Supplementary Material (ESI) for Chemical Science This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _publ_contact_author_name 'Ma, Shengming' _publ_contact_author_address ; ; _publ_contact_author_email masm@sioc.ac.cn _publ_author_name 'Shengming Ma' data_z _database_code_depnum_ccdc_archive 'CCDC 771437' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H18 O2 S' _chemical_formula_weight 334.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6322(6) _cell_length_b 5.6630(3) _cell_length_c 13.3325(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.4790(10) _cell_angle_gamma 90.00 _cell_volume 857.51(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(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 0.52 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.818187 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 9963 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3027 _reflns_number_gt 2977 _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. ; _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^)+(0.0235P)^2^+0.5594P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.007(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(8) _refine_ls_number_reflns 3027 _refine_ls_number_parameters 218 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 S1 S 0.80230(5) 0.89233(10) 0.03627(4) 0.02512(15) Uani 1 1 d . . . O1 O 0.84267(16) 1.1277(3) 0.06773(13) 0.0327(4) Uani 1 1 d . . . O2 O 0.75705(16) 0.8484(4) -0.07135(12) 0.0394(5) Uani 1 1 d . . . C1 C 0.69097(19) 0.8136(4) 0.10238(18) 0.0278(5) Uani 1 1 d . . . C2 C 0.6266(2) 0.6101(5) 0.0732(2) 0.0361(6) Uani 1 1 d . . . H2A H 0.6436 0.5111 0.0208 0.043 Uiso 1 1 calc R . . C3 C 0.5362(2) 0.5540(5) 0.1226(2) 0.0466(8) Uani 1 1 d . . . H3A H 0.4913 0.4143 0.1045 0.056 Uiso 1 1 calc R . . C4 C 0.5118(2) 0.7027(6) 0.1984(2) 0.0465(7) Uani 1 1 d . . . H4A H 0.4492 0.6655 0.2311 0.056 Uiso 1 1 calc R . . C5 C 0.5773(2) 0.9018(7) 0.2260(2) 0.0500(7) Uani 1 1 d . . . H5A H 0.5603 1.0014 0.2783 0.060 Uiso 1 1 calc R . . C6 C 0.6681(2) 0.9598(4) 0.1785(2) 0.0348(6) Uani 1 1 d . . . H6A H 0.7138 1.0979 0.1979 0.042 Uiso 1 1 calc R . . C7 C 1.20505(19) 0.8437(4) 0.27789(17) 0.0254(5) Uani 1 1 d . . . C8 C 1.2270(2) 0.6784(5) 0.35765(19) 0.0303(5) Uani 1 1 d . . . H8A H 1.1799 0.5402 0.3532 0.036 Uiso 1 1 calc R . . C9 C 1.3174(2) 0.7148(5) 0.44346(19) 0.0327(6) Uani 1 1 d . . . H9A H 1.3321 0.6009 0.4970 0.039 Uiso 1 1 calc R . . C10 C 1.3857(2) 0.9162(5) 0.45099(18) 0.0353(6) Uani 1 1 d . . . H10A H 1.4467 0.9420 0.5100 0.042 Uiso 1 1 calc R . . C11 C 1.3647(2) 1.0808(5) 0.3719(2) 0.0334(6) Uani 1 1 d . . . H11A H 1.4116 1.2194 0.3769 0.040 Uiso 1 1 calc R . . C12 C 1.2758(2) 1.0440(5) 0.28573(19) 0.0296(5) Uani 1 1 d . . . H12A H 1.2631 1.1564 0.2315 0.036 Uiso 1 1 calc R . . C13 C 0.94672(18) 0.7172(4) 0.27180(17) 0.0236(5) Uani 1 1 d . . . C14 C 0.8798(2) 0.5201(4) 0.28417(18) 0.0272(5) Uani 1 1 d . . . H14A H 0.8708 0.3956 0.2353 0.033 Uiso 1 1 calc R . . C15 C 0.8258(2) 0.5038(5) 0.36745(19) 0.0317(5) Uani 1 1 d . . . H15A H 0.7810 0.3677 0.3757 0.038 Uiso 1 1 calc R . . C16 C 0.8375(2) 0.6858(5) 0.43838(19) 0.0315(5) Uani 1 1 d . . . H16A H 0.7997 0.6758 0.4947 0.038 Uiso 1 1 calc R . . C17 C 0.90424(18) 0.8821(5) 0.42713(16) 0.0299(5) Uani 1 1 d . . . H17A H 0.9133 1.0060 0.4763 0.036 Uiso 1 1 calc R . . C18 C 0.95811(17) 0.8980(5) 0.34394(15) 0.0255(4) Uani 1 1 d . . . H18A H 1.0032 1.0340 0.3362 0.031 Uiso 1 1 calc R . . C19 C 1.1120(2) 0.8070(4) 0.18474(18) 0.0265(5) Uani 1 1 d . . . H19A H 1.1334 0.8337 0.1208 0.032 Uiso 1 1 calc R . . C20 C 1.00124(19) 0.7404(4) 0.18076(16) 0.0216(5) Uani 1 1 d . . . C21 C 0.9223(2) 0.6905(4) 0.07623(17) 0.0254(5) Uani 1 1 d . . . H21A H 0.8896 0.5293 0.0773 0.030 Uiso 1 1 calc R . . H21B H 0.9714 0.6921 0.0241 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0284(3) 0.0241(3) 0.0227(2) -0.0013(2) 0.00507(19) -0.0010(3) O1 0.0384(10) 0.0251(9) 0.0361(9) -0.0002(7) 0.0109(8) -0.0027(7) O2 0.0421(9) 0.0498(12) 0.0245(8) -0.0012(8) 0.0032(7) 0.0044(9) C1 0.0214(11) 0.0303(12) 0.0292(12) 0.0017(10) -0.0002(9) 0.0005(9) C2 0.0319(13) 0.0325(14) 0.0413(14) -0.0015(12) 0.0019(11) -0.0012(11) C3 0.0297(14) 0.0398(16) 0.067(2) 0.0059(15) 0.0035(14) -0.0075(12) C4 0.0284(13) 0.0499(17) 0.0665(19) 0.0070(16) 0.0218(13) 0.0009(13) C5 0.0414(14) 0.0574(18) 0.0578(17) -0.0084(19) 0.0252(13) -0.0001(18) C6 0.0327(13) 0.0322(15) 0.0421(14) -0.0054(11) 0.0138(11) -0.0024(10) C7 0.0226(11) 0.0288(14) 0.0268(11) -0.0001(10) 0.0095(9) 0.0021(9) C8 0.0250(11) 0.0297(13) 0.0381(13) 0.0039(11) 0.0107(10) 0.0037(10) C9 0.0287(12) 0.0385(14) 0.0302(13) 0.0076(12) 0.0047(10) 0.0094(11) C10 0.0219(10) 0.0484(16) 0.0329(12) -0.0028(13) 0.0000(9) 0.0068(13) C11 0.0250(12) 0.0373(14) 0.0371(14) -0.0063(12) 0.0050(10) -0.0041(11) C12 0.0268(12) 0.0330(14) 0.0293(13) 0.0043(10) 0.0068(10) -0.0009(10) C13 0.0206(10) 0.0233(11) 0.0253(11) 0.0006(10) 0.0012(9) 0.0023(9) C14 0.0312(12) 0.0243(12) 0.0254(12) -0.0023(10) 0.0046(10) -0.0035(10) C15 0.0316(13) 0.0305(12) 0.0334(13) 0.0026(11) 0.0076(10) -0.0048(11) C16 0.0296(12) 0.0388(14) 0.0273(12) 0.0006(11) 0.0089(10) -0.0006(11) C17 0.0262(10) 0.0342(12) 0.0285(11) -0.0069(12) 0.0046(9) 0.0054(12) C18 0.0242(10) 0.0235(10) 0.0284(10) -0.0022(11) 0.0047(8) -0.0027(11) C19 0.0301(12) 0.0259(12) 0.0244(11) 0.0004(9) 0.0078(9) 0.0003(9) C20 0.0257(11) 0.0169(11) 0.0221(11) -0.0015(9) 0.0052(9) 0.0017(9) C21 0.0238(11) 0.0259(12) 0.0265(11) -0.0062(10) 0.0056(9) 0.0004(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 S1 O2 1.4391(17) . ? S1 O1 1.4449(18) . ? S1 C1 1.774(2) . ? S1 C21 1.794(2) . ? C1 C6 1.379(3) . ? C1 C2 1.384(3) . ? C2 C3 1.391(4) . ? C2 H2A 0.9500 . ? C3 C4 1.391(4) . ? C3 H3A 0.9500 . ? C4 C5 1.366(5) . ? C4 H4A 0.9500 . ? C5 C6 1.383(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.392(3) . ? C7 C8 1.398(3) . ? C7 C19 1.475(3) . ? C8 C9 1.391(3) . ? C8 H8A 0.9500 . ? C9 C10 1.381(4) . ? C9 H9A 0.9500 . ? C10 C11 1.389(4) . ? C10 H10A 0.9500 . ? C11 C12 1.385(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.391(3) . ? C13 C18 1.391(3) . ? C13 C20 1.492(3) . ? C14 C15 1.391(3) . ? C14 H14A 0.9500 . ? C15 C16 1.386(4) . ? C15 H15A 0.9500 . ? C16 C17 1.382(4) . ? C16 H16A 0.9500 . ? C17 C18 1.390(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.333(3) . ? C19 H19A 0.9500 . ? C20 C21 1.521(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 S1 O1 118.35(11) . . ? O2 S1 C1 107.63(11) . . ? O1 S1 C1 108.31(11) . . ? O2 S1 C21 106.22(11) . . ? O1 S1 C21 108.56(11) . . ? C1 S1 C21 107.27(11) . . ? C6 C1 C2 121.9(2) . . ? C6 C1 S1 119.48(19) . . ? C2 C1 S1 118.62(19) . . ? C1 C2 C3 118.4(3) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 118.8(3) . . ? C1 C6 H6A 120.6 . . ? C5 C6 H6A 120.6 . . ? C12 C7 C8 118.7(2) . . ? C12 C7 C19 119.5(2) . . ? C8 C7 C19 121.8(2) . . ? C9 C8 C7 120.5(2) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 119.7(2) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C7 120.6(2) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? C14 C13 C18 118.7(2) . . ? C14 C13 C20 121.0(2) . . ? C18 C13 C20 120.3(2) . . ? C13 C14 C15 120.6(2) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.0(2) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C13 120.8(2) . . ? C17 C18 H18A 119.6 . . ? C13 C18 H18A 119.6 . . ? C20 C19 C7 126.9(2) . . ? C20 C19 H19A 116.5 . . ? C7 C19 H19A 116.5 . . ? C19 C20 C13 124.7(2) . . ? C19 C20 C21 118.4(2) . . ? C13 C20 C21 116.78(19) . . ? C20 C21 S1 115.52(16) . . ? C20 C21 H21A 108.4 . . ? S1 C21 H21A 108.4 . . ? C20 C21 H21B 108.4 . . ? S1 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? 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 O2 S1 C1 C6 -136.4(2) . . . . ? O1 S1 C1 C6 -7.3(2) . . . . ? C21 S1 C1 C6 109.7(2) . . . . ? O2 S1 C1 C2 41.3(2) . . . . ? O1 S1 C1 C2 170.36(18) . . . . ? C21 S1 C1 C2 -72.6(2) . . . . ? C6 C1 C2 C3 0.1(4) . . . . ? S1 C1 C2 C3 -177.5(2) . . . . ? C1 C2 C3 C4 0.7(4) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C2 C1 C6 C5 -0.7(4) . . . . ? S1 C1 C6 C5 177.0(2) . . . . ? C4 C5 C6 C1 0.3(4) . . . . ? C12 C7 C8 C9 0.5(3) . . . . ? C19 C7 C8 C9 178.3(2) . . . . ? C7 C8 C9 C10 0.5(4) . . . . ? C8 C9 C10 C11 -0.8(4) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C10 C11 C12 C7 1.1(4) . . . . ? C8 C7 C12 C11 -1.3(3) . . . . ? C19 C7 C12 C11 -179.2(2) . . . . ? C18 C13 C14 C15 -0.4(3) . . . . ? C20 C13 C14 C15 -177.7(2) . . . . ? C13 C14 C15 C16 0.7(4) . . . . ? C14 C15 C16 C17 -1.0(4) . . . . ? C15 C16 C17 C18 0.9(4) . . . . ? C16 C17 C18 C13 -0.6(3) . . . . ? C14 C13 C18 C17 0.3(3) . . . . ? C20 C13 C18 C17 177.7(2) . . . . ? C12 C7 C19 C20 -134.6(2) . . . . ? C8 C7 C19 C20 47.6(3) . . . . ? C7 C19 C20 C13 7.5(4) . . . . ? C7 C19 C20 C21 -174.4(2) . . . . ? C14 C13 C20 C19 -134.1(2) . . . . ? C18 C13 C20 C19 48.6(3) . . . . ? C14 C13 C20 C21 47.7(3) . . . . ? C18 C13 C20 C21 -129.6(2) . . . . ? C19 C20 C21 S1 -113.0(2) . . . . ? C13 C20 C21 S1 65.3(2) . . . . ? O2 S1 C21 C20 166.86(18) . . . . ? O1 S1 C21 C20 38.6(2) . . . . ? C1 S1 C21 C20 -78.26(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.273 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.042 # Attachment '5c.cif' data_z_5c _database_code_depnum_ccdc_archive 'CCDC 771438' #TrackingRef '5c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H41 I2 O8 S2' _chemical_formula_weight 1063.73 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' I I -0.4742 1.8119 '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 10.4567(3) _cell_length_b 14.5947(4) _cell_length_c 16.0710(4) _cell_angle_alpha 82.1840(10) _cell_angle_beta 80.0170(10) _cell_angle_gamma 70.3230(10) _cell_volume 2266.47(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1062 _exptl_absorpt_coefficient_mu 1.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4808 _exptl_absorpt_correction_T_max 0.5521 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 26417 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7945 _reflns_number_gt 7211 _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. ; _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^)+(0.0326P)^2^+2.1325P] 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 7945 _refine_ls_number_parameters 554 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.624927(19) 0.589379(14) 0.344953(12) 0.05073(7) Uani 1 1 d . . . S1 S 0.22281(7) 0.59624(5) 0.38447(4) 0.04064(15) Uani 1 1 d . . . O1 O 0.11217(19) 0.57403(16) 0.35928(13) 0.0548(5) Uani 1 1 d . . . O2 O 0.2698(2) 0.67073(14) 0.33502(13) 0.0589(5) Uani 1 1 d . . . O3 O 0.45425(19) 0.31988(13) 0.42268(13) 0.0525(5) Uani 1 1 d . . . O4 O 0.2365(2) 0.39788(15) 0.46935(14) 0.0575(5) Uani 1 1 d . . . C1 C 0.1769(3) 0.62648(18) 0.49074(16) 0.0385(5) Uani 1 1 d . . . C2 C 0.0642(3) 0.6073(2) 0.53782(18) 0.0490(7) Uani 1 1 d . . . H2A H 0.0172 0.5742 0.5160 0.059 Uiso 1 1 calc R . . C3 C 0.0228(3) 0.6386(3) 0.6184(2) 0.0605(8) Uani 1 1 d . . . H3A H -0.0537 0.6271 0.6511 0.073 Uiso 1 1 calc R . . C4 C 0.0929(4) 0.6863(2) 0.6507(2) 0.0612(8) Uani 1 1 d . . . H4A H 0.0630 0.7077 0.7048 0.073 Uiso 1 1 calc R . . C5 C 0.2069(3) 0.7028(2) 0.6040(2) 0.0606(8) Uani 1 1 d . . . H5A H 0.2556 0.7337 0.6271 0.073 Uiso 1 1 calc R . . C6 C 0.2495(3) 0.6737(2) 0.52278(19) 0.0498(7) Uani 1 1 d . . . H6A H 0.3258 0.6857 0.4903 0.060 Uiso 1 1 calc R . . C7 C 0.4288(2) 0.40596(18) 0.24582(15) 0.0356(5) Uani 1 1 d . . . C8 C 0.5359(3) 0.32905(19) 0.21147(17) 0.0448(6) Uani 1 1 d . . . H8A H 0.6256 0.3220 0.2177 0.054 Uiso 1 1 calc R . . C9 C 0.5106(3) 0.2628(2) 0.16803(19) 0.0524(7) Uani 1 1 d . . . H9A H 0.5835 0.2119 0.1450 0.063 Uiso 1 1 calc R . . C10 C 0.3796(3) 0.2711(2) 0.15848(19) 0.0547(7) Uani 1 1 d . . . H10A H 0.3634 0.2258 0.1297 0.066 Uiso 1 1 calc R . . C11 C 0.2719(3) 0.3471(2) 0.19185(19) 0.0532(7) Uani 1 1 d . . . H11A H 0.1827 0.3533 0.1853 0.064 Uiso 1 1 calc R . . C12 C 0.2956(3) 0.4146(2) 0.23526(17) 0.0447(6) Uani 1 1 d . . . H12A H 0.2222 0.4658 0.2574 0.054 Uiso 1 1 calc R . . C13 C 0.6275(3) 0.51337(19) 0.17964(16) 0.0411(6) Uani 1 1 d . . . C14 C 0.7693(3) 0.4775(2) 0.16199(19) 0.0521(7) Uani 1 1 d . . . H14A H 0.8211 0.4546 0.2065 0.063 Uiso 1 1 calc R . . C15 C 0.8350(4) 0.4750(2) 0.0798(2) 0.0641(9) Uani 1 1 d . . . H15A H 0.9300 0.4492 0.0693 0.077 Uiso 1 1 calc R . . C16 C 0.7606(4) 0.5103(3) 0.0141(2) 0.0744(10) Uani 1 1 d . . . H16A H 0.8049 0.5091 -0.0413 0.089 Uiso 1 1 calc R . . C17 C 0.6212(5) 0.5475(3) 0.0294(2) 0.0763(11) Uani 1 1 d . . . H17A H 0.5709 0.5721 -0.0157 0.092 Uiso 1 1 calc R . . C18 C 0.5534(4) 0.5489(2) 0.11238(19) 0.0584(8) Uani 1 1 d . . . H18A H 0.4582 0.5738 0.1223 0.070 Uiso 1 1 calc R . . C19 C 0.3438(3) 0.39805(18) 0.43007(15) 0.0364(5) Uani 1 1 d . . . C20 C 0.3772(2) 0.48760(17) 0.38471(15) 0.0338(5) Uani 1 1 d . . . H20A H 0.4367 0.5015 0.4188 0.041 Uiso 1 1 calc R . . C21 C 0.4572(2) 0.47327(17) 0.29704(15) 0.0341(5) Uani 1 1 d . . . C22 C 0.5553(3) 0.51429(18) 0.26746(16) 0.0371(5) Uani 1 1 d . . . C23 C 0.4324(5) 0.2270(3) 0.4566(3) 0.0904(14) Uani 1 1 d . . . H23A H 0.4214 0.2225 0.5181 0.109 Uiso 1 1 calc R . . H23B H 0.3488 0.2248 0.4398 0.109 Uiso 1 1 calc R . . C24 C 0.5438(6) 0.1467(3) 0.4268(4) 0.1100(17) Uani 1 1 d . . . H24A H 0.5272 0.0870 0.4501 0.165 Uiso 1 1 calc R . . H24B H 0.6264 0.1485 0.4439 0.165 Uiso 1 1 calc R . . H24C H 0.5534 0.1503 0.3660 0.165 Uiso 1 1 calc R . . I2 I -0.196893(19) -0.015591(15) 0.155278(13) 0.05444(7) Uani 1 1 d . . . S2 S -0.00965(6) 0.19506(4) 0.10910(4) 0.03853(14) Uani 1 1 d . . . O5 O -0.1467(2) 0.20699(15) 0.14937(14) 0.0586(5) Uani 1 1 d . . . O6 O 0.0686(2) 0.24178(14) 0.14201(12) 0.0522(5) Uani 1 1 d . . . O7 O 0.27456(19) -0.06332(14) 0.07511(13) 0.0514(5) Uani 1 1 d . A . O8 O 0.2848(2) 0.08804(16) 0.04138(15) 0.0609(6) Uani 1 1 d . . . C25 C -0.0139(3) 0.23462(18) 0.00046(17) 0.0430(6) Uani 1 1 d . . . C26 C 0.0804(4) 0.2776(2) -0.04173(19) 0.0562(7) Uani 1 1 d . . . H26A H 0.1506 0.2812 -0.0151 0.067 Uiso 1 1 calc R . . C27 C 0.0681(5) 0.3154(3) -0.1249(2) 0.0805(12) Uani 1 1 d . . . H27A H 0.1298 0.3456 -0.1546 0.097 Uiso 1 1 calc R . . C28 C -0.0351(6) 0.3084(3) -0.1637(2) 0.0925(16) Uani 1 1 d . . . H28A H -0.0433 0.3345 -0.2194 0.111 Uiso 1 1 calc R . . C29 C -0.1257(5) 0.2636(3) -0.1213(3) 0.0865(13) Uani 1 1 d . . . H29A H -0.1938 0.2580 -0.1487 0.104 Uiso 1 1 calc R . . C30 C -0.1171(3) 0.2267(2) -0.0383(2) 0.0618(8) Uani 1 1 d . . . H30A H -0.1795 0.1970 -0.0089 0.074 Uiso 1 1 calc R . . C31 C 0.1719(3) -0.00493(19) 0.25303(16) 0.0401(6) Uani 1 1 d . . . C32 C 0.2293(3) -0.0984(2) 0.29031(18) 0.0490(6) Uani 1 1 d . . . H32A H 0.1895 -0.1462 0.2889 0.059 Uiso 1 1 calc R . . C33 C 0.3450(3) -0.1209(2) 0.3295(2) 0.0630(8) Uani 1 1 d . . . H33A H 0.3817 -0.1836 0.3547 0.076 Uiso 1 1 calc R . . C34 C 0.4063(4) -0.0520(3) 0.3317(2) 0.0728(10) Uani 1 1 d . . . H34A H 0.4853 -0.0680 0.3571 0.087 Uiso 1 1 calc R . . C35 C 0.3501(4) 0.0410(3) 0.2960(2) 0.0698(10) Uani 1 1 d . . . H35A H 0.3904 0.0884 0.2982 0.084 Uiso 1 1 calc R . . C36 C 0.2339(3) 0.0649(2) 0.25668(19) 0.0536(7) Uani 1 1 d . . . H36A H 0.1970 0.1281 0.2326 0.064 Uiso 1 1 calc R . . C37 C -0.0859(3) -0.0514(2) 0.32158(17) 0.0450(6) Uani 1 1 d . . . C38 C -0.1020(3) -0.1434(2) 0.3414(2) 0.0604(8) Uani 1 1 d . . . H38A H -0.0954 -0.1815 0.2980 0.073 Uiso 1 1 calc R . . C39 C -0.1273(4) -0.1782(3) 0.4242(3) 0.0760(11) Uani 1 1 d . . . H39A H -0.1352 -0.2404 0.4366 0.091 Uiso 1 1 calc R . . C40 C -0.1409(4) -0.1215(4) 0.4886(3) 0.0824(12) Uani 1 1 d . . . H40A H -0.1584 -0.1452 0.5446 0.099 Uiso 1 1 calc R . . C41 C -0.1288(4) -0.0302(3) 0.4705(2) 0.0776(11) Uani 1 1 d . . . H41A H -0.1396 0.0085 0.5144 0.093 Uiso 1 1 calc R . . C42 C -0.1002(3) 0.0053(3) 0.3866(2) 0.0597(8) Uani 1 1 d . . . H42A H -0.0908 0.0670 0.3746 0.072 Uiso 1 1 calc R . . C43 C 0.2242(3) 0.03318(19) 0.07219(16) 0.0393(6) Uani 1 1 d . . . C44 C 0.0748(2) 0.06223(17) 0.11323(15) 0.0349(5) Uani 1 1 d . . . H44A H 0.0267 0.0370 0.0793 0.042 Uiso 1 1 calc R . . C45 C 0.0559(2) 0.01515(17) 0.20255(15) 0.0353(5) Uani 1 1 d . . . C46 C -0.0524(3) -0.01468(18) 0.23269(16) 0.0393(5) Uani 1 1 d . . . C47 C 0.4195(4) -0.1038(3) 0.0441(3) 0.0792(12) Uani 1 1 d D . . C48 C 0.5005(7) -0.1496(9) 0.1149(4) 0.102(3) Uani 0.50 1 d PD A 1 H48A H 0.5167 -0.0999 0.1411 0.153 Uiso 0.50 1 calc PR A 1 H48B H 0.5867 -0.1949 0.0934 0.153 Uiso 0.50 1 calc PR A 1 H48C H 0.4506 -0.1836 0.1561 0.153 Uiso 0.50 1 calc PR A 1 C48' C 0.4746(8) -0.2066(4) 0.0781(6) 0.079(2) Uani 0.50 1 d PD A 2 H48D H 0.4510 -0.2479 0.0460 0.118 Uiso 0.50 1 calc PR A 2 H48E H 0.4360 -0.2135 0.1365 0.118 Uiso 0.50 1 calc PR A 2 H48F H 0.5725 -0.2250 0.0741 0.118 Uiso 0.50 1 calc PR A 2 H47A H 0.453(5) -0.081(4) 0.003(3) 0.13(2) 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 I1 0.05140(12) 0.05916(12) 0.05277(12) -0.01629(9) -0.00362(8) -0.02947(9) S1 0.0389(3) 0.0410(3) 0.0358(3) -0.0062(3) -0.0038(3) -0.0043(3) O1 0.0417(10) 0.0684(13) 0.0495(11) -0.0199(10) -0.0148(9) -0.0018(9) O2 0.0646(13) 0.0435(11) 0.0523(12) 0.0033(9) 0.0047(10) -0.0050(9) O3 0.0439(11) 0.0396(10) 0.0629(12) 0.0062(9) 0.0028(9) -0.0083(8) O4 0.0431(11) 0.0594(12) 0.0676(13) -0.0030(10) 0.0082(10) -0.0222(9) C1 0.0372(13) 0.0381(13) 0.0375(13) -0.0088(10) -0.0036(10) -0.0071(10) C2 0.0404(14) 0.0575(17) 0.0519(16) -0.0139(13) 0.0005(12) -0.0190(13) C3 0.0518(17) 0.075(2) 0.0496(17) -0.0122(15) 0.0099(14) -0.0191(16) C4 0.068(2) 0.0627(19) 0.0432(16) -0.0200(14) -0.0032(15) -0.0052(16) C5 0.064(2) 0.0612(19) 0.064(2) -0.0247(15) -0.0102(16) -0.0213(16) C6 0.0453(15) 0.0516(16) 0.0569(17) -0.0141(13) -0.0018(13) -0.0199(13) C7 0.0379(13) 0.0392(13) 0.0318(12) -0.0050(10) -0.0017(10) -0.0158(10) C8 0.0414(14) 0.0454(14) 0.0477(15) -0.0102(12) -0.0033(12) -0.0133(12) C9 0.0577(18) 0.0461(15) 0.0533(17) -0.0172(13) -0.0006(14) -0.0148(13) C10 0.074(2) 0.0558(17) 0.0476(16) -0.0160(13) -0.0010(14) -0.0367(16) C11 0.0529(17) 0.0700(19) 0.0501(16) -0.0152(14) -0.0041(13) -0.0347(15) C12 0.0403(14) 0.0552(16) 0.0428(15) -0.0149(12) -0.0009(11) -0.0189(12) C13 0.0489(15) 0.0406(13) 0.0377(13) -0.0024(10) -0.0026(11) -0.0213(12) C14 0.0486(16) 0.0550(16) 0.0508(17) -0.0017(13) 0.0032(13) -0.0199(13) C15 0.064(2) 0.066(2) 0.058(2) -0.0095(16) 0.0195(16) -0.0270(16) C16 0.096(3) 0.088(3) 0.0459(19) -0.0081(17) 0.0155(19) -0.049(2) C17 0.100(3) 0.098(3) 0.0436(18) 0.0104(18) -0.0173(19) -0.051(2) C18 0.0602(19) 0.071(2) 0.0490(17) 0.0038(15) -0.0088(14) -0.0306(16) C19 0.0364(13) 0.0424(13) 0.0329(12) -0.0054(10) -0.0043(10) -0.0151(11) C20 0.0312(12) 0.0360(12) 0.0353(12) -0.0069(10) -0.0046(10) -0.0110(10) C21 0.0319(12) 0.0361(12) 0.0339(12) -0.0058(10) -0.0031(10) -0.0099(10) C22 0.0388(13) 0.0367(12) 0.0382(13) -0.0064(10) -0.0058(10) -0.0138(10) C23 0.093(3) 0.0479(19) 0.109(3) 0.019(2) 0.016(2) -0.0186(19) C24 0.141(4) 0.053(2) 0.130(4) -0.009(2) 0.002(3) -0.032(3) I2 0.04627(11) 0.06102(13) 0.06488(13) -0.00320(9) -0.01416(9) -0.02629(9) S2 0.0403(3) 0.0360(3) 0.0381(3) -0.0053(2) -0.0031(3) -0.0111(3) O5 0.0440(11) 0.0483(11) 0.0701(14) -0.0044(10) 0.0111(10) -0.0069(9) O6 0.0691(13) 0.0445(10) 0.0503(11) -0.0093(8) -0.0188(10) -0.0204(9) O7 0.0396(10) 0.0450(10) 0.0626(12) -0.0103(9) 0.0068(9) -0.0090(8) O8 0.0428(11) 0.0570(12) 0.0780(15) 0.0009(11) 0.0086(10) -0.0204(10) C25 0.0504(15) 0.0360(13) 0.0418(14) -0.0046(11) -0.0101(12) -0.0106(11) C26 0.074(2) 0.0486(16) 0.0488(17) -0.0030(13) -0.0032(15) -0.0259(15) C27 0.127(4) 0.0528(19) 0.051(2) 0.0043(15) 0.006(2) -0.028(2) C28 0.151(4) 0.057(2) 0.046(2) -0.0035(16) -0.032(3) 0.007(2) C29 0.105(3) 0.078(3) 0.071(3) -0.014(2) -0.050(2) 0.000(2) C30 0.0619(19) 0.0609(19) 0.067(2) -0.0107(15) -0.0257(16) -0.0150(15) C31 0.0386(13) 0.0454(14) 0.0367(13) -0.0034(11) -0.0031(10) -0.0150(11) C32 0.0479(16) 0.0480(15) 0.0509(16) 0.0000(12) -0.0092(13) -0.0157(13) C33 0.0589(19) 0.0590(19) 0.068(2) 0.0097(16) -0.0233(16) -0.0138(15) C34 0.064(2) 0.087(3) 0.076(2) 0.0119(19) -0.0362(18) -0.0287(19) C35 0.077(2) 0.076(2) 0.077(2) 0.0096(18) -0.0366(19) -0.0452(19) C36 0.0615(18) 0.0530(16) 0.0560(17) 0.0073(13) -0.0241(14) -0.0278(14) C37 0.0355(13) 0.0511(15) 0.0461(15) -0.0031(12) 0.0021(11) -0.0152(12) C38 0.0589(19) 0.0571(18) 0.0615(19) 0.0000(15) 0.0096(15) -0.0243(15) C39 0.070(2) 0.077(2) 0.074(2) 0.020(2) 0.0034(19) -0.0313(19) C40 0.069(2) 0.118(3) 0.056(2) 0.020(2) 0.0011(18) -0.041(2) C41 0.068(2) 0.120(3) 0.0498(19) -0.020(2) 0.0032(17) -0.037(2) C42 0.0561(18) 0.071(2) 0.0546(18) -0.0114(15) 0.0038(14) -0.0270(16) C43 0.0364(13) 0.0456(14) 0.0367(13) -0.0046(11) -0.0030(10) -0.0148(11) C44 0.0325(12) 0.0358(12) 0.0379(13) -0.0072(10) -0.0024(10) -0.0125(10) C45 0.0363(13) 0.0331(12) 0.0363(13) -0.0065(10) -0.0019(10) -0.0110(10) C46 0.0357(13) 0.0385(13) 0.0442(14) -0.0066(11) -0.0036(11) -0.0122(10) C47 0.0405(18) 0.078(2) 0.088(3) 0.003(2) 0.0182(18) 0.0042(16) C48 0.044(4) 0.156(10) 0.079(6) -0.013(6) 0.009(4) -0.006(5) C48' 0.051(4) 0.062(4) 0.103(6) -0.011(4) 0.010(4) 0.000(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 I1 C22 2.122(2) . ? S1 O2 1.430(2) . ? S1 O1 1.435(2) . ? S1 C1 1.766(3) . ? S1 C20 1.843(2) . ? O3 C19 1.324(3) . ? O3 C23 1.468(4) . ? O4 C19 1.188(3) . ? C1 C2 1.376(4) . ? C1 C6 1.379(4) . ? C2 C3 1.381(4) . ? C2 H2A 0.9300 . ? C3 C4 1.365(5) . ? C3 H3A 0.9300 . ? C4 C5 1.370(5) . ? C4 H4A 0.9300 . ? C5 C6 1.381(4) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.388(4) . ? C7 C12 1.393(4) . ? C7 C21 1.494(3) . ? C8 C9 1.383(4) . ? C8 H8A 0.9300 . ? C9 C10 1.367(4) . ? C9 H9A 0.9300 . ? C10 C11 1.377(4) . ? C10 H10A 0.9300 . ? C11 C12 1.389(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C18 1.380(4) . ? C13 C14 1.388(4) . ? C13 C22 1.480(4) . ? C14 C15 1.378(4) . ? C14 H14A 0.9300 . ? C15 C16 1.362(5) . ? C15 H15A 0.9300 . ? C16 C17 1.364(6) . ? C16 H16A 0.9300 . ? C17 C18 1.396(5) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.524(3) . ? C20 C21 1.511(3) . ? C20 H20A 0.9800 . ? C21 C22 1.343(3) . ? C23 C24 1.414(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? I2 C46 2.121(3) . ? S2 O6 1.428(2) . ? S2 O5 1.430(2) . ? S2 C25 1.766(3) . ? S2 C44 1.837(2) . ? O7 C43 1.324(3) . ? O7 C47 1.452(4) . ? O8 C43 1.189(3) . ? C25 C26 1.377(4) . ? C25 C30 1.379(4) . ? C26 C27 1.386(5) . ? C26 H26A 0.9300 . ? C27 C28 1.374(7) . ? C27 H27A 0.9300 . ? C28 C29 1.364(7) . ? C28 H28A 0.9300 . ? C29 C30 1.375(5) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.389(4) . ? C31 C36 1.392(4) . ? C31 C45 1.500(4) . ? C32 C33 1.381(4) . ? C32 H32A 0.9300 . ? C33 C34 1.370(5) . ? C33 H33A 0.9300 . ? C34 C35 1.373(5) . ? C34 H34A 0.9300 . ? C35 C36 1.385(4) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C42 1.377(4) . ? C37 C38 1.396(4) . ? C37 C46 1.482(4) . ? C38 C39 1.371(5) . ? C38 H38A 0.9300 . ? C39 C40 1.371(6) . ? C39 H39A 0.9300 . ? C40 C41 1.368(6) . ? C40 H40A 0.9300 . ? C41 C42 1.397(5) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.526(3) . ? C44 C45 1.515(3) . ? C44 H44A 0.9800 . ? C45 C46 1.339(3) . ? C47 C48' 1.478(4) . ? C47 C48 1.486(5) . ? C47 H47A 0.79(5) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C48' H48D 0.9600 . ? C48' H48E 0.9600 . ? C48' H48F 0.9600 . ? 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 O2 S1 O1 118.42(14) . . ? O2 S1 C1 108.47(13) . . ? O1 S1 C1 108.55(12) . . ? O2 S1 C20 104.39(12) . . ? O1 S1 C20 110.86(12) . . ? C1 S1 C20 105.37(11) . . ? C19 O3 C23 115.3(2) . . ? C2 C1 C6 121.7(3) . . ? C2 C1 S1 118.9(2) . . ? C6 C1 S1 119.3(2) . . ? C1 C2 C3 118.2(3) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C1 C6 C5 118.8(3) . . ? C1 C6 H6A 120.6 . . ? C5 C6 H6A 120.6 . . ? C8 C7 C12 118.3(2) . . ? C8 C7 C21 119.9(2) . . ? C12 C7 C21 121.7(2) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 120.8(3) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 119.4(3) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C7 120.3(3) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? C18 C13 C14 118.1(3) . . ? C18 C13 C22 120.0(3) . . ? C14 C13 C22 122.0(2) . . ? C15 C14 C13 121.4(3) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C13 C18 C17 120.1(3) . . ? C13 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? O4 C19 O3 124.3(2) . . ? O4 C19 C20 125.7(2) . . ? O3 C19 C20 109.9(2) . . ? C21 C20 C19 114.9(2) . . ? C21 C20 S1 111.63(16) . . ? C19 C20 S1 111.55(16) . . ? C21 C20 H20A 106.0 . . ? C19 C20 H20A 106.0 . . ? S1 C20 H20A 106.0 . . ? C22 C21 C7 120.8(2) . . ? C22 C21 C20 122.1(2) . . ? C7 C21 C20 117.0(2) . . ? C21 C22 C13 125.6(2) . . ? C21 C22 I1 122.41(18) . . ? C13 C22 I1 111.98(17) . . ? C24 C23 O3 111.1(3) . . ? C24 C23 H23A 109.4 . . ? O3 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? O3 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O6 S2 O5 118.05(13) . . ? O6 S2 C25 108.24(12) . . ? O5 S2 C25 108.68(13) . . ? O6 S2 C44 110.96(12) . . ? O5 S2 C44 104.54(11) . . ? C25 S2 C44 105.67(12) . . ? C43 O7 C47 116.0(2) . . ? C26 C25 C30 121.9(3) . . ? C26 C25 S2 119.3(2) . . ? C30 C25 S2 118.7(2) . . ? C25 C26 C27 118.3(3) . . ? C25 C26 H26A 120.9 . . ? C27 C26 H26A 120.9 . . ? C28 C27 C26 120.1(4) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 120.7(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 120.4(4) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C29 C30 C25 118.6(4) . . ? C29 C30 H30A 120.7 . . ? C25 C30 H30A 120.7 . . ? C32 C31 C36 118.1(3) . . ? C32 C31 C45 119.8(2) . . ? C36 C31 C45 121.8(2) . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C34 C33 C32 120.7(3) . . ? C34 C33 H33A 119.6 . . ? C32 C33 H33A 119.6 . . ? C33 C34 C35 119.4(3) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C34 C35 C36 120.6(3) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C35 C36 C31 120.5(3) . . ? C35 C36 H36A 119.7 . . ? C31 C36 H36A 119.7 . . ? C42 C37 C38 118.8(3) . . ? C42 C37 C46 119.8(3) . . ? C38 C37 C46 121.4(3) . . ? C39 C38 C37 120.8(3) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C40 C39 C38 120.0(4) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C41 C40 C39 120.1(3) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41A 119.8 . . ? C42 C41 H41A 119.8 . . ? C37 C42 C41 119.9(3) . . ? C37 C42 H42A 120.1 . . ? C41 C42 H42A 120.1 . . ? O8 C43 O7 125.6(2) . . ? O8 C43 C44 125.7(2) . . ? O7 C43 C44 108.7(2) . . ? C45 C44 C43 113.1(2) . . ? C45 C44 S2 111.27(16) . . ? C43 C44 S2 113.09(17) . . ? C45 C44 H44A 106.3 . . ? C43 C44 H44A 106.3 . . ? S2 C44 H44A 106.3 . . ? C46 C45 C31 121.3(2) . . ? C46 C45 C44 122.2(2) . . ? C31 C45 C44 116.3(2) . . ? C45 C46 C37 125.4(2) . . ? C45 C46 I2 122.63(19) . . ? C37 C46 I2 112.00(17) . . ? O7 C47 C48' 110.7(4) . . ? O7 C47 C48 111.2(4) . . ? C48' C47 C48 48.0(5) . . ? O7 C47 H47A 122(4) . . ? C48' C47 H47A 124(4) . . ? C48 C47 H47A 120(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C48' H48D 109.5 . . ? C47 C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C47 C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 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 O2 S1 C1 C2 142.2(2) . . . . ? O1 S1 C1 C2 12.3(3) . . . . ? C20 S1 C1 C2 -106.5(2) . . . . ? O2 S1 C1 C6 -34.0(3) . . . . ? O1 S1 C1 C6 -163.9(2) . . . . ? C20 S1 C1 C6 77.3(2) . . . . ? C6 C1 C2 C3 1.4(4) . . . . ? S1 C1 C2 C3 -174.7(2) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? C3 C4 C5 C6 1.8(5) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? S1 C1 C6 C5 175.7(2) . . . . ? C4 C5 C6 C1 -1.2(5) . . . . ? C12 C7 C8 C9 -0.1(4) . . . . ? C21 C7 C8 C9 176.3(2) . . . . ? C7 C8 C9 C10 -0.5(4) . . . . ? C8 C9 C10 C11 0.7(5) . . . . ? C9 C10 C11 C12 -0.3(5) . . . . ? C10 C11 C12 C7 -0.2(4) . . . . ? C8 C7 C12 C11 0.4(4) . . . . ? C21 C7 C12 C11 -175.9(2) . . . . ? C18 C13 C14 C15 -1.5(4) . . . . ? C22 C13 C14 C15 178.5(3) . . . . ? C13 C14 C15 C16 1.5(5) . . . . ? C14 C15 C16 C17 -0.5(6) . . . . ? C15 C16 C17 C18 -0.6(6) . . . . ? C14 C13 C18 C17 0.4(5) . . . . ? C22 C13 C18 C17 -179.6(3) . . . . ? C16 C17 C18 C13 0.6(6) . . . . ? C23 O3 C19 O4 8.4(4) . . . . ? C23 O3 C19 C20 -174.3(3) . . . . ? O4 C19 C20 C21 -136.5(3) . . . . ? O3 C19 C20 C21 46.3(3) . . . . ? O4 C19 C20 S1 -8.2(3) . . . . ? O3 C19 C20 S1 174.60(17) . . . . ? O2 S1 C20 C21 -46.0(2) . . . . ? O1 S1 C20 C21 82.60(19) . . . . ? C1 S1 C20 C21 -160.15(17) . . . . ? O2 S1 C20 C19 -176.02(18) . . . . ? O1 S1 C20 C19 -47.4(2) . . . . ? C1 S1 C20 C19 69.80(19) . . . . ? C8 C7 C21 C22 50.1(3) . . . . ? C12 C7 C21 C22 -133.6(3) . . . . ? C8 C7 C21 C20 -126.2(2) . . . . ? C12 C7 C21 C20 50.0(3) . . . . ? C19 C20 C21 C22 -142.6(2) . . . . ? S1 C20 C21 C22 89.1(3) . . . . ? C19 C20 C21 C7 33.7(3) . . . . ? S1 C20 C21 C7 -94.6(2) . . . . ? C7 C21 C22 C13 11.1(4) . . . . ? C20 C21 C22 C13 -172.7(2) . . . . ? C7 C21 C22 I1 -168.77(17) . . . . ? C20 C21 C22 I1 7.4(3) . . . . ? C18 C13 C22 C21 55.7(4) . . . . ? C14 C13 C22 C21 -124.3(3) . . . . ? C18 C13 C22 I1 -124.4(2) . . . . ? C14 C13 C22 I1 55.6(3) . . . . ? C19 O3 C23 C24 164.5(4) . . . . ? O6 S2 C25 C26 17.5(3) . . . . ? O5 S2 C25 C26 146.8(2) . . . . ? C44 S2 C25 C26 -101.4(2) . . . . ? O6 S2 C25 C30 -158.7(2) . . . . ? O5 S2 C25 C30 -29.4(3) . . . . ? C44 S2 C25 C30 82.4(2) . . . . ? C30 C25 C26 C27 1.4(5) . . . . ? S2 C25 C26 C27 -174.7(2) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C29 -0.6(6) . . . . ? C27 C28 C29 C30 1.5(6) . . . . ? C28 C29 C30 C25 -1.0(6) . . . . ? C26 C25 C30 C29 -0.5(5) . . . . ? S2 C25 C30 C29 175.6(3) . . . . ? C36 C31 C32 C33 -0.3(4) . . . . ? C45 C31 C32 C33 173.2(3) . . . . ? C31 C32 C33 C34 -0.7(5) . . . . ? C32 C33 C34 C35 1.4(6) . . . . ? C33 C34 C35 C36 -1.1(6) . . . . ? C34 C35 C36 C31 0.2(6) . . . . ? C32 C31 C36 C35 0.5(5) . . . . ? C45 C31 C36 C35 -172.9(3) . . . . ? C42 C37 C38 C39 -2.0(5) . . . . ? C46 C37 C38 C39 177.2(3) . . . . ? C37 C38 C39 C40 1.8(6) . . . . ? C38 C39 C40 C41 -0.3(6) . . . . ? C39 C40 C41 C42 -1.1(6) . . . . ? C38 C37 C42 C41 0.7(5) . . . . ? C46 C37 C42 C41 -178.6(3) . . . . ? C40 C41 C42 C37 0.9(5) . . . . ? C47 O7 C43 O8 5.5(4) . . . . ? C47 O7 C43 C44 -175.7(3) . . . . ? O8 C43 C44 C45 -126.3(3) . . . . ? O7 C43 C44 C45 54.9(3) . . . . ? O8 C43 C44 S2 1.3(4) . . . . ? O7 C43 C44 S2 -177.48(17) . . . . ? O6 S2 C44 C45 76.35(19) . . . . ? O5 S2 C44 C45 -51.9(2) . . . . ? C25 S2 C44 C45 -166.54(18) . . . . ? O6 S2 C44 C43 -52.2(2) . . . . ? O5 S2 C44 C43 179.47(19) . . . . ? C25 S2 C44 C43 64.9(2) . . . . ? C32 C31 C45 C46 48.0(4) . . . . ? C36 C31 C45 C46 -138.7(3) . . . . ? C32 C31 C45 C44 -126.5(3) . . . . ? C36 C31 C45 C44 46.8(3) . . . . ? C43 C44 C45 C46 -143.2(2) . . . . ? S2 C44 C45 C46 88.2(3) . . . . ? C43 C44 C45 C31 31.3(3) . . . . ? S2 C44 C45 C31 -97.3(2) . . . . ? C31 C45 C46 C37 12.7(4) . . . . ? C44 C45 C46 C37 -173.1(2) . . . . ? C31 C45 C46 I2 -166.56(18) . . . . ? C44 C45 C46 I2 7.6(3) . . . . ? C42 C37 C46 C45 55.7(4) . . . . ? C38 C37 C46 C45 -123.5(3) . . . . ? C42 C37 C46 I2 -124.9(2) . . . . ? C38 C37 C46 I2 55.9(3) . . . . ? C43 O7 C47 C48' 159.2(5) . . . . ? C43 O7 C47 C48 107.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.821 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.056