# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1377 data_global _publ_contact_author 'Andrei S.Batsanov' _publ_contact_author_email a.s.batsanov@durham.ac.uk loop_ _publ_author_name 'Finn, Terry' 'Bryce, Martin R.' 'Batsanov, Andrei S.' 'Howard, Judith A. K.' _journal_name_full 'Chemical Communications' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1999' _ccdc_journal_depnumber '?' _publ_section_title ; The first brudged 9,10-bis(methylene)-9,10-dihydroanthracene derivatives: strained redox-active cyclophanes. ; #====================================================================== data_alpha-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H26 S6' _chemical_formula_weight 554.85 _ccdc_compound_id '\a-3' _ccdc_biological_activity '?' _ccdc_polymorph 'alpha (monoclinic) form' _ccdc_disorder ; C(25) and C(26) with their hydrogens are disordered over positions A [occupancy 82.3(6)%] and B [occupancy 17.7(6)%]. ; _ccdc_comments ; Obtained from the same crystallisation as the beta polymorph ; 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.139(2) _cell_length_b 11.041(1) _cell_length_c 14.406(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.05(1) _cell_angle_gamma 90.00 _cell_volume 2727.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 903 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 20.7 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8242 _exptl_absorpt_correction_T_max 0.8940 _exptl_absorpt_process_details 'XPREP (SHELX-97) program, before correction R(int)=0.044' 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 0.00 0.2100 1.00 0.00 0.00 0.2100 1.00 1.00 0.00 0.2050 -1.00 -1.00 0.00 0.2050 -1.00 1.00 0.00 0.2000 1.00 -1.00 0.00 0.2200 0.00 0.00 -1.00 0.1200 0.00 0.00 1.00 0.1200 -1.00 0.00 2.00 0.1600 1.00 0.00 -2.00 0.1600 _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 10 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 293(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 24278 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6247 _reflns_number_gt 4325 _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. Disordered H atoms were treated as 'riding' (constr), methyl groups as rigid bodies with a common (refined) isotropic U for 3 hydrogens, other H atoms were refined in isotropic approximation (refall). ; _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^)+(0.0481P)^2^+0.2227P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6247 _refine_ls_number_parameters 384 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.021 _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 0.11842(3) 0.06677(5) 0.37894(4) 0.05714(14) Uani 1 1 d . . . S2 S 0.21218(3) 0.03651(5) 0.58521(4) 0.05553(14) Uani 1 1 d . . . S3 S 0.34230(3) 0.45424(5) 0.34272(4) 0.05761(14) Uani 1 1 d . . . S4 S 0.43641(3) 0.41186(4) 0.54821(3) 0.04960(13) Uani 1 1 d . A . S5 S -0.01816(3) 0.17349(6) 0.42501(5) 0.06969(17) Uani 1 1 d . . . S6 S 0.30823(3) 0.71352(5) 0.37640(5) 0.07114(18) Uani 1 1 d . . . C1 C 0.22871(12) 0.0210(2) 0.25356(15) 0.0569(5) Uani 1 1 d . . . H1 H 0.1959(12) -0.0445(19) 0.2637(15) 0.058(6) Uiso 1 1 d . . . C2 C 0.22939(14) 0.0545(2) 0.16141(16) 0.0671(6) Uani 1 1 d . . . H2 H 0.1986(14) 0.014(2) 0.1062(18) 0.083(7) Uiso 1 1 d . . . C3 C 0.27881(14) 0.1439(2) 0.15077(16) 0.0663(6) Uani 1 1 d . . . H3 H 0.2805(13) 0.171(2) 0.0874(18) 0.081(7) Uiso 1 1 d . . . C4 C 0.32922(13) 0.2007(2) 0.23271(15) 0.0579(5) Uani 1 1 d . . . H4 H 0.3629(12) 0.257(2) 0.2260(15) 0.063(6) Uiso 1 1 d . . . C5 C 0.48764(11) 0.1391(2) 0.56563(15) 0.0528(5) Uani 1 1 d . . . H5 H 0.5212(12) 0.1922(18) 0.5554(14) 0.057(6) Uiso 1 1 d . . . C6 C 0.51139(12) 0.0568(2) 0.64219(15) 0.0596(5) Uani 1 1 d . . . H6 H 0.5658(13) 0.0586(18) 0.6854(16) 0.064(6) Uiso 1 1 d . . . C7 C 0.45915(13) -0.0253(2) 0.65638(15) 0.0620(6) Uani 1 1 d . . . H7 H 0.4687(13) -0.082(2) 0.7054(17) 0.069(6) Uiso 1 1 d . . . C8 C 0.38246(13) -0.02917(18) 0.59176(14) 0.0532(5) Uani 1 1 d . . . H8 H 0.3493(10) -0.0865(17) 0.6007(13) 0.045(5) Uiso 1 1 d . . . C9 C 0.27925(10) 0.05202(15) 0.43897(13) 0.0428(4) Uani 1 1 d . . . C10 C 0.38071(9) 0.22436(17) 0.41881(12) 0.0447(4) Uani 1 1 d . . . C11 C 0.27802(10) 0.07850(16) 0.33767(13) 0.0454(4) Uani 1 1 d . . . C12 C 0.32954(10) 0.16903(17) 0.32667(12) 0.0457(4) Uani 1 1 d . . . C13 C 0.41117(10) 0.13819(16) 0.50086(12) 0.0444(4) Uani 1 1 d . . . C14 C 0.35844(10) 0.05112(15) 0.51309(12) 0.0432(4) Uani 1 1 d . . . C15 C 0.21352(10) 0.04782(16) 0.46337(12) 0.0448(4) Uani 1 1 d . . . C16 C 0.07810(11) 0.11999(18) 0.46764(15) 0.0537(5) Uani 1 1 d . . . C17 C 0.12126(11) 0.10702(18) 0.56189(15) 0.0540(5) Uani 1 1 d . . . C18 C 0.38787(9) 0.34546(17) 0.43281(13) 0.0452(4) Uani 1 1 d . . . C19 C 0.35269(11) 0.57557(17) 0.42532(15) 0.0528(5) Uani 1 1 d . A . C20 C 0.39628(11) 0.55649(17) 0.51897(15) 0.0514(4) Uani 1 1 d . . . C21 C -0.01002(14) 0.3078(2) 0.35644(18) 0.0692(6) Uani 1 1 d . . . H211 H 0.0011(13) 0.282(2) 0.2988(18) 0.080(7) Uiso 1 1 d . . . H212 H -0.0626(15) 0.346(2) 0.3407(18) 0.092(8) Uiso 1 1 d . . . C22 C 0.04897(14) 0.4018(2) 0.41112(18) 0.0638(6) Uani 1 1 d . . . H221 H 0.0504(14) 0.409(2) 0.4748(19) 0.083(8) Uiso 1 1 d . . . H222 H 0.1023(13) 0.373(2) 0.4210(15) 0.069(6) Uiso 1 1 d . . . C23 C 0.03371(14) 0.5236(2) 0.36008(18) 0.0682(6) Uani 1 1 d . A . H231 H -0.0186(15) 0.556(2) 0.3604(17) 0.083(7) Uiso 1 1 d . . . H232 H 0.0336(14) 0.510(2) 0.294(2) 0.091(8) Uiso 1 1 d . . . C24 C 0.09344(13) 0.6213(2) 0.4064(2) 0.0673(6) Uani 1 1 d . . . H241 H 0.1060(13) 0.616(2) 0.4804(19) 0.082(7) Uiso 1 1 d . . . H242 H 0.0724(14) 0.711(2) 0.3825(17) 0.086(7) Uiso 1 1 d . . . C25A C 0.16574(15) 0.6078(3) 0.3769(2) 0.0598(8) Uani 0.823(6) 1 d P A 1 H251 H 0.1910 0.5314 0.4014 0.078 Uiso 0.823(6) 1 d PR A 1 H252 H 0.1512 0.6071 0.3058 0.078 Uiso 0.823(6) 1 d PR A 1 C26A C 0.22290(15) 0.7115(2) 0.4181(2) 0.0657(10) Uani 0.823(6) 1 d P A 1 H261 H 0.2409 0.7065 0.4893 0.085 Uiso 0.823(6) 1 d PR A 1 H262 H 0.1951 0.7875 0.3998 0.085 Uiso 0.823(6) 1 d PR A 1 C25B C 0.1875(10) 0.6360(18) 0.4319(15) 0.083(5) Uiso 0.177(6) 1 d P A 2 H253 H 0.2073 0.6964 0.4829 0.108 Uiso 0.177(6) 1 d PR A 2 H254 H 0.2135 0.5597 0.4553 0.108 Uiso 0.177(6) 1 d PR A 2 C26B C 0.2041(8) 0.6766(13) 0.3364(11) 0.074(5) Uiso 0.177(6) 1 d P A 2 H263 H 0.1729 0.7467 0.3073 0.096 Uiso 0.177(6) 1 d PR A 2 H264 H 0.1924 0.6114 0.2886 0.096 Uiso 0.177(6) 1 d PR A 2 C27 C 0.10119(14) 0.1461(2) 0.65103(17) 0.0746(7) Uani 1 1 d . . . H271 H 0.1380 0.2055 0.6873 0.139(7) Uiso 1 1 d R . . H272 H 0.1025 0.0771 0.6921 0.139(7) Uiso 1 1 d R . . H273 H 0.0498 0.1805 0.6301 0.139(7) Uiso 1 1 d R . . C28 C 0.41558(14) 0.6459(2) 0.60088(16) 0.0698(6) Uani 1 1 d . A . H281 H 0.4050 0.7265 0.5748 0.098(5) Uiso 1 1 d R . . H282 H 0.4698 0.6391 0.6390 0.098(5) Uiso 1 1 d R . . H283 H 0.3844 0.6295 0.6420 0.098(5) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0413(3) 0.0748(4) 0.0492(3) -0.0108(2) 0.0065(2) -0.0009(2) S2 0.0567(3) 0.0622(3) 0.0462(3) 0.0036(2) 0.0148(2) 0.0006(2) S3 0.0582(3) 0.0594(3) 0.0478(3) 0.0086(2) 0.0072(2) 0.0007(2) S4 0.0466(3) 0.0508(3) 0.0460(3) 0.0012(2) 0.0076(2) -0.0009(2) S5 0.0437(3) 0.0814(4) 0.0854(4) -0.0027(3) 0.0231(3) -0.0014(3) S6 0.0571(3) 0.0525(3) 0.0944(4) 0.0219(3) 0.0118(3) -0.0022(2) C1 0.0542(12) 0.0597(13) 0.0498(11) -0.0144(9) 0.0073(9) 0.0015(10) C2 0.0665(14) 0.0823(16) 0.0434(11) -0.0185(11) 0.0055(10) 0.0080(12) C3 0.0692(14) 0.0874(17) 0.0420(11) -0.0039(11) 0.0178(10) 0.0155(13) C4 0.0534(12) 0.0724(14) 0.0489(11) 0.0005(10) 0.0181(9) 0.0078(11) C5 0.0404(10) 0.0600(12) 0.0529(11) -0.0081(9) 0.0083(9) 0.0049(9) C6 0.0469(11) 0.0683(14) 0.0517(12) -0.0081(10) -0.0003(9) 0.0156(10) C7 0.0694(14) 0.0600(13) 0.0453(11) 0.0015(10) 0.0032(10) 0.0243(11) C8 0.0589(12) 0.0438(11) 0.0519(11) -0.0008(8) 0.0112(9) 0.0082(9) C9 0.0436(9) 0.0378(9) 0.0432(9) -0.0052(7) 0.0088(7) 0.0027(7) C10 0.0350(9) 0.0556(11) 0.0427(9) -0.0014(8) 0.0116(7) 0.0033(7) C11 0.0413(9) 0.0483(10) 0.0426(9) -0.0063(8) 0.0082(8) 0.0098(8) C12 0.0393(9) 0.0545(11) 0.0412(9) -0.0040(8) 0.0100(8) 0.0099(8) C13 0.0403(9) 0.0476(10) 0.0417(9) -0.0066(7) 0.0086(7) 0.0071(8) C14 0.0436(9) 0.0416(9) 0.0400(9) -0.0060(7) 0.0073(7) 0.0096(7) C15 0.0458(10) 0.0411(10) 0.0416(9) -0.0050(7) 0.0062(8) -0.0019(7) C16 0.0434(10) 0.0582(12) 0.0612(12) -0.0029(9) 0.0194(9) -0.0052(9) C17 0.0542(11) 0.0538(12) 0.0575(12) 0.0011(9) 0.0230(9) -0.0043(9) C18 0.0349(9) 0.0562(11) 0.0434(9) 0.0027(8) 0.0111(7) 0.0002(8) C19 0.0445(10) 0.0489(11) 0.0619(12) 0.0071(9) 0.0133(9) -0.0027(8) C20 0.0447(10) 0.0478(11) 0.0608(12) 0.0029(9) 0.0158(9) -0.0021(8) C21 0.0542(13) 0.0838(17) 0.0612(14) -0.0024(12) 0.0075(11) 0.0076(12) C22 0.0553(13) 0.0751(15) 0.0560(13) 0.0020(11) 0.0111(10) 0.0093(11) C23 0.0629(14) 0.0812(17) 0.0578(14) 0.0045(12) 0.0160(11) 0.0170(12) C24 0.0630(14) 0.0668(15) 0.0743(16) 0.0081(12) 0.0253(12) 0.0172(11) C25A 0.0519(15) 0.0561(16) 0.0669(19) -0.0061(13) 0.0134(13) 0.0048(12) C26A 0.0610(17) 0.0473(15) 0.082(2) -0.0033(13) 0.0144(14) 0.0061(12) C27 0.0838(16) 0.0859(17) 0.0664(14) 0.0028(12) 0.0415(13) 0.0022(13) C28 0.0788(15) 0.0564(13) 0.0677(14) -0.0057(11) 0.0150(11) 0.0015(11) _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 1.767(2) . ? S1 C15 1.7690(18) . ? S2 C17 1.754(2) . ? S2 C15 1.7677(18) . ? S3 C19 1.761(2) . ? S3 C18 1.7634(18) . ? S4 C20 1.7485(19) . ? S4 C18 1.7666(18) . ? S5 C16 1.753(2) . ? S5 C21 1.815(3) . ? S6 C19 1.759(2) . ? S6 C26B 1.831(14) . ? S6 C26A 1.834(3) . ? C1 C2 1.382(3) . ? C1 C11 1.401(3) . ? C2 C3 1.375(3) . ? C3 C4 1.385(3) . ? C4 C12 1.396(3) . ? C5 C6 1.385(3) . ? C5 C13 1.396(2) . ? C6 C7 1.374(3) . ? C7 C8 1.399(3) . ? C8 C14 1.392(3) . ? C9 C15 1.349(2) . ? C9 C11 1.481(3) . ? C9 C14 1.484(2) . ? C10 C18 1.352(3) . ? C10 C13 1.477(2) . ? C10 C12 1.481(2) . ? C11 C12 1.412(3) . ? C13 C14 1.407(3) . ? C16 C17 1.335(3) . ? C17 C27 1.508(3) . ? C19 C20 1.339(3) . ? C20 C28 1.490(3) . ? C21 C22 1.514(3) . ? C22 C23 1.514(3) . ? C23 C24 1.520(4) . ? C24 C25A 1.513(3) . ? C24 C25B 1.633(17) . ? C25A C26A 1.528(4) . ? C25B C26B 1.57(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 S1 C15 94.76(9) . . ? C17 S2 C15 95.46(9) . . ? C19 S3 C18 95.72(9) . . ? C20 S4 C18 96.42(9) . . ? C16 S5 C21 102.55(11) . . ? C19 S6 C26B 102.9(5) . . ? C19 S6 C26A 100.58(11) . . ? C26B S6 C26A 37.5(5) . . ? C2 C1 C11 120.4(2) . . ? C3 C2 C1 120.6(2) . . ? C2 C3 C4 120.2(2) . . ? C3 C4 C12 120.4(2) . . ? C6 C5 C13 120.7(2) . . ? C7 C6 C5 120.06(19) . . ? C6 C7 C8 120.4(2) . . ? C14 C8 C7 120.1(2) . . ? C15 C9 C11 122.20(15) . . ? C15 C9 C14 122.85(16) . . ? C11 C9 C14 114.20(15) . . ? C18 C10 C13 121.67(16) . . ? C18 C10 C12 122.91(16) . . ? C13 C10 C12 114.39(16) . . ? C1 C11 C12 118.86(17) . . ? C1 C11 C9 124.23(18) . . ? C12 C11 C9 116.90(15) . . ? C4 C12 C11 119.50(17) . . ? C4 C12 C10 124.67(18) . . ? C11 C12 C10 115.83(15) . . ? C5 C13 C14 119.25(17) . . ? C5 C13 C10 124.12(18) . . ? C14 C13 C10 116.64(15) . . ? C8 C14 C13 119.48(17) . . ? C8 C14 C9 124.22(17) . . ? C13 C14 C9 116.30(15) . . ? C9 C15 S2 124.10(13) . . ? C9 C15 S1 124.27(14) . . ? S2 C15 S1 111.39(10) . . ? C17 C16 S5 125.35(16) . . ? C17 C16 S1 117.12(15) . . ? S5 C16 S1 117.30(12) . . ? C16 C17 C27 127.7(2) . . ? C16 C17 S2 116.41(15) . . ? C27 C17 S2 115.92(16) . . ? C10 C18 S3 124.37(14) . . ? C10 C18 S4 123.01(14) . . ? S3 C18 S4 112.33(11) . . ? C20 C19 S6 125.62(16) . . ? C20 C19 S3 117.32(15) . . ? S6 C19 S3 117.00(11) . . ? C19 C20 C28 127.03(18) . . ? C19 C20 S4 116.67(15) . . ? C28 C20 S4 116.28(15) . . ? C22 C21 S5 116.51(17) . . ? C23 C22 C21 111.71(19) . . ? C22 C23 C24 115.2(2) . . ? C25A C24 C23 111.4(2) . . ? C25A C24 C25B 30.0(7) . . ? C23 C24 C25B 135.4(8) . . ? C24 C25A C26A 110.9(2) . . ? C25A C26A S6 114.8(2) . . ? C26B C25B C24 108.5(13) . . ? C25B C26B S6 105.1(11) . . ? 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 119.4(2) . . . . ? C16 S5 C21 C22 -54.9(2) . . . . ? S5 C21 C22 C23 -162.01(18) . . . . ? C21 C22 C23 C24 -176.1(2) . . . . ? C22 C23 C24 C25A 80.1(3) . . . . ? C23 C24 C25A C26A 176.1(2) . . . . ? C24 C25A C26A S6 -173.89(18) . . . . ? C25A C26A S6 C19 -63.0(2) . . . . ? C26A S6 C19 C20 -78.8(2) . . . . ? C22 C23 C24 C25B 58.0(11) . . . . ? C23 C24 C25B C26B 81.8(14) . . . . ? C24 C25B C26B S6 171.3(9) . . . . ? C25B C26B S6 C19 60.5(11) . . . . ? C26B S6 C19 C20 -117.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.217 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.042 #================================================END data_beta-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H26 S6' _chemical_formula_weight 554.85 _ccdc_compound_id '\b-3' _ccdc_biological_activity '?' _ccdc_polymorph 'beta (orthorhombic) form' _ccdc_disorder ; none ; _ccdc_comments ; Obtained from the same crystallisation as the alpha polymorph. ; 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.231(2) _cell_length_b 9.520(1) _cell_length_c 30.089(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5509(1) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 642 _cell_measurement_theta_min 10 _cell_measurement_theta_max 18 _exptl_crystal_description 'hexagon prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9081 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details 'XPREP (SHELX-97) program, before correction R(int)=0.083' 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 0.0500 0.00 0.00 -1.00 0.0600 0.00 0.00 1.00 0.0500 -1.00 0.00 1.00 0.0700 -1.00 0.00 -1.00 0.0500 1.00 0.00 1.00 0.0700 0.00 1.00 0.00 0.2000 -3.00 -2.00 1.00 0.1950 0.00 -1.00 1.00 0.2200 1.00 -1.00 -1.00 0.2100 _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 20 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 293(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 '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 31379 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9683 _reflns_number_gt 5758 _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^)+(0.0367P)^2^+0.8116P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.15(9) _refine_ls_number_reflns 9683 _refine_ls_number_parameters 617 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.011 _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 S1A S 0.37060(9) 1.05247(16) 0.28629(6) 0.0510(4) Uani 1 1 d . . . S2A S 0.23772(7) 0.99764(15) 0.32901(6) 0.0489(4) Uani 1 1 d . . . S3A S 0.53579(8) 0.82176(19) 0.45291(6) 0.0533(4) Uani 1 1 d . . . S4A S 0.4076(2) 0.75277(15) 0.50016(11) 0.0557(10) Uani 1 1 d . . . S5A S 0.34902(12) 1.36506(19) 0.28245(8) 0.0714(6) Uani 1 1 d . . . S6A S 0.58401(9) 1.03172(19) 0.52095(6) 0.0671(5) Uani 1 1 d . . . C1A C 0.4545(4) 0.7743(6) 0.2884(3) 0.0376(17) Uani 1 1 d . . . H1A H 0.4300 0.8072 0.2638 0.045 Uiso 1 1 d R . . C2A C 0.5211(6) 0.7301(6) 0.2826(4) 0.047(3) Uani 1 1 d . . . H2A H 0.5412 0.7305 0.2545 0.056 Uiso 1 1 d R . . C3A C 0.5591(3) 0.6843(7) 0.3191(2) 0.0449(15) Uani 1 1 d . . . H3A H 0.6053 0.6576 0.3157 0.054 Uiso 1 1 d R . . C4A C 0.5282(3) 0.6779(6) 0.36035(19) 0.0406(14) Uani 1 1 d . . . H4A H 0.5536 0.6461 0.3847 0.049 Uiso 1 1 d R . . C5A C 0.3140(3) 0.5799(6) 0.43467(19) 0.0514(16) Uani 1 1 d . . . H5A H 0.3385 0.5415 0.4584 0.062 Uiso 1 1 d R . . C6A C 0.2454(4) 0.5476(7) 0.4299(2) 0.0617(19) Uani 1 1 d . . . H6A H 0.2235 0.4890 0.4503 0.074 Uiso 1 1 d R . . C7A C 0.2081(4) 0.6022(7) 0.3946(3) 0.064(2) Uani 1 1 d . . . H7A H 0.1611 0.5815 0.3913 0.076 Uiso 1 1 d R . . C8A C 0.2411(3) 0.6883(7) 0.3637(2) 0.0489(16) Uani 1 1 d . . . H8A H 0.2168 0.7219 0.3392 0.059 Uiso 1 1 d R . . C9A C 0.3490(3) 0.8143(6) 0.33691(18) 0.0358(13) Uani 1 1 d . . . C10A C 0.4217(4) 0.7107(6) 0.4086(2) 0.0331(17) Uani 1 1 d . . . C11A C 0.4225(5) 0.7718(6) 0.3292(3) 0.035(2) Uani 1 1 d . . . C12A C 0.4589(5) 0.7197(6) 0.3659(3) 0.034(2) Uani 1 1 d . . . C13A C 0.3484(3) 0.6690(5) 0.40504(18) 0.0363(14) Uani 1 1 d . . . C14A C 0.3101(5) 0.7243(6) 0.3688(3) 0.032(2) Uani 1 1 d . . . C15A C 0.3230(3) 0.9343(6) 0.31977(17) 0.0384(13) Uani 1 1 d . . . C16A C 0.3175(4) 1.1976(7) 0.2987(2) 0.0474(18) Uani 1 1 d . . . C17A C 0.2570(4) 1.1748(6) 0.3181(2) 0.0497(16) Uani 1 1 d . . . C18A C 0.4528(6) 0.7503(5) 0.4468(4) 0.038(3) Uani 1 1 d . . . C19A C 0.5201(3) 0.9114(6) 0.5038(2) 0.0537(17) Uani 1 1 d . . . C20A C 0.4627(4) 0.8771(6) 0.52556(19) 0.0538(16) Uani 1 1 d . . . C21A C 0.4357(3) 1.3595(6) 0.3062(2) 0.0643(19) Uani 1 1 d . . . H211 H 0.4615 1.2843 0.2920 0.084 Uiso 1 1 d R . . H212 H 0.4591 1.4469 0.2992 0.084 Uiso 1 1 d R . . C22A C 0.4379(4) 1.3373(7) 0.3559(2) 0.068(2) Uani 1 1 d . . . H221 H 0.4219 1.4224 0.3703 0.089 Uiso 1 1 d R . . H222 H 0.4057 1.2628 0.3635 0.089 Uiso 1 1 d R . . C23A C 0.5072(5) 1.3017(9) 0.3743(3) 0.081(3) Uani 1 1 d . . . H231 H 0.5410 1.3681 0.3629 0.105 Uiso 1 1 d R . . H232 H 0.5202 1.2091 0.3637 0.105 Uiso 1 1 d R . . C24A C 0.5105(7) 1.3018(13) 0.4241(4) 0.119(4) Uani 1 1 d . . . H241 H 0.5261 1.3938 0.4336 0.154 Uiso 1 1 d R . . H242 H 0.4636 1.2891 0.4353 0.154 Uiso 1 1 d R . . C25A C 0.5548(6) 1.1960(11) 0.4445(4) 0.092(3) Uani 1 1 d . . . H251 H 0.6025 1.2149 0.4359 0.119 Uiso 1 1 d R . . H252 H 0.5425 1.1046 0.4326 0.119 Uiso 1 1 d R . . C26A C 0.5514(4) 1.1896(8) 0.4952(3) 0.078(2) Uani 1 1 d . . . H261 H 0.5033 1.2014 0.5041 0.102 Uiso 1 1 d R . . H262 H 0.5773 1.2686 0.5071 0.102 Uiso 1 1 d R . . C27A C 0.2021(5) 1.2796(8) 0.3320(4) 0.068(3) Uani 1 1 d . . . H271 H 0.2210 1.3726 0.3300 0.107(17) Uiso 1 1 d R . . H272 H 0.1880 1.2613 0.3620 0.107(17) Uiso 1 1 d R . . H273 H 0.1625 1.2718 0.3127 0.107(17) Uiso 1 1 d R . . C28A C 0.4368(4) 0.9339(7) 0.5699(2) 0.075(2) Uani 1 1 d . . . H281 H 0.4684 1.0044 0.5805 0.103(16) Uiso 1 1 d R . . H282 H 0.4342 0.8588 0.5911 0.103(16) Uiso 1 1 d R . . H283 H 0.3915 0.9744 0.5661 0.103(16) Uiso 1 1 d R . . S1B S 0.88228(10) 0.56261(17) 0.72281(7) 0.0570(5) Uani 1 1 d . . . S2B S 1.01375(7) 0.50870(15) 0.67844(6) 0.0504(4) Uani 1 1 d . . . S3B S 0.71396(8) 0.32785(19) 0.55602(6) 0.0555(4) Uani 1 1 d . . . S4B S 0.8415(2) 0.25740(16) 0.50919(11) 0.0531(9) Uani 1 1 d . . . S5B S 0.90188(12) 0.87466(19) 0.72700(7) 0.0703(6) Uani 1 1 d . . . S6B S 0.66564(9) 0.53741(18) 0.48820(6) 0.0627(5) Uani 1 1 d . . . C1B C 0.7955(4) 0.2981(7) 0.7206(3) 0.0496(18) Uani 1 1 d . . . H1B H 0.8201 0.3323 0.7449 0.060 Uiso 1 1 d R . . C2B C 0.7253(6) 0.2611(6) 0.7249(5) 0.054(3) Uani 1 1 d . . . H2B H 0.7032 0.2727 0.7521 0.065 Uiso 1 1 d R . . C3B C 0.6900(4) 0.2083(8) 0.6896(3) 0.0585(19) Uani 1 1 d . . . H3B H 0.6437 0.1821 0.6931 0.070 Uiso 1 1 d R . . C4B C 0.7221(3) 0.1936(7) 0.6487(2) 0.0470(15) Uani 1 1 d . . . H4B H 0.6968 0.1564 0.6252 0.056 Uiso 1 1 d R . . C5B C 0.9345(3) 0.0871(6) 0.57389(19) 0.0485(16) Uani 1 1 d . . . H5B H 0.9097 0.0468 0.5507 0.058 Uiso 1 1 d R . . C6B C 1.0054(4) 0.0564(6) 0.5793(2) 0.0583(18) Uani 1 1 d . . . H6B H 1.0280 -0.0004 0.5588 0.070 Uiso 1 1 d R . . C7B C 1.0420(3) 0.1099(7) 0.6146(2) 0.0570(18) Uani 1 1 d . . . H7B H 1.0886 0.0873 0.6182 0.068 Uiso 1 1 d R . . C8B C 1.0099(3) 0.1970(8) 0.6448(2) 0.0494(17) Uani 1 1 d . . . H8B H 1.0357 0.2333 0.6682 0.059 Uiso 1 1 d R . . C9B C 0.9021(3) 0.3259(6) 0.67149(17) 0.0372(14) Uani 1 1 d . . . C10B C 0.8280(5) 0.2185(7) 0.5992(3) 0.0395(19) Uani 1 1 d . . . C11B C 0.8292(5) 0.2835(7) 0.6789(3) 0.0352(19) Uani 1 1 d . . . C12B C 0.7904(5) 0.2322(6) 0.6420(3) 0.035(2) Uani 1 1 d . . . C13B C 0.9018(3) 0.1771(6) 0.60352(19) 0.0409(14) Uani 1 1 d . . . C14B C 0.9388(6) 0.2330(6) 0.6406(4) 0.044(3) Uani 1 1 d . . . C15B C 0.9291(3) 0.4445(6) 0.68922(18) 0.0413(14) Uani 1 1 d . . . C16B C 0.9331(4) 0.7114(8) 0.7099(3) 0.0506(19) Uani 1 1 d . . . C17B C 0.9947(4) 0.6871(7) 0.6901(2) 0.0510(17) Uani 1 1 d . . . C18B C 0.7995(6) 0.2564(5) 0.5594(4) 0.040(3) Uani 1 1 d . . . C19B C 0.7282(3) 0.4136(6) 0.5052(2) 0.0510(16) Uani 1 1 d . . . C20B C 0.7869(3) 0.3815(6) 0.48309(18) 0.0522(16) Uani 1 1 d . . . C21B C 0.8151(3) 0.8689(7) 0.7026(2) 0.0640(19) Uani 1 1 d . . . H213 H 0.7892 0.7935 0.7166 0.083 Uiso 1 1 d R . . H214 H 0.7914 0.9562 0.7093 0.083 Uiso 1 1 d R . . C22B C 0.8143(4) 0.8469(7) 0.6530(2) 0.0631(19) Uani 1 1 d . . . H223 H 0.8458 0.7709 0.6456 0.082 Uiso 1 1 d R . . H224 H 0.8313 0.9312 0.6386 0.082 Uiso 1 1 d R . . C23B C 0.7421(4) 0.8117(10) 0.6353(3) 0.076(2) Uani 1 1 d . . . H233 H 0.7096 0.8847 0.6438 0.098 Uiso 1 1 d R . . H234 H 0.7261 0.7237 0.6478 0.098 Uiso 1 1 d R . . C24B C 0.7449(6) 0.8011(13) 0.5832(4) 0.098(3) Uani 1 1 d . . . H243 H 0.7370 0.8937 0.5708 0.128 Uiso 1 1 d R . . H244 H 0.7914 0.7724 0.5745 0.128 Uiso 1 1 d R . . C25B C 0.6944(6) 0.7038(10) 0.5630(3) 0.082(3) Uani 1 1 d . . . H253 H 0.6478 0.7321 0.5713 0.106 Uiso 1 1 d R . . H254 H 0.7024 0.6106 0.5749 0.106 Uiso 1 1 d R . . C26B C 0.6992(4) 0.6965(8) 0.5136(3) 0.068(2) Uani 1 1 d . . . H263 H 0.7476 0.7069 0.5051 0.088 Uiso 1 1 d R . . H264 H 0.6740 0.7759 0.5014 0.088 Uiso 1 1 d R . . C27B C 1.0467(6) 0.7935(9) 0.6756(4) 0.079(3) Uani 1 1 d . . . H274 H 1.0304 0.8858 0.6831 0.093(16) Uiso 1 1 d R . . H275 H 1.0536 0.7872 0.6441 0.093(16) Uiso 1 1 d R . . H276 H 1.0900 0.7760 0.6906 0.093(16) Uiso 1 1 d R . . C28B C 0.8106(4) 0.4365(8) 0.43906(19) 0.074(2) Uani 1 1 d . . . H284 H 0.7802 0.5106 0.4297 0.088(14) Uiso 1 1 d R . . H285 H 0.8097 0.3621 0.4176 0.088(14) Uiso 1 1 d R . . H286 H 0.8572 0.4720 0.4417 0.088(14) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1A 0.0508(11) 0.0474(9) 0.0549(11) -0.0001(9) 0.0086(9) 0.0057(9) S2A 0.0345(8) 0.0513(9) 0.0610(10) -0.0087(8) -0.0055(7) 0.0043(8) S3A 0.0419(10) 0.0720(12) 0.0459(10) -0.0147(9) -0.0045(8) 0.0001(10) S4A 0.067(3) 0.0651(14) 0.034(2) -0.0009(7) 0.0019(19) -0.0072(8) S5A 0.0842(17) 0.0498(11) 0.0803(15) 0.0143(11) 0.0016(12) 0.0086(11) S6A 0.0593(11) 0.0792(12) 0.0628(11) -0.0181(9) -0.0195(9) -0.0018(10) C1A 0.034(4) 0.045(3) 0.033(4) 0.003(3) -0.001(3) 0.001(3) C2A 0.048(7) 0.056(4) 0.036(6) -0.002(3) 0.011(5) -0.007(4) C3A 0.029(4) 0.055(4) 0.051(4) -0.007(4) 0.007(3) 0.004(4) C4A 0.035(4) 0.046(4) 0.041(4) -0.003(3) -0.005(3) 0.004(3) C5A 0.061(5) 0.049(4) 0.044(4) -0.001(3) 0.012(3) -0.013(4) C6A 0.068(6) 0.062(4) 0.055(5) -0.012(4) 0.020(4) -0.022(4) C7A 0.045(4) 0.060(4) 0.086(6) -0.022(4) 0.020(4) -0.022(4) C8A 0.040(5) 0.047(4) 0.060(5) -0.016(4) 0.003(3) -0.004(4) C9A 0.029(3) 0.043(4) 0.035(3) -0.010(3) -0.002(3) -0.003(3) C10A 0.034(5) 0.030(3) 0.035(4) -0.008(4) -0.006(3) -0.002(4) C11A 0.028(5) 0.034(3) 0.042(5) 0.002(3) -0.003(4) -0.004(3) C12A 0.036(6) 0.029(3) 0.037(5) -0.009(3) 0.009(4) -0.008(4) C13A 0.042(4) 0.029(3) 0.037(3) -0.007(3) 0.007(3) -0.003(3) C14A 0.029(6) 0.036(3) 0.030(5) -0.007(3) 0.007(4) -0.009(3) C15A 0.037(3) 0.040(3) 0.038(3) -0.009(3) -0.004(3) 0.005(3) C16A 0.053(6) 0.037(4) 0.052(5) -0.007(4) -0.009(4) 0.001(4) C17A 0.042(4) 0.055(4) 0.052(4) -0.011(3) -0.011(4) 0.008(4) C18A 0.036(7) 0.039(5) 0.039(7) 0.001(2) 0.023(5) 0.005(3) C19A 0.058(4) 0.062(4) 0.042(4) -0.008(3) -0.013(3) -0.003(4) C20A 0.072(5) 0.054(4) 0.036(4) -0.001(3) -0.005(3) 0.004(4) C21A 0.083(5) 0.042(4) 0.068(5) 0.007(3) 0.012(4) -0.010(3) C22A 0.074(6) 0.056(5) 0.076(5) -0.006(4) 0.016(4) -0.004(4) C23A 0.084(7) 0.067(5) 0.093(7) -0.006(5) 0.005(5) 0.012(5) C24A 0.153(11) 0.111(8) 0.092(9) -0.025(8) -0.034(8) 0.027(9) C25A 0.089(7) 0.074(6) 0.112(9) -0.005(6) 0.020(6) 0.004(6) C26A 0.071(6) 0.080(5) 0.084(6) -0.027(5) -0.018(5) 0.001(5) C27A 0.053(6) 0.072(5) 0.078(7) -0.019(5) -0.011(5) 0.032(5) C28A 0.099(6) 0.087(5) 0.039(4) -0.009(4) 0.001(4) 0.003(5) S1B 0.0621(12) 0.0509(10) 0.0580(12) -0.0048(10) 0.0133(9) -0.0040(9) S2B 0.0383(8) 0.0576(10) 0.0554(10) 0.0086(8) -0.0043(7) -0.0058(8) S3B 0.0412(10) 0.0711(13) 0.0543(11) 0.0162(9) -0.0017(8) 0.0023(9) S4B 0.059(2) 0.0636(14) 0.036(2) -0.0014(7) 0.0072(18) 0.0094(8) S5B 0.0826(17) 0.0530(11) 0.0754(14) -0.0134(11) -0.0093(12) -0.0035(11) S6B 0.0561(11) 0.0747(11) 0.0574(11) 0.0127(9) -0.0167(8) 0.0046(9) C1B 0.056(5) 0.050(4) 0.043(4) 0.000(4) 0.001(4) -0.006(4) C2B 0.036(7) 0.063(5) 0.064(8) 0.018(4) 0.022(6) 0.003(3) C3B 0.033(4) 0.077(5) 0.065(5) 0.020(4) 0.003(4) 0.000(4) C4B 0.042(4) 0.051(4) 0.048(4) 0.013(3) -0.005(3) 0.000(3) C5B 0.054(4) 0.046(4) 0.045(4) 0.005(3) 0.010(3) 0.004(3) C6B 0.062(5) 0.053(4) 0.060(5) 0.009(4) 0.021(4) 0.023(4) C7B 0.037(4) 0.064(5) 0.070(5) 0.017(4) 0.017(4) 0.016(4) C8B 0.031(4) 0.054(4) 0.063(5) 0.013(4) -0.001(3) 0.001(4) C9B 0.037(4) 0.043(4) 0.032(3) 0.011(3) 0.001(3) 0.002(3) C10B 0.043(5) 0.038(3) 0.037(4) -0.002(4) 0.003(3) 0.001(4) C11B 0.036(5) 0.036(3) 0.034(5) 0.011(4) 0.005(4) -0.001(4) C12B 0.030(5) 0.039(4) 0.038(5) 0.007(3) -0.003(4) -0.005(3) C13B 0.043(4) 0.038(4) 0.041(4) 0.003(3) 0.007(3) 0.004(3) C14B 0.036(6) 0.039(4) 0.058(7) 0.010(3) 0.002(5) -0.004(3) C15B 0.039(3) 0.043(3) 0.042(4) 0.015(3) 0.000(3) 0.007(3) C16B 0.053(6) 0.046(4) 0.052(5) 0.001(4) -0.008(4) -0.013(4) C17B 0.049(5) 0.043(4) 0.061(4) 0.010(3) -0.014(4) -0.011(4) C18B 0.041(7) 0.044(5) 0.036(6) 0.005(2) -0.021(5) -0.009(3) C19B 0.047(4) 0.060(4) 0.045(4) 0.003(3) -0.008(3) -0.004(3) C20B 0.067(4) 0.060(4) 0.030(3) 0.002(3) -0.007(3) 0.002(4) C21B 0.063(5) 0.057(4) 0.072(5) -0.002(4) 0.007(4) 0.013(3) C22B 0.068(5) 0.061(5) 0.060(5) 0.004(4) 0.004(4) 0.005(4) C23B 0.085(7) 0.075(5) 0.067(6) -0.001(5) -0.001(4) -0.006(6) C24B 0.068(6) 0.135(8) 0.092(8) 0.005(7) -0.014(6) -0.038(7) C25B 0.114(8) 0.079(5) 0.052(6) -0.003(5) 0.003(5) -0.005(6) C26B 0.058(5) 0.070(5) 0.076(6) 0.011(5) -0.005(4) 0.003(5) C27B 0.075(7) 0.065(5) 0.096(8) 0.004(6) -0.004(6) -0.009(6) C28B 0.078(5) 0.105(6) 0.038(4) 0.011(4) 0.003(3) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1A C16A 1.758(7) . ? S1A C15A 1.766(6) . ? S2A C17A 1.757(7) . ? S2A C15A 1.768(5) . ? S3A C18A 1.745(11) . ? S3A C19A 1.778(6) . ? S4A C20A 1.763(7) . ? S4A C18A 1.827(11) . ? S5A C16A 1.775(7) . ? S5A C21A 1.814(7) . ? S6A C19A 1.758(6) . ? S6A C26A 1.803(8) . ? C1A C2A 1.359(12) . ? C1A C11A 1.376(12) . ? C2A C3A 1.389(13) . ? C3A C4A 1.377(8) . ? C4A C12A 1.402(11) . ? C5A C6A 1.363(8) . ? C5A C13A 1.397(7) . ? C6A C7A 1.383(9) . ? C7A C8A 1.393(9) . ? C8A C14A 1.379(12) . ? C9A C15A 1.351(7) . ? C9A C11A 1.487(10) . ? C9A C14A 1.488(10) . ? C10A C18A 1.349(13) . ? C10A C13A 1.468(9) . ? C10A C12A 1.472(12) . ? C11A C12A 1.397(12) . ? C13A C14A 1.417(11) . ? C16A C17A 1.320(9) . ? C17A C27A 1.512(11) . ? C19A C20A 1.324(8) . ? C20A C28A 1.524(8) . ? C21A C22A 1.511(9) . ? C22A C23A 1.482(10) . ? C23A C24A 1.500(13) . ? C24A C25A 1.454(14) . ? C25A C26A 1.528(12) . ? S1B C15B 1.760(6) . ? S1B C16B 1.764(8) . ? S2B C15B 1.769(6) . ? S2B C17B 1.773(7) . ? S3B C19B 1.756(6) . ? S3B C18B 1.783(10) . ? S4B C18B 1.714(12) . ? S4B C20B 1.765(7) . ? S5B C16B 1.743(8) . ? S5B C21B 1.824(6) . ? S6B C19B 1.760(6) . ? S6B C26B 1.814(8) . ? C1B C2B 1.401(13) . ? C1B C11B 1.419(11) . ? C2B C3B 1.356(14) . ? C3B C4B 1.385(9) . ? C4B C12B 1.378(11) . ? C5B C13B 1.387(7) . ? C5B C6B 1.403(8) . ? C6B C7B 1.370(9) . ? C7B C8B 1.375(9) . ? C8B C14B 1.416(13) . ? C9B C15B 1.353(7) . ? C9B C14B 1.464(12) . ? C9B C11B 1.475(10) . ? C10B C18B 1.365(13) . ? C10B C13B 1.480(10) . ? C10B C12B 1.483(13) . ? C11B C12B 1.424(12) . ? C13B C14B 1.426(13) . ? C16B C17B 1.346(10) . ? C17B C27B 1.489(12) . ? C19B C20B 1.345(8) . ? C20B C28B 1.496(8) . ? C21B C22B 1.507(8) . ? C22B C23B 1.525(10) . ? C23B C24B 1.572(13) . ? C24B C25B 1.473(13) . ? C25B C26B 1.492(11) . ? 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 C16A S1A C15A 94.4(3) . . ? C17A S2A C15A 95.9(3) . . ? C18A S3A C19A 97.0(4) . . ? C20A S4A C18A 96.0(4) . . ? C16A S5A C21A 100.3(3) . . ? C19A S6A C26A 100.0(3) . . ? C2A C1A C11A 122.0(9) . . ? C1A C2A C3A 119.5(10) . . ? C4A C3A C2A 120.0(7) . . ? C3A C4A C12A 120.3(6) . . ? C6A C5A C13A 121.9(6) . . ? C5A C6A C7A 119.9(6) . . ? C6A C7A C8A 119.8(6) . . ? C14A C8A C7A 120.7(7) . . ? C15A C9A C11A 121.5(6) . . ? C15A C9A C14A 123.2(6) . . ? C11A C9A C14A 114.9(6) . . ? C18A C10A C13A 124.2(8) . . ? C18A C10A C12A 120.8(8) . . ? C13A C10A C12A 114.7(7) . . ? C1A C11A C12A 119.2(8) . . ? C1A C11A C9A 124.0(8) . . ? C12A C11A C9A 116.7(8) . . ? C11A C12A C4A 118.9(8) . . ? C11A C12A C10A 117.8(8) . . ? C4A C12A C10A 123.3(8) . . ? C5A C13A C14A 118.1(6) . . ? C5A C13A C10A 124.9(6) . . ? C14A C13A C10A 117.0(6) . . ? C8A C14A C13A 119.6(7) . . ? C8A C14A C9A 123.7(8) . . ? C13A C14A C9A 116.7(7) . . ? C9A C15A S1A 124.3(4) . . ? C9A C15A S2A 124.9(4) . . ? S1A C15A S2A 110.7(3) . . ? C17A C16A S1A 118.5(6) . . ? C17A C16A S5A 124.8(6) . . ? S1A C16A S5A 116.7(5) . . ? C16A C17A C27A 129.0(7) . . ? C16A C17A S2A 115.2(5) . . ? C27A C17A S2A 115.8(7) . . ? C10A C18A S3A 127.2(8) . . ? C10A C18A S4A 122.8(8) . . ? S3A C18A S4A 109.7(6) . . ? C20A C19A S6A 126.7(5) . . ? C20A C19A S3A 116.7(5) . . ? S6A C19A S3A 116.5(4) . . ? C19A C20A C28A 128.2(6) . . ? C19A C20A S4A 116.8(5) . . ? C28A C20A S4A 115.0(5) . . ? C22A C21A S5A 114.8(5) . . ? C23A C22A C21A 115.4(6) . . ? C22A C23A C24A 114.3(8) . . ? C25A C24A C23A 116.4(9) . . ? C24A C25A C26A 115.0(8) . . ? C25A C26A S6A 116.6(6) . . ? C15B S1B C16B 95.9(3) . . ? C15B S2B C17B 96.0(3) . . ? C19B S3B C18B 94.8(4) . . ? C18B S4B C20B 96.6(4) . . ? C16B S5B C21B 99.8(3) . . ? C19B S6B C26B 101.2(3) . . ? C2B C1B C11B 119.8(9) . . ? C3B C2B C1B 120.3(11) . . ? C2B C3B C4B 120.6(8) . . ? C12B C4B C3B 121.9(7) . . ? C13B C5B C6B 119.6(6) . . ? C7B C6B C5B 120.7(6) . . ? C6B C7B C8B 120.4(6) . . ? C7B C8B C14B 121.3(8) . . ? C15B C9B C14B 124.7(6) . . ? C15B C9B C11B 122.3(6) . . ? C14B C9B C11B 112.9(7) . . ? C18B C10B C13B 122.2(8) . . ? C18B C10B C12B 122.9(8) . . ? C13B C10B C12B 114.5(7) . . ? C1B C11B C12B 118.9(8) . . ? C1B C11B C9B 122.7(7) . . ? C12B C11B C9B 118.4(8) . . ? C4B C12B C11B 118.5(9) . . ? C4B C12B C10B 124.6(8) . . ? C11B C12B C10B 116.8(8) . . ? C5B C13B C14B 120.5(7) . . ? C5B C13B C10B 122.9(6) . . ? C14B C13B C10B 116.6(7) . . ? C8B C14B C13B 117.4(9) . . ? C8B C14B C9B 123.8(9) . . ? C13B C14B C9B 118.8(9) . . ? C9B C15B S1B 124.3(4) . . ? C9B C15B S2B 124.7(4) . . ? S1B C15B S2B 110.8(3) . . ? C17B C16B S5B 125.9(6) . . ? C17B C16B S1B 116.5(6) . . ? S5B C16B S1B 117.4(5) . . ? C16B C17B C27B 127.2(8) . . ? C16B C17B S2B 115.8(6) . . ? C27B C17B S2B 117.0(8) . . ? C10B C18B S4B 125.8(8) . . ? C10B C18B S3B 121.4(8) . . ? S4B C18B S3B 112.5(5) . . ? C20B C19B S3B 117.1(5) . . ? C20B C19B S6B 125.6(5) . . ? S3B C19B S6B 117.2(4) . . ? C19B C20B C28B 127.9(6) . . ? C19B C20B S4B 115.6(5) . . ? C28B C20B S4B 116.5(5) . . ? C22B C21B S5B 114.3(5) . . ? C21B C22B C23B 112.8(6) . . ? C22B C23B C24B 109.4(7) . . ? C25B C24B C23B 115.4(8) . . ? C24B C25B C26B 113.6(8) . . ? C25B C26B S6B 115.9(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 C17A C16A S5A C21A 131.0(6) . . . . ? C16A S5A C21A C22A -58.7(5) . . . . ? S5A C21A C22A C23A 167.2(5) . . . . ? C21A C22A C23A C24A 171.2(8) . . . . ? C22A C23A C24A C25A 143.9(12) . . . . ? C23A C24A C25A C26A -174.2(9) . . . . ? C24A C25A C26A S6A 162.4(10) . . . . ? C25A C26A S6A C19A -69.0(8) . . . . ? C26A S6A C19A C20A -91.8(6) . . . . ? C17B C16B S5B C21B 130.9(7) . . . . ? C16B S5B C21B C22B -57.5(6) . . . . ? S5B C21B C22B C23B 167.8(5) . . . . ? C21B C22B C23B C24B 176.0(7) . . . . ? C22B C23B C24B C25B 150.3(11) . . . . ? C23B C24B C25B C26B -179.7(8) . . . . ? C24B C25B C26B S6B 156.8(9) . . . . ? C25B C26B S6B C19B -70.1(8) . . . . ? C26B S6B C19B C20B -89.0(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.215 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.049 #==================================================END data_(4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H24 S6' _chemical_formula_weight 540.82 _ccdc_compound_id '4' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; S(7), S(8), S(11), C(36), C(37), C(38), C(45), C(46), C(47), C(51) atoms (with their hydrogens) are disordered over 2 positions, A and B, with the occupancies 52.2(2) and 47.8(2)%, respectively. Thermal ellipsoids of other atoms suggest disorder, which was not resolved. ; _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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.944(4) _cell_length_b 14.591(5) _cell_length_c 16.924(7) _cell_angle_alpha 71.18(1) _cell_angle_beta 89.65(2) _cell_angle_gamma 85.66(1) _cell_volume 2550.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 483 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 19.9 _exptl_crystal_description prism _exptl_crystal_colour 'yellowish-green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8814 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details 'XPREP (SHELXTL) program; R(int)=0.058 before correction' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3.00 0.00 2.00 0.0200 3.00 0.00 -2.00 0.0200 1.00 0.00 1.00 0.0500 -1.00 0.00 -1.00 0.0500 0.00 1.00 0.00 0.1700 0.00 -1.00 0.00 0.1700 0.00 2.00 3.00 0.1500 _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 25 s), each set at different \f and/or 2\q angles, nominally covered over a hemisphere of reciprocal space. The first 50 scans (173 reflections) 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 '\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 23433 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11538 _reflns_number_gt 7045 _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^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11538 _refine_ls_number_parameters 678 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.006 _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 0.47761(6) 0.85876(5) 0.18065(5) 0.02843(18) Uani 1 1 d . . . S2 S 0.50293(7) 1.06075(5) 0.07872(5) 0.03112(19) Uani 1 1 d . . . S3 S 0.92918(7) 0.87805(5) 0.38300(4) 0.02653(18) Uani 1 1 d . . . S4 S 0.95816(6) 1.07715(5) 0.27730(4) 0.02336(16) Uani 1 1 d . . . S5 S 0.24078(7) 0.90637(6) 0.25646(7) 0.0465(3) Uani 1 1 d . . . S6 S 0.83152(8) 0.93858(6) 0.52837(5) 0.0357(2) Uani 1 1 d . . . C1 C 0.7320(3) 0.7405(2) 0.17185(19) 0.0262(7) Uani 1 1 d . . . H1 H 0.661(3) 0.737(2) 0.1404(19) 0.041(9) Uiso 1 1 d . . . C2 C 0.8008(3) 0.6559(2) 0.2182(2) 0.0293(7) Uani 1 1 d . . . H2 H 0.775(2) 0.597(2) 0.2170(16) 0.020(7) Uiso 1 1 d . . . C3 C 0.9050(3) 0.6611(2) 0.26114(19) 0.0297(7) Uani 1 1 d . . . H3 H 0.952(2) 0.604(2) 0.2924(17) 0.027(8) Uiso 1 1 d . . . C4 C 0.9421(3) 0.7508(2) 0.26035(18) 0.0239(6) Uani 1 1 d . . . H4 H 1.022(2) 0.7541(19) 0.2874(16) 0.022(7) Uiso 1 1 d . . . C5 C 0.9759(3) 1.0736(2) 0.08875(18) 0.0242(6) Uani 1 1 d . . . H5 H 1.047(3) 1.072(2) 0.1174(18) 0.034(9) Uiso 1 1 d . . . C6 C 0.9564(3) 1.1368(2) 0.00820(18) 0.0271(7) Uani 1 1 d . . . H6 H 1.018(2) 1.1814(18) -0.0154(15) 0.011(6) Uiso 1 1 d . . . C7 C 0.8506(3) 1.1338(2) -0.03610(19) 0.0297(7) Uani 1 1 d . . . H7 H 0.837(3) 1.181(2) -0.0918(19) 0.037(8) Uiso 1 1 d . . . C8 C 0.7656(3) 1.0671(2) 0.00042(19) 0.0273(7) Uani 1 1 d . . . H8 H 0.695(3) 1.067(2) -0.0313(17) 0.028(8) Uiso 1 1 d . . . C9 C 0.7026(2) 0.92583(19) 0.12238(18) 0.0225(6) Uani 1 1 d . . . C10 C 0.9074(2) 0.93402(19) 0.21091(17) 0.0188(6) Uani 1 1 d . . . C11 C 0.8923(2) 1.00577(19) 0.12566(16) 0.0196(6) Uani 1 1 d . . . C12 C 0.7856(2) 1.0021(2) 0.08040(17) 0.0223(6) Uani 1 1 d . . . C13 C 0.7675(2) 0.83112(19) 0.16993(17) 0.0208(6) Uani 1 1 d . . . C14 C 0.8734(2) 0.83600(19) 0.21508(17) 0.0200(6) Uani 1 1 d . . . C15 C 0.5795(2) 0.9444(2) 0.12516(18) 0.0261(7) Uani 1 1 d . . . C16 C 0.3633(3) 0.9471(2) 0.1900(2) 0.0329(8) Uani 1 1 d . . . C17 C 0.3754(3) 1.0398(2) 0.1442(2) 0.0330(8) Uani 1 1 d . . . C18 C 0.9327(2) 0.95824(19) 0.27927(17) 0.0203(6) Uani 1 1 d . . . C19 C 0.8832(3) 0.9723(2) 0.42516(18) 0.0272(7) Uani 1 1 d . . . C20 C 0.8939(3) 1.0638(2) 0.37612(18) 0.0269(7) Uani 1 1 d . . . C21 C 0.3220(3) 0.8573(3) 0.3574(2) 0.0427(9) Uani 1 1 d . . . H211 H 0.259(3) 0.850(2) 0.394(2) 0.053(11) Uiso 1 1 d . . . H212 H 0.362(3) 0.792(2) 0.3625(19) 0.041(9) Uiso 1 1 d . . . C22 C 0.4144(3) 0.9232(2) 0.3721(2) 0.0346(8) Uani 1 1 d . . . H221 H 0.471(2) 0.9445(19) 0.3230(17) 0.023(7) Uiso 1 1 d . . . H222 H 0.377(3) 0.984(2) 0.3692(19) 0.045(10) Uiso 1 1 d . . . C23 C 0.4933(3) 0.8763(2) 0.4499(2) 0.0366(8) Uani 1 1 d . . . H231 H 0.518(3) 0.814(3) 0.455(2) 0.048(10) Uiso 1 1 d . . . H232 H 0.444(3) 0.869(2) 0.5037(19) 0.036(8) Uiso 1 1 d . . . C24 C 0.6073(3) 0.9300(2) 0.4510(2) 0.0316(7) Uani 1 1 d . . . H241 H 0.654(3) 0.941(2) 0.3967(19) 0.036(9) Uiso 1 1 d . . . H242 H 0.583(3) 0.997(2) 0.4514(18) 0.035(8) Uiso 1 1 d . . . C25 C 0.6977(3) 0.8744(2) 0.5208(2) 0.0358(8) Uani 1 1 d . . . H251 H 0.719(3) 0.810(2) 0.5133(17) 0.032(8) Uiso 1 1 d . . . H252 H 0.661(3) 0.863(2) 0.577(2) 0.048(10) Uiso 1 1 d . . . C27 C 0.2933(3) 1.1281(2) 0.1424(3) 0.0485(10) Uani 1 1 d . . . H271 H 0.2276 1.1093 0.1826 0.061(12) Uiso 1 1 d R . . H272 H 0.2576 1.1582 0.0862 0.074(13) Uiso 1 1 d R . . H273 H 0.3415 1.1746 0.1567 0.053(10) Uiso 1 1 d R . . C28 C 0.8585(3) 1.1560(2) 0.3949(2) 0.0357(8) Uani 1 1 d . . . H281 H 0.8330 1.1406 0.4530 0.071(12) Uiso 1 1 d R . . H282 H 0.7904 1.1918 0.3577 0.084(14) Uiso 1 1 d R . . H283 H 0.9285 1.1960 0.3859 0.063(12) Uiso 1 1 d R . . S7A S 0.57158(18) 0.38054(16) 0.39193(12) 0.0270(4) Uani 0.5224(16) 1 d P A 1 S8A S 0.51405(19) 0.58449(15) 0.29388(11) 0.0272(4) Uani 0.5224(16) 1 d P A 1 S7B S 0.6152(2) 0.36838(18) 0.41803(13) 0.0270(4) Uani 0.48 1 d P A 2 S8B S 0.5362(2) 0.57236(16) 0.33241(13) 0.0272(4) Uani 0.48 1 d P A 2 S9 S 0.96427(6) 0.34560(5) 0.15345(4) 0.02308(16) Uani 1 1 d . . . S10 S 0.90129(6) 0.55175(5) 0.06202(4) 0.02291(16) Uani 1 1 d . . . S11A S 0.69407(17) 0.42912(14) 0.53217(11) 0.0323(4) Uani 0.5224(16) 1 d P A 1 S11B S 0.75188(19) 0.41374(16) 0.55511(12) 0.0323(4) Uani 0.48 1 d P A 2 S12 S 1.21853(7) 0.38092(6) 0.20118(5) 0.03254(19) Uani 1 1 d . . . C31 C 0.5337(3) 0.2587(2) 0.2794(2) 0.0439(9) Uani 1 1 d . . . H31 H 0.4730 0.2643 0.3183 0.053 Uiso 1 1 d R . . C32 C 0.5685(3) 0.1680(2) 0.2726(2) 0.0386(8) Uani 1 1 d . . . H32 H 0.5322 0.1121 0.3069 0.046 Uiso 1 1 d R . . C33 C 0.6567(3) 0.1591(2) 0.2162(2) 0.0334(8) Uani 1 1 d . . . H33 H 0.6806 0.0970 0.2119 0.040 Uiso 1 1 d R . . C34 C 0.7102(3) 0.2402(2) 0.16594(19) 0.0286(7) Uani 1 1 d . . . H34 H 0.7709 0.2333 0.1275 0.034 Uiso 1 1 d R . . C35 C 0.6258(3) 0.5755(2) 0.0111(2) 0.0446(9) Uani 1 1 d . . . H35 H 0.6900 0.5654 -0.0239 0.054 Uiso 1 1 d R A . C36A C 0.5480(5) 0.6521(4) -0.0245(4) 0.0227(14) Uiso 0.5224(16) 1 d P A 1 H36A H 0.5517 0.6927 -0.0810 0.027 Uiso 0.5224(16) 1 d PR A 1 C37A C 0.4594(5) 0.6650(4) 0.0326(4) 0.0178(12) Uiso 0.5224(16) 1 d P A 1 H37A H 0.4019 0.7202 0.0171 0.021 Uiso 0.5224(16) 1 d PR A 1 C38A C 0.4566(5) 0.5962(4) 0.1122(4) 0.0210(13) Uiso 0.5224(16) 1 d P A 1 H38A H 0.3883 0.6038 0.1450 0.025 Uiso 0.5224(16) 1 d PR A 1 C36B C 0.5250(6) 0.6560(4) 0.0064(5) 0.0206(14) Uiso 0.4776(16) 1 d P A 2 H36B H 0.5138 0.7060 -0.0459 0.025 Uiso 0.4776(16) 1 d PR A 2 C37B C 0.4472(6) 0.6643(5) 0.0702(4) 0.0258(15) Uiso 0.4776(16) 1 d P A 2 H37B H 0.3885 0.7184 0.0596 0.031 Uiso 0.4776(16) 1 d PR A 2 C38B C 0.4546(6) 0.5952(5) 0.1482(4) 0.0247(15) Uiso 0.4776(16) 1 d P A 2 H38B H 0.4076 0.5992 0.1945 0.030 Uiso 0.4776(16) 1 d PR A 2 C39 C 0.5536(3) 0.4406(2) 0.2324(3) 0.0440(10) Uani 1 1 d . . . C40 C 0.7243(2) 0.4236(2) 0.11956(18) 0.0260(7) Uani 1 1 d . . . C41 C 0.6299(3) 0.5072(2) 0.0908(2) 0.0339(8) Uani 1 1 d . A . C42 C 0.5429(3) 0.5163(2) 0.1502(3) 0.0463(10) Uani 1 1 d . A . C43 C 0.5864(3) 0.3414(2) 0.2297(2) 0.0360(8) Uani 1 1 d . A . C44 C 0.6753(2) 0.3325(2) 0.17103(19) 0.0281(7) Uani 1 1 d . A . C45A C 0.5401(5) 0.4633(4) 0.2901(4) 0.0177(12) Uiso 0.5224(16) 1 d P A 1 C46A C 0.6208(5) 0.4692(4) 0.4337(4) 0.0245(13) Uiso 0.5224(16) 1 d P A 1 C47A C 0.5966(6) 0.5618(4) 0.3890(4) 0.0232(13) Uiso 0.5224(16) 1 d P A 1 C45B C 0.5653(5) 0.4567(4) 0.3223(4) 0.0170(13) Uiso 0.4776(16) 1 d P A 2 C46B C 0.6661(6) 0.4558(4) 0.4607(4) 0.0206(14) Uiso 0.4776(16) 1 d P A 2 C47B C 0.6310(6) 0.5480(5) 0.4217(5) 0.0287(16) Uiso 0.4776(16) 1 d P A 2 C48 C 0.8447(2) 0.43681(19) 0.11066(16) 0.0207(6) Uani 1 1 d . A . C49 C 1.0755(2) 0.4281(2) 0.15170(17) 0.0229(6) Uani 1 1 d . . . C50 C 1.0464(2) 0.5219(2) 0.11037(16) 0.0228(6) Uani 1 1 d . . . C51A C 0.6324(6) 0.6502(4) 0.4078(4) 0.0326(15) Uiso 0.5224(16) 1 d P A 1 H511 H 0.6014 0.7088 0.3631 0.049 Uiso 0.5224(16) 1 d PR A 1 H512 H 0.7220 0.6484 0.4116 0.049 Uiso 0.5224(16) 1 d PR A 1 H513 H 0.5972 0.6511 0.4610 0.049 Uiso 0.5224(16) 1 d PR A 1 C51B C 0.6643(7) 0.6343(5) 0.4463(5) 0.0385(18) Uiso 0.4776(16) 1 d P A 2 H514 H 0.6259 0.6943 0.4068 0.058 Uiso 0.4776(16) 1 d PR A 2 H515 H 0.7536 0.6369 0.4454 0.058 Uiso 0.4776(16) 1 d PR A 2 H516 H 0.6353 0.6274 0.5027 0.058 Uiso 0.4776(16) 1 d PR A 2 C52 C 1.1241(3) 0.6051(2) 0.0997(2) 0.0341(8) Uani 1 1 d . . . H521 H 1.2038 0.5808 0.1276 0.051 Uiso 1 1 d R . . H522 H 1.0832 0.6512 0.1243 0.051 Uiso 1 1 d R . . H523 H 1.1363 0.6379 0.0401 0.051 Uiso 1 1 d R . . C53A C 0.8343(6) 0.3643(5) 0.5130(4) 0.0327(16) Uiso 0.5224(16) 1 d P A 1 H531 H 0.8819 0.3395 0.5661 0.043 Uiso 0.5224(16) 1 d PR A 1 H532 H 0.8101 0.3069 0.4996 0.043 Uiso 0.5224(16) 1 d PR A 1 C53B C 0.8900(6) 0.3585(5) 0.5237(4) 0.0275(15) Uiso 0.4776(16) 1 d P A 2 H533 H 0.9568 0.3511 0.5649 0.036 Uiso 0.4776(16) 1 d PR A 2 H534 H 0.8746 0.2932 0.5220 0.036 Uiso 0.4776(16) 1 d PR A 2 C54 C 0.9256(4) 0.4193(2) 0.4407(2) 0.0496(10) Uani 1 1 d . . . H541 H 0.9374 0.4794 0.4404 0.065 Uiso 1 1 d R A . H542 H 0.8714 0.4323 0.3917 0.065 Uiso 1 1 d R . . C55 C 1.0429(4) 0.3651(2) 0.42531(19) 0.0456(9) Uani 1 1 d . A . H551 H 1.1065 0.3672 0.4658 0.059 Uiso 1 1 d R . . H552 H 1.0281 0.2962 0.4354 0.059 Uiso 1 1 d R . . C56 C 1.0901(3) 0.4087(2) 0.33702(18) 0.0353(8) Uani 1 1 d . . . H561 H 1.0192 0.4306 0.2976 0.046 Uiso 1 1 d R A . H562 H 1.1346 0.4663 0.3339 0.046 Uiso 1 1 d R . . C57 C 1.1743(3) 0.3368(2) 0.31048(18) 0.0353(8) Uani 1 1 d . A . H571 H 1.1330 0.2762 0.3203 0.046 Uiso 1 1 d R . . H572 H 1.2493 0.3208 0.3461 0.046 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0180(4) 0.0220(4) 0.0480(5) -0.0147(4) -0.0009(3) -0.0025(3) S2 0.0205(4) 0.0215(4) 0.0507(5) -0.0110(4) -0.0095(3) 0.0008(3) S3 0.0338(4) 0.0204(4) 0.0232(4) -0.0051(3) 0.0042(3) 0.0024(3) S4 0.0260(4) 0.0194(4) 0.0253(4) -0.0078(3) 0.0013(3) -0.0036(3) S5 0.0152(4) 0.0372(5) 0.0949(8) -0.0313(5) 0.0101(4) -0.0077(4) S6 0.0471(5) 0.0335(5) 0.0252(4) -0.0089(4) 0.0080(4) 0.0025(4) C1 0.0210(16) 0.0258(17) 0.0358(17) -0.0148(14) 0.0034(13) -0.0048(13) C2 0.0301(18) 0.0198(16) 0.0414(19) -0.0142(14) 0.0081(14) -0.0045(13) C3 0.0319(18) 0.0209(16) 0.0346(17) -0.0081(14) 0.0038(14) 0.0042(14) C4 0.0204(15) 0.0205(15) 0.0297(16) -0.0079(13) -0.0005(13) 0.0037(12) C5 0.0180(15) 0.0233(16) 0.0310(16) -0.0083(13) -0.0003(13) -0.0007(12) C6 0.0255(16) 0.0217(16) 0.0309(17) -0.0033(13) 0.0013(13) -0.0047(13) C7 0.0351(18) 0.0221(16) 0.0279(17) -0.0032(14) -0.0048(14) 0.0018(14) C8 0.0227(16) 0.0244(16) 0.0348(17) -0.0100(14) -0.0095(13) -0.0001(13) C9 0.0211(15) 0.0178(14) 0.0312(16) -0.0113(12) -0.0040(12) -0.0018(12) C10 0.0121(13) 0.0163(14) 0.0278(15) -0.0073(12) 0.0004(11) 0.0006(11) C11 0.0184(14) 0.0158(14) 0.0250(15) -0.0079(12) 0.0011(11) 0.0024(11) C12 0.0172(14) 0.0212(15) 0.0314(16) -0.0126(13) -0.0025(12) -0.0008(12) C13 0.0145(14) 0.0191(14) 0.0298(16) -0.0094(12) 0.0033(11) -0.0016(11) C14 0.0177(14) 0.0180(14) 0.0250(15) -0.0084(12) 0.0059(11) -0.0001(11) C15 0.0203(15) 0.0192(15) 0.0393(18) -0.0106(13) -0.0067(13) 0.0004(12) C16 0.0139(15) 0.0318(18) 0.059(2) -0.0233(16) -0.0044(14) -0.0020(13) C17 0.0155(15) 0.0272(17) 0.062(2) -0.0220(16) -0.0076(14) 0.0007(13) C18 0.0167(14) 0.0183(14) 0.0245(15) -0.0056(12) 0.0008(11) 0.0003(11) C19 0.0320(17) 0.0242(16) 0.0262(16) -0.0103(13) 0.0062(13) 0.0023(13) C20 0.0263(16) 0.0287(17) 0.0279(16) -0.0134(13) 0.0037(13) 0.0021(13) C21 0.034(2) 0.029(2) 0.070(3) -0.0216(18) 0.0276(19) -0.0139(16) C22 0.0316(19) 0.0225(17) 0.053(2) -0.0156(16) 0.0183(16) -0.0080(14) C23 0.055(2) 0.0202(17) 0.038(2) -0.0125(15) 0.0232(17) -0.0097(16) C24 0.040(2) 0.0168(16) 0.0365(18) -0.0072(14) 0.0165(15) -0.0017(14) C25 0.055(2) 0.0238(17) 0.0283(18) -0.0092(14) 0.0131(16) -0.0001(16) C27 0.0218(18) 0.0301(19) 0.097(3) -0.027(2) -0.006(2) 0.0017(15) C28 0.044(2) 0.0264(17) 0.040(2) -0.0171(15) 0.0038(16) 0.0010(16) S7A 0.0333(12) 0.0235(7) 0.0205(10) -0.0018(8) 0.0024(6) -0.0034(8) S8A 0.0277(8) 0.0222(6) 0.0312(11) -0.0096(9) 0.0033(9) 0.0041(5) S7B 0.0333(12) 0.0235(7) 0.0205(10) -0.0018(8) 0.0024(6) -0.0034(8) S8B 0.0277(8) 0.0222(6) 0.0312(11) -0.0096(9) 0.0033(9) 0.0041(5) S9 0.0194(4) 0.0206(4) 0.0260(4) -0.0034(3) 0.0004(3) -0.0001(3) S10 0.0210(4) 0.0215(4) 0.0225(4) -0.0018(3) 0.0000(3) -0.0027(3) S11A 0.0354(11) 0.0406(8) 0.0214(8) -0.0117(7) 0.0031(6) 0.0021(8) S11B 0.0354(11) 0.0406(8) 0.0214(8) -0.0117(7) 0.0031(6) 0.0021(8) S12 0.0174(4) 0.0377(5) 0.0389(5) -0.0086(4) -0.0006(3) 0.0036(3) C31 0.0192(17) 0.0264(18) 0.081(3) -0.0097(18) 0.0166(16) -0.0075(14) C32 0.0237(17) 0.0189(16) 0.065(2) -0.0014(16) 0.0019(16) -0.0081(13) C33 0.0241(17) 0.0193(16) 0.055(2) -0.0102(15) -0.0126(15) 0.0005(13) C34 0.0183(15) 0.0238(16) 0.0429(18) -0.0104(14) -0.0082(13) 0.0012(13) C35 0.0269(18) 0.0242(18) 0.073(3) -0.0013(17) -0.0231(17) -0.0068(14) C39 0.0138(16) 0.0200(17) 0.094(3) -0.0121(18) 0.0203(17) -0.0045(13) C40 0.0194(15) 0.0202(15) 0.0360(17) -0.0057(13) -0.0058(12) -0.0013(12) C41 0.0148(15) 0.0174(15) 0.064(2) -0.0047(15) -0.0115(15) -0.0061(12) C42 0.0168(16) 0.0178(17) 0.098(3) -0.0097(18) -0.0025(18) -0.0042(13) C43 0.0176(16) 0.0172(15) 0.069(2) -0.0079(15) 0.0043(15) -0.0013(12) C44 0.0155(15) 0.0212(16) 0.0433(18) -0.0046(14) -0.0050(13) -0.0008(12) C48 0.0239(15) 0.0174(14) 0.0189(14) -0.0031(11) -0.0005(11) -0.0017(12) C49 0.0174(14) 0.0280(16) 0.0215(14) -0.0059(12) 0.0034(11) -0.0006(12) C50 0.0170(14) 0.0300(16) 0.0205(14) -0.0068(13) 0.0030(11) -0.0027(12) C52 0.0283(17) 0.0334(18) 0.0396(19) -0.0086(15) -0.0012(14) -0.0095(14) C54 0.097(3) 0.0272(19) 0.0259(18) -0.0091(15) 0.0179(18) -0.0119(19) C55 0.088(3) 0.0253(18) 0.0218(17) -0.0063(14) -0.0005(17) -0.0012(18) C56 0.049(2) 0.0258(17) 0.0274(17) -0.0048(14) -0.0069(14) 0.0021(15) C57 0.0335(18) 0.0334(18) 0.0324(17) -0.0033(14) -0.0112(14) 0.0060(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C15 1.768(3) . ? S1 C16 1.771(3) . ? S2 C17 1.759(3) . ? S2 C15 1.771(3) . ? S3 C18 1.770(3) . ? S3 C19 1.783(3) . ? S4 C18 1.768(3) . ? S4 C20 1.768(3) . ? S5 C16 1.757(3) . ? S5 C21 1.831(4) . ? S6 C19 1.757(3) . ? S6 C25 1.823(4) . ? C1 C2 1.395(4) . ? C1 C13 1.397(4) . ? C2 C3 1.375(4) . ? C3 C4 1.395(4) . ? C4 C14 1.396(4) . ? C5 C6 1.385(4) . ? C5 C11 1.392(4) . ? C6 C7 1.394(4) . ? C7 C8 1.392(4) . ? C8 C12 1.387(4) . ? C9 C15 1.357(4) . ? C9 C12 1.484(4) . ? C9 C13 1.484(4) . ? C10 C18 1.350(4) . ? C10 C14 1.484(4) . ? C10 C11 1.486(4) . ? C11 C12 1.414(4) . ? C13 C14 1.411(4) . ? C16 C17 1.341(4) . ? C17 C27 1.506(4) . ? C19 C20 1.338(4) . ? C20 C28 1.503(4) . ? C21 C22 1.521(5) . ? C22 C23 1.514(5) . ? C23 C24 1.526(5) . ? C24 C25 1.520(5) . ? S7A C45A 1.774(6) . ? S7A C46A 1.780(6) . ? S8A C47A 1.774(7) . ? S8A C45A 1.790(6) . ? S7B C45B 1.772(6) . ? S7B C46B 1.780(7) . ? S8B C45B 1.756(6) . ? S8B C47B 1.761(8) . ? S9 C49 1.768(3) . ? S9 C48 1.770(3) . ? S10 C50 1.750(3) . ? S10 C48 1.770(3) . ? S11A C46A 1.754(6) . ? S11A C53A 1.825(7) . ? S11B C46B 1.763(7) . ? S11B C53B 1.816(7) . ? S12 C49 1.763(3) . ? S12 C57 1.827(3) . ? C31 C32 1.389(4) . ? C31 C43 1.395(4) . ? C32 C33 1.383(4) . ? C33 C34 1.383(4) . ? C34 C44 1.401(4) . ? C35 C36A 1.328(6) . ? C35 C41 1.392(4) . ? C35 C36B 1.532(7) . ? C36A C37A 1.410(8) . ? C37A C38A 1.398(8) . ? C38A C42 1.422(6) . ? C36B C37B 1.402(10) . ? C37B C38B 1.376(9) . ? C38B C42 1.437(7) . ? C39 C45A 1.135(6) . ? C39 C42 1.470(5) . ? C39 C43 1.479(4) . ? C39 C45B 1.620(7) . ? C40 C48 1.347(4) . ? C40 C44 1.473(4) . ? C40 C41 1.491(4) . ? C41 C42 1.412(5) . ? C43 C44 1.415(4) . ? C46A C47A 1.325(8) . ? C47A C51A 1.504(8) . ? C46B C47B 1.320(9) . ? C47B C51B 1.518(10) . ? C49 C50 1.335(4) . ? C50 C52 1.498(4) . ? C53A C54 1.616(7) . ? C53B C54 1.467(7) . ? C54 C55 1.523(5) . ? C55 C56 1.527(4) . ? C56 C57 1.519(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 C15 S1 C16 94.80(14) . . ? C17 S2 C15 95.63(14) . . ? C18 S3 C19 93.76(13) . . ? C18 S4 C20 94.66(13) . . ? C16 S5 C21 100.59(16) . . ? C19 S6 C25 101.51(15) . . ? C2 C1 C13 120.1(3) . . ? C3 C2 C1 120.4(3) . . ? C2 C3 C4 120.5(3) . . ? C3 C4 C14 119.7(3) . . ? C6 C5 C11 120.9(3) . . ? C5 C6 C7 119.6(3) . . ? C8 C7 C6 120.0(3) . . ? C12 C8 C7 120.7(3) . . ? C15 C9 C12 122.8(2) . . ? C15 C9 C13 122.9(3) . . ? C12 C9 C13 113.9(2) . . ? C18 C10 C14 123.1(2) . . ? C18 C10 C11 123.4(2) . . ? C14 C10 C11 112.9(2) . . ? C5 C11 C12 119.4(2) . . ? C5 C11 C10 124.4(2) . . ? C12 C11 C10 116.2(2) . . ? C8 C12 C11 119.2(3) . . ? C8 C12 C9 124.1(3) . . ? C11 C12 C9 116.6(2) . . ? C1 C13 C14 119.3(3) . . ? C1 C13 C9 124.9(3) . . ? C14 C13 C9 115.8(2) . . ? C4 C14 C13 119.9(3) . . ? C4 C14 C10 122.8(3) . . ? C13 C14 C10 117.2(2) . . ? C9 C15 S1 124.8(2) . . ? C9 C15 S2 123.4(2) . . ? S1 C15 S2 111.68(15) . . ? C17 C16 S5 125.0(2) . . ? C17 C16 S1 117.4(2) . . ? S5 C16 S1 117.61(18) . . ? C16 C17 C27 127.8(3) . . ? C16 C17 S2 116.1(2) . . ? C27 C17 S2 116.2(2) . . ? C10 C18 S4 124.2(2) . . ? C10 C18 S3 124.3(2) . . ? S4 C18 S3 111.19(15) . . ? C20 C19 S6 124.9(2) . . ? C20 C19 S3 117.1(2) . . ? S6 C19 S3 117.92(16) . . ? C19 C20 C28 128.0(3) . . ? C19 C20 S4 115.7(2) . . ? C28 C20 S4 116.3(2) . . ? C22 C21 S5 113.9(3) . . ? C23 C22 C21 113.5(3) . . ? C22 C23 C24 112.7(3) . . ? C25 C24 C23 113.0(3) . . ? C24 C25 S6 114.7(2) . . ? C45A S7A C46A 95.0(3) . . ? C47A S8A C45A 95.3(3) . . ? C45B S7B C46B 93.7(3) . . ? C45B S8B C47B 95.0(3) . . ? C49 S9 C48 94.86(13) . . ? C50 S10 C48 95.81(13) . . ? C46A S11A C53A 102.4(3) . . ? C46B S11B C53B 101.5(3) . . ? C49 S12 C57 101.00(13) . . ? C32 C31 C43 120.8(3) . . ? C33 C32 C31 119.9(3) . . ? C32 C33 C34 120.4(3) . . ? C33 C34 C44 120.6(3) . . ? C36A C35 C41 131.5(4) . . ? C36A C35 C36B 22.7(3) . . ? C41 C35 C36B 109.6(4) . . ? C35 C36A C37A 110.9(5) . . ? C38A C37A C36A 119.7(5) . . ? C37A C38A C42 128.3(5) . . ? C37B C36B C35 127.5(5) . . ? C38B C37B C36B 121.0(6) . . ? C37B C38B C42 111.1(6) . . ? C45A C39 C42 118.3(4) . . ? C45A C39 C43 127.1(4) . . ? C42 C39 C43 114.6(3) . . ? C45A C39 C45B 14.0(4) . . ? C42 C39 C45B 126.9(3) . . ? C43 C39 C45B 116.8(3) . . ? C48 C40 C44 123.9(2) . . ? C48 C40 C41 121.1(3) . . ? C44 C40 C41 114.0(2) . . ? C35 C41 C42 119.9(3) . . ? C35 C41 C40 123.9(3) . . ? C42 C41 C40 116.2(3) . . ? C41 C42 C38A 109.2(4) . . ? C41 C42 C38B 130.3(4) . . ? C38A C42 C38B 24.4(3) . . ? C41 C42 C39 116.2(3) . . ? C38A C42 C39 134.4(4) . . ? C38B C42 C39 112.9(4) . . ? C31 C43 C44 119.2(3) . . ? C31 C43 C39 124.2(3) . . ? C44 C43 C39 116.6(3) . . ? C34 C44 C43 119.0(3) . . ? C34 C44 C40 125.2(3) . . ? C43 C44 C40 115.8(3) . . ? C39 C45A S7A 121.7(5) . . ? C39 C45A S8A 127.1(5) . . ? S7A C45A S8A 110.2(4) . . ? C47A C46A S11A 124.3(5) . . ? C47A C46A S7A 117.5(5) . . ? S11A C46A S7A 118.3(3) . . ? C46A C47A C51A 128.2(6) . . ? C46A C47A S8A 116.0(5) . . ? C51A C47A S8A 115.8(5) . . ? C39 C45B S8B 121.0(4) . . ? C39 C45B S7B 127.0(4) . . ? S8B C45B S7B 111.9(4) . . ? C47B C46B S11B 124.3(5) . . ? C47B C46B S7B 117.4(6) . . ? S11B C46B S7B 118.2(3) . . ? C46B C47B C51B 126.3(7) . . ? C46B C47B S8B 116.5(6) . . ? C51B C47B S8B 117.2(5) . . ? C40 C48 S10 123.0(2) . . ? C40 C48 S9 124.8(2) . . ? S10 C48 S9 111.97(15) . . ? C50 C49 S12 124.4(2) . . ? C50 C49 S9 117.4(2) . . ? S12 C49 S9 118.13(16) . . ? C49 C50 C52 127.6(3) . . ? C49 C50 S10 116.6(2) . . ? C52 C50 S10 115.8(2) . . ? C54 C53A S11A 119.9(4) . . ? C54 C53B S11B 109.7(4) . . ? C53B C54 C55 102.9(4) . . ? C53B C54 C53A 22.9(3) . . ? C55 C54 C53A 119.7(3) . . ? C54 C55 C56 112.6(3) . . ? C57 C56 C55 112.5(2) . . ? C56 C57 S12 114.0(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.460 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.070 #==================================================END