# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shuling Gong' _publ_contact_author_email gongsl@whu.edu.cn loop_ _publ_author_name 'Yan Li' 'Shuling Gong' # Attachment '- data 1-5.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 760511' #TrackingRef '- data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H56 O12 S4, 4 (C2H5OH), 2 (H2O)' _chemical_formula_sum 'C56 H84 O18 S4' _chemical_formula_weight 1173.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5110(13) _cell_length_b 16.749(2) _cell_length_c 18.137(2) _cell_angle_alpha 88.538(2) _cell_angle_beta 77.585(2) _cell_angle_gamma 87.949(2) _cell_volume 3115.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4243 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9575 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17971 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_sigmaI/netI 0.1356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10863 _reflns_number_gt 7702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+1.5362P] 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 10863 _refine_ls_number_parameters 741 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.2157 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.4579(4) 0.8254(3) 0.2757(2) 0.0178(9) Uani 1 1 d . . . C2 C 0.4305(4) 0.7453(3) 0.2892(2) 0.0210(10) Uani 1 1 d . . . H2 H 0.3973 0.7170 0.2530 0.025 Uiso 1 1 calc R . . C3 C 0.4500(4) 0.7047(3) 0.3545(2) 0.0242(10) Uani 1 1 d . . . C4 C 0.5026(4) 0.7476(2) 0.4049(2) 0.0185(9) Uani 1 1 d . . . H4 H 0.5201 0.7213 0.4488 0.022 Uiso 1 1 calc R . . C5 C 0.5303(4) 0.8284(2) 0.3926(2) 0.0173(9) Uani 1 1 d . . . C6 C 0.5037(4) 0.8682(2) 0.3295(2) 0.0175(9) Uani 1 1 d . . . C7 C 0.4154(5) 0.6172(3) 0.3680(3) 0.0307(11) Uani 1 1 d . . . C8 C 0.4508(7) 0.5828(3) 0.4391(4) 0.0602(19) Uani 1 1 d . . . H8A H 0.5437 0.5897 0.4367 0.090 Uiso 1 1 calc R . . H8B H 0.4322 0.5257 0.4435 0.090 Uiso 1 1 calc R . . H8C H 0.3993 0.6105 0.4831 0.090 Uiso 1 1 calc R . . C9 C 0.4881(7) 0.5677(3) 0.3004(4) 0.0625(19) Uani 1 1 d . . . H9A H 0.5822 0.5742 0.2938 0.094 Uiso 1 1 calc R . . H9B H 0.4602 0.5862 0.2545 0.094 Uiso 1 1 calc R . . H9C H 0.4682 0.5111 0.3098 0.094 Uiso 1 1 calc R . . C10 C 0.2680(6) 0.6104(4) 0.3741(4) 0.064(2) Uani 1 1 d . . . H10A H 0.2428 0.5554 0.3878 0.095 Uiso 1 1 calc R . . H10B H 0.2466 0.6251 0.3254 0.095 Uiso 1 1 calc R . . H10C H 0.2207 0.6466 0.4130 0.095 Uiso 1 1 calc R . . C11 C 0.4029(4) 0.9931(3) 0.3493(3) 0.0253(10) Uani 1 1 d . . . H11A H 0.3764 0.9833 0.4045 0.030 Uiso 1 1 calc R . . H11B H 0.3332 0.9744 0.3255 0.030 Uiso 1 1 calc R . . C12 C 0.4211(4) 1.0814(3) 0.3333(2) 0.0223(10) Uani 1 1 d . . . C13 C 0.7293(4) 0.9242(3) 0.4210(2) 0.0175(9) Uani 1 1 d . . . C14 C 0.8366(4) 0.8788(3) 0.3836(2) 0.0180(9) Uani 1 1 d . . . C15 C 0.9523(4) 0.9168(3) 0.3534(2) 0.0186(9) Uani 1 1 d . . . C16 C 0.9622(4) 0.9983(3) 0.3656(2) 0.0205(10) Uani 1 1 d . . . H16 H 1.0426 1.0233 0.3462 0.025 Uiso 1 1 calc R . . C17 C 0.8574(4) 1.0437(3) 0.4054(2) 0.0184(9) Uani 1 1 d . . . C18 C 0.7400(4) 1.0047(3) 0.4310(2) 0.0183(9) Uani 1 1 d . . . H18 H 0.6654 1.0348 0.4559 0.022 Uiso 1 1 calc R . . C19 C 0.8654(4) 1.1330(3) 0.4208(2) 0.0226(10) Uani 1 1 d . . . C20 C 0.8286(5) 1.1448(3) 0.5062(3) 0.0324(12) Uani 1 1 d . . . H20A H 0.8894 1.1136 0.5304 0.049 Uiso 1 1 calc R . . H20B H 0.7398 1.1269 0.5258 0.049 Uiso 1 1 calc R . . H20C H 0.8332 1.2016 0.5170 0.049 Uiso 1 1 calc R . . C21 C 0.7691(5) 1.1816(3) 0.3834(3) 0.0355(12) Uani 1 1 d . . . H21A H 0.7705 1.2381 0.3960 0.053 Uiso 1 1 calc R . . H21B H 0.6810 1.1619 0.4018 0.053 Uiso 1 1 calc R . . H21C H 0.7941 1.1759 0.3285 0.053 Uiso 1 1 calc R . . C22 C 1.0020(5) 1.1638(3) 0.3918(3) 0.0365(13) Uani 1 1 d . . . H22A H 1.0635 1.1336 0.4163 0.055 Uiso 1 1 calc R . . H22B H 1.0030 1.2206 0.4033 0.055 Uiso 1 1 calc R . . H22C H 1.0274 1.1569 0.3370 0.055 Uiso 1 1 calc R . . C23 C 0.8638(5) 0.7526(3) 0.4372(3) 0.0313(11) Uani 1 1 d . . . H23A H 0.8016 0.7656 0.4849 0.038 Uiso 1 1 calc R . . H23B H 0.9516 0.7678 0.4423 0.038 Uiso 1 1 calc R . . C24 C 0.8645(6) 0.6654(3) 0.4246(3) 0.0418(14) Uani 1 1 d . . . C25 C 1.0528(4) 0.8199(3) 0.2278(2) 0.0174(9) Uani 1 1 d . . . C26 C 1.0812(4) 0.7396(3) 0.2149(2) 0.0221(10) Uani 1 1 d . . . H26 H 1.1141 0.7082 0.2514 0.027 Uiso 1 1 calc R . . C27 C 1.0629(4) 0.7030(3) 0.1497(2) 0.0241(10) Uani 1 1 d . . . C28 C 1.0096(4) 0.7496(3) 0.0993(2) 0.0214(10) Uani 1 1 d . . . H28 H 0.9931 0.7256 0.0555 0.026 Uiso 1 1 calc R . . C29 C 0.9796(4) 0.8299(3) 0.1106(2) 0.0180(9) Uani 1 1 d . . . C30 C 1.0063(4) 0.8672(2) 0.1742(2) 0.0178(9) Uani 1 1 d . . . C31 C 1.0996(5) 0.6144(3) 0.1365(3) 0.0345(12) Uani 1 1 d . . . C32 C 1.0213(9) 0.5642(4) 0.2018(4) 0.076(2) Uani 1 1 d . . . H32A H 1.0434 0.5791 0.2494 0.114 Uiso 1 1 calc R . . H32B H 1.0428 0.5074 0.1928 0.114 Uiso 1 1 calc R . . H32C H 0.9279 0.5742 0.2050 0.114 Uiso 1 1 calc R . . C33 C 1.2467(7) 0.6017(4) 0.1317(4) 0.064(2) Uani 1 1 d . . . H33A H 1.2951 0.6294 0.0867 0.096 Uiso 1 1 calc R . . H33B H 1.2693 0.5445 0.1287 0.096 Uiso 1 1 calc R . . H33C H 1.2693 0.6233 0.1768 0.096 Uiso 1 1 calc R . . C34 C 1.0706(7) 0.5854(3) 0.0636(3) 0.0513(16) Uani 1 1 d . . . H34A H 0.9766 0.5905 0.0659 0.077 Uiso 1 1 calc R . . H34B H 1.0993 0.5293 0.0566 0.077 Uiso 1 1 calc R . . H34C H 1.1171 0.6177 0.0211 0.077 Uiso 1 1 calc R . . C35 C 1.1020(4) 0.9903(3) 0.1535(3) 0.0277(11) Uani 1 1 d . . . H35A H 1.1280 0.9833 0.0983 0.033 Uiso 1 1 calc R . . H35B H 1.1731 0.9676 0.1764 0.033 Uiso 1 1 calc R . . C36 C 1.0837(5) 1.0775(3) 0.1701(3) 0.0268(11) Uani 1 1 d . . . C37 C 0.7754(4) 0.9337(3) 0.0823(2) 0.0180(9) Uani 1 1 d . . . C38 C 0.6720(4) 0.8885(3) 0.1210(2) 0.0187(9) Uani 1 1 d . . . C39 C 0.5534(4) 0.9277(3) 0.1499(2) 0.0199(9) Uani 1 1 d . . . C40 C 0.5368(4) 1.0093(3) 0.1366(2) 0.0189(9) Uani 1 1 d . . . H40 H 0.4547 1.0349 0.1558 0.023 Uiso 1 1 calc R . . C41 C 0.6387(4) 1.0543(3) 0.0953(2) 0.0194(9) Uani 1 1 d . . . C42 C 0.7586(4) 1.0145(3) 0.0701(2) 0.0196(9) Uani 1 1 d . . . H42 H 0.8305 1.0440 0.0438 0.024 Uiso 1 1 calc R . . C43 C 0.6249(4) 1.1440(3) 0.0785(2) 0.0217(10) Uani 1 1 d . . . C44 C 0.7208(5) 1.1903(3) 0.1138(3) 0.0400(13) Uani 1 1 d . . . H44A H 0.6938 1.1874 0.1690 0.060 Uiso 1 1 calc R . . H44B H 0.7206 1.2463 0.0969 0.060 Uiso 1 1 calc R . . H44C H 0.8087 1.1666 0.0980 0.060 Uiso 1 1 calc R . . C45 C 0.4862(5) 1.1768(3) 0.1090(3) 0.0331(12) Uani 1 1 d . . . H45A H 0.4251 1.1492 0.0853 0.050 Uiso 1 1 calc R . . H45B H 0.4817 1.2342 0.0975 0.050 Uiso 1 1 calc R . . H45C H 0.4629 1.1680 0.1638 0.050 Uiso 1 1 calc R . . C46 C 0.6565(5) 1.1564(3) -0.0070(3) 0.0330(12) Uani 1 1 d . . . H46A H 0.7486 1.1425 -0.0270 0.050 Uiso 1 1 calc R . . H46B H 0.6392 1.2126 -0.0193 0.050 Uiso 1 1 calc R . . H46C H 0.6020 1.1223 -0.0297 0.050 Uiso 1 1 calc R . . C47 C 0.6580(5) 0.7647(3) 0.0688(3) 0.0326(12) Uani 1 1 d . . . H47A H 0.7211 0.7789 0.0218 0.039 Uiso 1 1 calc R . . H47B H 0.5696 0.7809 0.0621 0.039 Uiso 1 1 calc R . . C48 C 0.6649(5) 0.6774(3) 0.0824(3) 0.0394(13) Uani 1 1 d . . . C49 C 0.0515(9) 0.3210(5) 0.1155(5) 0.097(3) Uani 1 1 d D . . H49A H 0.0565 0.3621 0.0769 0.145 Uiso 0.51 1 d PR A 1 H49B H 0.0485 0.2691 0.0939 0.145 Uiso 0.51 1 d PR A 1 H49C H -0.0255 0.3301 0.1539 0.145 Uiso 0.51 1 d PR A 1 H49D H -0.0295 0.3491 0.1149 0.145 Uiso 0.49 1 d PR A 2 H49E H 0.1215 0.3521 0.0889 0.145 Uiso 0.49 1 d PR A 2 H49F H 0.0535 0.2701 0.0919 0.145 Uiso 0.49 1 d PR A 2 C51 C 0.6733(8) 0.4344(4) 0.1446(5) 0.080(2) Uani 1 1 d . . . H51A H 0.7526 0.4237 0.1060 0.120 Uiso 1 1 calc R . . H51B H 0.6595 0.3897 0.1810 0.120 Uiso 1 1 calc R . . H51C H 0.6828 0.4836 0.1708 0.120 Uiso 1 1 calc R . . C52 C 0.5607(9) 0.4438(5) 0.1084(5) 0.089(3) Uani 1 1 d . . . H52A H 0.5306 0.3905 0.0985 0.107 Uiso 1 1 calc R . . H52B H 0.4881 0.4723 0.1425 0.107 Uiso 1 1 calc R . . C53 C 0.4495(8) 0.3232(5) 0.3784(4) 0.075(2) Uani 1 1 d . . . H53A H 0.3932 0.3624 0.4101 0.112 Uiso 1 1 calc R B 1 H53B H 0.5401 0.3399 0.3689 0.112 Uiso 1 1 calc R B 1 H53C H 0.4426 0.2709 0.4042 0.112 Uiso 1 1 calc R B 1 C50 C 0.1718(12) 0.3251(7) 0.1497(7) 0.055(3) Uani 0.51 1 d PD C 1 H50A H 0.2506 0.3168 0.1092 0.066 Uiso 0.51 1 calc PR C 1 H50B H 0.1749 0.3794 0.1695 0.066 Uiso 0.51 1 calc PR C 1 C54 C 0.4100(10) 0.3177(5) 0.3085(5) 0.097(3) Uani 1 1 d . D 1 H54A H 0.4800 0.2922 0.2702 0.116 Uiso 1 1 calc R D 1 H54B H 0.3889 0.3715 0.2896 0.116 Uiso 1 1 calc R D 1 C50' C 0.0660(13) 0.3095(9) 0.1967(7) 0.079(5) Uani 0.49 1 d PD C 2 H50C H 0.0614 0.3627 0.2199 0.095 Uiso 0.49 1 calc PR C 2 H50D H -0.0090 0.2793 0.2248 0.095 Uiso 0.49 1 calc PR C 2 O1 O 0.5217(3) 0.95005(17) 0.32016(16) 0.0200(7) Uani 1 1 d . . . O2 O 0.5221(3) 1.11147(19) 0.3024(2) 0.0329(8) Uani 1 1 d . . . O3 O 0.3114(3) 1.1205(2) 0.3582(2) 0.0419(10) Uani 1 1 d . . . H3 H 0.3220 1.1696 0.3494 0.063 Uiso 1 1 calc R . . O4 O 0.6867(3) 0.80679(17) 0.13056(16) 0.0208(7) Uani 1 1 d . . . O5 O 0.6948(5) 0.6467(2) 0.1402(2) 0.0543(12) Uani 1 1 d . . . O6 O 0.6373(6) 0.6372(3) 0.0302(2) 0.0805(17) Uani 1 1 d . . . H6 H 0.6427 0.5883 0.0408 0.121 Uiso 1 1 calc R . . O7 O 0.9854(3) 0.94808(16) 0.18253(16) 0.0189(7) Uani 1 1 d . . . O8 O 1.1789(3) 1.1188(2) 0.1535(2) 0.0467(10) Uani 1 1 d . . . O9 O 0.9693(3) 1.10876(19) 0.19957(19) 0.0334(8) Uani 1 1 d . . . H9 H 0.9136 1.0730 0.2063 0.050 Uiso 1 1 calc R . . O10 O 0.8279(3) 0.79738(17) 0.37648(16) 0.0218(7) Uani 1 1 d . . . O11 O 0.8278(5) 0.6373(2) 0.3691(2) 0.0629(13) Uani 1 1 d . . . H11 H 0.8059 0.6750 0.3424 0.094 Uiso 1 1 calc R . . O12 O 0.9007(6) 0.6213(3) 0.4738(3) 0.0813(17) Uani 1 1 d . . . O13 O 0.7579(3) 1.03492(19) 0.24696(17) 0.0273(7) Uani 1 1 d . . . H13A H 0.7891 0.9892 0.2437 0.041 Uiso 1 1 d R . . H13B H 0.6844 1.0332 0.2737 0.041 Uiso 1 1 d R . . O14 O 0.7582(3) 0.7165(2) 0.25555(19) 0.0359(8) Uani 1 1 d . . . H14A H 0.7461 0.6889 0.2212 0.054 Uiso 1 1 d R . . H14B H 0.7469 0.7634 0.2437 0.054 Uiso 1 1 d R . . O15 O 0.1755(5) 0.2715(3) 0.2057(3) 0.0747(15) Uani 1 1 d D . . H15 H 0.1747 0.2251 0.1892 0.112 Uiso 1 1 calc R C 1 O17 O 0.5958(6) 0.4871(3) 0.0401(3) 0.0877(17) Uani 1 1 d . . . H17 H 0.5312 0.4923 0.0199 0.132 Uiso 1 1 calc R . . O18 O 0.2942(5) 0.2688(3) 0.3246(3) 0.0782(15) Uani 1 1 d . . . H18A H 0.2667 0.2637 0.2849 0.117 Uiso 1 1 calc R D 1 S1 S 0.41428(10) 0.87328(7) 0.19516(6) 0.0218(3) Uani 1 1 d . . . S2 S 0.92692(10) 0.88621(7) 0.03764(6) 0.0210(3) Uani 1 1 d . . . S3 S 1.09451(10) 0.86185(7) 0.30844(6) 0.0223(3) Uani 1 1 d . . . S4 S 0.58118(10) 0.87833(7) 0.46616(6) 0.0200(3) Uani 1 1 d . . . C55 C 0.843(3) 0.4209(17) 0.3573(15) 0.130(8) Uani 0.52 1 d PD E 1 H55A H 0.7757 0.4052 0.4008 0.195 Uiso 0.52 1 calc PR E 1 H55B H 0.8644 0.3762 0.3223 0.195 Uiso 0.52 1 calc PR E 1 H55C H 0.8118 0.4671 0.3314 0.195 Uiso 0.52 1 calc PR E 1 C56 C 0.966(2) 0.4428(15) 0.3842(10) 0.105(6) Uani 0.52 1 d PD E 1 H56A H 1.0229 0.3944 0.3826 0.126 Uiso 0.52 1 calc PR E 1 H56B H 1.0132 0.4824 0.3481 0.126 Uiso 0.52 1 calc PR E 1 O16 O 0.9444(14) 0.4733(9) 0.4551(8) 0.125(4) Uani 0.52 1 d PD E 1 H16A H 1.0141 0.4705 0.4708 0.187 Uiso 0.52 1 calc PR E 1 C55' C 0.810(2) 0.443(2) 0.343(2) 0.130(8) Uani 0.48 1 d PD F 2 H55D H 0.8562 0.4734 0.2996 0.195 Uiso 0.48 1 calc PR F 2 H55E H 0.7394 0.4759 0.3726 0.195 Uiso 0.48 1 calc PR F 2 H55F H 0.7731 0.3955 0.3255 0.195 Uiso 0.48 1 calc PR F 2 C56' C 0.9046(17) 0.4158(18) 0.3926(11) 0.105(6) Uani 0.48 1 d PD F 2 H56C H 0.8927 0.4523 0.4358 0.126 Uiso 0.48 1 calc PR F 2 H56D H 0.8813 0.3617 0.4133 0.126 Uiso 0.48 1 calc PR F 2 O16' O 1.0332(14) 0.4138(10) 0.3574(9) 0.125(4) Uani 0.48 1 d PD F 2 H16' H 1.0463 0.3791 0.3237 0.187 Uiso 0.48 1 calc PR F 2 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 0.012(2) 0.023(2) 0.019(2) 0.0044(17) -0.0036(17) -0.0078(17) C2 0.017(2) 0.025(2) 0.023(2) -0.0008(18) -0.0069(18) -0.0070(18) C3 0.022(2) 0.026(3) 0.025(2) 0.0046(19) -0.0042(19) -0.0073(19) C4 0.015(2) 0.019(2) 0.022(2) 0.0020(17) -0.0033(18) -0.0026(17) C5 0.010(2) 0.019(2) 0.021(2) -0.0016(17) 0.0004(17) -0.0024(16) C6 0.010(2) 0.019(2) 0.023(2) 0.0022(17) -0.0017(17) -0.0047(16) C7 0.039(3) 0.020(2) 0.036(3) 0.000(2) -0.012(2) -0.011(2) C8 0.101(6) 0.024(3) 0.066(4) 0.020(3) -0.040(4) -0.026(3) C9 0.097(6) 0.027(3) 0.061(4) -0.006(3) -0.011(4) -0.004(3) C10 0.058(4) 0.046(4) 0.093(5) 0.025(4) -0.029(4) -0.036(3) C11 0.018(2) 0.023(2) 0.030(3) -0.0007(19) 0.005(2) -0.0030(19) C12 0.017(2) 0.028(3) 0.021(2) 0.0040(19) -0.0033(19) 0.0004(19) C13 0.011(2) 0.025(2) 0.017(2) -0.0008(17) -0.0046(17) -0.0072(17) C14 0.018(2) 0.020(2) 0.017(2) -0.0003(17) -0.0080(18) -0.0028(18) C15 0.013(2) 0.030(3) 0.014(2) -0.0018(18) -0.0059(17) 0.0010(18) C16 0.013(2) 0.028(3) 0.021(2) -0.0006(18) -0.0044(18) -0.0057(18) C17 0.016(2) 0.022(2) 0.018(2) -0.0012(17) -0.0041(17) -0.0063(18) C18 0.013(2) 0.023(2) 0.020(2) -0.0062(18) -0.0040(17) -0.0030(17) C19 0.023(2) 0.021(2) 0.024(2) -0.0058(18) -0.0028(19) -0.0080(19) C20 0.033(3) 0.036(3) 0.030(3) -0.012(2) -0.009(2) -0.009(2) C21 0.040(3) 0.025(3) 0.044(3) 0.002(2) -0.015(3) -0.004(2) C22 0.028(3) 0.028(3) 0.051(3) -0.008(2) 0.000(2) -0.012(2) C23 0.035(3) 0.029(3) 0.033(3) 0.003(2) -0.014(2) -0.001(2) C24 0.057(4) 0.034(3) 0.038(3) 0.003(2) -0.020(3) 0.006(3) C25 0.010(2) 0.025(2) 0.016(2) -0.0012(17) -0.0006(17) 0.0004(17) C26 0.019(2) 0.021(2) 0.026(2) 0.0012(19) -0.0071(19) 0.0034(18) C27 0.019(2) 0.023(2) 0.027(2) -0.0011(19) 0.0005(19) 0.0023(19) C28 0.018(2) 0.024(2) 0.023(2) -0.0044(19) -0.0044(19) -0.0029(18) C29 0.012(2) 0.021(2) 0.019(2) 0.0026(17) 0.0007(17) -0.0021(17) C30 0.008(2) 0.019(2) 0.024(2) -0.0031(18) -0.0001(17) -0.0006(16) C31 0.050(3) 0.021(3) 0.033(3) -0.003(2) -0.011(2) 0.008(2) C32 0.120(7) 0.030(3) 0.065(5) 0.002(3) 0.004(4) 0.002(4) C33 0.066(5) 0.048(4) 0.082(5) -0.026(4) -0.025(4) 0.031(3) C34 0.069(4) 0.033(3) 0.057(4) -0.017(3) -0.025(3) 0.014(3) C35 0.016(2) 0.026(3) 0.038(3) 0.002(2) 0.001(2) -0.0067(19) C36 0.021(3) 0.026(3) 0.032(3) 0.004(2) -0.004(2) -0.008(2) C37 0.012(2) 0.026(2) 0.017(2) 0.0018(17) -0.0041(17) 0.0007(17) C38 0.021(2) 0.019(2) 0.018(2) 0.0037(17) -0.0067(18) -0.0025(18) C39 0.017(2) 0.029(3) 0.015(2) 0.0034(18) -0.0054(18) -0.0076(18) C40 0.015(2) 0.024(2) 0.018(2) 0.0027(17) -0.0041(17) -0.0011(18) C41 0.019(2) 0.025(2) 0.015(2) 0.0038(18) -0.0076(18) -0.0049(18) C42 0.015(2) 0.030(3) 0.013(2) 0.0043(18) -0.0009(17) -0.0056(18) C43 0.016(2) 0.023(2) 0.027(2) 0.0020(19) -0.0060(19) -0.0030(18) C44 0.040(3) 0.030(3) 0.055(3) 0.004(2) -0.022(3) 0.000(2) C45 0.029(3) 0.028(3) 0.038(3) 0.007(2) 0.002(2) 0.005(2) C46 0.032(3) 0.031(3) 0.034(3) 0.011(2) -0.003(2) 0.003(2) C47 0.038(3) 0.035(3) 0.032(3) -0.002(2) -0.020(2) -0.008(2) C48 0.040(3) 0.041(3) 0.042(3) -0.008(3) -0.016(3) -0.011(2) C49 0.130(8) 0.070(6) 0.105(7) -0.003(5) -0.061(6) 0.024(5) C51 0.095(6) 0.042(4) 0.093(6) -0.012(4) 0.002(5) 0.003(4) C52 0.094(7) 0.071(6) 0.100(7) 0.021(5) -0.017(5) -0.022(5) C53 0.084(6) 0.074(5) 0.081(5) -0.001(4) -0.047(4) -0.009(4) C50 0.085(10) 0.031(6) 0.054(8) 0.007(6) -0.024(7) -0.001(6) C54 0.152(9) 0.068(5) 0.081(6) 0.016(4) -0.040(6) -0.058(6) C50' 0.089(13) 0.068(11) 0.069(10) -0.034(8) 0.010(10) 0.002(9) O1 0.0137(15) 0.0171(15) 0.0281(17) 0.0020(12) -0.0016(13) -0.0043(12) O2 0.0227(18) 0.0229(18) 0.051(2) 0.0007(15) -0.0020(16) -0.0054(14) O3 0.0209(19) 0.0235(18) 0.074(3) 0.0040(18) 0.0056(18) 0.0018(14) O4 0.0195(16) 0.0196(16) 0.0255(16) 0.0030(13) -0.0100(13) -0.0028(12) O5 0.099(4) 0.025(2) 0.048(2) 0.0026(18) -0.034(2) -0.010(2) O6 0.159(5) 0.038(3) 0.061(3) -0.007(2) -0.053(3) -0.034(3) O7 0.0151(15) 0.0150(15) 0.0252(16) -0.0008(12) -0.0012(12) -0.0010(12) O8 0.027(2) 0.028(2) 0.082(3) -0.0071(19) -0.0024(19) -0.0114(16) O9 0.0215(18) 0.0252(18) 0.051(2) -0.0033(16) -0.0015(16) -0.0051(14) O10 0.0220(17) 0.0225(17) 0.0235(16) -0.0019(13) -0.0103(13) -0.0020(13) O11 0.117(4) 0.025(2) 0.055(3) 0.0039(19) -0.039(3) 0.002(2) O12 0.137(5) 0.052(3) 0.065(3) 0.013(2) -0.052(3) 0.027(3) O13 0.0189(17) 0.0326(18) 0.0289(17) -0.0023(14) -0.0013(13) -0.0012(14) O14 0.038(2) 0.0274(18) 0.043(2) -0.0042(16) -0.0108(17) -0.0021(16) O15 0.095(4) 0.043(3) 0.100(4) -0.007(3) -0.050(3) -0.007(3) O17 0.110(5) 0.070(4) 0.091(4) -0.017(3) -0.036(3) -0.018(3) O18 0.066(3) 0.037(3) 0.134(5) 0.008(3) -0.026(3) -0.013(2) S1 0.0138(6) 0.0309(6) 0.0220(6) 0.0093(5) -0.0062(4) -0.0087(4) S2 0.0160(6) 0.0277(6) 0.0181(6) 0.0037(4) -0.0013(4) 0.0007(4) S3 0.0136(5) 0.0316(6) 0.0227(6) -0.0064(5) -0.0055(4) 0.0025(4) S4 0.0161(6) 0.0251(6) 0.0184(6) -0.0034(4) -0.0009(4) -0.0080(4) C55 0.151(17) 0.092(18) 0.166(16) 0.068(13) -0.079(13) -0.053(14) C56 0.101(18) 0.101(18) 0.101(10) 0.000(9) 0.000(12) 0.000(12) O16 0.121(9) 0.121(8) 0.121(8) 0.000(6) 0.000(6) 0.000(7) C55' 0.151(17) 0.092(18) 0.166(16) 0.068(13) -0.079(13) -0.053(14) C56' 0.101(18) 0.101(18) 0.101(10) 0.000(9) 0.000(12) 0.000(12) O16' 0.121(9) 0.121(8) 0.121(8) 0.000(6) 0.000(6) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.387(6) . ? C1 C6 1.401(6) . ? C1 S1 1.785(4) . ? C2 C3 1.399(6) . ? C2 H2 0.9500 . ? C3 C4 1.392(6) . ? C3 C7 1.524(6) . ? C4 C5 1.397(6) . ? C4 H4 0.9500 . ? C5 C6 1.385(6) . ? C5 S4 1.778(4) . ? C6 O1 1.391(5) . ? C7 C8 1.511(7) . ? C7 C10 1.537(8) . ? C7 C9 1.543(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O1 1.424(5) . ? C11 C12 1.510(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O2 1.210(5) . ? C12 O3 1.303(5) . ? C13 C18 1.377(6) . ? C13 C14 1.395(6) . ? C13 S4 1.786(4) . ? C14 O10 1.382(5) . ? C14 C15 1.391(6) . ? C15 C16 1.399(6) . ? C15 S3 1.778(4) . ? C16 C17 1.392(6) . ? C16 H16 0.9500 . ? C17 C18 1.400(6) . ? C17 C19 1.538(6) . ? C18 H18 0.9500 . ? C19 C22 1.522(6) . ? C19 C20 1.530(6) . ? C19 C21 1.535(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O10 1.427(5) . ? C23 C24 1.482(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O12 1.256(6) . ? C24 O11 1.260(7) . ? C25 C26 1.383(6) . ? C25 C30 1.396(6) . ? C25 S3 1.781(4) . ? C26 C27 1.396(6) . ? C26 H26 0.9500 . ? C27 C28 1.383(6) . ? C27 C31 1.532(6) . ? C28 C29 1.380(6) . ? C28 H28 0.9500 . ? C29 C30 1.410(6) . ? C29 S2 1.778(4) . ? C30 O7 1.372(5) . ? C31 C34 1.514(7) . ? C31 C33 1.537(8) . ? C31 C32 1.540(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 O7 1.430(5) . ? C35 C36 1.495(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O8 1.217(6) . ? C36 O9 1.304(5) . ? C37 C42 1.378(6) . ? C37 C38 1.396(6) . ? C37 S2 1.792(4) . ? C38 O4 1.383(5) . ? C38 C39 1.393(6) . ? C39 C40 1.393(6) . ? C39 S1 1.784(4) . ? C40 C41 1.400(6) . ? C40 H40 0.9500 . ? C41 C42 1.395(6) . ? C41 C43 1.533(6) . ? C42 H42 0.9500 . ? C43 C46 1.526(6) . ? C43 C45 1.532(6) . ? C43 C44 1.545(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 O4 1.430(5) . ? C47 C48 1.479(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O5 1.251(6) . ? C48 O6 1.263(6) . ? C49 C50' 1.521(12) . ? C49 C50 1.529(12) . ? C49 H49A 0.9632 . ? C49 H49B 0.9670 . ? C49 H49C 0.9575 . ? C49 H49D 0.9590 . ? C49 H49E 0.9528 . ? C49 H49F 0.9614 . ? C51 C52 1.474(11) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O17 1.403(9) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.421(10) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C50 O15 1.344(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C54 O18 1.464(9) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C50' O15 1.334(11) . ? C50' H50C 0.9900 . ? C50' H50D 0.9900 . ? O3 H3 0.8400 . ? O6 H6 0.8400 . ? O9 H9 0.8400 . ? O11 H11 0.8400 . ? O13 H13A 0.8199 . ? O13 H13B 0.8199 . ? O14 H14A 0.8200 . ? O14 H14B 0.8200 . ? O15 H15 0.8400 . ? O17 H17 0.8400 . ? O18 H18A 0.8400 . ? C55 C56 1.529(10) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 O16 1.367(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? O16 H16A 0.8400 . ? C55' C56' 1.526(10) . ? C55' H55D 0.9800 . ? C55' H55E 0.9800 . ? C55' H55F 0.9800 . ? C56' O16' 1.364(10) . ? C56' H56C 0.9900 . ? C56' H56D 0.9900 . ? O16' H16' 0.8400 . ? 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 C1 C6 119.5(4) . . ? C2 C1 S1 118.2(3) . . ? C6 C1 S1 121.9(3) . . ? C1 C2 C3 122.2(4) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C4 C3 C2 117.1(4) . . ? C4 C3 C7 122.5(4) . . ? C2 C3 C7 120.4(4) . . ? C3 C4 C5 121.7(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 S4 122.6(3) . . ? C4 C5 S4 116.9(3) . . ? C5 C6 O1 120.1(4) . . ? C5 C6 C1 119.3(4) . . ? O1 C6 C1 120.6(4) . . ? C8 C7 C3 112.5(4) . . ? C8 C7 C10 109.2(5) . . ? C3 C7 C10 108.5(4) . . ? C8 C7 C9 108.5(5) . . ? C3 C7 C9 109.5(4) . . ? C10 C7 C9 108.6(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 109.8(3) . . ? O1 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O1 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O2 C12 O3 124.9(4) . . ? O2 C12 C11 125.3(4) . . ? O3 C12 C11 109.8(4) . . ? C18 C13 C14 120.3(4) . . ? C18 C13 S4 118.1(3) . . ? C14 C13 S4 121.3(3) . . ? O10 C14 C15 120.5(4) . . ? O10 C14 C13 120.4(4) . . ? C15 C14 C13 119.0(4) . . ? C14 C15 C16 119.8(4) . . ? C14 C15 S3 121.2(3) . . ? C16 C15 S3 118.6(3) . . ? C17 C16 C15 121.7(4) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 117.1(4) . . ? C16 C17 C19 123.1(4) . . ? C18 C17 C19 119.8(4) . . ? C13 C18 C17 121.9(4) . . ? C13 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C22 C19 C20 108.1(4) . . ? C22 C19 C21 109.2(4) . . ? C20 C19 C21 109.1(4) . . ? C22 C19 C17 112.2(4) . . ? C20 C19 C17 108.3(4) . . ? C21 C19 C17 109.8(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O10 C23 C24 111.4(4) . . ? O10 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? O10 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? O12 C24 O11 122.1(5) . . ? O12 C24 C23 115.8(5) . . ? O11 C24 C23 122.1(5) . . ? C26 C25 C30 119.8(4) . . ? C26 C25 S3 118.0(3) . . ? C30 C25 S3 121.9(3) . . ? C25 C26 C27 122.0(4) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C28 C27 C26 117.4(4) . . ? C28 C27 C31 122.2(4) . . ? C26 C27 C31 120.3(4) . . ? C29 C28 C27 122.0(4) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 119.9(4) . . ? C28 C29 S2 118.2(3) . . ? C30 C29 S2 121.4(3) . . ? O7 C30 C25 121.6(4) . . ? O7 C30 C29 119.9(4) . . ? C25 C30 C29 118.6(4) . . ? C34 C31 C27 112.6(4) . . ? C34 C31 C33 107.6(5) . . ? C27 C31 C33 108.9(5) . . ? C34 C31 C32 107.8(5) . . ? C27 C31 C32 109.3(4) . . ? C33 C31 C32 110.6(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O7 C35 C36 111.5(4) . . ? O7 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? O7 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? O8 C36 O9 120.9(4) . . ? O8 C36 C35 117.7(4) . . ? O9 C36 C35 121.4(4) . . ? C42 C37 C38 120.7(4) . . ? C42 C37 S2 118.1(3) . . ? C38 C37 S2 120.8(3) . . ? O4 C38 C39 120.6(4) . . ? O4 C38 C37 120.9(4) . . ? C39 C38 C37 118.5(4) . . ? C40 C39 C38 120.4(4) . . ? C40 C39 S1 118.3(3) . . ? C38 C39 S1 121.0(3) . . ? C39 C40 C41 121.3(4) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 117.3(4) . . ? C42 C41 C43 119.5(4) . . ? C40 C41 C43 123.2(4) . . ? C37 C42 C41 121.8(4) . . ? C37 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C46 C43 C45 108.1(4) . . ? C46 C43 C41 108.0(4) . . ? C45 C43 C41 112.1(4) . . ? C46 C43 C44 109.8(4) . . ? C45 C43 C44 109.0(4) . . ? C41 C43 C44 109.9(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O4 C47 C48 110.8(4) . . ? O4 C47 H47A 109.5 . . ? C48 C47 H47A 109.5 . . ? O4 C47 H47B 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 108.1 . . ? O5 C48 O6 123.6(5) . . ? O5 C48 C47 122.9(5) . . ? O6 C48 C47 113.5(5) . . ? C50' C49 C50 49.6(8) . . ? C50' C49 H49A 140.4 . . ? C50 C49 H49A 108.3 . . ? C50' C49 H49B 108.7 . . ? C50 C49 H49B 110.0 . . ? H49A C49 H49B 110.1 . . ? C50' C49 H49C 63.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.4 . . ? H49B C49 H49C 109.5 . . ? C50' C49 H49D 109.2 . . ? C50 C49 H49D 141.0 . . ? H49A C49 H49D 65.4 . . ? H49B C49 H49D 107.9 . . ? H49C C49 H49D 47.8 . . ? C50' C49 H49E 108.6 . . ? C50 C49 H49E 62.7 . . ? H49A C49 H49E 47.5 . . ? H49B C49 H49E 113.2 . . ? H49C C49 H49E 136.5 . . ? H49D C49 H49E 109.1 . . ? C50' C49 H49F 110.2 . . ? C50 C49 H49F 108.4 . . ? H49A C49 H49F 108.1 . . ? H49C C49 H49F 113.0 . . ? H49D C49 H49F 110.0 . . ? H49E C49 H49F 109.7 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O17 C52 C51 110.0(7) . . ? O17 C52 H52A 109.7 . . ? C51 C52 H52A 109.7 . . ? O17 C52 H52B 109.7 . . ? C51 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? O15 C50 C49 114.3(8) . . ? O15 C50 H49E 150.5 . . ? O15 C50 H50A 108.7 . . ? C49 C50 H50A 108.7 . . ? H49E C50 H50A 81.3 . . ? O15 C50 H50B 108.7 . . ? C49 C50 H50B 108.7 . . ? H49E C50 H50B 93.7 . . ? H50A C50 H50B 107.6 . . ? C53 C54 O18 105.6(6) . . ? C53 C54 H54A 110.6 . . ? O18 C54 H54A 110.6 . . ? C53 C54 H54B 110.6 . . ? O18 C54 H54B 110.6 . . ? H54A C54 H54B 108.8 . . ? O15 C50' C49 115.4(8) . . ? O15 C50' H49C 151.4 . . ? O15 C50' H50C 108.4 . . ? C49 C50' H50C 108.4 . . ? H49C C50' H50C 94.1 . . ? O15 C50' H50D 108.4 . . ? C49 C50' H50D 108.4 . . ? H49C C50' H50D 80.1 . . ? H50C C50' H50D 107.5 . . ? C6 O1 C11 110.3(3) . . ? C12 O3 H3 109.5 . . ? C38 O4 C47 111.4(3) . . ? C48 O6 H6 109.5 . . ? C30 O7 C35 111.3(3) . . ? C36 O9 H9 109.5 . . ? C14 O10 C23 112.7(3) . . ? C24 O11 H11 109.5 . . ? H9 O13 H13A 90.2 . . ? H9 O13 H13B 158.6 . . ? H13A O13 H13B 107.7 . . ? H14A O14 H14B 107.7 . . ? C50' O15 C50 57.0(9) . . ? C50' O15 H15 107.2 . . ? C50 O15 H15 109.5 . . ? C52 O17 H17 109.5 . . ? C54 O18 H18A 109.5 . . ? C39 S1 C1 105.60(19) . . ? C29 S2 C37 105.30(19) . . ? C15 S3 C25 104.96(19) . . ? C5 S4 C13 104.67(19) . . ? O16 C56 C55 115.5(11) . . ? O16 C56 H56A 108.4 . . ? C55 C56 H56A 108.4 . . ? O16 C56 H56B 108.4 . . ? C55 C56 H56B 108.4 . . ? H56A C56 H56B 107.5 . . ? C56 O16 H16A 109.5 . . ? C56' C55' H55D 109.5 . . ? C56' C55' H55E 109.5 . . ? H55D C55' H55E 109.5 . . ? C56' C55' H55F 109.5 . . ? H55D C55' H55F 109.5 . . ? H55E C55' H55F 109.5 . . ? O16' C56' C55' 115.5(11) . . ? O16' C56' H56C 108.4 . . ? C55' C56' H56C 108.4 . . ? O16' C56' H56D 108.4 . . ? C55' C56' H56D 108.4 . . ? H56C C56' H56D 107.5 . . ? C56' O16' H16' 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 C6 C1 C2 C3 -1.7(6) . . . . ? S1 C1 C2 C3 -174.0(3) . . . . ? C1 C2 C3 C4 -2.0(6) . . . . ? C1 C2 C3 C7 178.5(4) . . . . ? C2 C3 C4 C5 2.3(6) . . . . ? C7 C3 C4 C5 -178.2(4) . . . . ? C3 C4 C5 C6 1.0(6) . . . . ? C3 C4 C5 S4 173.7(3) . . . . ? C4 C5 C6 O1 175.0(4) . . . . ? S4 C5 C6 O1 2.7(5) . . . . ? C4 C5 C6 C1 -4.7(6) . . . . ? S4 C5 C6 C1 -176.9(3) . . . . ? C2 C1 C6 C5 5.0(6) . . . . ? S1 C1 C6 C5 177.0(3) . . . . ? C2 C1 C6 O1 -174.6(4) . . . . ? S1 C1 C6 O1 -2.6(6) . . . . ? C4 C3 C7 C8 -2.8(7) . . . . ? C2 C3 C7 C8 176.7(5) . . . . ? C4 C3 C7 C10 118.1(5) . . . . ? C2 C3 C7 C10 -62.4(6) . . . . ? C4 C3 C7 C9 -123.6(5) . . . . ? C2 C3 C7 C9 55.9(6) . . . . ? O1 C11 C12 O2 -2.0(7) . . . . ? O1 C11 C12 O3 178.3(4) . . . . ? C18 C13 C14 O10 177.1(4) . . . . ? S4 C13 C14 O10 4.3(5) . . . . ? C18 C13 C14 C15 -3.2(6) . . . . ? S4 C13 C14 C15 -176.0(3) . . . . ? O10 C14 C15 C16 -175.7(4) . . . . ? C13 C14 C15 C16 4.6(6) . . . . ? O10 C14 C15 S3 -2.8(5) . . . . ? C13 C14 C15 S3 177.5(3) . . . . ? C14 C15 C16 C17 -2.1(6) . . . . ? S3 C15 C16 C17 -175.2(3) . . . . ? C15 C16 C17 C18 -1.9(6) . . . . ? C15 C16 C17 C19 179.2(4) . . . . ? C14 C13 C18 C17 -0.9(6) . . . . ? S4 C13 C18 C17 172.2(3) . . . . ? C16 C17 C18 C13 3.4(6) . . . . ? C19 C17 C18 C13 -177.6(4) . . . . ? C16 C17 C19 C22 -3.5(6) . . . . ? C18 C17 C19 C22 177.5(4) . . . . ? C16 C17 C19 C20 -122.8(4) . . . . ? C18 C17 C19 C20 58.3(5) . . . . ? C16 C17 C19 C21 118.1(5) . . . . ? C18 C17 C19 C21 -60.8(5) . . . . ? O10 C23 C24 O12 177.0(5) . . . . ? O10 C23 C24 O11 -4.8(8) . . . . ? C30 C25 C26 C27 -1.0(6) . . . . ? S3 C25 C26 C27 -174.1(3) . . . . ? C25 C26 C27 C28 -2.7(7) . . . . ? C25 C26 C27 C31 178.1(4) . . . . ? C26 C27 C28 C29 2.4(7) . . . . ? C31 C27 C28 C29 -178.4(4) . . . . ? C27 C28 C29 C30 1.5(6) . . . . ? C27 C28 C29 S2 173.8(3) . . . . ? C26 C25 C30 O7 -175.5(4) . . . . ? S3 C25 C30 O7 -2.6(6) . . . . ? C26 C25 C30 C29 5.0(6) . . . . ? S3 C25 C30 C29 177.8(3) . . . . ? C28 C29 C30 O7 175.2(4) . . . . ? S2 C29 C30 O7 3.2(5) . . . . ? C28 C29 C30 C25 -5.2(6) . . . . ? S2 C29 C30 C25 -177.2(3) . . . . ? C28 C27 C31 C34 -0.2(7) . . . . ? C26 C27 C31 C34 179.0(5) . . . . ? C28 C27 C31 C33 119.2(5) . . . . ? C26 C27 C31 C33 -61.7(6) . . . . ? C28 C27 C31 C32 -120.0(6) . . . . ? C26 C27 C31 C32 59.2(7) . . . . ? O7 C35 C36 O8 174.4(4) . . . . ? O7 C35 C36 O9 -7.3(6) . . . . ? C42 C37 C38 O4 177.2(4) . . . . ? S2 C37 C38 O4 4.7(6) . . . . ? C42 C37 C38 C39 -2.9(6) . . . . ? S2 C37 C38 C39 -175.4(3) . . . . ? O4 C38 C39 C40 -176.4(4) . . . . ? C37 C38 C39 C40 3.6(6) . . . . ? O4 C38 C39 S1 -3.8(6) . . . . ? C37 C38 C39 S1 176.3(3) . . . . ? C38 C39 C40 C41 -1.3(6) . . . . ? S1 C39 C40 C41 -174.1(3) . . . . ? C39 C40 C41 C42 -1.9(6) . . . . ? C39 C40 C41 C43 179.4(4) . . . . ? C38 C37 C42 C41 -0.3(6) . . . . ? S2 C37 C42 C41 172.4(3) . . . . ? C40 C41 C42 C37 2.7(6) . . . . ? C43 C41 C42 C37 -178.5(4) . . . . ? C42 C41 C43 C46 59.9(5) . . . . ? C40 C41 C43 C46 -121.4(4) . . . . ? C42 C41 C43 C45 178.8(4) . . . . ? C40 C41 C43 C45 -2.5(6) . . . . ? C42 C41 C43 C44 -59.9(5) . . . . ? C40 C41 C43 C44 118.9(5) . . . . ? O4 C47 C48 O5 -1.4(8) . . . . ? O4 C47 C48 O6 178.5(5) . . . . ? C50' C49 C50 O15 37.1(9) . . . . ? C50 C49 C50' O15 -37.8(9) . . . . ? C5 C6 O1 C11 -93.8(4) . . . . ? C1 C6 O1 C11 85.8(5) . . . . ? C12 C11 O1 C6 -175.5(3) . . . . ? C39 C38 O4 C47 91.5(5) . . . . ? C37 C38 O4 C47 -88.6(5) . . . . ? C48 C47 O4 C38 -175.9(4) . . . . ? C25 C30 O7 C35 85.8(5) . . . . ? C29 C30 O7 C35 -94.6(4) . . . . ? C36 C35 O7 C30 -173.7(4) . . . . ? C15 C14 O10 C23 89.4(5) . . . . ? C13 C14 O10 C23 -90.9(5) . . . . ? C24 C23 O10 C14 -175.1(4) . . . . ? C49 C50' O15 C50 39.3(9) . . . . ? C49 C50 O15 C50' -38.6(9) . . . . ? C40 C39 S1 C1 -125.0(3) . . . . ? C38 C39 S1 C1 62.3(4) . . . . ? C2 C1 S1 C39 -133.7(3) . . . . ? C6 C1 S1 C39 54.2(4) . . . . ? C28 C29 S2 C37 126.4(3) . . . . ? C30 C29 S2 C37 -61.4(4) . . . . ? C42 C37 S2 C29 130.6(3) . . . . ? C38 C37 S2 C29 -56.7(4) . . . . ? C14 C15 S3 C25 64.0(4) . . . . ? C16 C15 S3 C25 -123.0(3) . . . . ? C26 C25 S3 C15 -131.9(3) . . . . ? C30 C25 S3 C15 55.1(4) . . . . ? C6 C5 S4 C13 -59.9(4) . . . . ? C4 C5 S4 C13 127.7(3) . . . . ? C18 C13 S4 C5 127.4(3) . . . . ? C14 C13 S4 C5 -59.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O18 H18A O15 0.84 1.89 2.713(7) 166.3 . O14 H14B O4 0.82 2.36 2.909(4) 124.6 . O14 H14A O5 0.82 1.84 2.641(5) 166.7 . O13 H13B O2 0.82 2.10 2.751(4) 136.7 . O13 H13B O1 0.82 2.25 2.948(4) 142.9 . O13 H13A O7 0.82 2.22 2.799(4) 128.1 . O11 H11 O14 0.84 1.87 2.641(5) 152.9 . O9 H9 O13 0.84 1.78 2.554(4) 152.9 . O6 H6 O17 0.84 1.78 2.563(7) 153.6 . O16 H16A O16 0.84 1.80 2.40(3) 127.8 2_766 O16 H16A O12 0.84 2.10 2.728(15) 131.8 2_766 O15 H15 O8 0.84 1.91 2.745(6) 177.7 1_445 O3 H3 O18 0.84 1.74 2.552(5) 161.4 1_565 C22 H22A O3 0.98 2.60 3.236(6) 123.1 1_655 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.194 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.097 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 832089' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H56 O12 S4, 2 (C3H6O), 2 (H2O)' _chemical_formula_sum 'C54 H72 O16 S4' _chemical_formula_weight 1105.40 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 monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.501(8) _cell_length_b 30.32(2) _cell_length_c 18.838(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.453(15) _cell_angle_gamma 90.00 _cell_volume 5879(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2048 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 17.92 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2348 _exptl_absorpt_coefficient_mu 0.225 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9648 _exptl_absorpt_correction_T_max 0.9778 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28197 _diffrn_reflns_av_R_equivalents 0.1160 _diffrn_reflns_av_sigmaI/netI 0.1406 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10260 _reflns_number_gt 6803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Several commands for restraints (including DFIX, SADI, SIMU, ISOR and FlAT commands) were applied on the atoms, the details are as follows: DFIX 0.82 0.01 O13 H13A O13 H13B O14 H14A O14 H14B O12 H12 DFIX 1.35 0.02 H13A H13B H14A H14B DFIX 1.54 0.01 C52 C53 C54 C53 DFIX 2.45 0.02 C52 C54 DFIX 1.28 0.01 C53 O16 SADI 0.01 C52 O16 C54 O16 simu 0.01 C9 C10 C11 C12 simu 0.01 C33 C34 C35 C36 simu 0.01 C45 C46 C47 C48 simu 0.01 3.8 $C isor 0.01 0.01 C52 C53 C54 FLAT C52 C53 C54 O16 ; _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^)+(0.1140P)^2^+1.3103P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.18(14) _refine_ls_number_reflns 10260 _refine_ls_number_parameters 702 _refine_ls_number_restraints 320 _refine_ls_R_factor_all 0.1585 _refine_ls_R_factor_gt 0.1143 _refine_ls_wR_factor_ref 0.2646 _refine_ls_wR_factor_gt 0.2411 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2216(7) 0.3550(3) 0.9729(4) 0.0290(18) Uani 1 1 d U . . C6 C 0.2664(8) 0.3338(3) 0.9212(5) 0.0336(18) Uani 1 1 d U . . C5 C 0.2926(8) 0.3557(3) 0.8611(5) 0.0344(19) Uani 1 1 d U . . C4 C 0.2667(8) 0.4007(3) 0.8577(5) 0.043(2) Uani 1 1 d U . . H4 H 0.2856 0.4163 0.8185 0.052 Uiso 1 1 calc R . . C3 C 0.2162(9) 0.4232(3) 0.9069(5) 0.043(2) Uani 1 1 d U . . C2 C 0.2005(9) 0.3998(3) 0.9662(5) 0.041(2) Uani 1 1 d U . . H2 H 0.1743 0.4147 1.0040 0.049 Uiso 1 1 calc R . . C11 C 0.1574(10) 0.2659(4) 0.8927(6) 0.057(3) Uani 1 1 d U . . H11A H 0.1252 0.2768 0.8440 0.069 Uiso 1 1 calc R . . H11B H 0.0933 0.2727 0.9218 0.069 Uiso 1 1 calc R . . C12 C 0.1774(10) 0.2170(4) 0.8908(6) 0.053(2) Uani 1 1 d U . . C7 C 0.1846(11) 0.4733(4) 0.8965(6) 0.058(3) Uani 1 1 d U . . C10 C 0.0473(16) 0.4811(6) 0.9015(10) 0.124(7) Uani 1 1 d U . . H10A H 0.0201 0.4589 0.9316 0.185 Uiso 1 1 calc R . . H10B H -0.0065 0.4798 0.8539 0.185 Uiso 1 1 calc R . . H10C H 0.0392 0.5097 0.9221 0.185 Uiso 1 1 calc R . . C8 C 0.2335(18) 0.4943(5) 0.8384(9) 0.115(6) Uani 1 1 d U . . H8A H 0.3252 0.4992 0.8533 0.173 Uiso 1 1 calc R . . H8B H 0.1902 0.5221 0.8269 0.173 Uiso 1 1 calc R . . H8C H 0.2174 0.4756 0.7964 0.173 Uiso 1 1 calc R . . C9 C 0.239(2) 0.4978(5) 0.9662(9) 0.127(7) Uani 1 1 d U . . H9A H 0.3241 0.5089 0.9644 0.190 Uiso 1 1 calc R . . H9B H 0.2450 0.4781 1.0066 0.190 Uiso 1 1 calc R . . H9C H 0.1829 0.5220 0.9718 0.190 Uiso 1 1 calc R . . C13 C 0.4898(8) 0.3007(3) 0.8255(5) 0.0353(19) Uani 1 1 d U . . C18 C 0.4978(7) 0.2558(3) 0.8122(5) 0.038(2) Uani 1 1 d U . . H18 H 0.4227 0.2412 0.7897 0.045 Uiso 1 1 calc R . . C17 C 0.6130(8) 0.2315(3) 0.8307(4) 0.0387(19) Uani 1 1 d U . . C16 C 0.7228(8) 0.2559(3) 0.8721(5) 0.039(2) Uani 1 1 d U . . H16 H 0.8023 0.2418 0.8868 0.046 Uiso 1 1 calc R . . C15 C 0.7104(8) 0.2996(3) 0.8897(4) 0.0320(18) Uani 1 1 d U . . C14 C 0.5957(9) 0.3228(3) 0.8661(5) 0.0331(18) Uani 1 1 d U . . C23 C 0.6178(16) 0.3948(4) 0.8212(7) 0.085(4) Uani 1 1 d U . . H23A H 0.5479 0.3924 0.7792 0.102 Uiso 1 1 calc R . . H23B H 0.6963 0.3837 0.8077 0.102 Uiso 1 1 calc R . . C24 C 0.6373(17) 0.4434(5) 0.8418(9) 0.095(4) Uani 1 1 d U . . C19 C 0.6235(8) 0.1840(3) 0.8106(5) 0.038(2) Uani 1 1 d U . . C22 C 0.7553(11) 0.1639(4) 0.8392(8) 0.088(5) Uani 1 1 d U . . H22A H 0.7839 0.1718 0.8891 0.132 Uiso 1 1 calc R . . H22B H 0.8165 0.1746 0.8115 0.132 Uiso 1 1 calc R . . H22C H 0.7494 0.1323 0.8350 0.132 Uiso 1 1 calc R . . C20 C 0.5942(12) 0.1808(3) 0.7278(5) 0.057(3) Uani 1 1 d U . . H20A H 0.6063 0.1509 0.7136 0.085 Uiso 1 1 calc R . . H20B H 0.6519 0.1998 0.7084 0.085 Uiso 1 1 calc R . . H20C H 0.5059 0.1896 0.7094 0.085 Uiso 1 1 calc R . . C21 C 0.5267(12) 0.1559(4) 0.8397(7) 0.069(3) Uani 1 1 d U . . H21A H 0.5397 0.1595 0.8913 0.103 Uiso 1 1 calc R . . H21B H 0.5389 0.1255 0.8285 0.103 Uiso 1 1 calc R . . H21C H 0.4401 0.1649 0.8178 0.103 Uiso 1 1 calc R . . C25 C 0.8135(8) 0.3479(3) 1.0178(5) 0.0347(19) Uani 1 1 d U . . C30 C 0.7641(7) 0.3207(3) 1.0672(5) 0.0261(18) Uani 1 1 d U . . C29 C 0.7435(7) 0.3401(3) 1.1289(4) 0.0293(18) Uani 1 1 d U . . C28 C 0.7750(8) 0.3836(3) 1.1469(4) 0.0313(18) Uani 1 1 d U . . H28 H 0.7577 0.3954 1.1895 0.038 Uiso 1 1 calc R . . C27 C 0.8315(9) 0.4091(3) 1.1019(4) 0.0394(19) Uani 1 1 d U . . C26 C 0.8501(9) 0.3924(3) 1.0364(5) 0.041(2) Uani 1 1 d U . . H26 H 0.8860 0.4099 1.0049 0.049 Uiso 1 1 calc R . . C35 C 0.8566(10) 0.2502(4) 1.0735(8) 0.077(3) Uani 1 1 d U . . H35A H 0.8850 0.2527 1.1255 0.092 Uiso 1 1 calc R . . H35B H 0.9261 0.2609 1.0511 0.092 Uiso 1 1 calc R . . C36 C 0.8327(11) 0.2040(4) 1.0547(8) 0.085(4) Uani 1 1 d U . . C31 C 0.8759(10) 0.4581(4) 1.1224(5) 0.053(2) Uani 1 1 d U . . C34 C 0.8453(17) 0.4727(4) 1.1931(8) 0.100(5) Uani 1 1 d U . . H34A H 0.8878 0.5002 1.2072 0.150 Uiso 1 1 calc R . . H34B H 0.8754 0.4509 1.2295 0.150 Uiso 1 1 calc R . . H34C H 0.7531 0.4763 1.1879 0.150 Uiso 1 1 calc R . . C33 C 1.0261(13) 0.4594(5) 1.1378(8) 0.092(5) Uani 1 1 d U . . H33A H 1.0570 0.4467 1.0978 0.139 Uiso 1 1 calc R . . H33B H 1.0596 0.4430 1.1810 0.139 Uiso 1 1 calc R . . H33C H 1.0550 0.4895 1.1441 0.139 Uiso 1 1 calc R . . C32 C 0.8339(19) 0.4886(5) 1.0630(8) 0.125(7) Uani 1 1 d U . . H32A H 0.8757 0.5166 1.0745 0.188 Uiso 1 1 calc R . . H32B H 0.7414 0.4923 1.0554 0.188 Uiso 1 1 calc R . . H32C H 0.8569 0.4771 1.0198 0.188 Uiso 1 1 calc R . . C37 C 0.5337(8) 0.2875(3) 1.1535(4) 0.0303(18) Uani 1 1 d U . . C42 C 0.5061(9) 0.2432(3) 1.1657(5) 0.0355(19) Uani 1 1 d U . . H42 H 0.5722 0.2257 1.1915 0.043 Uiso 1 1 calc R . . C41 C 0.3841(8) 0.2240(3) 1.1412(5) 0.0341(18) Uani 1 1 d U . . C40 C 0.2936(8) 0.2514(3) 1.1010(4) 0.0320(19) Uani 1 1 d U . . H40 H 0.2142 0.2394 1.0788 0.038 Uiso 1 1 calc R . . C39 C 0.3132(8) 0.2952(3) 1.0917(4) 0.0305(18) Uani 1 1 d U . . C38 C 0.4307(9) 0.3151(3) 1.1199(5) 0.0303(18) Uani 1 1 d U . . C47 C 0.4231(10) 0.3819(3) 1.1768(6) 0.053(2) Uani 1 1 d U . . H47A H 0.4879 0.3743 1.2193 0.063 Uiso 1 1 calc R . . H47B H 0.3386 0.3729 1.1850 0.063 Uiso 1 1 calc R . . C48 C 0.4244(12) 0.4311(4) 1.1633(7) 0.061(3) Uani 1 1 d U . . C43 C 0.3592(10) 0.1753(3) 1.1557(6) 0.052(3) Uani 1 1 d U . . C46 C 0.4437(17) 0.1598(5) 1.2267(9) 0.124(7) Uani 1 1 d U . . H46A H 0.4540 0.1834 1.2613 0.186 Uiso 1 1 calc R . . H46B H 0.5273 0.1511 1.2184 0.186 Uiso 1 1 calc R . . H46C H 0.4028 0.1351 1.2451 0.186 Uiso 1 1 calc R . . C45 C 0.2275(14) 0.1653(5) 1.1588(10) 0.114(6) Uani 1 1 d U . . H45A H 0.2203 0.1345 1.1694 0.171 Uiso 1 1 calc R . . H45B H 0.1723 0.1719 1.1130 0.171 Uiso 1 1 calc R . . H45C H 0.2013 0.1825 1.1962 0.171 Uiso 1 1 calc R . . C44 C 0.379(2) 0.1499(5) 1.0925(8) 0.123(6) Uani 1 1 d U . . H44A H 0.4702 0.1486 1.0919 0.185 Uiso 1 1 calc R . . H44B H 0.3339 0.1640 1.0490 0.185 Uiso 1 1 calc R . . H44C H 0.3460 0.1206 1.0951 0.185 Uiso 1 1 calc R . . C49 C 0.4708(17) 0.5631(5) 0.1155(9) 0.115(5) Uani 1 1 d U . . H49A H 0.5444 0.5605 0.1547 0.172 Uiso 1 1 calc R . . H49B H 0.4752 0.5906 0.0909 0.172 Uiso 1 1 calc R . . H49C H 0.4712 0.5392 0.0821 0.172 Uiso 1 1 calc R . . C50 C 0.3449(15) 0.5615(4) 0.1456(9) 0.083(4) Uani 1 1 d U . . C51 C 0.247(2) 0.5915(6) 0.1123(12) 0.161(9) Uani 1 1 d U . . H51A H 0.1708 0.5875 0.1321 0.242 Uiso 1 1 calc R . . H51B H 0.2271 0.5861 0.0611 0.242 Uiso 1 1 calc R . . H51C H 0.2785 0.6211 0.1211 0.242 Uiso 1 1 calc R . . C52 C 0.103(2) 0.0703(6) 0.9540(9) 0.161(8) Uani 1 1 d DU . . H52A H 0.0366 0.0899 0.9632 0.241 Uiso 1 1 calc R . . H52B H 0.1724 0.0692 0.9959 0.241 Uiso 1 1 calc R . . H52C H 0.0677 0.0413 0.9439 0.241 Uiso 1 1 calc R . . C53 C 0.1556(15) 0.0867(5) 0.8899(8) 0.209(12) Uani 1 1 d DU . . C54 C 0.2884(16) 0.0679(7) 0.8934(12) 0.207(12) Uani 1 1 d DU . . H54A H 0.3285 0.0819 0.8578 0.310 Uiso 1 1 calc R . . H54B H 0.2816 0.0367 0.8839 0.310 Uiso 1 1 calc R . . H54C H 0.3403 0.0728 0.9407 0.310 Uiso 1 1 calc R . . H13A H 0.50(3) 0.251(7) 0.021(12) 0.310 Uiso 1 1 d D . . H14A H 0.53(3) 0.410(11) 0.041(5) 0.310 Uiso 1 1 d D . . H13B H 0.47(3) 0.211(4) -0.008(16) 0.310 Uiso 1 1 d D . . H14B H 0.620(7) 0.418(10) 0.001(17) 0.310 Uiso 1 1 d D . . O1 O 0.2787(6) 0.2871(2) 0.9231(4) 0.0444(16) Uani 1 1 d . . . O2 O 0.2751(7) 0.1979(2) 0.9160(5) 0.067(2) Uani 1 1 d . . . O3 O 0.0720(7) 0.1988(2) 0.8580(5) 0.068(2) Uani 1 1 d . . . H3 H 0.0827 0.1720 0.8564 0.102 Uiso 1 1 calc R . . O10 O 0.4508(5) 0.36000(19) 1.1149(3) 0.0356(15) Uani 1 1 d . . . O11 O 0.4474(12) 0.4487(3) 1.1143(5) 0.109(4) Uani 1 1 d . . . O12 O 0.3969(12) 0.4513(3) 1.2194(5) 0.098(3) Uani 1 1 d . . . H12A H 0.4353 0.4750 1.2250 0.147 Uiso 1 1 calc R . . O7 O 0.7439(5) 0.27712(19) 1.0508(3) 0.0380(15) Uani 1 1 d . . . O9 O 0.7180(9) 0.1894(3) 1.0257(7) 0.109(4) Uani 1 1 d . . . H9 H 0.6627 0.2055 1.0372 0.164 Uiso 1 1 calc R . . O8 O 0.9300(9) 0.1792(3) 1.0620(9) 0.154(6) Uani 1 1 d . . . O4 O 0.5876(6) 0.3679(2) 0.8783(3) 0.0468(17) Uani 1 1 d . . . O5 O 0.6093(17) 0.4543(4) 0.9023(7) 0.127(5) Uani 1 1 d . . . O6 O 0.6708(15) 0.4672(4) 0.7992(6) 0.142(5) Uani 1 1 d . . . O13 O 0.5077(8) 0.2342(3) -0.0114(4) 0.0592(18) Uani 1 1 d D . . O14 O 0.5332(7) 0.4121(3) -0.0033(5) 0.072(2) Uani 1 1 d D . . O15 O 0.3304(13) 0.5366(3) 0.1900(7) 0.124(4) Uani 1 1 d . . . O16 O 0.1007(14) 0.1139(4) 0.8462(6) 0.185(8) Uani 1 1 d D . . S1 S 0.1772(2) 0.32850(8) 1.04945(12) 0.0402(6) Uani 1 1 d . . . S4 S 0.3407(2) 0.32828(9) 0.78868(12) 0.0456(7) Uani 1 1 d . . . S3 S 0.8535(2) 0.32763(9) 0.93647(13) 0.0462(7) Uani 1 1 d . . . S2 S 0.6869(2) 0.30796(8) 1.19630(12) 0.0366(6) Uani 1 1 d . . . H5 H 0.559(19) 0.436(6) 0.915(11) 0.15(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(4) 0.043(4) 0.027(4) -0.004(3) 0.003(3) 0.006(3) C6 0.022(4) 0.041(4) 0.035(4) -0.011(4) -0.001(3) 0.015(4) C5 0.023(4) 0.053(5) 0.026(4) 0.002(4) 0.002(3) 0.006(4) C4 0.030(4) 0.067(5) 0.033(4) 0.007(4) 0.007(4) 0.009(4) C3 0.039(4) 0.063(5) 0.025(4) 0.002(4) 0.004(3) 0.013(4) C2 0.032(4) 0.054(5) 0.035(4) -0.002(4) 0.001(4) 0.006(4) C11 0.034(5) 0.066(6) 0.066(6) -0.011(5) -0.002(4) -0.005(5) C12 0.045(5) 0.065(6) 0.046(5) 0.005(5) 0.002(4) -0.007(5) C7 0.074(6) 0.068(6) 0.037(5) 0.006(5) 0.027(5) 0.025(5) C10 0.108(13) 0.119(13) 0.159(17) 0.048(12) 0.063(12) 0.046(11) C8 0.149(16) 0.095(12) 0.113(13) 0.021(10) 0.056(12) 0.022(11) C9 0.187(19) 0.079(10) 0.098(12) -0.013(9) -0.014(11) 0.016(11) C13 0.019(4) 0.050(5) 0.035(4) -0.002(4) 0.002(3) 0.003(3) C18 0.011(3) 0.061(5) 0.039(4) -0.006(4) 0.002(3) 0.004(4) C17 0.024(4) 0.059(4) 0.029(4) -0.007(4) -0.004(3) 0.003(3) C16 0.023(4) 0.059(5) 0.033(4) -0.016(4) 0.003(3) -0.005(4) C15 0.024(4) 0.047(4) 0.027(4) -0.009(4) 0.008(3) 0.002(3) C14 0.030(4) 0.044(4) 0.025(4) -0.007(4) 0.004(3) -0.001(4) C23 0.140(10) 0.066(7) 0.059(7) 0.017(6) 0.043(7) -0.016(7) C24 0.135(11) 0.078(7) 0.079(8) 0.021(7) 0.034(8) -0.017(8) C19 0.027(4) 0.040(5) 0.040(5) -0.013(4) -0.007(4) 0.004(4) C22 0.046(7) 0.068(8) 0.138(13) -0.043(8) -0.011(7) 0.019(6) C20 0.095(9) 0.044(6) 0.031(5) -0.024(5) 0.011(5) -0.003(6) C21 0.075(8) 0.058(7) 0.078(8) 0.001(6) 0.029(7) -0.012(6) C25 0.021(4) 0.037(4) 0.043(4) -0.002(4) -0.001(3) 0.000(3) C30 0.015(3) 0.023(4) 0.035(4) 0.003(3) -0.006(3) 0.004(3) C29 0.022(4) 0.035(4) 0.030(4) 0.002(3) 0.002(3) -0.007(3) C28 0.027(4) 0.046(4) 0.018(4) 0.004(3) -0.001(3) 0.001(3) C27 0.037(4) 0.057(5) 0.023(4) 0.003(4) 0.003(3) -0.005(4) C26 0.037(4) 0.053(5) 0.035(4) 0.004(4) 0.010(4) -0.002(4) C35 0.022(5) 0.074(7) 0.123(9) -0.016(7) -0.013(5) 0.009(5) C36 0.037(6) 0.072(7) 0.135(9) -0.013(7) -0.012(6) 0.005(5) C31 0.059(6) 0.056(6) 0.043(5) -0.011(5) 0.009(5) -0.002(5) C34 0.143(14) 0.070(9) 0.100(11) -0.034(8) 0.054(10) -0.032(9) C33 0.078(9) 0.100(11) 0.099(11) -0.033(9) 0.017(8) -0.032(8) C32 0.181(19) 0.097(12) 0.075(10) 0.008(9) -0.029(11) -0.013(12) C37 0.027(4) 0.033(4) 0.029(4) 0.001(3) -0.001(3) -0.002(3) C42 0.031(4) 0.032(4) 0.040(4) 0.007(4) -0.004(3) -0.006(3) C41 0.027(4) 0.040(4) 0.037(4) 0.001(3) 0.010(3) -0.009(3) C40 0.026(4) 0.044(4) 0.027(4) 0.004(3) 0.009(3) -0.007(3) C39 0.030(4) 0.039(4) 0.024(4) 0.002(3) 0.008(3) -0.003(3) C38 0.032(4) 0.028(4) 0.029(4) 0.000(3) 0.002(3) -0.001(3) C47 0.056(6) 0.049(5) 0.058(6) 0.000(5) 0.021(5) -0.002(5) C48 0.071(7) 0.053(6) 0.059(6) 0.009(5) 0.012(5) 0.009(5) C43 0.043(5) 0.048(5) 0.060(6) 0.013(5) 0.002(5) -0.010(4) C46 0.138(15) 0.094(12) 0.115(13) 0.050(10) -0.035(11) -0.036(11) C45 0.069(9) 0.111(13) 0.168(18) 0.035(12) 0.036(10) -0.023(9) C44 0.188(19) 0.087(11) 0.099(12) -0.005(10) 0.042(13) -0.030(12) C49 0.132(15) 0.098(12) 0.116(13) -0.025(10) 0.029(11) -0.007(11) C50 0.120(12) 0.014(6) 0.127(13) -0.004(7) 0.050(10) 0.007(7) C51 0.20(2) 0.074(12) 0.21(2) 0.015(13) 0.037(18) 0.040(13) C52 0.166(11) 0.174(11) 0.159(11) -0.015(9) 0.071(9) -0.015(9) C53 0.223(14) 0.185(14) 0.213(14) -0.003(10) 0.023(10) -0.013(10) C54 0.205(14) 0.203(14) 0.212(15) 0.009(9) 0.038(9) -0.017(9) O1 0.032(3) 0.045(4) 0.050(4) -0.003(3) -0.005(3) 0.006(3) O2 0.041(4) 0.052(4) 0.095(6) -0.002(4) -0.016(4) 0.003(4) O3 0.051(4) 0.051(4) 0.089(6) -0.014(5) -0.013(4) -0.016(4) O10 0.041(4) 0.031(4) 0.037(4) 0.004(3) 0.013(3) -0.001(3) O11 0.224(13) 0.056(6) 0.070(6) 0.012(5) 0.087(7) -0.006(6) O12 0.186(11) 0.047(5) 0.079(6) -0.010(5) 0.072(7) 0.005(6) O7 0.021(3) 0.037(4) 0.052(4) -0.011(3) -0.002(3) 0.006(3) O9 0.079(6) 0.040(5) 0.177(10) -0.011(6) -0.051(7) -0.002(4) O8 0.052(6) 0.078(7) 0.294(17) -0.013(8) -0.055(8) 0.030(5) O4 0.049(4) 0.061(4) 0.034(4) -0.007(3) 0.019(3) -0.005(3) O5 0.240(17) 0.074(7) 0.075(8) -0.018(6) 0.055(9) -0.025(9) O6 0.227(16) 0.114(9) 0.100(9) 0.016(7) 0.066(10) -0.036(9) O13 0.043(3) 0.083(5) 0.048(4) -0.008(4) -0.001(3) -0.010(4) O14 0.040(4) 0.098(6) 0.083(5) -0.006(5) 0.022(4) 0.005(4) O15 0.173(12) 0.070(7) 0.146(10) 0.025(7) 0.075(9) 0.036(7) O16 0.245(16) 0.102(8) 0.139(10) 0.007(8) -0.133(11) -0.033(10) S1 0.0220(11) 0.0564(15) 0.0434(14) 0.0171(12) 0.0098(10) 0.0115(11) S4 0.0421(14) 0.0607(16) 0.0301(12) -0.0085(12) -0.0028(10) 0.0216(12) S3 0.0312(13) 0.0623(17) 0.0471(15) -0.0260(13) 0.0129(11) -0.0122(12) S2 0.0323(12) 0.0426(13) 0.0309(12) 0.0164(10) -0.0037(9) -0.0140(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.331(12) . ? C1 C2 1.377(12) . ? C1 S1 1.792(9) . ? C6 C5 1.387(13) . ? C6 O1 1.420(10) . ? C5 C4 1.389(13) . ? C5 S4 1.756(9) . ? C4 C3 1.344(12) . ? C4 H4 0.9300 . ? C3 C2 1.360(13) . ? C3 C7 1.560(14) . ? C2 H2 0.9300 . ? C11 O1 1.441(11) . ? C11 C12 1.499(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.191(12) . ? C12 O3 1.281(12) . ? C7 C8 1.445(16) . ? C7 C10 1.482(18) . ? C7 C9 1.519(18) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C13 C18 1.389(13) . ? C13 C14 1.390(12) . ? C13 S4 1.789(8) . ? C18 C17 1.401(12) . ? C18 H18 0.9300 . ? C17 C16 1.458(11) . ? C17 C19 1.498(13) . ? C16 C15 1.379(12) . ? C16 H16 0.9300 . ? C15 C14 1.388(12) . ? C15 S3 1.797(8) . ? C14 O4 1.393(10) . ? C23 O4 1.435(12) . ? C23 C24 1.53(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O6 1.182(16) . ? C24 O5 1.275(18) . ? C19 C21 1.510(14) . ? C19 C22 1.512(13) . ? C19 C20 1.533(12) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C25 C30 1.418(12) . ? C25 C26 1.426(13) . ? C25 S3 1.777(10) . ? C30 C29 1.358(12) . ? C30 O7 1.365(10) . ? C29 C28 1.385(11) . ? C29 S2 1.793(9) . ? C28 C27 1.367(12) . ? C28 H28 0.9300 . ? C27 C26 1.382(13) . ? C27 C31 1.583(14) . ? C26 H26 0.9300 . ? C35 O7 1.432(11) . ? C35 C36 1.455(16) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O8 1.253(14) . ? C36 O9 1.297(13) . ? C31 C32 1.451(17) . ? C31 C34 1.496(16) . ? C31 C33 1.547(17) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C37 C42 1.403(12) . ? C37 C38 1.413(11) . ? C37 S2 1.764(8) . ? C42 C41 1.400(12) . ? C42 H42 0.9300 . ? C41 C40 1.372(12) . ? C41 C43 1.531(13) . ? C40 C39 1.360(12) . ? C40 H40 0.9300 . ? C39 C38 1.381(12) . ? C39 S1 1.800(9) . ? C38 O10 1.385(11) . ? C47 O10 1.420(12) . ? C47 C48 1.513(15) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O11 1.134(13) . ? C48 O12 1.303(14) . ? C43 C45 1.430(16) . ? C43 C44 1.468(18) . ? C43 C46 1.526(17) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C49 C50 1.54(2) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 O15 1.159(15) . ? C50 C51 1.42(2) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.508(10) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 O16 1.224(9) . ? C53 C54 1.497(10) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? O3 H3 0.8200 . ? O12 H12A 0.8200 . ? O9 H9 0.8200 . ? O5 H5 0.83(19) . ? O13 H13A 0.820(10) . ? O13 H13B 0.820(10) . ? O14 H14B 0.922(11) . ? O14 H14A 0.846(10) . ? O14 H14B 0.922(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.9(9) . . ? C6 C1 S1 123.9(7) . . ? C2 C1 S1 117.0(7) . . ? C1 C6 C5 121.4(8) . . ? C1 C6 O1 120.5(9) . . ? C5 C6 O1 117.9(8) . . ? C6 C5 C4 116.1(8) . . ? C6 C5 S4 122.7(7) . . ? C4 C5 S4 120.9(7) . . ? C3 C4 C5 124.6(9) . . ? C3 C4 H4 117.7 . . ? C5 C4 H4 117.7 . . ? C4 C3 C2 115.5(9) . . ? C4 C3 C7 120.8(9) . . ? C2 C3 C7 123.7(8) . . ? C3 C2 C1 123.1(9) . . ? C3 C2 H2 118.4 . . ? C1 C2 H2 118.4 . . ? O1 C11 C12 109.5(8) . . ? O1 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O1 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? O2 C12 O3 125.1(10) . . ? O2 C12 C11 125.9(9) . . ? O3 C12 C11 109.1(9) . . ? C8 C7 C10 118.3(12) . . ? C8 C7 C9 108.0(13) . . ? C10 C7 C9 94.2(13) . . ? C8 C7 C3 115.2(9) . . ? C10 C7 C3 109.4(11) . . ? C9 C7 C3 109.5(9) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C18 C13 C14 120.1(8) . . ? C18 C13 S4 117.9(6) . . ? C14 C13 S4 122.1(7) . . ? C13 C18 C17 123.4(8) . . ? C13 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C18 C17 C16 114.7(8) . . ? C18 C17 C19 123.1(8) . . ? C16 C17 C19 122.2(8) . . ? C15 C16 C17 120.9(8) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C15 C14 121.8(8) . . ? C16 C15 S3 117.6(6) . . ? C14 C15 S3 120.4(7) . . ? C15 C14 C13 118.7(8) . . ? C15 C14 O4 121.4(8) . . ? C13 C14 O4 119.7(8) . . ? O4 C23 C24 113.4(11) . . ? O4 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? O4 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? O6 C24 O5 126.9(17) . . ? O6 C24 C23 117.3(16) . . ? O5 C24 C23 115.7(13) . . ? C17 C19 C21 111.2(8) . . ? C17 C19 C22 114.0(8) . . ? C21 C19 C22 106.1(9) . . ? C17 C19 C20 108.0(8) . . ? C21 C19 C20 108.6(8) . . ? C22 C19 C20 108.7(9) . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C30 C25 C26 120.3(8) . . ? C30 C25 S3 123.0(7) . . ? C26 C25 S3 116.2(7) . . ? C29 C30 O7 124.8(8) . . ? C29 C30 C25 116.8(8) . . ? O7 C30 C25 118.4(8) . . ? C30 C29 C28 123.4(8) . . ? C30 C29 S2 120.1(6) . . ? C28 C29 S2 116.2(6) . . ? C27 C28 C29 120.0(8) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C27 C26 120.1(9) . . ? C28 C27 C31 121.5(8) . . ? C26 C27 C31 118.4(8) . . ? C27 C26 C25 119.1(9) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? O7 C35 C36 112.6(9) . . ? O7 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? O7 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? O8 C36 O9 120.7(12) . . ? O8 C36 C35 116.9(10) . . ? O9 C36 C35 122.1(10) . . ? C32 C31 C34 114.4(12) . . ? C32 C31 C33 105.7(12) . . ? C34 C31 C33 102.5(10) . . ? C32 C31 C27 112.3(9) . . ? C34 C31 C27 112.9(9) . . ? C33 C31 C27 108.1(9) . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 C37 C38 118.4(8) . . ? C42 C37 S2 117.5(6) . . ? C38 C37 S2 122.9(6) . . ? C41 C42 C37 123.3(8) . . ? C41 C42 H42 118.3 . . ? C37 C42 H42 118.3 . . ? C40 C41 C42 114.7(8) . . ? C40 C41 C43 123.9(8) . . ? C42 C41 C43 121.3(8) . . ? C39 C40 C41 123.9(8) . . ? C39 C40 H40 118.1 . . ? C41 C40 H40 118.1 . . ? C40 C39 C38 121.5(8) . . ? C40 C39 S1 118.5(6) . . ? C38 C39 S1 119.7(7) . . ? C39 C38 O10 122.7(8) . . ? C39 C38 C37 117.4(8) . . ? O10 C38 C37 119.9(7) . . ? O10 C47 C48 108.2(9) . . ? O10 C47 H47A 110.1 . . ? C48 C47 H47A 110.1 . . ? O10 C47 H47B 110.1 . . ? C48 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? O11 C48 O12 123.8(11) . . ? O11 C48 C47 127.8(12) . . ? O12 C48 C47 108.4(10) . . ? C45 C43 C44 102.5(12) . . ? C45 C43 C46 107.2(12) . . ? C44 C43 C46 113.4(13) . . ? C45 C43 C41 114.5(10) . . ? C44 C43 C41 107.8(10) . . ? C46 C43 C41 111.3(9) . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O15 C50 C51 123.4(17) . . ? O15 C50 C49 122.2(15) . . ? C51 C50 C49 114.4(16) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O16 C53 C54 126.6(10) . . ? O16 C53 C52 124.3(9) . . ? C54 C53 C52 108.8(11) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C6 O1 C11 111.5(7) . . ? C12 O3 H3 109.5 . . ? C38 O10 C47 110.2(7) . . ? C48 O12 H12A 109.5 . . ? C30 O7 C35 113.8(7) . . ? C36 O9 H9 109.5 . . ? C14 O4 C23 113.9(8) . . ? C24 O5 H5 111(10) . . ? H13A O13 H13B 111(3) . . ? H14B O14 H14A 102(2) . . ? H14B O14 H14B 0(10) . . ? H14A O14 H14B 102(2) . . ? C1 S1 C39 107.3(4) . . ? C5 S4 C13 106.6(4) . . ? C25 S3 C15 105.6(4) . . ? C37 S2 C29 105.6(4) . . ? 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 C1 C6 C5 0.3(13) . . . . ? S1 C1 C6 C5 176.5(6) . . . . ? C2 C1 C6 O1 -174.6(7) . . . . ? S1 C1 C6 O1 1.6(11) . . . . ? C1 C6 C5 C4 -1.4(12) . . . . ? O1 C6 C5 C4 173.6(7) . . . . ? C1 C6 C5 S4 -175.4(6) . . . . ? O1 C6 C5 S4 -0.4(11) . . . . ? C6 C5 C4 C3 -1.6(13) . . . . ? S4 C5 C4 C3 172.5(7) . . . . ? C5 C4 C3 C2 5.4(13) . . . . ? C5 C4 C3 C7 -177.2(9) . . . . ? C4 C3 C2 C1 -6.5(13) . . . . ? C7 C3 C2 C1 176.1(9) . . . . ? C6 C1 C2 C3 3.9(13) . . . . ? S1 C1 C2 C3 -172.5(7) . . . . ? O1 C11 C12 O2 5.9(16) . . . . ? O1 C11 C12 O3 -174.4(9) . . . . ? C4 C3 C7 C8 -10.1(16) . . . . ? C2 C3 C7 C8 167.1(11) . . . . ? C4 C3 C7 C10 126.0(12) . . . . ? C2 C3 C7 C10 -56.7(15) . . . . ? C4 C3 C7 C9 -132.1(12) . . . . ? C2 C3 C7 C9 45.2(16) . . . . ? C14 C13 C18 C17 -7.3(14) . . . . ? S4 C13 C18 C17 172.5(7) . . . . ? C13 C18 C17 C16 5.9(13) . . . . ? C13 C18 C17 C19 -174.7(9) . . . . ? C18 C17 C16 C15 -0.7(13) . . . . ? C19 C17 C16 C15 179.8(9) . . . . ? C17 C16 C15 C14 -3.1(14) . . . . ? C17 C16 C15 S3 -176.7(7) . . . . ? C16 C15 C14 C13 2.0(14) . . . . ? S3 C15 C14 C13 175.4(7) . . . . ? C16 C15 C14 O4 -173.9(8) . . . . ? S3 C15 C14 O4 -0.5(12) . . . . ? C18 C13 C14 C15 3.1(14) . . . . ? S4 C13 C14 C15 -176.7(7) . . . . ? C18 C13 C14 O4 179.0(8) . . . . ? S4 C13 C14 O4 -0.7(12) . . . . ? O4 C23 C24 O6 175.2(16) . . . . ? O4 C23 C24 O5 -8(2) . . . . ? C18 C17 C19 C21 -57.5(12) . . . . ? C16 C17 C19 C21 121.9(10) . . . . ? C18 C17 C19 C22 -177.4(10) . . . . ? C16 C17 C19 C22 2.1(14) . . . . ? C18 C17 C19 C20 61.6(12) . . . . ? C16 C17 C19 C20 -118.9(10) . . . . ? C26 C25 C30 C29 5.5(11) . . . . ? S3 C25 C30 C29 177.0(6) . . . . ? C26 C25 C30 O7 -172.8(7) . . . . ? S3 C25 C30 O7 -1.3(10) . . . . ? O7 C30 C29 C28 174.5(7) . . . . ? C25 C30 C29 C28 -3.7(11) . . . . ? O7 C30 C29 S2 0.5(11) . . . . ? C25 C30 C29 S2 -177.7(6) . . . . ? C30 C29 C28 C27 -1.0(12) . . . . ? S2 C29 C28 C27 173.2(6) . . . . ? C29 C28 C27 C26 3.9(12) . . . . ? C29 C28 C27 C31 -176.7(8) . . . . ? C28 C27 C26 C25 -2.0(13) . . . . ? C31 C27 C26 C25 178.5(8) . . . . ? C30 C25 C26 C27 -2.7(12) . . . . ? S3 C25 C26 C27 -174.8(7) . . . . ? O7 C35 C36 O8 169.1(15) . . . . ? O7 C35 C36 O9 -5(2) . . . . ? C28 C27 C31 C32 -133.0(13) . . . . ? C26 C27 C31 C32 46.5(15) . . . . ? C28 C27 C31 C34 -1.8(14) . . . . ? C26 C27 C31 C34 177.6(11) . . . . ? C28 C27 C31 C33 110.9(10) . . . . ? C26 C27 C31 C33 -69.7(12) . . . . ? C38 C37 C42 C41 5.3(14) . . . . ? S2 C37 C42 C41 173.3(7) . . . . ? C37 C42 C41 C40 2.8(13) . . . . ? C37 C42 C41 C43 179.6(9) . . . . ? C42 C41 C40 C39 -7.2(13) . . . . ? C43 C41 C40 C39 176.1(9) . . . . ? C41 C40 C39 C38 3.2(14) . . . . ? C41 C40 C39 S1 -170.5(7) . . . . ? C40 C39 C38 O10 -176.0(8) . . . . ? S1 C39 C38 O10 -2.4(12) . . . . ? C40 C39 C38 C37 5.4(13) . . . . ? S1 C39 C38 C37 179.0(6) . . . . ? C42 C37 C38 C39 -9.3(13) . . . . ? S2 C37 C38 C39 -176.6(7) . . . . ? C42 C37 C38 O10 172.1(8) . . . . ? S2 C37 C38 O10 4.8(12) . . . . ? O10 C47 C48 O11 -2.6(18) . . . . ? O10 C47 C48 O12 179.0(10) . . . . ? C40 C41 C43 C45 -30.9(16) . . . . ? C42 C41 C43 C45 152.6(11) . . . . ? C40 C41 C43 C44 82.3(13) . . . . ? C42 C41 C43 C44 -94.2(13) . . . . ? C40 C41 C43 C46 -152.7(12) . . . . ? C42 C41 C43 C46 30.8(15) . . . . ? C1 C6 O1 C11 83.5(10) . . . . ? C5 C6 O1 C11 -91.5(10) . . . . ? C12 C11 O1 C6 175.8(8) . . . . ? C39 C38 O10 C47 91.4(10) . . . . ? C37 C38 O10 C47 -90.0(10) . . . . ? C48 C47 O10 C38 -170.6(8) . . . . ? C29 C30 O7 C35 -91.9(11) . . . . ? C25 C30 O7 C35 86.3(10) . . . . ? C36 C35 O7 C30 -179.4(11) . . . . ? C15 C14 O4 C23 90.7(12) . . . . ? C13 C14 O4 C23 -85.1(12) . . . . ? C24 C23 O4 C14 -167.6(11) . . . . ? C6 C1 S1 C39 52.8(8) . . . . ? C2 C1 S1 C39 -131.0(7) . . . . ? C40 C39 S1 C1 -124.2(7) . . . . ? C38 C39 S1 C1 62.1(8) . . . . ? C6 C5 S4 C13 -60.7(8) . . . . ? C4 C5 S4 C13 125.6(7) . . . . ? C18 C13 S4 C5 126.9(8) . . . . ? C14 C13 S4 C5 -53.4(9) . . . . ? C30 C25 S3 C15 53.6(8) . . . . ? C26 C25 S3 C15 -134.6(7) . . . . ? C16 C15 S3 C25 -123.0(7) . . . . ? C14 C15 S3 C25 63.3(8) . . . . ? C42 C37 S2 C29 136.7(7) . . . . ? C38 C37 S2 C29 -55.9(9) . . . . ? C30 C29 S2 C37 -61.8(7) . . . . ? C28 C29 S2 C37 123.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.575 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.080 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 832090' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H64 N O14 S4' _chemical_formula_weight 1067.29 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' N N 0.0061 0.0033 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.0728(15) _cell_length_b 20.2500(18) _cell_length_c 17.4372(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.453(2) _cell_angle_gamma 90.00 _cell_volume 5863.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9924 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 22.05 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 0.222 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9570 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14079 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.00 _reflns_number_total 14079 _reflns_number_gt 7747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Several commands for restraints (including DFIX, SADI, EADP and ISOR commands) were applied on the atoms, the details are as follows: EADP C22 C22' isor 0.01 0.01 C8' C9' C10' SADI 0.01 C8 C9 C8 C10 C9 C10 C8' C9' C9' C10' C8' C10' SADI 0.01 C7 C8 C7 C9 C7 C10 C7 C8' C7 C9' C7 C10' SADI 0.01 C44 C45 C44 C46 C45 C46 C44' C45' C44' C46' C45' C46' SADI 0.01 C43 C44 C43 C45 C43 C46 C43 C44' C43 C45' C43 C46' SADI 0.01 C31 C32 C31 C33 C31 C34 C31 C32' C31 C33' C31 C34' SADI 0.01 C32 C33 C32 C34 C33 C34 C32' C33' C32' C34' C33' C34' SADI 0.01 C20 C21 C20 C22 C21 C22 C20' C21' C20' C22' C21' C22' SADI 0.01 C19 C20 C19 C21 C19 C22 C19 C20' C19 C21' C19 C22' DFIX 0.85 0.01 H5A O5 H9 O9 DFIX 1.90 0.01 H5A H14D H9 H13D ; _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^)+(0.0780P)^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 14079 _refine_ls_number_parameters 774 _refine_ls_number_restraints 142 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.009 _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 0.58521(14) 0.37847(11) 0.54604(13) 0.0414(6) Uani 1 1 d . . . C2 C 0.52345(15) 0.39039(12) 0.58368(14) 0.0483(6) Uani 1 1 d . . . H2 H 0.4877 0.4247 0.5656 0.058 Uiso 1 1 calc R . . C3 C 0.51297(14) 0.35319(12) 0.64706(13) 0.0416(6) Uani 1 1 d . A . C4 C 0.56497(13) 0.29987(11) 0.66933(13) 0.0395(5) Uani 1 1 d . . . H4 H 0.5574 0.2722 0.7095 0.047 Uiso 1 1 calc R . . C5 C 0.62799(13) 0.28693(11) 0.63304(13) 0.0361(5) Uani 1 1 d . . . C6 C 0.63999(13) 0.32811(11) 0.57281(13) 0.0379(5) Uani 1 1 d . . . C7 C 0.44496(15) 0.36902(13) 0.68862(15) 0.0552(7) Uani 1 1 d D . . C8 C 0.4436(3) 0.3217(2) 0.7556(3) 0.0730(13) Uani 0.77 1 d PD A 1 H8A H 0.4947 0.3228 0.7929 0.109 Uiso 0.77 1 calc PR A 1 H8B H 0.4333 0.2777 0.7350 0.109 Uiso 0.77 1 calc PR A 1 H8C H 0.4019 0.3345 0.7812 0.109 Uiso 0.77 1 calc PR A 1 C9 C 0.3651(2) 0.3666(4) 0.6287(3) 0.133(3) Uani 0.77 1 d PD A 1 H9A H 0.3470 0.3217 0.6212 0.199 Uiso 0.77 1 calc PR A 1 H9B H 0.3715 0.3844 0.5794 0.199 Uiso 0.77 1 calc PR A 1 H9C H 0.3260 0.3923 0.6473 0.199 Uiso 0.77 1 calc PR A 1 C10 C 0.4596(3) 0.43869(19) 0.7232(3) 0.0959(17) Uani 0.77 1 d PD A 1 H10A H 0.4164 0.4507 0.7472 0.144 Uiso 0.77 1 calc PR A 1 H10B H 0.4618 0.4694 0.6818 0.144 Uiso 0.77 1 calc PR A 1 H10C H 0.5096 0.4396 0.7621 0.144 Uiso 0.77 1 calc PR A 1 C11 C 0.77510(15) 0.35219(14) 0.58236(17) 0.0593(7) Uani 1 1 d . . . H11A H 0.7888 0.3369 0.6366 0.071 Uiso 1 1 calc R . . H11B H 0.7649 0.3993 0.5825 0.071 Uiso 1 1 calc R . . C12 C 0.84319(17) 0.33863(15) 0.5441(2) 0.0601(7) Uani 1 1 d . . . C13 C 0.70888(12) 0.17333(10) 0.59635(12) 0.0320(5) Uani 1 1 d . . . C14 C 0.64397(12) 0.13916(11) 0.55035(12) 0.0320(5) Uani 1 1 d . . . C15 C 0.65708(12) 0.09606(10) 0.49241(12) 0.0307(5) Uani 1 1 d . . . C16 C 0.73527(12) 0.08501(10) 0.48434(12) 0.0335(5) Uani 1 1 d . . . H16 H 0.7433 0.0563 0.4452 0.040 Uiso 1 1 calc R . . C17 C 0.80139(12) 0.11522(11) 0.53250(12) 0.0339(5) Uani 1 1 d . B . C18 C 0.78631(13) 0.16040(11) 0.58724(13) 0.0377(5) Uani 1 1 d . . . H18 H 0.8295 0.1828 0.6189 0.045 Uiso 1 1 calc R . . C19 C 0.88761(13) 0.10018(12) 0.52580(14) 0.0464(6) Uani 1 1 d D . . C20 C 0.8909(2) 0.0522(2) 0.4608(2) 0.0774(15) Uani 0.802(4) 1 d PD B 1 H20A H 0.8663 0.0716 0.4108 0.116 Uiso 0.802(4) 1 calc PR B 1 H20B H 0.8626 0.0125 0.4680 0.116 Uiso 0.802(4) 1 calc PR B 1 H20C H 0.9461 0.0417 0.4622 0.116 Uiso 0.802(4) 1 calc PR B 1 C21 C 0.9349(2) 0.0721(2) 0.6054(2) 0.0735(13) Uani 0.802(4) 1 d PD B 1 H21A H 0.9113 0.0310 0.6157 0.110 Uiso 0.802(4) 1 calc PR B 1 H21B H 0.9331 0.1029 0.6467 0.110 Uiso 0.802(4) 1 calc PR B 1 H21C H 0.9899 0.0648 0.6032 0.110 Uiso 0.802(4) 1 calc PR B 1 C22 C 0.9289(2) 0.16484(18) 0.5108(3) 0.0863(15) Uani 0.802(4) 1 d PD B 1 H22A H 0.9290 0.1952 0.5530 0.129 Uiso 0.802(4) 1 calc PR B 1 H22B H 0.9002 0.1839 0.4619 0.129 Uiso 0.802(4) 1 calc PR B 1 H22C H 0.9834 0.1558 0.5080 0.129 Uiso 0.802(4) 1 calc PR B 1 C23 C 0.55462(15) 0.10195(13) 0.62282(17) 0.0567(7) Uani 1 1 d . . . H23A H 0.6018 0.1016 0.6664 0.068 Uiso 1 1 calc R . . H23B H 0.5480 0.0579 0.6005 0.068 Uiso 1 1 calc R . . C24 C 0.48296(16) 0.11852(16) 0.65335(16) 0.0601(8) Uani 1 1 d . . . C25 C 0.50190(12) 0.10174(11) 0.39186(12) 0.0337(5) Uani 1 1 d . . . C26 C 0.42505(13) 0.09113(11) 0.40360(13) 0.0383(5) Uani 1 1 d . . . H26 H 0.4175 0.0578 0.4378 0.046 Uiso 1 1 calc R . . C27 C 0.35943(13) 0.12859(12) 0.36594(13) 0.0393(5) Uani 1 1 d . C . C28 C 0.37405(13) 0.18090(12) 0.31946(13) 0.0423(6) Uani 1 1 d . . . H28 H 0.3317 0.2086 0.2963 0.051 Uiso 1 1 calc R . . C29 C 0.45002(13) 0.19287(12) 0.30675(13) 0.0388(5) Uani 1 1 d . . . C30 C 0.51383(12) 0.15159(11) 0.34060(12) 0.0355(5) Uani 1 1 d . . . C31 C 0.27522(14) 0.11171(13) 0.37621(15) 0.0553(7) Uani 1 1 d D . . C32 C 0.2785(5) 0.1095(4) 0.4647(3) 0.0673(19) Uani 0.59 1 d PD C 1 H32A H 0.2944 0.1519 0.4876 0.101 Uiso 0.59 1 calc PR C 1 H32B H 0.3168 0.0768 0.4894 0.101 Uiso 0.59 1 calc PR C 1 H32C H 0.2262 0.0984 0.4725 0.101 Uiso 0.59 1 calc PR C 1 C33 C 0.2565(5) 0.0405(3) 0.3448(4) 0.086(2) Uani 0.59 1 d PD C 1 H33A H 0.2932 0.0103 0.3772 0.130 Uiso 0.59 1 calc PR C 1 H33B H 0.2624 0.0379 0.2915 0.130 Uiso 0.59 1 calc PR C 1 H33C H 0.2023 0.0292 0.3464 0.130 Uiso 0.59 1 calc PR C 1 C34 C 0.2102(5) 0.1583(4) 0.3351(6) 0.110(4) Uani 0.59 1 d PD C 1 H34A H 0.2105 0.1608 0.2802 0.165 Uiso 0.59 1 calc PR C 1 H34B H 0.2198 0.2014 0.3583 0.165 Uiso 0.59 1 calc PR C 1 H34C H 0.1588 0.1425 0.3406 0.165 Uiso 0.59 1 calc PR C 1 C35 C 0.59646(15) 0.11762(16) 0.25873(15) 0.0613(8) Uani 1 1 d . . . H35A H 0.5607 0.1337 0.2107 0.074 Uiso 1 1 calc R . . H35B H 0.5801 0.0730 0.2678 0.074 Uiso 1 1 calc R . . C36 C 0.67971(17) 0.11632(15) 0.24786(17) 0.0573(7) Uani 1 1 d . . . C37 C 0.53986(13) 0.30708(11) 0.28694(14) 0.0390(5) Uani 1 1 d . . . C38 C 0.53486(14) 0.34412(12) 0.35273(14) 0.0412(6) Uani 1 1 d . . . C39 C 0.59928(14) 0.38465(11) 0.38780(14) 0.0415(6) Uani 1 1 d . . . C40 C 0.66350(14) 0.39236(11) 0.35204(14) 0.0433(6) Uani 1 1 d . . . H40 H 0.7058 0.4200 0.3754 0.052 Uiso 1 1 calc R . . C41 C 0.66633(13) 0.35987(12) 0.28231(13) 0.0399(6) Uani 1 1 d . D . C42 C 0.60451(13) 0.31549(11) 0.25244(14) 0.0399(5) Uani 1 1 d . . . H42 H 0.6067 0.2908 0.2080 0.048 Uiso 1 1 calc R . . C43 C 0.73570(14) 0.37093(12) 0.24166(14) 0.0488(6) Uani 1 1 d D . . C44 C 0.8158(3) 0.3588(5) 0.2977(4) 0.122(4) Uani 0.53 1 d PD D 1 H44A H 0.8145 0.3172 0.3238 0.182 Uiso 0.53 1 calc PR D 1 H44B H 0.8268 0.3935 0.3361 0.182 Uiso 0.53 1 calc PR D 1 H44C H 0.8573 0.3578 0.2688 0.182 Uiso 0.53 1 calc PR D 1 C45 C 0.7301(5) 0.3253(4) 0.1701(4) 0.103(3) Uani 0.53 1 d PD D 1 H45A H 0.6807 0.3337 0.1321 0.154 Uiso 0.53 1 calc PR D 1 H45B H 0.7315 0.2801 0.1869 0.154 Uiso 0.53 1 calc PR D 1 H45C H 0.7748 0.3337 0.1467 0.154 Uiso 0.53 1 calc PR D 1 C46 C 0.7307(6) 0.4413(3) 0.2107(6) 0.122(4) Uani 0.53 1 d PD D 1 H46A H 0.7321 0.4715 0.2534 0.183 Uiso 0.53 1 calc PR D 1 H46B H 0.6813 0.4471 0.1716 0.183 Uiso 0.53 1 calc PR D 1 H46C H 0.7755 0.4498 0.1876 0.183 Uiso 0.53 1 calc PR D 1 C47 C 0.40922(17) 0.38966(17) 0.3475(2) 0.0791(10) Uani 1 1 d . . . H47A H 0.3913 0.3807 0.2915 0.095 Uiso 1 1 calc R . . H47B H 0.4347 0.4328 0.3537 0.095 Uiso 1 1 calc R . . C48 C 0.33848(16) 0.39024(16) 0.38373(18) 0.0599(7) Uani 1 1 d . . . C49 C 0.09015(19) 0.47319(17) 0.37062(19) 0.0762(9) Uani 1 1 d . . . H49 H 0.0817 0.4694 0.3162 0.091 Uiso 1 1 calc R . . C50 C 0.02529(17) 0.48704(16) 0.40137(18) 0.0683(8) Uani 1 1 d . . . H50 H -0.0252 0.4927 0.3678 0.082 Uiso 1 1 calc R . . C51 C 0.03428(14) 0.49266(12) 0.48203(16) 0.0483(6) Uani 1 1 d . . . C52 C 0.11167(15) 0.48399(15) 0.52722(17) 0.0640(8) Uani 1 1 d . . . H52 H 0.1218 0.4871 0.5819 0.077 Uiso 1 1 calc R . . C53 C 0.17340(17) 0.47074(16) 0.4914(2) 0.0756(9) Uani 1 1 d . . . H53 H 0.2248 0.4655 0.5233 0.091 Uiso 1 1 calc R . . C8' C 0.4764(11) 0.3642(10) 0.7778(5) 0.137(8) Uani 0.23 1 d PDU A 2 H8'1 H 0.4320 0.3663 0.8028 0.205 Uiso 0.23 1 calc PR A 2 H8'2 H 0.5126 0.4002 0.7958 0.205 Uiso 0.23 1 calc PR A 2 H8'3 H 0.5044 0.3231 0.7907 0.205 Uiso 0.23 1 calc PR A 2 C9' C 0.3788(9) 0.3177(7) 0.6635(12) 0.139(8) Uani 0.23 1 d PDU A 2 H9'1 H 0.4014 0.2743 0.6739 0.208 Uiso 0.23 1 calc PR A 2 H9'2 H 0.3553 0.3222 0.6081 0.208 Uiso 0.23 1 calc PR A 2 H9'3 H 0.3381 0.3242 0.6926 0.208 Uiso 0.23 1 calc PR A 2 C10' C 0.4079(10) 0.4371(5) 0.6689(10) 0.099(6) Uani 0.23 1 d PDU A 2 H10D H 0.3640 0.4428 0.6940 0.149 Uiso 0.23 1 calc PR A 2 H10E H 0.3885 0.4412 0.6128 0.149 Uiso 0.23 1 calc PR A 2 H10F H 0.4480 0.4704 0.6874 0.149 Uiso 0.23 1 calc PR A 2 C20' C 0.8997(8) 0.0251(4) 0.5351(11) 0.097(9) Uani 0.198(4) 1 d PD B 2 H20D H 0.9502 0.0131 0.5237 0.145 Uiso 0.198(4) 1 calc PR B 2 H20E H 0.8567 0.0027 0.4991 0.145 Uiso 0.198(4) 1 calc PR B 2 H20F H 0.8997 0.0125 0.5882 0.145 Uiso 0.198(4) 1 calc PR B 2 C21' C 0.9536(7) 0.1346(8) 0.5855(8) 0.103(9) Uani 0.198(4) 1 d PD B 2 H21D H 0.9632 0.1113 0.6347 0.154 Uiso 0.198(4) 1 calc PR B 2 H21E H 0.9373 0.1790 0.5931 0.154 Uiso 0.198(4) 1 calc PR B 2 H21F H 1.0021 0.1353 0.5666 0.154 Uiso 0.198(4) 1 calc PR B 2 C22' C 0.8929(8) 0.1189(8) 0.4423(5) 0.0863(15) Uani 0.198(4) 1 d PD B 2 H22D H 0.9477 0.1151 0.4377 0.129 Uiso 0.198(4) 1 calc PR B 2 H22E H 0.8749 0.1636 0.4315 0.129 Uiso 0.198(4) 1 calc PR B 2 H22F H 0.8594 0.0898 0.4051 0.129 Uiso 0.198(4) 1 calc PR B 2 C32' C 0.2713(10) 0.0758(6) 0.4507(5) 0.152(9) Uani 0.41 1 d PD C 2 H32D H 0.2966 0.1020 0.4955 0.227 Uiso 0.41 1 calc PR C 2 H32E H 0.2988 0.0342 0.4525 0.227 Uiso 0.41 1 calc PR C 2 H32F H 0.2160 0.0682 0.4516 0.227 Uiso 0.41 1 calc PR C 2 C33' C 0.2327(7) 0.0715(6) 0.3034(6) 0.152(7) Uani 0.41 1 d PD C 2 H33D H 0.2645 0.0334 0.2983 0.228 Uiso 0.41 1 calc PR C 2 H33E H 0.2263 0.0984 0.2571 0.228 Uiso 0.41 1 calc PR C 2 H33F H 0.1807 0.0576 0.3096 0.228 Uiso 0.41 1 calc PR C 2 C34' C 0.2303(7) 0.1784(4) 0.3717(9) 0.129(7) Uani 0.41 1 d PD C 2 H34D H 0.2314 0.2001 0.3230 0.194 Uiso 0.41 1 calc PR C 2 H34E H 0.2561 0.2058 0.4152 0.194 Uiso 0.41 1 calc PR C 2 H34F H 0.1754 0.1706 0.3741 0.194 Uiso 0.41 1 calc PR C 2 C44' C 0.8004(4) 0.4163(4) 0.2918(4) 0.077(2) Uani 0.47 1 d PD D 2 H44D H 0.8132 0.4013 0.3455 0.116 Uiso 0.47 1 calc PR D 2 H44E H 0.7803 0.4607 0.2896 0.116 Uiso 0.47 1 calc PR D 2 H44F H 0.8481 0.4152 0.2714 0.116 Uiso 0.47 1 calc PR D 2 C45' C 0.7753(5) 0.3063(3) 0.2314(6) 0.084(2) Uani 0.47 1 d PD D 2 H45D H 0.7867 0.2826 0.2805 0.126 Uiso 0.47 1 calc PR D 2 H45E H 0.8246 0.3145 0.2156 0.126 Uiso 0.47 1 calc PR D 2 H45F H 0.7399 0.2806 0.1918 0.126 Uiso 0.47 1 calc PR D 2 C46' C 0.7011(4) 0.4037(4) 0.1644(4) 0.089(3) Uani 0.47 1 d PD D 2 H46D H 0.6651 0.4383 0.1719 0.134 Uiso 0.47 1 calc PR D 2 H46E H 0.6721 0.3718 0.1279 0.134 Uiso 0.47 1 calc PR D 2 H46F H 0.7439 0.4221 0.1439 0.134 Uiso 0.47 1 calc PR D 2 N1 N 0.16442(15) 0.46490(13) 0.41381(18) 0.0737(7) Uani 1 1 d . . . O1 O 0.70522(9) 0.31875(8) 0.53965(9) 0.0449(4) Uani 1 1 d . . . O2 O 0.83664(13) 0.31144(14) 0.48294(15) 0.1002(9) Uani 1 1 d . . . O3 O 0.91154(12) 0.36077(12) 0.58687(14) 0.0868(7) Uani 1 1 d . . . H3A H 0.9477 0.3530 0.5644 0.130 Uiso 1 1 calc R . . O4 O 0.56803(8) 0.14698(7) 0.56426(9) 0.0378(4) Uani 1 1 d . . . O5 O 0.43529(5) 0.16556(5) 0.62082(6) 0.0851(7) Uani 1 1 d D . . H5A H 0.4185 0.2019 0.6000 0.128 Uiso 1 1 d RD . . O6 O 0.47049(5) 0.08578(5) 0.70715(6) 0.0953(8) Uani 1 1 d R . . O7 O 0.58825(5) 0.15856(5) 0.32321(6) 0.0430(4) Uani 1 1 d R . . O9 O 0.73413(5) 0.15010(5) 0.29493(6) 0.0868(7) Uani 1 1 d RD . . H9 H 0.7579 0.1653 0.3389 0.130 Uiso 1 1 d RD . . O8 O 0.69476(14) 0.08306(13) 0.19616(13) 0.0919(7) Uani 1 1 d . . . O10 O 0.46637(9) 0.34087(8) 0.38320(10) 0.0510(5) Uani 1 1 d . . . O11 O 0.32792(12) 0.35224(13) 0.43172(14) 0.0902(8) Uani 1 1 d . . . O12 O 0.29058(13) 0.43880(13) 0.35428(15) 0.0977(8) Uani 1 1 d . . . H12 H 0.2555 0.4427 0.3791 0.147 Uiso 1 1 calc R . . O13 O 0.71834(12) 0.23189(10) 0.40256(12) 0.0751(6) Uani 1 1 d . . . H13C H 0.7150 0.2564 0.4412 0.113 Uiso 1 1 d R . . H13D H 0.6785 0.2092 0.3779 0.113 Uiso 1 1 d RD . . O14 O 0.43661(12) 0.24295(10) 0.50132(12) 0.0698(6) Uani 1 1 d . . . H14C H 0.4448 0.2710 0.4677 0.22(3) Uiso 1 1 d R . . H14D H 0.4741 0.2155 0.5194 0.324 Uiso 1 1 d RD . . S1 S 0.59860(5) 0.43478(3) 0.47172(4) 0.0556(2) Uani 1 1 d . . . S2 S 0.45992(4) 0.25491(4) 0.23726(4) 0.05239(19) Uani 1 1 d . . . S3 S 0.57982(3) 0.04635(3) 0.43518(4) 0.03954(15) Uani 1 1 d . . . S4 S 0.69785(4) 0.22451(3) 0.67573(3) 0.04128(16) 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 0.0491(14) 0.0390(13) 0.0412(13) -0.0003(11) 0.0209(11) 0.0048(11) C2 0.0546(16) 0.0452(15) 0.0510(15) 0.0021(12) 0.0244(13) 0.0145(12) C3 0.0418(13) 0.0485(15) 0.0393(13) -0.0016(11) 0.0189(11) 0.0069(11) C4 0.0399(13) 0.0452(14) 0.0359(12) -0.0016(11) 0.0138(10) 0.0032(11) C5 0.0332(12) 0.0387(13) 0.0369(12) -0.0071(10) 0.0092(10) 0.0024(10) C6 0.0393(13) 0.0390(13) 0.0390(13) -0.0094(10) 0.0165(11) 0.0000(10) C7 0.0486(16) 0.0706(19) 0.0539(16) 0.0056(14) 0.0274(13) 0.0202(14) C8 0.076(3) 0.079(3) 0.084(3) 0.017(2) 0.059(3) 0.019(2) C9 0.038(2) 0.294(9) 0.072(3) 0.008(5) 0.026(2) 0.049(4) C10 0.131(5) 0.073(3) 0.113(4) -0.011(3) 0.089(4) 0.020(3) C11 0.0510(16) 0.0617(18) 0.0705(19) -0.0102(15) 0.0249(14) -0.0122(14) C12 0.0491(17) 0.0590(19) 0.076(2) 0.0078(16) 0.0214(16) -0.0005(14) C13 0.0296(11) 0.0327(12) 0.0339(12) -0.0023(9) 0.0076(9) 0.0042(9) C14 0.0261(11) 0.0371(12) 0.0335(12) 0.0048(10) 0.0086(9) 0.0060(9) C15 0.0266(11) 0.0306(12) 0.0326(11) 0.0025(9) 0.0021(9) 0.0011(9) C16 0.0339(12) 0.0325(12) 0.0351(12) -0.0017(10) 0.0101(10) 0.0037(9) C17 0.0276(11) 0.0360(12) 0.0378(12) -0.0008(10) 0.0067(9) 0.0051(9) C18 0.0281(11) 0.0422(13) 0.0405(13) -0.0037(11) 0.0032(10) -0.0007(10) C19 0.0294(12) 0.0549(16) 0.0571(16) -0.0067(13) 0.0145(11) 0.0024(11) C20 0.041(2) 0.107(4) 0.087(3) -0.041(3) 0.023(2) 0.010(2) C21 0.037(2) 0.097(4) 0.080(3) 0.001(3) 0.0017(19) 0.021(2) C22 0.053(2) 0.074(3) 0.147(5) -0.006(3) 0.054(3) -0.009(2) C23 0.0489(16) 0.0527(17) 0.0777(19) 0.0102(15) 0.0333(14) 0.0009(13) C24 0.0516(17) 0.081(2) 0.0550(17) 0.0031(16) 0.0278(14) -0.0007(15) C25 0.0292(11) 0.0363(13) 0.0328(12) 0.0009(10) 0.0014(9) 0.0000(9) C26 0.0338(12) 0.0393(13) 0.0403(13) 0.0062(11) 0.0060(10) -0.0041(10) C27 0.0277(12) 0.0481(14) 0.0401(13) 0.0083(11) 0.0039(10) -0.0030(10) C28 0.0264(11) 0.0536(15) 0.0435(14) 0.0144(12) 0.0014(10) 0.0048(10) C29 0.0324(12) 0.0470(14) 0.0348(12) 0.0111(11) 0.0037(10) -0.0041(11) C30 0.0254(11) 0.0454(14) 0.0336(12) -0.0007(10) 0.0029(9) -0.0053(10) C31 0.0312(13) 0.0710(19) 0.0650(18) 0.0216(15) 0.0137(12) 0.0001(13) C32 0.046(3) 0.091(5) 0.075(4) 0.036(3) 0.035(3) -0.002(4) C33 0.056(5) 0.107(5) 0.090(5) 0.010(4) 0.005(4) -0.033(4) C34 0.026(4) 0.143(7) 0.154(8) 0.107(7) 0.005(4) 0.005(4) C35 0.0513(16) 0.091(2) 0.0443(16) -0.0095(15) 0.0162(13) -0.0008(15) C36 0.0585(18) 0.0676(19) 0.0514(17) 0.0055(15) 0.0241(14) 0.0062(15) C37 0.0304(12) 0.0425(14) 0.0443(14) 0.0142(11) 0.0091(10) 0.0013(10) C38 0.0363(13) 0.0468(15) 0.0448(14) 0.0193(12) 0.0180(11) 0.0089(11) C39 0.0489(14) 0.0374(13) 0.0438(14) 0.0102(11) 0.0224(12) 0.0093(11) C40 0.0420(14) 0.0405(14) 0.0519(15) 0.0047(12) 0.0198(12) -0.0019(11) C41 0.0389(13) 0.0437(14) 0.0411(13) 0.0084(11) 0.0172(11) 0.0038(11) C42 0.0415(13) 0.0423(14) 0.0384(13) 0.0079(11) 0.0141(11) 0.0008(11) C43 0.0464(15) 0.0569(16) 0.0518(15) -0.0002(13) 0.0287(13) -0.0079(13) C44 0.041(4) 0.246(12) 0.086(6) 0.041(8) 0.032(4) 0.015(6) C45 0.109(7) 0.125(7) 0.103(6) -0.039(5) 0.082(5) -0.033(5) C46 0.157(9) 0.074(5) 0.179(10) 0.034(6) 0.126(9) -0.005(5) C47 0.0526(17) 0.097(2) 0.101(2) 0.044(2) 0.0433(17) 0.0362(17) C48 0.0423(15) 0.077(2) 0.0659(19) 0.0124(16) 0.0236(14) 0.0119(15) C49 0.064(2) 0.100(3) 0.069(2) -0.0115(19) 0.0247(17) 0.0077(18) C50 0.0467(17) 0.090(2) 0.066(2) -0.0045(17) 0.0100(15) 0.0085(16) C51 0.0412(14) 0.0462(15) 0.0572(17) 0.0004(13) 0.0107(12) 0.0026(12) C52 0.0427(16) 0.084(2) 0.0648(19) 0.0011(16) 0.0110(14) 0.0096(15) C53 0.0430(17) 0.090(2) 0.091(3) 0.004(2) 0.0091(17) 0.0096(16) C8' 0.129(11) 0.175(12) 0.124(11) -0.012(9) 0.066(8) 0.035(9) C9' 0.116(11) 0.156(12) 0.167(12) -0.034(9) 0.079(9) -0.014(8) C10' 0.100(9) 0.090(9) 0.125(10) -0.004(8) 0.061(8) 0.022(7) C20' 0.046(9) 0.073(12) 0.19(3) 0.057(14) 0.067(13) 0.039(8) C21' 0.022(8) 0.18(3) 0.108(17) -0.057(18) 0.010(9) -0.003(11) C22' 0.053(2) 0.074(3) 0.147(5) -0.006(3) 0.054(3) -0.009(2) C32' 0.073(8) 0.184(18) 0.197(17) 0.146(14) 0.029(9) -0.020(11) C33' 0.049(7) 0.218(17) 0.188(15) -0.108(13) 0.026(9) -0.078(10) C34' 0.025(6) 0.158(12) 0.216(19) 0.073(11) 0.053(9) 0.018(7) C44' 0.050(4) 0.111(6) 0.081(5) -0.003(5) 0.035(4) -0.017(4) C45' 0.074(6) 0.070(5) 0.129(8) -0.009(5) 0.067(5) 0.001(4) C46' 0.075(5) 0.133(9) 0.075(6) 0.038(5) 0.050(4) 0.011(6) N1 0.0553(16) 0.0787(18) 0.093(2) -0.0059(16) 0.0295(15) 0.0111(13) O1 0.0404(9) 0.0511(10) 0.0496(10) -0.0065(8) 0.0236(8) 0.0027(8) O2 0.0628(15) 0.154(2) 0.0948(18) -0.0385(17) 0.0411(14) -0.0169(15) O3 0.0507(13) 0.0981(18) 0.1112(19) -0.0135(15) 0.0184(12) -0.0167(13) O4 0.0247(8) 0.0466(9) 0.0444(9) 0.0027(7) 0.0128(7) 0.0045(7) O5 0.0657(14) 0.1007(17) 0.1022(17) 0.0352(14) 0.0470(13) 0.0401(13) O6 0.0885(16) 0.129(2) 0.0857(16) 0.0399(15) 0.0549(14) 0.0223(15) O7 0.0292(8) 0.0564(10) 0.0449(10) 0.0007(8) 0.0122(7) -0.0046(7) O9 0.0495(12) 0.121(2) 0.0952(17) -0.0206(15) 0.0263(12) -0.0140(13) O8 0.0959(17) 0.1105(19) 0.0834(16) -0.0198(14) 0.0497(14) 0.0077(14) O10 0.0396(9) 0.0612(11) 0.0606(11) 0.0241(9) 0.0290(8) 0.0131(8) O11 0.0603(13) 0.123(2) 0.1023(18) 0.0461(16) 0.0491(13) 0.0273(13) O12 0.0673(15) 0.1166(19) 0.127(2) 0.0502(16) 0.0597(14) 0.0493(14) O13 0.0748(14) 0.0716(14) 0.0736(14) -0.0088(11) 0.0063(11) -0.0057(11) O14 0.0833(15) 0.0632(13) 0.0619(12) 0.0086(11) 0.0147(11) 0.0050(11) S1 0.0805(5) 0.0400(4) 0.0581(4) 0.0046(3) 0.0397(4) 0.0083(3) S2 0.0389(3) 0.0694(5) 0.0438(4) 0.0246(3) -0.0008(3) -0.0099(3) S3 0.0312(3) 0.0333(3) 0.0489(4) -0.0026(3) -0.0012(3) -0.0001(2) S4 0.0395(3) 0.0478(4) 0.0346(3) -0.0082(3) 0.0046(3) 0.0092(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 C1 C2 1.387(3) . ? C1 C6 1.389(3) . ? C1 S1 1.780(2) . ? C2 C3 1.383(3) . ? C2 H2 0.9300 . ? C3 C4 1.394(3) . ? C3 C7 1.539(3) . ? C4 C5 1.394(3) . ? C4 H4 0.9300 . ? C5 C6 1.393(3) . ? C5 S4 1.778(2) . ? C6 O1 1.382(2) . ? C7 C9 1.514(4) . ? C7 C8 1.515(4) . ? C7 C9' 1.522(7) . ? C7 C10' 1.523(7) . ? C7 C8' 1.525(7) . ? C7 C10 1.532(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.422(3) . ? C11 C12 1.494(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.182(3) . ? C12 O3 1.309(3) . ? C13 C14 1.392(3) . ? C13 C18 1.392(3) . ? C13 S4 1.774(2) . ? C14 O4 1.382(2) . ? C14 C15 1.392(3) . ? C15 C16 1.393(3) . ? C15 S3 1.771(2) . ? C16 C17 1.383(3) . ? C16 H16 0.9300 . ? C17 C18 1.389(3) . ? C17 C19 1.534(3) . ? C18 H18 0.9300 . ? C19 C20 1.504(4) . ? C19 C21' 1.514(6) . ? C19 C22' 1.528(7) . ? C19 C22 1.538(4) . ? C19 C20' 1.539(7) . ? C19 C21 1.543(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O4 1.427(3) . ? C23 C24 1.482(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O6 1.207(3) . ? C24 O5 1.295(3) . ? C25 C26 1.391(3) . ? C25 C30 1.394(3) . ? C25 S3 1.769(2) . ? C26 C27 1.385(3) . ? C26 H26 0.9300 . ? C27 C28 1.391(3) . ? C27 C31 1.528(3) . ? C28 C29 1.387(3) . ? C28 H28 0.9300 . ? C29 C30 1.391(3) . ? C29 S2 1.781(2) . ? C30 O7 1.380(2) . ? C31 C32' 1.503(6) . ? C31 C34 1.506(5) . ? C31 C32 1.532(5) . ? C31 C33' 1.540(6) . ? C31 C34' 1.545(6) . ? C31 C33 1.549(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 O7 1.430(3) . ? C35 C36 1.477(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 O8 1.200(3) . ? C36 O9 1.284(3) . ? C37 C42 1.385(3) . ? C37 C38 1.390(3) . ? C37 S2 1.783(2) . ? C38 O10 1.394(3) . ? C38 C39 1.394(3) . ? C39 C40 1.390(3) . ? C39 S1 1.783(2) . ? C40 C41 1.393(3) . ? C40 H40 0.9300 . ? C41 C42 1.392(3) . ? C41 C43 1.532(3) . ? C42 H42 0.9300 . ? C43 C46' 1.494(5) . ? C43 C45' 1.502(5) . ? C43 C44 1.505(5) . ? C43 C46 1.520(5) . ? C43 C45 1.537(5) . ? C43 C44' 1.543(5) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 O10 1.426(3) . ? C47 C48 1.488(3) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O11 1.181(3) . ? C48 O12 1.305(3) . ? C49 N1 1.326(4) . ? C49 C50 1.367(4) . ? C49 H49 0.9300 . ? C50 C51 1.384(4) . ? C50 H50 0.9300 . ? C51 C52 1.383(3) . ? C51 C51 1.481(5) 3_566 ? C52 C53 1.371(4) . ? C52 H52 0.9300 . ? C53 N1 1.330(4) . ? C53 H53 0.9300 . ? C8' H8'1 0.9600 . ? C8' H8'2 0.9600 . ? C8' H8'3 0.9600 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C20' H20D 0.9600 . ? C20' H20E 0.9600 . ? C20' H20F 0.9600 . ? C21' H21D 0.9600 . ? C21' H21E 0.9600 . ? C21' H21F 0.9600 . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C32' H32D 0.9600 . ? C32' H32E 0.9600 . ? C32' H32F 0.9600 . ? C33' H33D 0.9600 . ? C33' H33E 0.9600 . ? C33' H33F 0.9600 . ? C34' H34D 0.9600 . ? C34' H34E 0.9600 . ? C34' H34F 0.9600 . ? C44' H44D 0.9600 . ? C44' H44E 0.9600 . ? C44' H44F 0.9600 . ? C45' H45D 0.9600 . ? C45' H45E 0.9600 . ? C45' H45F 0.9600 . ? C46' H46D 0.9600 . ? C46' H46E 0.9600 . ? C46' H46F 0.9600 . ? O3 H3A 0.8200 . ? O5 H5A 0.8409 . ? O9 H9 0.8382 . ? O12 H12 0.8200 . ? O13 H13C 0.8500 . ? O13 H13D 0.8498 . ? O14 H14C 0.8500 . ? O14 H14D 0.8500 . ? 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 C1 C6 119.7(2) . . ? C2 C1 S1 118.26(18) . . ? C6 C1 S1 121.63(17) . . ? C3 C2 C1 122.5(2) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C2 C3 C4 116.9(2) . . ? C2 C3 C7 121.0(2) . . ? C4 C3 C7 122.1(2) . . ? C5 C4 C3 121.9(2) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 119.6(2) . . ? C6 C5 S4 122.63(16) . . ? C4 C5 S4 117.19(17) . . ? O1 C6 C1 120.3(2) . . ? O1 C6 C5 120.5(2) . . ? C1 C6 C5 119.16(19) . . ? C9 C7 C8 109.8(3) . . ? C9 C7 C9' 44.8(7) . . ? C8 C7 C9' 69.3(7) . . ? C9 C7 C10' 67.3(6) . . ? C8 C7 C10' 131.8(7) . . ? C9' C7 C10' 108.2(6) . . ? C9 C7 C8' 138.5(8) . . ? C8 C7 C8' 40.5(7) . . ? C9' C7 C8' 108.2(6) . . ? C10' C7 C8' 108.5(6) . . ? C9 C7 C10 109.8(3) . . ? C8 C7 C10 108.1(3) . . ? C9' C7 C10 141.6(7) . . ? C10' C7 C10 43.6(6) . . ? C8' C7 C10 70.8(7) . . ? C9 C7 C3 109.0(2) . . ? C8 C7 C3 112.3(2) . . ? C9' C7 C3 108.2(8) . . ? C10' C7 C3 113.7(6) . . ? C8' C7 C3 110.0(7) . . ? C10 C7 C3 107.8(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? O1 C11 C12 108.9(2) . . ? O1 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O1 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O2 C12 O3 123.9(3) . . ? O2 C12 C11 124.6(3) . . ? O3 C12 C11 111.5(3) . . ? C14 C13 C18 119.38(19) . . ? C14 C13 S4 121.70(15) . . ? C18 C13 S4 118.34(16) . . ? O4 C14 C13 119.70(18) . . ? O4 C14 C15 120.99(18) . . ? C13 C14 C15 119.28(18) . . ? C14 C15 C16 119.60(19) . . ? C14 C15 S3 122.74(15) . . ? C16 C15 S3 117.22(16) . . ? C17 C16 C15 122.25(19) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C18 116.95(19) . . ? C16 C17 C19 121.87(19) . . ? C18 C17 C19 121.18(19) . . ? C17 C18 C13 122.3(2) . . ? C17 C18 H18 118.8 . . ? C13 C18 H18 118.8 . . ? C20 C19 C21' 131.5(6) . . ? C20 C19 C22' 54.7(6) . . ? C21' C19 C22' 110.0(5) . . ? C20 C19 C17 113.0(2) . . ? C21' C19 C17 115.5(6) . . ? C22' C19 C17 107.1(6) . . ? C20 C19 C22 108.8(3) . . ? C21' C19 C22 55.1(7) . . ? C22' C19 C22 59.7(6) . . ? C17 C19 C22 109.3(2) . . ? C20 C19 C20' 54.0(6) . . ? C21' C19 C20' 108.8(5) . . ? C22' C19 C20' 108.0(5) . . ? C17 C19 C20' 107.2(5) . . ? C22 C19 C20' 143.5(5) . . ? C20 C19 C21 109.6(3) . . ? C21' C19 C21 53.2(7) . . ? C22' C19 C21 144.5(6) . . ? C17 C19 C21 108.4(2) . . ? C22 C19 C21 107.6(3) . . ? C20' C19 C21 60.7(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? O4 C23 C24 113.3(2) . . ? O4 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? O4 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? O6 C24 O5 122.5(2) . . ? O6 C24 C23 117.7(3) . . ? O5 C24 C23 119.8(2) . . ? C26 C25 C30 119.32(19) . . ? C26 C25 S3 118.72(17) . . ? C30 C25 S3 121.68(16) . . ? C27 C26 C25 122.2(2) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 117.26(19) . . ? C26 C27 C31 120.1(2) . . ? C28 C27 C31 122.7(2) . . ? C29 C28 C27 121.8(2) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C28 C29 C30 119.7(2) . . ? C28 C29 S2 118.19(17) . . ? C30 C29 S2 121.60(16) . . ? O7 C30 C29 121.01(19) . . ? O7 C30 C25 119.61(18) . . ? C29 C30 C25 119.37(19) . . ? C32' C31 C34 122.6(9) . . ? C32' C31 C27 116.2(6) . . ? C34 C31 C27 114.4(4) . . ? C32' C31 C32 27.7(6) . . ? C34 C31 C32 110.3(4) . . ? C27 C31 C32 108.1(3) . . ? C32' C31 C33' 110.4(5) . . ? C34 C31 C33' 77.6(6) . . ? C27 C31 C33' 107.3(5) . . ? C32 C31 C33' 135.6(6) . . ? C32' C31 C34' 110.2(5) . . ? C34 C31 C34' 29.1(7) . . ? C27 C31 C34' 105.6(5) . . ? C32 C31 C34' 88.7(7) . . ? C33' C31 C34' 106.6(5) . . ? C32' C31 C33 78.9(6) . . ? C34 C31 C33 110.3(4) . . ? C27 C31 C33 106.8(4) . . ? C32 C31 C33 106.6(3) . . ? C33' C31 C33 36.7(5) . . ? C34' C31 C33 137.4(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? O7 C35 C36 112.6(2) . . ? O7 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? O7 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? O8 C36 O9 122.0(3) . . ? O8 C36 C35 119.1(3) . . ? O9 C36 C35 118.9(2) . . ? C42 C37 C38 120.0(2) . . ? C42 C37 S2 117.33(19) . . ? C38 C37 S2 122.26(17) . . ? C37 C38 O10 120.5(2) . . ? C37 C38 C39 119.1(2) . . ? O10 C38 C39 120.4(2) . . ? C40 C39 C38 119.6(2) . . ? C40 C39 S1 117.42(19) . . ? C38 C39 S1 122.67(17) . . ? C39 C40 C41 122.0(2) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C42 C41 C40 117.0(2) . . ? C42 C41 C43 121.5(2) . . ? C40 C41 C43 121.5(2) . . ? C37 C42 C41 121.9(2) . . ? C37 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C46' C43 C45' 112.0(4) . . ? C46' C43 C44 140.1(4) . . ? C45' C43 C44 64.4(4) . . ? C46' C43 C46 44.4(4) . . ? C45' C43 C46 139.9(4) . . ? C44 C43 C46 110.6(4) . . ? C46' C43 C41 107.2(3) . . ? C45' C43 C41 110.2(3) . . ? C44 C43 C41 111.1(3) . . ? C46 C43 C41 108.4(3) . . ? C46' C43 C45 66.3(4) . . ? C45' C43 C45 47.6(4) . . ? C44 C43 C45 107.7(4) . . ? C46 C43 C45 106.7(4) . . ? C41 C43 C45 112.3(3) . . ? C46' C43 C44' 109.1(4) . . ? C45' C43 C44' 107.7(4) . . ? C44 C43 C44' 46.1(4) . . ? C46 C43 C44' 67.4(4) . . ? C41 C43 C44' 110.7(3) . . ? C45 C43 C44' 135.9(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? O10 C47 C48 111.2(2) . . ? O10 C47 H47A 109.4 . . ? C48 C47 H47A 109.4 . . ? O10 C47 H47B 109.4 . . ? C48 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? O11 C48 O12 125.8(3) . . ? O11 C48 C47 124.6(3) . . ? O12 C48 C47 109.6(3) . . ? N1 C49 C50 123.9(3) . . ? N1 C49 H49 118.0 . . ? C50 C49 H49 118.0 . . ? C49 C50 C51 120.5(3) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C52 C51 C50 115.7(2) . . ? C52 C51 C51 121.9(3) . 3_566 ? C50 C51 C51 122.3(3) . 3_566 ? C53 C52 C51 119.9(3) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? N1 C53 C52 124.2(3) . . ? N1 C53 H53 117.9 . . ? C52 C53 H53 117.9 . . ? C7 C8' H8'1 109.5 . . ? C7 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7 C9' H9'1 109.5 . . ? C7 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C7 C10' H10D 109.5 . . ? C7 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C19 C20' H20D 109.5 . . ? C19 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C19 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C19 C21' H21D 109.5 . . ? C19 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C19 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C19 C22' H22D 109.5 . . ? C19 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C19 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C31 C32' H32D 109.5 . . ? C31 C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C31 C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C31 C33' H33D 109.5 . . ? C31 C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? C31 C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? C31 C34' H34D 109.5 . . ? C31 C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C31 C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C43 C44' H44D 109.5 . . ? C43 C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C43 C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? C43 C45' H45D 109.5 . . ? C43 C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C43 C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? C43 C46' H46D 109.5 . . ? C43 C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? C43 C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? C49 N1 C53 115.8(3) . . ? C6 O1 C11 112.02(17) . . ? C12 O3 H3A 109.5 . . ? C14 O4 C23 111.44(16) . . ? C24 O5 H5A 161.7 . . ? C30 O7 C35 112.15(16) . . ? C36 O9 H9 154.8 . . ? C38 O10 C47 110.51(17) . . ? C48 O12 H12 109.5 . . ? H13C O13 H13D 121.6 . . ? H14C O14 H14D 117.5 . . ? C1 S1 C39 105.02(11) . . ? C29 S2 C37 105.70(10) . . ? C25 S3 C15 105.52(10) . . ? C13 S4 C5 105.74(10) . . ? 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 -1.0(4) . . . . ? S1 C1 C2 C3 -173.76(19) . . . . ? C1 C2 C3 C4 -3.6(4) . . . . ? C1 C2 C3 C7 178.5(2) . . . . ? C2 C3 C4 C5 4.1(3) . . . . ? C7 C3 C4 C5 -178.0(2) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C3 C4 C5 S4 171.66(18) . . . . ? C2 C1 C6 O1 -175.2(2) . . . . ? S1 C1 C6 O1 -2.7(3) . . . . ? C2 C1 C6 C5 5.2(3) . . . . ? S1 C1 C6 C5 177.75(17) . . . . ? C4 C5 C6 O1 175.7(2) . . . . ? S4 C5 C6 O1 4.6(3) . . . . ? C4 C5 C6 C1 -4.8(3) . . . . ? S4 C5 C6 C1 -175.89(17) . . . . ? C2 C3 C7 C9 57.2(4) . . . . ? C4 C3 C7 C9 -120.6(4) . . . . ? C2 C3 C7 C8 179.2(3) . . . . ? C4 C3 C7 C8 1.3(4) . . . . ? C2 C3 C7 C9' 104.7(9) . . . . ? C4 C3 C7 C9' -73.2(9) . . . . ? C2 C3 C7 C10' -15.5(8) . . . . ? C4 C3 C7 C10' 166.6(8) . . . . ? C2 C3 C7 C8' -137.4(8) . . . . ? C4 C3 C7 C8' 44.8(8) . . . . ? C2 C3 C7 C10 -61.9(4) . . . . ? C4 C3 C7 C10 120.3(3) . . . . ? O1 C11 C12 O2 8.6(4) . . . . ? O1 C11 C12 O3 -171.4(2) . . . . ? C18 C13 C14 O4 173.77(19) . . . . ? S4 C13 C14 O4 2.7(3) . . . . ? C18 C13 C14 C15 -4.4(3) . . . . ? S4 C13 C14 C15 -175.47(16) . . . . ? O4 C14 C15 C16 -174.54(19) . . . . ? C13 C14 C15 C16 3.6(3) . . . . ? O4 C14 C15 S3 -2.3(3) . . . . ? C13 C14 C15 S3 175.81(16) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? S3 C15 C16 C17 -172.25(17) . . . . ? C15 C16 C17 C18 -3.4(3) . . . . ? C15 C16 C17 C19 177.0(2) . . . . ? C16 C17 C18 C13 2.6(3) . . . . ? C19 C17 C18 C13 -177.8(2) . . . . ? C14 C13 C18 C17 1.3(3) . . . . ? S4 C13 C18 C17 172.65(17) . . . . ? C16 C17 C19 C20 2.0(4) . . . . ? C18 C17 C19 C20 -177.6(3) . . . . ? C16 C17 C19 C21' -177.0(8) . . . . ? C18 C17 C19 C21' 3.5(8) . . . . ? C16 C17 C19 C22' 60.2(7) . . . . ? C18 C17 C19 C22' -119.4(7) . . . . ? C16 C17 C19 C22 123.3(3) . . . . ? C18 C17 C19 C22 -56.2(3) . . . . ? C16 C17 C19 C20' -55.5(8) . . . . ? C18 C17 C19 C20' 124.9(7) . . . . ? C16 C17 C19 C21 -119.7(3) . . . . ? C18 C17 C19 C21 60.8(3) . . . . ? O4 C23 C24 O6 -174.8(2) . . . . ? O4 C23 C24 O5 7.1(4) . . . . ? C30 C25 C26 C27 0.0(3) . . . . ? S3 C25 C26 C27 -174.02(18) . . . . ? C25 C26 C27 C28 -4.3(3) . . . . ? C25 C26 C27 C31 175.6(2) . . . . ? C26 C27 C28 C29 4.1(4) . . . . ? C31 C27 C28 C29 -175.8(2) . . . . ? C27 C28 C29 C30 0.4(4) . . . . ? C27 C28 C29 S2 172.75(19) . . . . ? C28 C29 C30 O7 174.0(2) . . . . ? S2 C29 C30 O7 2.0(3) . . . . ? C28 C29 C30 C25 -4.9(3) . . . . ? S2 C29 C30 C25 -176.99(17) . . . . ? C26 C25 C30 O7 -174.21(19) . . . . ? S3 C25 C30 O7 -0.4(3) . . . . ? C26 C25 C30 C29 4.7(3) . . . . ? S3 C25 C30 C29 178.54(17) . . . . ? C26 C27 C31 C32' 25.3(7) . . . . ? C28 C27 C31 C32' -154.8(6) . . . . ? C26 C27 C31 C34 177.3(5) . . . . ? C28 C27 C31 C34 -2.8(5) . . . . ? C26 C27 C31 C32 53.9(4) . . . . ? C28 C27 C31 C32 -126.2(4) . . . . ? C26 C27 C31 C33' -98.8(6) . . . . ? C28 C27 C31 C33' 81.1(6) . . . . ? C26 C27 C31 C34' 147.8(6) . . . . ? C28 C27 C31 C34' -32.4(6) . . . . ? C26 C27 C31 C33 -60.4(4) . . . . ? C28 C27 C31 C33 119.5(3) . . . . ? O7 C35 C36 O8 179.1(3) . . . . ? O7 C35 C36 O9 0.2(4) . . . . ? C42 C37 C38 O10 173.63(19) . . . . ? S2 C37 C38 O10 0.9(3) . . . . ? C42 C37 C38 C39 -6.3(3) . . . . ? S2 C37 C38 C39 -178.99(17) . . . . ? C37 C38 C39 C40 6.4(3) . . . . ? O10 C38 C39 C40 -173.6(2) . . . . ? C37 C38 C39 S1 179.35(17) . . . . ? O10 C38 C39 S1 -0.6(3) . . . . ? C38 C39 C40 C41 -1.0(3) . . . . ? S1 C39 C40 C41 -174.36(18) . . . . ? C39 C40 C41 C42 -4.3(3) . . . . ? C39 C40 C41 C43 177.5(2) . . . . ? C38 C37 C42 C41 0.8(3) . . . . ? S2 C37 C42 C41 173.87(17) . . . . ? C40 C41 C42 C37 4.4(3) . . . . ? C43 C41 C42 C37 -177.4(2) . . . . ? C42 C41 C43 C46' 67.5(5) . . . . ? C40 C41 C43 C46' -114.3(4) . . . . ? C42 C41 C43 C45' -54.6(5) . . . . ? C40 C41 C43 C45' 123.6(4) . . . . ? C42 C41 C43 C44 -124.0(5) . . . . ? C40 C41 C43 C44 54.1(5) . . . . ? C42 C41 C43 C46 114.3(5) . . . . ? C40 C41 C43 C46 -67.6(5) . . . . ? C42 C41 C43 C45 -3.4(5) . . . . ? C40 C41 C43 C45 174.8(4) . . . . ? C42 C41 C43 C44' -173.6(4) . . . . ? C40 C41 C43 C44' 4.6(4) . . . . ? O10 C47 C48 O11 -5.1(5) . . . . ? O10 C47 C48 O12 174.9(3) . . . . ? N1 C49 C50 C51 -0.6(5) . . . . ? C49 C50 C51 C52 0.5(4) . . . . ? C49 C50 C51 C51 -179.8(3) . . . 3_566 ? C50 C51 C52 C53 0.0(4) . . . . ? C51 C51 C52 C53 -179.7(3) 3_566 . . . ? C51 C52 C53 N1 -0.5(5) . . . . ? C50 C49 N1 C53 0.1(5) . . . . ? C52 C53 N1 C49 0.4(5) . . . . ? C1 C6 O1 C11 93.9(3) . . . . ? C5 C6 O1 C11 -86.6(3) . . . . ? C12 C11 O1 C6 178.8(2) . . . . ? C13 C14 O4 C23 -87.4(2) . . . . ? C15 C14 O4 C23 90.7(2) . . . . ? C24 C23 O4 C14 166.4(2) . . . . ? C29 C30 O7 C35 -92.2(2) . . . . ? C25 C30 O7 C35 86.7(2) . . . . ? C36 C35 O7 C30 -170.7(2) . . . . ? C37 C38 O10 C47 -90.2(3) . . . . ? C39 C38 O10 C47 89.7(3) . . . . ? C48 C47 O10 C38 -175.7(3) . . . . ? C2 C1 S1 C39 -127.3(2) . . . . ? C6 C1 S1 C39 60.1(2) . . . . ? C40 C39 S1 C1 -127.94(19) . . . . ? C38 C39 S1 C1 58.9(2) . . . . ? C28 C29 S2 C37 129.2(2) . . . . ? C30 C29 S2 C37 -58.6(2) . . . . ? C42 C37 S2 C29 123.29(18) . . . . ? C38 C37 S2 C29 -63.8(2) . . . . ? C26 C25 S3 C15 -124.68(18) . . . . ? C30 C25 S3 C15 61.5(2) . . . . ? C14 C15 S3 C25 55.05(19) . . . . ? C16 C15 S3 C25 -132.56(17) . . . . ? C14 C13 S4 C5 -61.0(2) . . . . ? C18 C13 S4 C5 127.81(18) . . . . ? C6 C5 S4 C13 -56.6(2) . . . . ? C4 C5 S4 C13 132.04(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14D O4 0.85 2.13 2.978(2) 179.8 . O14 H14C O11 0.85 2.55 2.961(3) 110.9 . O14 H14C O10 0.85 2.14 2.986(3) 179.4 . O13 H13D O7 0.85 1.91 2.761(2) 179.3 . O13 H13C O1 0.85 2.17 3.018(2) 179.4 . O12 H12 N1 0.82 1.85 2.653(3) 165.6 . O9 H9 O13 0.84 1.96 2.564(2) 127.7 . O5 H5A O14 0.84 2.00 2.612(2) 129.1 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.503 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.060 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 832091' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H16 O7 S2' _chemical_formula_weight 396.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3369(8) _cell_length_b 13.2291(10) _cell_length_c 13.3387(11) _cell_angle_alpha 85.4050(10) _cell_angle_beta 79.6150(10) _cell_angle_gamma 81.5540(10) _cell_volume 1772.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3356 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 22.78 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9479 _exptl_absorpt_correction_T_max 0.9670 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12059 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6876 _reflns_number_gt 5029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two DFIX commands were applied on the water molecule (O13) to restrict the O-H distances. ; _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^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6876 _refine_ls_number_parameters 481 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 C6 C 0.1248(2) 0.31927(19) 0.3463(2) 0.0341(6) Uani 1 1 d . . . C1 C 0.0955(3) 0.2209(2) 0.3409(2) 0.0384(6) Uani 1 1 d . . . C2 C 0.0643(3) 0.1618(2) 0.4312(2) 0.0479(8) Uani 1 1 d . . . H2 H 0.0449 0.0957 0.4282 0.057 Uiso 1 1 calc R . . C3 C 0.0618(3) 0.2001(2) 0.5243(2) 0.0517(8) Uani 1 1 d . . . H32 H 0.0361 0.1615 0.5841 0.062 Uiso 1 1 calc R . . C4 C 0.0972(3) 0.2948(2) 0.5292(2) 0.0433(7) Uani 1 1 d . . . H4 H 0.0989 0.3192 0.5923 0.052 Uiso 1 1 calc R . . C5 C 0.1309(2) 0.35554(19) 0.4404(2) 0.0347(6) Uani 1 1 d . . . C9 C 0.3135(3) 0.49849(19) 0.3715(2) 0.0381(6) Uani 1 1 d . . . C10 C 0.4299(3) 0.43021(18) 0.3698(2) 0.0350(6) Uani 1 1 d . . . C11 C 0.5495(3) 0.45490(19) 0.3139(2) 0.0388(7) Uani 1 1 d . . . C12 C 0.5492(3) 0.5477(2) 0.2554(2) 0.0488(8) Uani 1 1 d . . . H33 H 0.6274 0.5638 0.2148 0.059 Uiso 1 1 calc R . . C13 C 0.4344(3) 0.6151(2) 0.2577(2) 0.0523(8) Uani 1 1 d . . . H13 H 0.4360 0.6774 0.2202 0.063 Uiso 1 1 calc R . . C14 C 0.3174(3) 0.5913(2) 0.3148(2) 0.0473(7) Uani 1 1 d . . . H34 H 0.2403 0.6375 0.3156 0.057 Uiso 1 1 calc R . . C17 C 0.6933(3) 0.2543(2) 0.3209(2) 0.0396(7) Uani 1 1 d . . . C22 C 0.6619(2) 0.21659(19) 0.2360(2) 0.0362(6) Uani 1 1 d . . . C21 C 0.6569(3) 0.11276(19) 0.2323(2) 0.0385(7) Uani 1 1 d . . . C20 C 0.6917(3) 0.0472(2) 0.3133(3) 0.0478(8) Uani 1 1 d . . . H20 H 0.6893 -0.0227 0.3115 0.057 Uiso 1 1 calc R . . C19 C 0.7290(3) 0.0836(2) 0.3948(3) 0.0523(8) Uani 1 1 d . . . H19 H 0.7545 0.0386 0.4472 0.063 Uiso 1 1 calc R . . C18 C 0.7290(3) 0.1872(2) 0.3995(2) 0.0493(8) Uani 1 1 d . . . H18 H 0.7530 0.2122 0.4558 0.059 Uiso 1 1 calc R . . C25 C 0.4712(3) 0.1185(2) 0.0994(2) 0.0422(7) Uani 1 1 d . . . C26 C 0.3543(3) 0.12536(19) 0.1724(2) 0.0387(7) Uani 1 1 d . . . C27 C 0.2348(3) 0.1697(2) 0.1431(2) 0.0418(7) Uani 1 1 d . . . C28 C 0.2316(3) 0.2038(2) 0.0427(2) 0.0516(8) Uani 1 1 d . . . H28 H 0.1519 0.2340 0.0236 0.062 Uiso 1 1 calc R . . C29 C 0.3461(4) 0.1932(2) -0.0295(3) 0.0591(9) Uani 1 1 d . . . H29 H 0.3430 0.2138 -0.0974 0.071 Uiso 1 1 calc R . . C30 C 0.4634(3) 0.1525(2) -0.0006(2) 0.0524(8) Uani 1 1 d . . . H30 H 0.5404 0.1474 -0.0493 0.063 Uiso 1 1 calc R . . C7 C 0.0470(3) 0.4628(2) 0.2454(2) 0.0439(7) Uani 1 1 d . . . H7A H 0.0743 0.5255 0.2624 0.053 Uiso 1 1 calc R . . H7B H -0.0337 0.4514 0.2920 0.053 Uiso 1 1 calc R . . C8 C 0.0208(3) 0.4736(2) 0.1390(2) 0.0426(7) Uani 1 1 d . . . C31 C 0.3859(3) -0.0120(2) 0.3001(3) 0.0567(9) Uani 1 1 d . . . H31A H 0.4081 -0.0200 0.3682 0.068 Uiso 1 1 calc R . . H31B H 0.4637 -0.0395 0.2531 0.068 Uiso 1 1 calc R . . C32 C 0.2760(4) -0.0720(3) 0.2970(3) 0.0605(9) Uani 1 1 d . . . C23 C 0.7510(3) 0.2846(2) 0.0760(3) 0.0573(9) Uani 1 1 d . . . H23A H 0.7676 0.2200 0.0430 0.069 Uiso 1 1 calc R . . H23B H 0.8275 0.2903 0.1069 0.069 Uiso 1 1 calc R . . C24 C 0.7355(3) 0.3706(2) -0.0029(2) 0.0465(7) Uani 1 1 d . . . C15 C 0.4334(3) 0.3309(2) 0.5255(2) 0.0487(8) Uani 1 1 d . . . H15A H 0.3667 0.3825 0.5590 0.058 Uiso 1 1 calc R . . H15B H 0.5199 0.3450 0.5347 0.058 Uiso 1 1 calc R . . C16 C 0.4100(3) 0.2263(2) 0.5727(3) 0.0569(9) Uani 1 1 d . . . C33 C 0.9570(6) 0.8329(5) 0.1834(4) 0.126(2) Uani 1 1 d . . . H33A H 0.8996 0.8596 0.2441 0.151 Uiso 1 1 calc R . . H33B H 0.9127 0.7832 0.1577 0.151 Uiso 1 1 calc R . . C34 C 0.9749(6) 0.9145(5) 0.1084(5) 0.143(2) Uani 1 1 d . . . H34A H 1.0132 0.9663 0.1351 0.214 Uiso 1 1 calc R . . H34B H 0.8906 0.9433 0.0909 0.214 Uiso 1 1 calc R . . H34C H 1.0331 0.8891 0.0486 0.214 Uiso 1 1 calc R . . O1 O 0.14818(17) 0.37952(13) 0.25711(13) 0.0382(4) Uani 1 1 d . . . O10 O 0.35392(19) 0.09496(14) 0.27393(14) 0.0442(5) Uani 1 1 d . . . O7 O 0.63667(17) 0.28406(13) 0.15419(14) 0.0398(5) Uani 1 1 d . . . O4 O 0.42706(18) 0.33467(12) 0.42085(15) 0.0396(5) Uani 1 1 d . . . O2 O 0.0860(2) 0.42366(16) 0.07032(17) 0.0590(6) Uani 1 1 d . . . O3 O -0.0778(2) 0.54569(17) 0.12799(16) 0.0569(6) Uani 1 1 d . . . H3 H -0.0839 0.5548 0.0674 0.085 Uiso 1 1 calc R . . O12 O 0.2701(3) -0.0983(3) 0.2091(2) 0.0958(10) Uani 1 1 d . . . H12 H 0.2052 -0.1281 0.2121 0.144 Uiso 1 1 calc R . . O11 O 0.1974(4) -0.0911(3) 0.3694(3) 0.1448(17) Uani 1 1 d . . . O9 O 0.6465(2) 0.44617(17) 0.02584(18) 0.0628(6) Uani 1 1 d . . . H9 H 0.6448 0.4905 -0.0207 0.094 Uiso 1 1 calc R . . O8 O 0.8083(2) 0.36712(16) -0.08430(17) 0.0655(7) Uani 1 1 d . . . O5 O 0.4025(3) 0.15688(16) 0.5081(2) 0.0724(7) Uani 1 1 d . . . H5A H 0.4064 0.1837 0.4503 0.109 Uiso 1 1 calc R . . O6 O 0.3985(3) 0.2060(2) 0.6614(2) 0.0941(9) Uani 1 1 d . . . O13 O 0.3796(2) 0.40652(18) 0.1060(2) 0.0619(6) Uani 1 1 d D . . H13B H 0.4527(19) 0.381(3) 0.118(3) 0.093 Uiso 1 1 d D . . H13A H 0.315(3) 0.383(3) 0.138(3) 0.093 Uiso 1 1 d D . . O14 O 1.0768(3) 0.7832(2) 0.2106(3) 0.0945(9) Uani 1 1 d . . . H14 H 1.1150 0.7450 0.1658 0.142 Uiso 1 1 calc R . . S4 S 0.16293(7) 0.48108(5) 0.45520(6) 0.0426(2) Uani 1 1 d . . . S1 S 0.07857(8) 0.17119(6) 0.22537(7) 0.0512(2) Uani 1 1 d . . . S2 S 0.62772(8) 0.05699(6) 0.12366(6) 0.0498(2) Uani 1 1 d . . . S3 S 0.70616(8) 0.38586(6) 0.32701(7) 0.0546(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 C6 0.0272(13) 0.0398(14) 0.0338(16) 0.0041(12) -0.0044(11) -0.0040(11) C1 0.0324(14) 0.0407(15) 0.0430(17) -0.0006(12) -0.0078(12) -0.0068(12) C2 0.0433(17) 0.0421(16) 0.058(2) 0.0078(14) -0.0045(15) -0.0159(13) C3 0.0544(19) 0.0564(19) 0.0411(19) 0.0163(15) -0.0014(15) -0.0158(15) C4 0.0435(16) 0.0513(17) 0.0320(17) 0.0015(13) -0.0023(13) -0.0036(13) C5 0.0314(14) 0.0376(14) 0.0341(16) -0.0001(11) -0.0044(12) -0.0044(11) C9 0.0464(16) 0.0377(15) 0.0331(16) -0.0036(12) -0.0107(13) -0.0096(12) C10 0.0461(16) 0.0277(13) 0.0336(16) -0.0036(11) -0.0089(12) -0.0096(11) C11 0.0454(16) 0.0339(14) 0.0393(17) -0.0096(12) -0.0048(13) -0.0118(12) C12 0.060(2) 0.0436(16) 0.0439(19) 0.0014(13) 0.0001(15) -0.0230(15) C13 0.074(2) 0.0392(16) 0.046(2) 0.0094(13) -0.0137(17) -0.0180(16) C14 0.0594(19) 0.0368(15) 0.0468(19) 0.0024(13) -0.0167(15) -0.0033(14) C17 0.0317(14) 0.0413(15) 0.0459(18) -0.0030(13) -0.0030(13) -0.0090(12) C22 0.0304(14) 0.0345(14) 0.0415(17) 0.0034(12) -0.0041(12) -0.0030(11) C21 0.0334(14) 0.0342(14) 0.0449(18) 0.0002(12) -0.0001(13) -0.0041(11) C20 0.0470(17) 0.0342(15) 0.057(2) 0.0056(14) -0.0025(15) 0.0002(13) C19 0.0498(19) 0.0535(19) 0.049(2) 0.0135(15) -0.0105(15) 0.0023(15) C18 0.0393(16) 0.065(2) 0.0439(19) -0.0042(15) -0.0128(14) -0.0012(14) C25 0.0523(18) 0.0324(14) 0.0435(18) -0.0084(12) -0.0068(14) -0.0098(12) C26 0.0499(17) 0.0289(13) 0.0404(17) -0.0066(12) -0.0107(14) -0.0089(12) C27 0.0517(17) 0.0346(14) 0.0440(18) -0.0080(12) -0.0152(14) -0.0096(13) C28 0.068(2) 0.0442(17) 0.048(2) -0.0074(14) -0.0250(17) -0.0040(15) C29 0.088(3) 0.0532(19) 0.039(2) -0.0052(15) -0.0179(19) -0.0085(18) C30 0.065(2) 0.0492(18) 0.041(2) -0.0128(14) 0.0021(16) -0.0097(16) C7 0.0421(16) 0.0467(16) 0.0416(18) 0.0083(13) -0.0097(13) -0.0047(13) C8 0.0437(17) 0.0399(16) 0.0461(19) 0.0082(14) -0.0134(14) -0.0104(13) C31 0.058(2) 0.0490(18) 0.063(2) 0.0154(15) -0.0143(17) -0.0113(15) C32 0.067(2) 0.0504(19) 0.064(3) 0.0043(17) -0.006(2) -0.0176(17) C23 0.0485(18) 0.0545(19) 0.060(2) 0.0068(16) 0.0056(16) -0.0001(15) C24 0.0487(18) 0.0445(17) 0.046(2) 0.0000(14) -0.0012(15) -0.0163(14) C15 0.0571(19) 0.0399(16) 0.051(2) 0.0089(14) -0.0181(16) -0.0092(14) C16 0.059(2) 0.0395(17) 0.070(3) 0.0144(17) -0.0136(18) -0.0050(15) C33 0.116(4) 0.146(5) 0.110(5) -0.023(4) -0.044(4) 0.036(4) C34 0.110(4) 0.136(5) 0.184(7) -0.026(5) -0.066(5) 0.031(4) O1 0.0364(10) 0.0432(10) 0.0324(11) 0.0091(8) -0.0049(8) -0.0040(8) O10 0.0514(12) 0.0430(11) 0.0378(12) 0.0057(9) -0.0099(9) -0.0068(9) O7 0.0376(10) 0.0373(10) 0.0409(12) 0.0058(8) -0.0010(9) -0.0044(8) O4 0.0461(11) 0.0269(9) 0.0461(12) 0.0016(8) -0.0078(9) -0.0084(8) O2 0.0829(16) 0.0493(12) 0.0450(14) -0.0012(10) -0.0268(12) 0.0098(11) O3 0.0535(13) 0.0638(14) 0.0503(14) 0.0098(11) -0.0168(11) 0.0054(11) O12 0.089(2) 0.128(3) 0.079(2) -0.0375(19) -0.0101(17) -0.0309(19) O11 0.156(3) 0.212(4) 0.088(3) 0.013(2) 0.003(2) -0.138(3) O9 0.0645(14) 0.0543(13) 0.0558(15) 0.0155(11) 0.0089(12) 0.0035(11) O8 0.0812(16) 0.0577(14) 0.0477(15) 0.0010(11) 0.0157(13) -0.0124(12) O5 0.0849(18) 0.0356(12) 0.092(2) 0.0091(12) -0.0041(16) -0.0127(12) O6 0.140(3) 0.0687(17) 0.076(2) 0.0367(15) -0.0329(19) -0.0262(17) O13 0.0440(13) 0.0638(15) 0.0715(17) 0.0245(12) -0.0048(13) -0.0074(12) O14 0.087(2) 0.098(2) 0.105(2) -0.0460(17) -0.0359(19) 0.0095(17) S4 0.0431(4) 0.0392(4) 0.0438(5) -0.0079(3) -0.0033(3) -0.0022(3) S1 0.0452(4) 0.0587(5) 0.0560(5) -0.0100(4) -0.0158(4) -0.0158(4) S2 0.0499(5) 0.0420(4) 0.0558(5) -0.0154(4) -0.0024(4) -0.0019(3) S3 0.0399(4) 0.0474(4) 0.0813(7) -0.0146(4) -0.0108(4) -0.0152(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 C6 O1 1.382(3) . ? C6 C1 1.389(4) . ? C6 C5 1.395(4) . ? C1 C2 1.396(4) . ? C1 S1 1.770(3) . ? C2 C3 1.374(4) . ? C2 H2 0.9300 . ? C3 C4 1.365(4) . ? C3 H32 0.9300 . ? C4 C5 1.396(4) . ? C4 H4 0.9300 . ? C5 S4 1.773(3) . ? C9 C14 1.392(4) . ? C9 C10 1.392(4) . ? C9 S4 1.777(3) . ? C10 O4 1.388(3) . ? C10 C11 1.393(4) . ? C11 C12 1.400(4) . ? C11 S3 1.769(3) . ? C12 C13 1.373(4) . ? C12 H33 0.9300 . ? C13 C14 1.372(4) . ? C13 H13 0.9300 . ? C14 H34 0.9300 . ? C17 C22 1.382(4) . ? C17 C18 1.384(4) . ? C17 S3 1.775(3) . ? C22 C21 1.387(4) . ? C22 O7 1.390(3) . ? C21 C20 1.395(4) . ? C21 S2 1.769(3) . ? C20 C19 1.362(4) . ? C20 H20 0.9300 . ? C19 C18 1.377(4) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C25 C30 1.386(4) . ? C25 C26 1.406(4) . ? C25 S2 1.773(3) . ? C26 O10 1.381(3) . ? C26 C27 1.395(4) . ? C27 C28 1.384(4) . ? C27 S1 1.780(3) . ? C28 C29 1.382(4) . ? C28 H28 0.9300 . ? C29 C30 1.361(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C7 O1 1.423(3) . ? C7 C8 1.485(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.214(3) . ? C8 O3 1.310(3) . ? C31 O10 1.435(3) . ? C31 C32 1.487(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O11 1.181(4) . ? C32 O12 1.264(4) . ? C23 O7 1.429(3) . ? C23 C24 1.498(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O8 1.204(3) . ? C24 O9 1.288(4) . ? C15 O4 1.406(3) . ? C15 C16 1.508(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O6 1.180(4) . ? C16 O5 1.328(4) . ? C33 O14 1.408(5) . ? C33 C34 1.421(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? O3 H3 0.8200 . ? O12 H12 0.8200 . ? O9 H9 0.8200 . ? O5 H5A 0.8200 . ? O13 H13B 0.818(10) . ? O13 H13A 0.815(10) . ? O14 H14 0.8200 . ? 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 C6 C1 118.8(2) . . ? O1 C6 C5 121.1(2) . . ? C1 C6 C5 120.0(2) . . ? C6 C1 C2 119.1(3) . . ? C6 C1 S1 122.8(2) . . ? C2 C1 S1 117.7(2) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H32 120.0 . . ? C2 C3 H32 120.0 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.1(2) . . ? C6 C5 S4 123.2(2) . . ? C4 C5 S4 117.4(2) . . ? C14 C9 C10 119.1(3) . . ? C14 C9 S4 117.2(2) . . ? C10 C9 S4 123.2(2) . . ? O4 C10 C9 120.2(2) . . ? O4 C10 C11 119.0(2) . . ? C9 C10 C11 120.7(2) . . ? C10 C11 C12 118.7(3) . . ? C10 C11 S3 123.7(2) . . ? C12 C11 S3 117.0(2) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H33 119.8 . . ? C11 C12 H33 119.8 . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C9 120.4(3) . . ? C13 C14 H34 119.8 . . ? C9 C14 H34 119.8 . . ? C22 C17 C18 119.7(3) . . ? C22 C17 S3 121.7(2) . . ? C18 C17 S3 118.2(2) . . ? C17 C22 C21 120.3(3) . . ? C17 C22 O7 119.0(2) . . ? C21 C22 O7 120.7(3) . . ? C22 C21 C20 118.6(3) . . ? C22 C21 S2 123.2(2) . . ? C20 C21 S2 117.8(2) . . ? C19 C20 C21 121.2(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C30 C25 C26 118.8(3) . . ? C30 C25 S2 116.8(2) . . ? C26 C25 S2 124.1(2) . . ? O10 C26 C27 118.3(2) . . ? O10 C26 C25 122.4(3) . . ? C27 C26 C25 119.2(3) . . ? C28 C27 C26 120.1(3) . . ? C28 C27 S1 116.4(2) . . ? C26 C27 S1 123.1(2) . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 119.7(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C25 121.8(3) . . ? C29 C30 H30 119.1 . . ? C25 C30 H30 119.1 . . ? O1 C7 C8 110.6(2) . . ? O1 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? O2 C8 O3 124.5(3) . . ? O2 C8 C7 123.7(3) . . ? O3 C8 C7 111.7(3) . . ? O10 C31 C32 113.2(3) . . ? O10 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? O10 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.8 . . ? O11 C32 O12 122.2(4) . . ? O11 C32 C31 123.5(4) . . ? O12 C32 C31 114.3(3) . . ? O7 C23 C24 112.6(2) . . ? O7 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? O7 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? O8 C24 O9 125.2(3) . . ? O8 C24 C23 119.6(3) . . ? O9 C24 C23 115.1(3) . . ? O4 C15 C16 109.6(3) . . ? O4 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? O4 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? O6 C16 O5 121.2(3) . . ? O6 C16 C15 123.0(3) . . ? O5 C16 C15 115.8(3) . . ? O14 C33 C34 113.3(5) . . ? O14 C33 H33A 108.9 . . ? C34 C33 H33A 108.9 . . ? O14 C33 H33B 108.9 . . ? C34 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C6 O1 C7 114.97(19) . . ? C26 O10 C31 118.2(2) . . ? C22 O7 C23 111.6(2) . . ? C10 O4 C15 116.03(19) . . ? C8 O3 H3 109.5 . . ? C32 O12 H12 109.5 . . ? C24 O9 H9 109.5 . . ? C16 O5 H5A 109.5 . . ? H13B O13 H13A 118(4) . . ? C33 O14 H14 109.5 . . ? C5 S4 C9 106.82(12) . . ? C1 S1 C27 106.82(13) . . ? C21 S2 C25 105.96(13) . . ? C11 S3 C17 107.00(12) . . ? 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 O1 C6 C1 C2 -176.3(2) . . . . ? C5 C6 C1 C2 4.0(4) . . . . ? O1 C6 C1 S1 -3.3(3) . . . . ? C5 C6 C1 S1 177.1(2) . . . . ? C6 C1 C2 C3 0.3(4) . . . . ? S1 C1 C2 C3 -173.2(2) . . . . ? C1 C2 C3 C4 -3.6(5) . . . . ? C2 C3 C4 C5 2.6(4) . . . . ? O1 C6 C5 C4 175.4(2) . . . . ? C1 C6 C5 C4 -4.9(4) . . . . ? O1 C6 C5 S4 2.2(3) . . . . ? C1 C6 C5 S4 -178.18(19) . . . . ? C3 C4 C5 C6 1.6(4) . . . . ? C3 C4 C5 S4 175.3(2) . . . . ? C14 C9 C10 O4 -176.2(2) . . . . ? S4 C9 C10 O4 12.2(4) . . . . ? C14 C9 C10 C11 1.2(4) . . . . ? S4 C9 C10 C11 -170.4(2) . . . . ? O4 C10 C11 C12 174.5(2) . . . . ? C9 C10 C11 C12 -3.0(4) . . . . ? O4 C10 C11 S3 -15.7(4) . . . . ? C9 C10 C11 S3 166.9(2) . . . . ? C10 C11 C12 C13 3.3(4) . . . . ? S3 C11 C12 C13 -167.2(2) . . . . ? C11 C12 C13 C14 -1.9(5) . . . . ? C12 C13 C14 C9 0.1(5) . . . . ? C10 C9 C14 C13 0.2(4) . . . . ? S4 C9 C14 C13 172.4(2) . . . . ? C18 C17 C22 C21 4.5(4) . . . . ? S3 C17 C22 C21 177.8(2) . . . . ? C18 C17 C22 O7 -174.9(2) . . . . ? S3 C17 C22 O7 -1.5(3) . . . . ? C17 C22 C21 C20 -3.6(4) . . . . ? O7 C22 C21 C20 175.7(2) . . . . ? C17 C22 C21 S2 -176.0(2) . . . . ? O7 C22 C21 S2 3.4(4) . . . . ? C22 C21 C20 C19 0.4(4) . . . . ? S2 C21 C20 C19 173.1(2) . . . . ? C21 C20 C19 C18 2.0(5) . . . . ? C20 C19 C18 C17 -1.1(5) . . . . ? C22 C17 C18 C19 -2.1(4) . . . . ? S3 C17 C18 C19 -175.7(2) . . . . ? C30 C25 C26 O10 -178.7(2) . . . . ? S2 C25 C26 O10 7.8(4) . . . . ? C30 C25 C26 C27 -2.4(4) . . . . ? S2 C25 C26 C27 -175.87(19) . . . . ? O10 C26 C27 C28 178.2(2) . . . . ? C25 C26 C27 C28 1.7(4) . . . . ? O10 C26 C27 S1 -9.9(3) . . . . ? C25 C26 C27 S1 173.60(19) . . . . ? C26 C27 C28 C29 0.7(4) . . . . ? S1 C27 C28 C29 -171.7(2) . . . . ? C27 C28 C29 C30 -2.5(4) . . . . ? C28 C29 C30 C25 1.7(5) . . . . ? C26 C25 C30 C29 0.7(4) . . . . ? S2 C25 C30 C29 174.6(2) . . . . ? O1 C7 C8 O2 -6.3(4) . . . . ? O1 C7 C8 O3 176.0(2) . . . . ? O10 C31 C32 O11 -94.6(5) . . . . ? O10 C31 C32 O12 83.0(4) . . . . ? O7 C23 C24 O8 -162.6(3) . . . . ? O7 C23 C24 O9 20.8(4) . . . . ? O4 C15 C16 O6 -173.1(3) . . . . ? O4 C15 C16 O5 6.8(4) . . . . ? C1 C6 O1 C7 109.4(3) . . . . ? C5 C6 O1 C7 -70.9(3) . . . . ? C8 C7 O1 C6 -138.1(2) . . . . ? C27 C26 O10 C31 116.0(3) . . . . ? C25 C26 O10 C31 -67.6(3) . . . . ? C32 C31 O10 C26 -75.8(4) . . . . ? C17 C22 O7 C23 97.7(3) . . . . ? C21 C22 O7 C23 -81.7(3) . . . . ? C24 C23 O7 C22 -168.7(3) . . . . ? C9 C10 O4 C15 -84.1(3) . . . . ? C11 C10 O4 C15 98.4(3) . . . . ? C16 C15 O4 C10 172.1(2) . . . . ? C6 C5 S4 C9 -54.4(2) . . . . ? C4 C5 S4 C9 132.2(2) . . . . ? C14 C9 S4 C5 136.4(2) . . . . ? C10 C9 S4 C5 -51.8(3) . . . . ? C6 C1 S1 C27 62.2(3) . . . . ? C2 C1 S1 C27 -124.6(2) . . . . ? C28 C27 S1 C1 -136.3(2) . . . . ? C26 C27 S1 C1 51.6(2) . . . . ? C22 C21 S2 C25 -59.0(3) . . . . ? C20 C21 S2 C25 128.6(2) . . . . ? C30 C25 S2 C21 132.8(2) . . . . ? C26 C25 S2 C21 -53.6(2) . . . . ? C10 C11 S3 C17 48.9(3) . . . . ? C12 C11 S3 C17 -141.1(2) . . . . ? C22 C17 S3 C11 60.3(3) . . . . ? C18 C17 S3 C11 -126.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13A O1 0.815(10) 2.13(2) 2.883(3) 154(4) . O13 H13B O9 0.818(10) 2.39(3) 2.881(3) 119(3) . O9 H9 O13 0.82 1.72 2.536(3) 170.9 2_665 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.427 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.059 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 832092' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H32 O14 S4' _chemical_formula_weight 804.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0799(16) _cell_length_b 10.1897(17) _cell_length_c 20.368(3) _cell_angle_alpha 98.999(2) _cell_angle_beta 90.299(2) _cell_angle_gamma 115.445(2) _cell_volume 1859.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9265 _exptl_absorpt_correction_T_max 0.9382 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10488 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7198 _reflns_number_gt 5492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.8346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0061(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7198 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C26 C 0.8337(2) 0.5750(2) 0.31831(10) 0.0387(5) Uani 1 1 d . . . C25 C 0.7852(2) 0.4546(3) 0.35114(11) 0.0432(5) Uani 1 1 d . . . C30 C 0.8032(3) 0.4785(3) 0.42028(12) 0.0530(6) Uani 1 1 d . . . H30 H 0.7696 0.3986 0.4426 0.064 Uiso 1 1 calc R . . C29 C 0.8706(3) 0.6198(3) 0.45579(12) 0.0566(7) Uani 1 1 d . . . H29 H 0.8842 0.6349 0.5020 0.068 Uiso 1 1 calc R . . C28 C 0.9181(3) 0.7392(3) 0.42363(12) 0.0512(6) Uani 1 1 d . . . H28 H 0.9636 0.8344 0.4482 0.061 Uiso 1 1 calc R . . C27 C 0.8986(2) 0.7185(3) 0.35471(11) 0.0411(5) Uani 1 1 d . . . C31 C 0.9386(3) 0.5443(3) 0.21753(11) 0.0572(7) Uani 1 1 d . . . H31A H 0.9536 0.4629 0.2294 0.069 Uiso 1 1 calc R . . H31B H 1.0273 0.6347 0.2323 0.069 Uiso 1 1 calc R . . C32 C 0.9093(3) 0.5214(4) 0.14358(13) 0.0636(8) Uani 1 1 d . . . C1 C 0.8403(2) 0.8614(2) 0.25814(10) 0.0400(5) Uani 1 1 d . . . C2 C 0.8747(3) 0.8749(3) 0.19270(12) 0.0503(6) Uani 1 1 d . . . H2 H 0.9659 0.8826 0.1800 0.060 Uiso 1 1 calc R . . C3 C 0.7765(3) 0.8772(3) 0.14665(12) 0.0535(6) Uani 1 1 d . . . H6 H 0.8022 0.8894 0.1035 0.064 Uiso 1 1 calc R . . C4 C 0.6402(3) 0.8614(3) 0.16446(11) 0.0487(6) Uani 1 1 d . . . H4 H 0.5727 0.8604 0.1328 0.058 Uiso 1 1 calc R . . C5 C 0.6018(2) 0.8469(2) 0.22915(10) 0.0393(5) Uani 1 1 d . . . C6 C 0.7044(2) 0.8516(2) 0.27674(10) 0.0353(5) Uani 1 1 d . . . C7 C 0.7384(3) 0.9753(2) 0.38857(11) 0.0461(5) Uani 1 1 d . . . H7A H 0.7771 1.0589 0.3655 0.055 Uiso 1 1 calc R . . H7B H 0.8200 0.9738 0.4133 0.055 Uiso 1 1 calc R . . C8 C 0.6312(3) 0.9904(3) 0.43513(10) 0.0460(6) Uani 1 1 d . . . C9 C 0.3341(2) 0.6796(3) 0.28309(10) 0.0401(5) Uani 1 1 d . . . C10 C 0.3162(2) 0.5414(2) 0.25122(9) 0.0365(5) Uani 1 1 d . . . C11 C 0.2265(2) 0.4150(3) 0.27662(10) 0.0424(5) Uani 1 1 d . . . C12 C 0.1558(2) 0.4305(3) 0.33381(12) 0.0540(7) Uani 1 1 d . . . H33 H 0.0973 0.3475 0.3516 0.065 Uiso 1 1 calc R . . C13 C 0.1717(3) 0.5668(3) 0.36409(12) 0.0576(7) Uani 1 1 d . . . H13 H 0.1223 0.5753 0.4018 0.069 Uiso 1 1 calc R . . C14 C 0.2595(2) 0.6902(3) 0.33935(11) 0.0497(6) Uani 1 1 d . . . H14 H 0.2695 0.7821 0.3604 0.060 Uiso 1 1 calc R . . C15 C 0.3049(3) 0.5057(3) 0.13537(10) 0.0529(6) Uani 1 1 d . . . H15A H 0.2769 0.5858 0.1358 0.064 Uiso 1 1 calc R . . H15B H 0.2157 0.4141 0.1313 0.064 Uiso 1 1 calc R . . C16 C 0.3939(3) 0.4992(3) 0.07748(11) 0.0452(5) Uani 1 1 d . . . C17 C 0.3474(3) 0.2284(2) 0.21504(11) 0.0458(6) Uani 1 1 d . . . C22 C 0.4566(2) 0.2562(2) 0.26436(10) 0.0392(5) Uani 1 1 d . . . C21 C 0.5853(3) 0.2455(2) 0.24682(12) 0.0458(5) Uani 1 1 d . . . C20 C 0.5993(3) 0.1987(3) 0.18036(13) 0.0580(7) Uani 1 1 d . . . H20 H 0.6843 0.1896 0.1685 0.070 Uiso 1 1 calc R . . C19 C 0.4890(4) 0.1659(3) 0.13236(13) 0.0655(8) Uani 1 1 d . . . H19 H 0.4980 0.1320 0.0883 0.079 Uiso 1 1 calc R . . C18 C 0.3650(3) 0.1830(3) 0.14920(12) 0.0594(7) Uani 1 1 d . . . H18 H 0.2920 0.1640 0.1161 0.071 Uiso 1 1 calc R . . C23 C 0.3583(3) 0.1657(3) 0.35966(12) 0.0566(7) Uani 1 1 d . . . H23A H 0.4047 0.0994 0.3514 0.068 Uiso 1 1 calc R . . H23B H 0.2589 0.1146 0.3382 0.068 Uiso 1 1 calc R . . C24 C 0.3508(3) 0.2023(3) 0.43270(11) 0.0484(6) Uani 1 1 d . . . C33 C 0.0429(6) 0.8167(7) -0.0018(4) 0.185(3) Uani 1 1 d . . . H33A H 0.0210 0.8876 0.0271 0.278 Uiso 1 1 calc R . . H33B H -0.0024 0.7231 0.0128 0.278 Uiso 1 1 calc R . . H33C H 0.0052 0.8065 -0.0466 0.278 Uiso 1 1 calc R . . C34 C 0.2014(5) 0.8664(5) 0.00037(17) 0.0937(11) Uani 1 1 d . . . C35 C 0.2675(6) 0.7858(5) 0.0309(2) 0.1337(17) Uani 1 1 d . . . H35A H 0.2329 0.6877 0.0058 0.201 Uiso 1 1 calc R . . H35B H 0.2402 0.7807 0.0759 0.201 Uiso 1 1 calc R . . H35C H 0.3728 0.8360 0.0313 0.201 Uiso 1 1 calc R . . H13A H 0.506(4) 0.513(4) 0.3966(17) 0.096(13) Uiso 1 1 d . . . H13B H 0.538(3) 0.652(4) 0.3904(15) 0.072(11) Uiso 1 1 d . . . O10 O 0.81692(15) 0.55337(17) 0.24952(7) 0.0410(4) Uani 1 1 d . . . O12 O 0.7877(2) 0.5185(3) 0.11994(8) 0.0681(5) Uani 1 1 d . . . H12 H 0.7396 0.5296 0.1508 0.102 Uiso 1 1 calc R . . O11 O 0.9947(3) 0.5075(4) 0.10710(11) 0.1305(13) Uani 1 1 d . . . O1 O 0.66683(16) 0.84159(16) 0.34129(7) 0.0411(4) Uani 1 1 d . . . O2 O 0.5093(2) 0.8933(2) 0.43713(8) 0.0624(5) Uani 1 1 d . . . O3 O 0.6868(2) 1.11990(18) 0.47473(8) 0.0615(5) Uani 1 1 d . . . H3 H 0.6278 1.1222 0.5019 0.092 Uiso 1 1 calc R . . O4 O 0.38953(15) 0.52857(16) 0.19529(6) 0.0381(3) Uani 1 1 d . . . O6 O 0.51895(18) 0.5183(2) 0.08201(8) 0.0600(5) Uani 1 1 d . . . O5 O 0.3159(2) 0.4700(3) 0.02157(8) 0.0915(8) Uani 1 1 d . . . H5 H 0.3670 0.4698 -0.0096 0.137 Uiso 1 1 calc R . . O7 O 0.43921(16) 0.29416(15) 0.33068(7) 0.0412(4) Uani 1 1 d . . . O9 O 0.4539(2) 0.3284(2) 0.46094(8) 0.0678(6) Uani 1 1 d . . . H9A H 0.4462 0.3400 0.5013 0.102 Uiso 1 1 calc R . . O8 O 0.2585(2) 0.1160(2) 0.46135(9) 0.0786(6) Uani 1 1 d . . . O14 O 0.2791(4) 0.9746(4) -0.02101(17) 0.1610(15) Uani 1 1 d . . . O13 O 0.5247(2) 0.5988(3) 0.41227(9) 0.0606(5) Uani 1 1 d . . . S1 S 0.97965(6) 0.87596(7) 0.31584(3) 0.05162(18) Uani 1 1 d . . . S4 S 0.42995(7) 0.84361(7) 0.25018(3) 0.05105(17) Uani 1 1 d . . . S3 S 0.17853(7) 0.23407(7) 0.23382(3) 0.05559(19) Uani 1 1 d . . . S2 S 0.72378(8) 0.27127(7) 0.30778(4) 0.05988(19) 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 C26 0.0305(10) 0.0515(13) 0.0386(11) 0.0114(10) 0.0014(8) 0.0209(10) C25 0.0353(11) 0.0493(14) 0.0515(13) 0.0178(11) 0.0048(9) 0.0215(10) C30 0.0484(14) 0.0690(18) 0.0524(14) 0.0281(13) 0.0101(11) 0.0297(13) C29 0.0620(16) 0.080(2) 0.0378(13) 0.0151(13) 0.0057(11) 0.0384(15) C28 0.0500(14) 0.0609(16) 0.0447(13) 0.0035(11) -0.0021(10) 0.0279(12) C27 0.0305(11) 0.0490(13) 0.0448(12) 0.0120(10) 0.0017(9) 0.0169(10) C31 0.0438(13) 0.092(2) 0.0440(13) 0.0120(13) 0.0031(10) 0.0379(14) C32 0.0517(15) 0.102(2) 0.0493(15) 0.0166(14) 0.0042(12) 0.0440(16) C1 0.0410(12) 0.0321(11) 0.0413(12) 0.0097(9) 0.0020(9) 0.0097(9) C2 0.0491(14) 0.0472(14) 0.0503(14) 0.0159(11) 0.0165(11) 0.0145(11) C3 0.0666(17) 0.0547(15) 0.0388(12) 0.0167(11) 0.0130(11) 0.0230(13) C4 0.0628(15) 0.0473(14) 0.0373(12) 0.0118(10) 0.0005(11) 0.0237(12) C5 0.0471(12) 0.0324(11) 0.0410(12) 0.0080(9) 0.0030(9) 0.0192(10) C6 0.0438(12) 0.0280(10) 0.0324(10) 0.0066(8) 0.0039(9) 0.0137(9) C7 0.0581(14) 0.0391(13) 0.0383(12) 0.0022(9) -0.0005(10) 0.0202(11) C8 0.0659(16) 0.0440(14) 0.0310(11) 0.0015(10) -0.0031(10) 0.0285(13) C9 0.0367(11) 0.0550(14) 0.0347(11) 0.0039(10) -0.0004(9) 0.0270(10) C10 0.0302(10) 0.0539(13) 0.0300(10) 0.0073(9) 0.0018(8) 0.0226(10) C11 0.0310(11) 0.0558(14) 0.0380(11) 0.0090(10) -0.0006(9) 0.0164(10) C12 0.0356(12) 0.0805(19) 0.0448(13) 0.0210(13) 0.0069(10) 0.0207(12) C13 0.0427(13) 0.098(2) 0.0354(12) 0.0060(13) 0.0076(10) 0.0359(14) C14 0.0418(13) 0.0740(18) 0.0388(12) -0.0016(11) 0.0000(10) 0.0341(13) C15 0.0445(13) 0.091(2) 0.0330(11) 0.0102(12) 0.0050(9) 0.0386(13) C16 0.0448(13) 0.0585(15) 0.0357(12) 0.0079(10) 0.0054(10) 0.0258(11) C17 0.0545(14) 0.0322(12) 0.0398(12) 0.0012(9) -0.0031(10) 0.0104(10) C22 0.0501(13) 0.0249(10) 0.0374(11) 0.0055(8) 0.0039(9) 0.0114(9) C21 0.0561(14) 0.0299(11) 0.0511(13) 0.0087(10) 0.0068(11) 0.0180(10) C20 0.0697(17) 0.0436(14) 0.0631(16) 0.0056(12) 0.0202(14) 0.0279(13) C19 0.093(2) 0.0541(16) 0.0426(14) -0.0025(12) 0.0111(14) 0.0292(15) C18 0.0792(19) 0.0488(15) 0.0394(13) -0.0005(11) -0.0061(12) 0.0208(14) C23 0.0671(16) 0.0390(13) 0.0467(13) 0.0114(11) 0.0038(12) 0.0061(12) C24 0.0513(14) 0.0472(14) 0.0447(13) 0.0188(11) 0.0033(11) 0.0161(12) C33 0.125(5) 0.151(5) 0.295(9) 0.047(5) 0.042(5) 0.072(4) C34 0.123(3) 0.083(3) 0.064(2) 0.0143(18) -0.002(2) 0.034(2) C35 0.173(5) 0.109(4) 0.122(4) 0.030(3) -0.017(3) 0.061(3) O10 0.0354(8) 0.0529(9) 0.0377(8) 0.0100(7) 0.0002(6) 0.0216(7) O12 0.0621(12) 0.1123(16) 0.0427(9) 0.0128(10) -0.0007(8) 0.0504(12) O11 0.1018(18) 0.284(4) 0.0554(13) 0.0237(18) 0.0196(13) 0.132(2) O1 0.0536(9) 0.0366(8) 0.0304(7) 0.0051(6) 0.0063(6) 0.0172(7) O2 0.0611(11) 0.0657(12) 0.0460(10) -0.0126(8) 0.0049(8) 0.0218(10) O3 0.0851(13) 0.0441(10) 0.0478(10) -0.0021(8) 0.0122(9) 0.0244(9) O4 0.0352(8) 0.0523(9) 0.0307(7) 0.0057(6) 0.0062(6) 0.0232(7) O6 0.0466(10) 0.0997(15) 0.0385(9) 0.0063(9) 0.0092(7) 0.0383(10) O5 0.0625(12) 0.190(3) 0.0342(9) 0.0166(13) 0.0075(8) 0.0673(15) O7 0.0487(9) 0.0348(8) 0.0327(7) 0.0064(6) 0.0036(6) 0.0113(7) O9 0.0867(14) 0.0526(11) 0.0391(9) 0.0077(8) 0.0127(9) 0.0071(10) O8 0.0728(13) 0.0786(14) 0.0563(11) 0.0294(10) 0.0065(9) 0.0009(11) O14 0.155(3) 0.164(3) 0.144(3) 0.091(3) -0.020(2) 0.030(3) O13 0.0900(15) 0.0441(12) 0.0440(10) 0.0105(9) 0.0020(9) 0.0250(11) S1 0.0343(3) 0.0486(4) 0.0623(4) 0.0164(3) -0.0025(3) 0.0069(3) S4 0.0565(4) 0.0521(4) 0.0583(4) 0.0115(3) 0.0042(3) 0.0359(3) S3 0.0419(3) 0.0491(4) 0.0597(4) 0.0074(3) -0.0072(3) 0.0057(3) S2 0.0625(4) 0.0479(4) 0.0791(5) 0.0162(3) -0.0022(3) 0.0317(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 C26 O10 1.382(2) . ? C26 C25 1.392(3) . ? C26 C27 1.396(3) . ? C25 C30 1.388(3) . ? C25 S2 1.771(2) . ? C30 C29 1.374(4) . ? C30 H30 0.9300 . ? C29 C28 1.375(4) . ? C29 H29 0.9300 . ? C28 C27 1.386(3) . ? C28 H28 0.9300 . ? C27 S1 1.774(2) . ? C31 O10 1.423(3) . ? C31 C32 1.495(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O11 1.180(3) . ? C32 O12 1.301(3) . ? C1 C6 1.388(3) . ? C1 C2 1.392(3) . ? C1 S1 1.768(2) . ? C2 C3 1.370(3) . ? C2 H2 0.9300 . ? C3 C4 1.371(3) . ? C3 H6 0.9300 . ? C4 C5 1.387(3) . ? C4 H4 0.9300 . ? C5 C6 1.394(3) . ? C5 S4 1.774(2) . ? C6 O1 1.377(2) . ? C7 O1 1.429(3) . ? C7 C8 1.482(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.208(3) . ? C8 O3 1.317(3) . ? C9 C14 1.389(3) . ? C9 C10 1.390(3) . ? C9 S4 1.773(2) . ? C10 O4 1.381(2) . ? C10 C11 1.399(3) . ? C11 C12 1.392(3) . ? C11 S3 1.767(2) . ? C12 C13 1.369(4) . ? C12 H33 0.9300 . ? C13 C14 1.366(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.415(2) . ? C15 C16 1.496(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O6 1.190(3) . ? C16 O5 1.299(3) . ? C17 C18 1.386(3) . ? C17 C22 1.390(3) . ? C17 S3 1.770(3) . ? C22 O7 1.379(2) . ? C22 C21 1.392(3) . ? C21 C20 1.392(3) . ? C21 S2 1.767(3) . ? C20 C19 1.368(4) . ? C20 H20 0.9300 . ? C19 C18 1.373(4) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C23 O7 1.434(3) . ? C23 C24 1.487(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O8 1.201(3) . ? C24 O9 1.295(3) . ? C33 C34 1.452(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O14 1.196(4) . ? C34 C35 1.460(6) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? O12 H12 0.8200 . ? O3 H3 0.8200 . ? O5 H5 0.8200 . ? O9 H9A 0.8200 . ? O13 H13A 0.82(4) . ? O13 H13B 0.72(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 C26 C25 120.2(2) . . ? O10 C26 C27 119.57(19) . . ? C25 C26 C27 120.20(19) . . ? C30 C25 C26 119.4(2) . . ? C30 C25 S2 117.88(18) . . ? C26 C25 S2 122.14(17) . . ? C29 C30 C25 120.2(2) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C30 C29 C28 120.6(2) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C28 C27 120.3(2) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C27 C26 119.2(2) . . ? C28 C27 S1 117.95(18) . . ? C26 C27 S1 122.32(16) . . ? O10 C31 C32 109.64(19) . . ? O10 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O10 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O11 C32 O12 120.3(2) . . ? O11 C32 C31 121.1(2) . . ? O12 C32 C31 118.6(2) . . ? C6 C1 C2 119.0(2) . . ? C6 C1 S1 122.82(16) . . ? C2 C1 S1 117.85(18) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H6 120.1 . . ? C4 C3 H6 120.1 . . ? C3 C4 C5 120.7(2) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.4(2) . . ? C4 C5 S4 117.94(17) . . ? C6 C5 S4 122.23(16) . . ? O1 C6 C1 121.09(18) . . ? O1 C6 C5 119.01(19) . . ? C1 C6 C5 119.86(18) . . ? O1 C7 C8 109.44(19) . . ? O1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? O2 C8 O3 124.7(2) . . ? O2 C8 C7 123.5(2) . . ? O3 C8 C7 111.8(2) . . ? C14 C9 C10 119.3(2) . . ? C14 C9 S4 116.95(18) . . ? C10 C9 S4 123.32(16) . . ? O4 C10 C9 120.18(19) . . ? O4 C10 C11 119.73(19) . . ? C9 C10 C11 120.08(19) . . ? C12 C11 C10 118.9(2) . . ? C12 C11 S3 117.53(19) . . ? C10 C11 S3 123.04(16) . . ? C13 C12 C11 120.6(2) . . ? C13 C12 H33 119.7 . . ? C11 C12 H33 119.7 . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C9 120.6(2) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O4 C15 C16 109.28(18) . . ? O4 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? O4 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? O6 C16 O5 124.7(2) . . ? O6 C16 C15 124.7(2) . . ? O5 C16 C15 110.6(2) . . ? C18 C17 C22 119.4(2) . . ? C18 C17 S3 118.12(19) . . ? C22 C17 S3 122.25(17) . . ? O7 C22 C17 120.9(2) . . ? O7 C22 C21 119.35(19) . . ? C17 C22 C21 119.8(2) . . ? C20 C21 C22 119.4(2) . . ? C20 C21 S2 118.7(2) . . ? C22 C21 S2 121.56(17) . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C18 C17 120.7(2) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? O7 C23 C24 112.54(19) . . ? O7 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? O7 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? O8 C24 O9 125.1(2) . . ? O8 C24 C23 120.6(2) . . ? O9 C24 C23 114.3(2) . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O14 C34 C33 121.0(5) . . ? O14 C34 C35 119.4(5) . . ? C33 C34 C35 119.5(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C26 O10 C31 114.04(16) . . ? C32 O12 H12 109.5 . . ? C6 O1 C7 115.25(16) . . ? C8 O3 H3 109.5 . . ? C10 O4 C15 112.55(15) . . ? C16 O5 H5 109.5 . . ? C22 O7 C23 111.32(16) . . ? C24 O9 H9A 109.5 . . ? H13A O13 H13B 120(3) . . ? C1 S1 C27 105.56(10) . . ? C9 S4 C5 106.28(10) . . ? C11 S3 C17 105.64(10) . . ? C21 S2 C25 105.80(10) . . ? 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 O10 C26 C25 C30 179.90(19) . . . . ? C27 C26 C25 C30 -0.6(3) . . . . ? O10 C26 C25 S2 8.7(3) . . . . ? C27 C26 C25 S2 -171.82(16) . . . . ? C26 C25 C30 C29 -1.1(3) . . . . ? S2 C25 C30 C29 170.52(19) . . . . ? C25 C30 C29 C28 1.4(4) . . . . ? C30 C29 C28 C27 0.0(4) . . . . ? C29 C28 C27 C26 -1.7(3) . . . . ? C29 C28 C27 S1 -173.43(19) . . . . ? O10 C26 C27 C28 -178.54(19) . . . . ? C25 C26 C27 C28 2.0(3) . . . . ? O10 C26 C27 S1 -7.2(3) . . . . ? C25 C26 C27 S1 173.35(16) . . . . ? O10 C31 C32 O11 -178.3(3) . . . . ? O10 C31 C32 O12 2.4(4) . . . . ? C6 C1 C2 C3 -0.7(3) . . . . ? S1 C1 C2 C3 -174.51(19) . . . . ? C1 C2 C3 C4 -2.0(4) . . . . ? C2 C3 C4 C5 1.6(4) . . . . ? C3 C4 C5 C6 1.4(3) . . . . ? C3 C4 C5 S4 174.43(19) . . . . ? C2 C1 C6 O1 -178.47(19) . . . . ? S1 C1 C6 O1 -4.9(3) . . . . ? C2 C1 C6 C5 3.7(3) . . . . ? S1 C1 C6 C5 177.22(16) . . . . ? C4 C5 C6 O1 178.06(19) . . . . ? S4 C5 C6 O1 5.3(3) . . . . ? C4 C5 C6 C1 -4.1(3) . . . . ? S4 C5 C6 C1 -176.80(16) . . . . ? O1 C7 C8 O2 9.2(3) . . . . ? O1 C7 C8 O3 -172.52(18) . . . . ? C14 C9 C10 O4 -179.90(18) . . . . ? S4 C9 C10 O4 8.1(3) . . . . ? C14 C9 C10 C11 -1.4(3) . . . . ? S4 C9 C10 C11 -173.36(15) . . . . ? O4 C10 C11 C12 178.71(18) . . . . ? C9 C10 C11 C12 0.2(3) . . . . ? O4 C10 C11 S3 -9.9(3) . . . . ? C9 C10 C11 S3 171.62(16) . . . . ? C10 C11 C12 C13 1.1(3) . . . . ? S3 C11 C12 C13 -170.74(18) . . . . ? C11 C12 C13 C14 -1.3(4) . . . . ? C12 C13 C14 C9 0.1(3) . . . . ? C10 C9 C14 C13 1.3(3) . . . . ? S4 C9 C14 C13 173.75(17) . . . . ? O4 C15 C16 O6 -3.7(4) . . . . ? O4 C15 C16 O5 176.4(2) . . . . ? C18 C17 C22 O7 -176.7(2) . . . . ? S3 C17 C22 O7 -1.9(3) . . . . ? C18 C17 C22 C21 3.2(3) . . . . ? S3 C17 C22 C21 177.89(16) . . . . ? O7 C22 C21 C20 176.19(19) . . . . ? C17 C22 C21 C20 -3.6(3) . . . . ? O7 C22 C21 S2 2.8(3) . . . . ? C17 C22 C21 S2 -177.00(16) . . . . ? C22 C21 C20 C19 1.1(4) . . . . ? S2 C21 C20 C19 174.7(2) . . . . ? C21 C20 C19 C18 1.9(4) . . . . ? C20 C19 C18 C17 -2.3(4) . . . . ? C22 C17 C18 C19 -0.2(4) . . . . ? S3 C17 C18 C19 -175.1(2) . . . . ? O7 C23 C24 O8 160.8(2) . . . . ? O7 C23 C24 O9 -22.0(3) . . . . ? C25 C26 O10 C31 -90.4(2) . . . . ? C27 C26 O10 C31 90.1(2) . . . . ? C32 C31 O10 C26 -179.8(2) . . . . ? C1 C6 O1 C7 74.0(2) . . . . ? C5 C6 O1 C7 -108.1(2) . . . . ? C8 C7 O1 C6 139.35(19) . . . . ? C9 C10 O4 C15 -92.3(2) . . . . ? C11 C10 O4 C15 89.2(2) . . . . ? C16 C15 O4 C10 177.71(19) . . . . ? C17 C22 O7 C23 84.6(2) . . . . ? C21 C22 O7 C23 -95.2(2) . . . . ? C24 C23 O7 C22 174.2(2) . . . . ? C6 C1 S1 C27 57.5(2) . . . . ? C2 C1 S1 C27 -128.93(19) . . . . ? C28 C27 S1 C1 -133.12(18) . . . . ? C26 C27 S1 C1 55.4(2) . . . . ? C14 C9 S4 C5 137.57(17) . . . . ? C10 C9 S4 C5 -50.3(2) . . . . ? C4 C5 S4 C9 125.44(18) . . . . ? C6 C5 S4 C9 -61.7(2) . . . . ? C12 C11 S3 C17 -134.92(18) . . . . ? C10 C11 S3 C17 53.6(2) . . . . ? C18 C17 S3 C11 -125.78(19) . . . . ? C22 C17 S3 C11 59.4(2) . . . . ? C20 C21 S2 C25 125.14(19) . . . . ? C22 C21 S2 C25 -61.5(2) . . . . ? C30 C25 S2 C21 134.81(19) . . . . ? C26 C25 S2 C21 -53.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O13 0.82 1.75 2.554(3) 165.3 2_666 O5 H5 O6 0.82 1.86 2.680(2) 175.6 2_665 O3 H3 O2 0.82 1.83 2.651(2) 173.9 2_676 O12 H12 O10 0.82 2.09 2.605(2) 120.5 . O13 H13B O2 0.72(3) 2.63(3) 3.035(3) 118(3) . O13 H13B O1 0.72(3) 2.21(3) 2.891(3) 157(3) . O13 H13A O9 0.82(4) 2.34(4) 2.874(3) 124(3) . O13 H13A O7 0.82(4) 2.24(4) 3.036(3) 166(3) . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.323 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.042 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 832093' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H44 N4 O14 S4' _chemical_formula_weight 1077.15 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' N N 0.0061 0.0033 '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 Pban loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x, -y+1/2, -z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x, y-1/2, z' 'x-1/2, -y, z' _cell_length_a 7.9311(7) _cell_length_b 19.6432(17) _cell_length_c 15.5657(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2425.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9682 _exptl_absorpt_correction_T_max 0.9734 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14971 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2932 _reflns_number_gt 2682 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A few of commands for restraints were applied on the atoms, the details are as follows: DFIX 0.82 0.01 O2 H2A ISOR 0.01 0.01 O4 ; _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^)+(0.0458P)^2^+28.7217P] 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 2932 _refine_ls_number_parameters 179 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.1231 _refine_ls_wR_factor_ref 0.2913 _refine_ls_wR_factor_gt 0.2887 _refine_ls_goodness_of_fit_ref 1.269 _refine_ls_restrained_S_all 1.268 _refine_ls_shift/su_max 0.004 _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 0.7500 0.94965(10) 0.0000 0.0199(5) Uani 1 2 d S . . O1 O 0.5997(5) 0.8583(2) 0.1404(3) 0.0184(9) Uani 1 1 d . . . O2 O 0.3825(8) 0.8510(3) 0.2723(4) 0.0368(13) Uani 1 1 d D . . O3 O 0.3380(7) 0.9630(3) 0.2698(4) 0.0418(15) Uani 1 1 d . . . C1 C 0.8585(7) 0.8912(3) 0.0675(4) 0.0172(11) Uani 1 1 d . . . C2 C 1.0317(8) 0.8825(3) 0.0582(4) 0.0209(12) Uani 1 1 d . . . H2 H 1.0899 0.9093 0.0189 0.025 Uiso 1 1 calc R . . C3 C 1.1188(7) 0.8352(3) 0.1059(4) 0.0208(12) Uani 1 1 d . . . H3 H 1.2348 0.8305 0.0997 0.025 Uiso 1 1 calc R . . C4 C 1.0307(8) 0.7946(3) 0.1634(4) 0.0214(12) Uani 1 1 d . . . H4 H 1.0882 0.7614 0.1945 0.026 Uiso 1 1 calc R . . C5 C 0.8586(7) 0.8024(3) 0.1755(4) 0.0161(11) Uani 1 1 d . . . C6 C 0.7720(8) 0.8520(3) 0.1290(4) 0.0185(12) Uani 1 1 d . . . C7 C 0.5434(8) 0.9214(3) 0.1765(4) 0.0243(13) Uani 1 1 d . . . H7A H 0.4958 0.9496 0.1314 0.029 Uiso 1 1 calc R . . H7B H 0.6388 0.9454 0.2009 0.029 Uiso 1 1 calc R . . C8 C 0.4126(9) 0.9098(3) 0.2453(4) 0.0259(14) Uani 1 1 d . . . S2 S 0.7500 0.7500 0.25068(13) 0.0203(5) Uani 1 2 d S . . C9 C -0.0129(9) 0.9038(4) 0.3469(4) 0.0299(15) Uani 1 1 d . . . C10 C -0.1578(10) 0.9012(6) 0.3908(5) 0.053(3) Uani 1 1 d . . . O4 O 0.2500 0.7500 0.3915(3) 0.215(11) Uani 1 2 d SU . . H4B H 0.1747 0.7589 0.3543 0.323 Uiso 1 1 d R . . N1 N 0.1247 0.9307 0.3869(3) 0.032(3) Uani 0.50 1 d PR . . C12 C -0.0083 0.9169 0.5227(3) 0.032(3) Uani 0.50 1 d PR . . C13 C 0.1303 0.9365 0.4734(3) 0.032(3) Uani 0.50 1 d PR . . C11 C -0.1727 0.8852 0.4749(3) 0.051(3) Uani 1 1 d R . . N1' N 0.1038 0.8552 0.3706(3) 0.033(3) Uani 0.50 1 d PR . . C12' C -0.0765 0.8283 0.4929(3) 0.038(4) Uani 0.50 1 d PR . . C13' C 0.0657 0.8190 0.4437(3) 0.042(4) Uani 0.50 1 d PR . . H2A H 0.285(8) 0.856(9) 0.289(11) 0.17(8) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0232(10) 0.0134(9) 0.0230(10) 0.000 0.0023(9) 0.000 O1 0.0135(19) 0.0178(19) 0.024(2) -0.0024(16) 0.0036(16) -0.0010(16) O2 0.045(3) 0.029(3) 0.037(3) 0.002(2) 0.023(3) 0.001(2) O3 0.051(3) 0.023(2) 0.051(3) -0.006(2) 0.032(3) -0.002(2) C1 0.017(3) 0.012(3) 0.022(3) -0.004(2) 0.001(2) 0.000(2) C2 0.021(3) 0.019(3) 0.023(3) -0.001(2) 0.004(2) -0.004(2) C3 0.009(2) 0.024(3) 0.029(3) -0.004(2) 0.001(2) -0.002(2) C4 0.020(3) 0.021(3) 0.023(3) -0.003(2) -0.003(2) 0.004(2) C5 0.020(3) 0.012(2) 0.016(2) -0.003(2) 0.003(2) -0.004(2) C6 0.018(3) 0.018(3) 0.020(3) -0.004(2) 0.003(2) -0.004(2) C7 0.020(3) 0.023(3) 0.029(3) -0.001(3) 0.010(3) 0.003(2) C8 0.027(3) 0.030(3) 0.021(3) -0.006(3) 0.007(3) -0.006(3) S2 0.0219(10) 0.0220(10) 0.0171(9) 0.000 0.000 -0.0041(9) C9 0.030(4) 0.031(3) 0.029(3) -0.002(3) 0.007(3) -0.001(3) C10 0.026(4) 0.112(8) 0.022(4) -0.017(4) 0.005(3) -0.009(5) O4 0.223(13) 0.210(13) 0.213(13) 0.000 0.000 -0.007(9) N1 0.032(6) 0.031(6) 0.034(6) -0.014(5) 0.019(5) -0.001(5) C12 0.021(6) 0.056(9) 0.021(6) -0.003(6) 0.006(5) -0.006(6) C13 0.031(7) 0.035(7) 0.031(7) -0.011(6) 0.012(6) 0.000(6) C11 0.059(6) 0.053(5) 0.043(5) 0.023(4) 0.030(4) 0.032(4) N1' 0.034(7) 0.041(7) 0.024(5) 0.001(5) 0.007(5) 0.013(6) C12' 0.034(8) 0.044(8) 0.036(8) 0.013(7) 0.017(7) 0.015(7) C13' 0.031(8) 0.049(9) 0.046(9) 0.009(7) 0.014(7) 0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.779(6) 4_655 ? S1 C1 1.779(6) . ? O1 C6 1.384(7) . ? O1 C7 1.432(7) . ? O2 H2A 0.820(10) . ? O2 C8 1.253(8) . ? O2 H2A 0.820(10) . ? O3 C8 1.260(8) . ? C1 C2 1.392(8) . ? C1 C6 1.406(8) . ? C2 C3 1.375(9) . ? C2 H2 0.9300 . ? C3 C4 1.389(9) . ? C3 H3 0.9300 . ? C4 C5 1.386(8) . ? C4 H4 0.9300 . ? C5 C6 1.394(8) . ? C5 S2 1.781(6) . ? C7 C8 1.508(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? S2 C5 1.781(6) 2_665 ? C9 C10 1.338(10) . ? C9 N1 1.362(8) . ? C9 N1' 1.380(7) . ? C10 C11 1.351(9) . ? O4 H4B 0.8501 . ? N1 C13 1.3523 . ? C12 C13 1.3952 . ? C12 C11 1.6257 . ? C11 C12' 1.3822 . ? C11 C11 1.455(5) 4_456 ? N1' C13' 1.3765 . ? C12' C13' 1.3743 . ? 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 C1 S1 C1 99.6(4) 4_655 . ? C6 O1 C7 115.8(5) . . ? H2A O2 C8 100(10) . . ? H2A O2 H2A 0(10) . . ? C8 O2 H2A 100(10) . . ? C2 C1 C6 119.0(6) . . ? C2 C1 S1 119.7(5) . . ? C6 C1 S1 121.3(5) . . ? C3 C2 C1 121.5(6) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 118.9(6) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 121.2(6) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 119.5(5) . . ? C4 C5 S2 120.0(5) . . ? C6 C5 S2 120.5(4) . . ? O1 C6 C5 118.8(5) . . ? O1 C6 C1 121.3(5) . . ? C5 C6 C1 119.7(5) . . ? O1 C7 C8 111.2(5) . . ? O1 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? O1 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? O2 C8 O3 125.0(6) . . ? O2 C8 C7 120.6(6) . . ? O3 C8 C7 114.4(6) . . ? C5 S2 C5 97.9(4) 2_665 . ? C10 C9 N1 118.0(6) . . ? C10 C9 N1' 114.4(7) . . ? N1 C9 N1' 67.0(4) . . ? C9 C10 C11 125.3(7) . . ? C13 N1 C9 120.9(3) . . ? C13 C12 C11 119.0 . . ? N1 C13 C12 119.9 . . ? C10 C11 C12' 109.7(5) . . ? C10 C11 C11 126.5(5) . 4_456 ? C12' C11 C11 110.86(15) . 4_456 ? C10 C11 C12 106.5(4) . . ? C12' C11 C12 77.0 . . ? C11 C11 C12 115.4(3) 4_456 . ? C13' N1' C9 115.5(3) . . ? C13' C12' C11 116.6 . . ? C12' C13' N1' 124.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.365 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.146 #===END