) 0.0230(7) 0.0226(7) -0.0015(6) 0.0036(6) -0.0028(6) C10 0.0191(6) 0.0193(6) 0.0256(7) 0.0014(5) 0.0056(6) -0.0004(5) C11 0.0170(6) 0.0198(6) 0.0244(7) -0.0015(5) 0.0049(5) -0.0015(5) C12 0.0247(7) 0.0264(7) 0.0299(8) 0.0070(6) 0.0078(6) 0.0021(6) C13 0.0436(11) 0.0498(11) 0.0299(10) 0.0132(8) -0.0065(8) -0.0171(9) C14 0.0195(6) 0.0194(6) 0.0187(7) 0.0002(5) 0.0025(5) -0.0024(5) C15 0.0217(7) 0.0190(6) 0.0301(8) 0.0007(6) 0.0057(6) -0.0024(6) C16 0.0236(7) 0.0177(6) 0.0230(7) 0.0000(5) 0.0054(6) -0.0003(5) C17 0.0226(7) 0.0184(6) 0.0236(7) 0.0013(5) 0.0056(6) 0.0012(5) C18 0.0270(7) 0.0225(7) 0.0246(7) -0.0022(6) 0.0081(6) -0.0026(6) C19 0.0395(9) 0.0203(7) 0.0512(11) 0.0021(7) 0.0184(8) -0.0036(7) _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 C3 1.7129(16) . ? S1 C4 1.7280(17) . ? S2 C9 1.7116(17) . ? S2 C10 1.7290(14) . ? S3 C15 1.7117(16) . ? S3 C16 1.7199(15) . ? O1 C6 1.222(2) . ? O2 C12 1.222(2) . ? O3 C18 1.225(2) . ? C1 C2 1.513(2) . ? C1 C8 1.523(2) . ? C1 C14 1.522(2) . ? C2 C3 1.370(2) . ? C2 C5 1.426(2) . ? C4 C5 1.377(2) . ? C4 C6 1.472(2) . ? C6 C7 1.485(3) . ? C8 C9 1.374(2) . ? C8 C11 1.418(2) . ? C10 C11 1.373(2) . ? C10 C12 1.459(2) . ? C12 C13 1.506(2) . ? C14 C15 1.367(2) . ? C14 C17 1.420(2) . ? C16 C17 1.373(2) . ? C16 C18 1.470(2) . ? C18 C19 1.500(2) . ? C001 O001 1.400(10) . ? O002 C002 1.400(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 C3 S1 C4 91.54(8) . . ? C9 S2 C10 91.47(7) . . ? C15 S3 C16 91.54(7) . . ? C2 C1 C8 114.13(12) . . ? C2 C1 C14 110.14(13) . . ? C8 C1 C14 111.40(12) . . ? C3 C2 C5 111.51(14) . . ? C3 C2 C1 123.19(14) . . ? C5 C2 C1 125.28(14) . . ? C2 C3 S1 112.80(12) . . ? C5 C4 C6 129.40(15) . . ? C5 C4 S1 111.16(12) . . ? C6 C4 S1 119.28(12) . . ? C4 C5 C2 112.97(14) . . ? O1 C6 C4 119.72(17) . . ? O1 C6 C7 121.60(15) . . ? C4 C6 C7 118.68(14) . . ? C9 C8 C11 111.42(14) . . ? C9 C8 C1 126.72(13) . . ? C11 C8 C1 121.79(12) . . ? C8 C9 S2 112.71(11) . . ? C11 C10 C12 129.21(13) . . ? C11 C10 S2 111.05(11) . . ? C12 C10 S2 119.74(11) . . ? C10 C11 C8 113.34(13) . . ? O2 C12 C10 121.18(14) . . ? O2 C12 C13 120.70(15) . . ? C10 C12 C13 118.12(15) . . ? C15 C14 C17 111.54(13) . . ? C15 C14 C1 124.73(13) . . ? C17 C14 C1 123.70(13) . . ? C14 C15 S3 112.65(11) . . ? C17 C16 C18 129.81(14) . . ? C17 C16 S3 111.22(11) . . ? C18 C16 S3 118.96(12) . . ? C16 C17 C14 113.04(14) . . ? O3 C18 C16 120.24(14) . . ? O3 C18 C19 121.65(15) . . ? C16 C18 C19 118.10(14) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.505 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.072 #===END data_MeOH/TATM _database_code_depnum_ccdc_archive 'CCDC 255671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TATM _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19.50 H18 O3.50 S3' _chemical_formula_weight 404.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1244(4) _cell_length_b 10.4462(5) _cell_length_c 12.2124(6) _cell_angle_alpha 94.5970(10) _cell_angle_beta 108.3720(10) _cell_angle_gamma 94.4360(10) _cell_volume 974.68(8) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 0.399 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 12189 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.59 _reflns_number_total 5351 _reflns_number_gt 4426 _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^)+(0.0758P)^2^+0.0462P] 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 5351 _refine_ls_number_parameters 314 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.005 _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 -0.43116(4) 0.30663(3) 0.49904(2) 0.03438(7) Uani 1 1 d . . . S2 S -0.23905(3) 0.04573(2) 0.98772(2) 0.02466(5) Uani 1 1 d . . . S3 S 0.42023(3) 0.32203(2) 0.84414(2) 0.02830(6) Uani 1 1 d . . . O1 O -0.48901(13) 0.07028(9) 0.33594(7) 0.0463(3) Uani 1 1 d . . . O2 O -0.06698(10) 0.04510(8) 1.24223(7) 0.03429(19) Uani 1 1 d . . . O3 O 0.64428(9) 0.56260(8) 0.85470(7) 0.03497(19) Uani 1 1 d . . . C1 C -0.08612(11) 0.33140(9) 0.82278(8) 0.0216(2) Uani 1 1 d . . . C2 C -0.19959(12) 0.29620(10) 0.69736(8) 0.0230(2) Uani 1 1 d . . . C3 C -0.31997(13) 0.37237(11) 0.63794(9) 0.0286(2) Uani 1 1 d . . . C4 C -0.31623(13) 0.17320(10) 0.51736(8) 0.0265(2) Uani 1 1 d . . . C5 C -0.19675(12) 0.18154(10) 0.62676(8) 0.0248(2) Uani 1 1 d . . . C6 C -0.36381(14) 0.06623(11) 0.42288(9) 0.0316(2) Uani 1 1 d . . . C7 C -0.25755(17) -0.04499(12) 0.43574(10) 0.0375(3) Uani 1 1 d . . . C8 C -0.11514(11) 0.23338(9) 0.90210(8) 0.0216(2) Uani 1 1 d . . . C9 C -0.23816(12) 0.12766(10) 0.87192(8) 0.0242(2) Uani 1 1 d . . . C10 C -0.07163(11) 0.15295(9) 1.08053(8) 0.0221(2) Uani 1 1 d . . . C11 C -0.01902(11) 0.24695(9) 1.02270(8) 0.0216(2) Uani 1 1 d . . . C12 C -0.00580(13) 0.13544(10) 1.20420(8) 0.0253(2) Uani 1 1 d . . . C13 C 0.13934(16) 0.23075(13) 1.28275(10) 0.0393(3) Uani 1 1 d . . . C14 C 0.10524(11) 0.35561(9) 0.83254(8) 0.0211(2) Uani 1 1 d . . . C15 C 0.21548(12) 0.26134(10) 0.83661(9) 0.0260(2) Uani 1 1 d . . . C16 C 0.36355(12) 0.47713(9) 0.84193(8) 0.0236(2) Uani 1 1 d . . . C17 C 0.19118(12) 0.48010(10) 0.83581(8) 0.0234(2) Uani 1 1 d . . . C18 C 0.49514(13) 0.58393(10) 0.84728(9) 0.0279(2) Uani 1 1 d . . . C19 C 0.44074(16) 0.71782(11) 0.84077(12) 0.0398(3) Uani 1 1 d . . . H1 H -0.1182(15) 0.4109(12) 0.8469(10) 0.025(3) Uiso 1 1 d . . . H3 H -0.3429(18) 0.4489(14) 0.6688(11) 0.039(4) Uiso 1 1 d . . . H4 H 0.1394(15) 0.5516(12) 0.8371(10) 0.022(3) Uiso 1 1 d . . . H5 H -0.1302(17) 0.1169(14) 0.6502(11) 0.038(4) Uiso 1 1 d . . . H9 H -0.3185(18) 0.0976(14) 0.7999(12) 0.043(4) Uiso 1 1 d . . . H11 H 0.0705(16) 0.3150(12) 1.0537(11) 0.030(3) Uiso 1 1 d . . . H15 H 0.1897(16) 0.1709(13) 0.8370(11) 0.033(3) Uiso 1 1 d . . . H7A H -0.175(2) -0.0360(18) 0.3999(16) 0.080(6) Uiso 1 1 d . . . H13A H 0.151(2) 0.3073(19) 1.2600(15) 0.074(6) Uiso 1 1 d . . . H19A H 0.535(2) 0.7765(16) 0.8506(14) 0.065(5) Uiso 1 1 d . . . H7B H -0.209(2) -0.0619(19) 0.5099(17) 0.082(6) Uiso 1 1 d . . . H13B H 0.137(2) 0.2378(17) 1.3602(15) 0.068(5) Uiso 1 1 d . . . H19B H 0.390(2) 0.7409(15) 0.8947(13) 0.054(4) Uiso 1 1 d . . . H7C H -0.331(2) -0.1256(18) 0.3928(15) 0.071(5) Uiso 1 1 d . . . H13C H 0.239(3) 0.1928(19) 1.3020(17) 0.080(6) Uiso 1 1 d . . . H19C H 0.370(2) 0.7236(18) 0.7655(16) 0.071(5) Uiso 1 1 d . . . O01 O 0.9585(6) 0.5285(5) 0.4875(5) 0.0983(17) Uani 0.315(2) 1 d PD A -1 H01 H 0.9466 0.4826 0.5385 0.148 Uiso 0.315(2) 1 calc PR A -1 C01 C 0.8202(7) 0.6076(6) 0.4576(5) 0.105(3) Uani 0.315(2) 1 d PD A -1 H01A H 0.7514 0.5989 0.5101 0.158 Uiso 0.315(2) 1 calc PR A -1 H01B H 0.7452 0.5806 0.3775 0.158 Uiso 0.315(2) 1 calc PR A -1 H01C H 0.8684 0.6979 0.4644 0.158 Uiso 0.315(2) 1 calc PR A -1 O02 O 1.0466(7) 0.6024(6) 0.5501(7) 0.0983(17) Uani 0.185(2) 1 d PRD A -2 H02 H 1.0215 0.5441 0.5875 0.148 Uiso 0.185(2) 1 calc PR A -2 C02 C 0.8972(14) 0.6205(15) 0.4582(9) 0.105(3) Uani 0.185(2) 1 d PD A -2 H02A H 0.7929 0.5823 0.4725 0.158 Uiso 0.185(2) 1 calc PR A -2 H02B H 0.9041 0.5787 0.3852 0.158 Uiso 0.185(2) 1 calc PR A -2 H02C H 0.8904 0.7132 0.4528 0.158 Uiso 0.185(2) 1 calc PR A -2 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 0.03129(12) 0.03630(14) 0.02590(12) 0.00267(10) -0.00392(10) 0.00251(11) S2 0.02396(10) 0.02114(11) 0.02710(10) -0.00237(8) 0.00839(8) -0.00373(9) S3 0.02142(9) 0.02436(11) 0.03901(12) 0.00028(9) 0.01046(9) 0.00225(9) O1 0.0505(5) 0.0420(5) 0.0291(4) -0.0030(4) -0.0068(4) -0.0089(4) O2 0.0418(4) 0.0306(4) 0.0303(3) 0.0050(3) 0.0126(3) -0.0025(3) O3 0.0251(3) 0.0347(4) 0.0439(4) -0.0073(3) 0.0144(3) -0.0060(3) C1 0.0182(3) 0.0229(4) 0.0214(4) -0.0009(3) 0.0042(3) 0.0006(3) C2 0.0189(4) 0.0268(4) 0.0212(4) 0.0016(3) 0.0047(3) -0.0015(3) C3 0.0249(4) 0.0303(5) 0.0259(4) 0.0009(4) 0.0021(4) 0.0026(4) C4 0.0261(4) 0.0268(5) 0.0231(4) 0.0010(3) 0.0051(3) -0.0038(4) C5 0.0226(4) 0.0277(5) 0.0215(4) 0.0014(3) 0.0048(3) -0.0011(4) C6 0.0362(5) 0.0314(5) 0.0226(4) 0.0005(4) 0.0072(4) -0.0107(4) C7 0.0477(6) 0.0357(6) 0.0269(5) -0.0027(4) 0.0120(4) -0.0027(5) C8 0.0173(3) 0.0232(4) 0.0228(4) -0.0011(3) 0.0054(3) 0.0014(3) C9 0.0217(4) 0.0263(4) 0.0215(4) -0.0032(3) 0.0047(3) -0.0008(3) C10 0.0200(4) 0.0217(4) 0.0232(4) -0.0014(3) 0.0064(3) 0.0009(3) C11 0.0185(3) 0.0212(4) 0.0226(4) -0.0025(3) 0.0048(3) -0.0004(3) C12 0.0257(4) 0.0244(4) 0.0252(4) 0.0026(3) 0.0073(3) 0.0034(4) C13 0.0386(6) 0.0436(6) 0.0251(5) 0.0071(5) -0.0019(4) -0.0109(5) C14 0.0196(4) 0.0217(4) 0.0197(4) -0.0014(3) 0.0043(3) 0.0002(3) C15 0.0219(4) 0.0223(4) 0.0326(4) 0.0004(4) 0.0084(3) -0.0004(3) C16 0.0220(4) 0.0216(4) 0.0255(4) -0.0024(3) 0.0070(3) -0.0001(3) C17 0.0215(4) 0.0223(4) 0.0242(4) -0.0008(3) 0.0059(3) -0.0002(3) C18 0.0275(4) 0.0266(5) 0.0280(4) -0.0056(4) 0.0104(3) -0.0047(4) C19 0.0417(5) 0.0241(5) 0.0570(6) -0.0010(5) 0.0240(5) -0.0044(5) O01 0.090(3) 0.117(4) 0.099(3) 0.002(3) 0.051(2) -0.005(3) C01 0.152(6) 0.107(4) 0.082(3) 0.009(3) 0.067(4) 0.038(5) O02 0.090(3) 0.117(4) 0.099(3) 0.002(3) 0.051(2) -0.005(3) C02 0.152(6) 0.107(4) 0.082(3) 0.009(3) 0.067(4) 0.038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C3 1.7078(10) . ? S1 C4 1.7275(11) . ? S2 C9 1.7123(11) . ? S2 C10 1.7258(9) . ? S3 C15 1.7055(10) . ? S3 C16 1.7182(10) . ? O1 C6 1.2234(13) . ? O2 C12 1.2233(13) . ? O3 C18 1.2255(13) . ? C1 C2 1.5160(12) . ? C1 C8 1.5191(14) . ? C1 C14 1.5208(13) . ? C2 C3 1.3718(14) . ? C2 C5 1.4247(14) . ? C4 C5 1.3732(12) . ? C4 C6 1.4747(14) . ? C6 C7 1.4896(18) . ? C8 C9 1.3735(13) . ? C8 C11 1.4225(12) . ? C10 C11 1.3720(14) . ? C10 C12 1.4665(13) . ? C12 C13 1.5014(14) . ? C14 C15 1.3749(14) . ? C14 C17 1.4191(14) . ? C16 C17 1.3817(14) . ? C16 C18 1.4668(14) . ? C18 C19 1.4997(16) . ? O01 C01 1.419(6) . ? O02 C02 1.407(8) . ? 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 C3 S1 C4 91.40(5) . . ? C9 S2 C10 91.40(5) . . ? C15 S3 C16 91.75(5) . . ? C2 C1 C8 112.98(8) . . ? C2 C1 C14 111.01(8) . . ? C8 C1 C14 111.80(7) . . ? C3 C2 C5 111.52(8) . . ? C3 C2 C1 123.33(9) . . ? C5 C2 C1 125.14(8) . . ? C2 C3 S1 112.87(8) . . ? C5 C4 C6 129.36(10) . . ? C5 C4 S1 111.47(8) . . ? C6 C4 S1 119.01(7) . . ? C4 C5 C2 112.73(9) . . ? O1 C6 C4 119.70(11) . . ? O1 C6 C7 121.36(10) . . ? C4 C6 C7 118.94(9) . . ? C9 C8 C11 111.40(9) . . ? C9 C8 C1 126.58(8) . . ? C11 C8 C1 121.93(8) . . ? C8 C9 S2 112.74(7) . . ? C11 C10 C12 128.99(8) . . ? C11 C10 S2 111.42(7) . . ? C12 C10 S2 119.59(7) . . ? C10 C11 C8 113.04(8) . . ? O2 C12 C10 120.84(9) . . ? O2 C12 C13 120.88(9) . . ? C10 C12 C13 118.28(9) . . ? C15 C14 C17 111.48(9) . . ? C15 C14 C1 125.04(9) . . ? C17 C14 C1 123.47(8) . . ? C14 C15 S3 112.72(7) . . ? C17 C16 C18 129.48(9) . . ? C17 C16 S3 111.26(7) . . ? C18 C16 S3 119.26(7) . . ? C16 C17 C14 112.79(9) . . ? O3 C18 C16 120.19(10) . . ? O3 C18 C19 121.55(10) . . ? C16 C18 C19 118.24(9) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 29.59 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.488 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.069 #===END data_EtOH/TATM _database_code_depnum_ccdc_archive 'CCDC 255672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TATM _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 O7 S6' _chemical_formula_weight 823.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2585(4) _cell_length_b 10.3109(4) _cell_length_c 12.4012(5) _cell_angle_alpha 82.7280(10) _cell_angle_beta 70.5960(10) _cell_angle_gamma 85.7780(10) _cell_volume 987.44(7) _cell_formula_units_Z 1 _cell_measurement_temperature 398(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 430 _exptl_absorpt_coefficient_mu 0.395 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 398(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 12423 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 29.59 _reflns_number_total 5450 _reflns_number_gt 4572 _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^)+(0.0636P)^2^+0.1805P] 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 5450 _refine_ls_number_parameters 322 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.94234(4) 0.29984(3) 0.49814(2) 0.03934(6) Uani 1 1 d . . . S2 S 1.22556(3) 0.04905(2) 0.015850(19) 0.02744(5) Uani 1 1 d . . . S3 S 0.43099(3) 0.32108(2) 0.15543(2) 0.03258(6) Uani 1 1 d . . . O1 O 0.82411(12) 0.06410(9) 0.66066(7) 0.0515(2) Uani 1 1 d . . . O2 O 1.30579(10) 0.04667(7) -0.23645(6) 0.03737(18) Uani 1 1 d . . . O3 O 0.21757(9) 0.56221(8) 0.14620(7) 0.03985(19) Uani 1 1 d . . . C1 C 0.90710(11) 0.33417(9) 0.17884(7) 0.02467(18) Uani 1 1 d . . . C2 C 0.89806(11) 0.29641(9) 0.30266(7) 0.02605(19) Uani 1 1 d . . . C3 C 0.96722(13) 0.36863(11) 0.36130(8) 0.0327(2) Uani 1 1 d . . . C4 C 0.83689(12) 0.16988(10) 0.48041(8) 0.0296(2) Uani 1 1 d . . . C5 C 0.82124(12) 0.18138(10) 0.37212(7) 0.0283(2) Uani 1 1 d . . . C6 C 0.78454(13) 0.06257(11) 0.57419(8) 0.0343(2) Uani 1 1 d . . . C7 C 0.68210(17) -0.04478(12) 0.56269(10) 0.0425(3) Uani 1 1 d . . . C8 C 1.01421(11) 0.23557(9) 0.09986(7) 0.02409(18) Uani 1 1 d . . . C9 C 1.11005(12) 0.13180(9) 0.12986(7) 0.02645(19) Uani 1 1 d . . . C10 C 1.14571(11) 0.15319(9) -0.07651(7) 0.02450(18) Uani 1 1 d . . . C11 C 1.03446(11) 0.24677(9) -0.01948(7) 0.02446(18) Uani 1 1 d . . . C12 C 1.20023(12) 0.13328(9) -0.19859(8) 0.0283(2) Uani 1 1 d . . . C13 C 1.12129(16) 0.22092(13) -0.27500(9) 0.0418(3) Uani 1 1 d . . . C14 C 0.72867(11) 0.35739(9) 0.16842(7) 0.02390(18) Uani 1 1 d . . . C15 C 0.62543(12) 0.26136(10) 0.16340(8) 0.0297(2) Uani 1 1 d . . . C16 C 0.48296(11) 0.47900(9) 0.15820(8) 0.02696(19) Uani 1 1 d . . . C17 C 0.64658(12) 0.48368(9) 0.16485(8) 0.02674(19) Uani 1 1 d . . . C18 C 0.35674(12) 0.58578(10) 0.15333(9) 0.0321(2) Uani 1 1 d . . . C19 C 0.40270(16) 0.72165(11) 0.16012(12) 0.0458(3) Uani 1 1 d . . . H1 H 0.9606(15) 0.4144(12) 0.1549(10) 0.031(3) Uiso 1 1 d . . . H3 H 1.0215(16) 0.4414(13) 0.3334(10) 0.036(3) Uiso 1 1 d . . . H5 H 0.7725(13) 0.1211(10) 0.3551(9) 0.019(2) Uiso 1 1 d . . . H9 H 1.1219(17) 0.1026(13) 0.2020(11) 0.042(4) Uiso 1 1 d . . . H11 H 0.9799(14) 0.3064(11) -0.0501(9) 0.024(3) Uiso 1 1 d . . . H15 H 0.6536(17) 0.1699(13) 0.1600(11) 0.042(4) Uiso 1 1 d . . . H17 H 0.6958(14) 0.5530(11) 0.1616(9) 0.022(3) Uiso 1 1 d . . . H7A H 0.564(2) -0.0218(17) 0.5984(14) 0.071(5) Uiso 1 1 d . . . H13A H 1.094(2) 0.3045(16) -0.2522(13) 0.061(5) Uiso 1 1 d . . . H19A H 0.511(2) 0.7429(16) 0.1055(14) 0.068(5) Uiso 1 1 d . . . H7B H 0.704(2) -0.1232(17) 0.6041(14) 0.067(5) Uiso 1 1 d . . . H13B H 1.1989(19) 0.2348(15) -0.3489(13) 0.056(4) Uiso 1 1 d . . . H19B H 0.317(2) 0.7704(19) 0.1529(16) 0.086(6) Uiso 1 1 d . . . H7C H 0.697(2) -0.0607(17) 0.4873(14) 0.068(5) Uiso 1 1 d . . . H13C H 1.040(3) 0.179(2) -0.2822(16) 0.087(6) Uiso 1 1 d . . . H19C H 0.407(2) 0.7269(18) 0.2337(16) 0.080(6) Uiso 1 1 d . . . O01 O 0.5173(5) 0.6684(4) 0.4387(4) 0.097(2) Uani 0.273(2) 1 d PD A -1 H01 H 0.5668 0.7364 0.4326 0.145 Uiso 0.273(2) 1 calc PR A -1 C01 C 0.5705(6) 0.5718(4) 0.5139(4) 0.0651(7) Uiso 0.273(2) 1 d PD A -1 H01A H 0.5426 0.6010 0.5895 0.078 Uiso 0.273(2) 1 calc PR A -1 H01B H 0.6935 0.5545 0.4840 0.078 Uiso 0.273(2) 1 calc PR A -1 C02 C 0.4756(7) 0.4512(4) 0.5206(6) 0.0651(7) Uiso 0.273(2) 1 d PD A -1 H02A H 0.5111 0.3817 0.5680 0.098 Uiso 0.273(2) 1 calc PR A -1 H02B H 0.5005 0.4258 0.4447 0.098 Uiso 0.273(2) 1 calc PR A -1 H02C H 0.3544 0.4688 0.5533 0.098 Uiso 0.273(2) 1 calc PR A -1 O02 O 0.6194(6) 0.6127(6) 0.5425(4) 0.099(2) Uani 0.227(2) 1 d PD A -2 H02 H 0.6663 0.6826 0.5171 0.148 Uiso 0.227(2) 1 calc PR A -2 C03 C 0.5443(7) 0.5754(5) 0.4635(5) 0.0651(7) Uiso 0.227(2) 1 d PD A -2 H03A H 0.6335 0.5683 0.3900 0.078 Uiso 0.227(2) 1 calc PR A -2 H03B H 0.4624 0.6435 0.4519 0.078 Uiso 0.227(2) 1 calc PR A -2 C04 C 0.4550(9) 0.4486(5) 0.5030(7) 0.0651(7) Uiso 0.227(2) 1 d PD A -2 H04A H 0.4066 0.4289 0.4467 0.098 Uiso 0.227(2) 1 calc PR A -2 H04B H 0.3651 0.4554 0.5750 0.098 Uiso 0.227(2) 1 calc PR A -2 H04C H 0.5360 0.3802 0.5125 0.098 Uiso 0.227(2) 1 calc PR A -2 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 0.04989(12) 0.04570(14) 0.03009(10) -0.00289(10) -0.02337(9) -0.00302(11) S2 0.02711(9) 0.02590(10) 0.02860(9) 0.00211(8) -0.01041(8) 0.00116(8) S3 0.02824(9) 0.02946(11) 0.04377(11) -0.00042(9) -0.01758(8) -0.00289(9) O1 0.0747(5) 0.0527(5) 0.0325(3) 0.0049(3) -0.0291(3) 0.0019(4) O2 0.0418(4) 0.0340(4) 0.0335(3) -0.0063(3) -0.0089(3) 0.0046(3) O3 0.0282(3) 0.0415(4) 0.0487(4) 0.0090(3) -0.0163(3) 0.0001(3) C1 0.0250(3) 0.0270(4) 0.0238(3) -0.0003(3) -0.0110(3) -0.0022(3) C2 0.0251(3) 0.0310(4) 0.0231(3) -0.0020(3) -0.0102(3) 0.0016(3) C3 0.0362(4) 0.0369(5) 0.0290(4) -0.0017(4) -0.0163(3) -0.0033(4) C4 0.0304(4) 0.0347(5) 0.0241(4) -0.0028(3) -0.0107(3) 0.0052(4) C5 0.0296(4) 0.0335(4) 0.0221(3) -0.0020(3) -0.0099(3) 0.0029(4) C6 0.0370(4) 0.0382(5) 0.0249(4) -0.0011(4) -0.0095(3) 0.0110(4) C7 0.0494(6) 0.0423(6) 0.0298(5) 0.0031(4) -0.0077(4) -0.0009(5) C8 0.0220(3) 0.0272(4) 0.0243(3) 0.0008(3) -0.0102(3) -0.0024(3) C9 0.0268(4) 0.0296(4) 0.0230(3) 0.0023(3) -0.0098(3) -0.0016(3) C10 0.0246(3) 0.0253(4) 0.0246(3) 0.0022(3) -0.0105(3) -0.0034(3) C11 0.0240(3) 0.0265(4) 0.0234(3) 0.0025(3) -0.0100(3) -0.0027(3) C12 0.0296(4) 0.0292(4) 0.0270(4) -0.0025(3) -0.0099(3) -0.0038(3) C13 0.0491(5) 0.0514(6) 0.0267(4) -0.0059(4) -0.0168(4) 0.0109(5) C14 0.0249(3) 0.0255(4) 0.0220(3) 0.0015(3) -0.0099(3) -0.0015(3) C15 0.0286(4) 0.0270(4) 0.0365(4) -0.0009(3) -0.0157(3) 0.0003(3) C16 0.0268(4) 0.0255(4) 0.0285(4) 0.0027(3) -0.0108(3) -0.0016(3) C17 0.0270(4) 0.0268(4) 0.0272(4) 0.0000(3) -0.0113(3) 0.0005(3) C18 0.0281(4) 0.0311(4) 0.0332(4) 0.0070(4) -0.0090(3) 0.0010(4) C19 0.0383(5) 0.0298(5) 0.0652(7) 0.0033(5) -0.0155(5) 0.0026(4) O01 0.063(3) 0.061(3) 0.130(4) 0.022(3) 0.001(3) 0.019(2) O02 0.126(5) 0.114(4) 0.058(3) -0.017(3) -0.016(3) -0.060(4) _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 C3 1.7058(10) . ? S1 C4 1.7251(11) . ? S2 C9 1.7107(9) . ? S2 C10 1.7280(9) . ? S3 C15 1.7065(10) . ? S3 C16 1.7215(10) . ? O1 C6 1.2226(14) . ? O2 C12 1.2237(12) . ? O3 C18 1.2256(13) . ? C1 C2 1.5139(12) . ? C1 C14 1.5206(12) . ? C1 C8 1.5229(12) . ? C2 C3 1.3731(14) . ? C2 C5 1.4283(13) . ? C4 C5 1.3810(13) . ? C4 C6 1.4746(14) . ? C6 C7 1.4897(18) . ? C8 C9 1.3710(13) . ? C8 C11 1.4237(12) . ? C10 C11 1.3733(12) . ? C10 C12 1.4660(13) . ? C12 C13 1.4988(15) . ? C14 C15 1.3734(14) . ? C14 C17 1.4257(13) . ? C16 C17 1.3855(13) . ? C16 C18 1.4692(13) . ? C18 C19 1.4977(17) . ? O01 C01 1.424(4) . ? C01 C02 1.497(4) . ? O02 C03 1.423(4) . ? C03 C04 1.494(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 C3 S1 C4 91.52(5) . . ? C9 S2 C10 91.34(4) . . ? C15 S3 C16 91.69(5) . . ? C2 C1 C14 111.30(7) . . ? C2 C1 C8 112.11(7) . . ? C14 C1 C8 111.96(8) . . ? C3 C2 C5 111.59(8) . . ? C3 C2 C1 123.45(8) . . ? C5 C2 C1 124.94(9) . . ? C2 C3 S1 112.98(8) . . ? C5 C4 C6 129.01(10) . . ? C5 C4 S1 111.59(7) . . ? C6 C4 S1 119.32(8) . . ? C4 C5 C2 112.31(9) . . ? O1 C6 C4 119.42(11) . . ? O1 C6 C7 121.14(10) . . ? C4 C6 C7 119.43(9) . . ? C9 C8 C11 111.36(8) . . ? C9 C8 C1 126.13(8) . . ? C11 C8 C1 122.40(8) . . ? C8 C9 S2 112.95(7) . . ? C11 C10 C12 129.19(8) . . ? C11 C10 S2 111.34(7) . . ? C12 C10 S2 119.48(7) . . ? C10 C11 C8 113.01(8) . . ? O2 C12 C10 120.80(9) . . ? O2 C12 C13 121.15(9) . . ? C10 C12 C13 118.04(8) . . ? C15 C14 C17 111.55(8) . . ? C15 C14 C1 125.11(8) . . ? C17 C14 C1 123.33(8) . . ? C14 C15 S3 112.92(7) . . ? C17 C16 C18 129.66(9) . . ? C17 C16 S3 111.38(7) . . ? C18 C16 S3 118.97(7) . . ? C16 C17 C14 112.46(9) . . ? O3 C18 C16 120.15(10) . . ? O3 C18 C19 121.94(10) . . ? C16 C18 C19 117.89(9) . . ? O01 C01 C02 106.3(4) . . ? O02 C03 C04 113.2(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 29.59 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.483 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.063 #===END data_Acetone/TATM _database_code_depnum_ccdc_archive 'CCDC 255673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TATM _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20.50 H19 O3.50 S3' _chemical_formula_weight 417.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 8.1161(4) _cell_length_b 10.5951(5) _cell_length_c 12.3577(6) _cell_angle_alpha 94.9120(10) _cell_angle_beta 107.8570(10) _cell_angle_gamma 95.9140(10) _cell_volume 998.33(8) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 12597 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 29.60 _reflns_number_total 5516 _reflns_number_gt 4211 _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^)+(0.0709P)^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 5516 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 S1 S 0.06931(4) 0.80648(3) 0.00754(3) 0.03697(8) Uani 1 1 d . . . S2 S 0.25340(3) 0.54128(3) 0.48848(2) 0.02551(6) Uani 1 1 d . . . S3 S 0.90957(3) 0.82749(3) 0.34055(2) 0.02772(7) Uani 1 1 d . . . O1 O 0.02246(14) 0.58032(10) -0.16234(8) 0.0514(3) Uani 1 1 d . . . O2 O 0.43995(11) 0.53578(8) 0.73753(7) 0.0353(2) Uani 1 1 d . . . O3 O 1.13977(10) 1.06676(8) 0.35651(7) 0.0340(2) Uani 1 1 d . . . C1 C 0.40616(12) 0.82917(10) 0.32851(8) 0.0227(2) Uani 1 1 d . . . C2 C 0.29362(13) 0.79425(11) 0.20432(9) 0.0250(2) Uani 1 1 d . . . C3 C 0.17626(14) 0.86907(12) 0.14693(10) 0.0306(3) Uani 1 1 d . . . C4 C 0.18160(14) 0.67565(11) 0.02342(9) 0.0292(3) Uani 1 1 d . . . C5 C 0.29679(14) 0.68230(11) 0.13234(9) 0.0270(3) Uani 1 1 d . . . C6 C 0.14008(16) 0.57434(12) -0.07414(10) 0.0351(3) Uani 1 1 d . . . C7 C 0.24577(18) 0.46576(14) -0.06300(11) 0.0420(3) Uani 1 1 d . . . C8 C 0.37695(12) 0.73010(10) 0.40529(8) 0.0218(2) Uani 1 1 d . . . C9 C 0.25028(13) 0.62567(10) 0.37575(9) 0.0250(2) Uani 1 1 d . . . C10 C 0.42822(12) 0.64585(10) 0.57895(9) 0.0223(2) Uani 1 1 d . . . C11 C 0.47985(12) 0.74045(10) 0.52266(9) 0.0217(2) Uani 1 1 d . . . C12 C 0.50124(14) 0.62499(11) 0.69961(9) 0.0272(3) Uani 1 1 d . . . C13 C 0.65470(18) 0.71789(15) 0.77404(11) 0.0459(4) Uani 1 1 d . . . C14 C 0.59769(13) 0.85677(10) 0.33765(8) 0.0215(2) Uani 1 1 d . . . C15 C 0.70412(13) 0.76476(10) 0.33408(9) 0.0254(2) Uani 1 1 d . . . C16 C 0.85889(13) 0.98094(10) 0.34949(9) 0.0228(2) Uani 1 1 d . . . C17 C 0.68791(13) 0.98210(10) 0.34747(9) 0.0230(2) Uani 1 1 d . . . C18 C 0.99322(14) 1.08786(11) 0.35590(9) 0.0266(2) Uani 1 1 d . . . C19 C 0.94551(16) 1.22054(12) 0.35871(12) 0.0370(3) Uani 1 1 d . . . H1 H 0.3761(14) 0.9069(11) 0.3545(9) 0.020(3) Uiso 1 1 d . . . H3 H 0.1491(17) 0.9442(13) 0.1758(11) 0.036(4) Uiso 1 1 d . . . H5 H 0.3588(14) 0.6191(11) 0.1543(9) 0.015(3) Uiso 1 1 d . . . H9 H 0.1689(17) 0.5953(13) 0.3069(11) 0.038(4) Uiso 1 1 d . . . H11 H 0.5703(14) 0.8047(11) 0.5548(10) 0.021(3) Uiso 1 1 d . . . H15 H 0.6418(13) 1.0463(10) 0.3506(8) 0.009(2) Uiso 1 1 d . . . H15 H 0.6778(15) 0.6746(12) 0.3304(10) 0.026(3) Uiso 1 1 d . . . H7A H 0.293(2) 0.4496(16) 0.0175(14) 0.069(5) Uiso 1 1 d . . . H13A H 0.648(2) 0.8018(19) 0.7625(16) 0.090(7) Uiso 1 1 d . . . H19A H 0.876(2) 1.2332(16) 0.4092(13) 0.060(5) Uiso 1 1 d . . . H7B H 0.188(2) 0.3916(18) -0.1026(15) 0.078(6) Uiso 1 1 d . . . H13B H 0.6686(19) 0.7162(15) 0.8560(13) 0.056(5) Uiso 1 1 d . . . H19B H 0.881(2) 1.2357(16) 0.2850(14) 0.067(5) Uiso 1 1 d . . . H7C H 0.329(2) 0.4878(18) -0.0941(16) 0.087(6) Uiso 1 1 d . . . H13C H 0.732(3) 0.705(2) 0.7633(18) 0.099(8) Uiso 1 1 d . . . H19C H 1.054(2) 1.2797(16) 0.3801(14) 0.065(5) Uiso 1 1 d . . . C24 C 0.6266(4) 0.8957(3) 1.0450(2) 0.0500(9) Uani 0.50 1 d P A -1 H24A H 0.6461 0.8075 1.0278 0.075 Uiso 0.50 1 calc PR A -1 H24B H 0.6043 0.9056 1.1186 0.075 Uiso 0.50 1 calc PR A -1 H24C H 0.7305 0.9544 1.0490 0.075 Uiso 0.50 1 calc PR A -1 O4 O 0.3952(3) 0.8475(2) 0.87169(19) 0.0594(7) Uani 0.50 1 d P A -1 C25 C 0.4719(3) 0.9256(3) 0.9523(2) 0.0398(7) Uani 0.50 1 d P A -1 C26 C 0.4200(5) 1.0541(3) 0.9671(3) 0.0559(9) Uani 0.50 1 d P A -1 H26A H 0.5197 1.1194 0.9764 0.084 Uiso 0.50 1 calc PR A -1 H26B H 0.3825 1.0629 1.0353 0.084 Uiso 0.50 1 calc PR A -1 H26C H 0.3234 1.0651 0.8995 0.084 Uiso 0.50 1 calc PR A -1 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 0.03062(14) 0.04141(16) 0.02951(14) 0.00700(12) -0.00244(11) -0.00218(12) S2 0.02355(11) 0.02279(12) 0.02828(12) -0.00242(10) 0.00977(9) -0.00566(9) S3 0.02127(10) 0.02548(13) 0.03665(14) 0.00143(11) 0.01116(10) 0.00015(10) O1 0.0572(6) 0.0492(6) 0.0291(4) 0.0002(4) -0.0058(4) -0.0120(5) O2 0.0417(4) 0.0320(4) 0.0329(4) 0.0069(3) 0.0144(3) -0.0024(4) O3 0.0234(3) 0.0349(4) 0.0416(4) -0.0045(4) 0.0129(3) -0.0060(3) C1 0.0179(4) 0.0263(5) 0.0218(4) 0.0003(4) 0.0050(3) -0.0004(4) C2 0.0184(4) 0.0303(5) 0.0236(5) 0.0029(4) 0.0054(4) -0.0043(4) C3 0.0244(5) 0.0346(6) 0.0284(5) 0.0034(5) 0.0036(4) -0.0008(4) C4 0.0252(5) 0.0344(6) 0.0241(5) 0.0028(4) 0.0061(4) -0.0077(4) C5 0.0225(4) 0.0332(5) 0.0225(5) 0.0032(4) 0.0059(4) -0.0044(4) C6 0.0361(5) 0.0401(6) 0.0241(5) 0.0016(5) 0.0097(4) -0.0156(5) C7 0.0418(6) 0.0510(8) 0.0301(6) -0.0053(6) 0.0135(5) -0.0052(6) C8 0.0176(4) 0.0250(5) 0.0228(4) 0.0004(4) 0.0076(3) 0.0012(4) C9 0.0219(4) 0.0275(5) 0.0232(5) -0.0018(4) 0.0067(4) -0.0026(4) C10 0.0190(4) 0.0220(5) 0.0243(4) -0.0013(4) 0.0071(4) -0.0016(4) C11 0.0167(4) 0.0234(5) 0.0238(4) -0.0021(4) 0.0071(3) -0.0004(4) C12 0.0263(5) 0.0282(5) 0.0268(5) 0.0023(4) 0.0095(4) 0.0005(4) C13 0.0406(7) 0.0584(8) 0.0272(6) 0.0086(6) 0.0008(5) -0.0171(6) C14 0.0187(4) 0.0230(5) 0.0199(4) 0.0001(4) 0.0045(3) -0.0023(4) C15 0.0216(4) 0.0242(5) 0.0291(5) 0.0016(4) 0.0081(4) -0.0021(4) C16 0.0222(4) 0.0220(5) 0.0227(4) 0.0003(4) 0.0071(4) -0.0014(4) C17 0.0215(4) 0.0237(5) 0.0219(4) 0.0004(4) 0.0062(4) -0.0013(4) C18 0.0242(4) 0.0272(5) 0.0258(5) -0.0030(4) 0.0085(4) -0.0050(4) C19 0.0359(6) 0.0243(5) 0.0495(7) 0.0003(5) 0.0157(5) -0.0048(5) C24 0.0526(16) 0.0641(19) 0.0263(12) 0.0086(13) 0.0041(12) 0.0006(15) O4 0.0580(12) 0.0595(13) 0.0472(11) -0.0087(10) 0.0021(10) 0.0052(11) C25 0.0396(12) 0.0509(15) 0.0290(11) 0.0044(11) 0.0142(10) -0.0028(12) C26 0.0619(18) 0.0506(19) 0.0638(19) 0.0092(15) 0.0328(15) 0.0051(15) _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 C3 1.7115(11) . ? S1 C4 1.7286(13) . ? S2 C9 1.7138(12) . ? S2 C10 1.7267(9) . ? S3 C15 1.7057(11) . ? S3 C16 1.7203(11) . ? O1 C6 1.2204(14) . ? O2 C12 1.2175(14) . ? O3 C18 1.2306(14) . ? C1 C2 1.5166(13) . ? C1 C14 1.5191(14) . ? C1 C8 1.5217(15) . ? C2 C3 1.3697(16) . ? C2 C5 1.4278(16) . ? C4 C5 1.3745(14) . ? C4 C6 1.4744(16) . ? C6 C7 1.495(2) . ? C8 C9 1.3714(14) . ? C8 C11 1.4227(13) . ? C10 C11 1.3695(15) . ? C10 C12 1.4713(15) . ? C12 C13 1.5020(16) . ? C14 C15 1.3740(16) . ? C14 C17 1.4254(14) . ? C16 C17 1.3816(15) . ? C16 C18 1.4681(15) . ? C18 C19 1.4965(17) . ? C24 C25 1.501(4) . ? O4 C25 1.198(3) . ? C25 C26 1.478(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 C3 S1 C4 91.33(5) . . ? C9 S2 C10 91.34(5) . . ? C15 S3 C16 91.73(5) . . ? C2 C1 C14 110.57(9) . . ? C2 C1 C8 113.30(8) . . ? C14 C1 C8 111.59(8) . . ? C3 C2 C5 111.55(9) . . ? C3 C2 C1 123.23(10) . . ? C5 C2 C1 125.22(9) . . ? C2 C3 S1 112.93(9) . . ? C5 C4 C6 129.61(11) . . ? C5 C4 S1 111.52(9) . . ? C6 C4 S1 118.83(8) . . ? C4 C5 C2 112.67(10) . . ? O1 C6 C4 120.20(12) . . ? O1 C6 C7 121.06(11) . . ? C4 C6 C7 118.73(10) . . ? C9 C8 C11 111.37(10) . . ? C9 C8 C1 126.80(9) . . ? C11 C8 C1 121.78(8) . . ? C8 C9 S2 112.75(7) . . ? C11 C10 C12 129.01(9) . . ? C11 C10 S2 111.38(7) . . ? C12 C10 S2 119.61(8) . . ? C10 C11 C8 113.16(8) . . ? O2 C12 C10 121.32(9) . . ? O2 C12 C13 121.33(10) . . ? C10 C12 C13 117.35(10) . . ? C15 C14 C17 111.54(9) . . ? C15 C14 C1 124.57(9) . . ? C17 C14 C1 123.86(9) . . ? C14 C15 S3 112.79(8) . . ? C17 C16 C18 129.71(10) . . ? C17 C16 S3 111.43(8) . . ? C18 C16 S3 118.85(8) . . ? C16 C17 C14 112.51(10) . . ? O3 C18 C16 119.87(10) . . ? O3 C18 C19 121.70(10) . . ? C16 C18 C19 118.41(10) . . ? O4 C25 C26 122.8(3) . . ? O4 C25 C24 120.6(3) . . ? C26 C25 C24 116.5(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 29.60 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.532 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.072 #===END