Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 188 # 1. SUBMISSION DETAILS _publ_contact_author 'Pierre Thuery' _publ_contact_address ; CEA/Saclay, SCM (CNRS URA 331) Bat. 125 91191 Gif-sur-Yvette France ; _publ_contact_author_phone '16(1)69 08 63 29' _publ_contact_author_fax '16(1)69 08 66 40' _publ_contact_author_email thuery@drecam.cea.fr _publ_requested_journal 'J. Chem. Soc., Perkin Trans. 2' loop_ _publ_author_name 'Asfari, Zouhair' 'Dozol, Jean-Francois' 'Lamare, Veronique' 'Nierlich, Martine' 'Thuery, Pierre' 'Vicens, Jacques' _publ_section_title ; Experimental and theoretical study of the first thiacalixcrowns and their alkali metal ion complexes ; data_BC5S _database_code_CSD 164775 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 O10 S4' _chemical_formula_weight 812.99 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 15.6139(6) _cell_length_b 16.7784(8) _cell_length_c 29.5847(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.689(2) _cell_angle_gamma 90.00 _cell_volume 7747.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25086 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method ? _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 25086 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.68 _reflns_number_total 13502 _reflns_number_gt 9862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. All non-hydrogen atoms have been refined anisotropically. Hydrogen atoms were introduced at calculated positions as riding atoms with a displacement parameter equal to 1.2 times that of the parent atom. The structure has been refined as corresponding to a racemic twin. 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^)+(0.0539P)^2^+10.6368P] 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 0.12(7) _refine_ls_number_reflns 13502 _refine_ls_number_parameters 974 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1442 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.481 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.053 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1A S 0.96350(11) 0.06463(9) 0.11570(5) 0.0574(4) Uani 1 1 d . . . S2A S 1.00167(9) 0.26495(8) 0.26494(5) 0.0461(3) Uani 1 1 d . . . S3A S 1.04707(10) 0.01092(9) 0.38545(5) 0.0503(3) Uani 1 1 d . . . S4A S 1.03159(9) -0.18836(8) 0.23477(5) 0.0499(3) Uani 1 1 d . . . O1A O 1.0784(2) -0.0454(2) 0.17331(13) 0.0526(10) Uani 1 1 d . . . O2A O 1.2625(2) -0.0627(2) 0.19318(13) 0.0531(10) Uani 1 1 d . . . O3A O 1.3790(2) 0.0431(2) 0.24137(12) 0.0468(9) Uani 1 1 d . . . O4A O 1.3166(2) 0.1473(2) 0.32081(13) 0.0494(9) Uani 1 1 d . . . O5A O 1.0911(2) 0.1138(2) 0.30058(12) 0.0403(8) Uani 1 1 d . . . O6A O 0.9075(2) 0.1493(2) 0.20031(12) 0.0435(8) Uani 1 1 d . . . O7A O 0.7562(2) 0.1858(2) 0.24418(12) 0.0465(9) Uani 1 1 d . . . O8A O 0.6349(2) 0.0201(2) 0.28670(14) 0.0518(9) Uani 1 1 d . . . O9A O 0.7744(2) -0.1098(2) 0.30683(13) 0.0502(9) Uani 1 1 d . . . O10A O 0.9583(2) -0.0793(2) 0.30930(12) 0.0412(8) Uani 1 1 d . . . C1A C 1.1279(4) 0.0016(4) 0.20485(19) 0.0490(13) Uani 1 1 d . . . H1A1 H 1.1312 -0.0244 0.2341 0.059 Uiso 1 1 calc R . . H1A2 H 1.1017 0.0536 0.2085 0.059 Uiso 1 1 calc R . . C2A C 1.2164(3) 0.0105(3) 0.18621(19) 0.0483(13) Uani 1 1 d . . . H2A1 H 1.2121 0.0227 0.1542 0.058 Uiso 1 1 calc R . . H2A2 H 1.2465 0.0538 0.2014 0.058 Uiso 1 1 calc R . . C3A C 1.3511(4) -0.0549(4) 0.1846(2) 0.0546(14) Uani 1 1 d . . . H3A1 H 1.3586 -0.0142 0.1618 0.066 Uiso 1 1 calc R . . H3A2 H 1.3720 -0.1048 0.1726 0.066 Uiso 1 1 calc R . . C4A C 1.4035(4) -0.0335(4) 0.2260(2) 0.0531(15) Uani 1 1 d . . . H4A1 H 1.3946 -0.0726 0.2495 0.064 Uiso 1 1 calc R . . H4A2 H 1.4638 -0.0333 0.2190 0.064 Uiso 1 1 calc R . . C5A C 1.4247(4) 0.0675(4) 0.2815(2) 0.0560(15) Uani 1 1 d . . . H5A1 H 1.4855 0.0703 0.2758 0.067 Uiso 1 1 calc R . . H5A2 H 1.4164 0.0288 0.3053 0.067 Uiso 1 1 calc R . . C6A C 1.3939(3) 0.1463(3) 0.2961(2) 0.0531(14) Uani 1 1 d . . . H6A1 H 1.4387 0.1710 0.3146 0.064 Uiso 1 1 calc R . . H6A2 H 1.3853 0.1793 0.2694 0.064 Uiso 1 1 calc R . . C7A C 1.2416(3) 0.1248(3) 0.29546(18) 0.0448(12) Uani 1 1 d . . . H7A1 H 1.2426 0.0682 0.2889 0.054 Uiso 1 1 calc R . . H7A2 H 1.2382 0.1538 0.2671 0.054 Uiso 1 1 calc R . . C8A C 1.1666(3) 0.1448(3) 0.32374(18) 0.0435(12) Uani 1 1 d . . . H8A1 H 1.1734 0.1208 0.3534 0.052 Uiso 1 1 calc R . . H8A2 H 1.1618 0.2021 0.3274 0.052 Uiso 1 1 calc R . . C9A C 0.8442(4) 0.2055(3) 0.1822(2) 0.0512(13) Uani 1 1 d . . . H9A1 H 0.8456 0.2067 0.1494 0.061 Uiso 1 1 calc R . . H9A2 H 0.8562 0.2587 0.1935 0.061 Uiso 1 1 calc R . . C10A C 0.7582(4) 0.1785(4) 0.19693(19) 0.0517(14) Uani 1 1 d . . . H10A H 0.7136 0.2110 0.1828 0.062 Uiso 1 1 calc R . . H10B H 0.7486 0.1234 0.1881 0.062 Uiso 1 1 calc R . . C11A C 0.6879(3) 0.1428(3) 0.2631(2) 0.0510(14) Uani 1 1 d . . . H11A H 0.6370 0.1486 0.2438 0.061 Uiso 1 1 calc R . . H11B H 0.6756 0.1652 0.2925 0.061 Uiso 1 1 calc R . . C12A C 0.7088(3) 0.0556(3) 0.26847(19) 0.0475(13) Uani 1 1 d . . . H12A H 0.7212 0.0320 0.2394 0.057 Uiso 1 1 calc R . . H12B H 0.7581 0.0484 0.2888 0.057 Uiso 1 1 calc R . . C13A C 0.6326(4) -0.0641(3) 0.2852(2) 0.0563(15) Uani 1 1 d . . . H13A H 0.6496 -0.0814 0.2555 0.068 Uiso 1 1 calc R . . H13B H 0.5740 -0.0814 0.2890 0.068 Uiso 1 1 calc R . . C14A C 0.6883(3) -0.1044(3) 0.3199(2) 0.0533(15) Uani 1 1 d . . . H14A H 0.6860 -0.0751 0.3481 0.064 Uiso 1 1 calc R . . H14B H 0.6664 -0.1576 0.3251 0.064 Uiso 1 1 calc R . . C15A C 0.8308(4) -0.1232(4) 0.3449(2) 0.0599(16) Uani 1 1 d . . . H15A H 0.8073 -0.1646 0.3637 0.072 Uiso 1 1 calc R . . H15B H 0.8351 -0.0748 0.3628 0.072 Uiso 1 1 calc R . . C16A C 0.9167(4) -0.1469(4) 0.3310(2) 0.0619(17) Uani 1 1 d . . . H16A H 0.9507 -0.1638 0.3573 0.074 Uiso 1 1 calc R . . H16B H 0.9123 -0.1913 0.3101 0.074 Uiso 1 1 calc R . . C17A C 0.9923(3) -0.0553(3) 0.18019(18) 0.0427(12) Uani 1 1 d . . . C18A C 0.9623(3) -0.1178(3) 0.20753(17) 0.0405(12) Uani 1 1 d . . . C19A C 0.8752(3) -0.1331(3) 0.20848(19) 0.0472(13) Uani 1 1 d . . . H19A H 0.8552 -0.1735 0.2269 0.057 Uiso 1 1 calc R . . C20A C 0.8178(3) -0.0891(3) 0.1824(2) 0.0493(13) Uani 1 1 d . . . H20A H 0.7595 -0.1006 0.1828 0.059 Uiso 1 1 calc R . . C21A C 0.8467(4) -0.0288(3) 0.15629(19) 0.0509(14) Uani 1 1 d . . . H21A H 0.8074 0.0004 0.1388 0.061 Uiso 1 1 calc R . . C22A C 0.9332(4) -0.0094(3) 0.15484(17) 0.0442(12) Uani 1 1 d . . . C23A C 1.0231(4) 0.1341(3) 0.14954(19) 0.0521(14) Uani 1 1 d . . . C24A C 0.9889(4) 0.1677(3) 0.18861(18) 0.0443(12) Uani 1 1 d . . . C25A C 1.0397(3) 0.2169(3) 0.21613(19) 0.0457(13) Uani 1 1 d . . . C26A C 1.1220(4) 0.2370(3) 0.2028(2) 0.0522(14) Uani 1 1 d . . . H26A H 1.1558 0.2707 0.2208 0.063 Uiso 1 1 calc R . . C27A C 1.1534(4) 0.2076(4) 0.1634(2) 0.0606(16) Uani 1 1 d . . . H27A H 1.2080 0.2221 0.1546 0.073 Uiso 1 1 calc R . . C28A C 1.1045(4) 0.1563(4) 0.1364(2) 0.0561(15) Uani 1 1 d . . . H28A H 1.1260 0.1367 0.1096 0.067 Uiso 1 1 calc R . . C29A C 0.9637(3) 0.1922(3) 0.30306(17) 0.0392(11) Uani 1 1 d . . . C30A C 1.0152(3) 0.1298(3) 0.32065(18) 0.0400(12) Uani 1 1 d . . . C31A C 0.9848(3) 0.0847(3) 0.35630(17) 0.0417(12) Uani 1 1 d . . . C32A C 0.9061(3) 0.1014(3) 0.37436(19) 0.0496(13) Uani 1 1 d . . . H32A H 0.8869 0.0710 0.3983 0.060 Uiso 1 1 calc R . . C33A C 0.8555(4) 0.1628(4) 0.35717(19) 0.0515(14) Uani 1 1 d . . . H33A H 0.8028 0.1737 0.3696 0.062 Uiso 1 1 calc R . . C34A C 0.8835(3) 0.2073(3) 0.3218(2) 0.0484(14) Uani 1 1 d . . . H34A H 0.8492 0.2480 0.3100 0.058 Uiso 1 1 calc R . . C35A C 1.0945(3) -0.0479(3) 0.34372(18) 0.0422(12) Uani 1 1 d . . . C36A C 1.0458(3) -0.0887(3) 0.31066(18) 0.0397(11) Uani 1 1 d . . . C37A C 1.0865(3) -0.1369(3) 0.27941(17) 0.0402(11) Uani 1 1 d . . . C38A C 1.1755(3) -0.1481(3) 0.28324(19) 0.0463(13) Uani 1 1 d . . . H38A H 1.2024 -0.1813 0.2629 0.056 Uiso 1 1 calc R . . C39A C 1.2236(4) -0.1105(3) 0.31687(19) 0.0490(14) Uani 1 1 d . . . H39A H 1.2825 -0.1189 0.3194 0.059 Uiso 1 1 calc R . . C40A C 1.1836(3) -0.0601(3) 0.34695(19) 0.0473(13) Uani 1 1 d . . . H40A H 1.2159 -0.0342 0.3694 0.057 Uiso 1 1 calc R . . S1B S 0.44223(9) -0.08838(9) 0.38566(5) 0.0472(3) Uani 1 1 d . . . S2B S 0.28626(9) -0.06266(14) 0.55106(6) 0.0739(5) Uani 1 1 d . . . S3B S 0.60313(10) 0.00533(13) 0.63386(5) 0.0713(5) Uani 1 1 d . . . S4B S 0.75835(9) -0.02666(9) 0.46810(5) 0.0499(3) Uani 1 1 d . . . O1B O 0.5788(2) 0.0148(2) 0.43466(12) 0.0477(9) Uani 1 1 d . . . O2B O 0.6565(3) 0.1849(3) 0.41321(17) 0.0729(13) Uani 1 1 d . . . O3B O 0.5415(3) 0.2854(3) 0.4636(2) 0.0943(17) Uani 1 1 d . . . O4B O 0.4323(4) 0.2349(4) 0.5466(3) 0.122(2) Uani 1 1 d . . . O5B O 0.4649(3) 0.0220(3) 0.55619(13) 0.0598(11) Uani 1 1 d . . . O6B O 0.4166(2) -0.1289(2) 0.48681(12) 0.0468(9) Uani 1 1 d . . . O7B O 0.4262(3) -0.3411(2) 0.48299(15) 0.0623(11) Uani 1 1 d . . . O8B O 0.6019(2) -0.3637(2) 0.53251(13) 0.0502(9) Uani 1 1 d . . . O9B O 0.6762(3) -0.2473(2) 0.60152(13) 0.0599(11) Uani 1 1 d . . . O10B O 0.6536(2) -0.0837(2) 0.54914(12) 0.0505(9) Uani 1 1 d . . . C1B C 0.5973(4) 0.0583(4) 0.3939(2) 0.0614(16) Uani 1 1 d . . . H1B1 H 0.5627 0.0374 0.3689 0.074 Uiso 1 1 calc R . . H1B2 H 0.6571 0.0511 0.3869 0.074 Uiso 1 1 calc R . . C2B C 0.5787(5) 0.1469(4) 0.3996(3) 0.080(2) Uani 1 1 d . . . H2B1 H 0.5570 0.1693 0.3713 0.096 Uiso 1 1 calc R . . H2B2 H 0.5358 0.1547 0.4223 0.096 Uiso 1 1 calc R . . C3B C 0.6500(5) 0.2672(4) 0.4106(2) 0.0694(18) Uani 1 1 d . . . H3B1 H 0.6103 0.2803 0.3858 0.083 Uiso 1 1 calc R . . H3B2 H 0.7056 0.2883 0.4030 0.083 Uiso 1 1 calc R . . C4B C 0.6213(5) 0.3090(4) 0.4518(3) 0.075(2) Uani 1 1 d . . . H4B1 H 0.6616 0.2983 0.4766 0.090 Uiso 1 1 calc R . . H4B2 H 0.6210 0.3660 0.4463 0.090 Uiso 1 1 calc R . . C5B C 0.5085(7) 0.3287(5) 0.5010(3) 0.098(3) Uani 1 1 d . . . H5B1 H 0.5517 0.3299 0.5253 0.118 Uiso 1 1 calc R . . H5B2 H 0.4974 0.3833 0.4917 0.118 Uiso 1 1 calc R . . C6B C 0.4339(8) 0.2960(7) 0.5172(4) 0.123(4) Uani 1 1 d . . . H6B1 H 0.4030 0.3394 0.5309 0.148 Uiso 1 1 calc R . . H6B2 H 0.4000 0.2795 0.4908 0.148 Uiso 1 1 calc R . . C7B C 0.4575(5) 0.1560(5) 0.5313(3) 0.082(2) Uani 1 1 d . . . H7B1 H 0.5181 0.1547 0.5250 0.098 Uiso 1 1 calc R . . H7B2 H 0.4252 0.1412 0.5040 0.098 Uiso 1 1 calc R . . C8B C 0.4376(4) 0.0999(5) 0.5697(2) 0.0668(18) Uani 1 1 d . . . H8B1 H 0.4682 0.1162 0.5972 0.080 Uiso 1 1 calc R . . H8B2 H 0.3767 0.1000 0.5752 0.080 Uiso 1 1 calc R . . C9B C 0.3830(4) -0.2062(4) 0.4763(2) 0.0551(15) Uani 1 1 d . . . H9B1 H 0.3848 -0.2164 0.4441 0.066 Uiso 1 1 calc R . . H9B2 H 0.3240 -0.2105 0.4856 0.066 Uiso 1 1 calc R . . C10B C 0.4399(4) -0.2654(4) 0.50260(19) 0.0547(14) Uani 1 1 d . . . H10C H 0.4997 -0.2503 0.5007 0.066 Uiso 1 1 calc R . . H10D H 0.4251 -0.2662 0.5342 0.066 Uiso 1 1 calc R . . C11B C 0.4544(4) -0.4069(3) 0.5100(2) 0.0543(15) Uani 1 1 d . . . H11C H 0.4250 -0.4547 0.4995 0.065 Uiso 1 1 calc R . . H11D H 0.4385 -0.3977 0.5410 0.065 Uiso 1 1 calc R . . C12B C 0.5506(4) -0.4211(4) 0.5091(2) 0.0586(16) Uani 1 1 d . . . H12C H 0.5629 -0.4732 0.5220 0.070 Uiso 1 1 calc R . . H12D H 0.5674 -0.4224 0.4778 0.070 Uiso 1 1 calc R . . C13B C 0.5959(5) -0.3689(4) 0.5798(2) 0.076(2) Uani 1 1 d . . . H13C H 0.5929 -0.4245 0.5886 0.091 Uiso 1 1 calc R . . H13D H 0.5436 -0.3430 0.5889 0.091 Uiso 1 1 calc R . . C14B C 0.6716(5) -0.3303(4) 0.6040(2) 0.076(2) Uani 1 1 d . . . H14C H 0.6708 -0.3453 0.6356 0.092 Uiso 1 1 calc R . . H14D H 0.7235 -0.3521 0.5917 0.092 Uiso 1 1 calc R . . C15B C 0.7050(6) -0.2175(4) 0.5623(2) 0.090(3) Uani 1 1 d . . . H15C H 0.6623 -0.2258 0.5383 0.107 Uiso 1 1 calc R . . H15D H 0.7568 -0.2454 0.5542 0.107 Uiso 1 1 calc R . . C16B C 0.7234(6) -0.1307(4) 0.5670(3) 0.094(3) Uani 1 1 d . . . H16C H 0.7332 -0.1179 0.5987 0.113 Uiso 1 1 calc R . . H16D H 0.7750 -0.1178 0.5512 0.113 Uiso 1 1 calc R . . C17B C 0.5979(3) -0.0659(3) 0.43186(18) 0.0429(12) Uani 1 1 d . . . C18B C 0.6769(3) -0.0924(3) 0.44901(17) 0.0428(12) Uani 1 1 d . . . C19B C 0.6964(3) -0.1739(3) 0.44662(18) 0.0480(13) Uani 1 1 d . . . H19B H 0.7487 -0.1923 0.4583 0.058 Uiso 1 1 calc R . . C20B C 0.6382(4) -0.2275(3) 0.42699(18) 0.0480(13) Uani 1 1 d . . . H20B H 0.6518 -0.2814 0.4253 0.058 Uiso 1 1 calc R . . C21B C 0.5599(4) -0.2002(3) 0.40996(18) 0.0491(13) Uani 1 1 d . . . H21B H 0.5210 -0.2359 0.3969 0.059 Uiso 1 1 calc R . . C22B C 0.5391(3) -0.1199(3) 0.41231(17) 0.0429(12) Uani 1 1 d . . . C23B C 0.3863(3) -0.0352(3) 0.42697(18) 0.0462(13) Uani 1 1 d . . . C24B C 0.3722(3) -0.0643(3) 0.47025(19) 0.0470(13) Uani 1 1 d . . . C25B C 0.3164(3) -0.0234(4) 0.49885(19) 0.0562(16) Uani 1 1 d . . . C26B C 0.2761(4) 0.0456(5) 0.4835(2) 0.0690(19) Uani 1 1 d . . . H26B H 0.2375 0.0714 0.5018 0.083 Uiso 1 1 calc R . . C27B C 0.2930(4) 0.0768(5) 0.4409(2) 0.070(2) Uani 1 1 d . . . H27B H 0.2676 0.1243 0.4314 0.084 Uiso 1 1 calc R . . C28B C 0.3477(4) 0.0365(4) 0.4129(2) 0.0584(16) Uani 1 1 d . . . H28B H 0.3590 0.0572 0.3845 0.070 Uiso 1 1 calc R . . C29B C 0.3807(4) -0.0879(4) 0.58234(19) 0.0591(16) Uani 1 1 d . . . C30B C 0.4532(4) -0.0392(4) 0.58608(19) 0.0557(15) Uani 1 1 d . . . C31B C 0.5178(3) -0.0587(4) 0.61853(19) 0.0569(16) Uani 1 1 d . . . C32B C 0.5091(4) -0.1268(5) 0.6452(2) 0.073(2) Uani 1 1 d . . . H32B H 0.5520 -0.1397 0.6664 0.087 Uiso 1 1 calc R . . C33B C 0.4386(5) -0.1751(5) 0.6406(2) 0.081(2) Uani 1 1 d . . . H33B H 0.4339 -0.2206 0.6583 0.097 Uiso 1 1 calc R . . C34B C 0.3750(4) -0.1557(5) 0.6096(2) 0.0680(19) Uani 1 1 d . . . H34B H 0.3270 -0.1883 0.6067 0.082 Uiso 1 1 calc R . . C35B C 0.6456(3) 0.0455(4) 0.58358(18) 0.0474(13) Uani 1 1 d . . . C36B C 0.6718(3) -0.0034(3) 0.54844(18) 0.0448(13) Uani 1 1 d . . . C37B C 0.7139(3) 0.0310(3) 0.51186(18) 0.0429(12) Uani 1 1 d . . . C38B C 0.7304(4) 0.1119(3) 0.5120(2) 0.0523(14) Uani 1 1 d . . . H38B H 0.7591 0.1345 0.4881 0.063 Uiso 1 1 calc R . . C39B C 0.7047(4) 0.1601(4) 0.5473(2) 0.0572(15) Uani 1 1 d . . . H39B H 0.7154 0.2146 0.5470 0.069 Uiso 1 1 calc R . . C40B C 0.6637(4) 0.1262(4) 0.5824(2) 0.0577(16) Uani 1 1 d . . . H40B H 0.6473 0.1583 0.6063 0.069 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 S1A 0.0789(10) 0.0519(9) 0.0417(8) -0.0016(7) 0.0081(7) -0.0014(8) S2A 0.0526(7) 0.0325(7) 0.0528(8) -0.0010(6) -0.0030(6) 0.0029(6) S3A 0.0637(9) 0.0493(8) 0.0381(7) 0.0001(6) 0.0020(7) 0.0091(7) S4A 0.0547(8) 0.0390(8) 0.0552(8) -0.0063(6) -0.0090(7) 0.0095(6) O1A 0.044(2) 0.057(2) 0.057(2) -0.0119(19) 0.0026(18) -0.0034(18) O2A 0.052(2) 0.044(2) 0.063(2) 0.0095(19) -0.0048(19) -0.0039(18) O3A 0.045(2) 0.043(2) 0.053(2) 0.0043(17) 0.0020(18) 0.0061(17) O4A 0.044(2) 0.048(2) 0.056(2) -0.0011(18) -0.0031(18) 0.0007(17) O5A 0.0374(18) 0.039(2) 0.0441(19) -0.0062(15) 0.0029(15) 0.0030(15) O6A 0.048(2) 0.039(2) 0.043(2) 0.0049(16) 0.0063(16) -0.0040(16) O7A 0.052(2) 0.040(2) 0.047(2) 0.0030(16) 0.0034(17) -0.0031(17) O8A 0.047(2) 0.040(2) 0.069(2) 0.0027(19) 0.0137(18) -0.0052(17) O9A 0.046(2) 0.048(2) 0.057(2) 0.0051(18) 0.0141(18) -0.0009(17) O10A 0.0380(18) 0.041(2) 0.0451(19) 0.0025(16) 0.0063(15) 0.0011(15) C1A 0.052(3) 0.052(3) 0.043(3) -0.005(3) 0.000(3) 0.003(3) C2A 0.046(3) 0.048(3) 0.051(3) 0.006(3) 0.001(3) 0.004(3) C3A 0.064(4) 0.049(3) 0.052(3) -0.002(3) 0.019(3) 0.010(3) C4A 0.042(3) 0.054(4) 0.063(4) 0.002(3) 0.004(3) 0.011(3) C5A 0.046(3) 0.055(4) 0.067(4) 0.007(3) -0.004(3) 0.006(3) C6A 0.042(3) 0.046(3) 0.071(4) -0.002(3) -0.002(3) -0.007(3) C7A 0.042(3) 0.045(3) 0.048(3) -0.002(2) -0.004(2) 0.003(2) C8A 0.042(3) 0.041(3) 0.047(3) -0.005(2) -0.006(2) 0.000(2) C9A 0.053(3) 0.049(3) 0.052(3) 0.011(3) 0.004(3) 0.007(3) C10A 0.056(3) 0.050(3) 0.049(3) 0.010(3) 0.003(3) -0.002(3) C11A 0.048(3) 0.044(3) 0.061(4) -0.002(3) 0.006(3) -0.002(3) C12A 0.050(3) 0.041(3) 0.052(3) 0.003(2) 0.006(3) -0.003(3) C13A 0.048(3) 0.035(3) 0.085(4) -0.002(3) -0.004(3) -0.003(3) C14A 0.042(3) 0.038(3) 0.080(4) 0.004(3) 0.009(3) -0.003(2) C15A 0.052(3) 0.065(4) 0.063(4) 0.015(3) 0.002(3) -0.002(3) C16A 0.057(4) 0.054(4) 0.075(4) 0.021(3) 0.005(3) -0.006(3) C17A 0.039(3) 0.040(3) 0.050(3) -0.011(2) 0.007(2) 0.000(2) C18A 0.045(3) 0.039(3) 0.038(3) -0.009(2) -0.001(2) 0.005(2) C19A 0.048(3) 0.038(3) 0.055(3) 0.000(2) 0.003(3) 0.000(2) C20A 0.038(3) 0.052(3) 0.058(3) 0.001(3) -0.006(3) 0.000(2) C21A 0.051(3) 0.049(3) 0.052(3) -0.002(3) -0.012(3) 0.001(3) C22A 0.055(3) 0.042(3) 0.036(3) 0.000(2) 0.000(2) 0.005(2) C23A 0.064(4) 0.050(3) 0.043(3) 0.005(3) 0.011(3) 0.000(3) C24A 0.053(3) 0.036(3) 0.044(3) 0.001(2) 0.007(2) -0.004(2) C25A 0.047(3) 0.037(3) 0.053(3) 0.008(2) 0.006(3) -0.001(2) C26A 0.050(3) 0.039(3) 0.068(4) 0.007(3) 0.009(3) -0.001(3) C27A 0.051(3) 0.059(4) 0.073(4) 0.013(3) 0.020(3) -0.002(3) C28A 0.062(4) 0.055(4) 0.052(3) 0.007(3) 0.023(3) 0.006(3) C29A 0.036(3) 0.041(3) 0.041(3) -0.008(2) -0.004(2) 0.006(2) C30A 0.040(3) 0.036(3) 0.044(3) -0.010(2) 0.001(2) 0.004(2) C31A 0.045(3) 0.043(3) 0.039(3) -0.009(2) 0.009(2) 0.004(2) C32A 0.051(3) 0.053(3) 0.044(3) -0.004(3) 0.004(3) 0.001(3) C33A 0.051(3) 0.062(4) 0.042(3) -0.016(3) 0.007(3) 0.005(3) C34A 0.044(3) 0.042(3) 0.059(3) -0.018(3) -0.005(3) 0.015(2) C35A 0.049(3) 0.034(3) 0.044(3) 0.002(2) 0.004(2) 0.004(2) C36A 0.039(3) 0.035(3) 0.045(3) 0.008(2) 0.003(2) 0.001(2) C37A 0.040(3) 0.035(3) 0.046(3) 0.004(2) 0.002(2) 0.002(2) C38A 0.046(3) 0.038(3) 0.055(3) 0.000(2) 0.005(3) 0.009(2) C39A 0.049(3) 0.043(3) 0.055(3) 0.005(3) -0.006(3) 0.006(3) C40A 0.050(3) 0.041(3) 0.052(3) 0.004(3) -0.001(3) 0.004(2) S1B 0.0480(7) 0.0505(8) 0.0426(7) -0.0026(6) -0.0048(6) 0.0034(6) S2B 0.0374(8) 0.1332(17) 0.0513(9) -0.0045(10) 0.0037(7) -0.0013(9) S3B 0.0489(8) 0.1272(17) 0.0377(8) -0.0019(9) 0.0010(7) -0.0176(9) S4B 0.0409(7) 0.0618(9) 0.0475(8) -0.0083(7) 0.0064(6) -0.0032(7) O1B 0.048(2) 0.047(2) 0.047(2) -0.0103(18) -0.0064(17) 0.0058(18) O2B 0.083(3) 0.046(3) 0.089(3) 0.006(2) 0.001(3) 0.000(2) O3B 0.091(4) 0.058(3) 0.136(5) -0.035(3) 0.050(3) -0.005(3) O4B 0.108(5) 0.111(5) 0.150(6) 0.038(5) 0.057(4) 0.053(4) O5B 0.048(2) 0.086(3) 0.045(2) 0.003(2) 0.0015(18) -0.001(2) O6B 0.0402(19) 0.052(2) 0.048(2) 0.0041(18) -0.0012(17) 0.0005(17) O7B 0.063(3) 0.056(3) 0.067(3) 0.003(2) -0.019(2) -0.009(2) O8B 0.056(2) 0.043(2) 0.052(2) -0.0005(17) 0.0002(18) -0.0093(18) O9B 0.082(3) 0.051(3) 0.047(2) -0.0040(19) 0.007(2) -0.014(2) O10B 0.059(2) 0.047(2) 0.046(2) 0.0005(17) 0.0006(18) -0.0224(18) C1B 0.070(4) 0.045(3) 0.070(4) 0.004(3) 0.005(3) 0.007(3) C2B 0.067(4) 0.071(5) 0.099(6) -0.012(4) -0.027(4) -0.002(4) C3B 0.086(5) 0.043(4) 0.080(5) 0.001(3) 0.017(4) 0.007(3) C4B 0.103(6) 0.042(4) 0.080(5) -0.005(3) 0.014(4) -0.002(4) C5B 0.132(8) 0.065(5) 0.099(6) -0.024(5) 0.027(6) 0.012(5) C6B 0.153(10) 0.114(8) 0.103(8) -0.014(6) 0.029(7) 0.054(8) C7B 0.059(4) 0.097(6) 0.089(5) 0.016(5) 0.006(4) 0.022(4) C8B 0.047(3) 0.091(5) 0.063(4) 0.008(4) 0.014(3) 0.015(3) C9B 0.044(3) 0.062(4) 0.059(4) 0.005(3) -0.005(3) -0.009(3) C10B 0.059(4) 0.056(4) 0.049(3) 0.000(3) -0.004(3) -0.009(3) C11B 0.059(3) 0.045(3) 0.059(4) 0.006(3) -0.011(3) -0.013(3) C12B 0.069(4) 0.047(3) 0.059(4) -0.004(3) -0.010(3) -0.012(3) C13B 0.110(6) 0.062(4) 0.055(4) 0.007(3) -0.014(4) -0.033(4) C14B 0.104(6) 0.058(4) 0.065(4) 0.018(3) -0.031(4) -0.027(4) C15B 0.152(8) 0.056(4) 0.060(4) 0.007(3) -0.006(5) -0.043(5) C16B 0.135(7) 0.052(4) 0.091(6) 0.014(4) -0.061(5) -0.022(4) C17B 0.052(3) 0.035(3) 0.042(3) -0.002(2) 0.005(2) 0.004(2) C18B 0.040(3) 0.051(3) 0.038(3) -0.002(2) 0.004(2) 0.002(2) C19B 0.041(3) 0.057(4) 0.045(3) -0.003(3) 0.002(2) 0.008(3) C20B 0.056(3) 0.044(3) 0.044(3) -0.008(2) 0.002(3) 0.008(3) C21B 0.051(3) 0.053(3) 0.044(3) -0.005(3) 0.004(3) 0.000(3) C22B 0.046(3) 0.044(3) 0.038(3) -0.007(2) 0.000(2) 0.009(2) C23B 0.038(3) 0.056(4) 0.044(3) -0.006(3) -0.004(2) 0.005(2) C24B 0.035(3) 0.059(4) 0.047(3) 0.000(3) -0.005(2) 0.004(2) C25B 0.035(3) 0.088(5) 0.046(3) -0.008(3) -0.005(3) 0.007(3) C26B 0.053(4) 0.096(5) 0.057(4) -0.024(4) -0.009(3) 0.025(4) C27B 0.067(4) 0.083(5) 0.059(4) -0.014(4) -0.021(3) 0.030(4) C28B 0.068(4) 0.061(4) 0.045(3) -0.005(3) -0.014(3) 0.017(3) C29B 0.042(3) 0.094(5) 0.042(3) -0.002(3) 0.011(3) -0.002(3) C30B 0.050(3) 0.077(4) 0.040(3) 0.001(3) 0.010(3) -0.008(3) C31B 0.034(3) 0.094(5) 0.043(3) 0.003(3) 0.001(2) -0.002(3) C32B 0.054(4) 0.113(6) 0.051(4) 0.022(4) 0.005(3) -0.003(4) C33B 0.067(4) 0.112(6) 0.064(4) 0.018(4) 0.011(4) -0.008(4) C34B 0.054(4) 0.092(5) 0.059(4) 0.006(4) 0.015(3) -0.015(3) C35B 0.036(3) 0.061(4) 0.045(3) -0.010(3) -0.001(2) -0.001(2) C36B 0.041(3) 0.053(3) 0.040(3) -0.003(2) -0.006(2) -0.004(2) C37B 0.036(3) 0.048(3) 0.045(3) 0.002(2) -0.001(2) -0.005(2) C38B 0.047(3) 0.049(4) 0.061(4) 0.004(3) -0.007(3) -0.005(3) C39B 0.061(4) 0.048(4) 0.062(4) -0.004(3) -0.015(3) 0.005(3) C40B 0.058(4) 0.062(4) 0.052(4) -0.013(3) -0.007(3) 0.009(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 S1A C22A 1.772(6) . ? S1A C23A 1.781(6) . ? S1A S2A 5.567(2) . ? S1A S4A 5.598(2) . ? S1A S3A 8.099(2) . ? S2A C25A 1.772(6) . ? S2A C29A 1.775(5) . ? S2A S3A 5.588(2) . ? S2A S4A 7.6738(19) . ? S3A C35A 1.761(5) . ? S3A C31A 1.781(5) . ? S3A S4A 5.572(2) . ? S4A C37A 1.777(5) . ? S4A C18A 1.781(5) . ? O1A C17A 1.376(6) . ? O1A C1A 1.432(6) . ? O2A C3A 1.421(7) . ? O2A C2A 1.435(6) . ? O3A C4A 1.420(6) . ? O3A C5A 1.428(7) . ? O4A C7A 1.422(6) . ? O4A C6A 1.430(7) . ? O5A C30A 1.368(6) . ? O5A C8A 1.442(6) . ? O6A C24A 1.363(6) . ? O6A C9A 1.458(6) . ? O7A C10A 1.405(6) . ? O7A C11A 1.416(6) . ? O8A C12A 1.419(6) . ? O8A C13A 1.415(6) . ? O9A C14A 1.412(6) . ? O9A C15A 1.426(7) . ? O10A C36A 1.375(6) . ? O10A C16A 1.466(7) . ? C1A C2A 1.510(7) . ? C3A C4A 1.495(8) . ? C5A C6A 1.476(8) . ? C7A C8A 1.498(7) . ? C9A C10A 1.494(8) . ? C11A C12A 1.507(8) . ? C13A C14A 1.487(8) . ? C15A C16A 1.468(9) . ? C17A C22A 1.402(7) . ? C17A C18A 1.413(7) . ? C18A C19A 1.385(7) . ? C19A C20A 1.379(7) . ? C20A C21A 1.359(8) . ? C21A C22A 1.391(8) . ? C23A C28A 1.390(8) . ? C23A C24A 1.405(8) . ? C24A C25A 1.391(8) . ? C25A C26A 1.397(7) . ? C26A C27A 1.370(9) . ? C27A C28A 1.389(9) . ? C29A C34A 1.407(7) . ? C29A C30A 1.410(7) . ? C30A C31A 1.392(7) . ? C31A C32A 1.383(7) . ? C32A C33A 1.386(8) . ? C33A C34A 1.368(8) . ? C35A C36A 1.399(7) . ? C35A C40A 1.406(7) . ? C36A C37A 1.395(7) . ? C37A C38A 1.404(7) . ? C38A C39A 1.382(8) . ? C39A C40A 1.390(8) . ? S1B C22B 1.767(5) . ? S1B C23B 1.765(6) . ? S1B S4B 5.5386(19) . ? S1B S2B 5.547(2) . ? S1B S3B 7.850(2) . ? S2B C25B 1.756(6) . ? S2B C29B 1.769(6) . ? S2B S3B 5.574(2) . ? S2B S4B 7.861(2) . ? S3B C31B 1.761(6) . ? S3B C35B 1.779(6) . ? S3B S4B 5.560(2) . ? S4B C18B 1.764(5) . ? S4B C37B 1.774(6) . ? O1B C17B 1.389(6) . ? O1B C1B 1.446(7) . ? O2B C3B 1.388(7) . ? O2B C2B 1.420(8) . ? O3B C4B 1.363(8) . ? O3B C5B 1.433(9) . ? O4B C6B 1.347(12) . ? O4B C7B 1.457(10) . ? O5B C30B 1.371(7) . ? O5B C8B 1.436(8) . ? O6B C24B 1.370(6) . ? O6B C9B 1.430(7) . ? O7B C10B 1.410(7) . ? O7B C11B 1.426(7) . ? O8B C13B 1.408(7) . ? O8B C12B 1.421(6) . ? O9B C15B 1.353(8) . ? O9B C14B 1.395(7) . ? O10B C36B 1.377(7) . ? O10B C16B 1.433(8) . ? C1B C2B 1.525(9) . ? C3B C4B 1.485(9) . ? C5B C6B 1.385(13) . ? C7B C8B 1.514(10) . ? C9B C10B 1.530(8) . ? C11B C12B 1.521(9) . ? C13B C14B 1.509(9) . ? C15B C16B 1.491(9) . ? C17B C18B 1.393(7) . ? C17B C22B 1.402(7) . ? C18B C19B 1.403(8) . ? C19B C20B 1.394(8) . ? C20B C21B 1.386(7) . ? C21B C22B 1.387(8) . ? C23B C24B 1.394(8) . ? C23B C28B 1.404(8) . ? C24B C25B 1.411(8) . ? C25B C26B 1.387(9) . ? C26B C27B 1.397(10) . ? C27B C28B 1.384(9) . ? C29B C30B 1.397(8) . ? C29B C34B 1.399(9) . ? C30B C31B 1.410(8) . ? C31B C32B 1.398(9) . ? C32B C33B 1.370(10) . ? C33B C34B 1.370(10) . ? C35B C40B 1.385(8) . ? C35B C36B 1.395(8) . ? C36B C37B 1.406(8) . ? C37B C38B 1.382(8) . ? C38B C39B 1.390(9) . ? C39B C40B 1.360(9) . ? 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 C22A S1A C23A 103.7(3) . . ? C22A S1A S2A 85.94(18) . . ? C23A S1A S2A 28.00(19) . . ? C22A S1A S4A 26.72(18) . . ? C23A S1A S4A 93.24(19) . . ? S2A S1A S4A 86.84(3) . . ? C22A S1A S3A 46.88(17) . . ? C23A S1A S3A 56.82(18) . . ? S2A S1A S3A 43.55(2) . . ? S4A S1A S3A 43.40(2) . . ? C25A S2A C29A 109.3(2) . . ? C25A S2A S1A 27.05(18) . . ? C29A S2A S1A 93.37(16) . . ? C25A S2A S3A 97.69(17) . . ? C29A S2A S3A 26.99(16) . . ? S1A S2A S3A 93.10(3) . . ? C25A S2A S4A 55.34(17) . . ? C29A S2A S4A 54.21(16) . . ? S1A S2A S4A 46.75(2) . . ? S3A S2A S4A 46.47(2) . . ? C35A S3A C31A 106.6(2) . . ? C35A S3A S4A 27.36(17) . . ? C31A S3A S4A 91.12(17) . . ? C35A S3A S2A 91.63(17) . . ? C31A S3A S2A 26.33(17) . . ? S4A S3A S2A 86.88(3) . . ? C35A S3A S1A 55.28(17) . . ? C31A S3A S1A 51.37(16) . . ? S4A S3A S1A 43.65(2) . . ? S2A S3A S1A 43.35(2) . . ? C37A S4A C18A 106.7(2) . . ? C37A S4A S3A 26.52(17) . . ? C18A S4A S3A 88.53(16) . . ? C37A S4A S1A 100.24(17) . . ? C18A S4A S1A 27.05(18) . . ? S3A S4A S1A 92.95(3) . . ? C37A S4A S2A 57.43(16) . . ? C18A S4A S2A 49.85(16) . . ? S3A S4A S2A 46.65(2) . . ? S1A S4A S2A 46.41(2) . . ? C17A O1A C1A 118.8(4) . . ? C3A O2A C2A 112.5(4) . . ? C4A O3A C5A 113.2(4) . . ? C7A O4A C6A 114.9(4) . . ? C30A O5A C8A 115.4(4) . . ? C24A O6A C9A 112.8(4) . . ? C10A O7A C11A 112.9(4) . . ? C12A O8A C13A 115.3(4) . . ? C14A O9A C15A 111.4(4) . . ? C36A O10A C16A 110.6(4) . . ? O1A C1A C2A 107.4(4) . . ? O2A C2A C1A 108.9(5) . . ? O2A C3A C4A 112.8(5) . . ? O3A C4A C3A 109.6(4) . . ? O3A C5A C6A 109.9(5) . . ? O4A C6A C5A 116.6(5) . . ? O4A C7A C8A 106.9(4) . . ? O5A C8A C7A 107.2(4) . . ? O6A C9A C10A 107.5(4) . . ? O7A C10A C9A 108.1(5) . . ? O7A C11A C12A 111.9(4) . . ? O8A C12A C11A 105.7(4) . . ? O8A C13A C14A 114.8(5) . . ? O9A C14A C13A 112.5(5) . . ? O9A C15A C16A 111.8(5) . . ? O10A C16A C15A 109.5(5) . . ? O1A C17A C22A 119.1(5) . . ? O1A C17A C18A 121.0(5) . . ? C22A C17A C18A 119.4(5) . . ? C19A C18A C17A 119.4(5) . . ? C19A C18A S4A 116.9(4) . . ? C17A C18A S4A 123.1(4) . . ? C20A C19A C18A 120.8(5) . . ? C21A C20A C19A 119.6(5) . . ? C20A C21A C22A 122.1(5) . . ? C21A C22A C17A 118.6(5) . . ? C21A C22A S1A 117.5(4) . . ? C17A C22A S1A 123.4(4) . . ? C28A C23A C24A 119.7(6) . . ? C28A C23A S1A 118.9(5) . . ? C24A C23A S1A 121.4(5) . . ? O6A C24A C25A 120.4(5) . . ? O6A C24A C23A 119.8(5) . . ? C25A C24A C23A 119.7(5) . . ? C24A C25A C26A 119.4(5) . . ? C24A C25A S2A 123.3(4) . . ? C26A C25A S2A 117.0(4) . . ? C27A C26A C25A 120.6(6) . . ? C26A C27A C28A 120.5(6) . . ? C23A C28A C27A 119.8(6) . . ? C34A C29A C30A 119.5(5) . . ? C34A C29A S2A 116.4(4) . . ? C30A C29A S2A 123.2(4) . . ? O5A C30A C31A 122.7(5) . . ? O5A C30A C29A 118.5(5) . . ? C31A C30A C29A 118.7(5) . . ? C32A C31A C30A 120.6(5) . . ? C32A C31A S3A 115.6(4) . . ? C30A C31A S3A 123.4(4) . . ? C31A C32A C33A 120.8(5) . . ? C34A C33A C32A 119.7(5) . . ? C33A C34A C29A 120.8(5) . . ? C36A C35A C40A 119.5(5) . . ? C36A C35A S3A 122.2(4) . . ? C40A C35A S3A 118.0(4) . . ? O10A C36A C37A 121.3(5) . . ? O10A C36A C35A 118.9(5) . . ? C37A C36A C35A 119.9(5) . . ? C36A C37A C38A 119.6(5) . . ? C36A C37A S4A 123.7(4) . . ? C38A C37A S4A 116.7(4) . . ? C39A C38A C37A 120.9(5) . . ? C38A C39A C40A 119.6(5) . . ? C39A C40A C35A 120.5(5) . . ? C22B S1B C23B 106.1(2) . . ? C22B S1B S4B 28.24(18) . . ? C23B S1B S4B 93.05(17) . . ? C22B S1B S2B 91.26(18) . . ? C23B S1B S2B 27.22(19) . . ? S4B S1B S2B 90.33(3) . . ? C22B S1B S3B 52.85(17) . . ? C23B S1B S3B 53.29(17) . . ? S4B S1B S3B 45.10(2) . . ? S2B S1B S3B 45.24(2) . . ? C25B S2B C29B 108.0(3) . . ? C25B S2B S1B 28.0(2) . . ? C29B S2B S1B 93.54(19) . . ? C25B S2B S3B 93.02(18) . . ? C29B S2B S3B 26.3(2) . . ? S1B S2B S3B 89.80(3) . . ? C25B S2B S4B 54.46(17) . . ? C29B S2B S4B 53.60(19) . . ? S1B S2B S4B 44.80(2) . . ? S3B S2B S4B 45.02(2) . . ? C31B S3B C35B 108.3(3) . . ? C31B S3B S4B 93.46(19) . . ? C35B S3B S4B 27.86(19) . . ? C31B S3B S2B 26.7(2) . . ? C35B S3B S2B 93.32(17) . . ? S4B S3B S2B 89.83(3) . . ? C31B S3B S1B 54.40(19) . . ? C35B S3B S1B 53.87(17) . . ? S4B S3B S1B 44.88(2) . . ? S2B S3B S1B 44.96(2) . . ? C18B S4B C37B 106.3(2) . . ? C18B S4B S1B 28.03(18) . . ? C37B S4B S1B 93.47(17) . . ? C18B S4B S3B 90.80(17) . . ? C37B S4B S3B 27.55(18) . . ? S1B S4B S3B 90.03(3) . . ? C18B S4B S2B 51.54(17) . . ? C37B S4B S2B 54.77(17) . . ? S1B S4B S2B 44.88(2) . . ? S3B S4B S2B 45.16(2) . . ? C17B O1B C1B 113.2(4) . . ? C3B O2B C2B 111.7(5) . . ? C4B O3B C5B 113.8(6) . . ? C6B O4B C7B 118.7(7) . . ? C30B O5B C8B 117.2(5) . . ? C24B O6B C9B 117.5(4) . . ? C10B O7B C11B 115.2(4) . . ? C13B O8B C12B 113.0(5) . . ? C15B O9B C14B 115.6(6) . . ? C36B O10B C16B 112.9(4) . . ? O1B C1B C2B 110.9(6) . . ? O2B C2B C1B 107.7(5) . . ? O2B C3B C4B 116.6(6) . . ? O3B C4B C3B 111.9(6) . . ? C6B C5B O3B 113.0(8) . . ? O4B C6B C5B 123.8(10) . . ? O4B C7B C8B 105.5(6) . . ? O5B C8B C7B 106.7(5) . . ? O6B C9B C10B 105.9(4) . . ? O7B C10B C9B 107.3(4) . . ? O7B C11B C12B 113.6(5) . . ? O8B C12B C11B 115.3(5) . . ? O8B C13B C14B 111.7(6) . . ? O9B C14B C13B 116.3(6) . . ? O9B C15B C16B 110.4(7) . . ? O10B C16B C15B 111.2(6) . . ? O1B C17B C18B 118.6(5) . . ? O1B C17B C22B 121.1(5) . . ? C18B C17B C22B 120.4(5) . . ? C17B C18B C19B 118.9(5) . . ? C17B C18B S4B 122.7(4) . . ? C19B C18B S4B 118.0(4) . . ? C20B C19B C18B 120.7(5) . . ? C21B C20B C19B 119.7(5) . . ? C20B C21B C22B 120.5(5) . . ? C21B C22B C17B 119.8(5) . . ? C21B C22B S1B 117.8(4) . . ? C17B C22B S1B 122.1(4) . . ? C24B C23B C28B 119.7(5) . . ? C24B C23B S1B 123.6(4) . . ? C28B C23B S1B 116.4(4) . . ? O6B C24B C23B 120.9(5) . . ? O6B C24B C25B 119.1(5) . . ? C23B C24B C25B 119.8(5) . . ? C26B C25B C24B 119.4(6) . . ? C26B C25B S2B 118.1(5) . . ? C24B C25B S2B 122.1(5) . . ? C25B C26B C27B 120.9(6) . . ? C28B C27B C26B 119.6(6) . . ? C27B C28B C23B 120.5(6) . . ? C30B C29B C34B 119.6(6) . . ? C30B C29B S2B 124.2(5) . . ? C34B C29B S2B 115.5(5) . . ? O5B C30B C29B 120.6(5) . . ? O5B C30B C31B 120.4(5) . . ? C29B C30B C31B 118.7(6) . . ? C32B C31B C30B 119.6(6) . . ? C32B C31B S3B 116.0(5) . . ? C30B C31B S3B 123.7(5) . . ? C33B C32B C31B 121.2(6) . . ? C34B C33B C32B 119.3(7) . . ? C33B C34B C29B 121.5(6) . . ? C40B C35B C36B 119.5(5) . . ? C40B C35B S3B 118.2(4) . . ? C36B C35B S3B 121.7(5) . . ? O10B C36B C35B 119.9(5) . . ? O10B C36B C37B 120.9(5) . . ? C35B C36B C37B 119.1(5) . . ? C38B C37B C36B 119.5(5) . . ? C38B C37B S4B 117.5(4) . . ? C36B C37B S4B 122.7(4) . . ? C37B C38B C39B 121.0(6) . . ? C40B C39B C38B 119.0(6) . . ? C39B C40B C35B 121.9(6) . . ? #===END data_BC6S _database_code_CSD 164776 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H52 O12 S4' _chemical_formula_weight 901.10 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 tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.798(2) _cell_length_b 14.798(2) _cell_length_c 40.113(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8784(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 42860 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method ? _exptl_crystal_F_000 3808 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; \f scans with 2\% steps ; _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 42860 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7935 _reflns_number_gt 3482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. All non-hydrogen atoms refined anisotropically. Hydrogen atoms introduced at calculated positions as riding atoms with displacement parameters equal to 1.2 times that of the parent atom. 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^)+(0.0788P)^2^] 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 0.5(2) _refine_ls_number_reflns 7935 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2036 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2326 _refine_ls_wR_factor_gt 0.1786 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.386 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.069 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 -0.02882(16) 0.68637(18) -0.00173(6) 0.0473(6) Uani 1 1 d . . . S2 S 0.2787(2) 0.47320(18) -0.00222(6) 0.0534(7) Uani 1 1 d . . . S3 S 0.49074(17) 0.7803(2) -0.00045(6) 0.0515(7) Uani 1 1 d . . . S4 S 0.18322(19) 0.99306(16) 0.00578(6) 0.0483(7) Uani 1 1 d . . . O1 O 0.0664(4) 0.8407(4) 0.03179(13) 0.0446(17) Uani 1 1 d . . . O2 O 0.0403(5) 0.8998(5) 0.10187(15) 0.062(2) Uani 1 1 d . . . O3 O 0.1863(5) 0.7740(5) 0.15427(16) 0.0557(19) Uani 1 1 d . . . O4 O 0.3577(6) 0.6767(5) 0.17402(16) 0.070(2) Uani 1 1 d . . . O5 O 0.4065(5) 0.5777(5) 0.09529(14) 0.056(2) Uani 1 1 d . . . O6 O 0.3948(4) 0.6224(5) 0.02807(13) 0.0487(18) Uani 1 1 d . . . O7 O 0.1198(4) 0.5682(4) -0.03205(12) 0.0427(16) Uani 1 1 d . . . O8 O 0.0587(5) 0.5491(5) -0.10089(16) 0.063(2) Uani 1 1 d . . . O9 O 0.1880(5) 0.6959(5) -0.15402(15) 0.0570(19) Uani 1 1 d . . . O10 O 0.2873(5) 0.8635(5) -0.17385(16) 0.063(2) Uani 1 1 d . . . O11 O 0.3815(5) 0.9127(5) -0.09392(14) 0.0566(19) Uani 1 1 d . . . O12 O 0.3386(4) 0.9013(5) -0.02710(13) 0.0463(18) Uani 1 1 d . . . C1 C -0.0069(7) 0.9004(8) 0.0434(2) 0.054(3) Uani 1 1 d . . . H1A H -0.0593 0.8928 0.0292 0.065 Uiso 1 1 calc R . . H1B H 0.0126 0.9628 0.0418 0.065 Uiso 1 1 calc R . . C2 C -0.0324(7) 0.8798(8) 0.0786(2) 0.059(3) Uani 1 1 d . . . H2A H -0.0853 0.9151 0.0846 0.071 Uiso 1 1 calc R . . H2B H -0.0483 0.8164 0.0804 0.071 Uiso 1 1 calc R . . C3 C 0.0908(7) 0.8251(6) 0.1114(2) 0.049(3) Uani 1 1 d . . . H3A H 0.1299 0.8057 0.0934 0.058 Uiso 1 1 calc R . . H3B H 0.0515 0.7754 0.1176 0.058 Uiso 1 1 calc R . . C4 C 0.1467(7) 0.8562(7) 0.14153(19) 0.040(2) Uani 1 1 d . . . H4A H 0.1932 0.8987 0.1348 0.049 Uiso 1 1 calc R . . H4B H 0.1086 0.8846 0.1582 0.049 Uiso 1 1 calc R . . C5 C 0.2380(7) 0.7919(8) 0.1834(2) 0.055(3) Uani 1 1 d . . . H5A H 0.1990 0.8129 0.2012 0.066 Uiso 1 1 calc R . . H5B H 0.2828 0.8382 0.1789 0.066 Uiso 1 1 calc R . . C6 C 0.2845(8) 0.7039(8) 0.1936(3) 0.060(3) Uani 1 1 d . . . H6A H 0.3053 0.7102 0.2164 0.072 Uiso 1 1 calc R . . H6B H 0.2397 0.6560 0.1934 0.072 Uiso 1 1 calc R . . C7 C 0.3356(7) 0.6386(7) 0.14311(19) 0.051(3) Uani 1 1 d . . . H7A H 0.3061 0.6830 0.1290 0.062 Uiso 1 1 calc R . . H7B H 0.2951 0.5876 0.1460 0.062 Uiso 1 1 calc R . . C8 C 0.4246(8) 0.6078(7) 0.1275(2) 0.066(4) Uani 1 1 d . . . H8A H 0.4671 0.6576 0.1268 0.079 Uiso 1 1 calc R . . H8B H 0.4509 0.5594 0.1406 0.079 Uiso 1 1 calc R . . C9 C 0.4851(8) 0.5801(7) 0.0754(2) 0.057(3) Uani 1 1 d . . . H9A H 0.5292 0.5376 0.0840 0.068 Uiso 1 1 calc R . . H9B H 0.5115 0.6401 0.0762 0.068 Uiso 1 1 calc R . . C10 C 0.4617(7) 0.5564(8) 0.0403(2) 0.061(3) Uani 1 1 d . . . H10A H 0.5154 0.5583 0.0264 0.073 Uiso 1 1 calc R . . H10B H 0.4367 0.4959 0.0393 0.073 Uiso 1 1 calc R . . C11 C 0.0576(7) 0.5008(8) -0.0430(2) 0.054(3) Uani 1 1 d . . . H11A H -0.0038 0.5228 -0.0406 0.065 Uiso 1 1 calc R . . H11B H 0.0641 0.4469 -0.0294 0.065 Uiso 1 1 calc R . . C12 C 0.0757(7) 0.4791(7) -0.07801(19) 0.047(3) Uani 1 1 d . . . H12A H 0.1386 0.4614 -0.0801 0.057 Uiso 1 1 calc R . . H12B H 0.0391 0.4273 -0.0842 0.057 Uiso 1 1 calc R . . C13 C 0.1327(7) 0.6005(7) -0.1117(3) 0.059(3) Uani 1 1 d . . . H13A H 0.1829 0.5606 -0.1167 0.071 Uiso 1 1 calc R . . H13B H 0.1515 0.6410 -0.0940 0.071 Uiso 1 1 calc R . . C14 C 0.1084(7) 0.6555(8) -0.1427(2) 0.055(3) Uani 1 1 d . . . H14A H 0.0834 0.6164 -0.1597 0.067 Uiso 1 1 calc R . . H14B H 0.0640 0.7013 -0.1372 0.067 Uiso 1 1 calc R . . C15 C 0.1768(7) 0.7432(8) -0.1849(2) 0.056(3) Uani 1 1 d . . . H15A H 0.1308 0.7894 -0.1827 0.068 Uiso 1 1 calc R . . H15B H 0.1586 0.7016 -0.2024 0.068 Uiso 1 1 calc R . . C16 C 0.2647(7) 0.7846(8) -0.1932(2) 0.060(3) Uani 1 1 d . . . H16A H 0.3117 0.7397 -0.1900 0.072 Uiso 1 1 calc R . . H16B H 0.2645 0.8010 -0.2166 0.072 Uiso 1 1 calc R . . C17 C 0.3298(7) 0.8408(8) -0.1441(2) 0.059(3) Uani 1 1 d . . . H17A H 0.3862 0.8095 -0.1483 0.071 Uiso 1 1 calc R . . H17B H 0.2913 0.8021 -0.1307 0.071 Uiso 1 1 calc R . . C18 C 0.3473(7) 0.9313(7) -0.1261(2) 0.054(3) Uani 1 1 d . . . H18A H 0.3906 0.9670 -0.1386 0.065 Uiso 1 1 calc R . . H18B H 0.2915 0.9654 -0.1244 0.065 Uiso 1 1 calc R . . C19 C 0.3784(8) 0.9930(8) -0.0732(2) 0.064(3) Uani 1 1 d . . . H19A H 0.3183 1.0190 -0.0737 0.076 Uiso 1 1 calc R . . H19B H 0.4208 1.0377 -0.0815 0.076 Uiso 1 1 calc R . . C20 C 0.4029(8) 0.9666(9) -0.0379(2) 0.064(4) Uani 1 1 d . . . H20A H 0.4634 0.9413 -0.0372 0.077 Uiso 1 1 calc R . . H20B H 0.4013 1.0192 -0.0235 0.077 Uiso 1 1 calc R . . C21 C 0.0763(6) 0.8410(7) -0.00269(19) 0.040(2) Uani 1 1 d . . . C22 C 0.1288(6) 0.9059(6) -0.0180(2) 0.040(2) Uani 1 1 d . . . C23 C 0.1372(7) 0.9058(8) -0.0526(2) 0.056(3) Uani 1 1 d . . . H23A H 0.1703 0.9509 -0.0631 0.067 Uiso 1 1 calc R . . C24 C 0.0961(7) 0.8383(7) -0.0713(2) 0.045(2) Uani 1 1 d . . . H24A H 0.1007 0.8388 -0.0944 0.054 Uiso 1 1 calc R . . C25 C 0.0490(7) 0.7712(7) -0.0557(2) 0.049(3) Uani 1 1 d . . . H25A H 0.0239 0.7244 -0.0681 0.059 Uiso 1 1 calc R . . C26 C 0.0382(7) 0.7726(7) -0.0210(2) 0.049(3) Uani 1 1 d . . . C27 C 0.0568(6) 0.6251(6) 0.0197(2) 0.038(2) Uani 1 1 d . . . C28 C 0.1248(6) 0.5771(6) 0.0024(2) 0.042(2) Uani 1 1 d . . . C29 C 0.1972(7) 0.5363(5) 0.01970(19) 0.042(2) Uani 1 1 d . . . C30 C 0.2019(8) 0.5464(6) 0.0538(2) 0.051(3) Uani 1 1 d . . . H30A H 0.2501 0.5207 0.0653 0.062 Uiso 1 1 calc R . . C31 C 0.1360(8) 0.5942(7) 0.07175(19) 0.051(3) Uani 1 1 d . . . H31A H 0.1393 0.5990 0.0948 0.062 Uiso 1 1 calc R . . C32 C 0.0658(7) 0.6342(6) 0.0541(2) 0.048(3) Uani 1 1 d . . . H32A H 0.0232 0.6683 0.0657 0.058 Uiso 1 1 calc R . . C33 C 0.3350(6) 0.5639(7) -0.0239(2) 0.045(3) Uani 1 1 d . . . C34 C 0.3872(6) 0.6269(7) -0.0055(2) 0.040(2) Uani 1 1 d . . . C35 C 0.4259(7) 0.6995(8) -0.0233(2) 0.052(3) Uani 1 1 d . . . C36 C 0.4144(7) 0.7042(9) -0.0578(2) 0.057(3) Uani 1 1 d . . . H36A H 0.4405 0.7521 -0.0693 0.068 Uiso 1 1 calc R . . C37 C 0.3668(6) 0.6423(8) -0.0750(2) 0.053(3) Uani 1 1 d . . . H37A H 0.3608 0.6476 -0.0980 0.063 Uiso 1 1 calc R . . C38 C 0.3264(8) 0.5699(7) -0.0582(2) 0.056(3) Uani 1 1 d . . . H38A H 0.2941 0.5264 -0.0699 0.067 Uiso 1 1 calc R . . C39 C 0.4027(6) 0.8331(7) 0.0230(2) 0.048(3) Uani 1 1 d . . . C40 C 0.3391(7) 0.8881(6) 0.00722(18) 0.040(2) Uani 1 1 d . . . C41 C 0.2689(7) 0.9282(5) 0.02542(19) 0.038(2) Uani 1 1 d . . . C42 C 0.2634(7) 0.9127(6) 0.0597(2) 0.044(2) Uani 1 1 d . . . H42A H 0.2152 0.9354 0.0720 0.053 Uiso 1 1 calc R . . C43 C 0.3327(7) 0.8617(7) 0.0756(2) 0.051(3) Uani 1 1 d . . . H43A H 0.3316 0.8535 0.0986 0.061 Uiso 1 1 calc R . . C44 C 0.4013(7) 0.8245(7) 0.0570(2) 0.047(3) Uani 1 1 d . . . H44A H 0.4475 0.7930 0.0676 0.057 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 0.0339(16) 0.0533(18) 0.0546(13) 0.0013(12) -0.0004(11) 0.0006(11) S2 0.072(2) 0.0379(17) 0.0501(12) -0.0019(11) -0.0037(13) 0.0157(13) S3 0.0330(16) 0.075(2) 0.0469(12) -0.0035(13) -0.0025(11) 0.0032(12) S4 0.0578(19) 0.0316(15) 0.0554(13) 0.0027(10) -0.0081(12) 0.0060(11) O1 0.036(4) 0.053(5) 0.044(3) -0.001(3) -0.006(3) 0.022(3) O2 0.084(6) 0.041(5) 0.061(4) 0.001(3) -0.024(4) 0.021(4) O3 0.064(5) 0.039(4) 0.064(4) -0.004(3) -0.014(4) -0.013(4) O4 0.089(7) 0.069(6) 0.054(4) -0.003(4) -0.007(4) 0.008(5) O5 0.080(6) 0.050(5) 0.039(3) -0.004(3) 0.001(3) 0.014(4) O6 0.050(5) 0.061(5) 0.035(3) 0.003(3) -0.008(3) 0.022(3) O7 0.040(4) 0.055(5) 0.033(3) -0.004(3) -0.011(3) -0.002(3) O8 0.051(5) 0.089(6) 0.050(4) 0.019(4) 0.008(3) -0.007(4) O9 0.039(5) 0.070(6) 0.062(4) 0.020(4) 0.008(3) -0.005(4) O10 0.059(5) 0.066(6) 0.063(4) 0.007(4) -0.007(4) 0.010(4) O11 0.045(5) 0.076(6) 0.048(3) 0.012(4) 0.001(3) 0.004(4) O12 0.036(4) 0.067(5) 0.037(3) -0.004(3) -0.001(3) -0.015(3) C1 0.040(7) 0.074(8) 0.048(5) 0.007(5) 0.003(4) 0.020(6) C2 0.058(8) 0.069(9) 0.052(6) 0.007(5) -0.001(5) 0.017(6) C3 0.073(8) 0.030(6) 0.042(5) 0.013(4) -0.007(5) 0.000(5) C4 0.040(6) 0.045(7) 0.036(4) 0.005(4) 0.001(4) 0.008(4) C5 0.052(7) 0.072(9) 0.040(5) -0.004(5) -0.008(4) 0.003(6) C6 0.049(8) 0.071(9) 0.060(6) 0.005(6) 0.004(5) -0.012(6) C7 0.057(7) 0.068(8) 0.029(4) 0.016(4) -0.005(4) 0.017(6) C8 0.108(11) 0.027(6) 0.064(6) -0.018(5) -0.032(6) 0.006(6) C9 0.059(8) 0.052(8) 0.059(6) 0.002(5) -0.013(5) 0.015(6) C10 0.040(7) 0.087(10) 0.056(6) -0.001(6) 0.002(5) 0.037(6) C11 0.057(8) 0.062(8) 0.043(5) -0.007(5) -0.009(5) -0.006(6) C12 0.045(7) 0.056(7) 0.041(5) 0.009(4) -0.003(4) -0.018(5) C13 0.051(8) 0.046(7) 0.081(6) -0.003(6) -0.001(6) -0.005(5) C14 0.057(8) 0.071(8) 0.039(5) 0.002(5) -0.009(5) 0.011(6) C15 0.041(7) 0.088(9) 0.040(5) 0.009(5) -0.008(4) 0.005(6) C16 0.058(8) 0.073(9) 0.048(6) -0.008(5) 0.012(5) -0.007(6) C17 0.046(7) 0.069(9) 0.063(6) 0.011(5) -0.008(5) 0.012(6) C18 0.042(7) 0.075(8) 0.045(5) -0.007(5) 0.000(4) 0.010(5) C19 0.090(10) 0.060(8) 0.041(5) 0.006(5) -0.014(5) -0.024(7) C20 0.065(8) 0.094(10) 0.034(4) 0.009(5) -0.002(5) -0.035(7) C21 0.032(6) 0.059(7) 0.029(4) 0.005(4) 0.006(4) 0.017(4) C22 0.034(6) 0.045(7) 0.041(5) 0.003(4) -0.007(4) -0.007(5) C23 0.037(7) 0.066(8) 0.065(6) 0.000(5) -0.003(5) 0.006(5) C24 0.032(6) 0.038(6) 0.064(6) -0.010(5) -0.007(5) 0.008(4) C25 0.040(7) 0.056(8) 0.050(5) 0.010(5) -0.005(4) 0.002(5) C26 0.050(7) 0.044(7) 0.054(5) 0.003(5) -0.011(5) 0.007(5) C27 0.029(6) 0.032(6) 0.054(5) 0.000(4) 0.003(4) -0.003(4) C28 0.035(6) 0.043(6) 0.048(5) 0.012(4) -0.005(4) 0.008(4) C29 0.082(8) 0.004(4) 0.042(4) -0.001(3) -0.009(4) 0.006(4) C30 0.083(9) 0.018(6) 0.053(5) 0.003(4) -0.008(5) 0.011(5) C31 0.073(8) 0.052(8) 0.029(4) -0.007(4) 0.010(5) -0.008(5) C32 0.068(8) 0.036(6) 0.040(5) 0.004(4) -0.005(5) -0.001(5) C33 0.028(6) 0.059(7) 0.049(5) 0.001(5) -0.002(4) 0.010(5) C34 0.036(6) 0.046(7) 0.040(5) -0.002(4) 0.000(4) 0.025(4) C35 0.060(8) 0.057(8) 0.039(5) -0.001(5) 0.004(5) 0.019(5) C36 0.031(7) 0.099(10) 0.040(5) -0.007(5) 0.001(4) 0.013(6) C37 0.023(6) 0.100(10) 0.035(4) 0.004(5) -0.004(4) 0.007(5) C38 0.075(9) 0.044(7) 0.049(5) -0.014(5) -0.002(5) 0.021(6) C39 0.025(6) 0.071(8) 0.050(5) 0.005(5) -0.007(4) -0.024(5) C40 0.052(7) 0.039(6) 0.029(4) 0.009(4) 0.004(4) 0.000(4) C41 0.065(7) 0.014(5) 0.036(4) 0.005(3) -0.010(4) -0.013(4) C42 0.039(7) 0.033(6) 0.060(5) -0.001(5) -0.005(4) -0.001(4) C43 0.066(8) 0.049(7) 0.037(5) 0.000(4) -0.009(5) -0.009(5) C44 0.045(7) 0.045(7) 0.053(5) 0.001(5) -0.002(4) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C27 1.779(9) . ? S1 C26 1.791(11) . ? S2 C29 1.761(10) . ? S2 C33 1.804(10) . ? S3 C35 1.785(11) . ? S3 C39 1.788(10) . ? S4 C41 1.775(9) . ? S4 C22 1.794(9) . ? O1 C21 1.391(9) . ? O1 C1 1.475(11) . ? O2 C3 1.388(11) . ? O2 C2 1.454(11) . ? O3 C5 1.423(10) . ? O3 C4 1.444(11) . ? O4 C7 1.401(11) . ? O4 C6 1.398(12) . ? O5 C8 1.391(10) . ? O5 C9 1.411(12) . ? O6 C34 1.354(10) . ? O6 C10 1.473(11) . ? O7 C28 1.389(10) . ? O7 C11 1.427(11) . ? O8 C13 1.401(12) . ? O8 C12 1.407(11) . ? O9 C14 1.398(12) . ? O9 C15 1.433(10) . ? O10 C17 1.392(10) . ? O10 C16 1.441(12) . ? O11 C18 1.415(10) . ? O11 C19 1.451(13) . ? O12 C40 1.391(9) . ? O12 C20 1.424(11) . ? C1 C2 1.494(12) . ? C3 C4 1.535(12) . ? C5 C6 1.528(16) . ? C7 C8 1.529(14) . ? C9 C10 1.495(13) . ? C11 C12 1.466(11) . ? C13 C14 1.529(14) . ? C15 C16 1.475(14) . ? C17 C18 1.542(14) . ? C19 C20 1.514(12) . ? C21 C26 1.371(13) . ? C21 C22 1.379(12) . ? C22 C23 1.394(13) . ? C23 C24 1.391(13) . ? C24 C25 1.365(14) . ? C25 C26 1.402(12) . ? C27 C32 1.394(11) . ? C27 C28 1.413(12) . ? C28 C29 1.412(12) . ? C29 C30 1.378(11) . ? C30 C31 1.402(14) . ? C31 C32 1.391(14) . ? C33 C38 1.384(12) . ? C33 C34 1.418(13) . ? C34 C35 1.411(14) . ? C35 C36 1.395(12) . ? C36 C37 1.347(15) . ? C37 C38 1.400(14) . ? C39 C44 1.368(12) . ? C39 C40 1.397(13) . ? C40 C41 1.401(13) . ? C41 C42 1.396(11) . ? C42 C43 1.425(13) . ? C43 C44 1.377(14) . ? 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 C27 S1 C26 100.2(4) . . ? C29 S2 C33 99.4(4) . . ? C35 S3 C39 99.9(5) . . ? C41 S4 C22 99.6(4) . . ? C21 O1 C1 113.0(6) . . ? C3 O2 C2 114.4(8) . . ? C5 O3 C4 110.6(7) . . ? C7 O4 C6 115.7(9) . . ? C8 O5 C9 110.9(9) . . ? C34 O6 C10 114.8(7) . . ? C28 O7 C11 113.9(7) . . ? C13 O8 C12 117.4(8) . . ? C14 O9 C15 113.2(7) . . ? C17 O10 C16 111.8(8) . . ? C18 O11 C19 110.6(8) . . ? C40 O12 C20 113.1(7) . . ? O1 C1 C2 111.3(8) . . ? O2 C2 C1 112.2(9) . . ? O2 C3 C4 105.6(7) . . ? O3 C4 C3 104.1(7) . . ? O3 C5 C6 107.7(9) . . ? O4 C6 C5 116.3(9) . . ? O4 C7 C8 106.4(8) . . ? O5 C8 C7 108.1(9) . . ? O5 C9 C10 109.6(9) . . ? O6 C10 C9 108.3(8) . . ? O7 C11 C12 109.3(8) . . ? O8 C12 C11 115.6(9) . . ? O8 C13 C14 110.8(9) . . ? O9 C14 C13 107.1(8) . . ? O9 C15 C16 107.2(8) . . ? O10 C16 C15 114.8(9) . . ? O10 C17 C18 105.5(8) . . ? O11 C18 C17 108.5(8) . . ? O11 C19 C20 108.5(9) . . ? O12 C20 C19 107.4(8) . . ? C26 C21 C22 120.6(8) . . ? C26 C21 O1 119.1(9) . . ? C22 C21 O1 120.2(9) . . ? C21 C22 C23 119.5(9) . . ? C21 C22 S4 121.2(7) . . ? C23 C22 S4 119.3(7) . . ? C22 C23 C24 120.0(10) . . ? C25 C24 C23 119.9(9) . . ? C24 C25 C26 120.1(10) . . ? C21 C26 C25 119.7(10) . . ? C21 C26 S1 121.5(7) . . ? C25 C26 S1 118.7(8) . . ? C32 C27 C28 117.9(9) . . ? C32 C27 S1 119.7(7) . . ? C28 C27 S1 121.8(6) . . ? O7 C28 C27 119.8(8) . . ? O7 C28 C29 119.3(8) . . ? C27 C28 C29 120.9(8) . . ? C30 C29 C28 118.7(9) . . ? C30 C29 S2 121.2(8) . . ? C28 C29 S2 120.0(6) . . ? C29 C30 C31 122.0(10) . . ? C32 C31 C30 118.2(8) . . ? C31 C32 C27 122.3(9) . . ? C38 C33 C34 121.7(10) . . ? C38 C33 S2 119.0(8) . . ? C34 C33 S2 119.3(7) . . ? O6 C34 C33 122.0(9) . . ? O6 C34 C35 120.5(9) . . ? C33 C34 C35 117.3(8) . . ? C36 C35 C34 119.2(10) . . ? C36 C35 S3 122.8(9) . . ? C34 C35 S3 118.0(7) . . ? C37 C36 C35 122.7(11) . . ? C36 C37 C38 119.7(9) . . ? C33 C38 C37 119.3(10) . . ? C44 C39 C40 119.8(9) . . ? C44 C39 S3 119.7(8) . . ? C40 C39 S3 120.4(7) . . ? C39 C40 O12 122.3(9) . . ? C39 C40 C41 120.7(7) . . ? O12 C40 C41 116.9(8) . . ? C42 C41 C40 119.1(9) . . ? C42 C41 S4 119.0(8) . . ? C40 C41 S4 121.8(6) . . ? C41 C42 C43 119.2(9) . . ? C44 C43 C42 119.9(8) . . ? C39 C44 C43 121.0(10) . . ? #===END