# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Parimal Paul' _publ_contact_author_email ppaul@csmcri.org _publ_section_title ; Effect of steric crowding on ion selectivity for calix-crown hybrid ionophores: Experimental, molecular modeling and crystallographic studies ; _publ_author_name 'Parimal Paul' # Attachment '- CIF (revised_ID NJ-ART-10-2009-000587).txt' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 749549' #TrackingRef '- CIF (revised_ID NJ-ART-10-2009-000587).txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H57 N O8 S' _chemical_formula_weight 820.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.9671(12) _cell_length_b 10.0972(7) _cell_length_c 25.6043(19) _cell_angle_alpha 90.00 _cell_angle_beta 104.276(2) _cell_angle_gamma 90.00 _cell_volume 4251.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCKS _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.9390 _exptl_absorpt_correction_T_max 0.9714 _exptl_special_details ; ? ; _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 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21383 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7930 _reflns_number_gt 6064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.17(12) _refine_ls_number_reflns 7930 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.93969(10) 0.84321(15) 0.00131(6) 0.0199(4) Uani 1 d . . . N1 N 0.9821(3) 0.8748(5) 0.06364(18) 0.0187(11) Uani 1 d . . . O1 O 1.0057(2) 0.9562(4) 0.37516(14) 0.0164(9) Uani 1 d . . . O2 O 1.0658(2) 0.5511(4) 0.33537(15) 0.0195(9) Uani 1 d . . . O3 O 1.1326(2) 0.8657(4) 0.26569(14) 0.0195(9) Uani 1 d . . . O4 O 1.1531(2) 0.9139(4) 0.13276(15) 0.0204(10) Uani 1 d . . . O5 O 0.8487(3) 0.7778(4) 0.12116(15) 0.0267(11) Uani 1 d . . . O6 O 0.8694(2) 0.7509(4) 0.24085(14) 0.0161(9) Uani 1 d . . . O7 O 0.9955(3) 0.8733(5) -0.03086(16) 0.0311(11) Uani 1 d . . . O8 O 0.9066(3) 0.7130(4) -0.00085(16) 0.0245(10) Uani 1 d . . . C1 C 0.9880(4) 1.0180(6) 0.3251(2) 0.0173(13) Uani 1 d . . . C2 C 0.9071(3) 1.0216(5) 0.2935(2) 0.0151(13) Uani 1 d . . . C3 C 0.8926(4) 1.0927(6) 0.2454(2) 0.0225(15) Uani 1 d . . . H3 H 0.8399 1.0973 0.2237 0.027 Uiso 1 calc R . . C4 C 0.9547(4) 1.1569(5) 0.2291(2) 0.0200(14) Uani 1 d . . . H4 H 0.9434 1.2066 0.1976 0.024 Uiso 1 calc R . . C5 C 1.0333(4) 1.1462(5) 0.2601(2) 0.0233(15) Uani 1 d . . . H5 H 1.0751 1.1872 0.2487 0.028 Uiso 1 calc R . . C6 C 1.0514(4) 1.0752(6) 0.3083(2) 0.0186(14) Uani 1 d . . . C7 C 1.1387(4) 1.0677(6) 0.3423(2) 0.0211(14) Uani 1 d . . . H7A H 1.1731 1.1136 0.3230 0.025 Uiso 1 calc R . . H7B H 1.1418 1.1160 0.3755 0.025 Uiso 1 calc R . . C8 C 1.1742(3) 0.9314(6) 0.3569(2) 0.0182(14) Uani 1 d . . . C9 C 1.2153(4) 0.9035(6) 0.4095(2) 0.0199(14) Uani 1 d . . . H9 H 1.2173 0.9676 0.4359 0.024 Uiso 1 calc R . . C10 C 1.2530(4) 0.7839(6) 0.4240(2) 0.0229(15) Uani 1 d . . . H10 H 1.2803 0.7672 0.4596 0.028 Uiso 1 calc R . . C11 C 1.2496(4) 0.6886(6) 0.3844(2) 0.0218(15) Uani 1 d . . . H11 H 1.2762 0.6084 0.3939 0.026 Uiso 1 calc R . . C12 C 1.2083(3) 0.7087(6) 0.3316(2) 0.0156(13) Uani 1 d . . . C13 C 1.1732(3) 0.8328(6) 0.3176(2) 0.0167(13) Uani 1 d . . . C14 C 1.2053(3) 0.5963(6) 0.2913(2) 0.0193(14) Uani 1 d . . . H14A H 1.2380 0.6224 0.2668 0.023 Uiso 1 calc R . . H14B H 1.2313 0.5195 0.3110 0.023 Uiso 1 calc R . . C15 C 1.1221(4) 0.5537(5) 0.2575(2) 0.0154(13) Uani 1 d . . . C16 C 1.1103(4) 0.5258(5) 0.2033(2) 0.0155(13) Uani 1 d . . . H16 H 1.1543 0.5322 0.1879 0.019 Uiso 1 calc R . . C17 C 1.0361(4) 0.4891(5) 0.1714(2) 0.0158(13) Uani 1 d . . . H17 H 1.0302 0.4711 0.1350 0.019 Uiso 1 calc R . . C18 C 0.9701(4) 0.4793(5) 0.1941(2) 0.0145(13) Uani 1 d . . . H18 H 0.9192 0.4579 0.1725 0.017 Uiso 1 calc R . . C19 C 0.9792(4) 0.5010(5) 0.2486(2) 0.0151(13) Uani 1 d . . . C20 C 1.0562(3) 0.5353(5) 0.2803(2) 0.0132(12) Uani 1 d . . . C21 C 0.9077(4) 0.4773(6) 0.2738(2) 0.0200(14) Uani 1 d . . . H21A H 0.8596 0.4626 0.2448 0.024 Uiso 1 calc R . . H21B H 0.9181 0.3960 0.2945 0.024 Uiso 1 calc R . . C22 C 0.8881(3) 0.5839(6) 0.3099(2) 0.0167(13) Uani 1 d . . . C23 C 0.8867(3) 0.5522(6) 0.3629(2) 0.0204(14) Uani 1 d . . . H23 H 0.9018 0.4674 0.3758 0.025 Uiso 1 calc R . . C24 C 0.8637(4) 0.6428(6) 0.3965(2) 0.0220(14) Uani 1 d . . . H24 H 0.8596 0.6180 0.4307 0.026 Uiso 1 calc R . . C25 C 0.8470(3) 0.7711(6) 0.3786(2) 0.0197(14) Uani 1 d . . . H25 H 0.8322 0.8332 0.4013 0.024 Uiso 1 calc R . . C26 C 0.8518(3) 0.8089(6) 0.3275(2) 0.0168(13) Uani 1 d . . . C27 C 0.8686(3) 0.7133(6) 0.2930(2) 0.0138(13) Uani 1 d . . . C28 C 0.8379(4) 0.9532(6) 0.3097(2) 0.0205(14) Uani 1 d . . . H28A H 0.7905 0.9568 0.2794 0.025 Uiso 1 calc R . . H28B H 0.8251 1.0031 0.3389 0.025 Uiso 1 calc R . . C29 C 0.9887(4) 1.0339(7) 0.4173(2) 0.0301(16) Uani 1 d . . . H29A H 0.9311 1.0283 0.4158 0.036 Uiso 1 calc R . . H29B H 1.0015 1.1258 0.4121 0.036 Uiso 1 calc R . . C30 C 1.0355(5) 0.9894(8) 0.4701(3) 0.046(2) Uani 1 d . . . H30A H 1.0131 1.0327 0.4970 0.055 Uiso 1 calc R . . H30B H 1.0906 1.0220 0.4749 0.055 Uiso 1 calc R . . C31 C 1.0408(4) 0.8474(8) 0.4826(3) 0.0410(19) Uani 1 d . . . H31A H 0.9880 0.8147 0.4834 0.062 Uiso 1 calc R . . H31B H 1.0778 0.8336 0.5171 0.062 Uiso 1 calc R . . H31C H 1.0600 0.8009 0.4555 0.062 Uiso 1 calc R . . C32 C 1.0999(4) 0.4373(6) 0.3669(2) 0.0211(14) Uani 1 d . . . H32A H 1.1523 0.4155 0.3604 0.025 Uiso 1 calc R . . H32B H 1.0641 0.3616 0.3569 0.025 Uiso 1 calc R . . C33 C 1.1094(4) 0.4692(6) 0.4250(2) 0.0247(15) Uani 1 d . . . H33A H 1.0561 0.4807 0.4319 0.030 Uiso 1 calc R . . H33B H 1.1388 0.5519 0.4334 0.030 Uiso 1 calc R . . C34 C 1.1548(4) 0.3607(7) 0.4612(2) 0.0356(17) Uani 1 d . . . H34A H 1.1251 0.2791 0.4536 0.053 Uiso 1 calc R . . H34B H 1.1603 0.3846 0.4982 0.053 Uiso 1 calc R . . H34C H 1.2078 0.3497 0.4547 0.053 Uiso 1 calc R . . C35 C 1.1740(3) 0.8529(6) 0.2237(2) 0.0185(13) Uani 1 d . . . H35A H 1.1637 0.7663 0.2070 0.022 Uiso 1 calc R . . H35B H 1.2322 0.8629 0.2382 0.022 Uiso 1 calc R . . C36 C 1.1424(4) 0.9592(6) 0.1833(2) 0.0194(14) Uani 1 d . . . H36A H 1.0853 0.9756 0.1809 0.023 Uiso 1 calc R . . H36B H 1.1723 1.0409 0.1937 0.023 Uiso 1 calc R . . C37 C 1.1158(4) 0.9975(6) 0.0887(2) 0.0220(14) Uani 1 d . . . H37A H 1.1313 0.9667 0.0567 0.026 Uiso 1 calc R . . H37B H 1.1372 1.0864 0.0963 0.026 Uiso 1 calc R . . C38 C 1.0234(4) 1.0039(6) 0.0763(2) 0.0201(14) Uani 1 d . . . H38A H 1.0080 1.0418 0.1072 0.024 Uiso 1 calc R . . H38B H 1.0041 1.0630 0.0460 0.024 Uiso 1 calc R . . C39 C 0.9817(4) 0.7818(6) 0.1071(2) 0.0182(13) Uani 1 d . . . H39A H 1.0375 0.7699 0.1276 0.022 Uiso 1 calc R . . H39B H 0.9630 0.6969 0.0909 0.022 Uiso 1 calc R . . C40 C 0.9319(4) 0.8157(6) 0.1456(2) 0.0224(14) Uani 1 d . . . H40A H 0.9519 0.7685 0.1792 0.027 Uiso 1 calc R . . H40B H 0.9350 0.9100 0.1530 0.027 Uiso 1 calc R . . C41 C 0.7927(4) 0.8104(7) 0.1519(2) 0.0266(16) Uani 1 d . . . H41A H 0.7382 0.8049 0.1287 0.032 Uiso 1 calc R . . H41B H 0.8018 0.9017 0.1637 0.032 Uiso 1 calc R . . C42 C 0.7967(4) 0.7254(7) 0.2006(2) 0.0261(15) Uani 1 d . . . H42A H 0.7500 0.7433 0.2150 0.031 Uiso 1 calc R . . H42B H 0.7950 0.6328 0.1903 0.031 Uiso 1 calc R . . C43 C 0.8582(4) 0.9565(6) -0.0189(2) 0.0185(14) Uani 1 d . . . C44 C 0.8640(4) 1.0604(6) -0.0534(2) 0.0201(14) Uani 1 d . . . H44 H 0.9112 1.0724 -0.0652 0.024 Uiso 1 calc R . . C45 C 0.7986(4) 1.1463(6) -0.0699(2) 0.0264(16) Uani 1 d . . . H45 H 0.8018 1.2152 -0.0934 0.032 Uiso 1 calc R . . C46 C 0.7286(4) 1.1306(6) -0.0519(2) 0.0214(14) Uani 1 d . . . C47 C 0.7239(4) 1.0266(6) -0.0174(2) 0.0201(14) Uani 1 d . . . H47 H 0.6766 1.0147 -0.0058 0.024 Uiso 1 calc R . . C48 C 0.7885(4) 0.9402(6) -0.0001(2) 0.0218(14) Uani 1 d . . . H48 H 0.7854 0.8722 0.0238 0.026 Uiso 1 calc R . . C49 C 0.6582(4) 1.2260(7) -0.0696(3) 0.0313(17) Uani 1 d . . . H49A H 0.6081 1.1808 -0.0705 0.047 Uiso 1 calc R . . H49B H 0.6572 1.2592 -0.1048 0.047 Uiso 1 calc R . . H49C H 0.6647 1.2984 -0.0446 0.047 Uiso 1 calc R . . S2 S 0.57812(12) 0.61542(17) 1.02527(7) 0.0335(4) Uani 1 d . . . O9 O 0.5100(2) 0.5253(4) 0.63036(15) 0.0187(9) Uani 1 d . . . O10 O 0.4164(2) 0.9340(4) 0.65742(15) 0.0185(9) Uani 1 d . . . O11 O 0.3917(3) 0.6336(4) 0.72681(17) 0.0294(11) Uani 1 d . . . O12 O 0.4140(3) 0.6328(4) 0.86910(15) 0.0256(10) Uani 1 d . . . O13 O 0.6860(3) 0.6763(5) 0.8645(2) 0.0520(15) Uani 1 d . . . O14 O 0.6242(2) 0.7872(4) 0.76186(15) 0.0200(9) Uani 1 d . . . O15 O 0.6054(3) 0.7458(5) 1.04321(18) 0.0501(15) Uani 1 d . . . O16 O 0.5096(3) 0.5574(6) 1.03990(19) 0.0496(15) Uani 1 d . . . N2 N 0.5568(3) 0.6197(5) 0.96022(19) 0.0273(13) Uani 1 d . . . C50 C 0.5256(3) 0.4731(5) 0.6818(2) 0.0142(13) Uani 1 d . . . C51 C 0.4635(4) 0.4057(5) 0.6966(2) 0.0172(13) Uani 1 d . . . C52 C 0.4799(3) 0.3481(6) 0.7473(2) 0.0184(13) Uani 1 d . . . H52 H 0.4400 0.2977 0.7571 0.022 Uiso 1 calc R . . C53 C 0.5543(4) 0.3641(6) 0.7834(2) 0.0217(14) Uani 1 d . . . H53 H 0.5650 0.3230 0.8169 0.026 Uiso 1 calc R . . C54 C 0.6126(4) 0.4415(6) 0.7694(2) 0.0199(14) Uani 1 d . . . H54 H 0.6612 0.4581 0.7947 0.024 Uiso 1 calc R . . C55 C 0.5999(4) 0.4953(6) 0.7177(2) 0.0172(13) Uani 1 d . . . C56 C 0.6679(4) 0.5748(6) 0.7020(2) 0.0231(15) Uani 1 d . . . H56A H 0.7123 0.5849 0.7339 0.028 Uiso 1 calc R . . H56B H 0.6882 0.5227 0.6762 0.028 Uiso 1 calc R . . C57 C 0.6457(3) 0.7094(6) 0.6782(2) 0.0170(13) Uani 1 d . . . C58 C 0.6483(4) 0.7372(6) 0.6254(2) 0.0226(15) Uani 1 d . . . H58 H 0.6661 0.6725 0.6052 0.027 Uiso 1 calc R . . C59 C 0.6249(3) 0.8591(6) 0.6026(2) 0.0206(14) Uani 1 d . . . H59 H 0.6273 0.8766 0.5674 0.025 Uiso 1 calc R . . C60 C 0.5977(4) 0.9556(6) 0.6326(2) 0.0234(15) Uani 1 d . . . H60 H 0.5805 1.0369 0.6167 0.028 Uiso 1 calc R . . C61 C 0.5958(3) 0.9330(6) 0.6859(2) 0.0171(13) Uani 1 d . . . C62 C 0.6224(3) 0.8105(6) 0.7081(2) 0.0166(14) Uani 1 d . . . C63 C 0.5679(4) 1.0408(6) 0.7181(3) 0.0281(16) Uani 1 d . . . H63A H 0.5513 1.1167 0.6948 0.034 Uiso 1 calc R . . H63B H 0.6138 1.0679 0.7468 0.034 Uiso 1 calc R . . C64 C 0.4976(4) 1.0029(5) 0.7431(2) 0.0181(14) Uani 1 d . . . C65 C 0.5054(4) 1.0247(6) 0.7981(2) 0.0232(14) Uani 1 d . . . H65 H 0.5536 1.0587 0.8194 0.028 Uiso 1 calc R . . C66 C 0.4415(4) 0.9957(6) 0.8208(3) 0.0270(16) Uani 1 d . . . H66 H 0.4462 1.0119 0.8572 0.032 Uiso 1 calc R . . C67 C 0.3702(4) 0.9422(6) 0.7891(2) 0.0219(15) Uani 1 d . . . H67 H 0.3275 0.9220 0.8046 0.026 Uiso 1 calc R . . C68 C 0.3617(4) 0.9187(6) 0.7349(2) 0.0188(14) Uani 1 d . . . C69 C 0.4256(4) 0.9542(5) 0.7122(2) 0.0166(13) Uani 1 d . . . C70 C 0.2840(4) 0.8608(6) 0.7010(2) 0.0244(15) Uani 1 d . . . H70A H 0.2538 0.9323 0.6797 0.029 Uiso 1 calc R . . H70B H 0.2520 0.8307 0.7253 0.029 Uiso 1 calc R . . C71 C 0.2883(4) 0.7464(6) 0.6624(2) 0.0176(14) Uani 1 d . . . C72 C 0.2387(4) 0.7514(6) 0.6099(2) 0.0257(15) Uani 1 d . . . H72 H 0.2054 0.8247 0.5991 0.031 Uiso 1 calc R . . C73 C 0.2383(4) 0.6494(6) 0.5739(2) 0.0249(15) Uani 1 d . . . H73 H 0.2059 0.6545 0.5390 0.030 Uiso 1 calc R . . C74 C 0.2866(4) 0.5397(6) 0.5905(2) 0.0209(14) Uani 1 d . . . H74 H 0.2865 0.4713 0.5662 0.025 Uiso 1 calc R . . C75 C 0.3356(3) 0.5290(6) 0.6429(2) 0.0166(13) Uani 1 d . . . C76 C 0.3355(3) 0.6340(6) 0.6771(2) 0.0175(13) Uani 1 d . . . C77 C 0.3794(4) 0.3981(6) 0.6595(2) 0.0202(14) Uani 1 d . . . H77A H 0.3458 0.3446 0.6769 0.024 Uiso 1 calc R . . H77B H 0.3833 0.3517 0.6270 0.024 Uiso 1 calc R . . C78 C 0.5277(4) 0.4391(7) 0.5909(2) 0.0331(17) Uani 1 d . . . H78A H 0.5135 0.3492 0.5982 0.040 Uiso 1 calc R . . H78B H 0.5856 0.4416 0.5932 0.040 Uiso 1 calc R . . C79 C 0.4833(7) 0.4760(8) 0.5365(3) 0.066(3) Uani 1 d . . . H79A H 0.5128 0.4385 0.5120 0.080 Uiso 1 calc R . . H79B H 0.4313 0.4307 0.5295 0.080 Uiso 1 calc R . . C80 C 0.4667(5) 0.6092(8) 0.5209(3) 0.052(2) Uani 1 d . . . H80A H 0.4497 0.6560 0.5488 0.078 Uiso 1 calc R . . H80B H 0.4242 0.6124 0.4882 0.078 Uiso 1 calc R . . H80C H 0.5149 0.6497 0.5149 0.078 Uiso 1 calc R . . C81 C 0.3822(4) 1.0453(6) 0.6256(2) 0.0288(16) Uani 1 d . . . H81A H 0.4184 1.1208 0.6346 0.035 Uiso 1 calc R . . H81B H 0.3305 1.0685 0.6329 0.035 Uiso 1 calc R . . C82 C 0.3701(4) 1.0115(7) 0.5669(2) 0.0292(16) Uani 1 d . . . H82A H 0.3350 0.9345 0.5584 0.035 Uiso 1 calc R . . H82B H 0.4221 0.9893 0.5598 0.035 Uiso 1 calc R . . C83 C 0.3320(4) 1.1269(7) 0.5309(2) 0.0366(18) Uani 1 d . . . H83A H 0.2798 1.1472 0.5371 0.055 Uiso 1 calc R . . H83B H 0.3255 1.1029 0.4938 0.055 Uiso 1 calc R . . H83C H 0.3667 1.2030 0.5391 0.055 Uiso 1 calc R . . C84 C 0.3652(4) 0.6046(6) 0.7721(2) 0.0284(16) Uani 1 d . . . H84A H 0.3479 0.5129 0.7715 0.034 Uiso 1 calc R . . H84B H 0.3198 0.6610 0.7742 0.034 Uiso 1 calc R . . C85 C 0.4372(4) 0.6294(7) 0.8199(2) 0.0324(17) Uani 1 d . . . H85A H 0.4772 0.5600 0.8214 0.039 Uiso 1 calc R . . H85B H 0.4623 0.7131 0.8147 0.039 Uiso 1 calc R . . C86 C 0.4310(4) 0.5187(7) 0.9025(3) 0.0282(16) Uani 1 d . . . H86A H 0.4126 0.4408 0.8807 0.034 Uiso 1 calc R . . H86B H 0.4003 0.5240 0.9297 0.034 Uiso 1 calc R . . C87 C 0.5199(4) 0.5020(6) 0.9300(3) 0.0294(16) Uani 1 d . . . H87A H 0.5258 0.4275 0.9546 0.035 Uiso 1 calc R . . H87B H 0.5493 0.4810 0.9031 0.035 Uiso 1 calc R . . C88 C 0.5991(5) 0.7113(7) 0.9305(3) 0.048(2) Uani 1 d . . . H88A H 0.6121 0.7921 0.9513 0.058 Uiso 1 calc R . . H88B H 0.5617 0.7343 0.8966 0.058 Uiso 1 calc R . . C89 C 0.6784(5) 0.6566(8) 0.9186(3) 0.047(2) Uani 1 d . . . H89A H 0.7244 0.6984 0.9432 0.056 Uiso 1 calc R . . H89B H 0.6816 0.5624 0.9262 0.056 Uiso 1 calc R . . C90 C 0.6960(6) 0.8045(8) 0.8544(3) 0.063(3) Uani 1 d . . . H90A H 0.7458 0.8363 0.8785 0.076 Uiso 1 calc R . . H90B H 0.6511 0.8550 0.8615 0.076 Uiso 1 calc R . . C91 C 0.7000(4) 0.8274(6) 0.7969(2) 0.0245(15) Uani 1 d . . . H91A H 0.7098 0.9204 0.7914 0.029 Uiso 1 calc R . . H91B H 0.7443 0.7765 0.7892 0.029 Uiso 1 calc R . . C92 C 0.6610(4) 0.5070(7) 1.0472(2) 0.0268(16) Uani 1 d . . . C93 C 0.7386(4) 0.5464(6) 1.0454(2) 0.0232(15) Uani 1 d . . . H93 H 0.7477 0.6332 1.0362 0.028 Uiso 1 calc R . . C94 C 0.8024(4) 0.4579(6) 1.0573(2) 0.0232(15) Uani 1 d . . . H94 H 0.8538 0.4849 1.0550 0.028 Uiso 1 calc R . . C95 C 0.7907(4) 0.3285(5) 1.0727(2) 0.0155(13) Uani 1 d . . . C96 C 0.7137(4) 0.2943(6) 1.0782(2) 0.0212(14) Uani 1 d . . . H96 H 0.7061 0.2109 1.0915 0.025 Uiso 1 calc R . . C97 C 0.6485(4) 0.3795(6) 1.0645(2) 0.0255(15) Uani 1 d . . . H97 H 0.5970 0.3524 1.0667 0.031 Uiso 1 calc R . . C98 C 0.8592(4) 0.2303(6) 1.0832(2) 0.0243(15) Uani 1 d . . . H98A H 0.8470 0.1586 1.1045 0.036 Uiso 1 calc R . . H98B H 0.9085 0.2731 1.1022 0.036 Uiso 1 calc R . . H98C H 0.8660 0.1965 1.0495 0.036 Uiso 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 0.0242(9) 0.0188(8) 0.0174(8) -0.0007(7) 0.0061(7) 0.0059(7) N1 0.023(3) 0.013(3) 0.020(3) 0.003(2) 0.005(2) 0.002(2) O1 0.016(2) 0.017(2) 0.016(2) 0.0037(17) 0.0039(17) 0.0024(18) O2 0.024(2) 0.018(2) 0.016(2) -0.0022(17) 0.0036(19) 0.0001(19) O3 0.018(2) 0.023(2) 0.016(2) -0.0017(18) 0.0016(18) 0.0081(19) O4 0.022(2) 0.020(2) 0.019(2) 0.0036(18) 0.0035(18) 0.0036(19) O5 0.020(3) 0.040(3) 0.019(2) -0.002(2) 0.0027(19) -0.004(2) O6 0.014(2) 0.021(2) 0.013(2) 0.0006(17) 0.0035(17) -0.0040(18) O7 0.032(3) 0.042(3) 0.022(2) 0.002(2) 0.011(2) 0.010(2) O8 0.034(3) 0.010(2) 0.026(2) -0.0075(18) 0.000(2) 0.008(2) C1 0.018(3) 0.014(3) 0.022(3) 0.001(3) 0.009(3) 0.005(3) C2 0.014(3) 0.010(3) 0.022(3) -0.006(2) 0.006(3) 0.002(3) C3 0.026(4) 0.017(3) 0.019(3) -0.006(3) -0.004(3) 0.005(3) C4 0.036(4) 0.006(3) 0.017(3) -0.002(2) 0.005(3) 0.003(3) C5 0.038(4) 0.007(3) 0.026(4) -0.002(3) 0.010(3) -0.006(3) C6 0.021(4) 0.014(3) 0.021(3) -0.007(3) 0.006(3) -0.002(3) C7 0.021(4) 0.018(3) 0.025(4) -0.005(3) 0.007(3) -0.005(3) C8 0.012(3) 0.019(3) 0.023(3) -0.005(3) 0.005(3) -0.008(3) C9 0.019(4) 0.022(3) 0.018(3) -0.008(3) 0.003(3) -0.006(3) C10 0.023(4) 0.027(4) 0.016(3) 0.003(3) 0.000(3) -0.003(3) C11 0.018(4) 0.019(3) 0.030(4) 0.003(3) 0.008(3) 0.005(3) C12 0.007(3) 0.021(3) 0.018(3) 0.000(3) 0.002(3) 0.002(3) C13 0.014(3) 0.024(3) 0.012(3) 0.002(3) 0.003(3) -0.006(3) C14 0.012(3) 0.023(3) 0.023(3) 0.004(3) 0.005(3) 0.007(3) C15 0.014(3) 0.014(3) 0.019(3) 0.003(2) 0.006(3) 0.005(3) C16 0.020(3) 0.011(3) 0.016(3) -0.001(2) 0.006(3) 0.007(3) C17 0.023(4) 0.011(3) 0.013(3) 0.001(2) 0.004(3) 0.001(3) C18 0.020(3) 0.006(3) 0.016(3) 0.003(2) 0.001(3) 0.000(2) C19 0.021(3) 0.007(3) 0.015(3) 0.002(2) -0.001(3) 0.001(3) C20 0.015(3) 0.008(3) 0.017(3) 0.001(2) 0.005(3) 0.004(2) C21 0.022(4) 0.016(3) 0.020(3) 0.003(3) 0.001(3) -0.006(3) C22 0.007(3) 0.024(4) 0.019(3) -0.002(3) 0.002(2) -0.008(3) C23 0.013(3) 0.019(3) 0.029(4) 0.007(3) 0.005(3) 0.001(3) C24 0.017(4) 0.031(4) 0.019(3) 0.003(3) 0.005(3) -0.001(3) C25 0.009(3) 0.028(4) 0.021(3) -0.005(3) 0.002(3) -0.002(3) C26 0.005(3) 0.020(3) 0.023(3) -0.001(3) -0.002(2) -0.001(3) C27 0.004(3) 0.020(3) 0.018(3) -0.001(3) 0.005(2) -0.006(3) C28 0.021(4) 0.020(3) 0.019(3) -0.006(3) 0.003(3) -0.002(3) C29 0.039(4) 0.029(4) 0.024(4) -0.001(3) 0.011(3) 0.010(3) C30 0.067(6) 0.047(5) 0.022(4) -0.010(4) 0.009(4) -0.002(4) C31 0.047(5) 0.046(5) 0.027(4) 0.010(4) 0.003(3) 0.020(4) C32 0.024(4) 0.014(3) 0.027(4) 0.002(3) 0.009(3) 0.002(3) C33 0.025(4) 0.031(4) 0.018(3) -0.001(3) 0.003(3) -0.010(3) C34 0.034(4) 0.049(5) 0.022(4) 0.007(3) 0.003(3) -0.005(4) C35 0.019(3) 0.020(3) 0.014(3) -0.008(3) 0.000(3) -0.005(3) C36 0.015(3) 0.019(3) 0.025(3) 0.001(3) 0.005(3) -0.001(3) C37 0.027(4) 0.020(3) 0.019(3) 0.004(3) 0.005(3) 0.000(3) C38 0.024(4) 0.020(3) 0.017(3) 0.000(3) 0.006(3) -0.001(3) C39 0.019(3) 0.013(3) 0.023(3) -0.001(3) 0.005(3) -0.001(3) C40 0.024(4) 0.018(3) 0.022(3) 0.002(3) 0.001(3) -0.003(3) C41 0.021(4) 0.037(4) 0.020(3) -0.002(3) 0.002(3) 0.006(3) C42 0.020(4) 0.038(4) 0.020(3) -0.003(3) 0.005(3) -0.010(3) C43 0.023(4) 0.019(3) 0.015(3) -0.006(3) 0.006(3) 0.000(3) C44 0.025(4) 0.024(3) 0.013(3) -0.003(3) 0.007(3) -0.004(3) C45 0.040(4) 0.020(4) 0.016(3) 0.008(3) 0.002(3) -0.002(3) C46 0.018(4) 0.032(4) 0.012(3) -0.007(3) -0.001(3) -0.005(3) C47 0.009(3) 0.030(4) 0.021(3) -0.004(3) 0.003(3) 0.000(3) C48 0.034(4) 0.015(3) 0.019(3) -0.001(3) 0.011(3) -0.005(3) C49 0.026(4) 0.036(4) 0.029(4) 0.006(3) 0.004(3) 0.016(3) S2 0.0424(12) 0.0315(10) 0.0223(9) 0.0026(8) 0.0000(8) 0.0167(9) O9 0.015(2) 0.023(2) 0.018(2) -0.0015(18) 0.0048(18) 0.0012(19) O10 0.025(2) 0.014(2) 0.018(2) -0.0023(17) 0.0057(18) -0.0018(18) O11 0.024(3) 0.030(3) 0.032(3) -0.002(2) 0.002(2) 0.003(2) O12 0.029(3) 0.029(3) 0.019(2) 0.003(2) 0.0055(19) 0.011(2) O13 0.060(4) 0.046(4) 0.042(3) 0.003(3) -0.005(3) 0.002(3) O14 0.016(2) 0.025(2) 0.019(2) 0.0021(18) 0.0030(18) -0.0064(19) O15 0.066(4) 0.035(3) 0.031(3) -0.009(2) -0.022(3) 0.029(3) O16 0.045(3) 0.068(4) 0.041(3) 0.017(3) 0.021(3) 0.026(3) N2 0.034(3) 0.018(3) 0.026(3) 0.002(2) 0.000(2) 0.001(3) C50 0.014(3) 0.013(3) 0.016(3) 0.001(2) 0.003(3) 0.010(3) C51 0.020(3) 0.007(3) 0.024(3) -0.004(2) 0.004(3) 0.002(3) C52 0.018(3) 0.014(3) 0.024(3) 0.002(3) 0.007(3) -0.001(3) C53 0.030(4) 0.015(3) 0.018(3) 0.002(3) 0.003(3) 0.006(3) C54 0.017(3) 0.016(3) 0.024(3) -0.006(3) 0.000(3) 0.001(3) C55 0.015(3) 0.012(3) 0.024(3) 0.003(3) 0.005(3) 0.008(3) C56 0.017(3) 0.028(4) 0.023(4) 0.002(3) 0.001(3) 0.005(3) C57 0.003(3) 0.024(3) 0.023(3) 0.000(3) 0.001(3) -0.006(3) C58 0.016(4) 0.031(4) 0.021(3) -0.007(3) 0.004(3) -0.004(3) C59 0.014(3) 0.031(4) 0.018(3) 0.008(3) 0.007(3) -0.003(3) C60 0.016(3) 0.025(4) 0.029(4) 0.009(3) 0.005(3) -0.008(3) C61 0.014(3) 0.014(3) 0.023(3) 0.000(3) 0.003(3) -0.001(3) C62 0.009(3) 0.027(4) 0.014(3) -0.002(3) 0.003(2) -0.009(3) C63 0.030(4) 0.024(4) 0.029(4) 0.007(3) 0.005(3) -0.004(3) C64 0.024(4) 0.005(3) 0.026(3) 0.000(3) 0.008(3) 0.005(3) C65 0.022(4) 0.018(3) 0.025(4) 0.001(3) -0.003(3) 0.003(3) C66 0.038(4) 0.021(4) 0.022(4) 0.001(3) 0.007(3) 0.006(3) C67 0.024(4) 0.015(3) 0.032(4) 0.001(3) 0.017(3) -0.003(3) C68 0.023(4) 0.011(3) 0.024(4) -0.004(3) 0.009(3) 0.006(3) C69 0.022(4) 0.005(3) 0.024(3) -0.003(2) 0.009(3) 0.005(3) C70 0.019(4) 0.024(4) 0.030(4) 0.002(3) 0.005(3) 0.006(3) C71 0.013(3) 0.018(3) 0.024(3) 0.004(3) 0.008(3) -0.005(3) C72 0.027(4) 0.024(4) 0.027(4) 0.009(3) 0.008(3) 0.006(3) C73 0.024(4) 0.032(4) 0.019(3) 0.005(3) 0.004(3) 0.003(3) C74 0.021(4) 0.026(4) 0.016(3) -0.003(3) 0.005(3) -0.005(3) C75 0.007(3) 0.017(3) 0.025(3) 0.002(3) 0.004(3) -0.004(3) C76 0.007(3) 0.022(3) 0.020(3) 0.000(3) -0.003(3) -0.003(3) C77 0.017(3) 0.014(3) 0.030(4) -0.001(3) 0.005(3) -0.001(3) C78 0.034(4) 0.035(4) 0.032(4) -0.003(3) 0.012(3) 0.005(3) C79 0.132(9) 0.037(5) 0.026(4) -0.006(4) 0.011(5) 0.008(6) C80 0.067(6) 0.057(6) 0.026(4) 0.002(4) 0.000(4) 0.016(5) C81 0.033(4) 0.022(4) 0.030(4) 0.006(3) 0.006(3) 0.004(3) C82 0.032(4) 0.028(4) 0.026(4) -0.003(3) 0.005(3) -0.012(3) C83 0.043(5) 0.042(5) 0.021(4) 0.004(3) 0.001(3) -0.005(4) C84 0.027(4) 0.017(3) 0.040(4) 0.008(3) 0.006(3) 0.002(3) C85 0.022(4) 0.044(4) 0.032(4) -0.004(3) 0.009(3) 0.000(3) C86 0.028(4) 0.027(4) 0.029(4) 0.009(3) 0.007(3) 0.009(3) C87 0.032(4) 0.021(4) 0.034(4) 0.005(3) 0.006(3) -0.004(3) C88 0.076(6) 0.024(4) 0.026(4) 0.011(3) -0.021(4) -0.029(4) C89 0.056(6) 0.057(5) 0.026(4) 0.006(4) 0.008(4) -0.024(5) C90 0.091(7) 0.035(5) 0.037(5) 0.003(4) -0.033(4) -0.023(5) C91 0.019(4) 0.024(4) 0.030(4) 0.005(3) 0.005(3) -0.001(3) C92 0.036(4) 0.031(4) 0.011(3) 0.000(3) 0.001(3) 0.008(3) C93 0.033(4) 0.015(3) 0.020(3) 0.002(3) 0.005(3) -0.002(3) C94 0.024(4) 0.028(4) 0.017(3) -0.003(3) 0.003(3) -0.009(3) C95 0.021(3) 0.011(3) 0.015(3) -0.004(2) 0.004(3) -0.005(3) C96 0.026(4) 0.018(3) 0.023(3) 0.003(3) 0.011(3) 0.000(3) C97 0.025(4) 0.029(4) 0.021(3) 0.003(3) 0.003(3) 0.000(3) C98 0.021(4) 0.025(4) 0.024(4) 0.000(3) 0.002(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O8 1.425(4) . ? S1 O7 1.433(4) . ? S1 N1 1.612(5) . ? S1 C43 1.771(6) . ? N1 C39 1.457(7) . ? N1 C38 1.478(7) . ? O1 C1 1.391(6) . ? O1 C29 1.420(7) . ? O2 C20 1.387(6) . ? O2 C32 1.441(7) . ? O3 C13 1.377(6) . ? O3 C35 1.426(6) . ? O4 C36 1.426(6) . ? O4 C37 1.427(6) . ? O5 C41 1.415(6) . ? O5 C40 1.447(7) . ? O6 C27 1.392(6) . ? O6 C42 1.422(7) . ? C1 C6 1.378(8) . ? C1 C2 1.411(8) . ? C2 C3 1.395(8) . ? C2 C28 1.507(8) . ? C3 C4 1.385(8) . ? C3 H3 0.9300 . ? C4 C5 1.378(9) . ? C4 H4 0.9300 . ? C5 C6 1.395(8) . ? C5 H5 0.9300 . ? C6 C7 1.524(8) . ? C7 C8 1.512(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.386(8) . ? C8 C13 1.413(7) . ? C9 C10 1.374(8) . ? C9 H9 0.9300 . ? C10 C11 1.389(8) . ? C10 H10 0.9300 . ? C11 C12 1.375(8) . ? C11 H11 0.9300 . ? C12 C13 1.397(8) . ? C12 C14 1.528(8) . ? C14 C15 1.525(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.380(7) . ? C15 C20 1.395(7) . ? C16 C17 1.372(8) . ? C16 H16 0.9300 . ? C17 C18 1.388(7) . ? C17 H17 0.9300 . ? C18 C19 1.382(7) . ? C18 H18 0.9300 . ? C19 C20 1.402(8) . ? C19 C21 1.527(8) . ? C21 C22 1.510(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.390(8) . ? C22 C23 1.399(8) . ? C23 C24 1.376(8) . ? C23 H23 0.9300 . ? C24 C25 1.380(8) . ? C24 H24 0.9300 . ? C25 C26 1.383(8) . ? C25 H25 0.9300 . ? C26 C27 1.386(8) . ? C26 C28 1.527(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.461(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.467(10) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.489(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.517(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.496(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.523(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.488(7) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.501(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.389(8) . ? C43 C48 1.393(8) . ? C44 C45 1.391(9) . ? C44 H44 0.9300 . ? C45 C46 1.385(8) . ? C45 H45 0.9300 . ? C46 C47 1.386(8) . ? C46 C49 1.514(9) . ? C47 C48 1.386(8) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? S2 O16 1.431(5) . ? S2 O15 1.433(5) . ? S2 N2 1.615(5) . ? S2 C92 1.761(7) . ? O9 C50 1.383(6) . ? O9 C78 1.421(7) . ? O10 C69 1.388(6) . ? O10 C81 1.425(7) . ? O11 C84 1.376(7) . ? O11 C76 1.390(7) . ? O12 C85 1.410(6) . ? O12 C86 1.421(7) . ? O13 C90 1.339(9) . ? O13 C89 1.437(7) . ? O14 C62 1.388(6) . ? O14 C91 1.434(7) . ? N2 C87 1.471(8) . ? N2 C88 1.488(8) . ? C50 C55 1.383(8) . ? C50 C51 1.384(8) . ? C51 C52 1.386(8) . ? C51 C77 1.509(8) . ? C52 C53 1.377(8) . ? C52 H52 0.9300 . ? C53 C54 1.375(8) . ? C53 H53 0.9300 . ? C54 C55 1.397(8) . ? C54 H54 0.9300 . ? C55 C56 1.539(8) . ? C56 C57 1.499(8) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C62 1.391(8) . ? C57 C58 1.392(8) . ? C58 C59 1.378(8) . ? C58 H58 0.9300 . ? C59 C60 1.387(8) . ? C59 H59 0.9300 . ? C60 C61 1.392(8) . ? C60 H60 0.9300 . ? C61 C62 1.390(8) . ? C61 C63 1.511(8) . ? C63 C64 1.534(8) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C69 1.373(8) . ? C64 C65 1.399(8) . ? C65 C66 1.381(8) . ? C65 H65 0.9300 . ? C66 C67 1.390(9) . ? C66 H66 0.9300 . ? C67 C68 1.379(8) . ? C67 H67 0.9300 . ? C68 C69 1.398(8) . ? C68 C70 1.506(8) . ? C70 C71 1.535(8) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C76 1.386(8) . ? C71 C72 1.398(8) . ? C72 C73 1.381(8) . ? C72 H72 0.9300 . ? C73 C74 1.381(9) . ? C73 H73 0.9300 . ? C74 C75 1.398(8) . ? C74 H74 0.9300 . ? C75 C76 1.376(8) . ? C75 C77 1.525(8) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.459(10) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 C80 1.411(11) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 C82 1.504(8) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C83 1.527(9) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 C85 1.520(9) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 C87 1.508(9) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 C89 1.554(10) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C91 1.508(9) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 C93 1.387(9) . ? C92 C97 1.394(9) . ? C93 C94 1.379(8) . ? C93 H93 0.9300 . ? C94 C95 1.393(8) . ? C94 H94 0.9300 . ? C95 C96 1.391(8) . ? C95 C98 1.501(8) . ? C96 C97 1.378(8) . ? C96 H96 0.9300 . ? C97 H97 0.9300 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 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 O8 S1 O7 118.9(3) . . ? O8 S1 N1 107.2(2) . . ? O7 S1 N1 109.3(3) . . ? O8 S1 C43 108.2(3) . . ? O7 S1 C43 105.9(3) . . ? N1 S1 C43 106.7(2) . . ? C39 N1 C38 119.5(5) . . ? C39 N1 S1 122.9(4) . . ? C38 N1 S1 117.6(4) . . ? C1 O1 C29 114.5(4) . . ? C20 O2 C32 114.1(4) . . ? C13 O3 C35 118.9(4) . . ? C36 O4 C37 113.4(4) . . ? C41 O5 C40 114.5(4) . . ? C27 O6 C42 115.7(4) . . ? C6 C1 O1 117.8(5) . . ? C6 C1 C2 122.3(5) . . ? O1 C1 C2 119.9(5) . . ? C3 C2 C1 117.0(5) . . ? C3 C2 C28 119.9(5) . . ? C1 C2 C28 123.0(5) . . ? C4 C3 C2 121.7(6) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.4(6) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 118.2(6) . . ? C1 C6 C7 121.7(5) . . ? C5 C6 C7 120.1(5) . . ? C8 C7 C6 117.3(5) . . ? C8 C7 H7A 108.0 . . ? C6 C7 H7A 108.0 . . ? C8 C7 H7B 108.0 . . ? C6 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C9 C8 C13 117.7(5) . . ? C9 C8 C7 120.0(5) . . ? C13 C8 C7 122.1(5) . . ? C10 C9 C8 122.0(6) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 118.7(6) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 122.3(6) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C13 117.9(5) . . ? C11 C12 C14 118.6(5) . . ? C13 C12 C14 123.4(5) . . ? O3 C13 C12 123.0(5) . . ? O3 C13 C8 115.7(5) . . ? C12 C13 C8 121.3(5) . . ? C15 C14 C12 117.7(5) . . ? C15 C14 H14A 107.9 . . ? C12 C14 H14A 107.9 . . ? C15 C14 H14B 107.9 . . ? C12 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C16 C15 C20 117.4(5) . . ? C16 C15 C14 120.8(5) . . ? C20 C15 C14 121.7(5) . . ? C17 C16 C15 122.6(5) . . ? C17 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C16 C17 C18 119.0(5) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 120.8(5) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 118.7(5) . . ? C18 C19 C21 119.9(5) . . ? C20 C19 C21 121.2(5) . . ? O2 C20 C15 120.3(5) . . ? O2 C20 C19 118.4(5) . . ? C15 C20 C19 121.2(5) . . ? C22 C21 C19 117.8(5) . . ? C22 C21 H21A 107.9 . . ? C19 C21 H21A 107.9 . . ? C22 C21 H21B 107.9 . . ? C19 C21 H21B 107.9 . . ? H21A C21 H21B 107.2 . . ? C27 C22 C23 117.2(5) . . ? C27 C22 C21 123.4(5) . . ? C23 C22 C21 119.3(5) . . ? C24 C23 C22 121.9(6) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 118.9(5) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C24 C25 C26 121.2(5) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C27 118.7(5) . . ? C25 C26 C28 120.3(5) . . ? C27 C26 C28 121.0(5) . . ? C26 C27 C22 121.8(5) . . ? C26 C27 O6 118.3(5) . . ? C22 C27 O6 119.8(5) . . ? C2 C28 C26 116.5(5) . . ? C2 C28 H28A 108.2 . . ? C26 C28 H28A 108.2 . . ? C2 C28 H28B 108.2 . . ? C26 C28 H28B 108.2 . . ? H28A C28 H28B 107.3 . . ? O1 C29 C30 111.5(5) . . ? O1 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? O1 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C31 119.5(6) . . ? C29 C30 H30A 107.4 . . ? C31 C30 H30A 107.4 . . ? C29 C30 H30B 107.4 . . ? C31 C30 H30B 107.4 . . ? H30A C30 H30B 107.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O2 C32 C33 108.5(5) . . ? O2 C32 H32A 110.0 . . ? C33 C32 H32A 110.0 . . ? O2 C32 H32B 110.0 . . ? C33 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? C32 C33 C34 111.6(5) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 C36 107.3(5) . . ? O3 C35 H35A 110.3 . . ? C36 C35 H35A 110.3 . . ? O3 C35 H35B 110.3 . . ? C36 C35 H35B 110.3 . . ? H35A C35 H35B 108.5 . . ? O4 C36 C35 107.1(4) . . ? O4 C36 H36A 110.3 . . ? C35 C36 H36A 110.3 . . ? O4 C36 H36B 110.3 . . ? C35 C36 H36B 110.3 . . ? H36A C36 H36B 108.6 . . ? O4 C37 C38 115.0(4) . . ? O4 C37 H37A 108.5 . . ? C38 C37 H37A 108.5 . . ? O4 C37 H37B 108.5 . . ? C38 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? N1 C38 C37 114.6(5) . . ? N1 C38 H38A 108.6 . . ? C37 C38 H38A 108.6 . . ? N1 C38 H38B 108.6 . . ? C37 C38 H38B 108.6 . . ? H38A C38 H38B 107.6 . . ? N1 C39 C40 117.9(5) . . ? N1 C39 H39A 107.8 . . ? C40 C39 H39A 107.8 . . ? N1 C39 H39B 107.8 . . ? C40 C39 H39B 107.8 . . ? H39A C39 H39B 107.2 . . ? O5 C40 C39 107.8(5) . . ? O5 C40 H40A 110.1 . . ? C39 C40 H40A 110.1 . . ? O5 C40 H40B 110.1 . . ? C39 C40 H40B 110.1 . . ? H40A C40 H40B 108.5 . . ? O5 C41 C42 115.4(5) . . ? O5 C41 H41A 108.4 . . ? C42 C41 H41A 108.4 . . ? O5 C41 H41B 108.4 . . ? C42 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? O6 C42 C41 110.6(5) . . ? O6 C42 H42A 109.5 . . ? C41 C42 H42A 109.5 . . ? O6 C42 H42B 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? C44 C43 C48 120.6(6) . . ? C44 C43 S1 120.0(4) . . ? C48 C43 S1 119.4(4) . . ? C43 C44 C45 119.2(6) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C46 C45 C44 120.8(5) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 119.2(6) . . ? C45 C46 C49 120.3(6) . . ? C47 C46 C49 120.5(5) . . ? C48 C47 C46 121.1(5) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C47 C48 C43 119.1(5) . . ? C47 C48 H48 120.5 . . ? C43 C48 H48 120.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O16 S2 O15 120.8(3) . . ? O16 S2 N2 106.9(3) . . ? O15 S2 N2 106.2(3) . . ? O16 S2 C92 107.3(3) . . ? O15 S2 C92 107.4(3) . . ? N2 S2 C92 107.7(3) . . ? C50 O9 C78 114.8(4) . . ? C69 O10 C81 113.0(4) . . ? C84 O11 C76 118.6(5) . . ? C85 O12 C86 117.3(5) . . ? C90 O13 C89 111.4(6) . . ? C62 O14 C91 111.7(4) . . ? C87 N2 C88 115.5(5) . . ? C87 N2 S2 118.6(4) . . ? C88 N2 S2 122.0(4) . . ? C55 C50 O9 120.0(5) . . ? C55 C50 C51 121.9(5) . . ? O9 C50 C51 117.9(5) . . ? C50 C51 C52 118.1(5) . . ? C50 C51 C77 121.2(5) . . ? C52 C51 C77 120.6(5) . . ? C53 C52 C51 121.2(5) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C54 C53 C52 119.4(5) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 121.0(6) . . ? C53 C54 H54 119.5 . . ? C55 C54 H54 119.5 . . ? C50 C55 C54 118.0(5) . . ? C50 C55 C56 122.0(5) . . ? C54 C55 C56 120.0(5) . . ? C57 C56 C55 116.7(5) . . ? C57 C56 H56A 108.1 . . ? C55 C56 H56A 108.1 . . ? C57 C56 H56B 108.1 . . ? C55 C56 H56B 108.1 . . ? H56A C56 H56B 107.3 . . ? C62 C57 C58 117.9(6) . . ? C62 C57 C56 121.2(5) . . ? C58 C57 C56 120.8(5) . . ? C59 C58 C57 121.1(6) . . ? C59 C58 H58 119.4 . . ? C57 C58 H58 119.4 . . ? C58 C59 C60 119.6(5) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.2 . . ? C59 C60 C61 121.2(6) . . ? C59 C60 H60 119.4 . . ? C61 C60 H60 119.4 . . ? C62 C61 C60 117.6(5) . . ? C62 C61 C63 122.1(5) . . ? C60 C61 C63 120.3(5) . . ? O14 C62 C61 118.8(5) . . ? O14 C62 C57 118.8(5) . . ? C61 C62 C57 122.3(5) . . ? C61 C63 C64 115.4(5) . . ? C61 C63 H63A 108.4 . . ? C64 C63 H63A 108.4 . . ? C61 C63 H63B 108.4 . . ? C64 C63 H63B 108.4 . . ? H63A C63 H63B 107.5 . . ? C69 C64 C65 119.1(5) . . ? C69 C64 C63 121.4(5) . . ? C65 C64 C63 119.4(6) . . ? C66 C65 C64 120.1(6) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C67 119.8(6) . . ? C65 C66 H66 120.1 . . ? C67 C66 H66 120.1 . . ? C68 C67 C66 121.0(6) . . ? C68 C67 H67 119.5 . . ? C66 C67 H67 119.5 . . ? C67 C68 C69 118.3(6) . . ? C67 C68 C70 120.4(5) . . ? C69 C68 C70 121.3(5) . . ? C64 C69 O10 119.9(5) . . ? C64 C69 C68 121.6(5) . . ? O10 C69 C68 118.4(5) . . ? C68 C70 C71 119.3(5) . . ? C68 C70 H70A 107.5 . . ? C71 C70 H70A 107.5 . . ? C68 C70 H70B 107.5 . . ? C71 C70 H70B 107.5 . . ? H70A C70 H70B 107.0 . . ? C76 C71 C72 117.5(5) . . ? C76 C71 C70 123.8(5) . . ? C72 C71 C70 118.6(5) . . ? C73 C72 C71 121.1(6) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C74 C73 C72 119.3(6) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C73 C74 C75 121.6(6) . . ? C73 C74 H74 119.2 . . ? C75 C74 H74 119.2 . . ? C76 C75 C74 117.2(5) . . ? C76 C75 C77 124.6(5) . . ? C74 C75 C77 117.9(5) . . ? C75 C76 C71 123.3(5) . . ? C75 C76 O11 118.1(5) . . ? C71 C76 O11 118.2(5) . . ? C51 C77 C75 116.8(5) . . ? C51 C77 H77A 108.1 . . ? C75 C77 H77A 108.1 . . ? C51 C77 H77B 108.1 . . ? C75 C77 H77B 108.1 . . ? H77A C77 H77B 107.3 . . ? O9 C78 C79 111.9(6) . . ? O9 C78 H78A 109.2 . . ? C79 C78 H78A 109.2 . . ? O9 C78 H78B 109.2 . . ? C79 C78 H78B 109.2 . . ? H78A C78 H78B 107.9 . . ? C80 C79 C78 122.2(7) . . ? C80 C79 H79A 106.8 . . ? C78 C79 H79A 106.8 . . ? C80 C79 H79B 106.8 . . ? C78 C79 H79B 106.8 . . ? H79A C79 H79B 106.6 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O10 C81 C82 109.2(5) . . ? O10 C81 H81A 109.8 . . ? C82 C81 H81A 109.8 . . ? O10 C81 H81B 109.8 . . ? C82 C81 H81B 109.8 . . ? H81A C81 H81B 108.3 . . ? C81 C82 C83 111.3(5) . . ? C81 C82 H82A 109.4 . . ? C83 C82 H82A 109.4 . . ? C81 C82 H82B 109.4 . . ? C83 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? O11 C84 C85 106.1(5) . . ? O11 C84 H84A 110.5 . . ? C85 C84 H84A 110.5 . . ? O11 C84 H84B 110.5 . . ? C85 C84 H84B 110.5 . . ? H84A C84 H84B 108.7 . . ? O12 C85 C84 112.2(5) . . ? O12 C85 H85A 109.2 . . ? C84 C85 H85A 109.2 . . ? O12 C85 H85B 109.2 . . ? C84 C85 H85B 109.2 . . ? H85A C85 H85B 107.9 . . ? O12 C86 C87 113.8(5) . . ? O12 C86 H86A 108.8 . . ? C87 C86 H86A 108.8 . . ? O12 C86 H86B 108.8 . . ? C87 C86 H86B 108.8 . . ? H86A C86 H86B 107.7 . . ? N2 C87 C86 113.7(5) . . ? N2 C87 H87A 108.8 . . ? C86 C87 H87A 108.8 . . ? N2 C87 H87B 108.8 . . ? C86 C87 H87B 108.8 . . ? H87A C87 H87B 107.7 . . ? N2 C88 C89 115.5(6) . . ? N2 C88 H88A 108.4 . . ? C89 C88 H88A 108.4 . . ? N2 C88 H88B 108.4 . . ? C89 C88 H88B 108.4 . . ? H88A C88 H88B 107.5 . . ? O13 C89 C88 115.4(6) . . ? O13 C89 H89A 108.4 . . ? C88 C89 H89A 108.4 . . ? O13 C89 H89B 108.4 . . ? C88 C89 H89B 108.4 . . ? H89A C89 H89B 107.5 . . ? O13 C90 C91 112.0(6) . . ? O13 C90 H90A 109.2 . . ? C91 C90 H90A 109.2 . . ? O13 C90 H90B 109.2 . . ? C91 C90 H90B 109.2 . . ? H90A C90 H90B 107.9 . . ? O14 C91 C90 108.6(5) . . ? O14 C91 H91A 110.0 . . ? C90 C91 H91A 110.0 . . ? O14 C91 H91B 110.0 . . ? C90 C91 H91B 110.0 . . ? H91A C91 H91B 108.4 . . ? C93 C92 C97 119.7(6) . . ? C93 C92 S2 120.1(5) . . ? C97 C92 S2 120.2(5) . . ? C94 C93 C92 120.5(6) . . ? C94 C93 H93 119.8 . . ? C92 C93 H93 119.8 . . ? C93 C94 C95 120.8(6) . . ? C93 C94 H94 119.6 . . ? C95 C94 H94 119.6 . . ? C96 C95 C94 117.7(6) . . ? C96 C95 C98 121.5(5) . . ? C94 C95 C98 120.8(5) . . ? C97 C96 C95 122.3(6) . . ? C97 C96 H96 118.8 . . ? C95 C96 H96 118.8 . . ? C96 C97 C92 118.8(6) . . ? C96 C97 H97 120.6 . . ? C92 C97 H97 120.6 . . ? C95 C98 H98A 109.5 . . ? C95 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C95 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.994 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.065 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 749550' #TrackingRef '- CIF (revised_ID NJ-ART-10-2009-000587).txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H65 N O10 S' _chemical_formula_weight 908.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7394(11) _cell_length_b 17.0425(13) _cell_length_c 20.6798(16) _cell_angle_alpha 74.873(3) _cell_angle_beta 82.029(2) _cell_angle_gamma 75.019(2) _cell_volume 4830.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCKS _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.9326 _exptl_absorpt_correction_T_max 0.9655 _exptl_special_details ; ? ; _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 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41560 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 28.28 _reflns_number_total 21770 _reflns_number_gt 16706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.1226P)^2^+0.9870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21770 _refine_ls_number_parameters 1177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S2 S 0.37664(3) 0.59374(3) 0.31984(2) 0.02151(12) Uani 1 d . . . S1 S 0.12954(3) -0.08331(3) 0.19071(3) 0.02428(12) Uani 1 d . . . O1 O 0.75293(9) 0.09464(8) 0.08460(6) 0.0202(3) Uani 1 d . . . O2 O 0.55255(9) 0.15570(8) 0.35264(7) 0.0249(3) Uani 1 d . . . O3 O 0.43047(9) 0.25412(7) 0.12478(7) 0.0207(3) Uani 1 d . . . O4 O 0.32326(9) 0.29830(8) 0.00141(7) 0.0237(3) Uani 1 d . . . O5 O 0.21319(9) 0.16991(8) 0.04518(6) 0.0215(3) Uani 1 d . . . O6 O 0.43718(9) -0.19265(9) 0.16662(7) 0.0273(3) Uani 1 d . . . O7 O 0.62053(9) -0.24900(8) 0.21031(7) 0.0218(3) Uani 1 d . . . O8 O 0.60837(9) -0.09974(7) 0.26226(6) 0.0186(3) Uani 1 d . . . O9 O 0.04325(10) -0.03433(10) 0.16317(8) 0.0385(4) Uani 1 d . . . O10 O 0.16025(10) -0.16961(9) 0.18904(7) 0.0288(3) Uani 1 d . . . O11 O -0.24494(9) 0.39955(8) 0.40573(6) 0.0203(3) Uani 1 d . . . O12 O -0.02829(10) 0.36368(8) 0.13653(7) 0.0267(3) Uani 1 d . . . O13 O 0.08337(9) 0.25287(7) 0.36655(6) 0.0193(3) Uani 1 d . . . O14 O 0.18653(9) 0.20261(8) 0.49215(7) 0.0224(3) Uani 1 d . . . O15 O 0.29501(9) 0.33314(8) 0.45936(6) 0.0205(3) Uani 1 d . . . O16 O 0.06652(9) 0.69146(9) 0.34317(7) 0.0260(3) Uani 1 d . . . O17 O -0.11627(9) 0.75276(8) 0.29753(7) 0.0217(3) Uani 1 d . . . O18 O -0.10425(9) 0.60782(7) 0.23911(6) 0.0187(3) Uani 1 d . . . O19 O 0.46498(9) 0.54802(9) 0.34638(7) 0.0291(3) Uani 1 d . . . O20 O 0.34144(9) 0.67981(8) 0.32172(7) 0.0263(3) Uani 1 d . . . N1 N 0.21337(11) -0.03845(10) 0.15034(8) 0.0250(4) Uani 1 d . . . N2 N 0.29623(11) 0.54478(9) 0.36142(8) 0.0210(3) Uani 1 d . . . C1 C 0.66998(13) 0.07090(11) 0.08308(9) 0.0177(4) Uani 1 d . . . C2 C 0.66490(13) -0.01195(11) 0.11198(9) 0.0178(4) Uani 1 d . . . C3 C 0.58180(13) -0.03475(11) 0.10859(9) 0.0195(4) Uani 1 d . . . H3 H 0.5769 -0.0896 0.1271 0.023 Uiso 1 calc R . . C4 C 0.50643(13) 0.02351(11) 0.07793(9) 0.0195(4) Uani 1 d . . . H4 H 0.4528 0.0068 0.0735 0.023 Uiso 1 calc R . . C5 C 0.51056(13) 0.10668(11) 0.05383(9) 0.0190(4) Uani 1 d . . . H5 H 0.4583 0.1459 0.0357 0.023 Uiso 1 calc R . . C6 C 0.59205(13) 0.13161(11) 0.05662(9) 0.0181(4) Uani 1 d . . . C7 C 0.59434(13) 0.22347(11) 0.03705(9) 0.0207(4) Uani 1 d . . . H7A H 0.6506 0.2309 0.0079 0.025 Uiso 1 calc R . . H7B H 0.5399 0.2558 0.0126 0.025 Uiso 1 calc R . . C8 C 0.59392(13) 0.25424(10) 0.09949(9) 0.0197(4) Uani 1 d . . . C9 C 0.67528(14) 0.26858(11) 0.11720(10) 0.0231(4) Uani 1 d . . . H9 H 0.7296 0.2638 0.0882 0.028 Uiso 1 calc R . . C10 C 0.67625(14) 0.28982(11) 0.17728(10) 0.0251(4) Uani 1 d . . . H10 H 0.7301 0.3016 0.1875 0.030 Uiso 1 calc R . . C11 C 0.59746(14) 0.29352(11) 0.22196(10) 0.0240(4) Uani 1 d . . . H11 H 0.5995 0.3054 0.2631 0.029 Uiso 1 calc R . . C12 C 0.51458(13) 0.27966(11) 0.20624(10) 0.0216(4) Uani 1 d . . . C13 C 0.51356(13) 0.26359(10) 0.14356(9) 0.0191(4) Uani 1 d . . . C14 C 0.43039(14) 0.27571(12) 0.25730(10) 0.0253(4) Uani 1 d . . . H14A H 0.3733 0.3089 0.2364 0.030 Uiso 1 calc R . . H14B H 0.4376 0.2987 0.2941 0.030 Uiso 1 calc R . . C15 C 0.42269(13) 0.18545(12) 0.28411(9) 0.0225(4) Uani 1 d . . . C16 C 0.35629(13) 0.15564(12) 0.26160(10) 0.0249(4) Uani 1 d . . . H16 H 0.3114 0.1929 0.2340 0.030 Uiso 1 calc R . . C17 C 0.35578(14) 0.07156(13) 0.27950(10) 0.0259(4) Uani 1 d . . . H17 H 0.3085 0.0532 0.2665 0.031 Uiso 1 calc R . . C18 C 0.42641(14) 0.01484(13) 0.31695(10) 0.0258(4) Uani 1 d . . . H18 H 0.4281 -0.0419 0.3267 0.031 Uiso 1 calc R . . C19 C 0.49478(13) 0.04173(12) 0.34022(9) 0.0230(4) Uani 1 d . . . C20 C 0.48798(13) 0.12805(12) 0.32656(9) 0.0213(4) Uani 1 d . . . C21 C 0.57879(13) -0.02040(12) 0.37332(9) 0.0241(4) Uani 1 d . . . H21A H 0.5657 -0.0755 0.3877 0.029 Uiso 1 calc R . . H21B H 0.5900 -0.0044 0.4127 0.029 Uiso 1 calc R . . C22 C 0.66579(13) -0.02282(11) 0.32431(9) 0.0207(4) Uani 1 d . . . C23 C 0.73584(14) 0.01573(12) 0.33019(10) 0.0251(4) Uani 1 d . . . H23 H 0.7325 0.0382 0.3671 0.030 Uiso 1 calc R . . C24 C 0.81004(13) 0.02108(12) 0.28195(10) 0.0248(4) Uani 1 d . . . H24 H 0.8576 0.0449 0.2876 0.030 Uiso 1 calc R . . C25 C 0.81426(13) -0.00870(11) 0.22508(10) 0.0224(4) Uani 1 d . . . H25 H 0.8632 -0.0026 0.1920 0.027 Uiso 1 calc R . . C26 C 0.74571(13) -0.04766(10) 0.21720(9) 0.0185(4) Uani 1 d . . . C27 C 0.67424(12) -0.05739(10) 0.26860(9) 0.0179(4) Uani 1 d . . . C28 C 0.74376(13) -0.07280(11) 0.15219(9) 0.0204(4) Uani 1 d . . . H28A H 0.7338 -0.1289 0.1622 0.024 Uiso 1 calc R . . H28B H 0.8037 -0.0725 0.1260 0.024 Uiso 1 calc R . . C29 C 0.81517(14) 0.08955(13) 0.02523(10) 0.0271(4) Uani 1 d . . . H29A H 0.7835 0.1239 -0.0142 0.033 Uiso 1 calc R . . H29B H 0.8343 0.0323 0.0206 0.033 Uiso 1 calc R . . C30 C 0.90000(14) 0.11995(14) 0.03150(11) 0.0319(5) Uani 1 d . . . H30A H 0.9343 0.0820 0.0685 0.038 Uiso 1 calc R . . H30B H 0.8793 0.1745 0.0418 0.038 Uiso 1 calc R . . C31 C 0.96588(16) 0.12615(17) -0.03270(13) 0.0424(6) Uani 1 d . . . H31A H 0.9874 0.0721 -0.0427 0.064 Uiso 1 calc R . . H31B H 1.0189 0.1455 -0.0264 0.064 Uiso 1 calc R . . H31C H 0.9326 0.1647 -0.0693 0.064 Uiso 1 calc R . . C32 C 0.51199(16) 0.20187(14) 0.40418(11) 0.0331(5) Uani 1 d . . . H32A H 0.4460 0.2271 0.3973 0.040 Uiso 1 calc R . . H32B H 0.5437 0.2465 0.3995 0.040 Uiso 1 calc R . . C33 C 0.52024(16) 0.14772(15) 0.47333(11) 0.0357(5) Uani 1 d . . . H33A H 0.4924 0.1010 0.4767 0.043 Uiso 1 calc R . . H33B H 0.4842 0.1795 0.5049 0.043 Uiso 1 calc R . . C34 C 0.62084(17) 0.11396(17) 0.49372(12) 0.0416(6) Uani 1 d . . . H34A H 0.6573 0.0826 0.4627 0.062 Uiso 1 calc R . . H34B H 0.6208 0.0783 0.5381 0.062 Uiso 1 calc R . . H34C H 0.6479 0.1597 0.4932 0.062 Uiso 1 calc R . . C35 C 0.37358(14) 0.33360(11) 0.09268(11) 0.0259(4) Uani 1 d . . . H35A H 0.4113 0.3629 0.0570 0.031 Uiso 1 calc R . . H35B H 0.3502 0.3677 0.1251 0.031 Uiso 1 calc R . . C36 C 0.29219(14) 0.31953(12) 0.06418(10) 0.0252(4) Uani 1 d . . . H36A H 0.2680 0.2747 0.0950 0.030 Uiso 1 calc R . . H36B H 0.2419 0.3698 0.0581 0.030 Uiso 1 calc R . . C37 C 0.24937(13) 0.29084(12) -0.03267(9) 0.0222(4) Uani 1 d . . . H37A H 0.2593 0.3151 -0.0803 0.027 Uiso 1 calc R . . H37B H 0.1898 0.3223 -0.0163 0.027 Uiso 1 calc R . . C38 C 0.24400(14) 0.20153(11) -0.02291(9) 0.0218(4) Uani 1 d . . . H38A H 0.2003 0.1984 -0.0526 0.026 Uiso 1 calc R . . H38B H 0.3055 0.1681 -0.0338 0.026 Uiso 1 calc R . . C39 C 0.22146(13) 0.08282(11) 0.05906(9) 0.0206(4) Uani 1 d . . . H39A H 0.2861 0.0546 0.0494 0.025 Uiso 1 calc R . . H39B H 0.1818 0.0704 0.0312 0.025 Uiso 1 calc R . . C40 C 0.19170(17) 0.05320(12) 0.13175(11) 0.0334(5) Uani 1 d . . . H40A H 0.2246 0.0735 0.1592 0.040 Uiso 1 calc R . . H40B H 0.1246 0.0751 0.1398 0.040 Uiso 1 calc R . . C41 C 0.30889(13) -0.08177(12) 0.17055(10) 0.0240(4) Uani 1 d . . . H41A H 0.3044 -0.1127 0.2170 0.029 Uiso 1 calc R . . H41B H 0.3445 -0.0403 0.1680 0.029 Uiso 1 calc R . . C42 C 0.36253(12) -0.14179(11) 0.12781(9) 0.0205(4) Uani 1 d . . . H42A H 0.3226 -0.1750 0.1198 0.025 Uiso 1 calc R . . H42B H 0.3864 -0.1118 0.0849 0.025 Uiso 1 calc R . . C43 C 0.50788(13) -0.24508(12) 0.13318(10) 0.0229(4) Uani 1 d . . . H43A H 0.5399 -0.2118 0.0962 0.028 Uiso 1 calc R . . H43B H 0.4802 -0.2802 0.1154 0.028 Uiso 1 calc R . . C44 C 0.57625(13) -0.29811(11) 0.18408(10) 0.0228(4) Uani 1 d . . . H44A H 0.5431 -0.3308 0.2207 0.027 Uiso 1 calc R . . H44B H 0.6242 -0.3367 0.1632 0.027 Uiso 1 calc R . . C45 C 0.57639(13) -0.23387(11) 0.27347(10) 0.0223(4) Uani 1 d . . . H45A H 0.5755 -0.2866 0.3056 0.027 Uiso 1 calc R . . H45B H 0.5118 -0.2023 0.2680 0.027 Uiso 1 calc R . . C46 C 0.62994(13) -0.18582(11) 0.29890(10) 0.0214(4) Uani 1 d . . . H46A H 0.6128 -0.1894 0.3464 0.026 Uiso 1 calc R . . H46B H 0.6970 -0.2095 0.2931 0.026 Uiso 1 calc R . . C47 C 0.12465(13) -0.07619(12) 0.27464(10) 0.0228(4) Uani 1 d . . . C48 C 0.18124(14) -0.13877(12) 0.31994(10) 0.0274(4) Uani 1 d . . . H48 H 0.2182 -0.1862 0.3071 0.033 Uiso 1 calc R . . C49 C 0.18159(15) -0.12925(13) 0.38402(11) 0.0301(5) Uani 1 d . . . H49 H 0.2200 -0.1705 0.4141 0.036 Uiso 1 calc R . . C50 C 0.12557(15) -0.05910(13) 0.40512(11) 0.0292(4) Uani 1 d . . . C51 C 0.06835(14) 0.00168(12) 0.35931(10) 0.0270(4) Uani 1 d . . . H51 H 0.0297 0.0482 0.3725 0.032 Uiso 1 calc R . . C52 C 0.06822(13) -0.00617(12) 0.29428(10) 0.0256(4) Uani 1 d . . . H52 H 0.0305 0.0353 0.2639 0.031 Uiso 1 calc R . . C53 C 0.12723(18) -0.05006(16) 0.47529(12) 0.0422(6) Uani 1 d . . . H53A H 0.0786 -0.0030 0.4830 0.063 Uiso 1 calc R . . H53B H 0.1874 -0.0416 0.4807 0.063 Uiso 1 calc R . . H53C H 0.1168 -0.0998 0.5070 0.063 Uiso 1 calc R . . C54 C -0.16493(12) 0.42604(11) 0.41033(9) 0.0174(4) Uani 1 d . . . C55 C -0.16389(13) 0.51027(11) 0.38495(9) 0.0178(4) Uani 1 d . . . C56 C -0.08356(13) 0.53556(11) 0.39163(9) 0.0191(4) Uani 1 d . . . H56 H -0.0814 0.5914 0.3757 0.023 Uiso 1 calc R . . C57 C -0.00708(13) 0.47845(11) 0.42170(9) 0.0191(4) Uani 1 d . . . H57 H 0.0444 0.4966 0.4283 0.023 Uiso 1 calc R . . C58 C -0.00704(13) 0.39399(11) 0.44198(9) 0.0190(4) Uani 1 d . . . H58 H 0.0462 0.3556 0.4595 0.023 Uiso 1 calc R . . C59 C -0.08584(13) 0.36648(11) 0.43630(9) 0.0179(4) Uani 1 d . . . C60 C -0.08327(13) 0.27370(11) 0.45258(9) 0.0202(4) Uani 1 d . . . H60A H -0.0287 0.2423 0.4772 0.024 Uiso 1 calc R . . H60B H -0.1393 0.2630 0.4806 0.024 Uiso 1 calc R . . C61 C -0.07848(13) 0.24577(10) 0.38802(9) 0.0200(4) Uani 1 d . . . C62 C -0.15631(14) 0.22966(11) 0.36706(10) 0.0229(4) Uani 1 d . . . H62 H -0.2112 0.2302 0.3954 0.028 Uiso 1 calc R . . C63 C -0.15337(14) 0.21279(11) 0.30473(10) 0.0252(4) Uani 1 d . . . H63 H -0.2048 0.1995 0.2923 0.030 Uiso 1 calc R . . C64 C -0.07334(14) 0.21577(11) 0.26076(10) 0.0244(4) Uani 1 d . . . H64 H -0.0729 0.2073 0.2181 0.029 Uiso 1 calc R . . C65 C 0.00599(13) 0.23116(11) 0.27961(9) 0.0209(4) Uani 1 d . . . C66 C 0.00326(13) 0.24232(10) 0.34467(9) 0.0190(4) Uani 1 d . . . C67 C 0.09073(14) 0.24250(11) 0.22997(10) 0.0242(4) Uani 1 d . . . H67A H 0.0859 0.2238 0.1904 0.029 Uiso 1 calc R . . H67B H 0.1480 0.2088 0.2503 0.029 Uiso 1 calc R . . C68 C 0.09508(13) 0.33415(12) 0.20984(9) 0.0214(4) Uani 1 d . . . C69 C 0.15839(13) 0.36355(12) 0.23575(10) 0.0239(4) Uani 1 d . . . H69 H 0.2029 0.3260 0.2635 0.029 Uiso 1 calc R . . C70 C 0.15605(14) 0.44817(13) 0.22074(10) 0.0260(4) Uani 1 d . . . H70 H 0.2015 0.4667 0.2359 0.031 Uiso 1 calc R . . C71 C 0.08601(14) 0.50526(12) 0.18314(10) 0.0253(4) Uani 1 d . . . H71 H 0.0825 0.5622 0.1755 0.030 Uiso 1 calc R . . C72 C 0.02093(13) 0.47817(12) 0.15680(9) 0.0213(4) Uani 1 d . . . C73 C 0.02990(13) 0.39225(12) 0.16782(9) 0.0210(4) Uani 1 d . . . C74 C -0.06348(14) 0.53885(12) 0.12268(9) 0.0241(4) Uani 1 d . . . H74A H -0.0703 0.5245 0.0815 0.029 Uiso 1 calc R . . H74B H -0.0537 0.5951 0.1112 0.029 Uiso 1 calc R . . C75 C -0.15247(13) 0.53523(11) 0.16933(9) 0.0206(4) Uani 1 d . . . C76 C -0.21867(14) 0.49612(12) 0.15791(10) 0.0248(4) Uani 1 d . . . H76 H -0.2122 0.4778 0.1186 0.030 Uiso 1 calc R . . C77 C -0.29426(14) 0.48411(11) 0.20453(10) 0.0244(4) Uani 1 d . . . H77 H -0.3391 0.4594 0.1956 0.029 Uiso 1 calc R . . C78 C -0.30304(13) 0.50887(11) 0.26442(10) 0.0226(4) Uani 1 d . . . H78 H -0.3522 0.4984 0.2963 0.027 Uiso 1 calc R . . C79 C -0.23887(13) 0.54922(11) 0.27720(9) 0.0193(4) Uani 1 d . . . C80 C -0.16638(12) 0.56459(10) 0.22804(9) 0.0180(4) Uani 1 d . . . C81 C -0.24281(13) 0.57061(11) 0.34442(9) 0.0208(4) Uani 1 d . . . H81A H -0.3032 0.5668 0.3689 0.025 Uiso 1 calc R . . H81B H -0.2361 0.6274 0.3374 0.025 Uiso 1 calc R . . C82 C -0.31119(14) 0.40252(14) 0.46307(11) 0.0293(5) Uani 1 d . . . H82A H -0.3336 0.4596 0.4679 0.035 Uiso 1 calc R . . H82B H -0.2814 0.3688 0.5034 0.035 Uiso 1 calc R . . C83 C -0.39237(14) 0.36938(14) 0.45310(11) 0.0308(5) Uani 1 d . . . H83A H -0.3681 0.3141 0.4446 0.037 Uiso 1 calc R . . H83B H -0.4231 0.4053 0.4138 0.037 Uiso 1 calc R . . C84 C -0.46459(17) 0.36431(18) 0.51311(14) 0.0485(7) Uani 1 d . . . H84A H -0.4350 0.3276 0.5520 0.073 Uiso 1 calc R . . H84B H -0.5146 0.3431 0.5040 0.073 Uiso 1 calc R . . H84C H -0.4898 0.4190 0.5213 0.073 Uiso 1 calc R . . C85 C 0.02196(19) 0.34636(15) 0.07360(11) 0.0410(6) Uani 1 d . . . H85A H 0.0328 0.3980 0.0439 0.049 Uiso 1 calc R . . H85B H 0.0828 0.3086 0.0830 0.049 Uiso 1 calc R . . C86 C -0.0309(2) 0.30914(17) 0.04010(13) 0.0488(6) Uani 1 d . . . H86A H -0.0463 0.2604 0.0716 0.059 Uiso 1 calc R . . H86B H 0.0091 0.2903 0.0031 0.059 Uiso 1 calc R . . C87 C -0.12008(18) 0.36642(19) 0.01342(14) 0.0506(7) Uani 1 d . . . H87A H -0.1640 0.3791 0.0502 0.076 Uiso 1 calc R . . H87B H -0.1468 0.3397 -0.0123 0.076 Uiso 1 calc R . . H87C H -0.1066 0.4172 -0.0148 0.076 Uiso 1 calc R . . C88 C 0.14349(14) 0.17373(11) 0.39559(10) 0.0246(4) Uani 1 d . . . H88A H 0.1698 0.1435 0.3610 0.030 Uiso 1 calc R . . H88B H 0.1070 0.1404 0.4291 0.030 Uiso 1 calc R . . C89 C 0.22181(13) 0.18772(12) 0.42766(10) 0.0240(4) Uani 1 d . . . H89A H 0.2740 0.1390 0.4322 0.029 Uiso 1 calc R . . H89B H 0.2442 0.2354 0.3999 0.029 Uiso 1 calc R . . C90 C 0.25724(13) 0.20837(11) 0.53000(9) 0.0214(4) Uani 1 d . . . H90A H 0.3183 0.1792 0.5138 0.026 Uiso 1 calc R . . H90B H 0.2456 0.1811 0.5768 0.026 Uiso 1 calc R . . C91 C 0.25929(13) 0.29754(11) 0.52509(9) 0.0203(4) Uani 1 d . . . H91A H 0.1962 0.3294 0.5344 0.024 Uiso 1 calc R . . H91B H 0.2990 0.2995 0.5581 0.024 Uiso 1 calc R . . C92 C 0.28053(13) 0.42071(11) 0.44817(9) 0.0199(4) Uani 1 d . . . H92A H 0.3112 0.4344 0.4810 0.024 Uiso 1 calc R . . H92B H 0.2137 0.4462 0.4524 0.024 Uiso 1 calc R . . C93 C 0.32182(14) 0.45285(11) 0.37812(10) 0.0229(4) Uani 1 d . . . H93A H 0.3898 0.4331 0.3758 0.027 Uiso 1 calc R . . H93B H 0.2976 0.4322 0.3461 0.027 Uiso 1 calc R . . C94 C 0.19926(12) 0.58409(11) 0.34076(9) 0.0200(4) Uani 1 d . . . H94A H 0.1668 0.5404 0.3436 0.024 Uiso 1 calc R . . H94B H 0.2029 0.6147 0.2942 0.024 Uiso 1 calc R . . C95 C 0.14198(12) 0.64299(11) 0.38262(9) 0.0203(4) Uani 1 d . . . H95A H 0.1187 0.6122 0.4254 0.024 Uiso 1 calc R . . H95B H 0.1793 0.6782 0.3909 0.024 Uiso 1 calc R . . C96 C -0.00384(13) 0.74476(12) 0.37598(10) 0.0227(4) Uani 1 d . . . H96A H 0.0246 0.7786 0.3946 0.027 Uiso 1 calc R . . H96B H -0.0372 0.7119 0.4124 0.027 Uiso 1 calc R . . C97 C -0.07089(13) 0.79989(11) 0.32502(10) 0.0228(4) Uani 1 d . . . H97A H -0.1182 0.8386 0.3461 0.027 Uiso 1 calc R . . H97B H -0.0366 0.8323 0.2890 0.027 Uiso 1 calc R . . C98 C -0.07375(13) 0.74108(11) 0.23346(9) 0.0217(4) Uani 1 d . . . H98A H -0.0091 0.7093 0.2377 0.026 Uiso 1 calc R . . H98B H -0.0734 0.7949 0.2028 0.026 Uiso 1 calc R . . C99 C -0.12826(13) 0.69507(11) 0.20642(10) 0.0217(4) Uani 1 d . . . H99A H -0.1953 0.7174 0.2144 0.026 Uiso 1 calc R . . H99B H -0.1134 0.7023 0.1583 0.026 Uiso 1 calc R . . C100 C 0.38052(13) 0.58590(11) 0.23619(9) 0.0217(4) Uani 1 d . . . C101 C 0.32020(13) 0.64641(11) 0.19181(10) 0.0246(4) Uani 1 d . . . H101 H 0.2825 0.6934 0.2049 0.029 Uiso 1 calc R . . C102 C 0.31740(14) 0.63546(12) 0.12832(10) 0.0272(4) Uani 1 d . . . H102 H 0.2764 0.6751 0.0990 0.033 Uiso 1 calc R . . C103 C 0.37477(15) 0.56620(12) 0.10710(10) 0.0272(4) Uani 1 d . . . C104 C 0.43644(14) 0.50791(12) 0.15162(10) 0.0272(4) Uani 1 d . . . H104 H 0.4766 0.4624 0.1378 0.033 Uiso 1 calc R . . C105 C 0.43868(13) 0.51683(12) 0.21570(10) 0.0244(4) Uani 1 d . . . H105 H 0.4790 0.4768 0.2452 0.029 Uiso 1 calc R . . C106 C 0.37042(18) 0.55544(14) 0.03785(11) 0.0391(5) Uani 1 d . . . H10A H 0.3119 0.5419 0.0352 0.059 Uiso 1 calc R . . H10B H 0.4219 0.5111 0.0287 0.059 Uiso 1 calc R . . H10C H 0.3746 0.6065 0.0054 0.059 Uiso 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 S2 0.0155(2) 0.0192(2) 0.0267(3) -0.00185(18) 0.00025(18) -0.00323(18) S1 0.0164(2) 0.0232(2) 0.0289(3) -0.00290(19) -0.00129(18) -0.00047(18) O1 0.0184(6) 0.0209(6) 0.0226(7) -0.0049(5) -0.0022(5) -0.0070(5) O2 0.0237(7) 0.0295(7) 0.0213(7) -0.0099(6) -0.0053(5) -0.0002(6) O3 0.0211(7) 0.0138(6) 0.0273(7) -0.0037(5) -0.0113(5) -0.0005(5) O4 0.0223(7) 0.0247(7) 0.0245(7) -0.0039(5) -0.0069(5) -0.0051(5) O5 0.0283(7) 0.0150(6) 0.0187(6) -0.0017(5) -0.0011(5) -0.0033(5) O6 0.0173(7) 0.0368(8) 0.0253(7) -0.0111(6) -0.0021(5) 0.0021(6) O7 0.0170(6) 0.0191(6) 0.0293(7) -0.0050(5) -0.0018(5) -0.0049(5) O8 0.0178(6) 0.0136(6) 0.0217(7) 0.0004(5) -0.0064(5) -0.0010(5) O9 0.0231(8) 0.0471(10) 0.0383(9) -0.0116(7) -0.0071(6) 0.0082(7) O10 0.0229(7) 0.0247(7) 0.0386(8) -0.0067(6) 0.0008(6) -0.0080(6) O11 0.0178(6) 0.0209(6) 0.0240(7) -0.0052(5) -0.0027(5) -0.0071(5) O12 0.0318(8) 0.0257(7) 0.0242(7) -0.0080(6) -0.0110(6) -0.0025(6) O13 0.0200(6) 0.0133(6) 0.0245(7) -0.0032(5) -0.0090(5) -0.0008(5) O14 0.0185(6) 0.0268(7) 0.0219(7) -0.0034(5) -0.0047(5) -0.0060(5) O15 0.0244(7) 0.0152(6) 0.0195(6) -0.0015(5) 0.0005(5) -0.0041(5) O16 0.0188(7) 0.0303(7) 0.0260(7) -0.0089(6) -0.0046(5) 0.0033(6) O17 0.0164(6) 0.0203(6) 0.0292(7) -0.0063(5) -0.0023(5) -0.0049(5) O18 0.0192(6) 0.0129(6) 0.0222(7) -0.0004(5) -0.0069(5) -0.0016(5) O19 0.0184(7) 0.0323(8) 0.0334(8) -0.0060(6) -0.0021(6) -0.0020(6) O20 0.0241(7) 0.0200(7) 0.0335(8) -0.0052(6) 0.0016(6) -0.0060(6) N1 0.0248(8) 0.0147(7) 0.0286(9) 0.0004(6) 0.0036(7) -0.0010(6) N2 0.0166(8) 0.0157(7) 0.0259(8) 0.0000(6) 0.0007(6) -0.0015(6) C1 0.0198(9) 0.0175(8) 0.0165(8) -0.0040(7) -0.0018(7) -0.0054(7) C2 0.0204(9) 0.0152(8) 0.0168(8) -0.0048(7) -0.0002(7) -0.0023(7) C3 0.0264(10) 0.0153(8) 0.0182(9) -0.0049(7) 0.0004(7) -0.0076(7) C4 0.0208(9) 0.0218(9) 0.0183(9) -0.0049(7) -0.0010(7) -0.0093(7) C5 0.0198(9) 0.0206(9) 0.0159(8) -0.0032(7) -0.0035(7) -0.0033(7) C6 0.0228(9) 0.0162(8) 0.0153(8) -0.0029(7) -0.0017(7) -0.0052(7) C7 0.0252(10) 0.0165(8) 0.0201(9) 0.0001(7) -0.0053(7) -0.0067(7) C8 0.0265(10) 0.0092(7) 0.0224(9) 0.0006(7) -0.0087(7) -0.0030(7) C9 0.0255(10) 0.0160(8) 0.0262(10) 0.0005(7) -0.0074(8) -0.0046(7) C10 0.0275(10) 0.0169(9) 0.0321(11) -0.0022(8) -0.0140(8) -0.0050(8) C11 0.0310(11) 0.0150(8) 0.0272(10) -0.0064(7) -0.0136(8) -0.0003(8) C12 0.0245(10) 0.0123(8) 0.0266(10) -0.0059(7) -0.0086(8) 0.0030(7) C13 0.0210(9) 0.0102(7) 0.0247(9) -0.0017(7) -0.0097(7) 0.0003(7) C14 0.0252(10) 0.0216(9) 0.0277(10) -0.0112(8) -0.0076(8) 0.0056(8) C15 0.0198(9) 0.0254(9) 0.0194(9) -0.0093(8) 0.0010(7) 0.0023(8) C16 0.0182(9) 0.0292(10) 0.0230(10) -0.0083(8) -0.0024(7) 0.0046(8) C17 0.0211(10) 0.0329(11) 0.0239(10) -0.0087(8) -0.0009(8) -0.0050(8) C18 0.0254(10) 0.0266(10) 0.0226(10) -0.0058(8) 0.0010(8) -0.0025(8) C19 0.0213(9) 0.0269(10) 0.0165(9) -0.0051(7) -0.0005(7) 0.0012(8) C20 0.0175(9) 0.0274(10) 0.0178(9) -0.0088(7) -0.0011(7) 0.0002(7) C21 0.0251(10) 0.0260(10) 0.0173(9) -0.0028(7) -0.0034(7) -0.0004(8) C22 0.0201(9) 0.0176(8) 0.0209(9) -0.0018(7) -0.0072(7) 0.0020(7) C23 0.0259(10) 0.0201(9) 0.0292(10) -0.0096(8) -0.0109(8) 0.0031(8) C24 0.0203(9) 0.0190(9) 0.0361(11) -0.0073(8) -0.0107(8) -0.0012(7) C25 0.0180(9) 0.0166(8) 0.0294(10) -0.0035(7) -0.0046(7) 0.0010(7) C26 0.0192(9) 0.0116(8) 0.0209(9) -0.0014(7) -0.0048(7) 0.0023(7) C27 0.0164(8) 0.0128(8) 0.0215(9) -0.0006(7) -0.0064(7) 0.0011(7) C28 0.0215(9) 0.0146(8) 0.0221(9) -0.0038(7) -0.0001(7) -0.0005(7) C29 0.0244(10) 0.0323(11) 0.0268(10) -0.0082(8) 0.0002(8) -0.0104(8) C30 0.0216(10) 0.0371(12) 0.0402(12) -0.0116(10) -0.0009(9) -0.0105(9) C31 0.0272(12) 0.0552(15) 0.0499(15) -0.0165(12) 0.0065(10) -0.0192(11) C32 0.0355(12) 0.0356(12) 0.0315(12) -0.0181(9) -0.0050(9) -0.0026(9) C33 0.0349(12) 0.0446(13) 0.0287(11) -0.0133(10) 0.0024(9) -0.0090(10) C34 0.0386(13) 0.0572(16) 0.0285(12) -0.0146(11) -0.0049(10) -0.0046(11) C35 0.0262(10) 0.0151(9) 0.0351(11) -0.0049(8) -0.0146(8) 0.0029(7) C36 0.0242(10) 0.0220(9) 0.0290(10) -0.0081(8) -0.0098(8) 0.0013(8) C37 0.0234(10) 0.0214(9) 0.0203(9) 0.0015(7) -0.0091(7) -0.0054(8) C38 0.0268(10) 0.0223(9) 0.0159(9) -0.0027(7) -0.0031(7) -0.0060(8) C39 0.0228(9) 0.0147(8) 0.0237(9) -0.0034(7) -0.0043(7) -0.0033(7) C40 0.0469(13) 0.0163(9) 0.0283(11) -0.0014(8) 0.0074(9) -0.0013(9) C41 0.0203(9) 0.0252(10) 0.0276(10) -0.0076(8) 0.0029(8) -0.0084(8) C42 0.0170(9) 0.0202(9) 0.0231(9) -0.0031(7) -0.0016(7) -0.0043(7) C43 0.0188(9) 0.0241(9) 0.0269(10) -0.0085(8) 0.0004(7) -0.0051(8) C44 0.0196(9) 0.0167(8) 0.0325(11) -0.0067(8) -0.0003(8) -0.0052(7) C45 0.0196(9) 0.0197(9) 0.0252(10) 0.0001(7) -0.0023(7) -0.0053(7) C46 0.0218(9) 0.0148(8) 0.0237(10) 0.0026(7) -0.0072(7) -0.0019(7) C47 0.0161(9) 0.0210(9) 0.0275(10) 0.0013(8) 0.0002(7) -0.0057(7) C48 0.0233(10) 0.0187(9) 0.0320(11) 0.0034(8) 0.0033(8) -0.0027(8) C49 0.0265(10) 0.0233(10) 0.0302(11) 0.0079(8) -0.0028(8) -0.0022(8) C50 0.0282(11) 0.0263(10) 0.0299(11) 0.0016(8) -0.0017(8) -0.0093(9) C51 0.0240(10) 0.0209(9) 0.0326(11) -0.0034(8) -0.0014(8) -0.0021(8) C52 0.0187(9) 0.0211(9) 0.0320(11) -0.0001(8) -0.0020(8) -0.0022(7) C53 0.0460(14) 0.0402(13) 0.0335(13) -0.0031(10) -0.0071(11) -0.0016(11) C54 0.0181(9) 0.0193(8) 0.0161(8) -0.0048(7) -0.0003(7) -0.0065(7) C55 0.0189(9) 0.0157(8) 0.0182(9) -0.0057(7) -0.0001(7) -0.0016(7) C56 0.0238(9) 0.0173(8) 0.0178(9) -0.0064(7) 0.0018(7) -0.0069(7) C57 0.0188(9) 0.0236(9) 0.0179(9) -0.0069(7) 0.0004(7) -0.0092(7) C58 0.0189(9) 0.0214(9) 0.0151(8) -0.0035(7) -0.0015(7) -0.0028(7) C59 0.0226(9) 0.0164(8) 0.0147(8) -0.0029(7) -0.0008(7) -0.0056(7) C60 0.0242(9) 0.0172(8) 0.0181(9) -0.0002(7) -0.0042(7) -0.0058(7) C61 0.0259(10) 0.0117(8) 0.0214(9) -0.0002(7) -0.0088(7) -0.0025(7) C62 0.0247(10) 0.0145(8) 0.0285(10) 0.0003(7) -0.0079(8) -0.0050(7) C63 0.0293(11) 0.0149(8) 0.0327(11) -0.0025(8) -0.0159(8) -0.0034(8) C64 0.0328(11) 0.0161(8) 0.0250(10) -0.0055(7) -0.0142(8) 0.0001(8) C65 0.0232(9) 0.0130(8) 0.0235(9) -0.0045(7) -0.0076(7) 0.0043(7) C66 0.0220(9) 0.0117(8) 0.0225(9) -0.0020(7) -0.0102(7) -0.0002(7) C67 0.0256(10) 0.0201(9) 0.0245(10) -0.0092(8) -0.0055(8) 0.0045(8) C68 0.0206(9) 0.0229(9) 0.0184(9) -0.0088(7) 0.0009(7) 0.0018(7) C69 0.0172(9) 0.0270(10) 0.0238(10) -0.0072(8) -0.0019(7) 0.0028(8) C70 0.0195(9) 0.0310(10) 0.0281(10) -0.0106(8) -0.0020(8) -0.0030(8) C71 0.0252(10) 0.0228(9) 0.0257(10) -0.0057(8) 0.0002(8) -0.0031(8) C72 0.0212(9) 0.0226(9) 0.0158(9) -0.0037(7) 0.0000(7) 0.0011(7) C73 0.0204(9) 0.0254(9) 0.0167(9) -0.0081(7) -0.0007(7) -0.0016(7) C74 0.0291(10) 0.0209(9) 0.0185(9) -0.0019(7) -0.0038(8) -0.0011(8) C75 0.0211(9) 0.0161(8) 0.0207(9) -0.0015(7) -0.0063(7) 0.0020(7) C76 0.0277(10) 0.0193(9) 0.0265(10) -0.0069(8) -0.0105(8) 0.0023(8) C77 0.0225(10) 0.0167(9) 0.0354(11) -0.0071(8) -0.0112(8) -0.0014(7) C78 0.0196(9) 0.0162(8) 0.0298(10) -0.0020(7) -0.0070(8) -0.0009(7) C79 0.0193(9) 0.0127(8) 0.0223(9) -0.0026(7) -0.0050(7) 0.0024(7) C80 0.0169(9) 0.0121(8) 0.0228(9) -0.0017(7) -0.0075(7) 0.0012(7) C81 0.0195(9) 0.0168(8) 0.0250(10) -0.0058(7) -0.0024(7) -0.0009(7) C82 0.0238(10) 0.0364(11) 0.0328(11) -0.0139(9) 0.0051(8) -0.0139(9) C83 0.0223(10) 0.0374(12) 0.0339(12) -0.0044(9) -0.0042(8) -0.0118(9) C84 0.0294(12) 0.0639(17) 0.0584(17) -0.0191(14) 0.0098(11) -0.0239(12) C85 0.0640(16) 0.0383(13) 0.0246(11) -0.0105(10) -0.0038(11) -0.0154(12) C86 0.0612(17) 0.0509(15) 0.0415(14) -0.0167(12) -0.0067(12) -0.0183(13) C87 0.0392(14) 0.0687(19) 0.0538(16) -0.0239(14) -0.0052(12) -0.0196(13) C88 0.0250(10) 0.0164(9) 0.0315(11) -0.0055(8) -0.0129(8) 0.0022(7) C89 0.0206(9) 0.0239(9) 0.0269(10) -0.0074(8) -0.0066(8) -0.0001(8) C90 0.0209(9) 0.0215(9) 0.0196(9) 0.0025(7) -0.0069(7) -0.0057(7) C91 0.0227(9) 0.0219(9) 0.0149(9) -0.0006(7) -0.0031(7) -0.0056(7) C92 0.0198(9) 0.0154(8) 0.0226(9) -0.0033(7) -0.0021(7) -0.0016(7) C93 0.0239(10) 0.0148(8) 0.0253(10) -0.0020(7) 0.0008(8) -0.0004(7) C94 0.0166(9) 0.0203(9) 0.0215(9) -0.0029(7) -0.0009(7) -0.0039(7) C95 0.0164(9) 0.0199(9) 0.0229(9) -0.0031(7) -0.0029(7) -0.0025(7) C96 0.0198(9) 0.0214(9) 0.0282(10) -0.0095(8) 0.0002(7) -0.0045(7) C97 0.0189(9) 0.0170(9) 0.0331(11) -0.0074(8) -0.0017(8) -0.0040(7) C98 0.0197(9) 0.0178(9) 0.0253(10) -0.0002(7) -0.0027(7) -0.0047(7) C99 0.0226(9) 0.0139(8) 0.0258(10) 0.0013(7) -0.0080(7) -0.0019(7) C100 0.0190(9) 0.0190(9) 0.0236(10) 0.0009(7) 0.0022(7) -0.0059(7) C101 0.0205(9) 0.0157(8) 0.0313(11) 0.0014(8) 0.0014(8) -0.0020(7) C102 0.0258(10) 0.0193(9) 0.0288(11) 0.0081(8) -0.0036(8) -0.0045(8) C103 0.0311(11) 0.0208(9) 0.0273(10) 0.0019(8) -0.0013(8) -0.0097(8) C104 0.0271(10) 0.0182(9) 0.0320(11) -0.0034(8) 0.0008(8) -0.0021(8) C105 0.0194(9) 0.0180(9) 0.0309(11) 0.0001(8) -0.0013(8) -0.0018(7) C106 0.0540(15) 0.0280(11) 0.0307(12) -0.0020(9) -0.0084(11) -0.0039(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 S2 O20 1.4328(14) . ? S2 O19 1.4332(14) . ? S2 N2 1.6414(15) . ? S2 C100 1.762(2) . ? S1 O9 1.4291(15) . ? S1 O10 1.4307(14) . ? S1 N1 1.6363(16) . ? S1 C47 1.762(2) . ? O1 C1 1.390(2) . ? O1 C29 1.435(2) . ? O2 C20 1.388(2) . ? O2 C32 1.460(2) . ? O3 C13 1.394(2) . ? O3 C35 1.441(2) . ? O4 C36 1.421(2) . ? O4 C37 1.425(2) . ? O5 C39 1.412(2) . ? O5 C38 1.426(2) . ? O6 C42 1.412(2) . ? O6 C43 1.416(2) . ? O7 C44 1.428(2) . ? O7 C45 1.432(2) . ? O8 C27 1.388(2) . ? O8 C46 1.440(2) . ? O11 C54 1.390(2) . ? O11 C82 1.431(2) . ? O12 C73 1.388(2) . ? O12 C85 1.466(3) . ? O13 C66 1.390(2) . ? O13 C88 1.439(2) . ? O14 C90 1.424(2) . ? O14 C89 1.425(2) . ? O15 C92 1.413(2) . ? O15 C91 1.425(2) . ? O16 C96 1.414(2) . ? O16 C95 1.418(2) . ? O17 C98 1.425(2) . ? O17 C97 1.427(2) . ? O18 C80 1.389(2) . ? O18 C99 1.436(2) . ? N1 C40 1.467(2) . ? N1 C41 1.472(2) . ? N2 C93 1.471(2) . ? N2 C94 1.483(2) . ? C1 C6 1.398(2) . ? C1 C2 1.399(2) . ? C2 C3 1.393(2) . ? C2 C28 1.521(2) . ? C3 C4 1.385(3) . ? C3 H3 0.9300 . ? C4 C5 1.389(2) . ? C4 H4 0.9300 . ? C5 C6 1.386(2) . ? C5 H5 0.9300 . ? C6 C7 1.519(2) . ? C7 C8 1.514(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.392(3) . ? C8 C9 1.397(3) . ? C9 C10 1.385(3) . ? C9 H9 0.9300 . ? C10 C11 1.379(3) . ? C10 H10 0.9300 . ? C11 C12 1.398(3) . ? C11 H11 0.9300 . ? C12 C13 1.396(3) . ? C12 C14 1.517(3) . ? C14 C15 1.521(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.393(3) . ? C15 C20 1.397(3) . ? C16 C17 1.385(3) . ? C16 H16 0.9300 . ? C17 C18 1.389(3) . ? C17 H17 0.9300 . ? C18 C19 1.395(3) . ? C18 H18 0.9300 . ? C19 C20 1.403(3) . ? C19 C21 1.517(2) . ? C21 C22 1.519(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.393(3) . ? C22 C27 1.402(3) . ? C23 C24 1.379(3) . ? C23 H23 0.9300 . ? C24 C25 1.385(3) . ? C24 H24 0.9300 . ? C25 C26 1.392(3) . ? C25 H25 0.9300 . ? C26 C27 1.398(2) . ? C26 C28 1.520(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.504(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.529(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.488(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.521(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.504(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.504(3) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.497(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.521(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.506(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.498(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C52 1.388(3) . ? C47 C48 1.395(3) . ? C48 C49 1.377(3) . ? C48 H48 0.9300 . ? C49 C50 1.401(3) . ? C49 H49 0.9300 . ? C50 C51 1.393(3) . ? C50 C53 1.503(3) . ? C51 C52 1.386(3) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.397(2) . ? C54 C59 1.398(2) . ? C55 C56 1.395(2) . ? C55 C81 1.521(2) . ? C56 C57 1.384(3) . ? C56 H56 0.9300 . ? C57 C58 1.390(2) . ? C57 H57 0.9300 . ? C58 C59 1.390(2) . ? C58 H58 0.9300 . ? C59 C60 1.520(2) . ? C60 C61 1.517(3) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.394(3) . ? C61 C66 1.396(3) . ? C62 C63 1.385(3) . ? C62 H62 0.9300 . ? C63 C64 1.389(3) . ? C63 H63 0.9300 . ? C64 C65 1.388(3) . ? C64 H64 0.9300 . ? C65 C66 1.401(3) . ? C65 C67 1.522(3) . ? C67 C68 1.524(3) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.389(3) . ? C68 C73 1.396(3) . ? C69 C70 1.386(3) . ? C69 H69 0.9300 . ? C70 C71 1.388(3) . ? C70 H70 0.9300 . ? C71 C72 1.391(3) . ? C71 H71 0.9300 . ? C72 C73 1.395(3) . ? C72 C74 1.521(3) . ? C74 C75 1.521(3) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.391(3) . ? C75 C80 1.401(3) . ? C76 C77 1.389(3) . ? C76 H76 0.9300 . ? C77 C78 1.389(3) . ? C77 H77 0.9300 . ? C78 C79 1.392(3) . ? C78 H78 0.9300 . ? C79 C80 1.396(3) . ? C79 C81 1.516(3) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C83 1.507(3) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C84 1.519(3) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 C86 1.458(3) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 C87 1.497(4) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 C89 1.505(3) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C91 1.504(3) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 C93 1.511(3) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 C95 1.511(3) . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C95 H95A 0.9700 . ? C95 H95B 0.9700 . ? C96 C97 1.504(3) . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 C99 1.501(3) . ? C98 H98A 0.9700 . ? C98 H98B 0.9700 . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 C105 1.392(3) . ? C100 C101 1.398(3) . ? C101 C102 1.381(3) . ? C101 H101 0.9300 . ? C102 C103 1.397(3) . ? C102 H102 0.9300 . ? C103 C104 1.396(3) . ? C103 C106 1.502(3) . ? C104 C105 1.378(3) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? C106 H10A 0.9600 . ? C106 H10B 0.9600 . ? C106 H10C 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 O20 S2 O19 120.08(9) . . ? O20 S2 N2 106.32(8) . . ? O19 S2 N2 107.12(8) . . ? O20 S2 C100 108.29(9) . . ? O19 S2 C100 108.53(9) . . ? N2 S2 C100 105.59(9) . . ? O9 S1 O10 119.97(10) . . ? O9 S1 N1 107.13(9) . . ? O10 S1 N1 106.41(8) . . ? O9 S1 C47 108.31(9) . . ? O10 S1 C47 108.20(9) . . ? N1 S1 C47 106.01(9) . . ? C1 O1 C29 113.08(14) . . ? C20 O2 C32 114.36(15) . . ? C13 O3 C35 111.03(13) . . ? C36 O4 C37 113.57(14) . . ? C39 O5 C38 111.14(14) . . ? C42 O6 C43 115.41(14) . . ? C44 O7 C45 112.85(14) . . ? C27 O8 C46 112.32(13) . . ? C54 O11 C82 113.48(14) . . ? C73 O12 C85 107.93(15) . . ? C66 O13 C88 111.34(13) . . ? C90 O14 C89 113.36(14) . . ? C92 O15 C91 111.42(13) . . ? C96 O16 C95 114.55(14) . . ? C98 O17 C97 112.52(14) . . ? C80 O18 C99 112.49(13) . . ? C40 N1 C41 117.09(17) . . ? C40 N1 S1 117.55(13) . . ? C41 N1 S1 115.10(12) . . ? C93 N2 C94 115.75(15) . . ? C93 N2 S2 117.56(12) . . ? C94 N2 S2 114.61(12) . . ? O1 C1 C6 119.03(15) . . ? O1 C1 C2 119.08(16) . . ? C6 C1 C2 121.75(16) . . ? C3 C2 C1 118.08(16) . . ? C3 C2 C28 120.82(15) . . ? C1 C2 C28 120.80(16) . . ? C4 C3 C2 120.56(16) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.36(16) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.49(17) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 118.40(16) . . ? C5 C6 C7 120.96(16) . . ? C1 C6 C7 120.43(16) . . ? C8 C7 C6 109.79(14) . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C13 C8 C9 117.84(17) . . ? C13 C8 C7 120.59(16) . . ? C9 C8 C7 121.42(17) . . ? C10 C9 C8 120.95(19) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 120.03(18) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.84(18) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 117.98(18) . . ? C13 C12 C14 120.52(17) . . ? C11 C12 C14 121.35(17) . . ? C8 C13 O3 118.45(16) . . ? C8 C13 C12 122.08(17) . . ? O3 C13 C12 119.45(17) . . ? C12 C14 C15 109.73(15) . . ? C12 C14 H14A 109.7 . . ? C15 C14 H14A 109.7 . . ? C12 C14 H14B 109.7 . . ? C15 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C20 117.92(18) . . ? C16 C15 C14 120.77(17) . . ? C20 C15 C14 120.99(17) . . ? C17 C16 C15 121.28(18) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 119.58(19) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 121.03(18) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C20 117.82(17) . . ? C18 C19 C21 121.01(17) . . ? C20 C19 C21 120.92(17) . . ? O2 C20 C15 119.78(17) . . ? O2 C20 C19 118.28(16) . . ? C15 C20 C19 121.79(18) . . ? C19 C21 C22 110.15(15) . . ? C19 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C19 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C27 117.89(17) . . ? C23 C22 C21 120.76(17) . . ? C27 C22 C21 121.12(17) . . ? C24 C23 C22 120.88(18) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.52(18) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 120.42(18) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 118.33(17) . . ? C25 C26 C28 121.01(17) . . ? C27 C26 C28 120.49(16) . . ? O8 C27 C26 118.39(16) . . ? O8 C27 C22 119.88(16) . . ? C26 C27 C22 121.68(17) . . ? C26 C28 C2 109.65(14) . . ? C26 C28 H28A 109.7 . . ? C2 C28 H28A 109.7 . . ? C26 C28 H28B 109.7 . . ? C2 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? O1 C29 C30 108.15(16) . . ? O1 C29 H29A 110.1 . . ? C30 C29 H29A 110.1 . . ? O1 C29 H29B 110.1 . . ? C30 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? C29 C30 C31 112.28(18) . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O2 C32 C33 112.44(17) . . ? O2 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? O2 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C32 C33 C34 114.20(19) . . ? C32 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? C32 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 C36 109.30(15) . . ? O3 C35 H35A 109.8 . . ? C36 C35 H35A 109.8 . . ? O3 C35 H35B 109.8 . . ? C36 C35 H35B 109.8 . . ? H35A C35 H35B 108.3 . . ? O4 C36 C35 109.16(16) . . ? O4 C36 H36A 109.8 . . ? C35 C36 H36A 109.8 . . ? O4 C36 H36B 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? O4 C37 C38 112.47(15) . . ? O4 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? O4 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? O5 C38 C37 109.46(15) . . ? O5 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? O5 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? O5 C39 C40 108.41(15) . . ? O5 C39 H39A 110.0 . . ? C40 C39 H39A 110.0 . . ? O5 C39 H39B 110.0 . . ? C40 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? N1 C40 C39 109.73(16) . . ? N1 C40 H40A 109.7 . . ? C39 C40 H40A 109.7 . . ? N1 C40 H40B 109.7 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? N1 C41 C42 113.93(16) . . ? N1 C41 H41A 108.8 . . ? C42 C41 H41A 108.8 . . ? N1 C41 H41B 108.8 . . ? C42 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? O6 C42 C41 103.95(15) . . ? O6 C42 H42A 111.0 . . ? C41 C42 H42A 111.0 . . ? O6 C42 H42B 111.0 . . ? C41 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? O6 C43 C44 107.09(15) . . ? O6 C43 H43A 110.3 . . ? C44 C43 H43A 110.3 . . ? O6 C43 H43B 110.3 . . ? C44 C43 H43B 110.3 . . ? H43A C43 H43B 108.6 . . ? O7 C44 C43 112.16(15) . . ? O7 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? O7 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? O7 C45 C46 109.32(15) . . ? O7 C45 H45A 109.8 . . ? C46 C45 H45A 109.8 . . ? O7 C45 H45B 109.8 . . ? C46 C45 H45B 109.8 . . ? H45A C45 H45B 108.3 . . ? O8 C46 C45 109.42(14) . . ? O8 C46 H46A 109.8 . . ? C45 C46 H46A 109.8 . . ? O8 C46 H46B 109.8 . . ? C45 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? C52 C47 C48 120.47(19) . . ? C52 C47 S1 119.66(15) . . ? C48 C47 S1 119.78(15) . . ? C49 C48 C47 118.99(19) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? C48 C49 C50 121.75(19) . . ? C48 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? C51 C50 C49 118.1(2) . . ? C51 C50 C53 121.1(2) . . ? C49 C50 C53 120.78(19) . . ? C52 C51 C50 120.96(19) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C47 119.72(18) . . ? C51 C52 H52 120.1 . . ? C47 C52 H52 120.1 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O11 C54 C55 119.07(16) . . ? O11 C54 C59 118.77(15) . . ? C55 C54 C59 122.03(16) . . ? C56 C55 C54 117.89(16) . . ? C56 C55 C81 120.64(15) . . ? C54 C55 C81 121.12(16) . . ? C57 C56 C55 120.75(16) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 120.22(16) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C59 C58 C57 120.56(17) . . ? C59 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? C58 C59 C54 118.19(16) . . ? C58 C59 C60 120.77(16) . . ? C54 C59 C60 120.86(16) . . ? C61 C60 C59 109.71(14) . . ? C61 C60 H60A 109.7 . . ? C59 C60 H60A 109.7 . . ? C61 C60 H60B 109.7 . . ? C59 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? C62 C61 C66 117.70(17) . . ? C62 C61 C60 122.05(18) . . ? C66 C61 C60 120.04(16) . . ? C63 C62 C61 121.12(19) . . ? C63 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C62 C63 C64 119.81(18) . . ? C62 C63 H63 120.1 . . ? C64 C63 H63 120.1 . . ? C65 C64 C63 120.98(18) . . ? C65 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C64 C65 C66 117.89(18) . . ? C64 C65 C67 121.53(17) . . ? C66 C65 C67 120.42(17) . . ? O13 C66 C61 118.43(16) . . ? O13 C66 C65 119.38(17) . . ? C61 C66 C65 122.16(17) . . ? C65 C67 C68 110.07(14) . . ? C65 C67 H67A 109.6 . . ? C68 C67 H67A 109.6 . . ? C65 C67 H67B 109.6 . . ? C68 C67 H67B 109.6 . . ? H67A C67 H67B 108.2 . . ? C69 C68 C73 118.00(17) . . ? C69 C68 C67 121.93(17) . . ? C73 C68 C67 119.92(17) . . ? C70 C69 C68 120.81(18) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C69 C70 C71 120.05(18) . . ? C69 C70 H70 120.0 . . ? C71 C70 H70 120.0 . . ? C70 C71 C72 120.63(18) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? C71 C72 C73 118.05(17) . . ? C71 C72 C74 121.91(17) . . ? C73 C72 C74 119.79(17) . . ? O12 C73 C72 119.02(16) . . ? O12 C73 C68 118.97(16) . . ? C72 C73 C68 122.01(17) . . ? C72 C74 C75 109.97(15) . . ? C72 C74 H74A 109.7 . . ? C75 C74 H74A 109.7 . . ? C72 C74 H74B 109.7 . . ? C75 C74 H74B 109.7 . . ? H74A C74 H74B 108.2 . . ? C76 C75 C80 117.87(18) . . ? C76 C75 C74 120.79(17) . . ? C80 C75 C74 121.12(17) . . ? C77 C76 C75 120.85(18) . . ? C77 C76 H76 119.6 . . ? C75 C76 H76 119.6 . . ? C78 C77 C76 120.13(18) . . ? C78 C77 H77 119.9 . . ? C76 C77 H77 119.9 . . ? C77 C78 C79 120.61(18) . . ? C77 C78 H78 119.7 . . ? C79 C78 H78 119.7 . . ? C78 C79 C80 118.17(17) . . ? C78 C79 C81 121.31(17) . . ? C80 C79 C81 120.38(16) . . ? O18 C80 C79 118.64(16) . . ? O18 C80 C75 119.21(16) . . ? C79 C80 C75 122.11(17) . . ? C79 C81 C55 109.54(14) . . ? C79 C81 H81A 109.8 . . ? C55 C81 H81A 109.8 . . ? C79 C81 H81B 109.8 . . ? C55 C81 H81B 109.8 . . ? H81A C81 H81B 108.2 . . ? O11 C82 C83 108.27(16) . . ? O11 C82 H82A 110.0 . . ? C83 C82 H82A 110.0 . . ? O11 C82 H82B 110.0 . . ? C83 C82 H82B 110.0 . . ? H82A C82 H82B 108.4 . . ? C82 C83 C84 113.02(19) . . ? C82 C83 H83A 109.0 . . ? C84 C83 H83A 109.0 . . ? C82 C83 H83B 109.0 . . ? C84 C83 H83B 109.0 . . ? H83A C83 H83B 107.8 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 O12 111.6(2) . . ? C86 C85 H85A 109.3 . . ? O12 C85 H85A 109.3 . . ? C86 C85 H85B 109.3 . . ? O12 C85 H85B 109.3 . . ? H85A C85 H85B 108.0 . . ? C85 C86 C87 114.6(2) . . ? C85 C86 H86A 108.6 . . ? C87 C86 H86A 108.6 . . ? C85 C86 H86B 108.6 . . ? C87 C86 H86B 108.6 . . ? H86A C86 H86B 107.6 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? O13 C88 C89 109.79(15) . . ? O13 C88 H88A 109.7 . . ? C89 C88 H88A 109.7 . . ? O13 C88 H88B 109.7 . . ? C89 C88 H88B 109.7 . . ? H88A C88 H88B 108.2 . . ? O14 C89 C88 108.51(16) . . ? O14 C89 H89A 110.0 . . ? C88 C89 H89A 110.0 . . ? O14 C89 H89B 110.0 . . ? C88 C89 H89B 110.0 . . ? H89A C89 H89B 108.4 . . ? O14 C90 C91 112.16(15) . . ? O14 C90 H90A 109.2 . . ? C91 C90 H90A 109.2 . . ? O14 C90 H90B 109.2 . . ? C91 C90 H90B 109.2 . . ? H90A C90 H90B 107.9 . . ? O15 C91 C90 109.62(15) . . ? O15 C91 H91A 109.7 . . ? C90 C91 H91A 109.7 . . ? O15 C91 H91B 109.7 . . ? C90 C91 H91B 109.7 . . ? H91A C91 H91B 108.2 . . ? O15 C92 C93 107.83(14) . . ? O15 C92 H92A 110.1 . . ? C93 C92 H92A 110.1 . . ? O15 C92 H92B 110.1 . . ? C93 C92 H92B 110.1 . . ? H92A C92 H92B 108.5 . . ? N2 C93 C92 109.09(15) . . ? N2 C93 H93A 109.9 . . ? C92 C93 H93A 109.9 . . ? N2 C93 H93B 109.9 . . ? C92 C93 H93B 109.9 . . ? H93A C93 H93B 108.3 . . ? N2 C94 C95 113.97(15) . . ? N2 C94 H94A 108.8 . . ? C95 C94 H94A 108.8 . . ? N2 C94 H94B 108.8 . . ? C95 C94 H94B 108.8 . . ? H94A C94 H94B 107.7 . . ? O16 C95 C94 104.26(14) . . ? O16 C95 H95A 110.9 . . ? C94 C95 H95A 110.9 . . ? O16 C95 H95B 110.9 . . ? C94 C95 H95B 110.9 . . ? H95A C95 H95B 108.9 . . ? O16 C96 C97 107.92(15) . . ? O16 C96 H96A 110.1 . . ? C97 C96 H96A 110.1 . . ? O16 C96 H96B 110.1 . . ? C97 C96 H96B 110.1 . . ? H96A C96 H96B 108.4 . . ? O17 C97 C96 112.04(15) . . ? O17 C97 H97A 109.2 . . ? C96 C97 H97A 109.2 . . ? O17 C97 H97B 109.2 . . ? C96 C97 H97B 109.2 . . ? H97A C97 H97B 107.9 . . ? O17 C98 C99 109.31(15) . . ? O17 C98 H98A 109.8 . . ? C99 C98 H98A 109.8 . . ? O17 C98 H98B 109.8 . . ? C99 C98 H98B 109.8 . . ? H98A C98 H98B 108.3 . . ? O18 C99 C98 109.41(14) . . ? O18 C99 H99A 109.8 . . ? C98 C99 H99A 109.8 . . ? O18 C99 H99B 109.8 . . ? C98 C99 H99B 109.8 . . ? H99A C99 H99B 108.2 . . ? C105 C100 C101 120.13(18) . . ? C105 C100 S2 120.10(15) . . ? C101 C100 S2 119.62(15) . . ? C102 C101 C100 119.13(18) . . ? C102 C101 H101 120.4 . . ? C100 C101 H101 120.4 . . ? C101 C102 C103 121.47(18) . . ? C101 C102 H102 119.3 . . ? C103 C102 H102 119.3 . . ? C104 C103 C102 118.33(19) . . ? C104 C103 C106 121.09(19) . . ? C102 C103 C106 120.58(19) . . ? C105 C104 C103 120.98(19) . . ? C105 C104 H104 119.5 . . ? C103 C104 H104 119.5 . . ? C104 C105 C100 119.91(18) . . ? C104 C105 H105 120.0 . . ? C100 C105 H105 120.0 . . ? C103 C106 H10A 109.5 . . ? C103 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C103 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.360 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.095 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 749551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H89 N O8 S' _chemical_formula_weight 1044.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.3737(15) _cell_length_b 14.3951(15) _cell_length_c 27.451(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.396(2) _cell_angle_gamma 90.00 _cell_volume 5857.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATES _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9572 _exptl_absorpt_correction_T_max 0.9869 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _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 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31126 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11461 _reflns_number_gt 7897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0617P)^2^+2.8379P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11461 _refine_ls_number_parameters 691 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1425 _refine_ls_R_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1721 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.79702(7) 0.66645(7) 1.02333(4) 0.0232(2) Uani 1 d . . . O1 O 0.92771(18) 0.83642(17) 0.77100(9) 0.0243(6) Uani 1 d . . . O2 O 0.84353(17) 0.73657(18) 0.86732(9) 0.0244(6) Uani 1 d . . . O3 O 0.87956(17) 0.46158(18) 0.89358(9) 0.0235(6) Uani 1 d . . . O4 O 0.95802(15) 0.52489(16) 0.78548(9) 0.0158(6) Uani 1 d . . . O5 O 1.12476(16) 0.66434(17) 0.73753(9) 0.0209(6) Uani 1 d . . . O6 O 0.87914(15) 0.63235(17) 0.66673(9) 0.0188(6) Uani 1 d . . . O7 O 0.82665(19) 0.58365(19) 1.05175(10) 0.0324(7) Uani 1 d . . . O8 O 0.71364(17) 0.7093(2) 1.02348(10) 0.0300(7) Uani 1 d . . . N1 N 0.7919(2) 0.6423(2) 0.96434(11) 0.0211(7) Uani 1 d . . . C1 C 0.9540(2) 0.8325(2) 0.72609(13) 0.0146(8) Uani 1 d . . . C2 C 0.8896(2) 0.8300(2) 0.67975(14) 0.0160(8) Uani 1 d . . . C3 C 0.9160(2) 0.8526(2) 0.63663(13) 0.0165(8) Uani 1 d . . . H3 H 0.8733 0.8492 0.6055 0.020 Uiso 1 calc R . . C4 C 1.0032(2) 0.8802(2) 0.63772(13) 0.0163(8) Uani 1 d . . . C5 C 1.0663(2) 0.8755(2) 0.68413(13) 0.0159(8) Uani 1 d . . . H5 H 1.1261 0.8894 0.6859 0.019 Uiso 1 calc R . . C6 C 1.0438(2) 0.8507(2) 0.72856(13) 0.0144(8) Uani 1 d . . . C7 C 1.1167(2) 0.8511(3) 0.77796(14) 0.0227(9) Uani 1 d . . . H7A H 1.1037 0.9012 0.7986 0.027 Uiso 1 calc R . . H7B H 1.1735 0.8657 0.7706 0.027 Uiso 1 calc R . . C8 C 1.1297(2) 0.7630(3) 0.80923(13) 0.0160(8) Uani 1 d . . . C9 C 1.1404(2) 0.7702(3) 0.86128(14) 0.0176(8) Uani 1 d . . . H9 H 1.1376 0.8288 0.8751 0.021 Uiso 1 calc R . . C10 C 1.1551(2) 0.6943(3) 0.89305(13) 0.0167(8) Uani 1 d . . . C11 C 1.1568(2) 0.6065(2) 0.87086(13) 0.0151(8) Uani 1 d . . . H11 H 1.1653 0.5540 0.8914 0.018 Uiso 1 calc R . . C12 C 1.1462(2) 0.5955(3) 0.81935(13) 0.0168(8) Uani 1 d . . . C13 C 1.1350(2) 0.6748(2) 0.78908(13) 0.0148(8) Uani 1 d . . . C14 C 1.1514(2) 0.4992(3) 0.79785(13) 0.0178(8) Uani 1 d . . . H14A H 1.1527 0.4547 0.8246 0.021 Uiso 1 calc R . . H14B H 1.2088 0.4943 0.7896 0.021 Uiso 1 calc R . . C15 C 1.0782(2) 0.4685(2) 0.75158(13) 0.0143(8) Uani 1 d . . . C16 C 1.1023(2) 0.4234(2) 0.71224(13) 0.0151(8) Uani 1 d . . . H16 H 1.1634 0.4156 0.7147 0.018 Uiso 1 calc R . . C17 C 1.0401(2) 0.3895(2) 0.66949(13) 0.0159(8) Uani 1 d . . . C18 C 0.9497(2) 0.4038(2) 0.66701(13) 0.0150(8) Uani 1 d . . . H18 H 0.9062 0.3824 0.6389 0.018 Uiso 1 calc R . . C19 C 0.9216(2) 0.4490(2) 0.70512(14) 0.0163(8) Uani 1 d . . . C20 C 0.9864(2) 0.4796(2) 0.74746(13) 0.0134(8) Uani 1 d . . . C21 C 0.8218(2) 0.4560(2) 0.70140(14) 0.0180(8) Uani 1 d . . . H21A H 0.8106 0.4179 0.7283 0.022 Uiso 1 calc R . . H21B H 0.7900 0.4270 0.6698 0.022 Uiso 1 calc R . . C22 C 0.7767(2) 0.5500(2) 0.70382(13) 0.0135(8) Uani 1 d . . . C23 C 0.7009(2) 0.5519(3) 0.72197(13) 0.0164(8) Uani 1 d . . . H23 H 0.6825 0.4971 0.7342 0.020 Uiso 1 calc R . . C24 C 0.6508(2) 0.6327(2) 0.72260(13) 0.0137(8) Uani 1 d . . . C25 C 0.6839(2) 0.7133(3) 0.70724(13) 0.0165(8) Uani 1 d . . . H25 H 0.6532 0.7685 0.7087 0.020 Uiso 1 calc R . . C26 C 0.7607(2) 0.7165(2) 0.68958(13) 0.0161(8) Uani 1 d . . . C27 C 0.8043(2) 0.6329(2) 0.68605(13) 0.0138(8) Uani 1 d . . . C28 C 0.7902(2) 0.8107(3) 0.67456(15) 0.0205(9) Uani 1 d . . . H28A H 0.7582 0.8211 0.6395 0.025 Uiso 1 calc R . . H28B H 0.7692 0.8573 0.6943 0.025 Uiso 1 calc R . . C29 C 1.0256(3) 0.9158(3) 0.58983(14) 0.0223(9) Uani 1 d . . . C30 C 1.0118(3) 0.8373(3) 0.55029(14) 0.0272(10) Uani 1 d . . . H30A H 1.0543 0.7884 0.5628 0.041 Uiso 1 calc R . . H30B H 1.0209 0.8613 0.5194 0.041 Uiso 1 calc R . . H30C H 0.9515 0.8134 0.5441 0.041 Uiso 1 calc R . . C31 C 0.9618(3) 0.9965(3) 0.56860(15) 0.0356(11) Uani 1 d . . . H31A H 0.9005 0.9751 0.5609 0.053 Uiso 1 calc R . . H31B H 0.9746 1.0195 0.5384 0.053 Uiso 1 calc R . . H31C H 0.9704 1.0453 0.5932 0.053 Uiso 1 calc R . . C32 C 1.1229(3) 0.9507(3) 0.60011(16) 0.0337(11) Uani 1 d . . . H32A H 1.1329 0.9992 0.6250 0.051 Uiso 1 calc R . . H32B H 1.1330 0.9744 0.5694 0.051 Uiso 1 calc R . . H32C H 1.1637 0.9003 0.6124 0.051 Uiso 1 calc R . . C33 C 1.1677(2) 0.7025(3) 0.95022(13) 0.0186(8) Uani 1 d . . . C34 C 1.1653(3) 0.8037(3) 0.96760(14) 0.0259(9) Uani 1 d . . . H34A H 1.2124 0.8383 0.9589 0.039 Uiso 1 calc R . . H34B H 1.1741 0.8053 1.0035 0.039 Uiso 1 calc R . . H34C H 1.1079 0.8307 0.9512 0.039 Uiso 1 calc R . . C35 C 1.2589(2) 0.6603(3) 0.97790(14) 0.0257(9) Uani 1 d . . . H35A H 1.2593 0.5954 0.9699 0.039 Uiso 1 calc R . . H35B H 1.2683 0.6677 1.0137 0.039 Uiso 1 calc R . . H35C H 1.3062 0.6913 0.9674 0.039 Uiso 1 calc R . . C36 C 1.0923(2) 0.6498(3) 0.96483(14) 0.0237(9) Uani 1 d . . . H36A H 1.0353 0.6779 0.9487 0.036 Uiso 1 calc R . . H36B H 1.1019 0.6521 1.0008 0.036 Uiso 1 calc R . . H36C H 1.0922 0.5863 0.9542 0.036 Uiso 1 calc R . . C37 C 1.0712(2) 0.3372(3) 0.62806(14) 0.0210(9) Uani 1 d . . . C38 C 0.9927(3) 0.3085(3) 0.58362(15) 0.0299(10) Uani 1 d . . . H38A H 0.9530 0.2681 0.5954 0.045 Uiso 1 calc R . . H38B H 1.0157 0.2766 0.5589 0.045 Uiso 1 calc R . . H38C H 0.9603 0.3629 0.5686 0.045 Uiso 1 calc R . . C39 C 1.1212(3) 0.2486(3) 0.65080(15) 0.0265(10) Uani 1 d . . . H39A H 1.1725 0.2649 0.6780 0.040 Uiso 1 calc R . . H39B H 1.1410 0.2159 0.6252 0.040 Uiso 1 calc R . . H39C H 1.0814 0.2097 0.6634 0.040 Uiso 1 calc R . . C40 C 1.1358(3) 0.3995(3) 0.60808(15) 0.0265(9) Uani 1 d . . . H40A H 1.1051 0.4554 0.5941 0.040 Uiso 1 calc R . . H40B H 1.1554 0.3668 0.5824 0.040 Uiso 1 calc R . . H40C H 1.1873 0.4151 0.6354 0.040 Uiso 1 calc R . . C41 C 0.5629(2) 0.6289(2) 0.73966(14) 0.0168(8) Uani 1 d . . . C42 C 0.5844(3) 0.5964(3) 0.79475(15) 0.0319(10) Uani 1 d . . . H42A H 0.6130 0.5366 0.7978 0.048 Uiso 1 calc R . . H42B H 0.5295 0.5920 0.8050 0.048 Uiso 1 calc R . . H42C H 0.6242 0.6402 0.8160 0.048 Uiso 1 calc R . . C43 C 0.4980(2) 0.5605(3) 0.70583(15) 0.0230(9) Uani 1 d . . . H43A H 0.4830 0.5823 0.6716 0.035 Uiso 1 calc R . . H43B H 0.4441 0.5555 0.7170 0.035 Uiso 1 calc R . . H43C H 0.5263 0.5006 0.7077 0.035 Uiso 1 calc R . . C44 C 0.5156(2) 0.7232(3) 0.73462(16) 0.0245(9) Uani 1 d . . . H44A H 0.5538 0.7673 0.7565 0.037 Uiso 1 calc R . . H44B H 0.4599 0.7173 0.7439 0.037 Uiso 1 calc R . . H44C H 0.5033 0.7442 0.7003 0.037 Uiso 1 calc R . . C45 C 0.9080(2) 0.7561(3) 0.79713(13) 0.0190(8) Uani 1 d . . . H45A H 0.9568 0.7112 0.8029 0.023 Uiso 1 calc R . . H45B H 0.8525 0.7265 0.7784 0.023 Uiso 1 calc R . . C46 C 0.8984(2) 0.7960(3) 0.84656(14) 0.0219(9) Uani 1 d . . . H46A H 0.9575 0.8023 0.8702 0.026 Uiso 1 calc R . . H46B H 0.8712 0.8572 0.8407 0.026 Uiso 1 calc R . . C47 C 0.8233(3) 0.7761(3) 0.91037(14) 0.0218(9) Uani 1 d . . . H47A H 0.7987 0.8380 0.9024 0.026 Uiso 1 calc R . . H47B H 0.8778 0.7809 0.9378 0.026 Uiso 1 calc R . . C48 C 0.7546(2) 0.7144(3) 0.92633(14) 0.0254(9) Uani 1 d . . . H48A H 0.7152 0.7540 0.9396 0.030 Uiso 1 calc R . . H48B H 0.7176 0.6840 0.8964 0.030 Uiso 1 calc R . . C49 C 0.8822(3) 0.7513(3) 1.04332(14) 0.0222(9) Uani 1 d . . . C50 C 0.9716(3) 0.7246(3) 1.06401(14) 0.0270(10) Uani 1 d . . . H50 H 0.9863 0.6621 1.0694 0.032 Uiso 1 calc R . . C51 C 1.0380(3) 0.7916(3) 1.07645(15) 0.0303(10) Uani 1 d . . . H51 H 1.0975 0.7735 1.0905 0.036 Uiso 1 calc R . . C52 C 1.0183(3) 0.8851(3) 1.06854(15) 0.0286(10) Uani 1 d . . . C53 C 0.9287(3) 0.9104(3) 1.04855(15) 0.0293(10) Uani 1 d . . . H53 H 0.9139 0.9729 1.0434 0.035 Uiso 1 calc R . . C54 C 0.8610(3) 0.8445(3) 1.03610(14) 0.0243(9) Uani 1 d . . . H54 H 0.8013 0.8628 1.0229 0.029 Uiso 1 calc R . . C55 C 1.0912(3) 0.9576(3) 1.08186(17) 0.0409(12) Uani 1 d . . . H55A H 1.1192 0.9559 1.1175 0.061 Uiso 1 calc R . . H55B H 1.0654 1.0179 1.0727 0.061 Uiso 1 calc R . . H55C H 1.1357 0.9452 1.0639 0.061 Uiso 1 calc R . . C56 C 0.8600(2) 0.5802(3) 0.95270(14) 0.0216(9) Uani 1 d . . . H56A H 0.8961 0.5525 0.9837 0.026 Uiso 1 calc R . . H56B H 0.9000 0.6162 0.9379 0.026 Uiso 1 calc R . . C57 C 0.8158(2) 0.5039(3) 0.91623(15) 0.0249(9) Uani 1 d . . . H57A H 0.7910 0.4572 0.9342 0.030 Uiso 1 calc R . . H57B H 0.7665 0.5299 0.8901 0.030 Uiso 1 calc R . . C58 C 0.8892(3) 0.5146(3) 0.85140(15) 0.0288(10) Uani 1 d . . . H58A H 0.9118 0.5760 0.8626 0.035 Uiso 1 calc R . . H58B H 0.8309 0.5216 0.8271 0.035 Uiso 1 calc R . . C59 C 0.9528(3) 0.4672(3) 0.82700(14) 0.0219(9) Uani 1 d . . . H59A H 1.0118 0.4607 0.8507 0.026 Uiso 1 calc R . . H59B H 0.9305 0.4060 0.8152 0.026 Uiso 1 calc R . . C60 C 1.2056(3) 0.6746(3) 0.72223(14) 0.0326(11) Uani 1 d . . . H60A H 1.2493 0.6280 0.7385 0.039 Uiso 1 calc R . . H60B H 1.2316 0.7355 0.7317 0.039 Uiso 1 calc R . . C61 C 1.1821(3) 0.6628(3) 0.66540(15) 0.0339(11) Uani 1 d . . . H61A H 1.1568 0.6014 0.6568 0.041 Uiso 1 calc R . . H61B H 1.1361 0.7079 0.6499 0.041 Uiso 1 calc R . . C62 C 1.2610(4) 0.6748(5) 0.6439(2) 0.083(2) Uani 1 d . . . H62A H 1.2909 0.7323 0.6557 0.125 Uiso 1 calc R . . H62B H 1.2406 0.6757 0.6077 0.125 Uiso 1 calc R . . H62C H 1.3023 0.6241 0.6546 0.125 Uiso 1 calc R . . C63 C 0.8570(3) 0.6151(3) 0.61341(14) 0.0241(9) Uani 1 d . . . H63A H 0.8178 0.6638 0.5954 0.029 Uiso 1 calc R . . H63B H 0.8256 0.5563 0.6057 0.029 Uiso 1 calc R . . C64 C 0.9431(3) 0.6127(3) 0.59719(15) 0.0284(10) Uani 1 d . . . H64A H 0.9826 0.5652 0.6162 0.034 Uiso 1 calc R . . H64B H 0.9737 0.6721 0.6047 0.034 Uiso 1 calc R . . C65 C 0.9252(3) 0.5925(3) 0.54076(17) 0.0456(13) Uani 1 d . . . H65A H 0.8938 0.5345 0.5331 0.068 Uiso 1 calc R . . H65B H 0.9815 0.5891 0.5319 0.068 Uiso 1 calc R . . H65C H 0.8889 0.6414 0.5218 0.068 Uiso 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 0.0282(6) 0.0263(6) 0.0202(5) 0.0015(4) 0.0154(5) -0.0021(4) O1 0.0420(17) 0.0147(14) 0.0241(15) 0.0041(11) 0.0223(13) 0.0018(12) O2 0.0322(16) 0.0252(16) 0.0201(15) -0.0009(12) 0.0143(13) -0.0034(12) O3 0.0267(15) 0.0250(16) 0.0242(15) 0.0030(12) 0.0165(13) 0.0012(12) O4 0.0179(13) 0.0146(13) 0.0189(14) -0.0005(10) 0.0120(11) 0.0031(10) O5 0.0232(14) 0.0263(15) 0.0130(14) 0.0014(11) 0.0046(12) 0.0008(12) O6 0.0151(13) 0.0212(15) 0.0227(15) 0.0030(11) 0.0093(12) 0.0028(11) O7 0.0513(19) 0.0284(17) 0.0233(16) 0.0077(13) 0.0200(15) 0.0007(14) O8 0.0240(15) 0.0429(19) 0.0307(17) -0.0012(14) 0.0208(13) 0.0000(13) N1 0.0228(18) 0.0241(19) 0.0187(18) -0.0022(14) 0.0097(15) -0.0014(14) C1 0.021(2) 0.0088(18) 0.017(2) 0.0010(15) 0.0102(17) 0.0035(15) C2 0.020(2) 0.0076(18) 0.023(2) 0.0020(15) 0.0094(17) -0.0009(15) C3 0.017(2) 0.018(2) 0.0114(19) 0.0034(15) -0.0016(16) 0.0014(15) C4 0.019(2) 0.017(2) 0.015(2) 0.0045(15) 0.0080(17) -0.0002(15) C5 0.0111(18) 0.016(2) 0.023(2) 0.0015(16) 0.0078(17) 0.0012(15) C6 0.020(2) 0.0099(19) 0.0118(19) 0.0011(14) 0.0019(16) 0.0027(15) C7 0.022(2) 0.022(2) 0.022(2) 0.0023(17) 0.0014(18) 0.0010(16) C8 0.0093(18) 0.023(2) 0.014(2) 0.0017(16) 0.0002(15) 0.0019(15) C9 0.0121(19) 0.017(2) 0.023(2) -0.0040(16) 0.0043(16) -0.0004(15) C10 0.0103(18) 0.023(2) 0.018(2) 0.0017(16) 0.0045(16) -0.0003(15) C11 0.0095(18) 0.015(2) 0.019(2) 0.0066(15) -0.0002(15) 0.0018(14) C12 0.0070(18) 0.024(2) 0.017(2) -0.0057(16) -0.0011(16) -0.0009(15) C13 0.0106(18) 0.022(2) 0.0114(19) 0.0016(15) 0.0021(15) 0.0024(15) C14 0.0156(19) 0.022(2) 0.017(2) 0.0034(16) 0.0066(16) 0.0035(16) C15 0.0164(19) 0.0133(19) 0.0136(19) 0.0053(15) 0.0045(16) 0.0049(15) C16 0.0121(18) 0.015(2) 0.018(2) 0.0037(15) 0.0038(16) 0.0033(15) C17 0.019(2) 0.014(2) 0.016(2) 0.0052(15) 0.0078(17) 0.0031(15) C18 0.0176(19) 0.0126(19) 0.015(2) 0.0009(15) 0.0057(16) 0.0026(15) C19 0.0156(19) 0.0123(19) 0.023(2) 0.0051(16) 0.0097(17) 0.0007(15) C20 0.0197(19) 0.0102(18) 0.0134(19) 0.0022(14) 0.0098(16) 0.0050(15) C21 0.021(2) 0.016(2) 0.019(2) -0.0024(16) 0.0094(17) -0.0045(16) C22 0.0071(17) 0.017(2) 0.0141(19) -0.0021(15) -0.0004(15) 0.0010(14) C23 0.0166(19) 0.018(2) 0.016(2) -0.0003(15) 0.0070(16) -0.0049(15) C24 0.0142(19) 0.018(2) 0.0093(18) -0.0032(15) 0.0034(15) -0.0005(15) C25 0.0136(19) 0.017(2) 0.018(2) -0.0007(16) 0.0027(16) 0.0028(15) C26 0.0121(18) 0.018(2) 0.018(2) 0.0036(16) 0.0040(16) -0.0019(15) C27 0.0071(17) 0.020(2) 0.0139(19) -0.0007(15) 0.0028(15) -0.0025(14) C28 0.0144(19) 0.019(2) 0.030(2) 0.0044(17) 0.0102(18) -0.0002(16) C29 0.029(2) 0.027(2) 0.012(2) 0.0009(17) 0.0090(18) -0.0069(18) C30 0.034(2) 0.033(3) 0.019(2) 0.0068(18) 0.0141(19) -0.0053(19) C31 0.059(3) 0.029(3) 0.023(2) 0.0108(19) 0.018(2) 0.001(2) C32 0.034(2) 0.045(3) 0.028(2) 0.007(2) 0.018(2) -0.016(2) C33 0.016(2) 0.024(2) 0.016(2) 0.0012(16) 0.0054(17) -0.0026(16) C34 0.030(2) 0.031(2) 0.017(2) -0.0073(18) 0.0077(18) -0.0085(18) C35 0.022(2) 0.040(3) 0.015(2) 0.0027(18) 0.0049(18) 0.0010(18) C36 0.024(2) 0.028(2) 0.020(2) 0.0002(17) 0.0083(18) -0.0051(17) C37 0.019(2) 0.027(2) 0.019(2) -0.0034(17) 0.0072(17) 0.0049(17) C38 0.024(2) 0.041(3) 0.029(2) -0.012(2) 0.0138(19) 0.0094(19) C39 0.025(2) 0.029(2) 0.030(2) -0.0076(19) 0.0145(19) 0.0035(18) C40 0.029(2) 0.032(2) 0.024(2) -0.0010(18) 0.0162(19) 0.0018(18) C41 0.0155(19) 0.017(2) 0.022(2) 0.0017(16) 0.0127(17) 0.0008(15) C42 0.028(2) 0.042(3) 0.029(2) 0.001(2) 0.014(2) 0.002(2) C43 0.016(2) 0.018(2) 0.038(3) -0.0017(18) 0.0128(19) 0.0020(16) C44 0.021(2) 0.019(2) 0.042(3) -0.0009(18) 0.0229(19) 0.0025(17) C45 0.022(2) 0.020(2) 0.017(2) 0.0044(16) 0.0086(17) -0.0009(16) C46 0.021(2) 0.022(2) 0.025(2) 0.0028(17) 0.0099(18) -0.0040(16) C47 0.024(2) 0.024(2) 0.019(2) -0.0012(17) 0.0102(18) 0.0012(17) C48 0.018(2) 0.039(3) 0.020(2) -0.0047(19) 0.0068(18) 0.0017(18) C49 0.028(2) 0.028(2) 0.014(2) 0.0004(17) 0.0123(18) 0.0023(17) C50 0.033(2) 0.028(2) 0.023(2) 0.0019(18) 0.012(2) 0.0045(19) C51 0.024(2) 0.041(3) 0.026(2) -0.002(2) 0.0079(19) 0.002(2) C52 0.025(2) 0.043(3) 0.020(2) -0.0038(19) 0.0078(19) -0.007(2) C53 0.041(3) 0.023(2) 0.026(2) -0.0041(18) 0.012(2) -0.0009(19) C54 0.025(2) 0.026(2) 0.023(2) -0.0026(18) 0.0078(18) 0.0036(18) C55 0.044(3) 0.043(3) 0.033(3) -0.007(2) 0.007(2) -0.013(2) C56 0.022(2) 0.026(2) 0.019(2) 0.0030(17) 0.0109(18) 0.0015(17) C57 0.023(2) 0.030(2) 0.027(2) -0.0044(18) 0.0151(19) -0.0073(18) C58 0.031(2) 0.036(3) 0.024(2) 0.0065(19) 0.017(2) 0.0055(19) C59 0.027(2) 0.017(2) 0.025(2) 0.0037(17) 0.0133(19) 0.0002(16) C60 0.031(2) 0.050(3) 0.017(2) 0.002(2) 0.0061(19) 0.003(2) C61 0.035(3) 0.046(3) 0.023(2) 0.005(2) 0.010(2) 0.009(2) C62 0.052(4) 0.166(7) 0.040(3) 0.027(4) 0.027(3) 0.031(4) C63 0.026(2) 0.028(2) 0.022(2) 0.0049(18) 0.0127(19) 0.0024(18) C64 0.030(2) 0.030(2) 0.033(3) 0.0111(19) 0.022(2) 0.0082(18) C65 0.067(3) 0.040(3) 0.042(3) 0.003(2) 0.037(3) 0.009(2) _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 O8 1.424(3) . ? S1 O7 1.431(3) . ? S1 N1 1.637(3) . ? S1 C49 1.769(4) . ? O1 C1 1.397(4) . ? O1 C45 1.435(4) . ? O2 C47 1.419(4) . ? O2 C46 1.423(4) . ? O3 C58 1.427(4) . ? O3 C57 1.429(4) . ? O4 C20 1.395(4) . ? O4 C59 1.429(4) . ? O5 C13 1.390(4) . ? O5 C60 1.422(4) . ? O6 C27 1.388(4) . ? O6 C63 1.434(4) . ? N1 C48 1.475(5) . ? N1 C56 1.476(4) . ? C1 C6 1.390(5) . ? C1 C2 1.390(5) . ? C2 C3 1.388(5) . ? C2 C28 1.521(5) . ? C3 C4 1.390(5) . ? C3 H3 0.9300 . ? C4 C5 1.383(5) . ? C4 C29 1.533(5) . ? C5 C6 1.399(5) . ? C5 H5 0.9300 . ? C6 C7 1.512(5) . ? C7 C8 1.514(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.396(5) . ? C8 C9 1.398(5) . ? C9 C10 1.379(5) . ? C9 H9 0.9300 . ? C10 C11 1.407(5) . ? C10 C33 1.534(5) . ? C11 C12 1.389(5) . ? C11 H11 0.9300 . ? C12 C13 1.396(5) . ? C12 C14 1.518(5) . ? C14 C15 1.522(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.393(5) . ? C15 C20 1.395(5) . ? C16 C17 1.392(5) . ? C16 H16 0.9300 . ? C17 C18 1.388(5) . ? C17 C37 1.541(5) . ? C18 C19 1.394(5) . ? C18 H18 0.9300 . ? C19 C20 1.386(5) . ? C19 C21 1.515(5) . ? C21 C22 1.530(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.384(5) . ? C22 C27 1.398(5) . ? C23 C24 1.398(5) . ? C23 H23 0.9300 . ? C24 C25 1.378(5) . ? C24 C41 1.544(4) . ? C25 C26 1.392(5) . ? C25 H25 0.9300 . ? C26 C27 1.393(5) . ? C26 C28 1.521(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C31 1.531(6) . ? C29 C32 1.531(5) . ? C29 C30 1.542(5) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C36 1.525(5) . ? C33 C35 1.531(5) . ? C33 C34 1.536(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.527(5) . ? C37 C39 1.534(5) . ? C37 C40 1.544(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C43 1.528(5) . ? C41 C44 1.529(5) . ? C41 C42 1.533(5) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.517(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.530(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C54 1.382(5) . ? C49 C50 1.394(5) . ? C50 C51 1.380(6) . ? C50 H50 0.9300 . ? C51 C52 1.384(6) . ? C51 H51 0.9300 . ? C52 C53 1.389(6) . ? C52 C55 1.505(6) . ? C53 C54 1.382(5) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.520(5) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.489(5) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.514(5) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.493(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.505(5) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.527(6) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 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 O8 S1 O7 121.06(17) . . ? O8 S1 N1 106.71(17) . . ? O7 S1 N1 106.70(16) . . ? O8 S1 C49 107.04(18) . . ? O7 S1 C49 107.69(18) . . ? N1 S1 C49 106.88(16) . . ? C1 O1 C45 123.9(3) . . ? C47 O2 C46 112.2(3) . . ? C58 O3 C57 110.9(3) . . ? C20 O4 C59 114.9(3) . . ? C13 O5 C60 114.7(3) . . ? C27 O6 C63 113.2(3) . . ? C48 N1 C56 116.0(3) . . ? C48 N1 S1 117.3(2) . . ? C56 N1 S1 119.5(3) . . ? C6 C1 C2 120.5(3) . . ? C6 C1 O1 117.8(3) . . ? C2 C1 O1 120.4(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 C28 118.5(3) . . ? C1 C2 C28 123.0(3) . . ? C2 C3 C4 123.2(3) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C5 C4 C3 116.3(3) . . ? C5 C4 C29 122.9(3) . . ? C3 C4 C29 120.8(3) . . ? C4 C5 C6 122.7(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 118.5(3) . . ? C1 C6 C7 122.3(3) . . ? C5 C6 C7 119.0(3) . . ? C6 C7 C8 117.4(3) . . ? C6 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? C6 C7 H7B 108.0 . . ? C8 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? C13 C8 C9 117.9(3) . . ? C13 C8 C7 123.3(3) . . ? C9 C8 C7 118.7(3) . . ? C10 C9 C8 122.9(3) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C9 C10 C11 117.2(3) . . ? C9 C10 C33 122.8(3) . . ? C11 C10 C33 120.0(3) . . ? C12 C11 C10 122.2(3) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C13 118.4(3) . . ? C11 C12 C14 119.7(3) . . ? C13 C12 C14 121.8(3) . . ? O5 C13 C8 120.0(3) . . ? O5 C13 C12 118.7(3) . . ? C8 C13 C12 121.3(3) . . ? C12 C14 C15 119.0(3) . . ? C12 C14 H14A 107.6 . . ? C15 C14 H14A 107.6 . . ? C12 C14 H14B 107.6 . . ? C15 C14 H14B 107.6 . . ? H14A C14 H14B 107.0 . . ? C16 C15 C20 117.6(3) . . ? C16 C15 C14 119.4(3) . . ? C20 C15 C14 122.9(3) . . ? C17 C16 C15 123.5(3) . . ? C17 C16 H16 118.2 . . ? C15 C16 H16 118.2 . . ? C18 C17 C16 116.4(3) . . ? C18 C17 C37 122.6(3) . . ? C16 C17 C37 121.0(3) . . ? C17 C18 C19 122.5(3) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C20 C19 C18 118.8(3) . . ? C20 C19 C21 121.6(3) . . ? C18 C19 C21 119.4(3) . . ? C19 C20 O4 118.6(3) . . ? C19 C20 C15 121.1(3) . . ? O4 C20 C15 120.2(3) . . ? C19 C21 C22 121.2(3) . . ? C19 C21 H21A 107.0 . . ? C22 C21 H21A 107.0 . . ? C19 C21 H21B 107.0 . . ? C22 C21 H21B 107.0 . . ? H21A C21 H21B 106.8 . . ? C23 C22 C27 118.2(3) . . ? C23 C22 C21 117.9(3) . . ? C27 C22 C21 123.9(3) . . ? C22 C23 C24 122.7(3) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 116.6(3) . . ? C25 C24 C41 123.1(3) . . ? C23 C24 C41 120.2(3) . . ? C24 C25 C26 123.4(3) . . ? C24 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C25 C26 C27 117.7(3) . . ? C25 C26 C28 117.7(3) . . ? C27 C26 C28 124.6(3) . . ? O6 C27 C26 119.6(3) . . ? O6 C27 C22 119.2(3) . . ? C26 C27 C22 121.1(3) . . ? C2 C28 C26 120.1(3) . . ? C2 C28 H28A 107.3 . . ? C26 C28 H28A 107.3 . . ? C2 C28 H28B 107.3 . . ? C26 C28 H28B 107.3 . . ? H28A C28 H28B 106.9 . . ? C31 C29 C32 108.5(3) . . ? C31 C29 C4 108.3(3) . . ? C32 C29 C4 112.5(3) . . ? C31 C29 C30 109.5(3) . . ? C32 C29 C30 108.4(3) . . ? C4 C29 C30 109.7(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 109.4(3) . . ? C36 C33 C10 109.4(3) . . ? C35 C33 C10 109.1(3) . . ? C36 C33 C34 107.9(3) . . ? C35 C33 C34 108.4(3) . . ? C10 C33 C34 112.5(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 107.7(3) . . ? C38 C37 C17 112.8(3) . . ? C39 C37 C17 109.0(3) . . ? C38 C37 C40 108.6(3) . . ? C39 C37 C40 109.1(3) . . ? C17 C37 C40 109.5(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44 107.4(3) . . ? C43 C41 C42 109.8(3) . . ? C44 C41 C42 109.5(3) . . ? C43 C41 C24 108.7(3) . . ? C44 C41 C24 112.0(3) . . ? C42 C41 C24 109.5(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O1 C45 C46 103.0(3) . . ? O1 C45 H45A 111.2 . . ? C46 C45 H45A 111.2 . . ? O1 C45 H45B 111.2 . . ? C46 C45 H45B 111.2 . . ? H45A C45 H45B 109.1 . . ? O2 C46 C45 109.8(3) . . ? O2 C46 H46A 109.7 . . ? C45 C46 H46A 109.7 . . ? O2 C46 H46B 109.7 . . ? C45 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? O2 C47 C48 109.1(3) . . ? O2 C47 H47A 109.9 . . ? C48 C47 H47A 109.9 . . ? O2 C47 H47B 109.9 . . ? C48 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? N1 C48 C47 116.2(3) . . ? N1 C48 H48A 108.2 . . ? C47 C48 H48A 108.2 . . ? N1 C48 H48B 108.2 . . ? C47 C48 H48B 108.2 . . ? H48A C48 H48B 107.4 . . ? C54 C49 C50 119.7(4) . . ? C54 C49 S1 119.9(3) . . ? C50 C49 S1 120.3(3) . . ? C51 C50 C49 119.5(4) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C52 121.6(4) . . ? C50 C51 H51 119.2 . . ? C52 C51 H51 119.2 . . ? C51 C52 C53 118.1(4) . . ? C51 C52 C55 121.2(4) . . ? C53 C52 C55 120.7(4) . . ? C54 C53 C52 121.3(4) . . ? C54 C53 H53 119.3 . . ? C52 C53 H53 119.3 . . ? C49 C54 C53 119.8(4) . . ? C49 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N1 C56 C57 111.2(3) . . ? N1 C56 H56A 109.4 . . ? C57 C56 H56A 109.4 . . ? N1 C56 H56B 109.4 . . ? C57 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? O3 C57 C56 110.8(3) . . ? O3 C57 H57A 109.5 . . ? C56 C57 H57A 109.5 . . ? O3 C57 H57B 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? O3 C58 C59 110.0(3) . . ? O3 C58 H58A 109.7 . . ? C59 C58 H58A 109.7 . . ? O3 C58 H58B 109.7 . . ? C59 C58 H58B 109.7 . . ? H58A C58 H58B 108.2 . . ? O4 C59 C58 106.0(3) . . ? O4 C59 H59A 110.5 . . ? C58 C59 H59A 110.5 . . ? O4 C59 H59B 110.5 . . ? C58 C59 H59B 110.5 . . ? H59A C59 H59B 108.7 . . ? O5 C60 C61 107.7(3) . . ? O5 C60 H60A 110.2 . . ? C61 C60 H60A 110.2 . . ? O5 C60 H60B 110.2 . . ? C61 C60 H60B 110.2 . . ? H60A C60 H60B 108.5 . . ? C62 C61 C60 113.4(4) . . ? C62 C61 H61A 108.9 . . ? C60 C61 H61A 108.9 . . ? C62 C61 H61B 108.9 . . ? C60 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O6 C63 C64 108.5(3) . . ? O6 C63 H63A 110.0 . . ? C64 C63 H63A 110.0 . . ? O6 C63 H63B 110.0 . . ? C64 C63 H63B 110.0 . . ? H63A C63 H63B 108.4 . . ? C63 C64 C65 111.6(4) . . ? C63 C64 H64A 109.3 . . ? C65 C64 H64A 109.3 . . ? C63 C64 H64B 109.3 . . ? C65 C64 H64B 109.3 . . ? H64A C64 H64B 108.0 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.370 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.068 #===END data_compoun4 _database_code_depnum_ccdc_archive 'CCDC 749552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H71 N3 O10 S3' _chemical_formula_weight 1126.41 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.422(2) _cell_length_b 16.931(2) _cell_length_c 20.781(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.187(2) _cell_angle_gamma 90.00 _cell_volume 5753.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCKS _exptl_crystal_colour P21/c _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9275 _exptl_absorpt_correction_T_max 0.9556 _exptl_absorpt_process_detail 'BRUKER SADABS' _exptl_special_details ; ? ; _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 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28620 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10100 _reflns_number_gt 7634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0516P)^2^+11.5169P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10100 _refine_ls_number_parameters 717 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1328 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.2051 _refine_ls_wR_factor_gt 0.1916 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.19314(8) 0.92957(7) 0.21787(7) 0.0273(3) Uani 1 d . . . S2 S 0.07687(8) 0.70503(8) 0.05572(7) 0.0241(3) Uani 1 d . . . S3 S 0.19700(9) 0.49466(8) 0.26707(7) 0.0291(3) Uani 1 d . . . O1 O 0.57083(19) 0.77210(19) 0.49653(17) 0.0219(8) Uani 1 d . . . O2 O 0.45587(18) 0.84124(17) 0.31964(16) 0.0169(7) Uani 1 d . . . O3 O 0.2254(2) 0.9395(2) 0.2907(2) 0.0394(10) Uani 1 d . . . O4 O 0.1911(3) 0.9960(2) 0.1754(2) 0.0444(11) Uani 1 d . . . O5 O 0.0669(2) 0.7725(2) 0.01238(19) 0.0381(10) Uani 1 d . . . O6 O 0.0154(2) 0.6827(2) 0.08295(19) 0.0294(9) Uani 1 d . . . O7 O 0.1567(2) 0.4574(2) 0.20198(19) 0.0344(9) Uani 1 d . . . O8 O 0.2475(3) 0.4498(2) 0.3247(2) 0.0482(12) Uani 1 d . . . O9 O 0.45906(19) 0.61904(18) 0.36721(16) 0.0191(7) Uani 1 d . . . O10 O 0.61017(18) 0.72884(18) 0.33905(16) 0.0170(7) Uani 1 d . . . N1 N 0.2459(2) 0.8589(2) 0.1999(2) 0.0232(10) Uani 1 d . . . N2 N 0.1609(2) 0.7199(2) 0.1205(2) 0.0209(9) Uani 1 d . . . N3 N 0.2563(2) 0.5620(2) 0.2541(2) 0.0240(10) Uani 1 d . . . C1 C 0.4511(3) 0.6952(3) 0.4887(2) 0.0182(11) Uani 1 d . . . C2 C 0.3673(3) 0.6933(3) 0.4740(2) 0.0242(12) Uani 1 d . . . H2 H 0.3428 0.6468 0.4810 0.029 Uiso 1 calc R . . C3 C 0.3195(3) 0.7590(3) 0.4492(3) 0.0272(12) Uani 1 d . . . H3 H 0.2632 0.7569 0.4391 0.033 Uiso 1 calc R . . C4 C 0.3563(3) 0.8284(3) 0.4395(2) 0.0221(11) Uani 1 d . . . H4 H 0.3240 0.8724 0.4220 0.026 Uiso 1 calc R . . C5 C 0.4401(3) 0.8335(3) 0.4554(2) 0.0173(11) Uani 1 d . . . C6 C 0.4877(3) 0.7663(3) 0.4819(2) 0.0157(10) Uani 1 d . . . C7 C 0.4780(3) 0.9124(3) 0.4490(3) 0.0222(11) Uani 1 d . . . H7A H 0.5039 0.9328 0.4950 0.027 Uiso 1 calc R . . H7B H 0.4335 0.9481 0.4257 0.027 Uiso 1 calc R . . C8 C 0.5403(3) 0.9184(2) 0.4127(3) 0.0176(11) Uani 1 d . . . C9 C 0.6115(3) 0.9626(3) 0.4425(3) 0.0199(11) Uani 1 d . . . H9 H 0.6214 0.9863 0.4849 0.024 Uiso 1 calc R . . C10 C 0.6672(3) 0.9713(3) 0.4093(3) 0.0222(12) Uani 1 d . . . H10 H 0.7148 1.0001 0.4299 0.027 Uiso 1 calc R . . C11 C 0.6524(3) 0.9375(3) 0.3459(3) 0.0217(11) Uani 1 d . . . H11 H 0.6906 0.9434 0.3241 0.026 Uiso 1 calc R . . C12 C 0.5815(3) 0.8945(2) 0.3139(2) 0.0165(10) Uani 1 d . . . C13 C 0.5268(3) 0.8862(3) 0.3486(2) 0.0186(11) Uani 1 d . . . C14 C 0.5660(3) 0.8606(3) 0.2432(2) 0.0207(11) Uani 1 d . . . H14A H 0.6175 0.8614 0.2349 0.025 Uiso 1 calc R . . H14B H 0.5292 0.8962 0.2102 0.025 Uiso 1 calc R . . C15 C 0.5309(3) 0.7779(3) 0.2274(2) 0.0188(11) Uani 1 d . . . C16 C 0.4727(3) 0.7634(3) 0.1638(3) 0.0237(12) Uani 1 d . . . H16 H 0.4525 0.8052 0.1337 0.028 Uiso 1 calc R . . C17 C 0.4441(3) 0.6878(3) 0.1441(3) 0.0257(12) Uani 1 d . . . H17 H 0.4046 0.6788 0.1012 0.031 Uiso 1 calc R . . C18 C 0.4747(3) 0.6258(3) 0.1888(3) 0.0248(12) Uani 1 d . . . H18 H 0.4563 0.5749 0.1752 0.030 Uiso 1 calc R . . C19 C 0.5323(3) 0.6377(3) 0.2534(3) 0.0182(11) Uani 1 d . . . C20 C 0.5596(3) 0.7150(3) 0.2724(2) 0.0157(10) Uani 1 d . . . C21 C 0.5703(3) 0.5661(3) 0.2964(3) 0.0234(12) Uani 1 d . . . H21A H 0.6201 0.5538 0.2876 0.028 Uiso 1 calc R . . H21B H 0.5332 0.5221 0.2792 0.028 Uiso 1 calc R . . C22 C 0.5916(3) 0.5681(3) 0.3738(3) 0.0213(11) Uani 1 d . . . C23 C 0.6690(3) 0.5439(3) 0.4153(3) 0.0296(13) Uani 1 d . . . H23 H 0.7062 0.5262 0.3954 0.036 Uiso 1 calc R . . C24 C 0.6913(3) 0.5458(3) 0.4858(3) 0.0335(14) Uani 1 d . . . H24 H 0.7431 0.5289 0.5131 0.040 Uiso 1 calc R . . C25 C 0.6374(3) 0.5725(3) 0.5159(3) 0.0285(13) Uani 1 d . . . H25 H 0.6538 0.5749 0.5634 0.034 Uiso 1 calc R . . C26 C 0.5588(3) 0.5958(3) 0.4767(3) 0.0228(12) Uani 1 d . . . C27 C 0.5369(3) 0.5925(3) 0.4054(3) 0.0193(11) Uani 1 d . . . C28 C 0.4990(3) 0.6187(3) 0.5121(3) 0.0262(12) Uani 1 d . . . H28A H 0.5291 0.6230 0.5608 0.031 Uiso 1 calc R . . H28B H 0.4600 0.5760 0.5058 0.031 Uiso 1 calc R . . C29 C 0.6223(3) 0.7694(3) 0.5679(3) 0.0298(13) Uani 1 d . . . H29A H 0.6753 0.7482 0.5714 0.036 Uiso 1 calc R . . H29B H 0.5981 0.7339 0.5922 0.036 Uiso 1 calc R . . C30 C 0.6339(3) 0.8487(3) 0.6016(3) 0.0330(13) Uani 1 d . . . H30A H 0.5817 0.8681 0.6019 0.040 Uiso 1 calc R . . H30B H 0.6541 0.8856 0.5755 0.040 Uiso 1 calc R . . C31 C 0.6944(4) 0.8447(4) 0.6753(3) 0.0447(16) Uani 1 d . . . H31A H 0.6732 0.8104 0.7019 0.067 Uiso 1 calc R . . H31B H 0.7021 0.8967 0.6951 0.067 Uiso 1 calc R . . H31C H 0.7459 0.8246 0.6752 0.067 Uiso 1 calc R . . C32 C 0.3905(3) 0.8841(3) 0.2715(3) 0.0194(11) Uani 1 d . . . H32A H 0.4036 0.8976 0.2311 0.023 Uiso 1 calc R . . H32B H 0.3791 0.9323 0.2919 0.023 Uiso 1 calc R . . C33 C 0.3181(3) 0.8282(3) 0.2535(3) 0.0210(11) Uani 1 d . . . H33A H 0.3335 0.7783 0.2384 0.025 Uiso 1 calc R . . H33B H 0.3047 0.8180 0.2943 0.025 Uiso 1 calc R . . C34 C 0.2363(3) 0.8460(3) 0.1279(3) 0.0270(12) Uani 1 d . . . H34A H 0.2829 0.8686 0.1192 0.032 Uiso 1 calc R . . H34B H 0.1877 0.8736 0.0992 0.032 Uiso 1 calc R . . C35 C 0.2291(3) 0.7598(3) 0.1078(3) 0.0268(12) Uani 1 d . . . H35A H 0.2217 0.7556 0.0595 0.032 Uiso 1 calc R . . H35B H 0.2797 0.7331 0.1335 0.032 Uiso 1 calc R . . C36 C 0.1774(3) 0.6737(3) 0.1837(2) 0.0210(11) Uani 1 d . . . H36A H 0.1259 0.6550 0.1863 0.025 Uiso 1 calc R . . H36B H 0.2025 0.7078 0.2228 0.025 Uiso 1 calc R . . C37 C 0.2332(3) 0.6029(3) 0.1882(3) 0.0220(11) Uani 1 d . . . H37A H 0.2056 0.5659 0.1520 0.026 Uiso 1 calc R . . H37B H 0.2824 0.6207 0.1808 0.026 Uiso 1 calc R . . C38 C 0.3197(3) 0.5993(3) 0.3135(3) 0.0276(12) Uani 1 d . . . H38A H 0.3045 0.5934 0.3540 0.033 Uiso 1 calc R . . H38B H 0.3222 0.6553 0.3047 0.033 Uiso 1 calc R . . C39 C 0.4023(3) 0.5632(3) 0.3268(3) 0.0224(11) Uani 1 d . . . H39A H 0.4070 0.5136 0.3511 0.027 Uiso 1 calc R . . H39B H 0.4116 0.5536 0.2840 0.027 Uiso 1 calc R . . C40 C 0.0935(3) 0.8923(3) 0.1941(3) 0.0363(15) Uani 1 d . . . C41 C 0.0756(4) 0.8385(3) 0.2369(4) 0.0524(19) Uani 1 d . . . H41 H 0.1154 0.8215 0.2772 0.063 Uiso 1 calc R . . C42 C -0.0057(6) 0.8101(4) 0.2169(5) 0.072(3) Uani 1 d . . . H42 H -0.0202 0.7740 0.2445 0.087 Uiso 1 calc R . . C43 C -0.0642(5) 0.8362(5) 0.1558(6) 0.081(3) Uani 1 d . . . C44 C -0.0440(5) 0.8872(5) 0.1150(6) 0.083(3) Uani 1 d . . . H44 H -0.0828 0.9025 0.0736 0.099 Uiso 1 calc R . . C45 C 0.0339(4) 0.9166(4) 0.1344(4) 0.062(2) Uani 1 d . . . H45 H 0.0468 0.9537 0.1067 0.075 Uiso 1 calc R . . C46 C -0.1501(5) 0.8000(6) 0.1380(7) 0.148(6) Uani 1 d . . . H46A H -0.1877 0.8277 0.0999 0.223 Uiso 1 calc R . . H46B H -0.1676 0.8043 0.1769 0.223 Uiso 1 calc R . . H46C H -0.1485 0.7453 0.1263 0.223 Uiso 1 calc R . . C47 C 0.0956(3) 0.6229(3) 0.0104(2) 0.0228(12) Uani 1 d . . . C48 C 0.0894(3) 0.5472(3) 0.0339(3) 0.0235(12) Uani 1 d . . . H48 H 0.0709 0.5396 0.0705 0.028 Uiso 1 calc R . . C49 C 0.1109(3) 0.4833(3) 0.0024(3) 0.0267(12) Uani 1 d . . . H49 H 0.1077 0.4327 0.0188 0.032 Uiso 1 calc R . . C50 C 0.1371(3) 0.4925(3) -0.0528(3) 0.0300(13) Uani 1 d . . . C51 C 0.1415(3) 0.5686(4) -0.0760(3) 0.0391(15) Uani 1 d . . . H51 H 0.1593 0.5763 -0.1129 0.047 Uiso 1 calc R . . C52 C 0.1196(3) 0.6337(3) -0.0452(3) 0.0348(14) Uani 1 d . . . H52 H 0.1213 0.6842 -0.0623 0.042 Uiso 1 calc R . . C53 C 0.1619(3) 0.4226(4) -0.0848(3) 0.0465(17) Uani 1 d . . . H53A H 0.1821 0.4401 -0.1200 0.070 Uiso 1 calc R . . H53B H 0.1156 0.3887 -0.1046 0.070 Uiso 1 calc R . . H53C H 0.2042 0.3941 -0.0505 0.070 Uiso 1 calc R . . C54 C 0.1215(3) 0.5417(3) 0.2921(3) 0.0299(13) Uani 1 d . . . C55 C 0.1402(4) 0.5750(4) 0.3565(3) 0.0465(17) Uani 1 d . . . H55 H 0.1934 0.5716 0.3876 0.056 Uiso 1 calc R . . C56 C 0.0815(4) 0.6128(4) 0.3752(4) 0.055(2) Uani 1 d . . . H56 H 0.0953 0.6346 0.4188 0.067 Uiso 1 calc R . . C57 C 0.0024(4) 0.6190(4) 0.3304(4) 0.0516(18) Uani 1 d . . . C58 C -0.0169(4) 0.5840(4) 0.2667(3) 0.0485(17) Uani 1 d . . . H58 H -0.0706 0.5860 0.2366 0.058 Uiso 1 calc R . . C59 C 0.0410(4) 0.5466(4) 0.2468(3) 0.0394(15) Uani 1 d . . . H59 H 0.0267 0.5245 0.2033 0.047 Uiso 1 calc R . . C60 C -0.0625(5) 0.6596(5) 0.3500(4) 0.079(3) Uani 1 d . . . H60A H -0.0668 0.6351 0.3903 0.119 Uiso 1 calc R . . H60B H -0.1139 0.6554 0.3131 0.119 Uiso 1 calc R . . H60C H -0.0485 0.7143 0.3592 0.119 Uiso 1 calc R . . C61 C 0.6960(3) 0.7302(3) 0.3525(3) 0.0241(12) Uani 1 d . . . H61A H 0.7093 0.7693 0.3239 0.029 Uiso 1 calc R . . H61B H 0.7146 0.6789 0.3429 0.029 Uiso 1 calc R . . C62 C 0.7367(3) 0.7509(3) 0.4276(3) 0.0257(12) Uani 1 d . . . H62A H 0.7185 0.8027 0.4361 0.031 Uiso 1 calc R . . H62B H 0.7204 0.7130 0.4554 0.031 Uiso 1 calc R . . C63 C 0.8277(4) 0.7509(4) 0.4479(4) 0.058(2) Uani 1 d . . . H63A H 0.8464 0.6984 0.4439 0.088 Uiso 1 calc R . . H63B H 0.8516 0.7685 0.4945 0.088 Uiso 1 calc R . . H63C H 0.8438 0.7858 0.4184 0.088 Uiso 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 0.0234(7) 0.0221(7) 0.0375(9) -0.0037(6) 0.0118(7) -0.0025(6) S2 0.0190(7) 0.0271(7) 0.0199(7) 0.0018(6) -0.0010(6) -0.0014(5) S3 0.0395(8) 0.0221(7) 0.0202(7) 0.0014(6) 0.0031(6) -0.0028(6) O1 0.0165(18) 0.0235(18) 0.026(2) -0.0008(15) 0.0071(16) 0.0000(14) O2 0.0185(17) 0.0140(16) 0.0171(18) -0.0002(14) 0.0047(15) -0.0052(14) O3 0.033(2) 0.050(3) 0.036(2) -0.016(2) 0.013(2) 0.0001(19) O4 0.058(3) 0.022(2) 0.061(3) 0.004(2) 0.030(2) -0.0043(19) O5 0.045(2) 0.033(2) 0.023(2) 0.0079(17) -0.0050(19) -0.0004(18) O6 0.0172(19) 0.033(2) 0.035(2) -0.0009(17) 0.0055(17) -0.0027(16) O7 0.042(2) 0.031(2) 0.027(2) -0.0113(17) 0.0080(19) -0.0104(18) O8 0.069(3) 0.031(2) 0.032(2) 0.0130(19) 0.001(2) 0.005(2) O9 0.0208(18) 0.0157(17) 0.0168(18) -0.0018(14) 0.0015(15) 0.0008(14) O10 0.0170(17) 0.0193(17) 0.0136(17) -0.0037(14) 0.0039(15) -0.0026(14) N1 0.016(2) 0.027(2) 0.024(2) -0.0043(19) 0.003(2) -0.0028(18) N2 0.018(2) 0.028(2) 0.016(2) 0.0037(18) 0.0051(19) -0.0036(18) N3 0.022(2) 0.023(2) 0.019(2) -0.0012(18) -0.0032(19) 0.0028(18) C1 0.022(3) 0.024(3) 0.009(2) -0.004(2) 0.006(2) -0.008(2) C2 0.027(3) 0.029(3) 0.018(3) -0.005(2) 0.010(2) -0.016(2) C3 0.019(3) 0.043(3) 0.021(3) -0.003(3) 0.009(2) -0.004(2) C4 0.024(3) 0.026(3) 0.018(3) -0.002(2) 0.008(2) 0.005(2) C5 0.019(3) 0.022(3) 0.010(2) -0.008(2) 0.004(2) -0.001(2) C6 0.019(3) 0.019(2) 0.009(2) -0.005(2) 0.005(2) -0.005(2) C7 0.028(3) 0.017(3) 0.025(3) -0.005(2) 0.013(2) 0.003(2) C8 0.021(3) 0.007(2) 0.025(3) 0.003(2) 0.009(2) 0.003(2) C9 0.027(3) 0.010(2) 0.019(3) -0.002(2) 0.003(2) 0.000(2) C10 0.013(3) 0.017(3) 0.029(3) 0.002(2) -0.001(2) -0.003(2) C11 0.023(3) 0.013(2) 0.032(3) 0.007(2) 0.013(2) 0.000(2) C12 0.021(3) 0.007(2) 0.023(3) 0.004(2) 0.010(2) 0.0002(19) C13 0.019(3) 0.013(2) 0.021(3) 0.000(2) 0.004(2) -0.001(2) C14 0.024(3) 0.021(3) 0.021(3) 0.002(2) 0.013(2) 0.001(2) C15 0.019(3) 0.022(3) 0.019(3) 0.000(2) 0.010(2) -0.001(2) C16 0.030(3) 0.028(3) 0.017(3) 0.002(2) 0.012(2) 0.004(2) C17 0.026(3) 0.039(3) 0.012(3) -0.008(2) 0.007(2) -0.010(2) C18 0.028(3) 0.024(3) 0.026(3) -0.008(2) 0.013(3) -0.008(2) C19 0.019(3) 0.019(3) 0.023(3) -0.006(2) 0.016(2) -0.001(2) C20 0.016(2) 0.021(3) 0.011(2) -0.005(2) 0.005(2) 0.001(2) C21 0.029(3) 0.017(3) 0.027(3) -0.009(2) 0.013(3) -0.003(2) C22 0.028(3) 0.007(2) 0.031(3) 0.000(2) 0.013(3) 0.004(2) C23 0.028(3) 0.021(3) 0.043(4) 0.002(3) 0.016(3) 0.004(2) C24 0.024(3) 0.019(3) 0.047(4) 0.011(3) -0.001(3) 0.008(2) C25 0.033(3) 0.022(3) 0.023(3) 0.011(2) -0.001(3) 0.001(2) C26 0.028(3) 0.012(2) 0.024(3) 0.004(2) 0.003(2) -0.007(2) C27 0.021(3) 0.007(2) 0.027(3) 0.004(2) 0.005(2) 0.000(2) C28 0.039(3) 0.023(3) 0.016(3) 0.002(2) 0.008(3) -0.003(2) C29 0.031(3) 0.029(3) 0.030(3) 0.000(2) 0.010(3) -0.004(2) C30 0.035(3) 0.040(3) 0.024(3) 0.000(3) 0.010(3) -0.009(3) C31 0.045(4) 0.064(4) 0.027(3) -0.008(3) 0.014(3) -0.017(3) C32 0.018(3) 0.015(2) 0.023(3) 0.001(2) 0.005(2) -0.001(2) C33 0.018(3) 0.025(3) 0.020(3) 0.000(2) 0.006(2) -0.008(2) C34 0.024(3) 0.029(3) 0.027(3) 0.005(2) 0.008(3) -0.008(2) C35 0.031(3) 0.029(3) 0.019(3) 0.000(2) 0.007(3) 0.000(2) C36 0.019(3) 0.024(3) 0.018(3) 0.000(2) 0.004(2) -0.001(2) C37 0.021(3) 0.024(3) 0.021(3) 0.000(2) 0.007(2) 0.004(2) C38 0.027(3) 0.027(3) 0.023(3) -0.008(2) 0.002(2) 0.002(2) C39 0.022(3) 0.019(3) 0.024(3) 0.001(2) 0.005(2) -0.003(2) C40 0.024(3) 0.027(3) 0.059(4) -0.008(3) 0.017(3) 0.003(2) C41 0.053(4) 0.031(3) 0.095(6) -0.003(4) 0.054(4) -0.002(3) C42 0.088(6) 0.033(4) 0.129(8) -0.027(5) 0.081(7) -0.020(4) C43 0.043(5) 0.062(6) 0.146(10) -0.052(6) 0.041(6) 0.009(4) C44 0.040(5) 0.070(6) 0.119(8) -0.037(6) 0.002(5) -0.001(4) C45 0.033(4) 0.052(4) 0.081(6) -0.007(4) -0.005(4) 0.008(3) C46 0.048(5) 0.107(8) 0.307(17) -0.130(10) 0.082(8) -0.034(5) C47 0.016(3) 0.034(3) 0.014(3) -0.003(2) -0.001(2) -0.009(2) C48 0.014(3) 0.039(3) 0.015(3) 0.001(2) 0.003(2) -0.006(2) C49 0.017(3) 0.030(3) 0.033(3) -0.008(2) 0.008(2) -0.010(2) C50 0.014(3) 0.047(4) 0.027(3) -0.005(3) 0.004(2) -0.002(2) C51 0.036(3) 0.066(4) 0.020(3) -0.004(3) 0.015(3) -0.011(3) C52 0.039(3) 0.038(3) 0.029(3) 0.001(3) 0.015(3) -0.015(3) C53 0.028(3) 0.073(5) 0.040(4) -0.020(3) 0.013(3) 0.003(3) C54 0.042(3) 0.026(3) 0.024(3) 0.004(2) 0.013(3) -0.009(3) C55 0.057(4) 0.056(4) 0.027(3) -0.005(3) 0.016(3) -0.028(3) C56 0.061(5) 0.072(5) 0.047(4) -0.027(4) 0.036(4) -0.030(4) C57 0.053(4) 0.066(5) 0.049(4) -0.018(4) 0.035(4) -0.029(4) C58 0.031(3) 0.073(5) 0.044(4) -0.014(4) 0.017(3) -0.017(3) C59 0.045(4) 0.051(4) 0.022(3) -0.007(3) 0.012(3) -0.018(3) C60 0.074(5) 0.102(7) 0.084(6) -0.048(5) 0.056(5) -0.036(5) C61 0.023(3) 0.024(3) 0.025(3) -0.007(2) 0.007(2) 0.004(2) C62 0.020(3) 0.029(3) 0.024(3) -0.004(2) 0.003(2) 0.003(2) C63 0.035(4) 0.083(5) 0.046(4) -0.021(4) 0.000(3) -0.004(4) _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 O4 1.422(4) . ? S1 O3 1.432(4) . ? S1 N1 1.628(4) . ? S1 C40 1.750(6) . ? S2 O6 1.425(4) . ? S2 O5 1.428(4) . ? S2 N2 1.630(4) . ? S2 C47 1.772(5) . ? S3 O8 1.435(4) . ? S3 O7 1.437(4) . ? S3 N3 1.622(4) . ? S3 C54 1.763(6) . ? O1 C6 1.377(5) . ? O1 C29 1.446(6) . ? O2 C13 1.398(5) . ? O2 C32 1.428(5) . ? O9 C27 1.389(5) . ? O9 C39 1.415(5) . ? O10 C20 1.381(5) . ? O10 C61 1.424(6) . ? N1 C33 1.458(6) . ? N1 C34 1.464(6) . ? N2 C35 1.467(6) . ? N2 C36 1.470(6) . ? N3 C37 1.461(6) . ? N3 C38 1.483(6) . ? C1 C2 1.385(7) . ? C1 C6 1.392(6) . ? C1 C28 1.525(7) . ? C2 C3 1.379(7) . ? C3 C4 1.385(7) . ? C4 C5 1.384(7) . ? C5 C6 1.404(6) . ? C5 C7 1.515(7) . ? C7 C8 1.524(6) . ? C8 C13 1.381(7) . ? C8 C9 1.398(6) . ? C9 C10 1.376(7) . ? C10 C11 1.378(7) . ? C11 C12 1.390(6) . ? C12 C13 1.387(6) . ? C12 C14 1.513(7) . ? C14 C15 1.518(6) . ? C15 C16 1.382(7) . ? C15 C20 1.391(6) . ? C16 C17 1.383(7) . ? C17 C18 1.381(7) . ? C18 C19 1.385(7) . ? C19 C20 1.402(6) . ? C19 C21 1.517(7) . ? C21 C22 1.520(7) . ? C22 C23 1.388(7) . ? C22 C27 1.394(7) . ? C23 C24 1.382(8) . ? C24 C25 1.371(8) . ? C25 C26 1.387(7) . ? C26 C27 1.397(7) . ? C26 C28 1.519(7) . ? C29 C30 1.496(7) . ? C30 C31 1.532(8) . ? C32 C33 1.517(6) . ? C34 C35 1.511(7) . ? C36 C37 1.525(6) . ? C38 C39 1.499(7) . ? C40 C45 1.379(9) . ? C40 C41 1.382(9) . ? C41 C42 1.415(10) . ? C42 C43 1.398(12) . ? C43 C44 1.339(13) . ? C43 C46 1.540(11) . ? C44 C45 1.369(10) . ? C47 C52 1.370(7) . ? C47 C48 1.390(7) . ? C48 C49 1.381(7) . ? C49 C50 1.384(7) . ? C50 C51 1.387(8) . ? C50 C53 1.492(8) . ? C51 C52 1.392(8) . ? C54 C55 1.384(8) . ? C54 C59 1.395(8) . ? C55 C56 1.373(9) . ? C56 C57 1.375(9) . ? C57 C58 1.380(9) . ? C57 C60 1.495(9) . ? C58 C59 1.370(8) . ? C61 C62 1.516(7) . ? C62 C63 1.494(8) . ? 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 O4 S1 O3 118.7(2) . . ? O4 S1 N1 109.5(2) . . ? O3 S1 N1 106.4(2) . . ? O4 S1 C40 107.5(3) . . ? O3 S1 C40 109.2(3) . . ? N1 S1 C40 104.7(2) . . ? O6 S2 O5 121.2(2) . . ? O6 S2 N2 107.3(2) . . ? O5 S2 N2 106.0(2) . . ? O6 S2 C47 107.7(2) . . ? O5 S2 C47 107.3(2) . . ? N2 S2 C47 106.4(2) . . ? O8 S3 O7 120.9(2) . . ? O8 S3 N3 105.6(2) . . ? O7 S3 N3 106.5(2) . . ? O8 S3 C54 107.3(3) . . ? O7 S3 C54 107.7(3) . . ? N3 S3 C54 108.3(2) . . ? C6 O1 C29 117.2(4) . . ? C13 O2 C32 113.4(3) . . ? C27 O9 C39 117.9(3) . . ? C20 O10 C61 117.6(4) . . ? C33 N1 C34 119.4(4) . . ? C33 N1 S1 119.7(3) . . ? C34 N1 S1 118.0(3) . . ? C35 N2 C36 119.0(4) . . ? C35 N2 S2 118.4(3) . . ? C36 N2 S2 119.9(3) . . ? C37 N3 C38 117.6(4) . . ? C37 N3 S3 120.2(3) . . ? C38 N3 S3 119.7(3) . . ? C2 C1 C6 118.8(4) . . ? C2 C1 C28 118.0(4) . . ? C6 C1 C28 123.2(4) . . ? C3 C2 C1 121.2(5) . . ? C2 C3 C4 119.2(5) . . ? C5 C4 C3 121.5(5) . . ? C4 C5 C6 118.3(4) . . ? C4 C5 C7 119.3(4) . . ? C6 C5 C7 122.2(4) . . ? O1 C6 C1 121.5(4) . . ? O1 C6 C5 117.6(4) . . ? C1 C6 C5 120.8(4) . . ? C5 C7 C8 120.5(4) . . ? C13 C8 C9 117.9(4) . . ? C13 C8 C7 122.5(4) . . ? C9 C8 C7 119.5(4) . . ? C10 C9 C8 120.5(5) . . ? C9 C10 C11 120.2(4) . . ? C10 C11 C12 121.1(5) . . ? C13 C12 C11 117.5(4) . . ? C13 C12 C14 122.9(4) . . ? C11 C12 C14 119.6(4) . . ? C8 C13 C12 122.9(4) . . ? C8 C13 O2 117.5(4) . . ? C12 C13 O2 119.6(4) . . ? C12 C14 C15 118.9(4) . . ? C16 C15 C20 118.8(4) . . ? C16 C15 C14 118.5(4) . . ? C20 C15 C14 122.4(4) . . ? C15 C16 C17 121.2(5) . . ? C18 C17 C16 119.1(5) . . ? C17 C18 C19 121.6(5) . . ? C18 C19 C20 118.1(5) . . ? C18 C19 C21 118.5(4) . . ? C20 C19 C21 122.9(4) . . ? O10 C20 C15 120.1(4) . . ? O10 C20 C19 118.6(4) . . ? C15 C20 C19 121.1(4) . . ? C19 C21 C22 120.2(4) . . ? C23 C22 C27 118.0(5) . . ? C23 C22 C21 118.7(5) . . ? C27 C22 C21 123.2(4) . . ? C24 C23 C22 120.6(5) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C26 121.2(5) . . ? C25 C26 C27 117.7(5) . . ? C25 C26 C28 119.4(5) . . ? C27 C26 C28 122.8(4) . . ? O9 C27 C22 121.2(4) . . ? O9 C27 C26 116.6(4) . . ? C22 C27 C26 122.1(5) . . ? C26 C28 C1 117.0(4) . . ? O1 C29 C30 112.8(4) . . ? C29 C30 C31 111.3(5) . . ? O2 C32 C33 104.4(4) . . ? N1 C33 C32 112.9(4) . . ? N1 C34 C35 113.3(4) . . ? N2 C35 C34 112.9(4) . . ? N2 C36 C37 113.4(4) . . ? N3 C37 C36 113.2(4) . . ? N3 C38 C39 111.9(4) . . ? O9 C39 C38 105.5(4) . . ? C45 C40 C41 120.5(6) . . ? C45 C40 S1 120.8(5) . . ? C41 C40 S1 118.7(5) . . ? C40 C41 C42 117.5(7) . . ? C43 C42 C41 120.1(8) . . ? C44 C43 C42 120.7(8) . . ? C44 C43 C46 123.4(11) . . ? C42 C43 C46 115.8(11) . . ? C43 C44 C45 119.9(9) . . ? C44 C45 C40 121.2(8) . . ? C52 C47 C48 120.3(5) . . ? C52 C47 S2 120.6(4) . . ? C48 C47 S2 119.1(4) . . ? C49 C48 C47 119.3(5) . . ? C48 C49 C50 121.7(5) . . ? C49 C50 C51 117.8(5) . . ? C49 C50 C53 120.7(5) . . ? C51 C50 C53 121.5(5) . . ? C50 C51 C52 121.3(5) . . ? C47 C52 C51 119.5(5) . . ? C55 C54 C59 118.3(6) . . ? C55 C54 S3 121.2(5) . . ? C59 C54 S3 120.5(4) . . ? C56 C55 C54 120.9(6) . . ? C55 C56 C57 120.9(6) . . ? C56 C57 C58 118.2(6) . . ? C56 C57 C60 121.7(6) . . ? C58 C57 C60 120.1(7) . . ? C59 C58 C57 121.8(6) . . ? C58 C59 C54 119.8(5) . . ? O10 C61 C62 107.0(4) . . ? C63 C62 C61 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.455 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.077