# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Lin, Li' 'Zhang, Jiaxin' 'Wu, Xiangxiang' 'Liang, Guoxin' 'He, Lan' 'Gong, Bing' _publ_contact_author_name 'Gong, Bing' _publ_contact_author_email bgong@buffalo.edu _publ_section_title ; Double-decked Molecular Crescents ; # Attachment '2a.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 784328' #TrackingRef '2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H60 O16 S4' _chemical_formula_weight 1261.40 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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.300(3) _cell_length_b 24.855(5) _cell_length_c 15.010(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6081(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10154 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8404 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku raxis Rapid IP Area Detector' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10154 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.1263 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5370 _reflns_number_gt 2686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto(Rigaku 2001)' _computing_cell_refinement 'Rapid Auto(Rigaku 2001)' _computing_data_reduction 'Rapid Auto(Rigaku 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0623P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5370 _refine_ls_number_parameters 488 _refine_ls_number_restraints 621 _refine_ls_R_factor_all 0.1778 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.07061(10) 0.18840(7) 0.34517(10) 0.0682(5) Uani 1 1 d D . . S2 S -1.00836(9) 0.25400(6) 1.10955(10) 0.0585(5) Uani 1 1 d D . . O1 O -0.8586(3) 0.1100(2) 1.0611(3) 0.0456(15) Uani 0.727(5) 1 d PDU A 1 O2 O -0.7882(3) 0.18678(18) 1.0406(3) 0.0377(12) Uani 0.727(5) 1 d PDU A 1 C10 C -0.5906(6) 0.1021(2) 0.9348(9) 0.0333(18) Uani 0.727(5) 1 d PDU A 1 H10 H -0.5408 0.1202 0.9212 0.040 Uiso 0.727(5) 1 calc PR A 1 C11 C -0.6561(5) 0.1307(3) 0.9693(6) 0.0312(16) Uani 0.727(5) 1 d PDU A 1 H11 H -0.6517 0.1684 0.9778 0.037 Uiso 0.727(5) 1 calc PR A 1 C12 C -0.7282(4) 0.1042(3) 0.9914(5) 0.0298(15) Uani 0.727(5) 1 d PDU A 1 C13 C -0.7355(5) 0.0496(3) 0.9768(7) 0.0346(17) Uani 0.727(5) 1 d PDU A 1 H13 H -0.7856 0.0318 0.9901 0.041 Uiso 0.727(5) 1 calc PR A 1 C14 C -0.6708(4) 0.0212(3) 0.9432(10) 0.0357(19) Uani 0.727(5) 1 d PDU A 1 H14 H -0.6758 -0.0166 0.9356 0.043 Uiso 0.727(5) 1 calc PR A 1 C15 C -0.7994(4) 0.1330(2) 1.0336(5) 0.0350(16) Uani 0.727(5) 1 d PDU A 1 C16 C -0.8511(4) 0.2147(3) 1.0924(4) 0.0434(17) Uani 0.727(5) 1 d PDU A 1 H16A H -0.8280 0.2486 1.1161 0.052 Uiso 0.727(5) 1 calc PR A 1 H16B H -0.8671 0.1920 1.1437 0.052 Uiso 0.727(5) 1 calc PR A 1 C34 C -0.9260(4) 0.2272(3) 1.0380(5) 0.042(2) Uani 0.727(5) 1 d PDU A 1 H34A H -0.9454 0.1941 1.0079 0.050 Uiso 0.727(5) 1 calc PR A 1 H34B H -0.9120 0.2540 0.9916 0.050 Uiso 0.727(5) 1 calc PR A 1 O1' O -0.7467(8) 0.2113(5) 1.0275(10) 0.054(4) Uani 0.273(5) 1 d PDU A 2 O2' O -0.8324(7) 0.1430(5) 1.0576(10) 0.041(2) Uani 0.273(5) 1 d PDU A 2 C10' C -0.6786(9) 0.0319(7) 0.938(3) 0.034(3) Uani 0.273(5) 1 d PDU A 2 H10' H -0.6972 -0.0033 0.9241 0.041 Uiso 0.273(5) 1 calc PR A 2 C11' C -0.7320(12) 0.0686(6) 0.9766(19) 0.033(3) Uani 0.273(5) 1 d PDU A 2 H11' H -0.7845 0.0575 0.9969 0.040 Uiso 0.273(5) 1 calc PR A 2 C12' C -0.7077(9) 0.1221(5) 0.9851(16) 0.031(2) Uani 0.273(5) 1 d PDU A 2 C13' C -0.6311(10) 0.1382(7) 0.9574(18) 0.030(3) Uani 0.273(5) 1 d PDU A 2 H13' H -0.6150 0.1747 0.9636 0.036 Uiso 0.273(5) 1 calc PR A 2 C14' C -0.5782(15) 0.1017(4) 0.921(3) 0.033(3) Uani 0.273(5) 1 d PDU A 2 H14' H -0.5278 0.1137 0.8961 0.039 Uiso 0.273(5) 1 calc PR A 2 C15' C -0.7632(9) 0.1647(5) 1.0232(13) 0.036(2) Uani 0.273(5) 1 d PDU A 2 C16' C -0.8836(9) 0.1809(7) 1.1076(10) 0.042(3) Uani 0.273(5) 1 d PDU A 2 H16C H -0.8482 0.2057 1.1420 0.051 Uiso 0.273(5) 1 calc PR A 2 H16D H -0.9185 0.1609 1.1502 0.051 Uiso 0.273(5) 1 calc PR A 2 C34' C -0.9367(13) 0.2126(9) 1.0456(10) 0.042(3) Uani 0.273(5) 1 d PDU A 2 H34C H -0.9676 0.1878 1.0063 0.051 Uiso 0.273(5) 1 calc PR A 2 H34D H -0.9021 0.2360 1.0076 0.051 Uiso 0.273(5) 1 calc PR A 2 O3 O -0.4588(2) -0.22332(13) 0.8426(2) 0.0509(10) Uani 1 1 d U . . O4 O -0.34898(19) -0.23361(12) 0.7537(2) 0.0445(9) Uani 1 1 d U . . O5 O -0.2530(2) -0.33241(15) 0.7962(2) 0.0566(10) Uani 1 1 d U . . O6 O -0.1346(2) -0.34653(14) 0.9348(3) 0.0591(10) Uani 1 1 d U . . O7 O 0.1736(2) 0.07257(15) 0.5276(3) 0.0627(11) Uani 1 1 d DU . . O8 O 0.0875(2) 0.14356(14) 0.5448(2) 0.0556(10) Uani 1 1 d DU . . C1 C -0.4194(3) -0.05479(18) 0.8319(3) 0.0309(11) Uani 1 1 d U . . C2 C -0.4351(3) -0.10993(18) 0.8336(3) 0.0315(11) Uani 1 1 d U . . H2A H -0.4858 -0.1224 0.8571 0.038 Uiso 1 1 calc R . . C3 C -0.3788(2) -0.14692(17) 0.8021(3) 0.0295(11) Uani 1 1 d U . . C4 C -0.3041(3) -0.12882(17) 0.7692(3) 0.0294(11) Uani 1 1 d U . . H4A H -0.2651 -0.1540 0.7476 0.035 Uiso 1 1 calc R . . C5 C -0.2855(3) -0.07339(17) 0.7674(3) 0.0300(10) Uani 1 1 d U . . C6 C -0.3438(3) -0.03720(17) 0.7988(3) 0.0327(11) Uani 1 1 d U . . H6A H -0.3321 0.0002 0.7978 0.039 Uiso 1 1 calc R . . C7 C -0.4801(3) -0.01747(18) 0.8630(3) 0.0316(11) Uani 1 1 d U . . C8 C -0.5324(3) 0.01310(18) 0.8871(3) 0.0344(11) Uani 1 1 d U A . C9 C -0.5972(2) 0.04661(16) 0.9198(3) 0.0310(10) Uani 1 1 d DU . . C17 C -0.4009(3) -0.20497(19) 0.8035(3) 0.0373(12) Uani 1 1 d U . . C18 C -0.3696(3) -0.28856(17) 0.7368(4) 0.0478(13) Uani 1 1 d U . . H18A H -0.4080 -0.2911 0.6859 0.057 Uiso 1 1 calc R . . H18B H -0.3959 -0.3048 0.7898 0.057 Uiso 1 1 calc R . . C19 C -0.2911(3) -0.31706(19) 0.7157(3) 0.0505(14) Uani 1 1 d U . . H19A H -0.3025 -0.3493 0.6790 0.061 Uiso 1 1 calc R . . H19B H -0.2544 -0.2930 0.6816 0.061 Uiso 1 1 calc R . . C20 C -0.1749(3) -0.3575(2) 0.7843(4) 0.0603(15) Uani 1 1 d U . . H20A H -0.1332 -0.3300 0.7688 0.072 Uiso 1 1 calc R . . H20B H -0.1778 -0.3839 0.7350 0.072 Uiso 1 1 calc R . . C21 C -0.1513(3) -0.3852(2) 0.8685(4) 0.0589(15) Uani 1 1 d U . . H21A H -0.1965 -0.4089 0.8882 0.071 Uiso 1 1 calc R . . H21B H -0.1021 -0.4077 0.8582 0.071 Uiso 1 1 calc R . . C22 C -0.1278(4) -0.3703(2) 1.0199(4) 0.0727(19) Uani 1 1 d U . . H22A H -0.1160 -0.3425 1.0642 0.109 Uiso 1 1 calc R . . H22B H -0.0831 -0.3967 1.0194 0.109 Uiso 1 1 calc R . . H22C H -0.1794 -0.3884 1.0350 0.109 Uiso 1 1 calc R . . C23 C -0.2093(3) -0.05352(19) 0.7316(3) 0.0355(11) Uani 1 1 d U . . C24 C -0.1491(3) -0.03430(19) 0.7015(3) 0.0374(12) Uani 1 1 d U . . C25 C -0.0817(3) -0.00460(19) 0.6651(3) 0.0365(11) Uani 1 1 d U . . C26 C -0.0110(3) -0.02836(19) 0.6333(3) 0.0362(12) Uani 1 1 d U . . H26A H -0.0050 -0.0663 0.6359 0.043 Uiso 1 1 calc R . . C27 C 0.0509(3) 0.0026(2) 0.5978(3) 0.0392(12) Uani 1 1 d U . . H27A H 0.0995 -0.0141 0.5763 0.047 Uiso 1 1 calc R . . C28 C 0.0429(3) 0.0578(2) 0.5932(3) 0.0424(12) Uani 1 1 d DU . . C29 C -0.0275(3) 0.0818(2) 0.6265(3) 0.0460(13) Uani 1 1 d U . . H29A H -0.0333 0.1199 0.6248 0.055 Uiso 1 1 calc R . . C30 C -0.0884(3) 0.05067(19) 0.6618(3) 0.0448(13) Uani 1 1 d U . . H30A H -0.1363 0.0674 0.6847 0.054 Uiso 1 1 calc R . . C31 C 0.1097(3) 0.0912(2) 0.5506(3) 0.0475(13) Uani 1 1 d DU . . C32 C 0.1473(3) 0.1831(2) 0.5123(4) 0.0640(16) Uani 1 1 d DU . . H32A H 0.1285 0.2196 0.5290 0.077 Uiso 1 1 calc R . . H32B H 0.2005 0.1766 0.5422 0.077 Uiso 1 1 calc R . . C33 C 0.1595(3) 0.1810(2) 0.4156(3) 0.0679(17) Uani 1 1 d DU . . H33A H 0.1856 0.1461 0.4011 0.081 Uiso 1 1 calc R . . H33B H 0.1990 0.2096 0.3994 0.081 Uiso 1 1 calc 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 0.0772(11) 0.0814(12) 0.0461(10) 0.0137(9) 0.0068(9) -0.0026(9) S2 0.0547(9) 0.0565(9) 0.0642(11) -0.0159(8) 0.0031(8) 0.0197(8) O1 0.032(3) 0.037(3) 0.068(3) -0.003(3) 0.018(3) -0.003(2) O2 0.033(3) 0.034(3) 0.046(3) -0.006(2) 0.009(2) 0.006(2) C10 0.031(3) 0.040(3) 0.030(4) -0.002(3) 0.002(3) 0.002(3) C11 0.032(4) 0.030(3) 0.032(3) -0.001(3) 0.002(3) 0.006(3) C12 0.028(3) 0.031(3) 0.031(3) 0.001(3) 0.000(3) 0.002(3) C13 0.029(3) 0.034(4) 0.041(3) 0.000(4) 0.007(3) -0.002(3) C14 0.029(3) 0.035(3) 0.044(4) -0.001(4) 0.001(3) 0.005(3) C15 0.034(3) 0.033(3) 0.038(3) 0.001(3) 0.001(3) 0.000(3) C16 0.044(3) 0.036(3) 0.051(4) -0.008(3) 0.007(3) 0.007(3) C34 0.041(4) 0.034(4) 0.050(4) -0.007(3) 0.010(3) 0.006(3) O1' 0.044(6) 0.047(7) 0.071(7) -0.009(6) 0.010(6) -0.009(5) O2' 0.038(4) 0.037(4) 0.047(4) -0.003(4) 0.007(4) 0.003(4) C10' 0.029(4) 0.033(5) 0.040(5) 0.001(5) 0.003(4) 0.000(4) C11' 0.028(4) 0.033(5) 0.038(4) 0.001(4) 0.006(4) -0.001(4) C12' 0.029(4) 0.032(4) 0.033(4) 0.001(4) 0.001(4) 0.003(4) C13' 0.026(5) 0.032(5) 0.032(5) 0.001(4) 0.003(5) 0.004(4) C14' 0.028(5) 0.038(4) 0.032(5) 0.000(4) 0.002(4) 0.005(4) C15' 0.033(4) 0.036(4) 0.040(4) -0.001(4) 0.002(4) 0.001(4) C16' 0.038(5) 0.041(5) 0.048(5) -0.007(5) 0.013(5) 0.007(5) C34' 0.040(5) 0.038(6) 0.049(5) -0.008(5) 0.012(5) 0.007(5) O3 0.051(2) 0.046(2) 0.056(3) -0.0011(19) 0.017(2) -0.0131(18) O4 0.044(2) 0.0318(18) 0.057(2) -0.0038(17) 0.0035(18) -0.0013(15) O5 0.056(2) 0.069(2) 0.045(2) -0.003(2) 0.0036(19) 0.0217(19) O6 0.059(2) 0.057(2) 0.061(3) 0.002(2) -0.009(2) 0.0016(19) O7 0.043(2) 0.080(3) 0.065(3) -0.015(2) 0.019(2) -0.016(2) O8 0.057(2) 0.058(2) 0.052(2) 0.0109(19) -0.0041(19) -0.018(2) C1 0.027(2) 0.040(3) 0.026(2) -0.002(2) -0.003(2) 0.005(2) C2 0.021(2) 0.050(3) 0.023(3) 0.000(2) 0.001(2) -0.002(2) C3 0.025(2) 0.037(3) 0.026(2) 0.002(2) -0.004(2) 0.003(2) C4 0.025(2) 0.037(3) 0.027(3) -0.004(2) 0.004(2) 0.008(2) C5 0.025(2) 0.038(3) 0.027(2) -0.002(2) 0.000(2) 0.004(2) C6 0.037(3) 0.027(2) 0.034(3) -0.002(2) 0.001(2) 0.001(2) C7 0.028(2) 0.036(3) 0.031(3) -0.001(2) -0.002(2) 0.000(2) C8 0.028(3) 0.041(3) 0.035(3) 0.001(2) -0.004(2) 0.001(2) C9 0.025(2) 0.038(2) 0.031(2) 0.002(2) 0.001(2) 0.004(2) C17 0.034(3) 0.041(3) 0.037(3) 0.003(2) -0.004(2) -0.002(2) C18 0.052(3) 0.034(3) 0.058(3) -0.004(3) -0.005(3) 0.002(2) C19 0.069(3) 0.037(3) 0.046(3) -0.007(3) 0.002(3) 0.001(3) C20 0.059(3) 0.068(4) 0.054(4) -0.012(3) 0.009(3) 0.015(3) C21 0.053(3) 0.051(3) 0.073(4) -0.012(3) -0.006(3) 0.013(3) C22 0.058(4) 0.089(5) 0.071(5) 0.019(4) -0.019(4) -0.013(3) C23 0.031(3) 0.043(3) 0.033(3) -0.003(2) 0.005(2) 0.008(2) C24 0.034(3) 0.041(3) 0.037(3) 0.001(2) 0.003(2) 0.007(2) C25 0.031(2) 0.043(3) 0.035(3) 0.003(2) -0.001(2) 0.001(2) C26 0.036(3) 0.037(3) 0.036(3) 0.000(2) 0.002(2) 0.002(2) C27 0.026(2) 0.055(3) 0.036(3) -0.007(2) 0.006(2) -0.001(2) C28 0.040(3) 0.053(3) 0.034(3) -0.001(2) -0.001(2) -0.009(2) C29 0.047(3) 0.037(3) 0.053(3) 0.007(2) -0.002(3) -0.001(2) C30 0.030(3) 0.047(3) 0.057(3) 0.005(3) 0.005(3) 0.007(2) C31 0.040(3) 0.064(3) 0.038(3) -0.010(3) -0.003(3) -0.011(3) C32 0.059(3) 0.080(4) 0.054(4) -0.003(3) 0.001(3) -0.026(3) C33 0.062(4) 0.081(4) 0.061(4) 0.004(3) 0.018(3) -0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C33 1.802(5) . ? S1 S2 2.037(2) 3_456 ? S2 C34' 1.829(8) . ? S2 C34 1.843(5) . ? S2 S1 2.037(2) 3_456 ? O1 C15 1.195(6) . ? O2 C15 1.354(6) . ? O2 C16 1.462(6) . ? C10 C11 1.382(10) . ? C10 C9 1.402(6) . ? C10 H10 0.9500 . ? C11 C12 1.387(9) . ? C11 H11 0.9500 . ? C12 C13 1.381(8) . ? C12 C15 1.502(7) . ? C13 C14 1.366(9) . ? C13 H13 0.9500 . ? C14 C9 1.401(6) . ? C14 H14 0.9500 . ? C16 C34 1.502(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O1' C15' 1.190(9) . ? O2' C15' 1.353(8) . ? O2' C16' 1.467(8) . ? C10' C11' 1.388(14) . ? C10' C9 1.403(8) . ? C10' H10' 0.9500 . ? C11' C12' 1.393(12) . ? C11' H11' 0.9500 . ? C12' C13' 1.375(11) . ? C12' C15' 1.506(9) . ? C13' C14' 1.366(13) . ? C13' H13' 0.9500 . ? C14' C9 1.404(8) . ? C14' H14' 0.9500 . ? C16' C34' 1.496(9) . ? C16' H16C 0.9900 . ? C16' H16D 0.9900 . ? C34' H34C 0.9900 . ? C34' H34D 0.9900 . ? O3 C17 1.201(5) . ? O4 C17 1.335(5) . ? O4 C18 1.429(5) . ? O5 C19 1.411(6) . ? O5 C20 1.429(6) . ? O6 C21 1.410(6) . ? O6 C22 1.411(6) . ? O7 C31 1.191(5) . ? O8 C31 1.354(5) . ? O8 C32 1.467(5) . ? C1 C2 1.395(6) . ? C1 C6 1.398(6) . ? C1 C7 1.435(6) . ? C2 C3 1.383(6) . ? C2 H2A 0.9500 . ? C3 C4 1.389(6) . ? C3 C17 1.488(6) . ? C4 C5 1.411(6) . ? C4 H4A 0.9500 . ? C5 C6 1.391(6) . ? C5 C23 1.441(6) . ? C6 H6A 0.9500 . ? C7 C8 1.198(6) . ? C8 C9 1.431(6) . ? C18 C19 1.495(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.489(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.181(6) . ? C24 C25 1.432(6) . ? C25 C30 1.379(6) . ? C25 C26 1.381(6) . ? C26 C27 1.377(6) . ? C26 H26A 0.9500 . ? C27 C28 1.379(6) . ? C27 H27A 0.9500 . ? C28 C29 1.387(6) . ? C28 C31 1.512(6) . ? C29 C30 1.367(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C32 C33 1.466(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 C33 S1 S2 106.6(2) . 3_456 ? C34' S2 C34 13.1(10) . . ? C34' S2 S1 92.5(9) . 3_456 ? C34 S2 S1 105.5(3) . 3_456 ? C15 O2 C16 114.5(5) . . ? C11 C10 C9 120.4(7) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.1(7) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0(5) . . ? C13 C12 C15 117.9(6) . . ? C11 C12 C15 122.0(6) . . ? C14 C13 C12 120.1(7) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C9 121.3(7) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? O1 C15 O2 123.6(6) . . ? O1 C15 C12 122.9(6) . . ? O2 C15 C12 113.5(5) . . ? O2 C16 C34 112.3(5) . . ? O2 C16 H16A 109.1 . . ? C34 C16 H16A 109.1 . . ? O2 C16 H16B 109.1 . . ? C34 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 C34 S2 110.5(5) . . ? C16 C34 H34A 109.6 . . ? S2 C34 H34A 109.6 . . ? C16 C34 H34B 109.6 . . ? S2 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C15' O2' C16' 114.4(10) . . ? C11' C10' C9 120.2(14) . . ? C11' C10' H10' 119.9 . . ? C9 C10' H10' 119.9 . . ? C10' C11' C12' 119.2(14) . . ? C10' C11' H11' 120.4 . . ? C12' C11' H11' 120.4 . . ? C13' C12' C11' 120.5(9) . . ? C13' C12' C15' 117.2(10) . . ? C11' C12' C15' 122.3(10) . . ? C14' C13' C12' 120.1(14) . . ? C14' C13' H13' 119.9 . . ? C12' C13' H13' 119.9 . . ? C13' C14' C9 120.8(14) . . ? C13' C14' H14' 119.6 . . ? C9 C14' H14' 119.6 . . ? O1' C15' O2' 123.9(11) . . ? O1' C15' C12' 124.6(11) . . ? O2' C15' C12' 111.4(8) . . ? O2' C16' C34' 110.5(10) . . ? O2' C16' H16C 109.6 . . ? C34' C16' H16C 109.6 . . ? O2' C16' H16D 109.6 . . ? C34' C16' H16D 109.6 . . ? H16C C16' H16D 108.1 . . ? C16' C34' S2 109.8(9) . . ? C16' C34' H34C 109.7 . . ? S2 C34' H34C 109.7 . . ? C16' C34' H34D 109.7 . . ? S2 C34' H34D 109.7 . . ? H34C C34' H34D 108.2 . . ? C17 O4 C18 117.4(4) . . ? C19 O5 C20 113.7(4) . . ? C21 O6 C22 111.6(4) . . ? C31 O8 C32 119.1(4) . . ? C2 C1 C6 118.4(4) . . ? C2 C1 C7 120.1(4) . . ? C6 C1 C7 121.4(4) . . ? C3 C2 C1 121.7(4) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 C17 118.6(4) . . ? C4 C3 C17 122.2(4) . . ? C3 C4 C5 120.8(4) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 118.6(4) . . ? C6 C5 C23 119.6(4) . . ? C4 C5 C23 121.8(4) . . ? C5 C6 C1 121.4(4) . . ? C5 C6 H6A 119.3 . . ? C1 C6 H6A 119.3 . . ? C8 C7 C1 178.1(5) . . ? C7 C8 C9 175.9(5) . . ? C14 C9 C10 118.0(5) . . ? C14 C9 C10' 12.5(14) . . ? C10 C9 C10' 107.3(10) . . ? C14 C9 C14' 128.8(10) . . ? C10 C9 C14' 11.9(12) . . ? C10' C9 C14' 117.4(9) . . ? C14 C9 C8 117.1(5) . . ? C10 C9 C8 124.8(5) . . ? C10' C9 C8 127.8(8) . . ? C14' C9 C8 114.1(8) . . ? O3 C17 O4 124.7(4) . . ? O3 C17 C3 124.5(5) . . ? O4 C17 C3 110.8(4) . . ? O4 C18 C19 106.8(4) . . ? O4 C18 H18A 110.4 . . ? C19 C18 H18A 110.4 . . ? O4 C18 H18B 110.4 . . ? C19 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? O5 C19 C18 108.9(4) . . ? O5 C19 H19A 109.9 . . ? C18 C19 H19A 109.9 . . ? O5 C19 H19B 109.9 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? O5 C20 C21 108.9(4) . . ? O5 C20 H20A 109.9 . . ? C21 C20 H20A 109.9 . . ? O5 C20 H20B 109.9 . . ? C21 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? O6 C21 C20 109.5(5) . . ? O6 C21 H21A 109.8 . . ? C20 C21 H21A 109.8 . . ? O6 C21 H21B 109.8 . . ? C20 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? O6 C22 H22A 109.5 . . ? O6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C5 176.0(5) . . ? C23 C24 C25 172.7(5) . . ? C30 C25 C26 118.6(4) . . ? C30 C25 C24 117.8(4) . . ? C26 C25 C24 123.5(4) . . ? C27 C26 C25 120.5(5) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C28 120.4(5) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C27 C28 C29 119.3(5) . . ? C27 C28 C31 119.9(5) . . ? C29 C28 C31 120.8(5) . . ? C30 C29 C28 119.8(5) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C25 121.4(5) . . ? C29 C30 H30A 119.3 . . ? C25 C30 H30A 119.3 . . ? O7 C31 O8 126.1(5) . . ? O7 C31 C28 122.6(5) . . ? O8 C31 C28 111.2(4) . . ? C33 C32 O8 113.3(4) . . ? C33 C32 H32A 108.9 . . ? O8 C32 H32A 108.9 . . ? C33 C32 H32B 108.9 . . ? O8 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C32 C33 S1 117.9(4) . . ? C32 C33 H33A 107.8 . . ? S1 C33 H33A 107.8 . . ? C32 C33 H33B 107.8 . . ? S1 C33 H33B 107.8 . . ? H33A C33 H33B 107.2 . . ? 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 C9 C10 C11 C12 1.6(16) . . . . ? C10 C11 C12 C13 -1.7(14) . . . . ? C10 C11 C12 C15 176.7(9) . . . . ? C11 C12 C13 C14 2.1(14) . . . . ? C15 C12 C13 C14 -176.4(9) . . . . ? C12 C13 C14 C9 -2.4(17) . . . . ? C16 O2 C15 O1 5.4(10) . . . . ? C16 O2 C15 C12 -171.9(6) . . . . ? C13 C12 C15 O1 6.1(12) . . . . ? C11 C12 C15 O1 -172.3(8) . . . . ? C13 C12 C15 O2 -176.6(7) . . . . ? C11 C12 C15 O2 5.0(11) . . . . ? C15 O2 C16 C34 -82.8(8) . . . . ? O2 C16 C34 S2 172.4(5) . . . . ? C34' S2 C34 C16 -87(3) . . . . ? S1 S2 C34 C16 -87.7(6) 3_456 . . . ? C9 C10' C11' C12' 9(5) . . . . ? C10' C11' C12' C13' -1(4) . . . . ? C10' C11' C12' C15' 178(3) . . . . ? C11' C12' C13' C14' 0(4) . . . . ? C15' C12' C13' C14' -179(3) . . . . ? C12' C13' C14' C9 -7(5) . . . . ? C16' O2' C15' O1' -5(3) . . . . ? C16' O2' C15' C12' 171.4(16) . . . . ? C13' C12' C15' O1' 3(4) . . . . ? C11' C12' C15' O1' -176(2) . . . . ? C13' C12' C15' O2' -173(2) . . . . ? C11' C12' C15' O2' 8(3) . . . . ? C15' O2' C16' C34' 83(2) . . . . ? O2' C16' C34' S2 173.5(13) . . . . ? C34 S2 C34' C16' 112(4) . . . . ? S1 S2 C34' C16' -67.8(17) 3_456 . . . ? C6 C1 C2 C3 -1.3(7) . . . . ? C7 C1 C2 C3 178.3(4) . . . . ? C1 C2 C3 C4 1.1(7) . . . . ? C1 C2 C3 C17 -178.2(4) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C17 C3 C4 C5 179.0(4) . . . . ? C3 C4 C5 C6 -0.4(7) . . . . ? C3 C4 C5 C23 -178.4(4) . . . . ? C4 C5 C6 C1 0.2(7) . . . . ? C23 C5 C6 C1 178.3(4) . . . . ? C2 C1 C6 C5 0.6(7) . . . . ? C7 C1 C6 C5 -179.0(4) . . . . ? C2 C1 C7 C8 -59(16) . . . . ? C6 C1 C7 C8 121(16) . . . . ? C1 C7 C8 C9 84(18) . . . . ? C13 C14 C9 C10 2.2(17) . . . . ? C13 C14 C9 C10' -30(9) . . . . ? C13 C14 C9 C14' -4(3) . . . . ? C13 C14 C9 C8 178.6(9) . . . . ? C11 C10 C9 C14 -1.8(16) . . . . ? C11 C10 C9 C10' 5(2) . . . . ? C11 C10 C9 C14' 155(12) . . . . ? C11 C10 C9 C8 -177.9(8) . . . . ? C11' C10' C9 C14 142(12) . . . . ? C11' C10' C9 C10 -9(4) . . . . ? C11' C10' C9 C14' -15(4) . . . . ? C11' C10' C9 C8 175(2) . . . . ? C13' C14' C9 C14 8(5) . . . . ? C13' C14' C9 C10 -19(8) . . . . ? C13' C14' C9 C10' 14(4) . . . . ? C13' C14' C9 C8 -174(2) . . . . ? C7 C8 C9 C14 -30(7) . . . . ? C7 C8 C9 C10 146(7) . . . . ? C7 C8 C9 C10' -38(8) . . . . ? C7 C8 C9 C14' 152(7) . . . . ? C18 O4 C17 O3 8.1(7) . . . . ? C18 O4 C17 C3 -170.2(4) . . . . ? C2 C3 C17 O3 -12.1(7) . . . . ? C4 C3 C17 O3 168.6(5) . . . . ? C2 C3 C17 O4 166.3(4) . . . . ? C4 C3 C17 O4 -13.0(6) . . . . ? C17 O4 C18 C19 -156.6(4) . . . . ? C20 O5 C19 C18 -176.7(4) . . . . ? O4 C18 C19 O5 84.2(5) . . . . ? C19 O5 C20 C21 -164.5(4) . . . . ? C22 O6 C21 C20 168.5(4) . . . . ? O5 C20 C21 O6 -68.8(6) . . . . ? C6 C5 C23 C24 -20(8) . . . . ? C4 C5 C23 C24 158(7) . . . . ? C5 C23 C24 C25 6(11) . . . . ? C23 C24 C25 C30 8(4) . . . . ? C23 C24 C25 C26 -172(4) . . . . ? C30 C25 C26 C27 -1.0(7) . . . . ? C24 C25 C26 C27 178.9(5) . . . . ? C25 C26 C27 C28 -0.3(7) . . . . ? C26 C27 C28 C29 1.4(7) . . . . ? C26 C27 C28 C31 -177.5(4) . . . . ? C27 C28 C29 C30 -1.2(8) . . . . ? C31 C28 C29 C30 177.7(5) . . . . ? C28 C29 C30 C25 -0.1(8) . . . . ? C26 C25 C30 C29 1.3(8) . . . . ? C24 C25 C30 C29 -178.7(5) . . . . ? C32 O8 C31 O7 -3.7(8) . . . . ? C32 O8 C31 C28 174.8(4) . . . . ? C27 C28 C31 O7 -7.2(8) . . . . ? C29 C28 C31 O7 173.9(5) . . . . ? C27 C28 C31 O8 174.3(4) . . . . ? C29 C28 C31 O8 -4.6(7) . . . . ? C31 O8 C32 C33 75.6(6) . . . . ? O8 C32 C33 S1 55.8(7) . . . . ? S2 S1 C33 C32 48.6(5) 3_456 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.499 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.065 # Attachment '2d.cif' data_sx2777d _database_code_depnum_ccdc_archive 'CCDC 784329' #TrackingRef '2d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H46 O12 S6, C4 H10 O' _chemical_formula_sum 'C66 H56 O13 S6' _chemical_formula_weight 1249.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 7.6656(15) _cell_length_b 27.416(6) _cell_length_c 29.336(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.51(3) _cell_angle_gamma 90.00 _cell_volume 6159(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1204 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 68.22 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 2.581 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4250 _exptl_absorpt_correction_T_max 0.6829 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54186 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku raxis Rapid IP Area Detector' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43226 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 68.25 _reflns_number_total 11099 _reflns_number_gt 6520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto(Rigaku 2001)' _computing_cell_refinement 'Rapid Auto(Rigaku 2001)' _computing_data_reduction 'Rapid Auto(Rigaku 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00069(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11099 _refine_ls_number_parameters 769 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1254 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2178 _refine_ls_wR_factor_gt 0.1830 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.05659(16) 0.54332(4) 0.12244(4) 0.0493(3) Uani 1 1 d . . . S2 S 0.03883(16) 0.61723(4) 0.12549(4) 0.0498(3) Uani 1 1 d . . . S3 S -0.41329(17) 1.01244(4) -0.20294(4) 0.0521(4) Uani 1 1 d . . . S4 S -0.62997(17) 1.03310(4) -0.24073(4) 0.0535(4) Uani 1 1 d . . . S5 S -1.11201(19) 0.57781(5) -0.63410(5) 0.0660(4) Uani 1 1 d . . . S6 S -1.03979(18) 0.50948(5) -0.61648(5) 0.0642(4) Uani 1 1 d . . . O1 O 0.2080(4) 0.64288(10) 0.02614(10) 0.0430(8) Uani 1 1 d . . . O2 O 0.3906(4) 0.70704(11) 0.03232(11) 0.0549(9) Uani 1 1 d . . . O3 O -0.3853(4) 0.91566(10) -0.33602(10) 0.0494(8) Uani 1 1 d . . . O4 O -0.2443(4) 0.93691(10) -0.27002(10) 0.0437(8) Uani 1 1 d . . . O5 O -0.7887(4) 0.89425(11) -0.23766(10) 0.0526(9) Uani 1 1 d . . . O6 O -0.6858(5) 0.86860(12) -0.16936(12) 0.0711(11) Uani 1 1 d . . . O7 O -1.3912(4) 0.72017(13) -0.56293(12) 0.0666(11) Uani 1 1 d . . . O8 O -1.2622(4) 0.64689(13) -0.55787(11) 0.0607(10) Uani 1 1 d . . . O9 O -0.6991(4) 0.57333(11) -0.52903(11) 0.0533(9) Uani 1 1 d . . . O10 O -0.6789(4) 0.51133(11) -0.47923(10) 0.0534(9) Uani 1 1 d . . . O11 O -0.2965(4) 0.49567(11) -0.01412(10) 0.0510(9) Uani 1 1 d . . . O12 O -0.3063(4) 0.56420(11) 0.02720(10) 0.0491(8) Uani 1 1 d . . . O13 O -0.0236(4) 0.60758(11) -0.24179(11) 0.0550(9) Uani 1 1 d . . . C1 C -0.2454(6) 0.53778(19) 0.06711(16) 0.0559(14) Uani 1 1 d . . . H1A H -0.3058 0.5059 0.0680 0.067 Uiso 1 1 calc R . . H1B H -0.2745 0.5563 0.0947 0.067 Uiso 1 1 calc R . . C2 C -0.0499(6) 0.52949(18) 0.06736(17) 0.0564(14) Uani 1 1 d . . . H2A H 0.0007 0.5503 0.0437 0.068 Uiso 1 1 calc R . . H2B H -0.0269 0.4950 0.0595 0.068 Uiso 1 1 calc R . . C3 C 0.2554(6) 0.63603(16) 0.10963(15) 0.0468(12) Uani 1 1 d . . . H3A H 0.2611 0.6721 0.1108 0.056 Uiso 1 1 calc R . . H3B H 0.3415 0.6234 0.1328 0.056 Uiso 1 1 calc R . . C4 C 0.3097(6) 0.61982(16) 0.06337(15) 0.0453(12) Uani 1 1 d . . . H4A H 0.4347 0.6276 0.0603 0.054 Uiso 1 1 calc R . . H4B H 0.2963 0.5840 0.0610 0.054 Uiso 1 1 calc R . . C5 C 0.2690(6) 0.68671(16) 0.01307(16) 0.0430(11) Uani 1 1 d . . . C6 C 0.1698(5) 0.70701(15) -0.02736(15) 0.0378(11) Uani 1 1 d . . . C7 C 0.2193(6) 0.75216(16) -0.04360(15) 0.0452(12) Uani 1 1 d . . . H7A H 0.3108 0.7697 -0.0281 0.054 Uiso 1 1 calc R . . C8 C 0.1371(6) 0.77197(16) -0.08206(15) 0.0464(12) Uani 1 1 d . . . H8A H 0.1729 0.8029 -0.0928 0.056 Uiso 1 1 calc R . . C9 C 0.0024(6) 0.74700(16) -0.10520(15) 0.0420(11) Uani 1 1 d . . . C10 C -0.0492(6) 0.70199(16) -0.08840(15) 0.0462(12) Uani 1 1 d . . . H10A H -0.1421 0.6847 -0.1035 0.055 Uiso 1 1 calc R . . C11 C 0.0336(6) 0.68231(16) -0.04988(16) 0.0436(12) Uani 1 1 d . . . H11A H -0.0030 0.6516 -0.0387 0.052 Uiso 1 1 calc R . . C12 C -0.0803(6) 0.76612(16) -0.14686(17) 0.0452(12) Uani 1 1 d . . . C13 C -0.1454(6) 0.77957(16) -0.18143(17) 0.0458(12) Uani 1 1 d . . . C14 C -0.2209(6) 0.79351(16) -0.22556(15) 0.0401(11) Uani 1 1 d . . . C15 C -0.2294(5) 0.84190(15) -0.23990(15) 0.0398(11) Uani 1 1 d . . . H15A H -0.1894 0.8672 -0.2199 0.048 Uiso 1 1 calc R . . C16 C -0.2966(6) 0.85344(15) -0.28376(15) 0.0373(11) Uani 1 1 d . . . C17 C -0.3489(5) 0.81606(16) -0.31333(15) 0.0407(11) Uani 1 1 d . . . H17A H -0.3904 0.8238 -0.3435 0.049 Uiso 1 1 calc R . . C18 C -0.3414(5) 0.76771(14) -0.29962(15) 0.0348(10) Uani 1 1 d . . . C19 C -0.2793(5) 0.75706(16) -0.25557(15) 0.0412(11) Uani 1 1 d . . . H19A H -0.2765 0.7241 -0.2457 0.049 Uiso 1 1 calc R . . C20 C -0.3139(6) 0.90445(15) -0.29979(16) 0.0393(11) Uani 1 1 d . . . C21 C -0.2558(6) 0.98777(14) -0.28359(16) 0.0470(12) Uani 1 1 d . . . H21A H -0.3693 0.9940 -0.3000 0.056 Uiso 1 1 calc R . . H21B H -0.1614 0.9957 -0.3043 0.056 Uiso 1 1 calc R . . C22 C -0.2393(6) 1.01869(16) -0.24211(15) 0.0513(13) Uani 1 1 d . . . H22A H -0.2333 1.0532 -0.2517 0.062 Uiso 1 1 calc R . . H22B H -0.1274 1.0107 -0.2256 0.062 Uiso 1 1 calc R . . C23 C -0.7196(6) 0.97517(16) -0.26066(16) 0.0508(13) Uani 1 1 d . . . H23A H -0.8217 0.9813 -0.2817 0.061 Uiso 1 1 calc R . . H23B H -0.6307 0.9575 -0.2778 0.061 Uiso 1 1 calc R . . C24 C -0.7742(7) 0.94425(16) -0.22187(16) 0.0521(13) Uani 1 1 d . . . H24A H -0.6867 0.9465 -0.1961 0.062 Uiso 1 1 calc R . . H24B H -0.8880 0.9556 -0.2112 0.062 Uiso 1 1 calc R . . C25 C -0.7350(6) 0.85990(17) -0.20833(18) 0.0479(12) Uani 1 1 d . . . C26 C -0.7384(6) 0.81057(15) -0.22850(15) 0.0414(11) Uani 1 1 d . . . C27 C -0.8078(6) 0.80179(16) -0.27238(15) 0.0434(12) Uani 1 1 d . . . H27A H -0.8540 0.8280 -0.2903 0.052 Uiso 1 1 calc R . . C28 C -0.8096(6) 0.75417(16) -0.29010(15) 0.0421(11) Uani 1 1 d . . . C29 C -0.7422(6) 0.71585(16) -0.26291(16) 0.0447(12) Uani 1 1 d . . . H29A H -0.7420 0.6835 -0.2746 0.054 Uiso 1 1 calc R . . C30 C -0.6760(6) 0.72502(16) -0.21899(17) 0.0458(12) Uani 1 1 d . . . C31 C -0.6736(6) 0.77238(16) -0.20187(16) 0.0437(11) Uani 1 1 d . . . H31A H -0.6274 0.7785 -0.1718 0.052 Uiso 1 1 calc R . . C32 C -0.8812(6) 0.74485(16) -0.33524(17) 0.0462(12) Uani 1 1 d . . . C33 C -0.9448(6) 0.73593(16) -0.37230(18) 0.0483(12) Uani 1 1 d . . . C34 C -1.0250(6) 0.72537(17) -0.41646(15) 0.0413(11) Uani 1 1 d . . . C35 C -1.1313(6) 0.76007(17) -0.43908(16) 0.0491(13) Uani 1 1 d . . . H35A H -1.1469 0.7915 -0.4262 0.059 Uiso 1 1 calc R . . C36 C -1.2131(6) 0.74803(18) -0.48035(16) 0.0505(13) Uani 1 1 d . . . H36A H -1.2871 0.7712 -0.4956 0.061 Uiso 1 1 calc R . . C37 C -1.1895(6) 0.70322(18) -0.49982(16) 0.0461(12) Uani 1 1 d . . . C38 C -1.0818(6) 0.66915(18) -0.47809(16) 0.0481(12) Uani 1 1 d . . . H38A H -1.0645 0.6383 -0.4919 0.058 Uiso 1 1 calc R . . C39 C -0.9994(6) 0.67981(17) -0.43658(16) 0.0486(12) Uani 1 1 d . . . H39A H -0.9256 0.6563 -0.4217 0.058 Uiso 1 1 calc R . . C40 C -1.2922(6) 0.69229(19) -0.54357(17) 0.0503(13) Uani 1 1 d . . . C41 C -1.3705(7) 0.6327(2) -0.59834(17) 0.0634(15) Uani 1 1 d . . . H41A H -1.4958 0.6357 -0.5920 0.076 Uiso 1 1 calc R . . H41B H -1.3457 0.6542 -0.6244 0.076 Uiso 1 1 calc R . . C42 C -1.3288(6) 0.58291(19) -0.60898(19) 0.0655(16) Uani 1 1 d . . . H42A H -1.4192 0.5697 -0.6308 0.079 Uiso 1 1 calc R . . H42B H -1.3298 0.5631 -0.5808 0.079 Uiso 1 1 calc R . . C43 C -0.9294(6) 0.51936(18) -0.56181(16) 0.0559(14) Uani 1 1 d . . . H43A H -1.0003 0.5416 -0.5435 0.067 Uiso 1 1 calc R . . H43B H -0.9193 0.4879 -0.5454 0.067 Uiso 1 1 calc R . . C44 C -0.7519(6) 0.54060(18) -0.56578(17) 0.0577(14) Uani 1 1 d . . . H44A H -0.6662 0.5137 -0.5668 0.069 Uiso 1 1 calc R . . H44B H -0.7486 0.5585 -0.5950 0.069 Uiso 1 1 calc R . . C45 C -0.6635(6) 0.55414(17) -0.48761(16) 0.0442(12) Uani 1 1 d . . . C46 C -0.6052(5) 0.59208(15) -0.45428(15) 0.0377(11) Uani 1 1 d . . . C47 C -0.5712(6) 0.57912(16) -0.40873(15) 0.0482(13) Uani 1 1 d . . . H47A H -0.5845 0.5462 -0.3994 0.058 Uiso 1 1 calc R . . C48 C -0.5185(6) 0.61385(16) -0.37734(16) 0.0503(13) Uani 1 1 d . . . H48A H -0.4940 0.6044 -0.3466 0.060 Uiso 1 1 calc R . . C49 C -0.5003(6) 0.66255(15) -0.38953(15) 0.0393(11) Uani 1 1 d . . . C50 C -0.5364(6) 0.67562(15) -0.43530(15) 0.0439(12) Uani 1 1 d . . . H50A H -0.5241 0.7086 -0.4446 0.053 Uiso 1 1 calc R . . C51 C -0.5899(6) 0.64060(15) -0.46697(16) 0.0448(12) Uani 1 1 d . . . H51A H -0.6163 0.6499 -0.4977 0.054 Uiso 1 1 calc R . . C52 C -0.4446(6) 0.69861(16) -0.35705(15) 0.0419(11) Uani 1 1 d . . . C53 C -0.3984(6) 0.72957(16) -0.33111(16) 0.0422(11) Uani 1 1 d . . . C54 C -0.6092(6) 0.68676(17) -0.19007(17) 0.0486(12) Uani 1 1 d . . . C55 C -0.5551(6) 0.65797(18) -0.16195(18) 0.0517(13) Uani 1 1 d . . . C56 C -0.4950(6) 0.62748(16) -0.12473(17) 0.0456(12) Uani 1 1 d . . . C57 C -0.4582(6) 0.57788(16) -0.13079(17) 0.0469(12) Uani 1 1 d . . . H57A H -0.4703 0.5637 -0.1603 0.056 Uiso 1 1 calc R . . C58 C -0.4044(6) 0.54956(16) -0.09375(16) 0.0461(12) Uani 1 1 d . . . H58A H -0.3815 0.5158 -0.0978 0.055 Uiso 1 1 calc R . . C59 C -0.3838(6) 0.57045(15) -0.05052(15) 0.0394(11) Uani 1 1 d . . . C60 C -0.4167(6) 0.61978(16) -0.04494(17) 0.0487(12) Uani 1 1 d . . . H60A H -0.4012 0.6342 -0.0156 0.058 Uiso 1 1 calc R . . C61 C -0.4717(6) 0.64788(17) -0.08162(17) 0.0514(13) Uani 1 1 d . . . H61A H -0.4940 0.6816 -0.0774 0.062 Uiso 1 1 calc R . . C62 C -0.3245(6) 0.53902(17) -0.01187(16) 0.0435(11) Uani 1 1 d . . . C63 C 0.0046(7) 0.59292(18) -0.16206(18) 0.0687(16) Uani 1 1 d . . . H63A H -0.0212 0.6061 -0.1320 0.103 Uiso 1 1 calc R . . H63B H 0.1312 0.5899 -0.1644 0.103 Uiso 1 1 calc R . . H63C H -0.0498 0.5607 -0.1659 0.103 Uiso 1 1 calc R . . C64 C -0.0671(7) 0.62681(17) -0.19870(18) 0.0598(14) Uani 1 1 d . . . H64A H -0.1955 0.6295 -0.1970 0.072 Uiso 1 1 calc R . . H64B H -0.0160 0.6597 -0.1944 0.072 Uiso 1 1 calc R . . C65 C -0.1038(6) 0.63390(16) -0.27922(18) 0.0555(14) Uani 1 1 d . . . H65A H -0.0678 0.6686 -0.2777 0.067 Uiso 1 1 calc R . . H65B H -0.2325 0.6324 -0.2777 0.067 Uiso 1 1 calc R . . C66 C -0.0480(7) 0.61143(18) -0.32299(17) 0.0629(15) Uani 1 1 d . . . H66A H -0.0971 0.6302 -0.3489 0.094 Uiso 1 1 calc R . . H66B H -0.0903 0.5777 -0.3250 0.094 Uiso 1 1 calc R . . H66C H 0.0797 0.6117 -0.3235 0.094 Uiso 1 1 calc 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 0.0575(8) 0.0417(7) 0.0482(8) 0.0077(6) -0.0048(6) -0.0009(6) S2 0.0555(8) 0.0432(7) 0.0508(8) -0.0038(6) 0.0046(6) 0.0014(6) S3 0.0692(9) 0.0418(7) 0.0448(8) -0.0073(6) -0.0032(6) 0.0034(6) S4 0.0662(9) 0.0394(7) 0.0551(8) 0.0018(6) 0.0036(7) 0.0117(6) S5 0.0703(10) 0.0760(10) 0.0518(8) 0.0001(7) 0.0030(7) 0.0181(8) S6 0.0671(10) 0.0689(10) 0.0560(9) -0.0148(7) -0.0045(7) -0.0064(7) O1 0.0461(19) 0.0355(17) 0.0470(19) 0.0084(14) -0.0001(15) -0.0053(14) O2 0.057(2) 0.0424(19) 0.064(2) 0.0051(17) -0.0109(18) -0.0119(16) O3 0.067(2) 0.0359(18) 0.044(2) 0.0023(15) -0.0084(17) -0.0064(15) O4 0.056(2) 0.0268(16) 0.0479(19) -0.0070(14) 0.0016(16) -0.0012(14) O5 0.070(2) 0.0416(19) 0.045(2) -0.0027(16) -0.0061(17) 0.0039(17) O6 0.104(3) 0.053(2) 0.053(2) -0.0112(18) -0.023(2) 0.009(2) O7 0.057(2) 0.084(3) 0.058(2) -0.004(2) -0.0034(19) 0.005(2) O8 0.051(2) 0.074(3) 0.057(2) -0.0219(19) -0.0021(18) -0.0032(18) O9 0.067(2) 0.050(2) 0.042(2) -0.0044(16) -0.0088(17) -0.0127(16) O10 0.067(2) 0.0402(19) 0.053(2) -0.0019(16) -0.0020(18) -0.0070(17) O11 0.063(2) 0.0413(19) 0.049(2) -0.0036(16) 0.0058(17) 0.0030(16) O12 0.054(2) 0.048(2) 0.044(2) -0.0074(16) -0.0019(16) 0.0019(16) O13 0.058(2) 0.0420(19) 0.065(2) -0.0074(18) 0.0001(18) 0.0121(16) C1 0.054(3) 0.072(4) 0.042(3) 0.000(3) 0.001(3) 0.000(3) C2 0.051(3) 0.058(3) 0.060(3) -0.014(3) 0.000(3) -0.001(3) C3 0.055(3) 0.037(3) 0.048(3) 0.004(2) 0.000(2) 0.001(2) C4 0.048(3) 0.034(3) 0.053(3) 0.006(2) 0.002(2) 0.005(2) C5 0.043(3) 0.039(3) 0.047(3) 0.006(2) 0.007(2) 0.000(2) C6 0.034(3) 0.035(2) 0.044(3) -0.003(2) 0.000(2) -0.0018(19) C7 0.051(3) 0.040(3) 0.044(3) -0.002(2) -0.005(2) -0.008(2) C8 0.054(3) 0.039(3) 0.046(3) 0.003(2) -0.001(2) -0.008(2) C9 0.045(3) 0.040(3) 0.041(3) -0.002(2) 0.004(2) 0.001(2) C10 0.052(3) 0.037(3) 0.049(3) -0.001(2) -0.003(2) -0.007(2) C11 0.043(3) 0.037(3) 0.051(3) 0.001(2) 0.006(2) -0.009(2) C12 0.049(3) 0.040(3) 0.047(3) -0.003(2) 0.003(2) 0.001(2) C13 0.051(3) 0.034(3) 0.052(3) -0.005(2) -0.001(3) 0.001(2) C14 0.042(3) 0.035(2) 0.043(3) -0.001(2) 0.001(2) -0.005(2) C15 0.044(3) 0.033(2) 0.042(3) -0.002(2) 0.005(2) -0.004(2) C16 0.041(3) 0.033(2) 0.038(3) 0.001(2) 0.003(2) 0.0011(19) C17 0.036(3) 0.043(3) 0.043(3) -0.006(2) 0.000(2) -0.003(2) C18 0.039(3) 0.025(2) 0.040(3) -0.0024(19) 0.002(2) -0.0014(18) C19 0.045(3) 0.036(3) 0.043(3) -0.003(2) 0.002(2) 0.003(2) C20 0.042(3) 0.032(2) 0.044(3) -0.001(2) 0.009(2) -0.006(2) C21 0.061(3) 0.027(2) 0.054(3) -0.002(2) 0.011(3) -0.001(2) C22 0.065(3) 0.033(3) 0.056(3) -0.002(2) 0.001(3) -0.011(2) C23 0.055(3) 0.051(3) 0.046(3) 0.002(2) -0.006(2) 0.002(2) C24 0.067(3) 0.038(3) 0.052(3) -0.003(2) 0.010(3) 0.000(2) C25 0.048(3) 0.045(3) 0.051(3) -0.008(3) 0.003(2) 0.004(2) C26 0.044(3) 0.037(3) 0.044(3) -0.001(2) 0.000(2) -0.002(2) C27 0.047(3) 0.040(3) 0.043(3) 0.000(2) -0.003(2) -0.003(2) C28 0.042(3) 0.044(3) 0.041(3) -0.001(2) 0.006(2) -0.001(2) C29 0.043(3) 0.039(3) 0.052(3) -0.001(2) 0.006(2) -0.007(2) C30 0.048(3) 0.039(3) 0.051(3) 0.002(2) 0.004(2) 0.004(2) C31 0.043(3) 0.045(3) 0.043(3) 0.000(2) 0.002(2) 0.001(2) C32 0.046(3) 0.043(3) 0.050(3) 0.001(2) 0.001(2) -0.007(2) C33 0.049(3) 0.038(3) 0.057(3) -0.002(2) 0.002(3) -0.005(2) C34 0.038(3) 0.049(3) 0.037(3) -0.001(2) 0.006(2) -0.007(2) C35 0.048(3) 0.046(3) 0.053(3) -0.005(2) 0.000(2) -0.007(2) C36 0.044(3) 0.052(3) 0.056(3) -0.001(3) 0.001(3) 0.000(2) C37 0.037(3) 0.064(3) 0.038(3) -0.005(2) 0.005(2) 0.002(2) C38 0.046(3) 0.054(3) 0.044(3) -0.012(2) 0.007(2) -0.006(2) C39 0.048(3) 0.050(3) 0.049(3) -0.002(2) 0.006(2) -0.002(2) C40 0.042(3) 0.060(3) 0.049(3) -0.005(3) 0.008(2) 0.004(3) C41 0.053(3) 0.079(4) 0.057(4) -0.014(3) -0.008(3) -0.007(3) C42 0.056(3) 0.064(4) 0.076(4) -0.018(3) -0.007(3) 0.003(3) C43 0.061(3) 0.060(3) 0.047(3) 0.002(3) -0.001(3) -0.011(3) C44 0.064(4) 0.056(3) 0.053(3) -0.008(3) 0.002(3) -0.011(3) C45 0.051(3) 0.038(3) 0.043(3) -0.001(2) 0.001(2) -0.005(2) C46 0.041(3) 0.031(2) 0.042(3) -0.001(2) -0.001(2) -0.0069(19) C47 0.066(3) 0.032(3) 0.045(3) 0.006(2) -0.004(3) -0.003(2) C48 0.077(4) 0.036(3) 0.037(3) -0.001(2) -0.007(3) -0.008(2) C49 0.046(3) 0.030(2) 0.042(3) -0.003(2) 0.004(2) -0.002(2) C50 0.058(3) 0.027(2) 0.047(3) 0.002(2) 0.003(2) -0.001(2) C51 0.055(3) 0.036(3) 0.043(3) 0.002(2) 0.000(2) -0.006(2) C52 0.050(3) 0.033(3) 0.042(3) -0.002(2) 0.002(2) -0.001(2) C53 0.046(3) 0.035(3) 0.045(3) 0.002(2) 0.003(2) 0.000(2) C54 0.045(3) 0.047(3) 0.054(3) -0.001(3) -0.001(2) 0.002(2) C55 0.049(3) 0.046(3) 0.061(4) -0.003(3) 0.005(3) -0.004(2) C56 0.043(3) 0.038(3) 0.056(3) 0.004(2) 0.002(2) -0.003(2) C57 0.046(3) 0.042(3) 0.052(3) -0.009(2) -0.002(2) -0.001(2) C58 0.054(3) 0.033(3) 0.051(3) -0.001(2) 0.002(2) -0.001(2) C59 0.045(3) 0.033(2) 0.040(3) 0.000(2) 0.004(2) 0.000(2) C60 0.060(3) 0.039(3) 0.048(3) -0.007(2) 0.009(3) -0.004(2) C61 0.063(3) 0.037(3) 0.055(3) -0.001(2) 0.012(3) -0.003(2) C62 0.041(3) 0.041(3) 0.049(3) -0.010(2) 0.002(2) 0.002(2) C63 0.085(4) 0.047(3) 0.076(4) -0.006(3) 0.011(3) 0.008(3) C64 0.065(4) 0.043(3) 0.073(4) -0.016(3) 0.015(3) 0.002(3) C65 0.056(3) 0.033(3) 0.079(4) 0.002(3) 0.006(3) 0.003(2) C66 0.075(4) 0.049(3) 0.066(4) 0.003(3) 0.007(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C2 1.818(5) . ? S1 S2 2.0330(18) . ? S2 C3 1.818(5) . ? S3 C22 1.807(5) . ? S3 S4 2.0366(19) . ? S4 C23 1.817(5) . ? S5 C42 1.853(5) . ? S5 S6 2.014(2) . ? S6 C43 1.801(5) . ? O1 C5 1.351(5) . ? O1 C4 1.458(5) . ? O2 C5 1.205(5) . ? O3 C20 1.213(5) . ? O4 C20 1.341(5) . ? O4 C21 1.452(5) . ? O5 C25 1.329(5) . ? O5 C24 1.450(5) . ? O6 C25 1.212(5) . ? O7 C40 1.202(5) . ? O8 C40 1.337(5) . ? O8 C41 1.471(5) . ? O9 C45 1.341(5) . ? O9 C44 1.447(5) . ? O10 C45 1.206(5) . ? O11 C62 1.210(5) . ? O12 C62 1.340(5) . ? O12 C1 1.437(5) . ? O13 C64 1.423(5) . ? O13 C65 1.430(5) . ? C1 C2 1.515(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.504(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.489(6) . ? C6 C7 1.385(6) . ? C6 C11 1.387(5) . ? C7 C8 1.379(6) . ? C7 H7A 0.9500 . ? C8 C9 1.391(6) . ? C8 H8A 0.9500 . ? C9 C10 1.392(6) . ? C9 C12 1.450(6) . ? C10 C11 1.381(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.170(6) . ? C13 C14 1.446(6) . ? C14 C15 1.392(5) . ? C14 C19 1.393(6) . ? C15 C16 1.401(5) . ? C15 H15A 0.9500 . ? C16 C17 1.390(5) . ? C16 C20 1.479(5) . ? C17 C18 1.385(5) . ? C17 H17A 0.9500 . ? C18 C19 1.389(5) . ? C18 C53 1.450(6) . ? C19 H19A 0.9500 . ? C21 C22 1.484(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.494(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.476(6) . ? C26 C31 1.385(6) . ? C26 C27 1.392(5) . ? C27 C28 1.405(6) . ? C27 H27A 0.9500 . ? C28 C29 1.404(6) . ? C28 C32 1.434(6) . ? C29 C30 1.387(6) . ? C29 H29A 0.9500 . ? C30 C31 1.392(6) . ? C30 C54 1.430(6) . ? C31 H31A 0.9500 . ? C32 C33 1.197(6) . ? C33 C34 1.439(6) . ? C34 C39 1.399(6) . ? C34 C35 1.401(6) . ? C35 C36 1.379(6) . ? C35 H35A 0.9500 . ? C36 C37 1.370(6) . ? C36 H36A 0.9500 . ? C37 C38 1.384(6) . ? C37 C40 1.506(6) . ? C38 C39 1.379(6) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C41 C42 1.440(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.489(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.483(6) . ? C46 C51 1.388(5) . ? C46 C47 1.396(6) . ? C47 C48 1.373(6) . ? C47 H47A 0.9500 . ? C48 C49 1.391(5) . ? C48 H48A 0.9500 . ? C49 C50 1.405(6) . ? C49 C52 1.426(6) . ? C50 C51 1.385(5) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.184(5) . ? C54 C55 1.202(6) . ? C55 C56 1.435(6) . ? C56 C61 1.387(6) . ? C56 C57 1.402(6) . ? C57 C58 1.384(6) . ? C57 H57A 0.9500 . ? C58 C59 1.394(6) . ? C58 H58A 0.9500 . ? C59 C60 1.387(5) . ? C59 C62 1.480(6) . ? C60 C61 1.374(6) . ? C60 H60A 0.9500 . ? C61 H61A 0.9500 . ? C63 C64 1.506(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.503(6) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? 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 C2 S1 S2 102.62(17) . . ? C3 S2 S1 101.99(15) . . ? C22 S3 S4 103.58(17) . . ? C23 S4 S3 102.71(16) . . ? C42 S5 S6 102.09(19) . . ? C43 S6 S5 101.63(18) . . ? C5 O1 C4 114.7(3) . . ? C20 O4 C21 116.2(3) . . ? C25 O5 C24 116.5(4) . . ? C40 O8 C41 113.6(4) . . ? C45 O9 C44 118.1(4) . . ? C62 O12 C1 117.1(4) . . ? C64 O13 C65 112.7(4) . . ? O12 C1 C2 111.4(4) . . ? O12 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? O12 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C1 C2 S1 112.2(4) . . ? C1 C2 H2A 109.2 . . ? S1 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? S1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 S2 116.1(3) . . ? C4 C3 H3A 108.3 . . ? S2 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? S2 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? O1 C4 C3 112.8(3) . . ? O1 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? O1 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O2 C5 O1 123.3(4) . . ? O2 C5 C6 123.9(4) . . ? O1 C5 C6 112.8(4) . . ? C7 C6 C11 118.9(4) . . ? C7 C6 C5 118.0(4) . . ? C11 C6 C5 123.0(4) . . ? C8 C7 C6 120.8(4) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C7 C8 C9 120.5(4) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C8 C9 C10 118.7(4) . . ? C8 C9 C12 121.4(4) . . ? C10 C9 C12 119.9(4) . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C6 120.6(4) . . ? C10 C11 H11A 119.7 . . ? C6 C11 H11A 119.7 . . ? C13 C12 C9 176.9(5) . . ? C12 C13 C14 176.3(5) . . ? C15 C14 C19 118.9(4) . . ? C15 C14 C13 122.3(4) . . ? C19 C14 C13 118.8(4) . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 C20 118.6(4) . . ? C15 C16 C20 122.0(4) . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 118.6(4) . . ? C17 C18 C53 119.8(4) . . ? C19 C18 C53 121.5(4) . . ? C18 C19 C14 121.7(4) . . ? C18 C19 H19A 119.2 . . ? C14 C19 H19A 119.2 . . ? O3 C20 O4 123.6(4) . . ? O3 C20 C16 123.3(4) . . ? O4 C20 C16 113.1(4) . . ? O4 C21 C22 108.8(4) . . ? O4 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? O4 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? C21 C22 S3 115.4(3) . . ? C21 C22 H22A 108.4 . . ? S3 C22 H22A 108.4 . . ? C21 C22 H22B 108.4 . . ? S3 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C24 C23 S4 111.5(3) . . ? C24 C23 H23A 109.3 . . ? S4 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? S4 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? O5 C24 C23 108.3(4) . . ? O5 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? O5 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? O6 C25 O5 123.1(4) . . ? O6 C25 C26 123.9(5) . . ? O5 C25 C26 113.0(4) . . ? C31 C26 C27 120.2(4) . . ? C31 C26 C25 117.8(4) . . ? C27 C26 C25 121.9(4) . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C29 C28 C27 119.2(4) . . ? C29 C28 C32 120.5(4) . . ? C27 C28 C32 120.3(4) . . ? C30 C29 C28 120.2(4) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C31 120.2(4) . . ? C29 C30 C54 121.7(4) . . ? C31 C30 C54 118.1(4) . . ? C26 C31 C30 120.2(4) . . ? C26 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C33 C32 C28 177.7(5) . . ? C32 C33 C34 178.7(6) . . ? C39 C34 C35 119.7(4) . . ? C39 C34 C33 119.8(4) . . ? C35 C34 C33 120.5(4) . . ? C36 C35 C34 119.1(5) . . ? C36 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? C37 C36 C35 121.2(5) . . ? C37 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? C36 C37 C38 120.0(4) . . ? C36 C37 C40 117.4(4) . . ? C38 C37 C40 122.5(5) . . ? C39 C38 C37 120.3(5) . . ? C39 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C38 C39 C34 119.6(5) . . ? C38 C39 H39A 120.2 . . ? C34 C39 H39A 120.2 . . ? O7 C40 O8 123.9(5) . . ? O7 C40 C37 124.9(5) . . ? O8 C40 C37 111.2(4) . . ? C42 C41 O8 107.6(4) . . ? C42 C41 H41A 110.2 . . ? O8 C41 H41A 110.2 . . ? C42 C41 H41B 110.2 . . ? O8 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? C41 C42 S5 111.7(4) . . ? C41 C42 H42A 109.3 . . ? S5 C42 H42A 109.3 . . ? C41 C42 H42B 109.3 . . ? S5 C42 H42B 109.3 . . ? H42A C42 H42B 107.9 . . ? C44 C43 S6 112.6(4) . . ? C44 C43 H43A 109.1 . . ? S6 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? S6 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? O9 C44 C43 114.3(4) . . ? O9 C44 H44A 108.7 . . ? C43 C44 H44A 108.7 . . ? O9 C44 H44B 108.7 . . ? C43 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? O10 C45 O9 123.3(4) . . ? O10 C45 C46 125.3(4) . . ? O9 C45 C46 111.4(4) . . ? C51 C46 C47 119.1(4) . . ? C51 C46 C45 121.5(4) . . ? C47 C46 C45 119.4(4) . . ? C48 C47 C46 120.2(4) . . ? C48 C47 H47A 119.9 . . ? C46 C47 H47A 119.9 . . ? C47 C48 C49 121.5(4) . . ? C47 C48 H48A 119.2 . . ? C49 C48 H48A 119.2 . . ? C48 C49 C50 118.2(4) . . ? C48 C49 C52 121.6(4) . . ? C50 C49 C52 120.2(4) . . ? C51 C50 C49 120.3(4) . . ? C51 C50 H50A 119.9 . . ? C49 C50 H50A 119.9 . . ? C50 C51 C46 120.7(4) . . ? C50 C51 H51A 119.7 . . ? C46 C51 H51A 119.7 . . ? C53 C52 C49 178.0(5) . . ? C52 C53 C18 179.6(5) . . ? C55 C54 C30 173.0(5) . . ? C54 C55 C56 173.8(5) . . ? C61 C56 C57 119.2(4) . . ? C61 C56 C55 118.9(4) . . ? C57 C56 C55 121.9(5) . . ? C58 C57 C56 120.0(4) . . ? C58 C57 H57A 120.0 . . ? C56 C57 H57A 120.0 . . ? C57 C58 C59 120.1(4) . . ? C57 C58 H58A 119.9 . . ? C59 C58 H58A 119.9 . . ? C60 C59 C58 119.6(4) . . ? C60 C59 C62 121.9(4) . . ? C58 C59 C62 118.5(4) . . ? C61 C60 C59 120.4(5) . . ? C61 C60 H60A 119.8 . . ? C59 C60 H60A 119.8 . . ? C60 C61 C56 120.7(5) . . ? C60 C61 H61A 119.6 . . ? C56 C61 H61A 119.6 . . ? O11 C62 O12 122.7(4) . . ? O11 C62 C59 125.4(4) . . ? O12 C62 C59 111.9(4) . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O13 C64 C63 108.2(4) . . ? O13 C64 H64A 110.0 . . ? C63 C64 H64A 110.0 . . ? O13 C64 H64B 110.0 . . ? C63 C64 H64B 110.0 . . ? H64A C64 H64B 108.4 . . ? O13 C65 C66 108.7(4) . . ? O13 C65 H65A 110.0 . . ? C66 C65 H65A 110.0 . . ? O13 C65 H65B 110.0 . . ? C66 C65 H65B 110.0 . . ? H65A C65 H65B 108.3 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? 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 C2 S1 S2 C3 -100.0(2) . . . . ? C22 S3 S4 C23 96.4(2) . . . . ? C42 S5 S6 C43 -89.2(2) . . . . ? C62 O12 C1 C2 77.9(5) . . . . ? O12 C1 C2 S1 133.9(4) . . . . ? S2 S1 C2 C1 -70.6(4) . . . . ? S1 S2 C3 C4 59.4(3) . . . . ? C5 O1 C4 C3 86.2(5) . . . . ? S2 C3 C4 O1 67.3(4) . . . . ? C4 O1 C5 O2 -4.8(6) . . . . ? C4 O1 C5 C6 175.4(3) . . . . ? O2 C5 C6 C7 -0.6(7) . . . . ? O1 C5 C6 C7 179.3(4) . . . . ? O2 C5 C6 C11 177.9(5) . . . . ? O1 C5 C6 C11 -2.2(6) . . . . ? C11 C6 C7 C8 -1.3(7) . . . . ? C5 C6 C7 C8 177.3(4) . . . . ? C6 C7 C8 C9 0.2(7) . . . . ? C7 C8 C9 C10 0.8(7) . . . . ? C7 C8 C9 C12 -177.1(4) . . . . ? C8 C9 C10 C11 -0.9(7) . . . . ? C12 C9 C10 C11 177.1(4) . . . . ? C9 C10 C11 C6 -0.1(7) . . . . ? C7 C6 C11 C10 1.2(7) . . . . ? C5 C6 C11 C10 -177.3(4) . . . . ? C8 C9 C12 C13 126(10) . . . . ? C10 C9 C12 C13 -52(10) . . . . ? C9 C12 C13 C14 -12(17) . . . . ? C12 C13 C14 C15 -140(8) . . . . ? C12 C13 C14 C19 36(9) . . . . ? C19 C14 C15 C16 0.4(7) . . . . ? C13 C14 C15 C16 177.1(4) . . . . ? C14 C15 C16 C17 -2.3(7) . . . . ? C14 C15 C16 C20 177.8(4) . . . . ? C15 C16 C17 C18 2.3(6) . . . . ? C20 C16 C17 C18 -177.7(4) . . . . ? C16 C17 C18 C19 -0.4(6) . . . . ? C16 C17 C18 C53 179.4(4) . . . . ? C17 C18 C19 C14 -1.6(7) . . . . ? C53 C18 C19 C14 178.6(4) . . . . ? C15 C14 C19 C18 1.6(7) . . . . ? C13 C14 C19 C18 -175.3(4) . . . . ? C21 O4 C20 O3 -0.9(6) . . . . ? C21 O4 C20 C16 179.8(4) . . . . ? C17 C16 C20 O3 6.6(7) . . . . ? C15 C16 C20 O3 -173.5(4) . . . . ? C17 C16 C20 O4 -174.0(4) . . . . ? C15 C16 C20 O4 5.9(6) . . . . ? C20 O4 C21 C22 158.1(4) . . . . ? O4 C21 C22 S3 -64.7(5) . . . . ? S4 S3 C22 C21 -60.9(4) . . . . ? S3 S4 C23 C24 63.6(4) . . . . ? C25 O5 C24 C23 141.6(4) . . . . ? S4 C23 C24 O5 -161.3(3) . . . . ? C24 O5 C25 O6 4.3(7) . . . . ? C24 O5 C25 C26 -174.5(4) . . . . ? O6 C25 C26 C31 -3.2(7) . . . . ? O5 C25 C26 C31 175.6(4) . . . . ? O6 C25 C26 C27 175.2(5) . . . . ? O5 C25 C26 C27 -5.9(6) . . . . ? C31 C26 C27 C28 -1.1(7) . . . . ? C25 C26 C27 C28 -179.5(4) . . . . ? C26 C27 C28 C29 0.6(7) . . . . ? C26 C27 C28 C32 179.9(4) . . . . ? C27 C28 C29 C30 0.4(7) . . . . ? C32 C28 C29 C30 -178.9(4) . . . . ? C28 C29 C30 C31 -0.9(7) . . . . ? C28 C29 C30 C54 178.9(4) . . . . ? C27 C26 C31 C30 0.6(7) . . . . ? C25 C26 C31 C30 179.1(4) . . . . ? C29 C30 C31 C26 0.4(7) . . . . ? C54 C30 C31 C26 -179.4(4) . . . . ? C29 C28 C32 C33 55(15) . . . . ? C27 C28 C32 C33 -124(15) . . . . ? C28 C32 C33 C34 51(33) . . . . ? C32 C33 C34 C39 -120(23) . . . . ? C32 C33 C34 C35 59(23) . . . . ? C39 C34 C35 C36 1.9(7) . . . . ? C33 C34 C35 C36 -176.9(4) . . . . ? C34 C35 C36 C37 -1.2(7) . . . . ? C35 C36 C37 C38 -0.1(7) . . . . ? C35 C36 C37 C40 176.5(4) . . . . ? C36 C37 C38 C39 0.8(7) . . . . ? C40 C37 C38 C39 -175.7(4) . . . . ? C37 C38 C39 C34 -0.1(7) . . . . ? C35 C34 C39 C38 -1.3(7) . . . . ? C33 C34 C39 C38 177.6(4) . . . . ? C41 O8 C40 O7 -3.7(7) . . . . ? C41 O8 C40 C37 175.0(4) . . . . ? C36 C37 C40 O7 1.1(8) . . . . ? C38 C37 C40 O7 177.7(5) . . . . ? C36 C37 C40 O8 -177.6(4) . . . . ? C38 C37 C40 O8 -1.0(6) . . . . ? C40 O8 C41 C42 -178.2(4) . . . . ? O8 C41 C42 S5 -73.2(5) . . . . ? S6 S5 C42 C41 153.1(4) . . . . ? S5 S6 C43 C44 -75.9(4) . . . . ? C45 O9 C44 C43 70.6(6) . . . . ? S6 C43 C44 O9 146.8(3) . . . . ? C44 O9 C45 O10 -2.5(7) . . . . ? C44 O9 C45 C46 177.9(4) . . . . ? O10 C45 C46 C51 179.5(5) . . . . ? O9 C45 C46 C51 -0.9(6) . . . . ? O10 C45 C46 C47 -2.9(7) . . . . ? O9 C45 C46 C47 176.7(4) . . . . ? C51 C46 C47 C48 -1.8(7) . . . . ? C45 C46 C47 C48 -179.5(4) . . . . ? C46 C47 C48 C49 1.0(7) . . . . ? C47 C48 C49 C50 -0.3(7) . . . . ? C47 C48 C49 C52 -179.6(4) . . . . ? C48 C49 C50 C51 0.5(7) . . . . ? C52 C49 C50 C51 179.7(4) . . . . ? C49 C50 C51 C46 -1.3(7) . . . . ? C47 C46 C51 C50 2.0(7) . . . . ? C45 C46 C51 C50 179.6(4) . . . . ? C48 C49 C52 C53 177(100) . . . . ? C50 C49 C52 C53 -2(15) . . . . ? C49 C52 C53 C18 -24(100) . . . . ? C17 C18 C53 C52 36(100) . . . . ? C19 C18 C53 C52 -144(100) . . . . ? C29 C30 C54 C55 -162(4) . . . . ? C31 C30 C54 C55 18(5) . . . . ? C30 C54 C55 C56 5(9) . . . . ? C54 C55 C56 C61 -13(5) . . . . ? C54 C55 C56 C57 167(5) . . . . ? C61 C56 C57 C58 1.9(7) . . . . ? C55 C56 C57 C58 -178.5(4) . . . . ? C56 C57 C58 C59 -1.1(7) . . . . ? C57 C58 C59 C60 -0.3(7) . . . . ? C57 C58 C59 C62 -179.5(4) . . . . ? C58 C59 C60 C61 0.9(7) . . . . ? C62 C59 C60 C61 -180.0(4) . . . . ? C59 C60 C61 C56 -0.1(7) . . . . ? C57 C56 C61 C60 -1.4(7) . . . . ? C55 C56 C61 C60 179.1(4) . . . . ? C1 O12 C62 O11 2.0(6) . . . . ? C1 O12 C62 C59 -178.7(4) . . . . ? C60 C59 C62 O11 178.5(4) . . . . ? C58 C59 C62 O11 -2.3(7) . . . . ? C60 C59 C62 O12 -0.7(6) . . . . ? C58 C59 C62 O12 178.4(4) . . . . ? C65 O13 C64 C63 172.9(4) . . . . ? C64 O13 C65 C66 179.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.871 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.121