# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 188 _publ_requested_journal Perkin Transactions 2 data_c:\dejana\struct~1\1 _database_code_CSD 161745 _audit_creation_method SHELXL-97 _chemical_name_systematic 1 ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H28 O3' _chemical_formula_weight 496.57 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' _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 8.6441(5) _cell_length_b 12.3085(8) _cell_length_c 13.7443(9) _cell_angle_alpha 109.514(3) _cell_angle_beta 94.460(3) _cell_angle_gamma 104.182(3) _cell_volume 1315.79(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 6393 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.77 _reflns_number_total 4887 _reflns_number_gt 3664 _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^)+(0.0536P)^2^+0.5110P] 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 4887 _refine_ls_number_parameters 353 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.013 _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 O9B O 0.23055(17) 0.10249(13) 0.76264(11) 0.0386(4) Uani 1 1 d D . . O9A O 0.71891(17) 0.68976(12) 0.90576(11) 0.0364(4) Uani 1 1 d D . . C10B C 0.1188(2) 0.07279(16) 0.58884(14) 0.0289(4) Uani 1 1 d . . . C5AA C 0.5584(2) 0.76615(16) 0.71749(15) 0.0313(4) Uani 1 1 d . . . C9A C 0.7524(2) 0.78045(16) 0.86050(14) 0.0290(4) Uani 1 1 d . . . C10A C 0.8827(2) 0.89398(16) 0.93341(14) 0.0274(4) Uani 1 1 d . . . C5BB C 0.4827(2) 0.30015(17) 0.67246(14) 0.0314(4) Uani 1 1 d . . . C1AA C 0.7972(2) 0.72121(16) 0.75482(15) 0.0294(4) Uani 1 1 d . . . C4AA C 0.6800(2) 0.70940(16) 0.67242(14) 0.0304(4) Uani 1 1 d . . . C4BB C 0.3648(2) 0.36451(17) 0.71207(14) 0.0308(4) Uani 1 1 d . . . C1BB C 0.2290(2) 0.28278(17) 0.72250(14) 0.0300(4) Uani 1 1 d . . . C8A C 0.5016(2) 0.86545(18) 0.88888(17) 0.0392(5) Uani 1 1 d . . . H8A H 0.5274 0.8929 0.9616 0.047 Uiso 1 1 calc R . . C12A C 0.9460(2) 0.90578(18) 1.03311(15) 0.0358(5) Uani 1 1 d . . . H12A H 0.9101 0.8429 1.0567 0.043 Uiso 1 1 calc R . . C9B C 0.2475(2) 0.15574(17) 0.68539(15) 0.0300(4) Uani 1 1 d . . . C2B C 0.1072(3) 0.4412(2) 0.78489(17) 0.0460(6) Uani 1 1 d . . . H2B H 0.0204 0.4676 0.8090 0.055 Uiso 1 1 calc R . . C11B C 0.1074(2) 0.10244(18) 0.50053(16) 0.0381(5) Uani 1 1 d . . . H11B H 0.1799 0.1719 0.5002 0.046 Uiso 1 1 calc R . . C4B C 0.3725(3) 0.48507(18) 0.73850(16) 0.0396(5) Uani 1 1 d . . . H4B H 0.4631 0.5395 0.7318 0.048 Uiso 1 1 calc R . . C1A C 0.9268(2) 0.67633(18) 0.73401(17) 0.0388(5) Uani 1 1 d . . . H1A H 1.0053 0.6849 0.7885 0.047 Uiso 1 1 calc R . . C3A C 0.8215(3) 0.60346(19) 0.54923(17) 0.0446(6) Uani 1 1 d . . . H3A H 0.8303 0.5631 0.4803 0.053 Uiso 1 1 calc R . . C12B C 0.0098(2) -0.03090(17) 0.58770(15) 0.0342(5) Uani 1 1 d . . . H12B H 0.0149 -0.0528 0.6462 0.041 Uiso 1 1 calc R . . C1B C 0.1006(2) 0.32081(19) 0.75903(16) 0.0388(5) Uani 1 1 d . . . H1B H 0.0104 0.2666 0.7663 0.047 Uiso 1 1 calc R . . C11A C 0.9379(2) 0.98997(18) 0.90156(16) 0.0377(5) Uani 1 1 d . . . H11A H 0.8963 0.9843 0.8350 0.045 Uiso 1 1 calc R . . C4A C 0.6909(3) 0.64865(18) 0.56974(16) 0.0386(5) Uani 1 1 d . . . H4A H 0.6115 0.6383 0.5151 0.046 Uiso 1 1 calc R . . C8AA C 0.5974(2) 0.80854(16) 0.82672(15) 0.0301(4) Uani 1 1 d . . . C5A C 0.4224(3) 0.78228(19) 0.66937(18) 0.0415(5) Uani 1 1 d . . . H5A H 0.3959 0.7548 0.5967 0.050 Uiso 1 1 calc R . . C8BB C 0.4185(2) 0.17901(17) 0.65888(14) 0.0318(5) Uani 1 1 d . . . C7A C 0.3650(3) 0.88088(19) 0.8402(2) 0.0475(6) Uani 1 1 d . . . H7A H 0.2988 0.9188 0.8809 0.057 Uiso 1 1 calc R . . C8B C 0.5081(3) 0.0990(2) 0.62634(17) 0.0431(5) Uani 1 1 d . . . H8B H 0.4669 0.0189 0.6190 0.052 Uiso 1 1 calc R . . C6B C 0.7229(3) 0.2593(2) 0.61523(17) 0.0486(6) Uani 1 1 d . . . H6B H 0.8246 0.2849 0.5989 0.058 Uiso 1 1 calc R . . C5B C 0.6357(2) 0.3411(2) 0.64972(16) 0.0413(5) Uani 1 1 d . . . H5B H 0.6780 0.4212 0.6575 0.050 Uiso 1 1 calc R . . C6A C 0.3275(3) 0.84039(19) 0.7325(2) 0.0480(6) Uani 1 1 d . . . H6A H 0.2366 0.8523 0.7016 0.058 Uiso 1 1 calc R . . C3B C 0.2425(3) 0.52257(19) 0.77497(17) 0.0458(6) Uani 1 1 d . . . H3B H 0.2457 0.6031 0.7930 0.055 Uiso 1 1 calc R . . C2A C 0.9389(3) 0.6179(2) 0.63044(18) 0.0463(6) Uani 1 1 d . . . H2A H 1.0269 0.5882 0.6156 0.056 Uiso 1 1 calc R . . C7B C 0.6619(3) 0.1407(2) 0.60462(18) 0.0512(6) Uani 1 1 d . . . H7B H 0.7238 0.0879 0.5828 0.061 Uiso 1 1 calc R . . O1G O 0.4779(2) 0.27178(16) 0.93456(12) 0.0592(5) Uani 1 1 d . . . C1G C 0.6175(3) 0.3113(2) 0.92937(18) 0.0554(7) Uani 1 1 d . . . C2G C 0.6907(5) 0.4403(3) 0.9473(3) 0.1049(14) Uani 1 1 d . . . H2G1 H 0.6952 0.4501 0.8810 0.157 Uiso 1 1 calc R . . H2G2 H 0.7984 0.4672 0.9868 0.157 Uiso 1 1 calc R . . H2G3 H 0.6260 0.4870 0.9855 0.157 Uiso 1 1 calc R . . C3G C 0.7198(5) 0.2295(4) 0.9016(3) 0.1113(14) Uani 1 1 d . . . H3G1 H 0.6568 0.1490 0.8903 0.167 Uiso 1 1 calc R . . H3G2 H 0.8095 0.2547 0.9578 0.167 Uiso 1 1 calc R . . H3G3 H 0.7598 0.2315 0.8388 0.167 Uiso 1 1 calc R . . H9B H 0.302(3) 0.153(2) 0.8212(18) 0.062(8) Uiso 1 1 d D . . H9A H 0.660(3) 0.710(2) 0.9591(19) 0.065(8) Uiso 1 1 d 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 O9B 0.0374(8) 0.0368(8) 0.0365(8) 0.0166(6) -0.0022(6) -0.0002(6) O9A 0.0354(8) 0.0312(8) 0.0380(8) 0.0135(6) 0.0028(7) 0.0012(6) C10B 0.0218(9) 0.0260(10) 0.0362(10) 0.0104(8) 0.0033(8) 0.0044(8) C5AA 0.0270(10) 0.0254(10) 0.0390(11) 0.0127(8) 0.0019(8) 0.0031(8) C9A 0.0247(10) 0.0241(9) 0.0337(10) 0.0087(8) 0.0022(8) 0.0027(8) C10A 0.0218(9) 0.0287(10) 0.0291(10) 0.0075(8) 0.0051(7) 0.0069(8) C5BB 0.0214(10) 0.0367(11) 0.0298(10) 0.0107(8) -0.0021(8) 0.0013(8) C1AA 0.0255(10) 0.0225(9) 0.0343(10) 0.0074(8) 0.0028(8) 0.0016(8) C4AA 0.0295(10) 0.0238(10) 0.0332(10) 0.0110(8) 0.0029(8) -0.0005(8) C4BB 0.0252(10) 0.0291(10) 0.0308(10) 0.0092(8) -0.0034(8) -0.0001(8) C1BB 0.0237(10) 0.0304(10) 0.0291(10) 0.0074(8) -0.0013(8) 0.0027(8) C8A 0.0310(11) 0.0296(11) 0.0463(12) 0.0046(9) 0.0057(9) 0.0032(9) C12A 0.0329(11) 0.0325(11) 0.0369(11) 0.0145(9) 0.0024(9) -0.0008(9) C9B 0.0244(10) 0.0283(10) 0.0340(10) 0.0120(8) 0.0021(8) 0.0020(8) C2B 0.0385(13) 0.0439(13) 0.0471(13) 0.0040(10) -0.0007(10) 0.0172(11) C11B 0.0358(12) 0.0286(10) 0.0427(12) 0.0162(9) -0.0003(9) -0.0056(9) C4B 0.0354(12) 0.0298(11) 0.0449(12) 0.0117(9) -0.0048(9) 0.0004(9) C1A 0.0282(11) 0.0355(11) 0.0450(12) 0.0077(9) 0.0028(9) 0.0064(9) C3A 0.0560(15) 0.0358(12) 0.0355(12) 0.0063(9) 0.0164(10) 0.0088(11) C12B 0.0321(11) 0.0331(11) 0.0356(11) 0.0169(9) 0.0009(8) 0.0018(9) C1B 0.0266(11) 0.0408(12) 0.0411(12) 0.0094(9) 0.0031(9) 0.0042(9) C11A 0.0366(11) 0.0372(11) 0.0314(10) 0.0135(9) -0.0046(9) -0.0013(9) C4A 0.0437(13) 0.0335(11) 0.0343(11) 0.0125(9) 0.0043(9) 0.0040(10) C8AA 0.0221(9) 0.0234(9) 0.0381(11) 0.0080(8) 0.0017(8) 0.0004(8) C5A 0.0361(12) 0.0373(12) 0.0482(13) 0.0180(10) -0.0041(10) 0.0055(10) C8BB 0.0238(10) 0.0341(11) 0.0309(10) 0.0081(8) -0.0019(8) 0.0041(8) C7A 0.0298(12) 0.0348(12) 0.0694(16) 0.0080(11) 0.0082(11) 0.0102(9) C8B 0.0346(12) 0.0406(12) 0.0472(12) 0.0088(10) 0.0001(10) 0.0112(10) C6B 0.0212(11) 0.0751(18) 0.0413(12) 0.0162(11) 0.0031(9) 0.0070(11) C5B 0.0261(11) 0.0488(13) 0.0396(12) 0.0149(10) -0.0002(9) -0.0019(10) C6A 0.0293(12) 0.0371(12) 0.0760(17) 0.0222(12) -0.0035(11) 0.0087(10) C3B 0.0462(14) 0.0290(11) 0.0505(13) 0.0051(9) -0.0092(10) 0.0093(10) C2A 0.0396(13) 0.0403(12) 0.0533(14) 0.0072(10) 0.0159(11) 0.0127(10) C7B 0.0342(13) 0.0633(16) 0.0480(13) 0.0059(11) 0.0036(10) 0.0213(12) O1G 0.0440(10) 0.0742(12) 0.0438(9) 0.0139(8) 0.0079(7) 0.0006(9) C1G 0.0479(15) 0.0734(18) 0.0364(13) 0.0234(12) 0.0009(11) 0.0000(13) C2G 0.120(3) 0.084(2) 0.075(2) 0.0355(18) -0.016(2) -0.032(2) C3G 0.090(3) 0.172(4) 0.108(3) 0.065(3) 0.051(2) 0.069(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 O9B C9B 1.421(2) . ? O9A C9A 1.432(2) . ? C10B C11B 1.382(3) . ? C10B C12B 1.383(3) . ? C10B C9B 1.533(2) . ? C5AA C5A 1.393(3) . ? C5AA C8AA 1.397(3) . ? C5AA C4AA 1.466(3) . ? C9A C1AA 1.520(3) . ? C9A C10A 1.531(2) . ? C9A C8AA 1.538(3) . ? C10A C12A 1.382(3) . ? C10A C11A 1.385(3) . ? C5BB C5B 1.394(3) . ? C5BB C8BB 1.400(3) . ? C5BB C4BB 1.468(3) . ? C1AA C1A 1.374(3) . ? C1AA C4AA 1.404(3) . ? C4AA C4A 1.382(3) . ? C4BB C4B 1.388(3) . ? C4BB C1BB 1.398(3) . ? C1BB C1B 1.374(3) . ? C1BB C9B 1.527(3) . ? C8A C8AA 1.379(3) . ? C8A C7A 1.396(3) . ? C12A C11A 1.385(3) 2_777 ? C9B C8BB 1.531(3) . ? C2B C1B 1.389(3) . ? C2B C3B 1.390(3) . ? C11B C12B 1.390(3) 2_556 ? C4B C3B 1.384(3) . ? C1A C2A 1.389(3) . ? C3A C2A 1.382(3) . ? C3A C4A 1.384(3) . ? C12B C11B 1.390(3) 2_556 ? C11A C12A 1.385(3) 2_777 ? C5A C6A 1.386(3) . ? C8BB C8B 1.379(3) . ? C7A C6A 1.378(3) . ? C8B C7B 1.396(3) . ? C6B C7B 1.378(4) . ? C6B C5B 1.383(3) . ? O1G C1G 1.203(3) . ? C1G C3G 1.474(5) . ? C1G C2G 1.484(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 C11B C10B C12B 118.25(17) . . ? C11B C10B C9B 119.86(17) . . ? C12B C10B C9B 121.87(17) . . ? C5A C5AA C8AA 120.28(19) . . ? C5A C5AA C4AA 130.76(19) . . ? C8AA C5AA C4AA 108.96(16) . . ? O9A C9A C1AA 105.70(15) . . ? O9A C9A C10A 111.51(14) . . ? C1AA C9A C10A 114.09(16) . . ? O9A C9A C8AA 111.85(15) . . ? C1AA C9A C8AA 101.14(15) . . ? C10A C9A C8AA 111.99(15) . . ? C12A C10A C11A 117.87(17) . . ? C12A C10A C9A 121.78(17) . . ? C11A C10A C9A 120.34(16) . . ? C5B C5BB C8BB 120.64(19) . . ? C5B C5BB C4BB 130.86(19) . . ? C8BB C5BB C4BB 108.50(17) . . ? C1A C1AA C4AA 120.35(18) . . ? C1A C1AA C9A 128.58(17) . . ? C4AA C1AA C9A 110.99(16) . . ? C4A C4AA C1AA 120.18(19) . . ? C4A C4AA C5AA 131.42(18) . . ? C1AA C4AA C5AA 108.37(16) . . ? C4B C4BB C1BB 120.76(19) . . ? C4B C4BB C5BB 130.48(18) . . ? C1BB C4BB C5BB 108.76(16) . . ? C1B C1BB C4BB 120.32(18) . . ? C1B C1BB C9B 128.88(18) . . ? C4BB C1BB C9B 110.76(17) . . ? C8AA C8A C7A 118.5(2) . . ? C10A C12A C11A 120.87(18) . 2_777 ? O9B C9B C1BB 113.14(16) . . ? O9B C9B C8BB 113.02(15) . . ? C1BB C9B C8BB 101.11(15) . . ? O9B C9B C10B 107.18(15) . . ? C1BB C9B C10B 110.37(15) . . ? C8BB C9B C10B 112.05(16) . . ? C1B C2B C3B 120.5(2) . . ? C10B C11B C12B 121.57(18) . 2_556 ? C3B C4B C4BB 118.6(2) . . ? C1AA C1A C2A 119.06(19) . . ? C2A C3A C4A 120.4(2) . . ? C10B C12B C11B 120.18(18) . 2_556 ? C1BB C1B C2B 119.2(2) . . ? C10A C11A C12A 121.27(18) . 2_777 ? C4AA C4A C3A 119.21(19) . . ? C8A C8AA C5AA 120.98(18) . . ? C8A C8AA C9A 128.61(18) . . ? C5AA C8AA C9A 110.41(17) . . ? C6A C5A C5AA 118.3(2) . . ? C8B C8BB C5BB 120.43(19) . . ? C8B C8BB C9B 128.83(19) . . ? C5BB C8BB C9B 110.74(17) . . ? C6A C7A C8A 120.6(2) . . ? C8BB C8B C7B 118.7(2) . . ? C7B C6B C5B 121.2(2) . . ? C6B C5B C5BB 118.3(2) . . ? C7A C6A C5A 121.3(2) . . ? C4B C3B C2B 120.7(2) . . ? C3A C2A C1A 120.7(2) . . ? C6B C7B C8B 120.7(2) . . ? O1G C1G C3G 119.6(3) . . ? O1G C1G C2G 122.2(3) . . ? C3G C1G C2G 118.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9A C9A C10A C12A -4.9(3) . . . . ? C1AA C9A C10A C12A -124.5(2) . . . . ? C8AA C9A C10A C12A 121.3(2) . . . . ? O9A C9A C10A C11A 176.77(18) . . . . ? C1AA C9A C10A C11A 57.1(2) . . . . ? C8AA C9A C10A C11A -57.0(2) . . . . ? O9A C9A C1AA C1A -63.5(2) . . . . ? C10A C9A C1AA C1A 59.4(3) . . . . ? C8AA C9A C1AA C1A 179.83(19) . . . . ? O9A C9A C1AA C4AA 113.16(16) . . . . ? C10A C9A C1AA C4AA -123.95(17) . . . . ? C8AA C9A C1AA C4AA -3.55(19) . . . . ? C1A C1AA C4AA C4A 2.3(3) . . . . ? C9A C1AA C4AA C4A -174.60(17) . . . . ? C1A C1AA C4AA C5AA -179.40(17) . . . . ? C9A C1AA C4AA C5AA 3.7(2) . . . . ? C5A C5AA C4AA C4A -4.7(4) . . . . ? C8AA C5AA C4AA C4A 175.8(2) . . . . ? C5A C5AA C4AA C1AA 177.4(2) . . . . ? C8AA C5AA C4AA C1AA -2.1(2) . . . . ? C5B C5BB C4BB C4B -0.2(3) . . . . ? C8BB C5BB C4BB C4B 179.38(19) . . . . ? C5B C5BB C4BB C1BB -179.62(19) . . . . ? C8BB C5BB C4BB C1BB -0.1(2) . . . . ? C4B C4BB C1BB C1B 0.1(3) . . . . ? C5BB C4BB C1BB C1B 179.63(16) . . . . ? C4B C4BB C1BB C9B 178.26(16) . . . . ? C5BB C4BB C1BB C9B -2.2(2) . . . . ? C11A C10A C12A C11A -0.6(3) . . . 2_777 ? C9A C10A C12A C11A -179.01(18) . . . 2_777 ? C1B C1BB C9B O9B -57.5(2) . . . . ? C4BB C1BB C9B O9B 124.55(17) . . . . ? C1B C1BB C9B C8BB -178.68(19) . . . . ? C4BB C1BB C9B C8BB 3.39(19) . . . . ? C1B C1BB C9B C10B 62.6(3) . . . . ? C4BB C1BB C9B C10B -115.37(17) . . . . ? C11B C10B C9B O9B -179.83(17) . . . . ? C12B C10B C9B O9B 1.6(2) . . . . ? C11B C10B C9B C1BB 56.6(2) . . . . ? C12B C10B C9B C1BB -122.0(2) . . . . ? C11B C10B C9B C8BB -55.3(2) . . . . ? C12B C10B C9B C8BB 126.2(2) . . . . ? C12B C10B C11B C12B 0.0(3) . . . 2_556 ? C9B C10B C11B C12B -178.62(19) . . . 2_556 ? C1BB C4BB C4B C3B -0.3(3) . . . . ? C5BB C4BB C4B C3B -179.67(19) . . . . ? C4AA C1AA C1A C2A -0.8(3) . . . . ? C9A C1AA C1A C2A 175.56(19) . . . . ? C11B C10B C12B C11B 0.0(3) . . . 2_556 ? C9B C10B C12B C11B 178.59(19) . . . 2_556 ? C4BB C1BB C1B C2B 0.3(3) . . . . ? C9B C1BB C1B C2B -177.43(18) . . . . ? C3B C2B C1B C1BB -0.6(3) . . . . ? C12A C10A C11A C12A 0.6(3) . . . 2_777 ? C9A C10A C11A C12A 179.03(18) . . . 2_777 ? C1AA C4AA C4A C3A -2.2(3) . . . . ? C5AA C4AA C4A C3A 180.0(2) . . . . ? C2A C3A C4A C4AA 0.6(3) . . . . ? C7A C8A C8AA C5AA -0.6(3) . . . . ? C7A C8A C8AA C9A -179.84(18) . . . . ? C5A C5AA C8AA C8A 0.9(3) . . . . ? C4AA C5AA C8AA C8A -179.58(17) . . . . ? C5A C5AA C8AA C9A -179.74(17) . . . . ? C4AA C5AA C8AA C9A -0.2(2) . . . . ? O9A C9A C8AA C8A 69.4(2) . . . . ? C1AA C9A C8AA C8A -178.47(19) . . . . ? C10A C9A C8AA C8A -56.6(3) . . . . ? O9A C9A C8AA C5AA -109.91(18) . . . . ? C1AA C9A C8AA C5AA 2.19(19) . . . . ? C10A C9A C8AA C5AA 124.07(17) . . . . ? C8AA C5AA C5A C6A -0.4(3) . . . . ? C4AA C5AA C5A C6A -179.83(19) . . . . ? C5B C5BB C8BB C8B 2.3(3) . . . . ? C4BB C5BB C8BB C8B -177.26(17) . . . . ? C5B C5BB C8BB C9B -178.05(16) . . . . ? C4BB C5BB C8BB C9B 2.3(2) . . . . ? O9B C9B C8BB C8B 54.9(3) . . . . ? C1BB C9B C8BB C8B 176.12(19) . . . . ? C10B C9B C8BB C8B -66.3(3) . . . . ? O9B C9B C8BB C5BB -124.67(17) . . . . ? C1BB C9B C8BB C5BB -3.43(19) . . . . ? C10B C9B C8BB C5BB 114.10(17) . . . . ? C8AA C8A C7A C6A -0.2(3) . . . . ? C5BB C8BB C8B C7B -1.7(3) . . . . ? C9B C8BB C8B C7B 178.78(19) . . . . ? C7B C6B C5B C5BB -0.8(3) . . . . ? C8BB C5BB C5B C6B -1.1(3) . . . . ? C4BB C5BB C5B C6B 178.42(19) . . . . ? C8A C7A C6A C5A 0.7(3) . . . . ? C5AA C5A C6A C7A -0.4(3) . . . . ? C4BB C4B C3B C2B 0.0(3) . . . . ? C1B C2B C3B C4B 0.5(3) . . . . ? C4A C3A C2A C1A 1.0(3) . . . . ? C1AA C1A C2A C3A -0.9(3) . . . . ? C5B C6B C7B C8B 1.4(3) . . . . ? C8BB C8B C7B C6B -0.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.196 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.045 data_c:\dejana\struct~1\2 _database_code_CSD 161746 _audit_creation_method SHELXL-97 _chemical_name_systematic 2 ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 O3 S' _chemical_formula_weight 516.66 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 8.5651(3) _cell_length_b 12.4402(4) _cell_length_c 13.8939(3) _cell_angle_alpha 109.148(2) _cell_angle_beta 93.849(2) _cell_angle_gamma 104.6200(10) _cell_volume 1334.90(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 8926 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4771 _reflns_number_gt 3838 _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^)+(0.0779P)^2^+0.6840P] 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 SHELXL _refine_ls_extinction_coef 0.009(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4771 _refine_ls_number_parameters 370 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.721 _refine_ls_shift/su_mean 0.002 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 C3B C 0.3366(3) 0.8480(2) 0.7317(2) 0.0465(7) Uani 1 1 d . . . H3B H 0.2474 0.8612 0.7004 0.056 Uiso 1 1 calc R . . C7B C 0.9495(3) 0.62267(19) 0.6368(2) 0.0433(6) Uani 1 1 d . . . H7B H 1.0385 0.5934 0.6229 0.052 Uiso 1 1 calc R . . C2B C 0.3714(3) 0.8881(2) 0.8384(2) 0.0468(7) Uani 1 1 d . . . H2B H 0.3051 0.9273 0.8777 0.056 Uiso 1 1 calc R . . C4B C 0.4320(3) 0.78863(19) 0.6709(2) 0.0401(6) Uani 1 1 d . . . H4B H 0.4076 0.7615 0.5992 0.048 Uiso 1 1 calc R . . C6B C 0.8341(3) 0.60945(19) 0.55609(19) 0.0412(6) Uani 1 1 d . . . H6B H 0.8453 0.5703 0.4884 0.049 Uiso 1 1 calc R . . C1B C 0.5054(2) 0.87034(18) 0.88750(19) 0.0369(5) Uani 1 1 d . . . H1B H 0.5295 0.8975 0.9592 0.044 Uiso 1 1 calc R . . C5B C 0.7021(3) 0.65393(18) 0.57498(18) 0.0353(5) Uani 1 1 d . . . H5B H 0.6240 0.6445 0.5207 0.042 Uiso 1 1 calc R . . C8B C 0.9341(3) 0.67930(18) 0.73866(18) 0.0374(5) Uani 1 1 d . . . H8B H 1.0114 0.6871 0.7928 0.045 Uiso 1 1 calc R . . C11B C 0.9323(2) 0.91033(17) 1.03600(17) 0.0310(5) Uani 1 1 d . . . H11B H 0.8880 0.8507 1.0613 0.037 Uiso 1 1 calc R . . C10B C 0.8848(2) 0.89398(16) 0.93357(15) 0.0245(4) Uani 1 1 d . . . C9B C 0.7541(2) 0.78192(16) 0.86172(16) 0.0266(4) Uani 1 1 d . . . C4BB C 0.5653(2) 0.77053(16) 0.71961(17) 0.0293(5) Uani 1 1 d . . . C8BB C 0.8027(2) 0.72366(15) 0.75823(16) 0.0271(4) Uani 1 1 d . . . C5BB C 0.6884(2) 0.71274(16) 0.67609(16) 0.0273(5) Uani 1 1 d . . . C1BB C 0.6014(2) 0.81141(16) 0.82686(16) 0.0274(5) Uani 1 1 d . . . O9B O 0.71636(18) 0.69269(12) 0.90717(12) 0.0342(4) Uani 1 1 d D . . H9B H 0.650(3) 0.713(2) 0.958(2) 0.063(9) Uiso 1 1 d D . . C5AA C 0.3688(2) 0.36391(16) 0.70201(16) 0.0274(4) Uani 1 1 d . . . C4AA C 0.4874(2) 0.29980(17) 0.66248(16) 0.0283(5) Uani 1 1 d . . . C9A C 0.2504(2) 0.15775(16) 0.67976(15) 0.0259(4) Uani 1 1 d . . . C8AA C 0.2322(2) 0.28356(16) 0.71420(15) 0.0262(4) Uani 1 1 d . . . C1AA C 0.4224(2) 0.18060(17) 0.65127(15) 0.0272(4) Uani 1 1 d . . . C6A C 0.2462(3) 0.52009(18) 0.76264(18) 0.0411(6) Uani 1 1 d . . . H6A H 0.2496 0.5995 0.7791 0.049 Uiso 1 1 calc R . . C8A C 0.1020(2) 0.32138(18) 0.75097(17) 0.0347(5) Uani 1 1 d . . . H8A H 0.0108 0.2683 0.7596 0.042 Uiso 1 1 calc R . . C5A C 0.3769(3) 0.48288(17) 0.72634(17) 0.0353(5) Uani 1 1 d . . . H5A H 0.4683 0.5363 0.7184 0.042 Uiso 1 1 calc R . . C7A C 0.1104(3) 0.4408(2) 0.77492(18) 0.0423(6) Uani 1 1 d . . . H7A H 0.0235 0.4676 0.7994 0.051 Uiso 1 1 calc R . . O9A O 0.23617(18) 0.10834(12) 0.75869(12) 0.0338(4) Uani 1 1 d D . . C10A C 0.1199(2) 0.07402(15) 0.58649(15) 0.0240(4) Uani 1 1 d . . . C12A C 0.0129(2) -0.02943(17) 0.58718(16) 0.0295(5) Uani 1 1 d . . . H12A H 0.0199 -0.0503 0.6454 0.035 Uiso 1 1 calc R . . C11A C 0.1051(2) 0.10238(17) 0.49860(16) 0.0320(5) Uani 1 1 d . . . H11A H 0.1757 0.1719 0.4969 0.038 Uiso 1 1 calc R . . O1G O 0.46499(19) 0.26230(17) 0.93278(14) 0.0552(5) Uani 1 1 d . . . C1G C 0.7080(5) 0.4479(3) 0.9477(3) 0.0918(13) Uani 1 1 d . . . S1GA S 0.64250(11) 0.31288(9) 0.97790(8) 0.0343(3) Uani 0.60 1 d P . . S1GB S 0.6431(3) 0.2969(2) 0.9060(3) 0.1022(11) Uani 0.40 1 d P . . C1A C 0.5129(3) 0.10148(19) 0.61962(18) 0.0369(5) Uani 1 1 d . . . H1A H 0.4709 0.0224 0.6132 0.044 Uiso 1 1 calc R . . C4A C 0.6418(2) 0.3403(2) 0.63930(18) 0.0376(5) Uani 1 1 d . . . H4A H 0.6845 0.4194 0.6458 0.045 Uiso 1 1 calc R . . C3A C 0.7304(3) 0.2597(2) 0.60629(19) 0.0452(6) Uani 1 1 d . . . H3A H 0.8335 0.2850 0.5898 0.054 Uiso 1 1 calc R . . C2A C 0.6685(3) 0.1426(2) 0.59752(19) 0.0452(6) Uani 1 1 d . . . H2A H 0.7312 0.0905 0.5766 0.054 Uiso 1 1 calc R . . C12B C 1.0461(2) 1.01549(17) 1.10146(17) 0.0329(5) Uani 1 1 d . . . H12B H 1.0761 1.0250 1.1700 0.039 Uiso 1 1 calc R . . H9A H 0.318(3) 0.158(2) 0.8120(18) 0.050(7) Uiso 1 1 d D . . C2GB C 0.7261(5) 0.2137(5) 0.8797(4) 0.0811(16) Uani 0.70 1 d P . . C2GA C 0.7919(16) 0.2694(12) 0.9705(14) 0.105(5) Uani 0.30 1 d P . . 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 C3B 0.0332(12) 0.0383(12) 0.066(2) 0.0175(12) -0.0070(11) 0.0122(9) C7B 0.0433(13) 0.0358(12) 0.0450(18) 0.0030(10) 0.0135(11) 0.0154(10) C2B 0.0338(12) 0.0336(11) 0.067(2) 0.0092(11) 0.0072(11) 0.0126(9) C4B 0.0387(12) 0.0361(11) 0.0427(16) 0.0147(10) -0.0062(10) 0.0087(9) C6B 0.0555(14) 0.0330(11) 0.0289(16) 0.0039(9) 0.0144(11) 0.0100(10) C1B 0.0331(11) 0.0278(10) 0.0419(16) 0.0038(9) 0.0060(9) 0.0070(8) C5B 0.0464(12) 0.0296(10) 0.0257(15) 0.0099(9) 0.0028(9) 0.0048(9) C8B 0.0337(11) 0.0336(11) 0.0389(16) 0.0043(10) 0.0015(9) 0.0123(9) C11B 0.0323(10) 0.0269(10) 0.0293(15) 0.0099(8) 0.0007(8) 0.0026(8) C10B 0.0247(9) 0.0242(9) 0.0214(14) 0.0040(8) 0.0020(7) 0.0077(7) C9B 0.0274(9) 0.0233(9) 0.0261(13) 0.0067(8) 0.0003(8) 0.0059(7) C4BB 0.0275(10) 0.0242(9) 0.0327(16) 0.0104(9) -0.0009(8) 0.0029(7) C8BB 0.0282(9) 0.0196(8) 0.0276(14) 0.0042(8) 0.0013(8) 0.0034(7) C5BB 0.0314(10) 0.0217(9) 0.0254(14) 0.0082(8) 0.0030(8) 0.0027(7) C1BB 0.0246(9) 0.0211(9) 0.0306(16) 0.0060(8) 0.0011(8) 0.0018(7) O9B 0.0407(8) 0.0265(7) 0.0317(10) 0.0108(6) 0.0016(7) 0.0037(6) C5AA 0.0275(9) 0.0260(9) 0.0213(13) 0.0049(8) -0.0050(7) 0.0019(7) C4AA 0.0259(9) 0.0308(10) 0.0216(13) 0.0071(8) -0.0035(7) 0.0021(7) C9A 0.0264(9) 0.0239(9) 0.0230(13) 0.0066(8) 0.0001(7) 0.0036(7) C8AA 0.0274(9) 0.0262(9) 0.0175(13) 0.0021(8) -0.0029(7) 0.0044(7) C1AA 0.0253(9) 0.0307(10) 0.0187(13) 0.0035(8) -0.0040(7) 0.0054(7) C6A 0.0517(13) 0.0257(10) 0.0370(16) 0.0011(9) -0.0064(10) 0.0128(9) C8A 0.0300(10) 0.0348(11) 0.0304(15) 0.0029(9) 0.0023(8) 0.0064(8) C5A 0.0386(11) 0.0246(10) 0.0336(15) 0.0062(9) -0.0049(9) 0.0018(8) C7A 0.0431(13) 0.0405(12) 0.0368(16) 0.0001(10) 0.0012(10) 0.0206(10) O9A 0.0386(8) 0.0329(8) 0.0240(10) 0.0115(6) -0.0043(6) 0.0006(6) C10A 0.0233(9) 0.0215(9) 0.0235(13) 0.0050(8) 0.0024(7) 0.0048(7) C12A 0.0324(10) 0.0292(10) 0.0250(14) 0.0120(8) 0.0002(8) 0.0036(8) C11A 0.0338(10) 0.0249(9) 0.0307(15) 0.0122(9) -0.0017(8) -0.0041(8) O1G 0.0383(9) 0.0695(12) 0.0401(12) 0.0175(9) -0.0044(7) -0.0088(8) C1G 0.087(2) 0.082(2) 0.089(3) 0.052(2) -0.020(2) -0.0243(19) S1GA 0.0343(5) 0.0557(6) 0.0000(6) 0.0087(4) -0.0024(4) -0.0059(4) S1GB 0.0459(12) 0.0693(15) 0.174(4) 0.0372(19) 0.0000(17) 0.0009(10) C1A 0.0358(11) 0.0359(11) 0.0301(15) 0.0012(9) -0.0041(9) 0.0120(9) C4A 0.0284(10) 0.0467(12) 0.0302(15) 0.0132(10) -0.0012(8) 0.0002(9) C3A 0.0241(10) 0.0701(17) 0.0320(16) 0.0108(12) 0.0011(9) 0.0083(10) C2A 0.0332(11) 0.0593(15) 0.0346(16) 0.0013(11) -0.0005(9) 0.0210(11) C12B 0.0395(11) 0.0307(10) 0.0221(14) 0.0085(8) -0.0017(8) 0.0024(8) C2GB 0.041(2) 0.131(5) 0.058(3) 0.008(3) 0.009(2) 0.037(3) C2GA 0.072(8) 0.084(8) 0.160(15) 0.060(9) -0.030(8) 0.016(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 C3B C2B 1.383(4) . ? C3B C4B 1.384(3) . ? C7B C6B 1.382(4) . ? C7B C8B 1.391(3) . ? C2B C1B 1.398(3) . ? C4B C4BB 1.393(3) . ? C6B C5B 1.383(3) . ? C1B C1BB 1.384(3) . ? C5B C5BB 1.384(3) . ? C8B C8BB 1.379(3) . ? C11B C10B 1.387(3) . ? C11B C12B 1.395(3) . ? C10B C12B 1.385(3) 2_777 ? C10B C9B 1.530(3) . ? C9B O9B 1.429(2) . ? C9B C8BB 1.521(3) . ? C9B C1BB 1.534(3) . ? C4BB C1BB 1.391(3) . ? C4BB C5BB 1.475(3) . ? C8BB C5BB 1.400(3) . ? C5AA C5A 1.388(3) . ? C5AA C8AA 1.395(3) . ? C5AA C4AA 1.471(3) . ? C4AA C4A 1.391(3) . ? C4AA C1AA 1.398(3) . ? C9A O9A 1.420(2) . ? C9A C8AA 1.531(3) . ? C9A C10A 1.532(3) . ? C9A C1AA 1.533(3) . ? C8AA C8A 1.382(3) . ? C1AA C1A 1.382(3) . ? C6A C5A 1.380(3) . ? C6A C7A 1.383(3) . ? C8A C7A 1.394(3) . ? C10A C12A 1.382(3) . ? C10A C11A 1.384(3) . ? C12A C11A 1.389(3) 2_556 ? C11A C12A 1.389(3) 2_556 ? O1G S1GA 1.4936(18) . ? O1G S1GB 1.581(3) . ? C1G S1GB 1.699(4) . ? C1G S1GA 1.825(3) . ? S1GA S1GB 0.952(4) . ? S1GA C2GA 1.507(13) . ? S1GA C2GB 1.835(5) . ? S1GB C2GB 1.367(5) . ? S1GB C2GA 1.677(12) . ? C1A C2A 1.395(3) . ? C4A C3A 1.386(3) . ? C3A C2A 1.379(4) . ? C12B C10B 1.385(3) 2_777 ? C2GB C2GA 1.234(16) . ? 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 C2B C3B C4B 121.2(2) . . ? C6B C7B C8B 120.7(2) . . ? C3B C2B C1B 120.5(2) . . ? C3B C4B C4BB 118.4(2) . . ? C7B C6B C5B 120.6(2) . . ? C1BB C1B C2B 118.4(2) . . ? C6B C5B C5BB 118.8(2) . . ? C8BB C8B C7B 119.0(2) . . ? C10B C11B C12B 120.56(19) . . ? C12B C10B C11B 118.12(18) 2_777 . ? C12B C10B C9B 120.36(18) 2_777 . ? C11B C10B C9B 121.47(17) . . ? O9B C9B C8BB 106.09(15) . . ? O9B C9B C10B 111.53(16) . . ? C8BB C9B C10B 113.99(16) . . ? O9B C9B C1BB 112.37(15) . . ? C8BB C9B C1BB 101.03(16) . . ? C10B C9B C1BB 111.34(14) . . ? C1BB C4BB C4B 120.6(2) . . ? C1BB C4BB C5BB 108.80(17) . . ? C4B C4BB C5BB 130.6(2) . . ? C8B C8BB C5BB 119.99(19) . . ? C8B C8BB C9B 128.79(18) . . ? C5BB C8BB C9B 111.16(16) . . ? C5B C5BB C8BB 120.75(19) . . ? C5B C5BB C4BB 131.18(19) . . ? C8BB C5BB C4BB 108.07(18) . . ? C1B C1BB C4BB 120.91(19) . . ? C1B C1BB C9B 128.3(2) . . ? C4BB C1BB C9B 110.78(17) . . ? C5A C5AA C8AA 120.89(19) . . ? C5A C5AA C4AA 130.53(18) . . ? C8AA C5AA C4AA 108.58(16) . . ? C4A C4AA C1AA 120.84(19) . . ? C4A C4AA C5AA 130.63(18) . . ? C1AA C4AA C5AA 108.53(16) . . ? O9A C9A C8AA 112.88(16) . . ? O9A C9A C10A 107.80(15) . . ? C8AA C9A C10A 110.59(15) . . ? O9A C9A C1AA 112.82(15) . . ? C8AA C9A C1AA 100.75(14) . . ? C10A C9A C1AA 111.98(16) . . ? C8A C8AA C5AA 120.33(18) . . ? C8A C8AA C9A 128.55(17) . . ? C5AA C8AA C9A 111.11(16) . . ? C1A C1AA C4AA 120.35(19) . . ? C1A C1AA C9A 128.69(18) . . ? C4AA C1AA C9A 110.94(16) . . ? C5A C6A C7A 120.84(19) . . ? C8AA C8A C7A 118.6(2) . . ? C6A C5A C5AA 118.6(2) . . ? C6A C7A C8A 120.8(2) . . ? C12A C10A C11A 118.09(17) . . ? C12A C10A C9A 122.13(17) . . ? C11A C10A C9A 119.78(16) . . ? C10A C12A C11A 120.38(19) . 2_556 ? C10A C11A C12A 121.53(17) . 2_556 ? S1GA O1G S1GB 35.95(14) . . ? S1GB C1G S1GA 31.10(15) . . ? S1GB S1GA O1G 77.05(17) . . ? S1GB S1GA C2GA 82.7(7) . . ? O1G S1GA C2GA 136.6(6) . . ? S1GB S1GA C1G 67.2(2) . . ? O1G S1GA C1G 104.32(15) . . ? C2GA S1GA C1G 102.4(5) . . ? S1GB S1GA C2GB 46.5(2) . . ? O1G S1GA C2GB 99.70(18) . . ? C2GA S1GA C2GB 41.9(6) . . ? C1G S1GA C2GB 99.9(3) . . ? S1GA S1GB C2GB 103.1(4) . . ? S1GA S1GB O1G 67.0(2) . . ? C2GB S1GB O1G 119.9(3) . . ? S1GA S1GB C2GA 63.0(7) . . ? C2GB S1GB C2GA 46.5(6) . . ? O1G S1GB C2GA 117.6(6) . . ? S1GA S1GB C1G 81.7(3) . . ? C2GB S1GB C1G 131.7(3) . . ? O1G S1GB C1G 106.4(2) . . ? C2GA S1GB C1G 100.9(5) . . ? C1AA C1A C2A 118.7(2) . . ? C3A C4A C4AA 118.2(2) . . ? C2A C3A C4A 121.2(2) . . ? C3A C2A C1A 120.7(2) . . ? C10B C12B C11B 121.3(2) 2_777 . ? C2GA C2GB S1GB 80.1(7) . . ? C2GA C2GB S1GA 54.7(7) . . ? S1GB C2GB S1GA 30.4(2) . . ? C2GB C2GA S1GA 83.4(7) . . ? C2GB C2GA S1GB 53.4(5) . . ? S1GA C2GA S1GB 34.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4B C3B C2B C1B 0.5(4) . . . . ? C2B C3B C4B C4BB -0.4(3) . . . . ? C8B C7B C6B C5B 1.0(3) . . . . ? C3B C2B C1B C1BB -0.3(3) . . . . ? C7B C6B C5B C5BB 0.5(3) . . . . ? C6B C7B C8B C8BB -0.8(3) . . . . ? C12B C11B C10B C12B 0.3(3) . . . 2_777 ? C12B C11B C10B C9B -177.01(18) . . . . ? C12B C10B C9B O9B 171.39(17) 2_777 . . . ? C11B C10B C9B O9B -11.4(2) . . . . ? C12B C10B C9B C8BB 51.3(2) 2_777 . . . ? C11B C10B C9B C8BB -131.50(19) . . . . ? C12B C10B C9B C1BB -62.2(2) 2_777 . . . ? C11B C10B C9B C1BB 115.0(2) . . . . ? C3B C4B C4BB C1BB -0.1(3) . . . . ? C3B C4B C4BB C5BB -179.1(2) . . . . ? C7B C8B C8BB C5BB -0.8(3) . . . . ? C7B C8B C8BB C9B 176.04(19) . . . . ? O9B C9B C8BB C8B -63.8(2) . . . . ? C10B C9B C8BB C8B 59.3(3) . . . . ? C1BB C9B C8BB C8B 178.82(19) . . . . ? O9B C9B C8BB C5BB 113.31(16) . . . . ? C10B C9B C8BB C5BB -123.57(17) . . . . ? C1BB C9B C8BB C5BB -4.07(19) . . . . ? C6B C5B C5BB C8BB -2.2(3) . . . . ? C6B C5B C5BB C4BB 178.83(19) . . . . ? C8B C8BB C5BB C5B 2.4(3) . . . . ? C9B C8BB C5BB C5B -175.04(16) . . . . ? C8B C8BB C5BB C4BB -178.43(17) . . . . ? C9B C8BB C5BB C4BB 4.2(2) . . . . ? C1BB C4BB C5BB C5B 176.66(19) . . . . ? C4B C4BB C5BB C5B -4.2(3) . . . . ? C1BB C4BB C5BB C8BB -2.4(2) . . . . ? C4B C4BB C5BB C8BB 176.7(2) . . . . ? C2B C1B C1BB C4BB -0.1(3) . . . . ? C2B C1B C1BB C9B 179.54(19) . . . . ? C4B C4BB C1BB C1B 0.3(3) . . . . ? C5BB C4BB C1BB C1B 179.51(17) . . . . ? C4B C4BB C1BB C9B -179.43(17) . . . . ? C5BB C4BB C1BB C9B -0.2(2) . . . . ? O9B C9B C1BB C1B 70.1(2) . . . . ? C8BB C9B C1BB C1B -177.20(19) . . . . ? C10B C9B C1BB C1B -55.8(3) . . . . ? O9B C9B C1BB C4BB -110.17(19) . . . . ? C8BB C9B C1BB C4BB 2.51(19) . . . . ? C10B C9B C1BB C4BB 123.90(18) . . . . ? C5A C5AA C4AA C4A 0.8(4) . . . . ? C8AA C5AA C4AA C4A -179.0(2) . . . . ? C5A C5AA C4AA C1AA 179.5(2) . . . . ? C8AA C5AA C4AA C1AA -0.3(2) . . . . ? C5A C5AA C8AA C8A 0.0(3) . . . . ? C4AA C5AA C8AA C8A 179.75(18) . . . . ? C5A C5AA C8AA C9A 178.54(17) . . . . ? C4AA C5AA C8AA C9A -1.7(2) . . . . ? O9A C9A C8AA C8A -58.3(3) . . . . ? C10A C9A C8AA C8A 62.6(3) . . . . ? C1AA C9A C8AA C8A -178.9(2) . . . . ? O9A C9A C8AA C5AA 123.28(18) . . . . ? C10A C9A C8AA C5AA -115.86(18) . . . . ? C1AA C9A C8AA C5AA 2.7(2) . . . . ? C4A C4AA C1AA C1A 1.8(3) . . . . ? C5AA C4AA C1AA C1A -177.02(19) . . . . ? C4A C4AA C1AA C9A -179.04(18) . . . . ? C5AA C4AA C1AA C9A 2.1(2) . . . . ? O9A C9A C1AA C1A 55.5(3) . . . . ? C8AA C9A C1AA C1A 176.1(2) . . . . ? C10A C9A C1AA C1A -66.3(3) . . . . ? O9A C9A C1AA C4AA -123.49(17) . . . . ? C8AA C9A C1AA C4AA -2.9(2) . . . . ? C10A C9A C1AA C4AA 114.68(18) . . . . ? C5AA C8AA C8A C7A 0.3(3) . . . . ? C9A C8AA C8A C7A -178.0(2) . . . . ? C7A C6A C5A C5AA 0.2(3) . . . . ? C8AA C5AA C5A C6A -0.2(3) . . . . ? C4AA C5AA C5A C6A -180.0(2) . . . . ? C5A C6A C7A C8A 0.0(4) . . . . ? C8AA C8A C7A C6A -0.3(3) . . . . ? O9A C9A C10A C12A 0.0(2) . . . . ? C8AA C9A C10A C12A -123.80(19) . . . . ? C1AA C9A C10A C12A 124.70(19) . . . . ? O9A C9A C10A C11A 178.97(17) . . . . ? C8AA C9A C10A C11A 55.1(2) . . . . ? C1AA C9A C10A C11A -56.4(2) . . . . ? C11A C10A C12A C11A 0.3(3) . . . 2_556 ? C9A C10A C12A C11A 179.26(18) . . . 2_556 ? C12A C10A C11A C12A -0.3(3) . . . 2_556 ? C9A C10A C11A C12A -179.29(18) . . . 2_556 ? S1GB O1G S1GA C2GA -64.3(9) . . . . ? S1GB O1G S1GA C1G 62.0(2) . . . . ? S1GB O1G S1GA C2GB -40.9(3) . . . . ? S1GB C1G S1GA O1G -69.0(2) . . . . ? S1GB C1G S1GA C2GA 76.4(7) . . . . ? S1GB C1G S1GA C2GB 33.8(2) . . . . ? O1G S1GA S1GB C2GB -117.2(3) . . . . ? C2GA S1GA S1GB C2GB 24.2(6) . . . . ? C1G S1GA S1GB C2GB 131.0(3) . . . . ? C2GA S1GA S1GB O1G 141.3(5) . . . . ? C1G S1GA S1GB O1G -111.86(18) . . . . ? C2GB S1GA S1GB O1G 117.2(3) . . . . ? O1G S1GA S1GB C2GA -141.3(5) . . . . ? C1G S1GA S1GB C2GA 106.8(5) . . . . ? C2GB S1GA S1GB C2GA -24.2(6) . . . . ? O1G S1GA S1GB C1G 111.86(18) . . . . ? C2GA S1GA S1GB C1G -106.8(5) . . . . ? C2GB S1GA S1GB C1G -131.0(3) . . . . ? S1GA O1G S1GB C2GB 92.4(4) . . . . ? S1GA O1G S1GB C2GA 38.9(7) . . . . ? S1GA O1G S1GB C1G -73.3(3) . . . . ? S1GA C1G S1GB C2GB -100.3(5) . . . . ? S1GA C1G S1GB O1G 63.0(2) . . . . ? S1GA C1G S1GB C2GA -60.4(7) . . . . ? C4AA C1AA C1A C2A -1.1(3) . . . . ? C9A C1AA C1A C2A 180.0(2) . . . . ? C1AA C4AA C4A C3A -1.0(3) . . . . ? C5AA C4AA C4A C3A 177.6(2) . . . . ? C4AA C4A C3A C2A -0.7(3) . . . . ? C4A C3A C2A C1A 1.4(4) . . . . ? C1AA C1A C2A C3A -0.5(3) . . . . ? C10B C11B C12B C10B -0.3(3) . . . 2_777 ? S1GA S1GB C2GB C2GA -30.2(8) . . . . ? O1G S1GB C2GB C2GA -101.1(8) . . . . ? C1G S1GB C2GB C2GA 60.4(9) . . . . ? O1G S1GB C2GB S1GA -70.8(4) . . . . ? C2GA S1GB C2GB S1GA 30.2(8) . . . . ? C1G S1GB C2GB S1GA 90.6(5) . . . . ? S1GB S1GA C2GB C2GA 142.6(9) . . . . ? O1G S1GA C2GB C2GA -155.9(8) . . . . ? C1G S1GA C2GB C2GA 97.6(8) . . . . ? O1G S1GA C2GB S1GB 61.6(3) . . . . ? C2GA S1GA C2GB S1GB -142.6(9) . . . . ? C1G S1GA C2GB S1GB -44.9(3) . . . . ? S1GB C2GB C2GA S1GA 18.2(4) . . . . ? S1GA C2GB C2GA S1GB -18.2(4) . . . . ? S1GB S1GA C2GA C2GB -26.4(6) . . . . ? O1G S1GA C2GA C2GB 35.9(12) . . . . ? C1G S1GA C2GA C2GB -91.0(7) . . . . ? O1G S1GA C2GA S1GB 62.3(7) . . . . ? C1G S1GA C2GA S1GB -64.6(3) . . . . ? C2GB S1GA C2GA S1GB 26.4(7) . . . . ? S1GA S1GB C2GA C2GB 146.6(8) . . . . ? O1G S1GB C2GA C2GB 106.2(7) . . . . ? C1G S1GB C2GA C2GB -138.6(6) . . . . ? C2GB S1GB C2GA S1GA -146.6(8) . . . . ? O1G S1GB C2GA S1GA -40.5(5) . . . . ? C1G S1GB C2GA S1GA 74.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.718 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.718 _refine_diff_density_max 0.359 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.049 data_c:\dejana\struct~1\3 _database_code_CSD 161747 _audit_creation_method SHELXL-97 _chemical_name_systematic 3 ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.42 H28 O3 S0.58' _chemical_formula_weight 508.24 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 8.5652(2) _cell_length_b 12.4265(3) _cell_length_c 13.8868(3) _cell_angle_alpha 109.155(2) _cell_angle_beta 93.853(3) _cell_angle_gamma 104.6010(10) _cell_volume 1332.83(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 7226 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.34 _reflns_number_total 4794 _reflns_number_gt 3937 _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^)+(0.0903P)^2^+2.1607P] 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 4794 _refine_ls_number_parameters 362 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1787 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 O9A O 0.7646(2) 0.89227(18) 0.74121(15) 0.0310(5) Uani 1 1 d D . . C4AA C 0.6315(3) 0.6359(2) 0.7980(2) 0.0259(6) Uani 1 1 d . . . C10A C 0.8800(3) 0.9261(2) 0.91312(19) 0.0214(6) Uani 1 1 d . . . C11A C 0.8950(3) 0.8974(2) 1.0016(2) 0.0289(6) Uani 1 1 d . . . H11A H 0.8245 0.8278 1.0032 0.035 Uiso 1 1 calc R . . C5A C 0.3584(3) 0.6598(3) 0.8603(2) 0.0351(7) Uani 1 1 d . . . H5A H 0.3157 0.5805 0.8535 0.042 Uiso 1 1 calc R . . C5AA C 0.5130(3) 0.7005(3) 0.8372(2) 0.0267(6) Uani 1 1 d . . . C9A C 0.7495(3) 0.8421(2) 0.8199(2) 0.0241(6) Uani 1 1 d . . . C3A C 0.7548(4) 0.4801(3) 0.7371(2) 0.0387(7) Uani 1 1 d . . . H3A H 0.7517 0.4007 0.7209 0.046 Uiso 1 1 calc R . . C8AA C 0.5780(3) 0.8196(2) 0.8486(2) 0.0249(6) Uani 1 1 d . . . C4A C 0.6233(4) 0.5172(3) 0.7734(2) 0.0333(7) Uani 1 1 d . . . H4A H 0.5317 0.4636 0.7810 0.040 Uiso 1 1 calc R . . C1AA C 0.7684(3) 0.7167(2) 0.78577(19) 0.0244(6) Uani 1 1 d . . . C2A C 0.8900(4) 0.5589(3) 0.7247(2) 0.0398(8) Uani 1 1 d . . . H2A H 0.9766 0.5320 0.6998 0.048 Uiso 1 1 calc R . . C12A C 0.9873(3) 1.0296(2) 0.9127(2) 0.0276(6) Uani 1 1 d . . . H12A H 0.9806 1.0506 0.8544 0.033 Uiso 1 1 calc R . . C1A C 0.8985(4) 0.6790(3) 0.7489(2) 0.0327(7) Uani 1 1 d . . . H1A H 0.9897 0.7322 0.7404 0.039 Uiso 1 1 calc R . . C6A C 0.2697(4) 0.7404(3) 0.8937(2) 0.0425(8) Uani 1 1 d . . . H6A H 0.1669 0.7152 0.9106 0.051 Uiso 1 1 calc R . . C8A C 0.4874(4) 0.8987(3) 0.8798(2) 0.0347(7) Uani 1 1 d . . . H8A H 0.5292 0.9777 0.8857 0.042 Uiso 1 1 calc R . . C7A C 0.3319(4) 0.8577(3) 0.9023(2) 0.0424(8) Uani 1 1 d . . . H7A H 0.2695 0.9100 0.9234 0.051 Uiso 1 1 calc R . . O9B O 0.2837(3) 0.30766(17) 0.59315(15) 0.0312(5) Uani 1 1 d D . . C9B C 0.2462(3) 0.2181(2) 0.6383(2) 0.0244(6) Uani 1 1 d . . . C8BB C 0.1972(3) 0.2764(2) 0.7422(2) 0.0249(6) Uani 1 1 d . . . C10B C 0.1157(3) 0.1061(2) 0.5663(2) 0.0226(6) Uani 1 1 d . . . C5BB C 0.3119(3) 0.2871(2) 0.8237(2) 0.0257(6) Uani 1 1 d . . . C11B C 0.0671(3) 0.0899(3) 0.4643(2) 0.0279(6) Uani 1 1 d . . . H11B H 0.1110 0.1498 0.4391 0.034 Uiso 1 1 calc R . . C4BB C 0.4350(3) 0.2296(2) 0.7807(2) 0.0267(6) Uani 1 1 d . . . C5B C 0.2987(4) 0.3465(3) 0.9255(2) 0.0330(7) Uani 1 1 d . . . H5B H 0.3771 0.3563 0.9798 0.040 Uiso 1 1 calc R . . C6B C 0.1664(4) 0.3910(3) 0.9442(2) 0.0382(7) Uani 1 1 d . . . H6B H 0.1554 0.4305 1.0118 0.046 Uiso 1 1 calc R . . C12B C 0.0464(4) 0.0146(3) 0.6012(2) 0.0303(6) Uani 1 1 d . . . H12B H 0.0768 0.0236 0.6696 0.036 Uiso 1 1 calc R . . C1BB C 0.3988(3) 0.1885(2) 0.6730(2) 0.0245(6) Uani 1 1 d . . . C8B C 0.0653(4) 0.3204(3) 0.7615(2) 0.0346(7) Uani 1 1 d . . . H8B H -0.0123 0.3121 0.7074 0.042 Uiso 1 1 calc R . . C1B C 0.4953(4) 0.1296(3) 0.6127(2) 0.0334(7) Uani 1 1 d . . . H1B H 0.4678 0.1003 0.5411 0.040 Uiso 1 1 calc R . . C4B C 0.5685(4) 0.2118(3) 0.8291(3) 0.0366(7) Uani 1 1 d . . . H4B H 0.5931 0.2393 0.9008 0.044 Uiso 1 1 calc R . . C7B C 0.0506(4) 0.3773(3) 0.8637(3) 0.0396(8) Uani 1 1 d . . . H7B H -0.0385 0.4066 0.8778 0.048 Uiso 1 1 calc R . . C3B C 0.6646(4) 0.1522(3) 0.7683(3) 0.0440(8) Uani 1 1 d . . . H3B H 0.7515 0.1369 0.7998 0.053 Uiso 1 1 calc R . . C2B C 0.63230(11) 0.11426(9) 0.65850(7) 0.0431(8) Uani 1 1 d . . . H2B H 0.7019 0.0798 0.6185 0.052 Uiso 1 1 calc R . . S1G S 0.35664(11) 0.68716(9) 0.52504(7) 0.0428(4) Uani 0.742(3) 1 d PR . . O1G O 0.53394(11) 0.73795(9) 0.56754(7) 0.0508(7) Uani 1 1 d R . . S2G S 0.37055(11) 0.71536(9) 0.61624(7) 0.0557(14) Uani 0.258(3) 1 d PR . . C1G C 0.2927(6) 0.5522(5) 0.5521(4) 0.0855(17) Uani 1 1 d . . . C3G C 0.2732(7) 0.7850(7) 0.6190(5) 0.087(3) Uani 0.796(12) 1 d P . . C2G C 0.2132(19) 0.7306(16) 0.5266(15) 0.045(6) Uani 0.204(12) 1 d P . . H9A H 0.679(4) 0.842(3) 0.688(2) 0.054(11) Uiso 1 1 d D . . H9B H 0.352(4) 0.287(4) 0.545(3) 0.061(12) Uiso 1 1 d 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 O9A 0.0356(11) 0.0281(11) 0.0233(10) 0.0106(8) -0.0024(8) -0.0011(9) C4AA 0.0261(14) 0.0254(14) 0.0200(13) 0.0055(11) -0.0041(10) 0.0021(11) C10A 0.0209(12) 0.0184(13) 0.0215(13) 0.0051(10) 0.0006(10) 0.0032(10) C11A 0.0307(15) 0.0220(14) 0.0269(14) 0.0101(11) -0.0027(11) -0.0045(11) C5A 0.0242(14) 0.0416(18) 0.0309(16) 0.0119(14) -0.0019(12) -0.0022(13) C5AA 0.0234(13) 0.0310(15) 0.0219(14) 0.0096(12) -0.0023(10) 0.0027(11) C9A 0.0264(14) 0.0217(14) 0.0207(13) 0.0065(11) 0.0004(11) 0.0036(11) C3A 0.0481(19) 0.0242(15) 0.0349(17) 0.0016(13) -0.0067(14) 0.0110(14) C8AA 0.0235(13) 0.0263(14) 0.0180(13) 0.0031(11) -0.0040(10) 0.0041(11) C4A 0.0361(16) 0.0221(14) 0.0322(16) 0.0057(12) -0.0058(12) 0.0004(12) C1AA 0.0248(13) 0.0236(14) 0.0171(13) 0.0025(11) -0.0026(10) 0.0017(11) C2A 0.0389(17) 0.0393(18) 0.0348(17) 0.0003(14) 0.0018(13) 0.0187(15) C12A 0.0310(15) 0.0258(15) 0.0233(14) 0.0115(11) 0.0000(11) 0.0013(12) C1A 0.0287(15) 0.0322(16) 0.0291(15) 0.0028(12) 0.0033(12) 0.0064(12) C6A 0.0220(15) 0.065(2) 0.0318(17) 0.0106(16) 0.0013(12) 0.0066(15) C8A 0.0340(16) 0.0311(16) 0.0304(16) 0.0014(13) -0.0022(12) 0.0096(13) C7A 0.0300(16) 0.057(2) 0.0320(17) 0.0013(15) -0.0015(13) 0.0191(15) O9B 0.0388(12) 0.0219(10) 0.0285(11) 0.0090(8) 0.0012(9) 0.0023(9) C9B 0.0253(13) 0.0202(13) 0.0231(14) 0.0051(11) 0.0002(11) 0.0032(11) C8BB 0.0269(14) 0.0180(13) 0.0257(14) 0.0049(11) 0.0030(11) 0.0036(11) C10B 0.0218(13) 0.0219(13) 0.0210(13) 0.0040(11) 0.0013(10) 0.0062(11) C5BB 0.0291(14) 0.0181(13) 0.0262(14) 0.0080(11) 0.0019(11) 0.0013(11) C11B 0.0315(15) 0.0253(14) 0.0242(14) 0.0101(11) 0.0009(11) 0.0028(12) C4BB 0.0267(14) 0.0194(13) 0.0303(15) 0.0088(11) -0.0005(11) 0.0019(11) C5B 0.0427(17) 0.0279(15) 0.0247(15) 0.0101(12) 0.0029(12) 0.0038(13) C6B 0.0506(19) 0.0295(16) 0.0292(16) 0.0044(13) 0.0139(14) 0.0090(14) C12B 0.0346(15) 0.0287(15) 0.0211(14) 0.0078(12) -0.0020(11) 0.0010(12) C1BB 0.0223(13) 0.0165(13) 0.0282(14) 0.0040(11) 0.0007(11) 0.0007(10) C8B 0.0308(15) 0.0303(16) 0.0360(17) 0.0033(13) 0.0005(13) 0.0099(13) C1B 0.0317(15) 0.0248(15) 0.0359(17) 0.0029(12) 0.0045(13) 0.0056(12) C4B 0.0356(16) 0.0325(16) 0.0385(17) 0.0132(14) -0.0058(13) 0.0069(13) C7B 0.0386(17) 0.0322(17) 0.0429(19) 0.0037(14) 0.0135(14) 0.0126(14) C3B 0.0309(16) 0.0365(18) 0.066(2) 0.0206(17) -0.0037(15) 0.0121(14) C2B 0.0310(16) 0.0316(17) 0.061(2) 0.0075(15) 0.0057(15) 0.0122(13) S1G 0.0349(6) 0.0541(8) 0.0275(7) 0.0140(5) -0.0013(4) -0.0051(5) O1G 0.0369(13) 0.0641(17) 0.0342(13) 0.0154(12) -0.0052(10) -0.0091(11) S2G 0.057(2) 0.071(3) 0.042(3) 0.0255(19) 0.0135(17) 0.014(2) C1G 0.080(3) 0.078(3) 0.084(3) 0.051(3) -0.020(3) -0.023(3) C3G 0.053(3) 0.136(7) 0.060(4) 0.012(4) 0.015(3) 0.039(4) C2G 0.029(9) 0.048(11) 0.056(13) 0.017(9) -0.002(7) 0.009(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 O9A C9A 1.423(3) . ? C4AA C4A 1.383(4) . ? C4AA C1AA 1.399(4) . ? C4AA C5AA 1.472(4) . ? C10A C12A 1.382(4) . ? C10A C11A 1.394(4) . ? C10A C9A 1.532(4) . ? C11A C12A 1.387(4) 2_777 ? C5A C6A 1.386(5) . ? C5A C5AA 1.393(4) . ? C5AA C8AA 1.394(4) . ? C9A C1AA 1.527(4) . ? C9A C8AA 1.530(4) . ? C3A C2A 1.377(5) . ? C3A C4A 1.386(5) . ? C8AA C8A 1.381(4) . ? C1AA C1A 1.380(4) . ? C2A C1A 1.399(5) . ? C12A C11A 1.387(4) 2_777 ? C6A C7A 1.381(5) . ? C8A C7A 1.397(5) . ? O9B C9B 1.428(3) . ? C9B C8BB 1.527(4) . ? C9B C10B 1.529(4) . ? C9B C1BB 1.533(4) . ? C8BB C8B 1.379(4) . ? C8BB C5BB 1.396(4) . ? C10B C11B 1.383(4) . ? C10B C12B 1.393(4) . ? C5BB C5B 1.390(4) . ? C5BB C4BB 1.471(4) . ? C11B C12B 1.388(4) 2_556 ? C4BB C4B 1.389(4) . ? C4BB C1BB 1.397(4) . ? C5B C6B 1.385(5) . ? C6B C7B 1.380(5) . ? C12B C11B 1.388(4) 2_556 ? C1BB C1B 1.384(4) . ? C8B C7B 1.393(4) . ? C1B C2B 1.383(3) . ? C4B C3B 1.388(5) . ? C3B C2B 1.425(4) . ? S1G S2G 1.1868 . ? S1G C2G 1.460(17) . ? S1G O1G 1.4848 . ? S1G C3G 1.793(6) . ? S1G C1G 1.797(5) . ? O1G S2G 1.5964 . ? S2G C3G 1.339(7) . ? S2G C1G 1.844(5) . ? S2G C2G 1.860(17) . ? C3G C2G 1.239(19) . ? 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 C4A C4AA C1AA 120.9(3) . . ? C4A C4AA C5AA 130.7(3) . . ? C1AA C4AA C5AA 108.3(2) . . ? C12A C10A C11A 117.9(2) . . ? C12A C10A C9A 122.4(2) . . ? C11A C10A C9A 119.6(2) . . ? C12A C11A C10A 121.5(3) 2_777 . ? C6A C5A C5AA 118.3(3) . . ? C5A C5AA C8AA 120.9(3) . . ? C5A C5AA C4AA 130.4(3) . . ? C8AA C5AA C4AA 108.7(2) . . ? O9A C9A C1AA 113.1(2) . . ? O9A C9A C8AA 113.1(2) . . ? C1AA C9A C8AA 101.0(2) . . ? O9A C9A C10A 107.3(2) . . ? C1AA C9A C10A 110.4(2) . . ? C8AA C9A C10A 111.9(2) . . ? C2A C3A C4A 121.0(3) . . ? C8A C8AA C5AA 120.4(3) . . ? C8A C8AA C9A 128.7(3) . . ? C5AA C8AA C9A 110.8(2) . . ? C4AA C4A C3A 118.4(3) . . ? C1A C1AA C4AA 120.4(3) . . ? C1A C1AA C9A 128.6(3) . . ? C4AA C1AA C9A 111.0(2) . . ? C3A C2A C1A 120.8(3) . . ? C10A C12A C11A 120.6(3) . 2_777 ? C1AA C1A C2A 118.5(3) . . ? C7A C6A C5A 120.9(3) . . ? C8AA C8A C7A 118.6(3) . . ? C6A C7A C8A 120.8(3) . . ? O9B C9B C8BB 106.0(2) . . ? O9B C9B C10B 111.5(2) . . ? C8BB C9B C10B 114.0(2) . . ? O9B C9B C1BB 112.5(2) . . ? C8BB C9B C1BB 101.1(2) . . ? C10B C9B C1BB 111.3(2) . . ? C8B C8BB C5BB 120.5(3) . . ? C8B C8BB C9B 128.6(3) . . ? C5BB C8BB C9B 110.8(2) . . ? C11B C10B C12B 117.8(2) . . ? C11B C10B C9B 121.8(2) . . ? C12B C10B C9B 120.4(2) . . ? C5B C5BB C8BB 120.5(3) . . ? C5B C5BB C4BB 130.8(3) . . ? C8BB C5BB C4BB 108.7(2) . . ? C10B C11B C12B 120.9(3) . 2_556 ? C4B C4BB C1BB 120.5(3) . . ? C4B C4BB C5BB 130.9(3) . . ? C1BB C4BB C5BB 108.6(2) . . ? C6B C5B C5BB 118.6(3) . . ? C7B C6B C5B 120.8(3) . . ? C11B C12B C10B 121.3(3) 2_556 . ? C1B C1BB C4BB 120.6(3) . . ? C1B C1BB C9B 128.6(3) . . ? C4BB C1BB C9B 110.7(2) . . ? C8BB C8B C7B 118.7(3) . . ? C2B C1B C1BB 120.3(3) . . ? C3B C4B C4BB 118.7(3) . . ? C6B C7B C8B 120.8(3) . . ? C4B C3B C2B 121.1(3) . . ? C1B C2B C3B 118.60(19) . . ? S2G S1G C2G 88.7(8) . . ? S2G S1G O1G 72.4 . . ? C2G S1G O1G 137.0(7) . . ? S2G S1G C3G 48.3(2) . . ? C2G S1G C3G 43.3(7) . . ? O1G S1G C3G 101.0(2) . . ? S2G S1G C1G 73.15(18) . . ? C2G S1G C1G 105.3(7) . . ? O1G S1G C1G 105.41(16) . . ? C3G S1G C1G 101.8(3) . . ? S1G O1G S2G 45.1 . . ? S1G S2G C3G 90.2(3) . . ? S1G S2G O1G 62.5 . . ? C3G S2G O1G 119.4(3) . . ? S1G S2G C1G 68.84(15) . . ? C3G S2G C1G 121.3(4) . . ? O1G S2G C1G 98.81(19) . . ? S1G S2G C2G 51.7(6) . . ? C3G S2G C2G 41.7(6) . . ? O1G S2G C2G 104.6(6) . . ? C1G S2G C2G 89.0(6) . . ? S1G C1G S2G 38.02(10) . . ? C2G C3G S2G 92.3(9) . . ? C2G C3G S1G 53.9(8) . . ? S2G C3G S1G 41.45(18) . . ? C3G C2G S1G 82.8(10) . . ? C3G C2G S2G 46.0(6) . . ? S1G C2G S2G 39.6(4) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.537 _refine_diff_density_min -1.864 _refine_diff_density_rms 0.069 data_c:\dejana\struct~1\4 _database_code_CSD 161748 _audit_creation_method SHELXL-97 _chemical_name_systematic 4 ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H38 O4' _chemical_formula_weight 558.72 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' _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 8.3480(10) _cell_length_b 9.2270(10) _cell_length_c 10.369(2) _cell_angle_alpha 96.095(8) _cell_angle_beta 96.159(8) _cell_angle_gamma 106.679(7) _cell_volume 752.77(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 298 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 3460 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.71 _reflns_number_total 2517 _reflns_number_gt 1565 _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^)+(0.0549P)^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 SHELXL _refine_ls_extinction_coef 0.016(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2517 _refine_ls_number_parameters 202 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 O9 O 0.11307(18) 0.49662(15) 0.67030(14) 0.0310(4) Uani 1 1 d D . . C10 C 0.0768(2) 0.5552(2) 0.8932(2) 0.0246(5) Uani 1 1 d . . . C5A C 0.2908(3) 0.8866(2) 0.7869(2) 0.0308(6) Uani 1 1 d . . . C1A C 0.3592(3) 0.6648(2) 0.82341(19) 0.0275(6) Uani 1 1 d . . . C4A C 0.4264(3) 0.8241(2) 0.8327(2) 0.0311(6) Uani 1 1 d . . . C8A C 0.1405(3) 0.7663(2) 0.7504(2) 0.0276(6) Uani 1 1 d . . . C8 C -0.0044(3) 0.7915(3) 0.6938(2) 0.0342(6) Uani 1 1 d . . . H8 H -0.1038 0.7111 0.6690 0.041 Uiso 1 1 calc R . . C9 C 0.1684(3) 0.6159(2) 0.7804(2) 0.0266(6) Uani 1 1 d . . . C1 C 0.4617(3) 0.5760(3) 0.8511(2) 0.0364(6) Uani 1 1 d . . . H1 H 0.4164 0.4704 0.8440 0.044 Uiso 1 1 calc R . . C6 C 0.1474(3) 1.0592(3) 0.7128(2) 0.0440(7) Uani 1 1 d . . . H6 H 0.1483 1.1576 0.7000 0.053 Uiso 1 1 calc R . . C4 C 0.5982(3) 0.8927(3) 0.8740(2) 0.0411(7) Uani 1 1 d . . . H4 H 0.6441 0.9984 0.8826 0.049 Uiso 1 1 calc R . . C5 C 0.2933(3) 1.0342(3) 0.7704(2) 0.0392(7) Uani 1 1 d . . . H5 H 0.3914 1.1155 0.7974 0.047 Uiso 1 1 calc R . . C3 C 0.6999(3) 0.8026(3) 0.9019(2) 0.0470(7) Uani 1 1 d . . . H3 H 0.8149 0.8482 0.9295 0.056 Uiso 1 1 calc R . . C7 C 0.0012(3) 0.9390(3) 0.6745(2) 0.0428(7) Uani 1 1 d . . . H7 H -0.0952 0.9573 0.6351 0.051 Uiso 1 1 calc R . . C2 C 0.6334(3) 0.6455(3) 0.8897(2) 0.0447(7) Uani 1 1 d . . . H2 H 0.7041 0.5862 0.9074 0.054 Uiso 1 1 calc R . . O1G O 0.2297(2) 0.57125(17) 0.44344(15) 0.0360(5) Uani 1 1 d D . . C1G C 0.3544(3) 0.6944(2) 0.4020(2) 0.0344(6) Uani 1 1 d . . . H1GA H 0.3617 0.6658 0.3095 0.041 Uiso 1 1 calc R . . C3G C 0.5215(3) 0.7108(3) 0.4815(3) 0.0454(7) Uani 1 1 d . . . H3G1 H 0.5137 0.7308 0.5730 0.068 Uiso 1 1 calc R . . H3G2 H 0.6069 0.7941 0.4579 0.068 Uiso 1 1 calc R . . H3G3 H 0.5508 0.6180 0.4645 0.068 Uiso 1 1 calc R . . C2G C 0.3034(3) 0.8382(3) 0.4151(3) 0.0457(7) Uani 1 1 d . . . H2G1 H 0.1929 0.8189 0.3668 0.069 Uiso 1 1 calc R . . H2G2 H 0.3831 0.9169 0.3811 0.069 Uiso 1 1 calc R . . H2G3 H 0.3017 0.8707 0.5059 0.069 Uiso 1 1 calc R . . C11 C 0.0020(3) 0.3998(2) 0.8924(2) 0.0301(6) Uani 1 1 d . . . H11 H 0.0031 0.3309 0.8204 0.036 Uiso 1 1 calc R . . C12 C -0.0741(3) 0.3463(2) 0.9973(2) 0.0300(6) Uani 1 1 d . . . H12 H -0.1245 0.2418 0.9942 0.035(6) Uiso 1 1 calc R . . H9 H 0.173(3) 0.526(2) 0.596(2) 0.061(8) Uiso 1 1 d D . . H1G H 0.124(3) 0.563(3) 0.398(3) 0.078(10) Uiso 1 1 d 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 O9 0.0315(9) 0.0326(9) 0.0259(9) 0.0026(8) 0.0051(7) 0.0049(7) C10 0.0188(12) 0.0275(13) 0.0275(13) 0.0074(11) 0.0020(9) 0.0063(10) C5A 0.0328(14) 0.0307(14) 0.0286(13) 0.0056(11) 0.0115(11) 0.0060(11) C1A 0.0256(13) 0.0372(14) 0.0208(13) 0.0071(11) 0.0061(10) 0.0092(11) C4A 0.0265(14) 0.0385(14) 0.0252(13) 0.0052(11) 0.0081(10) 0.0035(11) C8A 0.0303(14) 0.0311(13) 0.0247(13) 0.0071(10) 0.0101(10) 0.0110(11) C8 0.0307(14) 0.0352(14) 0.0416(15) 0.0129(11) 0.0103(11) 0.0134(11) C9 0.0233(13) 0.0297(13) 0.0275(13) 0.0068(11) 0.0042(10) 0.0078(10) C1 0.0317(15) 0.0475(15) 0.0334(14) 0.0106(12) 0.0071(11) 0.0148(12) C6 0.0570(19) 0.0349(15) 0.0507(17) 0.0155(13) 0.0221(14) 0.0221(14) C4 0.0311(16) 0.0491(16) 0.0357(15) 0.0028(12) 0.0089(12) 0.0006(13) C5 0.0467(17) 0.0321(15) 0.0366(15) 0.0018(12) 0.0162(13) 0.0058(12) C3 0.0232(14) 0.072(2) 0.0409(16) 0.0061(14) 0.0039(12) 0.0073(14) C7 0.0440(16) 0.0461(17) 0.0485(16) 0.0159(13) 0.0145(13) 0.0235(13) C2 0.0312(16) 0.0656(19) 0.0414(16) 0.0105(14) 0.0068(12) 0.0196(14) O1G 0.0307(10) 0.0378(10) 0.0374(10) 0.0110(8) 0.0059(8) 0.0048(8) C1G 0.0332(14) 0.0341(14) 0.0366(14) 0.0094(11) 0.0091(11) 0.0085(11) C3G 0.0357(15) 0.0449(15) 0.0571(18) 0.0169(13) 0.0107(13) 0.0099(12) C2G 0.0437(16) 0.0412(15) 0.0522(17) 0.0059(13) 0.0030(13) 0.0145(12) C11 0.0321(13) 0.0290(14) 0.0294(13) 0.0026(11) 0.0072(11) 0.0090(10) C12 0.0285(13) 0.0251(14) 0.0338(14) 0.0059(11) 0.0040(10) 0.0033(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 O9 C9 1.434(3) . ? C10 C12 1.383(3) 2_567 ? C10 C11 1.389(3) . ? C10 C9 1.533(3) . ? C5A C5 1.385(3) . ? C5A C8A 1.399(3) . ? C5A C4A 1.470(3) . ? C1A C1 1.373(3) . ? C1A C4A 1.403(3) . ? C1A C9 1.527(3) . ? C4A C4 1.389(3) . ? C8A C8 1.379(3) . ? C8A C9 1.529(3) . ? C8 C7 1.385(3) . ? C1 C2 1.386(3) . ? C6 C7 1.380(3) . ? C6 C5 1.388(3) . ? C4 C3 1.378(3) . ? C3 C2 1.382(3) . ? O1G C1G 1.442(2) . ? C1G C3G 1.501(3) . ? C1G C2G 1.504(3) . ? C11 C12 1.384(3) . ? C12 C10 1.383(3) 2_567 ? 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 C12 C10 C11 117.75(19) 2_567 . ? C12 C10 C9 120.72(18) 2_567 . ? C11 C10 C9 121.4(2) . . ? C5 C5A C8A 119.8(2) . . ? C5 C5A C4A 131.3(2) . . ? C8A C5A C4A 108.82(19) . . ? C1 C1A C4A 120.8(2) . . ? C1 C1A C9 128.99(19) . . ? C4A C1A C9 110.2(2) . . ? C4 C4A C1A 119.4(2) . . ? C4 C4A C5A 131.9(2) . . ? C1A C4A C5A 108.67(18) . . ? C8 C8A C5A 120.9(2) . . ? C8 C8A C9 128.87(18) . . ? C5A C8A C9 110.17(19) . . ? C8A C8 C7 118.6(2) . . ? O9 C9 C1A 113.00(17) . . ? O9 C9 C8A 113.29(17) . . ? C1A C9 C8A 101.70(16) . . ? O9 C9 C10 107.15(16) . . ? C1A C9 C10 109.64(16) . . ? C8A C9 C10 112.07(18) . . ? C1A C1 C2 119.2(2) . . ? C7 C6 C5 120.5(2) . . ? C3 C4 C4A 119.3(2) . . ? C5A C5 C6 119.1(2) . . ? C4 C3 C2 121.0(2) . . ? C6 C7 C8 121.1(2) . . ? C3 C2 C1 120.2(2) . . ? O1G C1G C3G 107.43(17) . . ? O1G C1G C2G 110.44(18) . . ? C3G C1G C2G 113.3(2) . . ? C12 C11 C10 120.8(2) . . ? C10 C12 C11 121.45(19) 2_567 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C1A C4A C4 -1.8(3) . . . . ? C9 C1A C4A C4 178.31(19) . . . . ? C1 C1A C4A C5A 175.22(19) . . . . ? C9 C1A C4A C5A -4.7(2) . . . . ? C5 C5A C4A C4 0.3(4) . . . . ? C8A C5A C4A C4 176.9(2) . . . . ? C5 C5A C4A C1A -176.2(2) . . . . ? C8A C5A C4A C1A 0.4(2) . . . . ? C5 C5A C8A C8 2.3(3) . . . . ? C4A C5A C8A C8 -174.76(18) . . . . ? C5 C5A C8A C9 -178.92(19) . . . . ? C4A C5A C8A C9 4.0(2) . . . . ? C5A C8A C8 C7 -0.5(3) . . . . ? C9 C8A C8 C7 -179.1(2) . . . . ? C1 C1A C9 O9 -51.4(3) . . . . ? C4A C1A C9 O9 128.45(18) . . . . ? C1 C1A C9 C8A -173.2(2) . . . . ? C4A C1A C9 C8A 6.7(2) . . . . ? C1 C1A C9 C10 68.0(3) . . . . ? C4A C1A C9 C10 -112.11(19) . . . . ? C8 C8A C9 O9 50.7(3) . . . . ? C5A C8A C9 O9 -128.00(18) . . . . ? C8 C8A C9 C1A 172.3(2) . . . . ? C5A C8A C9 C1A -6.4(2) . . . . ? C8 C8A C9 C10 -70.7(3) . . . . ? C5A C8A C9 C10 110.60(19) . . . . ? C12 C10 C9 O9 -165.44(19) 2_567 . . . ? C11 C10 C9 O9 18.1(3) . . . . ? C12 C10 C9 C1A 71.6(3) 2_567 . . . ? C11 C10 C9 C1A -104.9(2) . . . . ? C12 C10 C9 C8A -40.6(3) 2_567 . . . ? C11 C10 C9 C8A 143.0(2) . . . . ? C4A C1A C1 C2 0.5(3) . . . . ? C9 C1A C1 C2 -179.6(2) . . . . ? C1A C4A C4 C3 1.5(3) . . . . ? C5A C4A C4 C3 -174.7(2) . . . . ? C8A C5A C5 C6 -2.5(3) . . . . ? C4A C5A C5 C6 173.8(2) . . . . ? C7 C6 C5 C5A 1.0(3) . . . . ? C4A C4 C3 C2 -0.1(3) . . . . ? C5 C6 C7 C8 0.8(4) . . . . ? C8A C8 C7 C6 -1.0(3) . . . . ? C4 C3 C2 C1 -1.2(3) . . . . ? C1A C1 C2 C3 0.9(3) . . . . ? C12 C10 C11 C12 0.7(3) 2_567 . . . ? C9 C10 C11 C12 177.27(19) . . . . ? C10 C11 C12 C10 -0.7(4) . . . 2_567 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.204 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.048