# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2010 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_recoll _database_code_depnum_ccdc_archive 'CCDC 783815' #TrackingRef '2009src1321r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H42 O S9' _chemical_formula_weight 863.31 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 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 18.4493(18) _cell_length_b 16.6052(16) _cell_length_c 14.1055(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.196(4) _cell_angle_gamma 90.00 _cell_volume 4265.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 222105 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9065 _exptl_absorpt_correction_T_max 0.9950 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX2 Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 51176 _diffrn_reflns_av_R_equivalents 0.1372 _diffrn_reflns_av_sigmaI/netI 0.1340 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9743 _reflns_number_gt 5462 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'Sheldrick, G.M. (2008). Acta Cryst. A64, 112-1' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0000P)^2^+63.1247P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9743 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2375 _refine_ls_R_factor_gt 0.1478 _refine_ls_wR_factor_ref 0.2903 _refine_ls_wR_factor_gt 0.2442 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7112(6) 0.4491(6) -0.0463(7) 0.042(2) Uani 1 1 d . . . C2 C 0.6143(5) 0.5657(6) -0.0683(6) 0.033(2) Uani 1 1 d . . . C3 C 0.6445(5) 0.5634(6) -0.1553(6) 0.034(2) Uani 1 1 d . . . C4 C 0.5589(5) 0.6200(6) -0.0694(6) 0.034(2) Uani 1 1 d . . . C5 C 0.6135(5) 0.6163(6) -0.2224(6) 0.034(2) Uani 1 1 d . . . C6 C 0.5142(5) 0.6382(5) 0.0043(6) 0.028(2) Uani 1 1 d . . . C7 C 0.4550(5) 0.6881(5) -0.0006(6) 0.033(2) Uani 1 1 d . . . H7 H 0.4361 0.7183 -0.0563 0.039 Uiso 1 1 calc R . . C8 C 0.4246(5) 0.6906(5) 0.0846(6) 0.034(2) Uani 1 1 d . . . H8 H 0.3833 0.7226 0.0924 0.040 Uiso 1 1 calc R . . C9 C 0.4609(5) 0.6418(6) 0.1555(6) 0.035(2) Uani 1 1 d . . . C10 C 0.4456(5) 0.6230(6) 0.2504(6) 0.035(2) Uani 1 1 d . . . C11 C 0.4725(6) 0.5630(7) 0.3107(7) 0.043(3) Uani 1 1 d . . . H11 H 0.5094 0.5267 0.2972 0.051 Uiso 1 1 calc R . . C12 C 0.4414(6) 0.5589(6) 0.3944(7) 0.042(2) Uani 1 1 d . . . H12 H 0.4560 0.5205 0.4436 0.050 Uiso 1 1 calc R . . C13 C 0.3882(5) 0.6148(6) 0.3990(6) 0.034(2) Uani 1 1 d . . . C14 C 0.3495(5) 0.6283(6) 0.4808(6) 0.037(2) Uani 1 1 d . . . C15 C 0.3176(6) 0.6236(6) 0.6461(7) 0.042(2) Uani 1 1 d . . . C16 C 0.3190(6) 0.6068(6) 0.7523(7) 0.048(3) Uani 1 1 d . . . H16A H 0.3648 0.6277 0.7889 0.072 Uiso 1 1 calc R . . H16B H 0.3162 0.5486 0.7625 0.072 Uiso 1 1 calc R . . H16C H 0.2771 0.6333 0.7739 0.072 Uiso 1 1 calc R . . C17 C 0.2669(6) 0.6631(6) 0.5825(7) 0.041(2) Uani 1 1 d . . . H17 H 0.2238 0.6866 0.5994 0.050 Uiso 1 1 calc R . . C18 C 0.2846(5) 0.6658(6) 0.4874(7) 0.035(2) Uani 1 1 d . . . C19 C 0.2360(6) 0.7066(7) 0.4070(7) 0.046(3) Uani 1 1 d . . . H19A H 0.2665 0.7402 0.3708 0.055 Uiso 1 1 calc R . . H19B H 0.2019 0.7429 0.4341 0.055 Uiso 1 1 calc R . . C20 C 0.1909(7) 0.6474(7) 0.3373(7) 0.061(3) Uani 1 1 d . . . H20A H 0.2229 0.6026 0.3232 0.073 Uiso 1 1 calc R . . H20B H 0.1510 0.6244 0.3681 0.073 Uiso 1 1 calc R . . C21 C 0.1579(7) 0.6886(9) 0.2435(9) 0.071(4) Uani 1 1 d . . . H21A H 0.1305 0.7369 0.2588 0.085 Uiso 1 1 calc R . . H21B H 0.1983 0.7070 0.2104 0.085 Uiso 1 1 calc R . . C22 C 0.1069(7) 0.6357(8) 0.1756(9) 0.065(3) Uani 1 1 d . . . H22A H 0.0648 0.6195 0.2070 0.078 Uiso 1 1 calc R . . H22B H 0.1334 0.5862 0.1620 0.078 Uiso 1 1 calc R . . C23 C 0.0779(8) 0.6787(10) 0.0802(10) 0.085(4) Uani 1 1 d . . . H23A H 0.0549 0.7302 0.0946 0.102 Uiso 1 1 calc R . . H23B H 0.1199 0.6916 0.0472 0.102 Uiso 1 1 calc R . . C24 C 0.0237(9) 0.6313(12) 0.0143(11) 0.111(6) Uani 1 1 d . . . H24A H 0.0462 0.5806 -0.0017 0.167 Uiso 1 1 calc R . . H24B H 0.0079 0.6622 -0.0446 0.167 Uiso 1 1 calc R . . H24C H -0.0189 0.6196 0.0455 0.167 Uiso 1 1 calc R . . C25 C 0.6243(6) 0.6288(6) -0.3198(7) 0.038(2) Uani 1 1 d . . . C26 C 0.5806(5) 0.6677(6) -0.3936(6) 0.035(2) Uani 1 1 d . . . H26 H 0.5369 0.6956 -0.3862 0.042 Uiso 1 1 calc R . . C27 C 0.6077(6) 0.6619(6) -0.4822(6) 0.039(2) Uani 1 1 d . . . H27 H 0.5834 0.6857 -0.5399 0.046 Uiso 1 1 calc R . . C28 C 0.6706(5) 0.6202(5) -0.4776(6) 0.032(2) Uani 1 1 d . . . C29 C 0.7159(5) 0.6022(6) -0.5491(7) 0.036(2) Uani 1 1 d . . . C30 C 0.7831(5) 0.5678(6) -0.5384(7) 0.041(2) Uani 1 1 d . . . H30 H 0.8080 0.5482 -0.4788 0.049 Uiso 1 1 calc R . . C31 C 0.8126(6) 0.5639(7) -0.6253(7) 0.054(3) Uani 1 1 d . . . H31 H 0.8597 0.5422 -0.6288 0.065 Uiso 1 1 calc R . . C32 C 0.7676(5) 0.5940(6) -0.7032(7) 0.041(2) Uani 1 1 d . . . C33 C 0.7796(5) 0.5994(6) -0.8024(7) 0.036(2) Uani 1 1 d . . . C34 C 0.7882(5) 0.6495(6) -0.9674(7) 0.038(2) Uani 1 1 d . . . C35 C 0.7814(7) 0.6964(7) -1.0578(7) 0.053(3) Uani 1 1 d . . . H35A H 0.8102 0.7461 -1.0465 0.079 Uiso 1 1 calc R . . H35B H 0.7298 0.7099 -1.0796 0.079 Uiso 1 1 calc R . . H35C H 0.7999 0.6642 -1.1070 0.079 Uiso 1 1 calc R . . C36 C 0.8274(5) 0.5809(6) -0.9427(7) 0.038(2) Uani 1 1 d . . . H36 H 0.8548 0.5550 -0.9854 0.046 Uiso 1 1 calc R . . C37 C 0.8244(5) 0.5505(6) -0.8489(7) 0.036(2) Uani 1 1 d . . . C38 C 0.8595(6) 0.4740(6) -0.8114(7) 0.043(3) Uani 1 1 d . . . H38A H 0.8490 0.4320 -0.8615 0.052 Uiso 1 1 calc R . . H38B H 0.8375 0.4565 -0.7553 0.052 Uiso 1 1 calc R . . C39 C 0.9430(6) 0.4810(7) -0.7815(8) 0.048(3) Uani 1 1 d . . . H39A H 0.9657 0.4965 -0.8378 0.058 Uiso 1 1 calc R . . H39B H 0.9541 0.5237 -0.7323 0.058 Uiso 1 1 calc R . . C40 C 0.9757(6) 0.4013(8) -0.7409(10) 0.063(3) Uani 1 1 d . . . H40A H 0.9570 0.3896 -0.6804 0.076 Uiso 1 1 calc R . . H40B H 0.9586 0.3577 -0.7869 0.076 Uiso 1 1 calc R . . C41 C 1.0592(7) 0.4005(9) -0.7211(12) 0.088(5) Uani 1 1 d . . . H41A H 1.0767 0.4457 -0.6776 0.106 Uiso 1 1 calc R . . H41B H 1.0781 0.4090 -0.7821 0.106 Uiso 1 1 calc R . . C42 C 1.0911(8) 0.3204(9) -0.6747(14) 0.104(6) Uani 1 1 d . . . H42A H 1.0707 0.3104 -0.6150 0.125 Uiso 1 1 calc R . . H42B H 1.1451 0.3252 -0.6575 0.125 Uiso 1 1 calc R . . C43 C 1.0723(8) 0.2478(9) -0.7445(13) 0.104(6) Uani 1 1 d . . . H43A H 1.0191 0.2391 -0.7559 0.156 Uiso 1 1 calc R . . H43B H 1.0970 0.1993 -0.7158 0.156 Uiso 1 1 calc R . . H43C H 1.0891 0.2594 -0.8056 0.156 Uiso 1 1 calc R . . O1 O 0.7493(4) 0.3936(4) -0.0165(5) 0.0510(19) Uani 1 1 d . . . S1 S 0.54405(14) 0.67142(15) -0.17891(16) 0.0347(6) Uani 1 1 d . . . S2 S 0.64796(14) 0.49555(15) 0.01970(16) 0.0358(6) Uani 1 1 d . . . S3 S 0.71364(14) 0.49300(15) -0.16154(17) 0.0374(6) Uani 1 1 d . . . S4 S 0.53363(13) 0.59344(16) 0.11609(16) 0.0363(6) Uani 1 1 d . . . S5 S 0.37748(14) 0.67552(15) 0.29780(16) 0.0338(5) Uani 1 1 d . . . S6 S 0.38850(15) 0.58889(16) 0.59054(17) 0.0394(6) Uani 1 1 d . . . S7 S 0.70002(14) 0.58675(16) -0.36066(16) 0.0379(6) Uani 1 1 d . . . S8 S 0.68582(14) 0.62611(16) -0.66908(17) 0.0386(6) Uani 1 1 d . . . S9 S 0.74474(15) 0.68027(16) -0.87267(17) 0.0412(6) Uani 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 C1 0.052(7) 0.043(6) 0.035(5) -0.003(5) 0.017(5) 0.002(5) C2 0.036(5) 0.035(5) 0.026(5) 0.004(4) 0.004(4) -0.007(4) C3 0.031(5) 0.038(5) 0.031(5) -0.006(4) 0.000(4) 0.006(4) C4 0.042(6) 0.032(5) 0.027(5) 0.002(4) 0.002(4) -0.004(4) C5 0.042(6) 0.034(5) 0.028(5) -0.012(4) 0.009(4) 0.003(4) C6 0.036(5) 0.026(5) 0.023(4) -0.002(4) 0.003(4) -0.010(4) C7 0.042(6) 0.032(5) 0.026(4) 0.001(4) 0.008(4) -0.001(4) C8 0.045(6) 0.026(5) 0.032(5) -0.007(4) 0.013(4) 0.002(4) C9 0.038(5) 0.043(6) 0.024(4) -0.006(4) 0.009(4) 0.002(4) C10 0.039(6) 0.041(6) 0.028(5) -0.007(4) 0.014(4) -0.003(4) C11 0.042(6) 0.055(7) 0.033(5) 0.003(5) 0.013(5) 0.015(5) C12 0.048(6) 0.042(6) 0.039(6) 0.009(5) 0.014(5) 0.005(5) C13 0.034(5) 0.040(6) 0.026(5) 0.004(4) 0.000(4) -0.009(4) C14 0.040(6) 0.044(6) 0.028(5) 0.005(4) 0.008(4) -0.010(5) C15 0.055(7) 0.042(6) 0.033(5) -0.006(4) 0.019(5) -0.009(5) C16 0.068(8) 0.046(6) 0.037(6) 0.003(5) 0.028(5) -0.005(6) C17 0.045(6) 0.045(6) 0.038(5) -0.009(5) 0.017(5) -0.004(5) C18 0.031(5) 0.039(6) 0.036(5) -0.002(4) 0.003(4) -0.007(4) C19 0.048(7) 0.055(7) 0.039(6) -0.001(5) 0.019(5) 0.012(5) C20 0.077(9) 0.067(8) 0.037(6) -0.002(6) 0.007(6) 0.012(7) C21 0.061(9) 0.085(10) 0.061(8) -0.004(7) -0.005(7) -0.010(7) C22 0.053(8) 0.086(10) 0.058(8) 0.006(7) 0.011(6) 0.001(7) C23 0.073(10) 0.111(13) 0.072(9) 0.007(9) 0.014(8) 0.000(9) C24 0.101(13) 0.148(17) 0.073(10) -0.015(11) -0.022(10) -0.028(12) C25 0.044(6) 0.040(6) 0.031(5) -0.015(4) 0.009(4) -0.007(5) C26 0.042(6) 0.033(5) 0.031(5) -0.003(4) 0.009(4) 0.002(4) C27 0.048(6) 0.043(6) 0.026(5) -0.003(4) 0.010(4) -0.002(5) C28 0.042(6) 0.033(5) 0.021(4) -0.001(4) 0.005(4) 0.002(4) C29 0.037(5) 0.039(5) 0.035(5) 0.002(4) 0.016(4) -0.004(4) C30 0.033(5) 0.060(7) 0.030(5) 0.004(5) 0.010(4) 0.001(5) C31 0.053(7) 0.073(8) 0.038(6) 0.002(6) 0.012(5) 0.019(6) C32 0.038(6) 0.038(6) 0.049(6) -0.002(5) 0.010(5) 0.000(5) C33 0.037(5) 0.037(5) 0.034(5) 0.002(4) 0.005(4) -0.009(4) C34 0.040(6) 0.040(6) 0.034(5) -0.005(4) 0.007(4) -0.010(5) C35 0.073(8) 0.051(7) 0.038(6) 0.003(5) 0.016(6) -0.005(6) C36 0.032(5) 0.052(6) 0.034(5) 0.006(5) 0.016(4) 0.003(5) C37 0.030(5) 0.045(6) 0.035(5) -0.006(4) 0.011(4) -0.001(4) C38 0.050(7) 0.049(6) 0.033(5) -0.003(5) 0.015(5) 0.007(5) C39 0.042(6) 0.055(7) 0.053(6) 0.004(5) 0.021(5) 0.012(5) C40 0.052(8) 0.062(8) 0.076(9) 0.013(7) 0.012(7) 0.002(6) C41 0.055(9) 0.066(9) 0.133(14) 0.014(9) -0.015(9) 0.013(7) C42 0.048(9) 0.071(10) 0.185(19) 0.002(11) -0.005(10) 0.001(8) C43 0.064(10) 0.073(11) 0.172(18) 0.007(11) 0.012(11) 0.002(9) O1 0.056(5) 0.047(5) 0.050(4) 0.006(4) 0.006(4) 0.015(4) S1 0.0386(14) 0.0415(14) 0.0251(11) 0.0018(10) 0.0080(10) 0.0062(11) S2 0.0404(14) 0.0380(13) 0.0299(12) 0.0046(10) 0.0085(10) 0.0047(11) S3 0.0400(14) 0.0415(14) 0.0309(12) 0.0009(11) 0.0066(10) 0.0064(12) S4 0.0355(13) 0.0480(15) 0.0270(11) 0.0022(11) 0.0096(10) 0.0075(12) S5 0.0401(14) 0.0367(13) 0.0259(11) -0.0003(10) 0.0095(10) 0.0032(11) S6 0.0464(15) 0.0424(14) 0.0311(12) 0.0028(11) 0.0114(11) -0.0020(12) S7 0.0392(14) 0.0472(15) 0.0288(12) 0.0009(11) 0.0105(10) 0.0064(12) S8 0.0401(14) 0.0477(15) 0.0296(12) -0.0002(11) 0.0107(11) 0.0029(12) S9 0.0471(16) 0.0416(15) 0.0360(13) -0.0003(11) 0.0104(12) 0.0019(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.193(12) . ? C1 S2 1.780(10) . ? C1 S3 1.789(10) . ? C2 C4 1.361(13) . ? C2 C3 1.428(12) . ? C2 S2 1.743(9) . ? C3 C5 1.350(13) . ? C3 S3 1.743(9) . ? C4 C6 1.458(13) . ? C4 S1 1.747(9) . ? C5 C25 1.434(12) . ? C5 S1 1.763(9) . ? C6 C7 1.363(13) . ? C6 S4 1.728(9) . ? C7 C8 1.405(12) . ? C8 C9 1.375(13) . ? C9 C10 1.445(12) . ? C9 S4 1.730(9) . ? C10 C11 1.353(13) . ? C10 S5 1.748(9) . ? C11 C12 1.394(13) . ? C12 C13 1.359(13) . ? C13 C14 1.468(13) . ? C13 S5 1.733(9) . ? C14 C18 1.366(13) . ? C14 S6 1.728(9) . ? C15 C17 1.357(14) . ? C15 C16 1.519(13) . ? C15 S6 1.729(10) . ? C17 C18 1.431(13) . ? C18 C19 1.491(13) . ? C19 C20 1.537(15) . ? C20 C21 1.527(16) . ? C21 C22 1.512(17) . ? C22 C23 1.542(17) . ? C23 C24 1.478(19) . ? C25 C26 1.372(13) . ? C25 S7 1.740(10) . ? C26 C27 1.421(12) . ? C27 C28 1.344(13) . ? C28 C29 1.440(12) . ? C28 S7 1.743(9) . ? C29 C30 1.351(13) . ? C29 S8 1.740(10) . ? C30 C31 1.420(13) . ? C31 C32 1.362(14) . ? C32 C33 1.454(13) . ? C32 S8 1.738(10) . ? C33 C37 1.395(13) . ? C33 S9 1.730(10) . ? C34 C36 1.365(14) . ? C34 C35 1.482(13) . ? C34 S9 1.740(10) . ? C36 C37 1.426(12) . ? C37 C38 1.484(14) . ? C38 C39 1.535(14) . ? C39 C40 1.528(15) . ? C40 C41 1.521(16) . ? C41 C42 1.555(19) . ? C42 C43 1.56(2) . ? 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 O1 C1 S2 123.2(8) . . ? O1 C1 S3 122.4(8) . . ? S2 C1 S3 114.4(6) . . ? C4 C2 C3 113.8(8) . . ? C4 C2 S2 129.3(7) . . ? C3 C2 S2 116.8(7) . . ? C5 C3 C2 113.9(8) . . ? C5 C3 S3 129.3(7) . . ? C2 C3 S3 116.8(7) . . ? C2 C4 C6 129.6(8) . . ? C2 C4 S1 110.2(7) . . ? C6 C4 S1 120.2(7) . . ? C3 C5 C25 131.1(9) . . ? C3 C5 S1 110.1(7) . . ? C25 C5 S1 118.6(7) . . ? C7 C6 C4 129.0(8) . . ? C7 C6 S4 110.8(7) . . ? C4 C6 S4 120.2(7) . . ? C6 C7 C8 113.6(8) . . ? C9 C8 C7 112.9(9) . . ? C8 C9 C10 131.0(9) . . ? C8 C9 S4 110.6(7) . . ? C10 C9 S4 118.3(7) . . ? C11 C10 C9 129.4(9) . . ? C11 C10 S5 109.9(7) . . ? C9 C10 S5 120.4(7) . . ? C10 C11 C12 114.2(9) . . ? C13 C12 C11 113.9(9) . . ? C12 C13 C14 126.0(9) . . ? C12 C13 S5 110.2(7) . . ? C14 C13 S5 123.6(7) . . ? C18 C14 C13 131.7(9) . . ? C18 C14 S6 110.9(7) . . ? C13 C14 S6 117.5(7) . . ? C17 C15 C16 130.0(10) . . ? C17 C15 S6 110.6(7) . . ? C16 C15 S6 119.4(8) . . ? C15 C17 C18 113.5(9) . . ? C14 C18 C17 112.5(9) . . ? C14 C18 C19 125.7(9) . . ? C17 C18 C19 121.8(9) . . ? C18 C19 C20 113.2(9) . . ? C21 C20 C19 111.6(10) . . ? C22 C21 C20 114.2(11) . . ? C21 C22 C23 112.2(12) . . ? C24 C23 C22 114.0(14) . . ? C26 C25 C5 129.7(9) . . ? C26 C25 S7 110.1(7) . . ? C5 C25 S7 120.1(8) . . ? C25 C26 C27 112.8(9) . . ? C28 C27 C26 114.5(9) . . ? C27 C28 C29 131.7(8) . . ? C27 C28 S7 110.2(7) . . ? C29 C28 S7 118.0(7) . . ? C30 C29 C28 129.3(9) . . ? C30 C29 S8 110.4(7) . . ? C28 C29 S8 120.2(7) . . ? C29 C30 C31 113.2(9) . . ? C32 C31 C30 114.3(10) . . ? C31 C32 C33 129.2(9) . . ? C31 C32 S8 109.4(8) . . ? C33 C32 S8 121.4(8) . . ? C37 C33 C32 127.5(9) . . ? C37 C33 S9 112.2(7) . . ? C32 C33 S9 119.9(8) . . ? C36 C34 C35 128.7(9) . . ? C36 C34 S9 109.9(7) . . ? C35 C34 S9 121.4(8) . . ? C34 C36 C37 115.8(9) . . ? C33 C37 C36 110.1(9) . . ? C33 C37 C38 126.1(9) . . ? C36 C37 C38 123.7(8) . . ? C37 C38 C39 113.2(9) . . ? C40 C39 C38 110.9(9) . . ? C41 C40 C39 113.9(10) . . ? C40 C41 C42 112.9(12) . . ? C41 C42 C43 111.4(14) . . ? C4 S1 C5 92.0(5) . . ? C2 S2 C1 96.1(5) . . ? C3 S3 C1 95.9(5) . . ? C6 S4 C9 92.0(4) . . ? C13 S5 C10 91.8(5) . . ? C14 S6 C15 92.5(5) . . ? C25 S7 C28 92.3(5) . . ? C32 S8 C29 92.5(5) . . ? C33 S9 C34 92.1(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.635 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.131 data_2010src0100 _database_code_depnum_ccdc_archive 'CCDC 783816' #TrackingRef '2010src0100.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H84 S20' _chemical_formula_weight 1770.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.7929(2) _cell_length_b 12.7339(3) _cell_length_c 15.5721(4) _cell_angle_alpha 82.8950(10) _cell_angle_beta 74.031(2) _cell_angle_gamma 66.263(2) _cell_volume 2057.80(8) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 28031 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description slab _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8948 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 37249 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9158 _reflns_number_gt 7216 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'Sheldrick, G.M. (2008). Acta Cryst. A64, 112-1' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0753P)^2^+3.0224P] 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 9158 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C44 C -0.5000 2.0000 1.0000 0.096(3) Uiso 1 2 d S . . S10 S -0.38431(11) 1.88945(11) 0.98800(8) 0.0587(3) Uiso 1 1 d . . . C1 C 0.5488(3) 0.8033(2) 0.32177(19) 0.0245(6) Uani 1 1 d . . . C2 C 0.5479(3) 0.7036(2) 0.36691(18) 0.0219(6) Uani 1 1 d . . . C3 C 0.6252(3) 0.6028(2) 0.31483(18) 0.0207(6) Uani 1 1 d . . . C4 C 0.6831(3) 0.6255(2) 0.22930(18) 0.0213(6) Uani 1 1 d . . . C5 C 0.5197(3) 0.5324(2) 0.46691(18) 0.0213(6) Uani 1 1 d . . . C6 C 0.4884(3) 0.9208(2) 0.35036(19) 0.0256(6) Uani 1 1 d . . . C7 C 0.5023(3) 1.0158(3) 0.3052(2) 0.0327(7) Uani 1 1 d . . . H7 H 0.5564 1.0132 0.2470 0.039 Uiso 1 1 calc R . . C8 C 0.4283(3) 1.1181(3) 0.3536(2) 0.0330(7) Uani 1 1 d . . . H8 H 0.4265 1.1914 0.3308 0.040 Uiso 1 1 calc R . . C9 C 0.3594(3) 1.1013(2) 0.4368(2) 0.0264(6) Uani 1 1 d . . . C10 C 0.2768(3) 1.1812(2) 0.5080(2) 0.0249(6) Uani 1 1 d . . . C11 C 0.2274(3) 1.1566(3) 0.5946(2) 0.0295(7) Uani 1 1 d . . . H11 H 0.2436 1.0806 0.6173 0.035 Uiso 1 1 calc R . . C12 C 0.1505(3) 1.2546(3) 0.6467(2) 0.0289(7) Uani 1 1 d . . . H12 H 0.1094 1.2514 0.7081 0.035 Uiso 1 1 calc R . . C13 C 0.1404(3) 1.3553(2) 0.60017(19) 0.0234(6) Uani 1 1 d . . . C14 C 0.0637(3) 1.4701(2) 0.63488(19) 0.0230(6) Uani 1 1 d . . . C15 C 0.0504(3) 1.5760(2) 0.5962(2) 0.0249(6) Uani 1 1 d . . . C16 C -0.0419(3) 1.6666(3) 0.6548(2) 0.0289(7) Uani 1 1 d . . . H16 H -0.0628 1.7455 0.6389 0.035 Uiso 1 1 calc R . . C17 C -0.0973(3) 1.6307(3) 0.7348(2) 0.0288(7) Uani 1 1 d . . . C18 C -0.1942(3) 1.7003(3) 0.8123(2) 0.0360(8) Uani 1 1 d . . . H18A H -0.2151 1.6489 0.8605 0.054 Uiso 1 1 calc R . . H18B H -0.2717 1.7503 0.7935 0.054 Uiso 1 1 calc R . . H18C H -0.1592 1.7472 0.8336 0.054 Uiso 1 1 calc R . . C19 C 0.1208(3) 1.5943(3) 0.5028(2) 0.0281(6) Uani 1 1 d . . . H19A H 0.0943 1.5626 0.4602 0.034 Uiso 1 1 calc R . . H19B H 0.2135 1.5502 0.4964 0.034 Uiso 1 1 calc R . . C20 C 0.0991(3) 1.7187(3) 0.4770(2) 0.0318(7) Uani 1 1 d . . . H20A H 0.1254 1.7512 0.5191 0.038 Uiso 1 1 calc R . . H20B H 0.0068 1.7633 0.4820 0.038 Uiso 1 1 calc R . . C21 C 0.1739(3) 1.7310(3) 0.3820(2) 0.0308(7) Uani 1 1 d . . . H21A H 0.2655 1.6820 0.3759 0.037 Uiso 1 1 calc R . . H21B H 0.1434 1.7034 0.3396 0.037 Uiso 1 1 calc R . . C22 C 0.1602(4) 1.8542(3) 0.3577(2) 0.0360(8) Uani 1 1 d . . . H22A H 0.0686 1.9023 0.3629 0.043 Uiso 1 1 calc R . . H22B H 0.1880 1.8821 0.4017 0.043 Uiso 1 1 calc R . . C23 C 0.2358(4) 1.8701(3) 0.2647(2) 0.0413(8) Uani 1 1 d . . . H23A H 0.2063 1.8451 0.2202 0.050 Uiso 1 1 calc R . . H23B H 0.3274 1.8210 0.2586 0.050 Uiso 1 1 calc R . . C24 C 0.2214(4) 1.9943(4) 0.2451(3) 0.0535(11) Uani 1 1 d . . . H24A H 0.2718 2.0008 0.1846 0.080 Uiso 1 1 calc R . . H24B H 0.2519 2.0191 0.2884 0.080 Uiso 1 1 calc R . . H24C H 0.1311 2.0430 0.2497 0.080 Uiso 1 1 calc R . . C25 C 0.7626(3) 0.5488(2) 0.15578(19) 0.0227(6) Uani 1 1 d . . . C26 C 0.7909(3) 0.5755(3) 0.0666(2) 0.0309(7) Uani 1 1 d . . . H26 H 0.7600 0.6514 0.0432 0.037 Uiso 1 1 calc R . . C27 C 0.8707(3) 0.4786(3) 0.0131(2) 0.0308(7) Uani 1 1 d . . . H27 H 0.8986 0.4829 -0.0501 0.037 Uiso 1 1 calc R . . C28 C 0.9040(3) 0.3780(2) 0.06100(18) 0.0226(6) Uani 1 1 d . . . C29 C 0.9847(3) 0.2624(2) 0.03078(19) 0.0233(6) Uani 1 1 d . . . C30 C 1.0290(3) 0.1659(3) 0.0807(2) 0.0274(6) Uani 1 1 d . . . H30 H 1.0140 0.1665 0.1438 0.033 Uiso 1 1 calc R . . C31 C 1.0989(3) 0.0650(3) 0.0303(2) 0.0279(6) Uani 1 1 d . . . H31 H 1.1349 -0.0087 0.0562 0.034 Uiso 1 1 calc R . . C32 C 1.1098(3) 0.0835(2) -0.0592(2) 0.0260(6) Uani 1 1 d . . . C33 C 1.1642(3) 0.0004(3) -0.1309(2) 0.0296(7) Uani 1 1 d . . . C34 C 1.2639(3) -0.1048(3) -0.1393(2) 0.0339(7) Uani 1 1 d . . . C35 C 1.2766(3) -0.1611(3) -0.2176(2) 0.0391(9) Uani 1 1 d . . . H35 H 1.3412 -0.2347 -0.2342 0.047 Uiso 1 1 calc R . . C36 C 1.1912(4) -0.1031(3) -0.2660(2) 0.0369(8) Uani 1 1 d . . . C37 C 1.1751(4) -0.1399(3) -0.3478(2) 0.0465(10) Uani 1 1 d . . . H37A H 1.1042 -0.0787 -0.3676 0.070 Uiso 1 1 calc R . . H37B H 1.1565 -0.2095 -0.3341 0.070 Uiso 1 1 calc R . . H37C H 1.2540 -0.1559 -0.3953 0.070 Uiso 1 1 calc R . . C38 C 1.3483(3) -0.1575(3) -0.0769(3) 0.0399(8) Uani 1 1 d . . . H38A H 1.3405 -0.0969 -0.0388 0.048 Uiso 1 1 calc R . . H38B H 1.4383 -0.1909 -0.1119 0.048 Uiso 1 1 calc R . . C39 C 1.3150(3) -0.2514(3) -0.0169(3) 0.0420(9) Uani 1 1 d . . . H39A H 1.2257 -0.2169 0.0191 0.050 Uiso 1 1 calc R . . H39B H 1.3196 -0.3100 -0.0554 0.050 Uiso 1 1 calc R . . C40 C 1.4016(3) -0.3104(3) 0.0461(3) 0.0414(9) Uani 1 1 d . . . H40A H 1.4908 -0.3472 0.0104 0.050 Uiso 1 1 calc R . . H40B H 1.3989 -0.2519 0.0839 0.050 Uiso 1 1 calc R . . C41 C 1.3634(4) -0.4004(3) 0.1058(3) 0.0452(9) Uani 1 1 d . . . H41A H 1.3683 -0.4595 0.0677 0.054 Uiso 1 1 calc R . . H41B H 1.2732 -0.3636 0.1397 0.054 Uiso 1 1 calc R . . C42 C 1.4450(4) -0.4589(3) 0.1715(3) 0.0507(10) Uani 1 1 d . . . H42A H 1.5351 -0.4964 0.1378 0.061 Uiso 1 1 calc R . . H42B H 1.4404 -0.3999 0.2097 0.061 Uiso 1 1 calc R . . C43 C 1.4050(4) -0.5476(4) 0.2307(3) 0.0564(11) Uani 1 1 d . . . H43A H 1.4615 -0.5821 0.2712 0.085 Uiso 1 1 calc R . . H43B H 1.4111 -0.6073 0.1936 0.085 Uiso 1 1 calc R . . H43C H 1.3166 -0.5109 0.2657 0.085 Uiso 1 1 calc R . . S1 S 0.64512(7) 0.77206(6) 0.21418(5) 0.02679(18) Uani 1 1 d . . . S2 S 0.46619(7) 0.68264(6) 0.47522(5) 0.02406(17) Uani 1 1 d . . . S3 S 0.63064(7) 0.47189(6) 0.36635(5) 0.02430(17) Uani 1 1 d . . . S4 S 0.38404(7) 0.95787(6) 0.45464(5) 0.02568(17) Uani 1 1 d . . . S5 S 0.22758(7) 1.32780(6) 0.49019(5) 0.02517(17) Uani 1 1 d . . . S6 S -0.03725(7) 1.48305(6) 0.74134(5) 0.02721(18) Uani 1 1 d . . . S7 S 0.83533(7) 0.40291(6) 0.17366(5) 0.02512(17) Uani 1 1 d . . . S8 S 1.03397(7) 0.22897(6) -0.08147(5) 0.02738(18) Uani 1 1 d . . . S9 S 1.08891(9) 0.02682(7) -0.21688(5) 0.0339(2) Uani 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 C1 0.0258(15) 0.0220(14) 0.0205(14) -0.0033(11) 0.0012(11) -0.0076(12) C2 0.0216(14) 0.0222(14) 0.0185(13) -0.0022(11) -0.0004(10) -0.0076(11) C3 0.0252(15) 0.0174(13) 0.0186(13) -0.0017(10) -0.0033(11) -0.0084(11) C4 0.0232(15) 0.0179(13) 0.0192(13) -0.0043(10) 0.0000(11) -0.0065(11) C5 0.0230(14) 0.0194(13) 0.0177(13) -0.0053(10) 0.0006(10) -0.0066(11) C6 0.0277(16) 0.0198(14) 0.0219(14) -0.0045(11) 0.0018(11) -0.0057(12) C7 0.0400(19) 0.0234(15) 0.0244(16) -0.0016(12) 0.0068(13) -0.0110(14) C8 0.0404(19) 0.0209(15) 0.0294(16) -0.0015(12) 0.0024(13) -0.0103(13) C9 0.0280(16) 0.0195(14) 0.0256(15) -0.0038(11) -0.0024(12) -0.0048(12) C10 0.0272(16) 0.0172(13) 0.0264(15) -0.0039(11) -0.0032(12) -0.0059(11) C11 0.0372(18) 0.0180(14) 0.0280(16) -0.0020(12) -0.0031(13) -0.0080(12) C12 0.0340(17) 0.0247(15) 0.0223(15) -0.0022(12) -0.0008(12) -0.0090(13) C13 0.0275(15) 0.0216(14) 0.0196(14) -0.0026(11) -0.0049(11) -0.0081(12) C14 0.0242(15) 0.0207(14) 0.0237(14) -0.0044(11) -0.0056(11) -0.0074(11) C15 0.0302(16) 0.0199(14) 0.0248(15) -0.0012(11) -0.0105(12) -0.0072(12) C16 0.0369(18) 0.0192(14) 0.0320(16) -0.0020(12) -0.0135(13) -0.0086(13) C17 0.0324(17) 0.0230(15) 0.0298(16) -0.0084(12) -0.0077(13) -0.0072(13) C18 0.0406(19) 0.0247(16) 0.0389(19) -0.0112(14) -0.0059(15) -0.0082(14) C19 0.0351(17) 0.0228(15) 0.0261(15) -0.0017(12) -0.0087(13) -0.0098(13) C20 0.0425(19) 0.0272(16) 0.0276(16) 0.0007(12) -0.0114(14) -0.0140(14) C21 0.0406(18) 0.0253(16) 0.0294(16) 0.0014(12) -0.0101(13) -0.0151(14) C22 0.050(2) 0.0279(17) 0.0345(18) 0.0048(14) -0.0153(15) -0.0175(15) C23 0.051(2) 0.040(2) 0.0368(19) 0.0090(15) -0.0138(16) -0.0230(17) C24 0.067(3) 0.051(2) 0.057(3) 0.027(2) -0.029(2) -0.036(2) C25 0.0237(15) 0.0188(13) 0.0222(14) -0.0044(11) -0.0007(11) -0.0068(11) C26 0.0401(18) 0.0211(15) 0.0216(15) -0.0014(11) 0.0010(13) -0.0072(13) C27 0.0400(18) 0.0256(15) 0.0186(14) -0.0044(12) 0.0006(12) -0.0084(13) C28 0.0262(15) 0.0231(14) 0.0176(13) -0.0067(11) -0.0013(11) -0.0093(12) C29 0.0249(15) 0.0252(15) 0.0189(14) -0.0078(11) 0.0014(11) -0.0110(12) C30 0.0319(17) 0.0251(15) 0.0236(15) -0.0062(12) -0.0021(12) -0.0110(13) C31 0.0303(16) 0.0209(14) 0.0291(16) -0.0027(12) -0.0028(12) -0.0087(12) C32 0.0256(16) 0.0200(14) 0.0281(15) -0.0083(12) 0.0040(12) -0.0091(12) C33 0.0326(17) 0.0236(15) 0.0301(16) -0.0110(12) 0.0086(12) -0.0160(13) C34 0.0281(17) 0.0271(16) 0.0431(19) -0.0126(14) 0.0069(14) -0.0140(13) C35 0.0369(19) 0.0316(17) 0.042(2) -0.0219(15) 0.0180(15) -0.0189(15) C36 0.047(2) 0.0298(17) 0.0280(17) -0.0117(13) 0.0125(15) -0.0199(15) C37 0.066(3) 0.038(2) 0.0307(18) -0.0180(15) 0.0098(17) -0.0238(18) C38 0.0262(18) 0.0305(17) 0.060(2) -0.0177(16) 0.0014(15) -0.0108(14) C39 0.0321(19) 0.0342(19) 0.059(2) -0.0165(17) -0.0064(16) -0.0111(15) C40 0.0309(19) 0.039(2) 0.055(2) -0.0164(17) -0.0078(16) -0.0114(15) C41 0.037(2) 0.0357(19) 0.066(3) -0.0150(18) -0.0193(18) -0.0088(16) C42 0.042(2) 0.040(2) 0.073(3) -0.016(2) -0.023(2) -0.0078(17) C43 0.052(3) 0.040(2) 0.081(3) -0.004(2) -0.036(2) -0.0085(19) S1 0.0340(4) 0.0194(3) 0.0195(4) -0.0025(3) 0.0039(3) -0.0089(3) S2 0.0295(4) 0.0177(3) 0.0183(3) -0.0039(3) 0.0033(3) -0.0073(3) S3 0.0303(4) 0.0176(3) 0.0185(3) -0.0039(3) 0.0029(3) -0.0076(3) S4 0.0322(4) 0.0170(3) 0.0211(4) -0.0031(3) 0.0026(3) -0.0079(3) S5 0.0309(4) 0.0174(3) 0.0224(4) -0.0023(3) -0.0025(3) -0.0066(3) S6 0.0323(4) 0.0209(4) 0.0247(4) -0.0060(3) -0.0010(3) -0.0089(3) S7 0.0313(4) 0.0208(3) 0.0178(3) -0.0052(3) 0.0005(3) -0.0074(3) S8 0.0340(4) 0.0218(4) 0.0209(4) -0.0073(3) 0.0035(3) -0.0100(3) S9 0.0505(5) 0.0242(4) 0.0219(4) -0.0082(3) 0.0052(3) -0.0162(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C44 S10 1.5022(12) . ? C44 S10 1.5022(12) 2_497 ? C1 C2 1.376(4) . ? C1 C6 1.441(4) . ? C1 S1 1.735(3) . ? C2 C3 1.430(4) . ? C2 S2 1.745(3) . ? C3 C4 1.374(4) . ? C3 S3 1.743(3) . ? C4 C25 1.447(4) . ? C4 S1 1.736(3) . ? C5 C5 1.339(6) 2_666 ? C5 S3 1.765(3) . ? C5 S2 1.767(3) . ? C6 C7 1.367(4) . ? C6 S4 1.731(3) . ? C7 C8 1.412(4) . ? C8 C9 1.371(4) . ? C9 C10 1.449(4) . ? C9 S4 1.729(3) . ? C10 C11 1.366(4) . ? C10 S5 1.728(3) . ? C11 C12 1.404(4) . ? C12 C13 1.370(4) . ? C13 C14 1.453(4) . ? C13 S5 1.733(3) . ? C14 C15 1.373(4) . ? C14 S6 1.737(3) . ? C15 C16 1.433(4) . ? C15 C19 1.505(4) . ? C16 C17 1.357(5) . ? C17 C18 1.495(4) . ? C17 S6 1.723(3) . ? C19 C20 1.520(4) . ? C20 C21 1.524(4) . ? C21 C22 1.520(4) . ? C22 C23 1.517(5) . ? C23 C24 1.521(5) . ? C25 C26 1.369(4) . ? C25 S7 1.728(3) . ? C26 C27 1.410(4) . ? C27 C28 1.369(4) . ? C28 C29 1.447(4) . ? C28 S7 1.727(3) . ? C29 C30 1.363(4) . ? C29 S8 1.732(3) . ? C30 C31 1.409(4) . ? C31 C32 1.364(4) . ? C32 C33 1.460(4) . ? C32 S8 1.740(3) . ? C33 C34 1.374(4) . ? C33 S9 1.731(4) . ? C34 C35 1.432(5) . ? C34 C38 1.490(5) . ? C35 C36 1.344(6) . ? C36 C37 1.494(5) . ? C36 S9 1.725(3) . ? C38 C39 1.535(5) . ? C39 C40 1.524(5) . ? C40 C41 1.518(6) . ? C41 C42 1.519(5) . ? C42 C43 1.509(6) . ? 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 S10 C44 S10 180.000(2) . 2_497 ? C2 C1 C6 131.0(3) . . ? C2 C1 S1 109.8(2) . . ? C6 C1 S1 119.1(2) . . ? C1 C2 C3 113.5(2) . . ? C1 C2 S2 130.2(2) . . ? C3 C2 S2 116.3(2) . . ? C4 C3 C2 113.4(2) . . ? C4 C3 S3 129.6(2) . . ? C2 C3 S3 117.0(2) . . ? C3 C4 C25 130.3(3) . . ? C3 C4 S1 109.9(2) . . ? C25 C4 S1 119.8(2) . . ? C5 C5 S3 121.8(3) 2_666 . ? C5 C5 S2 122.3(3) 2_666 . ? S3 C5 S2 115.91(16) . . ? C7 C6 C1 128.5(3) . . ? C7 C6 S4 110.5(2) . . ? C1 C6 S4 121.0(2) . . ? C6 C7 C8 113.4(3) . . ? C9 C8 C7 113.3(3) . . ? C8 C9 C10 130.8(3) . . ? C8 C9 S4 110.5(2) . . ? C10 C9 S4 118.7(2) . . ? C11 C10 C9 127.9(3) . . ? C11 C10 S5 110.7(2) . . ? C9 C10 S5 121.5(2) . . ? C10 C11 C12 113.5(3) . . ? C13 C12 C11 113.4(3) . . ? C12 C13 C14 126.1(3) . . ? C12 C13 S5 110.4(2) . . ? C14 C13 S5 123.5(2) . . ? C15 C14 C13 131.1(3) . . ? C15 C14 S6 111.1(2) . . ? C13 C14 S6 117.7(2) . . ? C14 C15 C16 111.5(3) . . ? C14 C15 C19 124.2(3) . . ? C16 C15 C19 124.3(3) . . ? C17 C16 C15 114.5(3) . . ? C16 C17 C18 129.2(3) . . ? C16 C17 S6 110.5(2) . . ? C18 C17 S6 120.3(2) . . ? C15 C19 C20 114.9(3) . . ? C19 C20 C21 112.1(3) . . ? C22 C21 C20 112.5(3) . . ? C23 C22 C21 114.4(3) . . ? C22 C23 C24 112.1(3) . . ? C26 C25 C4 128.2(3) . . ? C26 C25 S7 110.6(2) . . ? C4 C25 S7 121.2(2) . . ? C25 C26 C27 113.1(3) . . ? C28 C27 C26 113.4(3) . . ? C27 C28 C29 129.9(3) . . ? C27 C28 S7 110.5(2) . . ? C29 C28 S7 119.6(2) . . ? C30 C29 C28 128.5(3) . . ? C30 C29 S8 110.1(2) . . ? C28 C29 S8 121.4(2) . . ? C29 C30 C31 114.1(3) . . ? C32 C31 C30 113.3(3) . . ? C31 C32 C33 129.3(3) . . ? C31 C32 S8 110.2(2) . . ? C33 C32 S8 120.3(2) . . ? C34 C33 C32 130.0(3) . . ? C34 C33 S9 111.3(2) . . ? C32 C33 S9 118.4(2) . . ? C33 C34 C35 110.5(3) . . ? C33 C34 C38 126.4(3) . . ? C35 C34 C38 123.0(3) . . ? C36 C35 C34 115.7(3) . . ? C35 C36 C37 128.8(3) . . ? C35 C36 S9 109.8(3) . . ? C37 C36 S9 121.4(3) . . ? C34 C38 C39 112.5(3) . . ? C40 C39 C38 114.4(3) . . ? C41 C40 C39 112.7(3) . . ? C40 C41 C42 114.4(3) . . ? C43 C42 C41 113.6(3) . . ? C1 S1 C4 93.32(13) . . ? C2 S2 C5 95.42(13) . . ? C3 S3 C5 95.20(13) . . ? C9 S4 C6 92.36(14) . . ? C10 S5 C13 92.09(14) . . ? C17 S6 C14 92.48(15) . . ? C28 S7 C25 92.31(14) . . ? C29 S8 C32 92.32(14) . . ? C36 S9 C33 92.59(17) . . ? 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 C6 C1 C2 C3 -177.7(3) . . . . ? S1 C1 C2 C3 0.3(3) . . . . ? C6 C1 C2 S2 3.5(5) . . . . ? S1 C1 C2 S2 -178.55(19) . . . . ? C1 C2 C3 C4 -1.3(4) . . . . ? S2 C2 C3 C4 177.8(2) . . . . ? C1 C2 C3 S3 179.8(2) . . . . ? S2 C2 C3 S3 -1.1(3) . . . . ? C2 C3 C4 C25 -176.8(3) . . . . ? S3 C3 C4 C25 2.0(5) . . . . ? C2 C3 C4 S1 1.6(3) . . . . ? S3 C3 C4 S1 -179.66(19) . . . . ? C2 C1 C6 C7 173.2(3) . . . . ? S1 C1 C6 C7 -4.7(5) . . . . ? C2 C1 C6 S4 -5.9(5) . . . . ? S1 C1 C6 S4 176.22(17) . . . . ? C1 C6 C7 C8 -179.9(3) . . . . ? S4 C6 C7 C8 -0.7(4) . . . . ? C6 C7 C8 C9 1.2(5) . . . . ? C7 C8 C9 C10 177.2(3) . . . . ? C7 C8 C9 S4 -1.1(4) . . . . ? C8 C9 C10 C11 -168.2(4) . . . . ? S4 C9 C10 C11 10.0(5) . . . . ? C8 C9 C10 S5 11.9(5) . . . . ? S4 C9 C10 S5 -169.92(17) . . . . ? C9 C10 C11 C12 -180.0(3) . . . . ? S5 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? C11 C12 C13 C14 177.4(3) . . . . ? C11 C12 C13 S5 0.1(4) . . . . ? C12 C13 C14 C15 176.9(3) . . . . ? S5 C13 C14 C15 -6.1(5) . . . . ? C12 C13 C14 S6 -6.8(4) . . . . ? S5 C13 C14 S6 170.20(17) . . . . ? C13 C14 C15 C16 176.9(3) . . . . ? S6 C14 C15 C16 0.4(3) . . . . ? C13 C14 C15 C19 -1.1(5) . . . . ? S6 C14 C15 C19 -177.6(2) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C19 C15 C16 C17 177.7(3) . . . . ? C15 C16 C17 C18 178.4(3) . . . . ? C15 C16 C17 S6 0.1(4) . . . . ? C14 C15 C19 C20 -175.2(3) . . . . ? C16 C15 C19 C20 7.0(4) . . . . ? C15 C19 C20 C21 179.5(3) . . . . ? C19 C20 C21 C22 -176.1(3) . . . . ? C20 C21 C22 C23 178.4(3) . . . . ? C21 C22 C23 C24 -178.4(3) . . . . ? C3 C4 C25 C26 161.1(3) . . . . ? S1 C4 C25 C26 -17.1(5) . . . . ? C3 C4 C25 S7 -18.2(5) . . . . ? S1 C4 C25 S7 163.60(17) . . . . ? C4 C25 C26 C27 -179.3(3) . . . . ? S7 C25 C26 C27 0.1(4) . . . . ? C25 C26 C27 C28 -0.3(4) . . . . ? C26 C27 C28 C29 -179.1(3) . . . . ? C26 C27 C28 S7 0.3(4) . . . . ? C27 C28 C29 C30 171.1(3) . . . . ? S7 C28 C29 C30 -8.3(4) . . . . ? C27 C28 C29 S8 -11.6(5) . . . . ? S7 C28 C29 S8 169.07(16) . . . . ? C28 C29 C30 C31 175.9(3) . . . . ? S8 C29 C30 C31 -1.6(4) . . . . ? C29 C30 C31 C32 0.5(4) . . . . ? C30 C31 C32 C33 -173.8(3) . . . . ? C30 C31 C32 S8 0.9(4) . . . . ? C31 C32 C33 C34 -33.0(5) . . . . ? S8 C32 C33 C34 152.9(3) . . . . ? C31 C32 C33 S9 141.0(3) . . . . ? S8 C32 C33 S9 -33.1(3) . . . . ? C32 C33 C34 C35 174.9(3) . . . . ? S9 C33 C34 C35 0.5(3) . . . . ? C32 C33 C34 C38 -4.2(5) . . . . ? S9 C33 C34 C38 -178.6(3) . . . . ? C33 C34 C35 C36 -0.5(4) . . . . ? C38 C34 C35 C36 178.6(3) . . . . ? C34 C35 C36 C37 -176.9(3) . . . . ? C34 C35 C36 S9 0.2(4) . . . . ? C33 C34 C38 C39 103.5(4) . . . . ? C35 C34 C38 C39 -75.5(4) . . . . ? C34 C38 C39 C40 178.1(3) . . . . ? C38 C39 C40 C41 178.5(3) . . . . ? C39 C40 C41 C42 -178.3(3) . . . . ? C40 C41 C42 C43 179.7(3) . . . . ? C2 C1 S1 C4 0.5(2) . . . . ? C6 C1 S1 C4 178.8(3) . . . . ? C3 C4 S1 C1 -1.2(2) . . . . ? C25 C4 S1 C1 177.4(2) . . . . ? C1 C2 S2 C5 177.1(3) . . . . ? C3 C2 S2 C5 -1.8(3) . . . . ? C5 C5 S2 C2 -176.8(4) 2_666 . . . ? S3 C5 S2 C2 4.08(19) . . . . ? C4 C3 S3 C5 -175.3(3) . . . . ? C2 C3 S3 C5 3.4(2) . . . . ? C5 C5 S3 C3 176.3(4) 2_666 . . . ? S2 C5 S3 C3 -4.56(19) . . . . ? C8 C9 S4 C6 0.6(3) . . . . ? C10 C9 S4 C6 -178.0(3) . . . . ? C7 C6 S4 C9 0.1(3) . . . . ? C1 C6 S4 C9 179.3(3) . . . . ? C11 C10 S5 C13 0.1(3) . . . . ? C9 C10 S5 C13 180.0(3) . . . . ? C12 C13 S5 C10 -0.1(3) . . . . ? C14 C13 S5 C10 -177.5(3) . . . . ? C16 C17 S6 C14 0.1(3) . . . . ? C18 C17 S6 C14 -178.4(3) . . . . ? C15 C14 S6 C17 -0.3(2) . . . . ? C13 C14 S6 C17 -177.3(2) . . . . ? C27 C28 S7 C25 -0.2(3) . . . . ? C29 C28 S7 C25 179.2(2) . . . . ? C26 C25 S7 C28 0.1(3) . . . . ? C4 C25 S7 C28 179.5(3) . . . . ? C30 C29 S8 C32 1.8(2) . . . . ? C28 C29 S8 C32 -176.0(3) . . . . ? C31 C32 S8 C29 -1.5(2) . . . . ? C33 C32 S8 C29 173.7(3) . . . . ? C35 C36 S9 C33 0.1(3) . . . . ? C37 C36 S9 C33 177.5(3) . . . . ? C34 C33 S9 C36 -0.4(3) . . . . ? C32 C33 S9 C36 -175.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.370 _refine_diff_density_min -1.559 _refine_diff_density_rms 0.089