# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1460 data_global _publ_contact_author 'Andrei S.Batsanov' _publ_contact_author_email a.s.batsanov@durham.ac.uk loop_ _publ_author_name 'Christensen, Christian A.' 'Bryce, Martin R.' 'Batsanov, Andrei S.' 'Howard, Judith A. K.' 'Jeppesen, Jan O.' 'Becher, Jan' _journal_name_full 'Chemical Communications' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1999' _ccdc_journal_depnumber '?' _publ_section_title ; The first Diels-Alder reaction of a 9,10-bis(1,3-dithiol-2-ylidene)- 9,10-dihydroanthracene derivative: synthesis and crystal structure of a novel donor-\p-anthraquinone diad. ; #====================================================================== data_(10) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '229-230 deg.C' _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 O2 S6' _chemical_formula_weight 793.12 _ccdc_compound_id '10' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; none ; _ccdc_comments '?' 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 9.925(2) _cell_length_b 12.940(3) _cell_length_c 15.319(5) _cell_angle_alpha 94.16(1) _cell_angle_beta 94.13(1) _cell_angle_gamma 99.06(1) _cell_volume 1930.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 589 _cell_measurement_theta_min 12 _cell_measurement_theta_max 24 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8835 _exptl_absorpt_correction_T_max 0.9858 _exptl_absorpt_process_details 'numerical integration correction negligible' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 -1.00 0.0200 0.00 0.00 1.00 0.0200 0.00 -1.00 -1.00 0.0500 0.00 1.00 1.00 0.0500 1.00 -1.00 0.00 0.2100 -1.00 1.00 0.00 0.2100 _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 15 s), each set at different \f and/or 2\q angles, nominally covered over a hemisphere of reciprocal space. The first 50 scans were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13240 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6762 _reflns_number_gt 4525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6762 _refine_ls_number_parameters 629 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.014 _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 0.30878(7) 0.54504(5) 0.12221(4) 0.01908(17) Uani 1 1 d . . . S2 S 0.53966(7) 0.43195(5) 0.10516(5) 0.01992(17) Uani 1 1 d . . . S3 S -0.00704(7) 0.18244(5) 0.35898(4) 0.01990(17) Uani 1 1 d . . . S4 S 0.22808(7) 0.06787(5) 0.35859(4) 0.01880(17) Uani 1 1 d . . . S5 S 0.49087(8) 0.75684(5) 0.16131(5) 0.02497(19) Uani 1 1 d . . . S6 S 0.75409(8) 0.62251(6) 0.13966(5) 0.02845(19) Uani 1 1 d . . . O1 O -0.0825(2) 0.23837(15) 0.70157(12) 0.0295(5) Uani 1 1 d . . . O2 O 0.3289(2) 0.01605(15) 0.70487(12) 0.0280(5) Uani 1 1 d . . . C1 C 0.0464(3) 0.3765(2) 0.07216(17) 0.0189(6) Uani 1 1 d . . . H1 H 0.090(2) 0.4282(18) 0.0338(15) 0.011(6) Uiso 1 1 d . . . C2 C -0.0945(3) 0.3610(2) 0.07350(18) 0.0211(6) Uani 1 1 d . . . H2 H -0.149(3) 0.3975(18) 0.0384(15) 0.011(6) Uiso 1 1 d . . . C3 C -0.1594(3) 0.2844(2) 0.12241(19) 0.0217(6) Uani 1 1 d . . . H3 H -0.254(3) 0.274(2) 0.1259(17) 0.026(8) Uiso 1 1 d . . . C4 C -0.0815(3) 0.2243(2) 0.17027(17) 0.0168(6) Uani 1 1 d . . . H4 H -0.126(3) 0.169(2) 0.2031(16) 0.021(7) Uiso 1 1 d . . . C5 C 0.3111(3) 0.0522(2) 0.17044(17) 0.0185(6) Uani 1 1 d . . . H5 H 0.265(2) 0.0036(18) 0.2015(15) 0.008(6) Uiso 1 1 d . . . C6 C 0.4211(3) 0.0322(2) 0.12461(18) 0.0210(6) Uani 1 1 d . . . H6 H 0.452(3) -0.037(2) 0.1276(16) 0.020(7) Uiso 1 1 d . . . C7 C 0.4833(3) 0.1073(2) 0.07382(18) 0.0213(6) Uani 1 1 d . . . H7 H 0.555(3) 0.0921(19) 0.0399(16) 0.019(7) Uiso 1 1 d . . . C8 C 0.4356(3) 0.2020(2) 0.06937(18) 0.0185(6) Uani 1 1 d . . . H8 H 0.470(3) 0.251(2) 0.0305(17) 0.024(8) Uiso 1 1 d . . . C9 C 0.2764(3) 0.32645(19) 0.11594(16) 0.0151(6) Uani 1 1 d . . . C10 C 0.1480(3) 0.17350(18) 0.21689(16) 0.0149(6) Uani 1 1 d . . . C11 C 0.0613(3) 0.23953(19) 0.17042(16) 0.0156(6) Uani 1 1 d . . . C12 C 0.1270(3) 0.31754(19) 0.12010(16) 0.0158(6) Uani 1 1 d . . . C13 C 0.3289(3) 0.22555(19) 0.11725(16) 0.0154(6) Uani 1 1 d . . . C14 C 0.2637(3) 0.14820(19) 0.16930(16) 0.0149(6) Uani 1 1 d . . . C15 C 0.3614(3) 0.42016(19) 0.11358(16) 0.0159(6) Uani 1 1 d . . . C16 C 0.4743(3) 0.62000(19) 0.14308(16) 0.0175(6) Uani 1 1 d . . . C17 C 0.5803(3) 0.5676(2) 0.13433(17) 0.0201(6) Uani 1 1 d . . . C18 C 0.1249(3) 0.14367(19) 0.29833(17) 0.0167(6) Uani 1 1 d . . . C19 C 0.0577(3) 0.15060(19) 0.46104(17) 0.0187(6) Uani 1 1 d . . . C20 C 0.1673(3) 0.09574(19) 0.46126(16) 0.0168(6) Uani 1 1 d . . . C21 C 0.3985(3) 0.7754(2) 0.25868(19) 0.0260(7) Uani 1 1 d . . . H211 H 0.403(3) 0.850(2) 0.2645(19) 0.044(9) Uiso 1 1 d . . . H212 H 0.305(3) 0.7460(19) 0.2447(16) 0.017(7) Uiso 1 1 d . . . C22 C 0.4609(3) 0.7400(2) 0.34199(19) 0.0231(7) Uani 1 1 d . . . H221 H 0.558(3) 0.768(2) 0.3495(18) 0.028(8) Uiso 1 1 d . . . H222 H 0.459(3) 0.661(2) 0.3368(16) 0.023(7) Uiso 1 1 d . . . C23 C 0.3891(4) 0.7715(3) 0.4219(2) 0.0314(8) Uani 1 1 d . . . H231 H 0.391(3) 0.850(2) 0.4273(18) 0.036(8) Uiso 1 1 d . . . H232 H 0.291(4) 0.739(3) 0.410(2) 0.058(11) Uiso 1 1 d . . . C24 C 0.4445(4) 0.7359(3) 0.5081(2) 0.0297(7) Uani 1 1 d . . . H241 H 0.440(3) 0.658(2) 0.5020(17) 0.028(8) Uiso 1 1 d . . . H242 H 0.537(3) 0.766(2) 0.5169(19) 0.037(9) Uiso 1 1 d . . . C25 C 0.3692(5) 0.7669(3) 0.5864(2) 0.0475(10) Uani 1 1 d . . . H251 H 0.269(4) 0.737(3) 0.574(3) 0.080(14) Uiso 1 1 d . . . H252 H 0.378(3) 0.842(3) 0.591(2) 0.056(11) Uiso 1 1 d . . . C26 C 0.4218(5) 0.7310(4) 0.6730(3) 0.0523(11) Uani 1 1 d . . . H261 H 0.424(4) 0.647(3) 0.666(2) 0.074(12) Uiso 1 1 d . . . H262 H 0.375(5) 0.749(3) 0.718(3) 0.091(17) Uiso 1 1 d . . . H263 H 0.518(4) 0.755(3) 0.686(2) 0.071(14) Uiso 1 1 d . . . C27 C 0.8205(3) 0.5600(2) 0.2334(2) 0.0292(7) Uani 1 1 d . . . H271 H 0.805(3) 0.484(2) 0.2199(18) 0.033(8) Uiso 1 1 d . . . H272 H 0.912(3) 0.588(2) 0.2386(17) 0.022(8) Uiso 1 1 d . . . C28 C 0.7544(3) 0.5849(2) 0.3167(2) 0.0288(7) Uani 1 1 d . . . H281 H 0.657(3) 0.551(2) 0.3095(16) 0.022(7) Uiso 1 1 d . . . H282 H 0.764(3) 0.664(2) 0.3237(19) 0.046(9) Uiso 1 1 d . . . C29 C 0.8197(4) 0.5438(3) 0.3974(2) 0.0354(8) Uani 1 1 d . . . H291 H 0.915(3) 0.576(2) 0.4071(19) 0.039(9) Uiso 1 1 d . . . H292 H 0.815(3) 0.465(3) 0.3858(19) 0.046(9) Uiso 1 1 d . . . C30 C 0.7477(4) 0.5671(3) 0.4800(2) 0.0350(8) Uani 1 1 d . . . H301 H 0.750(3) 0.643(2) 0.4865(17) 0.032(8) Uiso 1 1 d . . . H302 H 0.643(3) 0.531(2) 0.4703(19) 0.043(9) Uiso 1 1 d . . . C31 C 0.8112(4) 0.5305(3) 0.5638(2) 0.0465(10) Uani 1 1 d . . . H311 H 0.807(3) 0.451(3) 0.553(2) 0.054(10) Uiso 1 1 d . . . H312 H 0.910(3) 0.563(2) 0.572(2) 0.047(10) Uiso 1 1 d . . . C32 C 0.7384(6) 0.5555(4) 0.6442(3) 0.0602(13) Uani 1 1 d . . . H321 H 0.730(4) 0.632(3) 0.652(2) 0.064(12) Uiso 1 1 d . . . H322 H 0.781(4) 0.531(3) 0.690(3) 0.086(16) Uiso 1 1 d . . . H323 H 0.638(4) 0.523(3) 0.635(2) 0.062(12) Uiso 1 1 d . . . C33 C 0.0001(3) 0.1773(2) 0.53960(19) 0.0214(7) Uani 1 1 d . . . H33 H -0.061(3) 0.214(2) 0.5411(19) 0.038(10) Uiso 1 1 d . . . C34 C 0.0577(3) 0.1454(2) 0.61871(17) 0.0205(6) Uani 1 1 d . . . C35 C 0.0001(3) 0.1774(2) 0.70168(18) 0.0236(7) Uani 1 1 d . . . C36 C 0.0485(3) 0.1357(2) 0.78404(18) 0.0217(6) Uani 1 1 d . . . C37 C -0.0110(3) 0.1568(2) 0.86169(19) 0.0261(7) Uani 1 1 d . . . H37 H -0.081(3) 0.1935(18) 0.8592(15) 0.009(7) Uiso 1 1 d . . . C38 C 0.0372(3) 0.1223(2) 0.9393(2) 0.0309(8) Uani 1 1 d . . . H38 H 0.000(3) 0.139(2) 0.9928(19) 0.034(9) Uiso 1 1 d . . . C39 C 0.1460(3) 0.0667(2) 0.9399(2) 0.0297(8) Uani 1 1 d . . . H39 H 0.173(3) 0.047(2) 0.9918(19) 0.029(8) Uiso 1 1 d . . . C40 C 0.2066(3) 0.0460(2) 0.86358(19) 0.0247(7) Uani 1 1 d . . . H40 H 0.281(3) 0.0098(19) 0.8631(16) 0.013(7) Uiso 1 1 d . . . C41 C 0.1585(3) 0.07932(19) 0.78499(18) 0.0210(6) Uani 1 1 d . . . C42 C 0.2261(3) 0.0578(2) 0.70343(18) 0.0221(6) Uani 1 1 d . . . C43 C 0.1668(3) 0.0899(2) 0.61926(17) 0.0196(6) Uani 1 1 d . . . C44 C 0.2258(3) 0.0640(2) 0.54018(18) 0.0211(6) Uani 1 1 d . . . H44 H 0.292(3) 0.026(2) 0.5397(17) 0.024(8) 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 S1 0.0197(4) 0.0150(3) 0.0232(4) 0.0038(3) 0.0033(3) 0.0031(3) S2 0.0164(4) 0.0154(3) 0.0276(4) 0.0009(3) 0.0042(3) 0.0007(3) S3 0.0186(4) 0.0260(4) 0.0171(4) 0.0061(3) 0.0043(3) 0.0066(3) S4 0.0214(4) 0.0212(4) 0.0159(4) 0.0052(3) 0.0037(3) 0.0072(3) S5 0.0361(5) 0.0143(3) 0.0249(4) 0.0016(3) 0.0110(4) 0.0013(3) S6 0.0212(4) 0.0253(4) 0.0359(5) -0.0015(3) 0.0071(4) -0.0055(3) O1 0.0258(12) 0.0390(12) 0.0251(12) 0.0003(9) 0.0063(10) 0.0088(10) O2 0.0299(12) 0.0334(11) 0.0219(11) 0.0052(9) -0.0003(10) 0.0087(10) C1 0.0223(17) 0.0189(14) 0.0159(15) 0.0044(12) 0.0023(13) 0.0022(12) C2 0.0219(17) 0.0219(15) 0.0207(16) 0.0053(12) -0.0034(14) 0.0081(12) C3 0.0144(16) 0.0236(15) 0.0264(17) 0.0019(12) 0.0012(14) 0.0010(13) C4 0.0175(16) 0.0197(14) 0.0135(14) 0.0036(12) 0.0034(12) 0.0024(12) C5 0.0224(17) 0.0178(14) 0.0141(15) 0.0030(12) 0.0013(13) -0.0010(12) C6 0.0254(17) 0.0158(14) 0.0229(16) 0.0004(12) 0.0025(13) 0.0073(12) C7 0.0192(16) 0.0231(15) 0.0223(16) -0.0021(12) 0.0065(13) 0.0055(13) C8 0.0202(16) 0.0198(14) 0.0139(15) 0.0007(12) 0.0043(13) -0.0021(12) C9 0.0178(15) 0.0176(13) 0.0098(14) 0.0031(11) -0.0002(12) 0.0026(11) C10 0.0155(15) 0.0134(13) 0.0147(14) 0.0002(11) 0.0006(12) 0.0001(11) C11 0.0176(15) 0.0166(13) 0.0127(14) -0.0020(11) 0.0016(12) 0.0048(11) C12 0.0187(15) 0.0159(13) 0.0121(14) -0.0020(11) 0.0020(12) 0.0018(11) C13 0.0155(15) 0.0154(13) 0.0146(14) 0.0014(11) -0.0018(12) 0.0012(11) C14 0.0172(15) 0.0149(13) 0.0109(14) -0.0016(11) -0.0030(12) 0.0003(11) C15 0.0185(15) 0.0184(13) 0.0120(14) 0.0035(11) 0.0029(12) 0.0050(11) C16 0.0217(16) 0.0147(13) 0.0151(14) 0.0011(11) 0.0038(12) -0.0013(12) C17 0.0225(16) 0.0169(13) 0.0196(15) 0.0009(11) 0.0048(13) -0.0021(12) C18 0.0139(15) 0.0165(13) 0.0202(15) 0.0017(11) 0.0021(12) 0.0036(11) C19 0.0190(16) 0.0192(14) 0.0167(15) 0.0039(11) 0.0016(12) -0.0019(12) C20 0.0181(15) 0.0166(13) 0.0146(14) 0.0015(11) 0.0023(12) -0.0008(11) C21 0.030(2) 0.0255(17) 0.0238(17) -0.0004(13) 0.0075(15) 0.0059(14) C22 0.0209(17) 0.0242(16) 0.0248(17) 0.0017(13) 0.0040(14) 0.0049(13) C23 0.038(2) 0.0342(18) 0.0255(18) 0.0007(14) 0.0061(16) 0.0152(16) C24 0.028(2) 0.0339(18) 0.0252(18) 0.0036(14) 0.0012(15) 0.0007(15) C25 0.062(3) 0.058(3) 0.026(2) 0.0034(18) 0.007(2) 0.021(2) C26 0.058(3) 0.069(3) 0.026(2) 0.007(2) 0.001(2) -0.001(2) C27 0.0164(18) 0.0286(17) 0.040(2) -0.0084(15) -0.0016(15) 0.0023(14) C28 0.0225(19) 0.0293(17) 0.0326(19) -0.0058(14) 0.0010(15) 0.0029(14) C29 0.029(2) 0.0318(18) 0.043(2) -0.0060(16) -0.0071(17) 0.0048(15) C30 0.041(2) 0.0286(18) 0.033(2) -0.0012(15) -0.0021(17) 0.0024(16) C31 0.054(3) 0.036(2) 0.044(2) 0.0004(17) -0.009(2) -0.0028(19) C32 0.081(4) 0.052(3) 0.038(3) 0.002(2) 0.001(3) -0.016(3) C33 0.0212(17) 0.0227(15) 0.0219(16) 0.0029(12) 0.0040(13) 0.0073(13) C34 0.0187(16) 0.0227(14) 0.0184(15) 0.0025(12) 0.0026(13) -0.0026(12) C35 0.0197(17) 0.0260(15) 0.0226(16) -0.0034(13) 0.0018(13) -0.0018(13) C36 0.0202(16) 0.0210(14) 0.0203(16) 0.0007(12) 0.0002(13) -0.0066(12) C37 0.0237(18) 0.0258(16) 0.0251(18) -0.0042(13) 0.0052(14) -0.0060(14) C38 0.036(2) 0.0319(17) 0.0181(17) -0.0019(14) 0.0050(15) -0.0130(15) C39 0.037(2) 0.0298(17) 0.0155(17) 0.0036(14) -0.0033(15) -0.0139(15) C40 0.0251(18) 0.0238(15) 0.0215(17) 0.0005(13) -0.0034(14) -0.0042(14) C41 0.0220(17) 0.0182(14) 0.0184(15) -0.0017(12) 0.0011(13) -0.0085(12) C42 0.0205(17) 0.0201(14) 0.0231(17) 0.0008(12) -0.0014(13) -0.0027(13) C43 0.0194(16) 0.0188(14) 0.0179(15) 0.0025(11) -0.0010(13) -0.0046(12) C44 0.0232(17) 0.0217(15) 0.0176(16) 0.0018(12) 0.0004(13) 0.0024(13) _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 C16 1.766(3) . ? S1 C15 1.774(3) . ? S2 C17 1.755(3) . ? S2 C15 1.766(3) . ? S3 C19 1.749(3) . ? S3 C18 1.774(3) . ? S4 C20 1.758(3) . ? S4 C18 1.782(3) . ? S5 C16 1.752(2) . ? S5 C21 1.827(3) . ? S6 C17 1.753(3) . ? S6 C27 1.830(3) . ? O1 C35 1.224(3) . ? O2 C42 1.227(3) . ? C1 C2 1.383(4) . ? C1 C12 1.397(4) . ? C2 C3 1.392(4) . ? C3 C4 1.389(4) . ? C4 C11 1.400(4) . ? C5 C6 1.387(4) . ? C5 C14 1.397(3) . ? C6 C7 1.386(4) . ? C7 C8 1.387(4) . ? C8 C13 1.390(4) . ? C9 C15 1.368(3) . ? C9 C12 1.475(4) . ? C9 C13 1.481(3) . ? C10 C18 1.357(3) . ? C10 C14 1.471(3) . ? C10 C11 1.486(3) . ? C11 C12 1.420(3) . ? C13 C14 1.429(3) . ? C16 C17 1.348(4) . ? C19 C20 1.389(4) . ? C19 C33 1.413(4) . ? C20 C44 1.419(4) . ? C21 C22 1.511(4) . ? C22 C23 1.522(4) . ? C23 C24 1.524(4) . ? C24 C25 1.521(5) . ? C25 C26 1.521(5) . ? C27 C28 1.512(4) . ? C28 C29 1.524(4) . ? C29 C30 1.530(4) . ? C30 C31 1.528(5) . ? C31 C32 1.512(6) . ? C33 C34 1.419(4) . ? C34 C43 1.391(4) . ? C34 C35 1.489(4) . ? C35 C36 1.486(4) . ? C36 C37 1.394(4) . ? C36 C41 1.405(4) . ? C37 C38 1.380(4) . ? C38 C39 1.388(5) . ? C39 C40 1.380(4) . ? C40 C41 1.386(4) . ? C41 C42 1.490(4) . ? C42 C43 1.492(4) . ? C43 C44 1.424(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 C16 S1 C15 96.65(12) . . ? C17 S2 C15 97.09(12) . . ? C19 S3 C18 96.37(13) . . ? C20 S4 C18 96.26(12) . . ? C16 S5 C21 103.44(13) . . ? C17 S6 C27 100.30(14) . . ? C2 C1 C12 121.5(3) . . ? C1 C2 C3 120.1(3) . . ? C4 C3 C2 119.5(3) . . ? C3 C4 C11 121.3(2) . . ? C6 C5 C14 121.6(2) . . ? C7 C6 C5 119.8(3) . . ? C6 C7 C8 119.8(3) . . ? C7 C8 C13 121.6(2) . . ? C15 C9 C12 123.3(2) . . ? C15 C9 C13 122.0(2) . . ? C12 C9 C13 114.6(2) . . ? C18 C10 C14 123.2(2) . . ? C18 C10 C11 122.2(2) . . ? C14 C10 C11 114.5(2) . . ? C4 C11 C12 119.0(2) . . ? C4 C11 C10 123.0(2) . . ? C12 C11 C10 117.8(2) . . ? C1 C12 C11 118.6(2) . . ? C1 C12 C9 123.3(2) . . ? C11 C12 C9 117.9(2) . . ? C8 C13 C14 118.9(2) . . ? C8 C13 C9 123.4(2) . . ? C14 C13 C9 117.7(2) . . ? C5 C14 C13 118.3(2) . . ? C5 C14 C10 123.7(2) . . ? C13 C14 C10 117.9(2) . . ? C9 C15 S2 123.9(2) . . ? C9 C15 S1 124.7(2) . . ? S2 C15 S1 111.35(14) . . ? C17 C16 S5 124.3(2) . . ? C17 C16 S1 116.40(19) . . ? S5 C16 S1 118.92(15) . . ? C16 C17 S6 126.6(2) . . ? C16 C17 S2 116.8(2) . . ? S6 C17 S2 116.36(15) . . ? C10 C18 S3 123.2(2) . . ? C10 C18 S4 124.3(2) . . ? S3 C18 S4 112.46(14) . . ? C20 C19 C33 121.3(2) . . ? C20 C19 S3 116.8(2) . . ? C33 C19 S3 121.9(2) . . ? C19 C20 C44 121.5(2) . . ? C19 C20 S4 116.2(2) . . ? C44 C20 S4 122.3(2) . . ? C22 C21 S5 115.4(2) . . ? C21 C22 C23 111.9(2) . . ? C22 C23 C24 114.7(3) . . ? C25 C24 C23 113.6(3) . . ? C24 C25 C26 114.4(3) . . ? C28 C27 S6 112.8(2) . . ? C27 C28 C29 113.4(3) . . ? C28 C29 C30 112.1(3) . . ? C31 C30 C29 114.5(3) . . ? C32 C31 C30 113.2(4) . . ? C19 C33 C34 117.5(3) . . ? C43 C34 C33 121.5(3) . . ? C43 C34 C35 121.2(2) . . ? C33 C34 C35 117.3(3) . . ? O1 C35 C36 121.4(3) . . ? O1 C35 C34 120.3(3) . . ? C36 C35 C34 118.2(2) . . ? C37 C36 C41 119.7(3) . . ? C37 C36 C35 119.9(3) . . ? C41 C36 C35 120.2(2) . . ? C38 C37 C36 120.4(3) . . ? C37 C38 C39 119.7(3) . . ? C40 C39 C38 120.6(3) . . ? C39 C40 C41 120.4(3) . . ? C40 C41 C36 119.3(3) . . ? C40 C41 C42 119.8(3) . . ? C36 C41 C42 120.9(2) . . ? O2 C42 C41 121.4(3) . . ? O2 C42 C43 120.4(3) . . ? C41 C42 C43 118.2(2) . . ? C34 C43 C44 121.0(3) . . ? C34 C43 C42 120.4(2) . . ? C44 C43 C42 118.6(2) . . ? C20 C44 C43 117.3(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 C17 C16 S5 C21 -126.9(2) . . . . ? C16 S5 C21 C22 65.7(3) . . . . ? S5 C21 C22 C23 172.3(2) . . . . ? C21 C22 C23 C24 178.6(3) . . . . ? C22 C23 C24 C25 -179.0(3) . . . . ? C23 C24 C25 C26 179.3(4) . . . . ? C16 C17 S6 C27 119.2(3) . . . . ? C17 S6 C27 C28 -59.6(2) . . . . ? S6 C27 C28 C29 -173.4(2) . . . . ? C27 C28 C29 C30 -178.2(3) . . . . ? C28 C29 C30 C31 -178.4(3) . . . . ? C29 C30 C31 C32 179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.321 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.057 #========================================================END data_(14) _ccdc_compound_id '14' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; Methyl and -C(O)H groups in both independent molecules are statistically mixed: the O(1A), O(2A), O(1B), O(2B) atoms and two (out of three) H atoms at C(33), C(34), C(67) and C(68), have 50% occupancies. One of hexyl chains is also disordered: C(61), C(63), C(64) and C(66) (with their H atoms) are disordered over two positions, A with 64% occupancy, B with 36% occupancy. ; _ccdc_comments '?' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '178-179 deg.C' _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 O S6' _chemical_formula_weight 655.00 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 15.208(3) _cell_length_b 16.298(3) _cell_length_c 16.510(3) _cell_angle_alpha 111.95(1) _cell_angle_beta 95.52(1) _cell_angle_gamma 113.86(1) _cell_volume 3320(1) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 863 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 22.5 _exptl_crystal_description plate _exptl_crystal_colour amber _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8619 _exptl_absorpt_correction_T_max 0.9827 _exptl_absorpt_process_details 'XPREP (SHELX) program, R(int)=0.043 before correction' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 -1.00 0.0400 -1.00 0.00 1.00 0.0400 0.00 1.00 -1.00 0.1200 -1.00 0.00 -1.00 0.1500 0.00 -1.00 1.00 0.1200 1.00 0.00 1.00 0.1600 _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 15 s), each set at different \f and/or 2\q angles, nominally covered over a hemisphere of reciprocal space. The first 50 scans were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25912 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12113 _reflns_number_gt 8781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.9952P] 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 12113 _refine_ls_number_parameters 759 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.063 _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 -0.05032(5) 0.58238(5) -0.00819(5) 0.02609(16) Uani 1 1 d . . . S2 S 0.16122(5) 0.72149(5) 0.09693(5) 0.02742(17) Uani 1 1 d . . . S3 S -0.05110(6) 0.90483(6) -0.16325(5) 0.03149(18) Uani 1 1 d . . . S4 S 0.16087(6) 1.04238(5) -0.05372(5) 0.03275(18) Uani 1 1 d . . . S5 S -0.10605(6) 0.53986(6) 0.14818(5) 0.03399(18) Uani 1 1 d . . . S6 S 0.13390(6) 0.70884(6) 0.27018(5) 0.03393(19) Uani 1 1 d . . . O1A O -0.1686(4) 1.0058(4) -0.1578(4) 0.0538(14) Uani 0.50 1 d P A 1 O1B O 0.2040(4) 1.2511(3) 0.0413(3) 0.0511(13) Uani 0.50 1 d P B 2 C1 C -0.0690(2) 0.6939(2) -0.27214(19) 0.0300(7) Uani 1 1 d . . . H1 H -0.0678 0.7390 -0.2959 0.036 Uiso 1 1 d R . . C2 C -0.1412(2) 0.5933(2) -0.3194(2) 0.0323(7) Uani 1 1 d . . . H2 H -0.1898 0.5705 -0.3742 0.039 Uiso 1 1 d R . . C3 C -0.1432(2) 0.5260(2) -0.2863(2) 0.0326(7) Uani 1 1 d . . . H3 H -0.1930 0.4573 -0.3183 0.039 Uiso 1 1 d R . . C4 C -0.0712(2) 0.5597(2) -0.20602(19) 0.0284(6) Uani 1 1 d . . . H4 H -0.0717 0.5132 -0.1843 0.034 Uiso 1 1 d R . . C5 C 0.2720(2) 0.7821(2) -0.0333(2) 0.0299(7) Uani 1 1 d . . . H5 H 0.2722 0.7351 -0.0125 0.036 Uiso 1 1 d R . . C6 C 0.3622(2) 0.8549(2) -0.0307(2) 0.0349(7) Uani 1 1 d . . . H6 H 0.4239 0.8593 -0.0058 0.042 Uiso 1 1 d R . . C7 C 0.3626(2) 0.9211(2) -0.0640(2) 0.0346(7) Uani 1 1 d . . . H7 H 0.4244 0.9697 -0.0636 0.042 Uiso 1 1 d R . . C8 C 0.2730(2) 0.9168(2) -0.09861(19) 0.0295(7) Uani 1 1 d . . . H8 H 0.2740 0.9624 -0.1218 0.035 Uiso 1 1 d R . . C9 C 0.0829(2) 0.8355(2) -0.13802(18) 0.0238(6) Uani 1 1 d . . . C10 C 0.0818(2) 0.70043(19) -0.07260(18) 0.0234(6) Uani 1 1 d . . . C11 C 0.1805(2) 0.7773(2) -0.06657(18) 0.0248(6) Uani 1 1 d . . . C12 C 0.1812(2) 0.8460(2) -0.09951(18) 0.0245(6) Uani 1 1 d . . . C13 C 0.0026(2) 0.7295(2) -0.19041(19) 0.0254(6) Uani 1 1 d . . . C14 C 0.0016(2) 0.6608(2) -0.15685(18) 0.0236(6) Uani 1 1 d . . . C15 C 0.0671(2) 0.67170(19) -0.00561(19) 0.0245(6) Uani 1 1 d . . . C16 C -0.0171(2) 0.6093(2) 0.10763(19) 0.0264(6) Uani 1 1 d . . . C17 C 0.0797(2) 0.6737(2) 0.15574(19) 0.0272(6) Uani 1 1 d . . . C18 C 0.0671(2) 0.9157(2) -0.12222(19) 0.0260(6) Uani 1 1 d . . . C19 C -0.0175(3) 1.0316(2) -0.0978(2) 0.0350(7) Uani 1 1 d . A . C20 C 0.0793(3) 1.0945(2) -0.0474(2) 0.0362(8) Uani 1 1 d . A . C21 C 0.1577(2) 0.8390(2) 0.3229(2) 0.0359(7) Uani 1 1 d . . . H211 H 0.1825 0.8675 0.3900 0.047 Uiso 1 1 d R . . H212 H 0.2107 0.8792 0.3026 0.047 Uiso 1 1 d R . . C22 C 0.0629(3) 0.8474(2) 0.2986(2) 0.0429(8) Uani 1 1 d . . . H221 H 0.0433 0.8269 0.2323 0.056 Uiso 1 1 d R . . H222 H 0.0075 0.7999 0.3112 0.056 Uiso 1 1 d R . . C23 C 0.0758(3) 0.9514(3) 0.3501(2) 0.0512(9) Uani 1 1 d . . . H231 H 0.1357 1.0000 0.3427 0.067 Uiso 1 1 d R . . H232 H 0.0882 0.9692 0.4158 0.067 Uiso 1 1 d R . . C24 C -0.0158(3) 0.9612(3) 0.3179(2) 0.0453(9) Uani 1 1 d . . . H241 H -0.0228 0.9517 0.2543 0.059 Uiso 1 1 d R . . H242 H -0.0768 0.9067 0.3176 0.059 Uiso 1 1 d R . . C25 C -0.0096(3) 1.0603(3) 0.3757(3) 0.0575(10) Uani 1 1 d . . . H251 H 0.0516 1.1150 0.3764 0.075 Uiso 1 1 d R . . H252 H -0.0033 1.0697 0.4392 0.075 Uiso 1 1 d R . . C26 C -0.1007(3) 1.0688(3) 0.3420(3) 0.0620(11) Uani 1 1 d . . . H261 H -0.1053 1.0635 0.2805 0.097(9) Uiso 1 1 d R . . H262 H -0.0937 1.1340 0.3835 0.097(9) Uiso 1 1 d R . . H263 H -0.1618 1.0145 0.3406 0.097(9) Uiso 1 1 d R . . C27 C -0.2194(2) 0.5417(2) 0.1044(2) 0.0327(7) Uani 1 1 d . . . H271 H -0.2357 0.5126 0.0371 0.043 Uiso 1 1 d R . . H272 H -0.2758 0.4977 0.1191 0.043 Uiso 1 1 d R . . C28 C -0.2132(2) 0.6449(2) 0.1409(2) 0.0355(7) Uani 1 1 d . . . H281 H -0.1656 0.6858 0.1173 0.046 Uiso 1 1 d R . . H282 H -0.1866 0.6791 0.2083 0.046 Uiso 1 1 d R . . C29 C -0.3147(2) 0.6391(2) 0.1141(2) 0.0388(8) Uani 1 1 d . . . H291 H -0.3631 0.5948 0.1346 0.050 Uiso 1 1 d R . . H292 H -0.3394 0.6080 0.0467 0.050 Uiso 1 1 d R . . C30 C -0.3126(3) 0.7409(3) 0.1536(2) 0.0464(9) Uani 1 1 d . . . H301 H -0.2856 0.7734 0.2209 0.060 Uiso 1 1 d R . . H302 H -0.2665 0.7845 0.1311 0.060 Uiso 1 1 d R . . C31 C -0.4139(3) 0.7338(3) 0.1295(3) 0.0583(10) Uani 1 1 d . . . H311 H -0.4596 0.6909 0.1529 0.076 Uiso 1 1 d R . . H312 H -0.4414 0.7001 0.0622 0.076 Uiso 1 1 d R . . C32 C -0.4128(4) 0.8350(3) 0.1672(3) 0.0725(13) Uani 1 1 d . . . H321 H -0.3930 0.8656 0.2340 0.089(8) Uiso 1 1 d R . . H322 H -0.4801 0.8252 0.1445 0.089(8) Uiso 1 1 d R . . H323 H -0.3647 0.8795 0.1474 0.089(8) Uiso 1 1 d R . . C33 C -0.0995(3) 1.0580(3) -0.1091(3) 0.0485(9) Uani 1 1 d . . . H331 H -0.0618 1.1307 -0.0635 0.073 Uiso 1 1 d R A 2 H332 H -0.1624 1.0227 -0.1088 0.073 Uiso 0.50 1 d PR A 2 H333 H -0.1382 1.0410 -0.1729 0.073 Uiso 0.50 1 d PR A 2 C34 C 0.1264(4) 1.2044(3) 0.0101(3) 0.0499(10) Uani 1 1 d . . . H341 H 0.0762 1.2278 0.0112 0.075 Uiso 1 1 d R B 1 H342 H 0.1792 1.2395 0.0707 0.075 Uiso 0.50 1 d PR B 1 H343 H 0.2045 1.2543 0.0056 0.075 Uiso 0.50 1 d PR B 1 S7 S 0.60203(5) 0.92688(5) 0.54173(5) 0.02556(16) Uani 1 1 d . E . S8 S 0.39038(5) 0.82226(5) 0.43476(5) 0.02542(16) Uani 1 1 d . . . S9 S 0.59863(5) 0.48788(5) 0.41137(5) 0.02621(16) Uani 1 1 d . . . S10 S 0.38277(5) 0.39489(5) 0.31898(5) 0.02770(17) Uani 1 1 d . . . S11 S 0.57170(6) 1.05044(5) 0.71294(5) 0.03187(18) Uani 1 1 d . E . S12 S 0.32471(6) 0.92799(7) 0.58721(6) 0.0379(2) Uani 1 1 d D . . O2A O 0.6472(2) 0.3945(2) 0.5182(2) 0.0340(7) Uani 0.67 1 d P C 1 O2B O 0.2616(7) 0.2228(7) 0.3494(6) 0.067(3) Uani 0.33 1 d P D 2 C35 C 0.7144(2) 0.8432(2) 0.41613(18) 0.0254(6) Uani 1 1 d . . . H35 H 0.7158 0.9064 0.4330 0.030 Uiso 1 1 d R . . C36 C 0.8040(2) 0.8387(2) 0.42295(19) 0.0305(7) Uani 1 1 d . . . H36 H 0.8661 0.8989 0.4458 0.037 Uiso 1 1 d R . . C37 C 0.8036(2) 0.7475(2) 0.3969(2) 0.0318(7) Uani 1 1 d . . . H37 H 0.8652 0.7452 0.4016 0.038 Uiso 1 1 d R . . C38 C 0.7129(2) 0.6597(2) 0.36385(19) 0.0271(6) Uani 1 1 d . . . H38 H 0.7127 0.5969 0.3449 0.033 Uiso 1 1 d R . . C39 C 0.3686(2) 0.4905(2) 0.19108(18) 0.0251(6) Uani 1 1 d . . . H39 H 0.3683 0.4278 0.1726 0.030 Uiso 1 1 d R . . C40 C 0.2962(2) 0.4973(2) 0.14004(19) 0.0280(6) Uani 1 1 d . . . H40 H 0.2459 0.4392 0.0878 0.034 Uiso 1 1 d R . . C41 C 0.2976(2) 0.5893(2) 0.16540(19) 0.0268(6) Uani 1 1 d . . . H41 H 0.2483 0.5942 0.1303 0.032 Uiso 1 1 d R . . C42 C 0.3706(2) 0.6740(2) 0.24190(18) 0.0254(6) Uani 1 1 d . . . H42 H 0.3715 0.7369 0.2585 0.031 Uiso 1 1 d R . . C43 C 0.5250(2) 0.75617(19) 0.37533(18) 0.0212(6) Uani 1 1 d . . . C44 C 0.5225(2) 0.5717(2) 0.32480(17) 0.0220(6) Uani 1 1 d . . . C45 C 0.4421(2) 0.5746(2) 0.26924(18) 0.0224(6) Uani 1 1 d . . . C46 C 0.44329(19) 0.66825(19) 0.29501(18) 0.0215(6) Uani 1 1 d . . . C47 C 0.6226(2) 0.7560(2) 0.38473(17) 0.0222(6) Uani 1 1 d . . . C48 C 0.6218(2) 0.6623(2) 0.35810(17) 0.0219(6) Uani 1 1 d . . . C49 C 0.50876(19) 0.82649(19) 0.43917(18) 0.0212(6) Uani 1 1 d . . . C50 C 0.5186(2) 0.9548(2) 0.59968(19) 0.0263(6) Uani 1 1 d . . . C51 C 0.4220(2) 0.9071(2) 0.55047(19) 0.0270(6) Uani 1 1 d . E . C52 C 0.5046(2) 0.4949(2) 0.34675(18) 0.0227(6) Uani 1 1 d . . . C53 C 0.5153(2) 0.3871(2) 0.42773(19) 0.0294(7) Uani 1 1 d . C . C54 C 0.4164(2) 0.3443(2) 0.38527(19) 0.0297(7) Uani 1 1 d . C . C55 C 0.6258(2) 0.9966(2) 0.7686(2) 0.0335(7) Uani 1 1 d . . . H551 H 0.6730 0.9805 0.7370 0.044 Uiso 1 1 d R E . H552 H 0.6648 1.0476 0.8325 0.044 Uiso 1 1 d R . . C56 C 0.5485(2) 0.9024(2) 0.7689(2) 0.0339(7) Uani 1 1 d . E . H561 H 0.5157 0.8485 0.7052 0.044 Uiso 1 1 d R . . H562 H 0.4961 0.9161 0.7929 0.044 Uiso 1 1 d R . . C57 C 0.5914(2) 0.8644(2) 0.8256(2) 0.0346(7) Uani 1 1 d . . . H571 H 0.6438 0.8504 0.8020 0.045 Uiso 1 1 d R E . H572 H 0.6233 0.9175 0.8896 0.045 Uiso 1 1 d R . . C58 C 0.5097(2) 0.7693(2) 0.8224(2) 0.0337(7) Uani 1 1 d . E . H581 H 0.4838 0.7146 0.7591 0.044 Uiso 1 1 d R . . H582 H 0.4533 0.7814 0.8378 0.044 Uiso 1 1 d R . . C59 C 0.5436(3) 0.7342(2) 0.8864(2) 0.0427(8) Uani 1 1 d . . . H591 H 0.5682 0.7878 0.9500 0.055 Uiso 1 1 d R E . H592 H 0.6001 0.7220 0.8716 0.055 Uiso 1 1 d R . . C60 C 0.4582(3) 0.6380(3) 0.8787(3) 0.0559(10) Uani 1 1 d . E . H601 H 0.4047 0.6515 0.8984 0.073(7) Uiso 1 1 d R . . H602 H 0.4839 0.6148 0.9175 0.073(7) Uiso 1 1 d R . . H603 H 0.4314 0.5859 0.8151 0.073(7) Uiso 1 1 d R . . C61A C 0.2945(3) 0.8619(3) 0.6538(3) 0.0305(10) Uiso 0.64 1 d PD E 1 H611 H 0.3578 0.8828 0.6976 0.040 Uiso 0.64 1 d PR E 1 H612 H 0.2527 0.8834 0.6900 0.040 Uiso 0.64 1 d PR E 1 C61B C 0.2281(8) 0.7892(7) 0.5521(7) 0.053(3) Uiso 0.36 1 d PD E 2 H613 H 0.1601 0.7830 0.5476 0.069 Uiso 0.36 1 d PR E 2 H614 H 0.2268 0.7458 0.4906 0.069 Uiso 0.36 1 d PR E 2 C62 C 0.2409(3) 0.7504(3) 0.6039(3) 0.0627(12) Uani 1 1 d D . . H621 H 0.1794 0.7301 0.5582 0.082 Uiso 0.64 1 d PR E 1 H622 H 0.2841 0.7293 0.5696 0.082 Uiso 0.64 1 d PR E 1 C63A C 0.2114(4) 0.6936(4) 0.6539(4) 0.0428(13) Uiso 0.64 1 d PD E 1 H631 H 0.1683 0.7143 0.6888 0.056 Uiso 0.64 1 d PR E 1 H632 H 0.2725 0.7116 0.6986 0.056 Uiso 0.64 1 d PR E 1 C64A C 0.1542(4) 0.5793(4) 0.5961(4) 0.0438(13) Uiso 0.64 1 d PD E 1 H641 H 0.1973 0.5591 0.5610 0.057 Uiso 0.64 1 d PR E 1 H642 H 0.0932 0.5617 0.5515 0.057 Uiso 0.64 1 d PR E 1 C63B C 0.1720(8) 0.6482(8) 0.5995(8) 0.063(3) Uiso 0.36 1 d PD E 2 H633 H 0.1072 0.6478 0.6030 0.082 Uiso 0.36 1 d PR E 2 H634 H 0.1588 0.5975 0.5368 0.082 Uiso 0.36 1 d PR E 2 C64B C 0.1931(10) 0.6077(9) 0.6592(10) 0.088(4) Uiso 0.36 1 d PD E 2 H643 H 0.2558 0.6037 0.6540 0.114 Uiso 0.36 1 d PR E 2 H644 H 0.2081 0.6579 0.7226 0.114 Uiso 0.36 1 d PR E 2 C65 C 0.1212(4) 0.5148(4) 0.6473(4) 0.0874(16) Uani 1 1 d D . . H651 H 0.1824 0.5312 0.6907 0.114 Uiso 0.64 1 d PR E 1 H652 H 0.0799 0.5366 0.6839 0.114 Uiso 0.64 1 d PR E 1 C66A C 0.0681(5) 0.4124(5) 0.5971(5) 0.0660(18) Uiso 0.64 1 d P E 1 H661 H 0.0524 0.3815 0.6383 0.099 Uiso 0.64 1 d PR E 1 H662 H 0.1084 0.3884 0.5619 0.099 Uiso 0.64 1 d PR E 1 H663 H 0.0054 0.3938 0.5553 0.099 Uiso 0.64 1 d PR E 1 C66B C 0.0840(11) 0.4075(10) 0.5479(10) 0.082(4) Uiso 0.36 1 d P E 2 H664 H 0.0349 0.3489 0.5523 0.122 Uiso 0.36 1 d PR E 2 H665 H 0.1428 0.3991 0.5375 0.122 Uiso 0.36 1 d PR E 2 H666 H 0.0534 0.4137 0.4969 0.122 Uiso 0.36 1 d PR E 2 C67 C 0.5635(3) 0.3560(2) 0.4838(2) 0.0421(9) Uani 1 1 d . . . H671 H 0.5230 0.2997 0.4901 0.063 Uiso 1 1 d R C 2 H672 H 0.5977 0.4115 0.5438 0.063 Uiso 0.50 1 d PR C 2 H673 H 0.6139 0.3440 0.4584 0.063 Uiso 0.50 1 d PR C 2 C68 C 0.3318(3) 0.2593(3) 0.3891(2) 0.0453(9) Uani 1 1 d . . . H681 H 0.3553 0.2179 0.4108 0.068 Uiso 1 1 d R D 1 H682 H 0.2794 0.2822 0.4202 0.068 Uiso 0.50 1 d PR D 1 H683 H 0.3008 0.2143 0.3426 0.068 Uiso 0.50 1 d PR D 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 0.0218(3) 0.0228(4) 0.0269(4) 0.0110(3) 0.0007(3) 0.0064(3) S2 0.0213(3) 0.0256(4) 0.0297(4) 0.0115(3) 0.0005(3) 0.0086(3) S3 0.0347(4) 0.0333(4) 0.0344(4) 0.0183(4) 0.0098(3) 0.0205(4) S4 0.0347(4) 0.0223(4) 0.0404(5) 0.0134(3) 0.0150(4) 0.0127(3) S5 0.0313(4) 0.0339(4) 0.0386(5) 0.0227(4) 0.0080(3) 0.0118(4) S6 0.0364(4) 0.0294(4) 0.0283(4) 0.0111(3) -0.0021(3) 0.0132(4) O1A 0.048(3) 0.058(4) 0.075(4) 0.036(3) 0.016(3) 0.037(3) O1B 0.057(3) 0.026(3) 0.057(3) 0.010(2) 0.011(3) 0.017(3) C1 0.0328(16) 0.0333(17) 0.0279(16) 0.0157(14) 0.0082(13) 0.0176(14) C2 0.0295(16) 0.0338(17) 0.0236(16) 0.0081(14) 0.0011(13) 0.0123(14) C3 0.0290(16) 0.0236(16) 0.0295(17) 0.0053(13) 0.0023(13) 0.0063(13) C4 0.0294(15) 0.0244(15) 0.0298(16) 0.0121(13) 0.0072(13) 0.0118(13) C5 0.0288(16) 0.0305(16) 0.0316(16) 0.0108(14) 0.0103(13) 0.0178(14) C6 0.0228(15) 0.0377(18) 0.0356(18) 0.0090(15) 0.0073(13) 0.0141(14) C7 0.0242(15) 0.0319(17) 0.0358(18) 0.0093(15) 0.0118(13) 0.0078(14) C8 0.0314(16) 0.0237(15) 0.0284(16) 0.0081(13) 0.0109(13) 0.0116(13) C9 0.0246(14) 0.0247(15) 0.0254(15) 0.0136(13) 0.0110(12) 0.0116(13) C10 0.0237(14) 0.0169(14) 0.0270(15) 0.0073(12) 0.0054(12) 0.0103(12) C11 0.0229(14) 0.0227(15) 0.0245(15) 0.0056(12) 0.0066(12) 0.0119(12) C12 0.0256(15) 0.0200(14) 0.0227(15) 0.0045(12) 0.0075(12) 0.0109(12) C13 0.0235(14) 0.0239(15) 0.0285(16) 0.0106(13) 0.0100(12) 0.0118(13) C14 0.0230(14) 0.0207(14) 0.0261(15) 0.0082(12) 0.0075(12) 0.0117(12) C15 0.0230(14) 0.0175(14) 0.0289(16) 0.0064(12) 0.0034(12) 0.0107(12) C16 0.0280(15) 0.0243(15) 0.0289(16) 0.0141(13) 0.0061(12) 0.0130(13) C17 0.0277(15) 0.0231(15) 0.0278(16) 0.0109(13) 0.0028(12) 0.0112(13) C18 0.0276(15) 0.0264(15) 0.0260(15) 0.0145(13) 0.0097(12) 0.0118(13) C19 0.052(2) 0.0369(18) 0.0368(18) 0.0244(15) 0.0238(16) 0.0306(17) C20 0.058(2) 0.0332(18) 0.0388(18) 0.0239(16) 0.0284(17) 0.0304(17) C21 0.0364(17) 0.0287(17) 0.0305(17) 0.0057(14) 0.0036(14) 0.0133(15) C22 0.046(2) 0.041(2) 0.041(2) 0.0180(17) 0.0076(16) 0.0221(17) C23 0.051(2) 0.052(2) 0.040(2) 0.0068(18) 0.0062(17) 0.0301(19) C24 0.048(2) 0.064(2) 0.042(2) 0.0303(19) 0.0233(17) 0.0352(19) C25 0.057(2) 0.064(3) 0.055(2) 0.024(2) 0.018(2) 0.033(2) C26 0.062(3) 0.081(3) 0.073(3) 0.044(2) 0.033(2) 0.050(2) C27 0.0271(16) 0.0328(17) 0.0354(17) 0.0166(15) 0.0081(13) 0.0108(14) C28 0.0360(17) 0.0337(18) 0.0341(18) 0.0134(15) 0.0111(14) 0.0159(15) C29 0.0411(19) 0.0425(19) 0.0348(18) 0.0170(16) 0.0137(15) 0.0217(16) C30 0.058(2) 0.052(2) 0.044(2) 0.0240(18) 0.0297(18) 0.0357(19) C31 0.070(3) 0.076(3) 0.047(2) 0.027(2) 0.020(2) 0.050(2) C32 0.095(3) 0.086(3) 0.072(3) 0.036(3) 0.041(3) 0.070(3) C33 0.076(3) 0.054(3) 0.045(2) 0.032(2) 0.029(2) 0.045(2) C34 0.076(3) 0.039(2) 0.056(2) 0.028(2) 0.037(2) 0.037(2) S7 0.0255(4) 0.0201(4) 0.0231(4) 0.0050(3) 0.0042(3) 0.0088(3) S8 0.0249(4) 0.0246(4) 0.0271(4) 0.0106(3) 0.0060(3) 0.0135(3) S9 0.0309(4) 0.0264(4) 0.0261(4) 0.0129(3) 0.0060(3) 0.0174(3) S10 0.0282(4) 0.0234(4) 0.0306(4) 0.0129(3) 0.0065(3) 0.0114(3) S11 0.0475(5) 0.0225(4) 0.0244(4) 0.0079(3) 0.0095(3) 0.0184(4) S12 0.0418(5) 0.0519(5) 0.0374(5) 0.0233(4) 0.0192(4) 0.0333(4) O2A 0.0382(19) 0.0370(19) 0.0283(17) 0.0152(15) -0.0001(15) 0.0211(16) O2B 0.050(5) 0.068(6) 0.078(6) 0.053(5) 0.011(5) 0.008(5) C35 0.0270(15) 0.0253(15) 0.0223(15) 0.0112(13) 0.0069(12) 0.0109(13) C36 0.0218(15) 0.0318(17) 0.0277(16) 0.0112(14) 0.0054(12) 0.0062(13) C37 0.0232(15) 0.0415(19) 0.0326(17) 0.0179(15) 0.0080(13) 0.0160(14) C38 0.0313(16) 0.0299(16) 0.0255(15) 0.0153(13) 0.0082(13) 0.0167(14) C39 0.0286(15) 0.0193(14) 0.0278(15) 0.0096(12) 0.0070(12) 0.0131(13) C40 0.0272(15) 0.0205(15) 0.0248(15) 0.0043(12) -0.0018(12) 0.0090(13) C41 0.0248(15) 0.0258(15) 0.0266(15) 0.0101(13) -0.0007(12) 0.0126(13) C42 0.0296(15) 0.0201(14) 0.0270(15) 0.0107(12) 0.0052(12) 0.0129(13) C43 0.0255(14) 0.0183(14) 0.0212(14) 0.0108(12) 0.0051(11) 0.0103(12) C44 0.0255(14) 0.0223(14) 0.0178(14) 0.0056(12) 0.0058(11) 0.0143(12) C45 0.0232(14) 0.0225(15) 0.0225(14) 0.0108(12) 0.0058(12) 0.0115(12) C46 0.0230(14) 0.0202(14) 0.0208(14) 0.0097(12) 0.0056(11) 0.0097(12) C47 0.0258(15) 0.0236(15) 0.0166(14) 0.0092(12) 0.0062(11) 0.0113(13) C48 0.0269(15) 0.0233(15) 0.0170(14) 0.0100(12) 0.0050(11) 0.0129(12) C49 0.0218(14) 0.0174(14) 0.0216(14) 0.0096(12) 0.0011(11) 0.0072(12) C50 0.0398(17) 0.0213(15) 0.0247(15) 0.0121(12) 0.0112(13) 0.0188(14) C51 0.0370(17) 0.0278(16) 0.0248(15) 0.0141(13) 0.0121(13) 0.0203(14) C52 0.0265(15) 0.0225(15) 0.0199(14) 0.0077(12) 0.0064(12) 0.0142(13) C53 0.0473(19) 0.0276(16) 0.0225(15) 0.0124(13) 0.0140(14) 0.0240(15) C54 0.0437(18) 0.0264(16) 0.0250(16) 0.0121(13) 0.0154(14) 0.0204(15) C55 0.0431(18) 0.0278(16) 0.0232(16) 0.0106(13) 0.0022(14) 0.0137(15) C56 0.0404(18) 0.0310(17) 0.0324(17) 0.0162(14) 0.0123(14) 0.0169(15) C57 0.0483(19) 0.0298(17) 0.0213(15) 0.0100(13) 0.0062(14) 0.0169(15) C58 0.0430(18) 0.0316(17) 0.0292(17) 0.0131(14) 0.0141(14) 0.0202(15) C59 0.057(2) 0.0340(18) 0.0340(18) 0.0152(15) 0.0129(16) 0.0197(17) C60 0.081(3) 0.035(2) 0.046(2) 0.0200(18) 0.027(2) 0.019(2) C62 0.046(2) 0.043(2) 0.100(3) 0.027(2) 0.036(2) 0.0232(19) C65 0.118(4) 0.093(4) 0.105(4) 0.074(3) 0.070(3) 0.062(3) C67 0.081(3) 0.0347(19) 0.0263(17) 0.0171(15) 0.0210(18) 0.038(2) C68 0.062(3) 0.030(2) 0.038(2) 0.0160(17) 0.0153(19) 0.0166(19) _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 C16 1.764(3) . ? S1 C15 1.773(3) . ? S2 C17 1.762(3) . ? S2 C15 1.772(3) . ? S3 C19 1.752(3) . ? S3 C18 1.772(3) . ? S4 C20 1.756(3) . ? S4 C18 1.771(3) . ? S5 C16 1.749(3) . ? S5 C27 1.820(3) . ? S6 C17 1.757(3) . ? S6 C21 1.824(3) . ? O1A C33 1.038(6) . ? O1B C34 1.049(6) . ? C1 C2 1.387(4) . ? C1 C13 1.402(4) . ? C2 C3 1.388(4) . ? C3 C4 1.395(4) . ? C4 C14 1.397(4) . ? C5 C6 1.387(4) . ? C5 C11 1.406(4) . ? C6 C7 1.380(4) . ? C7 C8 1.390(4) . ? C8 C12 1.401(4) . ? C9 C18 1.360(4) . ? C9 C12 1.481(4) . ? C9 C13 1.482(4) . ? C10 C15 1.357(4) . ? C10 C11 1.480(4) . ? C10 C14 1.485(4) . ? C11 C12 1.414(4) . ? C13 C14 1.418(4) . ? C16 C17 1.342(4) . ? C19 C20 1.347(5) . ? C19 C33 1.491(5) . ? C20 C34 1.477(5) . ? C21 C22 1.532(4) . ? C22 C23 1.502(5) . ? C23 C24 1.532(4) . ? C24 C25 1.496(5) . ? C25 C26 1.520(5) . ? C27 C28 1.519(4) . ? C28 C29 1.519(4) . ? C29 C30 1.525(4) . ? C30 C31 1.499(5) . ? C31 C32 1.523(5) . ? S7 C50 1.763(3) . ? S7 C49 1.774(3) . ? S8 C51 1.762(3) . ? S8 C49 1.767(3) . ? S9 C53 1.758(3) . ? S9 C52 1.768(3) . ? S10 C54 1.746(3) . ? S10 C52 1.771(3) . ? S11 C50 1.758(3) . ? S11 C55 1.826(3) . ? S12 C51 1.760(3) . ? S12 C61A 1.779(4) . ? S12 C61B 1.944(9) . ? O2A C67 1.134(4) . ? O2B C68 0.991(8) . ? C35 C36 1.391(4) . ? C35 C47 1.394(4) . ? C36 C37 1.381(4) . ? C37 C38 1.388(4) . ? C38 C48 1.399(4) . ? C39 C40 1.387(4) . ? C39 C45 1.398(4) . ? C40 C41 1.388(4) . ? C41 C42 1.386(4) . ? C42 C46 1.400(4) . ? C43 C49 1.364(4) . ? C43 C46 1.476(4) . ? C43 C47 1.478(4) . ? C44 C52 1.362(4) . ? C44 C48 1.480(4) . ? C44 C45 1.485(3) . ? C45 C46 1.414(4) . ? C47 C48 1.416(4) . ? C50 C51 1.340(4) . ? C53 C54 1.350(4) . ? C53 C67 1.474(4) . ? C54 C68 1.490(5) . ? C55 C56 1.511(4) . ? C56 C57 1.526(4) . ? C57 C58 1.523(4) . ? C58 C59 1.514(4) . ? C59 C60 1.527(5) . ? C61A C62 1.482(5) . ? C61B C62 1.280(9) . ? C62 C63A 1.431(6) . ? C62 C63B 1.537(10) . ? C63A C64A 1.529(7) . ? C64A C65 1.545(6) . ? C63B C64B 1.452(11) . ? C64B C65 1.386(11) . ? C65 C66A 1.369(8) . ? C65 C66B 1.716(14) . ? 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 C16 S1 C15 96.80(13) . . ? C17 S2 C15 96.63(13) . . ? C19 S3 C18 96.22(15) . . ? C20 S4 C18 96.09(15) . . ? C16 S5 C27 103.57(13) . . ? C17 S6 C21 99.82(14) . . ? C2 C1 C13 120.9(3) . . ? C1 C2 C3 120.2(3) . . ? C2 C3 C4 119.7(3) . . ? C3 C4 C14 121.1(3) . . ? C6 C5 C11 120.6(3) . . ? C7 C6 C5 120.2(3) . . ? C6 C7 C8 120.4(3) . . ? C7 C8 C12 120.6(3) . . ? C18 C9 C12 122.8(2) . . ? C18 C9 C13 123.5(2) . . ? C12 C9 C13 113.6(2) . . ? C15 C10 C11 122.3(2) . . ? C15 C10 C14 124.1(2) . . ? C11 C10 C14 113.6(2) . . ? C5 C11 C12 119.2(3) . . ? C5 C11 C10 123.1(3) . . ? C12 C11 C10 117.6(2) . . ? C8 C12 C11 119.1(2) . . ? C8 C12 C9 123.3(3) . . ? C11 C12 C9 117.6(2) . . ? C1 C13 C14 119.1(3) . . ? C1 C13 C9 123.4(2) . . ? C14 C13 C9 117.5(2) . . ? C4 C14 C13 119.0(2) . . ? C4 C14 C10 123.5(2) . . ? C13 C14 C10 117.4(2) . . ? C10 C15 S2 124.5(2) . . ? C10 C15 S1 124.0(2) . . ? S2 C15 S1 111.46(16) . . ? C17 C16 S5 124.1(2) . . ? C17 C16 S1 116.5(2) . . ? S5 C16 S1 118.80(16) . . ? C16 C17 S6 125.9(2) . . ? C16 C17 S2 117.0(2) . . ? S6 C17 S2 116.97(16) . . ? C9 C18 S4 123.7(2) . . ? C9 C18 S3 123.7(2) . . ? S4 C18 S3 112.59(15) . . ? C20 C19 C33 127.6(3) . . ? C20 C19 S3 117.1(2) . . ? C33 C19 S3 115.2(3) . . ? C19 C20 C34 127.2(3) . . ? C19 C20 S4 117.2(2) . . ? C34 C20 S4 115.6(3) . . ? C22 C21 S6 112.0(2) . . ? C23 C22 C21 113.6(3) . . ? C22 C23 C24 112.9(3) . . ? C25 C24 C23 113.7(3) . . ? C24 C25 C26 112.8(3) . . ? C28 C27 S5 115.2(2) . . ? C27 C28 C29 112.3(3) . . ? C28 C29 C30 113.9(3) . . ? C31 C30 C29 113.4(3) . . ? C30 C31 C32 114.0(4) . . ? O1A C33 C19 121.3(4) . . ? O1B C34 C20 123.9(5) . . ? C50 S7 C49 96.35(13) . . ? C51 S8 C49 96.30(13) . . ? C53 S9 C52 95.82(13) . . ? C54 S10 C52 96.62(14) . . ? C50 S11 C55 101.52(13) . . ? C51 S12 C61A 102.65(18) . .. ? C51 S12 C61B 98.2(3) . . ? C61A S12 C61B 49.6(3) . . ? C36 C35 C47 120.5(3) . . ? C37 C36 C35 120.7(3) . . ? C36 C37 C38 119.6(3) . . ? C37 C38 C48 120.9(3) . . ? C40 C39 C45 121.1(2) . . ? C39 C40 C41 119.8(3) . . ? C42 C41 C40 120.1(2) . . ? C41 C42 C46 120.8(2) . . ? C49 C43 C46 122.2(2) . . ? C49 C43 C47 123.3(2) . . ? C46 C43 C47 114.3(2) . . ? C52 C44 C48 123.6(2) . . ? C52 C44 C45 122.6(2) . . ? C48 C44 C45 113.7(2) . . ? C39 C45 C46 119.0(2) . . ? C39 C45 C44 123.0(2) . . ? C46 C45 C44 117.9(2) . . ? C42 C46 C45 119.1(2) . . ? C42 C46 C43 123.5(2) . . ? C45 C46 C43 117.3(2) . . ? C35 C47 C48 119.0(2) . . ? C35 C47 C43 122.9(2) . . ? C48 C47 C43 118.1(2) . . ? C38 C48 C47 119.3(2) . . ? C38 C48 C44 123.6(2) . . ? C47 C48 C44 117.1(2) . . ? C43 C49 S8 124.2(2) . . ? C43 C49 S7 123.7(2) . . ? S8 C49 S7 111.87(15) . . ? C51 C50 S11 126.2(2) . . ? C51 C50 S7 116.6(2) . . ? S11 C50 S7 116.92(17) . . ? C50 C51 S12 126.5(2) . . ? C50 C51 S8 117.1(2) . . ? S12 C51 S8 116.16(16) . . ? C44 C52 S9 123.9(2) . . ? C44 C52 S10 123.2(2) . . ? S9 C52 S10 112.76(15) . . ? C54 C53 C67 127.3(3) . . ? C54 C53 S9 117.6(2) . . ? C67 C53 S9 115.0(2) . . ? C53 C54 C68 127.6(3) . . ? C53 C54 S10 116.7(2) . . ? C68 C54 S10 115.7(2) . . ? C56 C55 S11 113.7(2) . . ? C55 C56 C57 114.1(3) . . ? C58 C57 C56 111.3(3) . . ? C59 C58 C57 114.5(3) . . ? C58 C59 C60 111.6(3) . . ? C62 C61A S12 117.0(3) . . ? C62 C61B S12 118.0(6) . . ? C61B C62 C63A 156.0(6) . . ? C61B C62 C61A 68.7(5) . . ? C63A C62 C61A 119.3(4) . . ? C61B C62 C63B 129.5(7) . . ? C63A C62 C63B 33.8(4) . . ? C61A C62 C63B 149.9(6) . . ? C62 C63A C64A 115.3(5) . . ? C63A C64A C65 117.2(5) . . ? C64B C63B C62 126.4(10) . . ? C65 C64B C63B 119.0(11) . . ? C66A C65 C64B 150.2(8) . . ? C66A C65 C64A 118.4(5) . . ? C64B C65 C64A 38.3(6) . . ? C66A C65 C66B 29.5(5) . . ? C64B C65 C66B 121.1(9) . . ? C64A C65 C66B 90.3(6) . . ? O2A C67 C53 124.7(3) . . ? O2B C68 C54 125.1(6) . . ? 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 C17 C16 S5 C21 29.7(2) . . . . ? C16 S5 C21 C22 96.0(2) . . . . ? S5 C21 C22 C23 171.1(3) . . . . ? C21 C22 C23 C24 174.0(3) . . . . ? C22 C23 C24 C25 172.9(3) . . . . ? C23 C24 C25 C26 179.4(3) . . . . ? C16 C17 S6 C27 -15.3(2) . . . . ? C17 S6 C27 C28 -94.0(2) . . . . ? S6 C27 C28 C29 -175.7(2) . . . . ? C27 C28 C29 C30 177.0(3) . . . . ? C28 C29 C30 C31 -177.9(3) . . . . ? C29 C30 C31 C32 -179.0(3) . . . . ? C51 C50 S11 C55 123.0(3) . . . . ? C50 S11 C55 C56 -64.6(2) . . . . ? S11 C55 C56 C57 -172.6(2) . . . . ? C55 C56 C57 C58 -179.7(3) . . . . ? C56 C57 C58 C59 -172.6(3) . . . . ? C57 C58 C59 C60 -179.3(3) . . . . ? C50 C51 S12 C61A -78.7(3) . . . . ? C51 S12 C61A C62 -72.0(3) . . . . ? S12 C61A C62 C63A -177.6(4) . . . . ? C61A C62 C63A C64A 178.5(4) . . . . ? C62 C63A C64A C65 179.7(4) . . . . ? C63A C64A C65 C66A 178.7(5) . . . . ? C51 S12 C61B C62 78.4(8) . . . . ? S12 C61B C62 C63B 172.7(7) . . . . ? C61B C62 C63B C64B 177.8(12) . . . . ? C62 C63B C64B C65 178.3(10) . . . . ? C63B C64B C65 C66B 63.0(16) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.455 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.056 #================================================END