# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Bryce, M.' 'Batsanov, A.' 'Moss, Kathryn' 'Helen, Vaughan' 'Dias, Fernando' 'Kamtekar, Kiran' 'Li, Haiying' 'Monkman, Andrew' _publ_contact_author_name 'Bryce, M.' _publ_contact_author_email m.r.bryce@durham.ac.uk _publ_section_title ; The interplay of conformation and photophysical properties in deep-blue fluorescent oligomers ; # Attachment '- Li.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 768385' #TrackingRef '- Li.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,7-bis(9,9-dihexylfluorene-2-yl)-2,8-difluorodibenzothiophene-S,S-dioxide ; _chemical_name_common ? _chemical_melting_point 463.0(3) _chemical_formula_moiety 'C62 H70 F2 O2 S' _chemical_formula_sum 'C62 H70 F2 O2 S' _chemical_formula_weight 917.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 18.901(5) _cell_length_b 19.072(5) _cell_length_c 29.787(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.21(2) _cell_angle_gamma 90.00 _cell_volume 10310(5) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4044 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.95 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 runs of narrow-frame \w-scans (scan width 0.3\% \w, 45s exposure), every run at a different \f angle. Crystal to detector distance 4.84 cm. Weak diffraction: mean I/\s(I)=2.6. 16743 unique reflections after merging Friedel equivalents. ; _diffrn_ambient_temperature 120(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 6000 CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 84802 _diffrn_reflns_av_R_equivalents 0.2082 _diffrn_reflns_av_sigmaI/netI 0.2754 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.71 _diffrn_reflns_theta_max 24.00 _reflns_number_total 32367 _reflns_number_gt 13682 _reflns_threshold_expression I>2\s(I) _reflns_Friedel_coverage 0.93 _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT version 6.45A (Bruker, 2003)' _computing_data_reduction 'SAINT version 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _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. C(27D) and C(28D) with attached hydrogens are disordered between 2 positions with occupancies 0.6 and 0.4, C(53) and C(54) with attached hydrogens are disordered between 2 positions with occupancies 0.55 and 0.45. The minor carbon positions are labelled E. ; _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^)+(0.1436P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 0.27(17) _refine_ls_number_reflns 32367 _refine_ls_number_parameters 1109 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.2490 _refine_ls_R_factor_gt 0.1192 _refine_ls_wR_factor_ref 0.3324 _refine_ls_wR_factor_gt 0.2630 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1A S 0.54064(17) 0.30199(14) 0.17648(10) 0.0261(7) Uani 1 1 d . . . F1A F 0.5893(3) 0.5346(3) 0.3062(2) 0.0324(16) Uiso 1 1 d . . . F2A F 0.3913(3) 0.5185(3) 0.0475(2) 0.0308(16) Uiso 1 1 d . . . O1A O 0.6053(4) 0.2737(4) 0.1675(3) 0.030(2) Uiso 1 1 d . . . O2A O 0.4885(4) 0.2532(4) 0.1857(3) 0.032(2) Uiso 1 1 d . . . C1A C 0.5953(6) 0.3566(7) 0.2665(4) 0.028(3) Uiso 1 1 d . . . H1A H 0.6104 0.3108 0.2776 0.034 Uiso 1 1 d R . . C2A C 0.6065(6) 0.4129(6) 0.2975(4) 0.022(3) Uiso 1 1 d . . . C3A C 0.5803(6) 0.4771(6) 0.2776(4) 0.021(3) Uiso 1 1 d . . . C4A C 0.5443(6) 0.4884(6) 0.2321(4) 0.025(3) Uiso 1 1 d . . . H4A H 0.5269 0.5337 0.2212 0.031 Uiso 1 1 d R . . C5A C 0.4594(5) 0.4805(6) 0.1208(3) 0.019(3) Uiso 1 1 d . . . H5A H 0.4586 0.5271 0.1319 0.023 Uiso 1 1 d R . . C6A C 0.4260(6) 0.4655(6) 0.0756(4) 0.021(3) Uiso 1 1 d . . . C7A C 0.4235(6) 0.3982(6) 0.0570(4) 0.022(3) Uiso 1 1 d . . . C8A C 0.4627(6) 0.3463(6) 0.0873(4) 0.026(3) Uiso 1 1 d . . . H8A H 0.4653 0.3002 0.0758 0.031 Uiso 1 1 d R . . C9A C 0.4966(6) 0.3612(6) 0.1328(4) 0.026(3) Uiso 1 1 d . . . C10A C 0.4947(6) 0.4295(6) 0.1503(4) 0.020(3) Uiso 1 1 d . . . C11A C 0.5340(5) 0.4312(5) 0.2014(3) 0.015(2) Uiso 1 1 d . . . C12A C 0.5622(5) 0.3678(6) 0.2203(3) 0.019(2) Uiso 1 1 d . . . C13A C 0.6412(6) 0.4028(6) 0.3488(4) 0.024(3) Uiso 1 1 d . . . C14A C 0.6243(6) 0.3407(6) 0.3690(4) 0.031(3) Uiso 1 1 d . . . H14A H 0.5919 0.3074 0.3502 0.038 Uiso 1 1 d R . . C15A C 0.6544(6) 0.3278(6) 0.4159(4) 0.022(3) Uiso 1 1 d . . . H15 H 0.6461 0.2837 0.4284 0.027 Uiso 1 1 d R . . C16A C 0.6976(6) 0.3783(6) 0.4453(4) 0.029(3) Uiso 1 1 d . . . C17A C 0.7335(6) 0.3790(6) 0.4948(4) 0.029(3) Uiso 1 1 d . . . C18A C 0.7342(7) 0.3280(7) 0.5287(4) 0.037(3) Uiso 1 1 d . . . H18A H 0.7096 0.2843 0.5212 0.044 Uiso 1 1 d R . . C19A C 0.7742(6) 0.3451(7) 0.5753(4) 0.037(3) Uiso 1 1 d . . . H19A H 0.7744 0.3126 0.5995 0.045 Uiso 1 1 d R . . C20A C 0.8134(6) 0.4080(6) 0.5865(4) 0.033(3) Uiso 1 1 d . . . H20A H 0.8407 0.4174 0.6179 0.040 Uiso 1 1 d R . . C21A C 0.8118(7) 0.4558(7) 0.5518(4) 0.038(3) Uiso 1 1 d . . . H21A H 0.8376 0.4989 0.5591 0.045 Uiso 1 1 d R . . C22A C 0.7712(6) 0.4404(6) 0.5053(4) 0.027(3) Uiso 1 1 d . . . C23A C 0.7623(6) 0.4893(6) 0.4628(4) 0.027(3) Uiso 1 1 d . . . C24A C 0.7134(6) 0.4396(6) 0.4246(4) 0.024(3) Uiso 1 1 d . . . C25A C 0.6862(6) 0.4524(6) 0.3764(4) 0.024(3) Uiso 1 1 d . . . H25A H 0.6991 0.4939 0.3629 0.029 Uiso 1 1 d R . . C26A C 0.8352(7) 0.5034(7) 0.4544(4) 0.039(3) Uiso 1 1 d . . . H261 H 0.8658 0.5299 0.4815 0.047 Uiso 1 1 d R . . H262 H 0.8270 0.5342 0.4267 0.047 Uiso 1 1 d R . . C27A C 0.8792(7) 0.4397(7) 0.4466(5) 0.048(4) Uiso 1 1 d . . . H271 H 0.8620 0.4257 0.4133 0.057 Uiso 1 1 d R . . H272 H 0.8697 0.4001 0.4656 0.057 Uiso 1 1 d R . . C28A C 0.9631(7) 0.4535(8) 0.4592(5) 0.054(4) Uiso 1 1 d . . . H281 H 0.9805 0.4631 0.4932 0.065 Uiso 1 1 d R . . H282 H 0.9715 0.4965 0.4428 0.065 Uiso 1 1 d R . . C29A C 1.0115(8) 0.3945(8) 0.4482(5) 0.057(4) Uiso 1 1 d . . . H291 H 1.0639 0.4034 0.4646 0.068 Uiso 1 1 d R . . H292 H 0.9974 0.3492 0.4595 0.068 Uiso 1 1 d R . . C30A C 1.0020(7) 0.3895(7) 0.3966(5) 0.051(4) Uiso 1 1 d . . . H301 H 1.0206 0.4333 0.3860 0.062 Uiso 1 1 d R . . H302 H 0.9488 0.3857 0.3801 0.062 Uiso 1 1 d R . . C31A C 1.0440(8) 0.3252(8) 0.3828(5) 0.064(4) Uiso 1 1 d . . . H311 H 1.0270 0.3185 0.3489 0.096 Uiso 1 1 d R . . H312 H 1.0337 0.2829 0.3985 0.096 Uiso 1 1 d R . . H313 H 1.0971 0.3343 0.3923 0.096 Uiso 1 1 d R . . C32A C 0.7237(7) 0.5570(7) 0.4692(4) 0.039(3) Uiso 1 1 d . . . H321 H 0.6843 0.5453 0.4841 0.046 Uiso 1 1 d R . . H322 H 0.7600 0.5867 0.4916 0.046 Uiso 1 1 d R . . C33A C 0.6902(7) 0.6011(7) 0.4258(4) 0.046(4) Uiso 1 1 d . . . H331 H 0.6451 0.5773 0.4069 0.055 Uiso 1 1 d R . . H332 H 0.7252 0.6038 0.4066 0.055 Uiso 1 1 d R . . C34A C 0.6691(7) 0.6763(6) 0.4373(4) 0.041(3) Uiso 1 1 d . . . H341 H 0.6334 0.6969 0.4096 0.049 Uiso 1 1 d R . . H342 H 0.6456 0.6746 0.4631 0.049 Uiso 1 1 d R . . C35A C 0.7383(7) 0.7226(7) 0.4508(4) 0.039(3) Uiso 1 1 d . . . H351 H 0.7633 0.7218 0.4257 0.047 Uiso 1 1 d R . . H352 H 0.7727 0.7033 0.4795 0.047 Uiso 1 1 d R . . C36A C 0.7187(7) 0.7991(7) 0.4609(4) 0.039(3) Uiso 1 1 d . . . H361 H 0.6832 0.8180 0.4325 0.047 Uiso 1 1 d R . . H362 H 0.6950 0.8001 0.4866 0.047 Uiso 1 1 d R . . C37A C 0.7864(8) 0.8450(9) 0.4730(5) 0.068(5) Uiso 1 1 d . . . H371 H 0.8106 0.8434 0.4479 0.101 Uiso 1 1 d R . . H372 H 0.8205 0.8281 0.5021 0.101 Uiso 1 1 d R . . H373 H 0.7721 0.8934 0.4773 0.101 Uiso 1 1 d R . . C38A C 0.3837(6) 0.3832(6) 0.0065(4) 0.027(3) Uiso 1 1 d . . . C39A C 0.4191(6) 0.3336(6) -0.0169(4) 0.025(3) Uiso 1 1 d . . . H39A H 0.4668 0.3162 -0.0015 0.030 Uiso 1 1 d R . . C40A C 0.3838(6) 0.3108(7) -0.0617(4) 0.031(3) Uiso 1 1 d . . . H40A H 0.4073 0.2796 -0.0778 0.037 Uiso 1 1 d R . . C41A C 0.3145(6) 0.3350(6) -0.0821(4) 0.023(3) Uiso 1 1 d . . . C42A C 0.2607(6) 0.3195(6) -0.1279(4) 0.028(3) Uiso 1 1 d . . . C43A C 0.2680(7) 0.2736(7) -0.1636(4) 0.035(3) Uiso 1 1 d . . . H43A H 0.3127 0.2487 -0.1605 0.041 Uiso 1 1 d R . . C44A C 0.2097(7) 0.2660(8) -0.2036(5) 0.046(4) Uiso 1 1 d . . . H44A H 0.2139 0.2360 -0.2282 0.055 Uiso 1 1 d R . . C45A C 0.1457(7) 0.3030(7) -0.2079(4) 0.043(3) Uiso 1 1 d . . . H45A H 0.1067 0.2985 -0.2359 0.052 Uiso 1 1 d R . . C46A C 0.1349(7) 0.3461(8) -0.1716(4) 0.046(4) Uiso 1 1 d . . . H46A H 0.0893 0.3689 -0.1741 0.056 Uiso 1 1 d R . . C47A C 0.1962(6) 0.3544(6) -0.1321(4) 0.028(3) Uiso 1 1 d . . . C48A C 0.2019(6) 0.3998(6) -0.0888(4) 0.028(3) Uiso 1 1 d . . . C49A C 0.2775(6) 0.3830(6) -0.0600(4) 0.021(3) Uiso 1 1 d . . . C50A C 0.3173(6) 0.4055(6) -0.0153(4) 0.027(3) Uiso 1 1 d . . . H50A H 0.2951 0.4390 0.0001 0.032 Uiso 1 1 d R . . C51A C 0.1909(7) 0.4779(7) -0.1027(4) 0.035(3) Uiso 1 1 d . . . H511 H 0.1406 0.4843 -0.1238 0.042 Uiso 1 1 d R . . H512 H 0.1947 0.5061 -0.0742 0.042 Uiso 1 1 d R . . C52A C 0.2475(7) 0.5060(7) -0.1273(5) 0.046(4) Uiso 1 1 d . . . H521 H 0.2962 0.5090 -0.1039 0.055 Uiso 1 1 d R . . H522 H 0.2517 0.4714 -0.1512 0.055 Uiso 1 1 d R . . C53A C 0.2295(7) 0.5773(7) -0.1506(4) 0.040(3) Uiso 1 1 d . . . H531 H 0.2627 0.5847 -0.1707 0.048 Uiso 1 1 d R . . H532 H 0.1785 0.5756 -0.1714 0.048 Uiso 1 1 d R . . C54A C 0.2353(7) 0.6389(7) -0.1196(4) 0.039(3) Uiso 1 1 d . . . H541 H 0.2841 0.6387 -0.0961 0.047 Uiso 1 1 d R . . H542 H 0.1970 0.6363 -0.1028 0.047 Uiso 1 1 d R . . C55A C 0.2265(8) 0.7071(7) -0.1477(5) 0.050(4) Uiso 1 1 d . . . H551 H 0.2627 0.7074 -0.1661 0.060 Uiso 1 1 d R . . H552 H 0.1766 0.7079 -0.1700 0.060 Uiso 1 1 d R . . C56A C 0.2365(9) 0.7735(9) -0.1176(6) 0.076(5) Uiso 1 1 d . . . H561 H 0.2322 0.8149 -0.1377 0.114 Uiso 1 1 d R . . H562 H 0.2853 0.7728 -0.0950 0.114 Uiso 1 1 d R . . H563 H 0.1986 0.7754 -0.1009 0.114 Uiso 1 1 d R . . C57A C 0.1424(6) 0.3787(6) -0.0642(4) 0.026(3) Uiso 1 1 d . . . H571 H 0.1445 0.4123 -0.0386 0.032 Uiso 1 1 d R . . H572 H 0.0932 0.3832 -0.0870 0.032 Uiso 1 1 d R . . C58A C 0.1500(6) 0.3047(7) -0.0441(4) 0.034(3) Uiso 1 1 d . . . H581 H 0.1589 0.2717 -0.0676 0.041 Uiso 1 1 d R . . H582 H 0.1934 0.3029 -0.0163 0.041 Uiso 1 1 d R . . C59A C 0.0816(7) 0.2802(7) -0.0295(5) 0.046(4) Uiso 1 1 d . . . H591 H 0.0390 0.2788 -0.0577 0.056 Uiso 1 1 d R . . H592 H 0.0899 0.2320 -0.0168 0.056 Uiso 1 1 d R . . C60A C 0.0634(8) 0.3270(8) 0.0057(5) 0.055(4) Uiso 1 1 d . . . H601 H 0.0560 0.3754 -0.0068 0.066 Uiso 1 1 d R . . H602 H 0.1057 0.3277 0.0341 0.066 Uiso 1 1 d R . . C61A C -0.0078(8) 0.3031(8) 0.0194(5) 0.060(4) Uiso 1 1 d . . . H611 H -0.0507 0.3052 -0.0087 0.072 Uiso 1 1 d R . . H612 H -0.0017 0.2537 0.0300 0.072 Uiso 1 1 d R . . C62A C -0.0219(9) 0.3462(9) 0.0562(5) 0.072(5) Uiso 1 1 d . . . H621 H -0.0250 0.3956 0.0467 0.108 Uiso 1 1 d R . . H622 H 0.0180 0.3403 0.0851 0.108 Uiso 1 1 d R . . H623 H -0.0686 0.3316 0.0615 0.108 Uiso 1 1 d R . . S1B S 0.50438(17) 0.32247(14) 0.48982(10) 0.0274(7) Uani 1 1 d . . . F1B F 0.4698(4) 0.5540(4) 0.3596(2) 0.0465(19) Uiso 1 1 d . . . F2B F 0.6543(3) 0.5402(3) 0.6186(2) 0.0341(16) Uiso 1 1 d . . . O1B O 0.4392(4) 0.2985(4) 0.4992(3) 0.034(2) Uiso 1 1 d . . . O2B O 0.5549(4) 0.2720(4) 0.4804(3) 0.0294(19) Uiso 1 1 d . . . C1B C 0.4518(6) 0.3778(6) 0.3992(4) 0.028(3) Uiso 1 1 d . . . H1B H 0.4337 0.3328 0.3880 0.033 Uiso 1 1 d R . . C2B C 0.4436(6) 0.4359(6) 0.3676(4) 0.025(3) Uiso 1 1 d . . . C3B C 0.4750(7) 0.4982(7) 0.3882(4) 0.037(3) Uiso 1 1 d . . . C4B C 0.5106(6) 0.5085(7) 0.4339(4) 0.033(3) Uiso 1 1 d . . . H4B H 0.5309 0.5531 0.4446 0.040 Uiso 1 1 d R . . C5B C 0.5890(6) 0.5019(6) 0.5451(4) 0.028(3) Uiso 1 1 d . . . H5B H 0.5901 0.5484 0.5339 0.034 Uiso 1 1 d R . . C6B C 0.6203(6) 0.4871(6) 0.5897(4) 0.025(3) Uiso 1 1 d . . . C7B C 0.6229(6) 0.4186(6) 0.6099(4) 0.023(3) Uiso 1 1 d . . . C8B C 0.5861(6) 0.3671(6) 0.5801(4) 0.030(3) Uiso 1 1 d . . . H8B H 0.5845 0.3209 0.5916 0.036 Uiso 1 1 d R . . C9B C 0.5512(6) 0.3815(6) 0.5333(4) 0.023(3) Uiso 1 1 d . . . C10B C 0.5536(6) 0.4477(6) 0.5141(4) 0.024(3) Uiso 1 1 d . . . C11B C 0.5170(6) 0.4533(6) 0.4646(4) 0.028(3) Uiso 1 1 d . . . C12B C 0.4859(6) 0.3877(6) 0.4452(4) 0.025(3) Uiso 1 1 d . . . C13B C 0.4098(6) 0.4271(6) 0.3174(4) 0.023(3) Uiso 1 1 d . . . C14B C 0.4255(6) 0.3672(6) 0.2944(4) 0.031(3) Uiso 1 1 d . . . H14B H 0.4577 0.3327 0.3122 0.037 Uiso 1 1 d R . . C15B C 0.3958(6) 0.3567(6) 0.2474(4) 0.024(3) Uiso 1 1 d . . . H15B H 0.4089 0.3171 0.2322 0.029 Uiso 1 1 d R . . C16B C 0.3464(6) 0.4064(6) 0.2229(4) 0.027(3) Uiso 1 1 d . . . C17B C 0.3049(6) 0.4078(6) 0.1720(4) 0.024(3) Uiso 1 1 d . . . C18B C 0.3057(6) 0.3632(6) 0.1358(4) 0.030(3) Uiso 1 1 d . . . H18B H 0.3363 0.3227 0.1410 0.036 Uiso 1 1 d R . . C19B C 0.2602(6) 0.3788(7) 0.0918(4) 0.036(3) Uiso 1 1 d . . . H19B H 0.2591 0.3488 0.0661 0.043 Uiso 1 1 d R . . C20B C 0.2152(7) 0.4387(7) 0.0846(5) 0.042(3) Uiso 1 1 d . . . H20B H 0.1855 0.4492 0.0540 0.050 Uiso 1 1 d R . . C21B C 0.2145(6) 0.4821(7) 0.1207(4) 0.036(3) Uiso 1 1 d . . . H21B H 0.1829 0.5219 0.1157 0.043 Uiso 1 1 d R . . C22B C 0.2603(6) 0.4671(6) 0.1648(4) 0.029(3) Uiso 1 1 d . . . C23B C 0.2689(6) 0.5096(6) 0.2095(4) 0.030(3) Uiso 1 1 d . . . C24B C 0.3271(6) 0.4650(6) 0.2443(4) 0.024(3) Uiso 1 1 d . . . C25B C 0.3605(6) 0.4772(6) 0.2911(4) 0.029(3) Uiso 1 1 d . . . H25B H 0.3506 0.5190 0.3056 0.035 Uiso 1 1 d R . . C26B C 0.1973(6) 0.5105(6) 0.2251(4) 0.033(3) Uiso 1 1 d . . . H263 H 0.2081 0.5330 0.2562 0.040 Uiso 1 1 d R . . H264 H 0.1608 0.5401 0.2029 0.040 Uiso 1 1 d R . . C27B C 0.1632(6) 0.4406(6) 0.2278(4) 0.035(3) Uiso 1 1 d . . . H273 H 0.2003 0.4094 0.2483 0.042 Uiso 1 1 d R . . H274 H 0.1481 0.4193 0.1962 0.042 Uiso 1 1 d R . . C28B C 0.0958(7) 0.4453(7) 0.2466(5) 0.047(4) Uiso 1 1 d . . . H283 H 0.0621 0.4816 0.2286 0.057 Uiso 1 1 d R . . H284 H 0.1124 0.4611 0.2795 0.057 Uiso 1 1 d R . . C29B C 0.0526(8) 0.3778(8) 0.2444(5) 0.054(4) Uiso 1 1 d . . . H293 H 0.0876 0.3397 0.2581 0.064 Uiso 1 1 d R . . H294 H 0.0179 0.3825 0.2637 0.064 Uiso 1 1 d R . . C30B C 0.0104(7) 0.3566(8) 0.1954(5) 0.051(4) Uiso 1 1 d . . . H303 H 0.0445 0.3541 0.1756 0.061 Uiso 1 1 d R . . H304 H -0.0268 0.3932 0.1823 0.061 Uiso 1 1 d R . . C31B C -0.0289(9) 0.2862(9) 0.1937(6) 0.079(5) Uiso 1 1 d . . . H314 H -0.0527 0.2732 0.1611 0.118 Uiso 1 1 d R . . H315 H -0.0661 0.2898 0.2108 0.118 Uiso 1 1 d R . . H316 H 0.0074 0.2503 0.2082 0.118 Uiso 1 1 d R . . C32B C 0.2930(6) 0.5851(6) 0.2052(4) 0.034(3) Uiso 1 1 d . . . H323 H 0.2519 0.6095 0.1827 0.040 Uiso 1 1 d R . . H324 H 0.3004 0.6084 0.2359 0.040 Uiso 1 1 d R . . C33B C 0.3602(6) 0.5954(6) 0.1899(4) 0.035(3) Uiso 1 1 d . . . H333 H 0.3533 0.5718 0.1594 0.042 Uiso 1 1 d R . . H334 H 0.4018 0.5721 0.2127 0.042 Uiso 1 1 d R . . C34B C 0.3804(7) 0.6723(7) 0.1849(5) 0.047(4) Uiso 1 1 d . . . H343 H 0.3398 0.6951 0.1609 0.057 Uiso 1 1 d R . . H344 H 0.3851 0.6966 0.2149 0.057 Uiso 1 1 d R . . C35B C 0.4524(7) 0.6826(7) 0.1712(5) 0.049(4) Uiso 1 1 d . . . H353 H 0.4458 0.6614 0.1400 0.059 Uiso 1 1 d R . . H354 H 0.4918 0.6559 0.1936 0.059 Uiso 1 1 d R . . C36B C 0.4790(8) 0.7591(8) 0.1700(5) 0.057(4) Uiso 1 1 d . . . H363 H 0.4819 0.7820 0.2003 0.069 Uiso 1 1 d R . . H364 H 0.5288 0.7597 0.1654 0.069 Uiso 1 1 d R . . C37B C 0.4273(9) 0.7994(10) 0.1316(6) 0.080(5) Uiso 1 1 d . . . H374 H 0.4244 0.7770 0.1015 0.120 Uiso 1 1 d R . . H375 H 0.4452 0.8476 0.1313 0.120 Uiso 1 1 d R . . H376 H 0.3782 0.8001 0.1366 0.120 Uiso 1 1 d R . . C38B C 0.6623(6) 0.4032(6) 0.6594(4) 0.030(3) Uiso 1 1 d . . . C39B C 0.6325(6) 0.3570(6) 0.6840(4) 0.028(3) Uiso 1 1 d . . . H39B H 0.5858 0.3367 0.6697 0.033 Uiso 1 1 d R . . C40B C 0.6700(6) 0.3393(6) 0.7308(4) 0.026(3) Uiso 1 1 d . . . H40B H 0.6484 0.3082 0.7481 0.031 Uiso 1 1 d R . . C41B C 0.7383(6) 0.3682(6) 0.7508(4) 0.023(3) Uiso 1 1 d . . . C42B C 0.7924(6) 0.3564(6) 0.7965(4) 0.030(3) Uiso 1 1 d . . . C43B C 0.7902(7) 0.3126(7) 0.8336(4) 0.037(3) Uiso 1 1 d . . . H43B H 0.7487 0.2835 0.8320 0.044 Uiso 1 1 d R . . C44B C 0.8503(7) 0.3136(7) 0.8735(4) 0.043(3) Uiso 1 1 d . . . H44B H 0.8491 0.2848 0.8994 0.051 Uiso 1 1 d R . . C45B C 0.9114(7) 0.3543(7) 0.8764(5) 0.045(4) Uiso 1 1 d . . . H45B H 0.9515 0.3539 0.9040 0.054 Uiso 1 1 d R . . C46B C 0.9144(7) 0.3963(7) 0.8395(4) 0.039(3) Uiso 1 1 d . . . H46B H 0.9569 0.4236 0.8408 0.047 Uiso 1 1 d R . . C47B C 0.8532(6) 0.3979(6) 0.7995(4) 0.030(3) Uiso 1 1 d . . . C48B C 0.8427(6) 0.4437(6) 0.7555(4) 0.030(3) Uiso 1 1 d . . . C49B C 0.7672(6) 0.4168(6) 0.7258(4) 0.025(3) Uiso 1 1 d . . . C50B C 0.7300(6) 0.4341(6) 0.6808(4) 0.025(3) Uiso 1 1 d . . . H50B H 0.7504 0.4673 0.6642 0.030 Uiso 1 1 d R . . C51B C 0.8379(6) 0.5222(6) 0.7675(4) 0.032(3) Uiso 1 1 d . . . H513 H 0.8857 0.5367 0.7891 0.038 Uiso 1 1 d R . . H514 H 0.8304 0.5498 0.7384 0.038 Uiso 1 1 d R . . C52B C 0.7776(6) 0.5403(6) 0.7891(4) 0.033(3) Uiso 1 1 d . . . H523 H 0.7774 0.5051 0.8135 0.039 Uiso 1 1 d R . . H524 H 0.7296 0.5375 0.7649 0.039 Uiso 1 1 d R . . C53B C 0.7852(7) 0.6130(6) 0.8111(4) 0.036(3) Uiso 1 1 d . . . H533 H 0.8325 0.6152 0.8360 0.044 Uiso 1 1 d R . . H534 H 0.7451 0.6200 0.8261 0.044 Uiso 1 1 d R . . C54B C 0.7835(7) 0.6737(7) 0.7766(4) 0.044(3) Uiso 1 1 d . . . H543 H 0.8287 0.6718 0.7661 0.053 Uiso 1 1 d R . . H544 H 0.7409 0.6665 0.7488 0.053 Uiso 1 1 d R . . C55B C 0.7778(8) 0.7457(8) 0.7964(5) 0.058(4) Uiso 1 1 d . . . H553 H 0.7806 0.7813 0.7727 0.069 Uiso 1 1 d R . . H554 H 0.7290 0.7504 0.8023 0.069 Uiso 1 1 d R . . C56B C 0.8360(8) 0.7621(8) 0.8407(5) 0.061(4) Uiso 1 1 d . . . H564 H 0.8846 0.7589 0.8351 0.091 Uiso 1 1 d R . . H565 H 0.8330 0.7279 0.8647 0.091 Uiso 1 1 d R . . H566 H 0.8289 0.8094 0.8515 0.091 Uiso 1 1 d R . . C57B C 0.9039(6) 0.4362(6) 0.7316(4) 0.029(3) Uiso 1 1 d . . . H573 H 0.8912 0.4664 0.7035 0.035 Uiso 1 1 d R . . H574 H 0.9500 0.4548 0.7530 0.035 Uiso 1 1 d R . . C58B C 0.9190(6) 0.3625(6) 0.7164(4) 0.031(3) Uiso 1 1 d . . . H583 H 0.9363 0.3324 0.7444 0.037 Uiso 1 1 d R . . H584 H 0.8730 0.3419 0.6962 0.037 Uiso 1 1 d R . . C59B C 0.9779(6) 0.3637(6) 0.6903(4) 0.028(3) Uiso 1 1 d . . . H593 H 0.9635 0.3994 0.6653 0.034 Uiso 1 1 d R . . H594 H 1.0252 0.3788 0.7121 0.034 Uiso 1 1 d R . . C60B C 0.9891(6) 0.2957(7) 0.6689(4) 0.039(3) Uiso 1 1 d . . . H603 H 0.9995 0.2590 0.6934 0.046 Uiso 1 1 d R . . H604 H 0.9430 0.2825 0.6451 0.046 Uiso 1 1 d R . . C61B C 1.0515(8) 0.2953(8) 0.6468(5) 0.054(4) Uiso 1 1 d . . . H613 H 1.0585 0.2472 0.6363 0.065 Uiso 1 1 d R . . H614 H 1.0976 0.3091 0.6705 0.065 Uiso 1 1 d R . . C62B C 1.0387(8) 0.3449(8) 0.6050(5) 0.056(4) Uiso 1 1 d . . . H624 H 0.9868 0.3434 0.5869 0.084 Uiso 1 1 d R . . H625 H 1.0695 0.3304 0.5851 0.084 Uiso 1 1 d R . . H626 H 1.0519 0.3928 0.6162 0.084 Uiso 1 1 d R . . S1C S 0.53432(16) 0.65913(14) 0.66890(11) 0.0273(8) Uani 1 1 d . . . F1C F 0.5662(3) 0.4282(4) 0.7998(2) 0.0387(17) Uiso 1 1 d . . . F2C F 0.3824(4) 0.4454(4) 0.5390(2) 0.0385(18) Uiso 1 1 d . . . O1C O 0.4847(4) 0.7102(4) 0.6764(3) 0.031(2) Uiso 1 1 d . . . O2C O 0.6017(4) 0.6846(5) 0.6608(3) 0.040(2) Uiso 1 1 d . . . C1C C 0.5832(6) 0.6026(6) 0.7594(4) 0.025(3) Uiso 1 1 d . . . H1C H 0.6026 0.6473 0.7706 0.031 Uiso 1 1 d R . . C2C C 0.5889(6) 0.5466(6) 0.7903(4) 0.025(3) Uiso 1 1 d . . . C3C C 0.5616(6) 0.4851(6) 0.7701(4) 0.028(3) Uiso 1 1 d . . . C4C C 0.5278(6) 0.4739(7) 0.7245(4) 0.028(3) Uiso 1 1 d . . . H4C H 0.5092 0.4288 0.7137 0.034 Uiso 1 1 d R . . C5C C 0.4500(6) 0.4812(6) 0.6142(4) 0.025(3) Uiso 1 1 d . . . H5C H 0.4491 0.4343 0.6247 0.030 Uiso 1 1 d R . . C6C C 0.4166(6) 0.4983(6) 0.5678(4) 0.027(3) Uiso 1 1 d . . . C7C C 0.4176(6) 0.5635(6) 0.5480(4) 0.024(3) Uiso 1 1 d . . . C8C C 0.4555(6) 0.6161(6) 0.5785(3) 0.021(3) Uiso 1 1 d . . . H8C H 0.4584 0.6622 0.5670 0.025 Uiso 1 1 d R . . C9C C 0.4883(6) 0.6013(6) 0.6240(4) 0.025(3) Uiso 1 1 d . . . C10C C 0.4845(6) 0.5334(6) 0.6448(4) 0.026(3) Uiso 1 1 d . . . C11C C 0.5199(6) 0.5299(6) 0.6933(4) 0.019(2) Uiso 1 1 d . . . C12C C 0.5499(6) 0.5934(6) 0.7141(4) 0.026(3) Uiso 1 1 d . . . C13C C 0.6224(6) 0.5588(6) 0.8414(4) 0.024(3) Uiso 1 1 d . . . C14C C 0.6087(6) 0.6201(6) 0.8625(4) 0.029(3) Uiso 1 1 d . . . H14C H 0.5791 0.6552 0.8435 0.035 Uiso 1 1 d R . . C15C C 0.6354(6) 0.6318(7) 0.9090(4) 0.038(3) Uiso 1 1 d . . . H15C H 0.6216 0.6731 0.9223 0.046 Uiso 1 1 d R . . C16C C 0.6824(6) 0.5849(6) 0.9369(4) 0.028(3) Uiso 1 1 d . . . C17C C 0.7203(7) 0.5813(7) 0.9872(4) 0.040(3) Uiso 1 1 d . . . C18C C 0.7210(7) 0.6325(8) 1.0214(5) 0.051(4) Uiso 1 1 d . . . H18C H 0.6938 0.6748 1.0137 0.061 Uiso 1 1 d R . . C19C C 0.7628(7) 0.6197(8) 1.0665(5) 0.051(4) Uiso 1 1 d . . . H19C H 0.7638 0.6535 1.0901 0.061 Uiso 1 1 d R . . C20C C 0.8026(7) 0.5592(8) 1.0778(5) 0.049(4) Uiso 1 1 d . . . H20C H 0.8307 0.5510 1.1092 0.059 Uiso 1 1 d R . . C21C C 0.8020(7) 0.5085(8) 1.0432(4) 0.042(3) Uiso 1 1 d . . . H21C H 0.8311 0.4673 1.0511 0.050 Uiso 1 1 d R . . C22C C 0.7594(7) 0.5179(7) 0.9976(4) 0.036(3) Uiso 1 1 d . . . C23C C 0.7532(7) 0.4773(7) 0.9541(4) 0.034(3) Uiso 1 1 d . . . C24C C 0.6991(6) 0.5218(6) 0.9170(4) 0.028(3) Uiso 1 1 d . . . C25C C 0.6703(6) 0.5084(7) 0.8699(4) 0.030(3) Uiso 1 1 d . . . H25C H 0.6820 0.4659 0.8569 0.036 Uiso 1 1 d R . . C26C C 0.8275(7) 0.4728(7) 0.9437(4) 0.039(3) Uiso 1 1 d . . . H265 H 0.8198 0.4522 0.9122 0.046 Uiso 1 1 d R . . H266 H 0.8599 0.4406 0.9665 0.046 Uiso 1 1 d R . . C27C C 0.8666(7) 0.5444(7) 0.9450(5) 0.048(4) Uiso 1 1 d . . . H275 H 0.8317 0.5786 0.9256 0.057 Uiso 1 1 d R . . H276 H 0.8804 0.5619 0.9776 0.057 Uiso 1 1 d R . . C28C C 0.9352(7) 0.5416(7) 0.9283(5) 0.049(4) Uiso 1 1 d . . . H285 H 0.9216 0.5273 0.8950 0.059 Uiso 1 1 d R . . H286 H 0.9696 0.5060 0.9465 0.059 Uiso 1 1 d R . . C29C C 0.9733(8) 0.6115(8) 0.9341(5) 0.055(4) Uiso 1 1 d . . . H295 H 0.9893 0.6238 0.9677 0.067 Uiso 1 1 d R . . H296 H 0.9371 0.6473 0.9180 0.067 Uiso 1 1 d R . . C30C C 1.0416(8) 0.6156(9) 0.9142(5) 0.065(4) Uiso 1 1 d . . . H305 H 1.0775 0.5795 0.9301 0.078 Uiso 1 1 d R . . H306 H 1.0655 0.6619 0.9220 0.078 Uiso 1 1 d R . . C31C C 1.0228(8) 0.6048(9) 0.8610(5) 0.066(4) Uiso 1 1 d . . . H317 H 0.9789 0.6320 0.8453 0.099 Uiso 1 1 d R . . H318 H 1.0134 0.5549 0.8538 0.099 Uiso 1 1 d R . . H319 H 1.0646 0.6203 0.8501 0.099 Uiso 1 1 d R . . C32C C 0.7163(7) 0.4027(8) 0.9554(5) 0.049(4) Uiso 1 1 d . . . H325 H 0.6660 0.4097 0.9585 0.058 Uiso 1 1 d R . . H326 H 0.7113 0.3799 0.9248 0.058 Uiso 1 1 d R . . C33C C 0.7567(10) 0.3545(9) 0.9928(6) 0.087(6) Uiso 1 1 d . . . H335 H 0.7549 0.3731 1.0235 0.104 Uiso 1 1 d R . . H336 H 0.8091 0.3521 0.9929 0.104 Uiso 1 1 d R . . C34C C 0.7211(12) 0.2780(11) 0.9859(7) 0.110(7) Uiso 1 1 d D . . H345 H 0.6677 0.2840 0.9708 0.131 Uiso 1 1 d R . . H346 H 0.7383 0.2549 1.0168 0.131 Uiso 1 1 d R . . C35C C 0.7493(15) 0.2310(11) 0.9556(9) 0.150(10) Uiso 1 1 d D . . H355 H 0.8033 0.2303 0.9698 0.180 Uiso 1 1 d R . . H356 H 0.7284 0.2533 0.9247 0.180 Uiso 1 1 d R . . C36C C 0.7287(12) 0.1548(10) 0.9426(7) 0.110(7) Uiso 1 1 d D . . H365 H 0.6753 0.1507 0.9393 0.132 Uiso 1 1 d R . . H366 H 0.7492 0.1372 0.9176 0.132 Uiso 1 1 d R . . C37C C 0.7690(11) 0.1193(11) 0.9859(7) 0.112(7) Uiso 1 1 d D . . H377 H 0.7620 0.0684 0.9824 0.168 Uiso 1 1 d R . . H378 H 0.8216 0.1304 0.9931 0.168 Uiso 1 1 d R . . H379 H 0.7497 0.1359 1.0113 0.168 Uiso 1 1 d R . . C38C C 0.3823(6) 0.5822(6) 0.4985(4) 0.022(3) Uiso 1 1 d . . . C39C C 0.4131(6) 0.6263(6) 0.4734(4) 0.030(3) Uiso 1 1 d . . . H39C H 0.4617 0.6425 0.4877 0.036 Uiso 1 1 d R . . C40C C 0.3796(6) 0.6485(6) 0.4290(4) 0.027(3) Uiso 1 1 d . . . H40C H 0.4040 0.6798 0.4135 0.032 Uiso 1 1 d R . . C41C C 0.3099(7) 0.6254(7) 0.4072(4) 0.033(3) Uiso 1 1 d . . . C42C C 0.2580(6) 0.6434(7) 0.3620(4) 0.032(3) Uiso 1 1 d . . . C43C C 0.2667(8) 0.6875(7) 0.3261(4) 0.046(4) Uiso 1 1 d . . . H43C H 0.3126 0.7086 0.3273 0.055 Uiso 1 1 d R . . C44C C 0.2063(7) 0.6977(7) 0.2896(5) 0.043(3) Uiso 1 1 d . . . H44C H 0.2098 0.7295 0.2658 0.052 Uiso 1 1 d R . . C45C C 0.1407(7) 0.6641(7) 0.2858(5) 0.043(3) Uiso 1 1 d . . . H45C H 0.0996 0.6741 0.2598 0.052 Uiso 1 1 d R . . C46C C 0.1322(7) 0.6156(7) 0.3196(4) 0.035(3) Uiso 1 1 d . . . H46C H 0.0879 0.5901 0.3163 0.042 Uiso 1 1 d R . . C47C C 0.1929(7) 0.6071(7) 0.3583(4) 0.035(3) Uiso 1 1 d . . . C48C C 0.1961(6) 0.5619(7) 0.4012(4) 0.033(3) Uiso 1 1 d . . . C49C C 0.2758(6) 0.5799(6) 0.4300(4) 0.027(3) Uiso 1 1 d . . . C50C C 0.3105(6) 0.5561(7) 0.4754(4) 0.033(3) Uiso 1 1 d . . . H50C H 0.2870 0.5228 0.4901 0.039 Uiso 1 1 d R . . C51C C 0.1377(6) 0.5836(6) 0.4252(4) 0.031(3) Uiso 1 1 d . . . H515 H 0.1421 0.5528 0.4526 0.038 Uiso 1 1 d R . . H516 H 0.0884 0.5757 0.4033 0.038 Uiso 1 1 d R . . C52C C 0.1423(6) 0.6612(6) 0.4413(4) 0.033(3) Uiso 1 1 d . . . H525 H 0.1852 0.6662 0.4692 0.039 Uiso 1 1 d R . . H526 H 0.1510 0.6914 0.4163 0.039 Uiso 1 1 d R . . C53C C 0.0748(6) 0.6864(6) 0.4533(4) 0.030(3) Uiso 1 1 d . . . H535 H 0.0817 0.7367 0.4615 0.036 Uiso 1 1 d R . . H536 H 0.0328 0.6828 0.4248 0.036 Uiso 1 1 d R . . C54C C 0.0536(7) 0.6495(7) 0.4922(4) 0.039(3) Uiso 1 1 d . . . H545 H 0.0938 0.6553 0.5214 0.046 Uiso 1 1 d R . . H546 H 0.0483 0.5988 0.4850 0.046 Uiso 1 1 d R . . C55C C -0.0168(8) 0.6763(9) 0.5004(5) 0.063(4) Uiso 1 1 d . . . H555 H -0.0140 0.7280 0.5037 0.076 Uiso 1 1 d R . . H556 H -0.0581 0.6651 0.4726 0.076 Uiso 1 1 d R . . C56C C -0.0331(8) 0.6456(8) 0.5429(5) 0.054(4) Uiso 1 1 d . . . H567 H -0.0367 0.5945 0.5396 0.080 Uiso 1 1 d R . . H568 H -0.0796 0.6644 0.5462 0.080 Uiso 1 1 d R . . H569 H 0.0070 0.6577 0.5706 0.080 Uiso 1 1 d R . . C57C C 0.1895(6) 0.4817(6) 0.3908(4) 0.029(3) Uiso 1 1 d . . . H575 H 0.1953 0.4563 0.4206 0.035 Uiso 1 1 d R . . H576 H 0.1398 0.4712 0.3702 0.035 Uiso 1 1 d R . . C58C C 0.2458(6) 0.4546(6) 0.3677(4) 0.024(3) Uiso 1 1 d . . . H585 H 0.2955 0.4633 0.3891 0.029 Uiso 1 1 d R . . H586 H 0.2416 0.4818 0.3388 0.029 Uiso 1 1 d R . . C59C C 0.2385(7) 0.3748(6) 0.3548(4) 0.035(3) Uiso 1 1 d . . . H595 H 0.1874 0.3650 0.3360 0.042 Uiso 1 1 d R . . H596 H 0.2718 0.3634 0.3354 0.042 Uiso 1 1 d R . . C60C C 0.2576(7) 0.3277(7) 0.3975(4) 0.039(3) Uiso 1 1 d . . . H605 H 0.2217 0.3356 0.4156 0.047 Uiso 1 1 d R . . H606 H 0.3073 0.3394 0.4177 0.047 Uiso 1 1 d R . . C61C C 0.2552(8) 0.2505(7) 0.3822(5) 0.051(4) Uiso 1 1 d . . . H615 H 0.2056 0.2399 0.3613 0.062 Uiso 1 1 d R . . H616 H 0.2912 0.2434 0.3640 0.062 Uiso 1 1 d R . . C62C C 0.2719(9) 0.1989(9) 0.4221(5) 0.074(5) Uiso 1 1 d . . . H627 H 0.2716 0.1510 0.4102 0.111 Uiso 1 1 d R . . H628 H 0.2345 0.2032 0.4391 0.111 Uiso 1 1 d R . . H629 H 0.3206 0.2094 0.4433 0.111 Uiso 1 1 d R . . S1D S 0.48513(17) 0.63857(15) 0.97622(10) 0.0304(8) Uani 1 1 d . . . F1D F 0.4336(3) 0.4152(3) 0.8389(2) 0.0345(16) Uiso 1 1 d . . . F2D F 0.6451(3) 0.4154(4) 1.0945(2) 0.0386(17) Uiso 1 1 d . . . O1D O 0.5320(4) 0.6939(4) 0.9689(3) 0.036(2) Uiso 1 1 d . . . O2D O 0.4183(5) 0.6587(5) 0.9881(3) 0.044(2) Uiso 1 1 d . . . C1D C 0.4308(6) 0.5903(6) 0.8843(4) 0.026(3) Uiso 1 1 d . . . H1D H 0.4144 0.6364 0.8745 0.032 Uiso 1 1 d R . . C2D C 0.4190(6) 0.5353(6) 0.8516(4) 0.025(3) Uiso 1 1 d . . . C3D C 0.4449(6) 0.4698(6) 0.8697(4) 0.029(3) Uiso 1 1 d . . . C4D C 0.4823(6) 0.4567(6) 0.9153(4) 0.026(3) Uiso 1 1 d . . . H4D H 0.4986 0.4105 0.9249 0.031 Uiso 1 1 d R . . C5D C 0.5732(6) 0.4575(6) 1.0231(4) 0.030(3) Uiso 1 1 d . . . H5D H 0.5742 0.4118 1.0106 0.036 Uiso 1 1 d R . . C6D C 0.6095(6) 0.4711(6) 1.0680(4) 0.031(3) Uiso 1 1 d . . . C7D C 0.6127(6) 0.5353(6) 1.0914(4) 0.026(3) Uiso 1 1 d . . . C8D C 0.5734(6) 0.5897(6) 1.0629(4) 0.027(3) Uiso 1 1 d . . . H8D H 0.5728 0.6352 1.0757 0.033 Uiso 1 1 d R . . C9D C 0.5355(6) 0.5775(6) 1.0166(4) 0.025(3) Uiso 1 1 d . . . C10D C 0.5334(6) 0.5125(6) 0.9952(4) 0.020(3) Uiso 1 1 d . . . C11D C 0.4957(6) 0.5115(6) 0.9472(4) 0.028(3) Uiso 1 1 d . . . C12D C 0.4655(6) 0.5773(6) 0.9293(4) 0.030(3) Uiso 1 1 d . . . C13D C 0.3843(6) 0.5476(6) 0.8013(4) 0.023(3) Uiso 1 1 d . . . C14D C 0.4064(6) 0.6057(6) 0.7797(4) 0.027(3) Uiso 1 1 d . . . H14D H 0.4431 0.6363 0.7977 0.032 Uiso 1 1 d R . . C15D C 0.3768(6) 0.6193(6) 0.7334(4) 0.024(3) Uiso 1 1 d . . . H15D H 0.3911 0.6598 0.7196 0.028 Uiso 1 1 d R . . C16D C 0.3253(6) 0.5728(6) 0.7069(4) 0.025(3) Uiso 1 1 d . . . C17D C 0.2865(6) 0.5713(6) 0.6558(4) 0.023(3) Uiso 1 1 d . . . C18D C 0.2932(7) 0.6145(7) 0.6200(4) 0.035(3) Uiso 1 1 d . . . H18D H 0.3260 0.6534 0.6261 0.042 Uiso 1 1 d R . . C19D C 0.2520(6) 0.6001(7) 0.5754(4) 0.035(3) Uiso 1 1 d . . . H19D H 0.2570 0.6286 0.5503 0.042 Uiso 1 1 d R . . C20D C 0.2043(7) 0.5451(7) 0.5664(4) 0.040(3) Uiso 1 1 d . . . H20D H 0.1752 0.5369 0.5352 0.048 Uiso 1 1 d R . . C21D C 0.1968(7) 0.5009(7) 0.6022(4) 0.037(3) Uiso 1 1 d . . . H21D H 0.1639 0.4621 0.5957 0.045 Uiso 1 1 d R . . C22D C 0.2388(6) 0.5151(6) 0.6471(4) 0.029(3) Uiso 1 1 d . . . C23D C 0.2385(6) 0.4769(6) 0.6924(4) 0.027(3) Uiso 1 1 d . . . C24D C 0.3000(6) 0.5163(6) 0.7272(4) 0.025(3) Uiso 1 1 d . . . C25D C 0.3293(6) 0.5032(6) 0.7748(4) 0.025(3) Uiso 1 1 d . . . H25D H 0.3121 0.4645 0.7888 0.030 Uiso 1 1 d R . . C26D C 0.1652(6) 0.4835(6) 0.7038(4) 0.034(3) Uiso 1 1 d . B . H267 H 0.1703 0.4613 0.7346 0.041 Uiso 1 1 d R . . H268 H 0.1276 0.4566 0.6803 0.041 Uiso 1 1 d R . . C27D C 0.1365(6) 0.5587(6) 0.7059(4) 0.036(3) Uiso 1 1 d D . . H277 H 0.1670 0.5816 0.7346 0.043 Uiso 0.60 1 d PR A 1 H278 H 0.1440 0.5849 0.6789 0.043 Uiso 0.60 1 d PR A 1 H279 H 0.1199 0.5790 0.6741 0.043 Uiso 0.40 1 d PR A 2 H280 H 0.1753 0.5892 0.7256 0.043 Uiso 0.40 1 d PR A 2 C28D C 0.0559(8) 0.5654(10) 0.7048(8) 0.039(6) Uiso 0.60 1 d PD B 1 H289 H 0.0504 0.5484 0.7350 0.047 Uiso 0.60 1 d PR B 1 H290 H 0.0261 0.5343 0.6800 0.047 Uiso 0.60 1 d PR B 1 C29D C 0.0252(9) 0.6413(9) 0.6970(8) 0.033(5) Uiso 0.60 1 d PD B 1 H299 H 0.0587 0.6747 0.7181 0.040 Uiso 0.60 1 d PR B 1 H300 H 0.0208 0.6555 0.6644 0.040 Uiso 0.60 1 d PR B 1 C28E C 0.0705(13) 0.5544(13) 0.7274(11) 0.031(8) Uiso 0.40 1 d PD B 2 H287 H 0.0878 0.5386 0.7603 0.037 Uiso 0.40 1 d PR B 2 H288 H 0.0341 0.5202 0.7094 0.037 Uiso 0.40 1 d PR B 2 C29E C 0.0345(10) 0.6285(14) 0.7253(11) 0.036(8) Uiso 0.40 1 d PD B 2 H297 H 0.0485 0.6481 0.7573 0.043 Uiso 0.40 1 d PR B 2 H298 H 0.0590 0.6578 0.7066 0.043 Uiso 0.40 1 d PR B 2 C30D C -0.0494(9) 0.6443(12) 0.7052(7) 0.114(7) Uiso 1 1 d D . . H307 H -0.0638 0.6931 0.7100 0.137 Uiso 0.60 1 d PR B 1 H308 H -0.0500 0.6159 0.7328 0.137 Uiso 0.60 1 d PR B 1 H309 H -0.0561 0.6957 0.7017 0.137 Uiso 0.40 1 d PR B 2 H310 H -0.0711 0.6305 0.7305 0.137 Uiso 0.40 1 d PR B 2 C31D C -0.0992(11) 0.6133(11) 0.6598(7) 0.110(7) Uiso 1 1 d . B . H31F H -0.0965 0.6415 0.6329 0.165 Uiso 1 1 d R . . H31G H -0.1500 0.6133 0.6621 0.165 Uiso 1 1 d R . . H31H H -0.0840 0.5651 0.6559 0.165 Uiso 1 1 d R . . C32D C 0.2569(6) 0.3986(6) 0.6912(4) 0.026(3) Uiso 1 1 d . . . H327 H 0.2559 0.3773 0.7213 0.031 Uiso 1 1 d R . . H328 H 0.2182 0.3754 0.6662 0.031 Uiso 1 1 d R . . C33D C 0.3303(6) 0.3831(6) 0.6832(4) 0.024(3) Uiso 1 1 d . . . H337 H 0.3692 0.4095 0.7062 0.029 Uiso 1 1 d R . . H338 H 0.3300 0.3988 0.6515 0.029 Uiso 1 1 d R . . C34D C 0.3474(6) 0.3035(6) 0.6881(4) 0.035(3) Uiso 1 1 d . . . H347 H 0.3448 0.2876 0.7192 0.042 Uiso 1 1 d R . . H348 H 0.3095 0.2776 0.6642 0.042 Uiso 1 1 d R . . C35D C 0.4230(7) 0.2856(7) 0.6830(5) 0.045(4) Uiso 1 1 d . . . H357 H 0.4602 0.3156 0.7044 0.054 Uiso 1 1 d R . . H358 H 0.4236 0.2968 0.6506 0.054 Uiso 1 1 d R . . C36D C 0.4453(6) 0.2079(6) 0.6932(4) 0.038(3) Uiso 1 1 d . . . H367 H 0.4456 0.1967 0.7257 0.045 Uiso 1 1 d R . . H368 H 0.4080 0.1776 0.6720 0.045 Uiso 1 1 d R . . C37D C 0.5203(8) 0.1915(8) 0.6868(5) 0.057(4) Uiso 1 1 d . . . H380 H 0.5190 0.1980 0.6540 0.086 Uiso 1 1 d R . . H381 H 0.5334 0.1428 0.6960 0.086 Uiso 1 1 d R . . H382 H 0.5572 0.2230 0.7065 0.086 Uiso 1 1 d R . . C38D C 0.6539(6) 0.5482(6) 1.1394(4) 0.028(3) Uiso 1 1 d . . . C39D C 0.6269(6) 0.5971(6) 1.1657(4) 0.027(3) Uiso 1 1 d . . . H39D H 0.5811 0.6191 1.1511 0.033 Uiso 1 1 d R . . C40D C 0.6612(6) 0.6149(6) 1.2103(4) 0.028(3) Uiso 1 1 d . . . H40D H 0.6407 0.6487 1.2266 0.034 Uiso 1 1 d R . . C41D C 0.7290(6) 0.5819(6) 1.2321(4) 0.029(3) Uiso 1 1 d . . . C42D C 0.7810(6) 0.5882(6) 1.2781(4) 0.028(3) Uiso 1 1 d . . . C43D C 0.7788(6) 0.6319(6) 1.3160(4) 0.027(3) Uiso 1 1 d . . . H43D H 0.7376 0.6613 1.3145 0.032 Uiso 1 1 d R . . C44D C 0.8389(7) 0.6307(7) 1.3558(4) 0.040(3) Uiso 1 1 d . . . H44D H 0.8388 0.6599 1.3816 0.048 Uiso 1 1 d R . . C45D C 0.8983(7) 0.5880(7) 1.3586(4) 0.040(3) Uiso 1 1 d . . . H45D H 0.9389 0.5886 1.3859 0.048 Uiso 1 1 d R . . C46D C 0.8996(6) 0.5436(6) 1.3215(4) 0.031(3) Uiso 1 1 d . . . H46D H 0.9400 0.5128 1.3239 0.037 Uiso 1 1 d R . . C47D C 0.8417(6) 0.5449(6) 1.2813(4) 0.028(3) Uiso 1 1 d . . . C48D C 0.8328(6) 0.5054(6) 1.2360(4) 0.031(3) Uiso 1 1 d . . . C49D C 0.7585(6) 0.5311(6) 1.2074(4) 0.028(3) Uiso 1 1 d . . . C50D C 0.7204(6) 0.5147(6) 1.1604(4) 0.029(3) Uiso 1 1 d . . . H50D H 0.7402 0.4812 1.1436 0.035 Uiso 1 1 d R . . C51D C 0.8942(7) 0.5227(7) 1.2144(5) 0.044(3) Uiso 1 1 d . D . H517 H 0.8859 0.4965 1.1847 0.053 Uiso 1 1 d R . . H518 H 0.9414 0.5062 1.2357 0.053 Uiso 1 1 d R . . C52D C 0.9026(8) 0.6019(8) 1.2037(5) 0.058(4) Uiso 1 1 d D . . H527 H 0.9156 0.6300 1.2327 0.069 Uiso 0.55 1 d PR C 1 H528 H 0.8571 0.6209 1.1819 0.069 Uiso 0.55 1 d PR C 1 H529 H 0.8586 0.6136 1.1777 0.069 Uiso 0.45 1 d PR C 2 H530 H 0.8966 0.6270 1.2315 0.069 Uiso 0.45 1 d PR C 2 C53D C 0.9671(10) 0.5994(11) 1.1813(7) 0.030(5) Uiso 0.55 1 d PD D 1 H537 H 1.0134 0.5861 1.2048 0.036 Uiso 0.55 1 d PR D 1 H538 H 0.9566 0.5642 1.1559 0.036 Uiso 0.55 1 d PR D 1 C54D C 0.9783(11) 0.6692(11) 1.1603(7) 0.036(6) Uiso 0.55 1 d PD D 1 H547 H 0.9936 0.7046 1.1854 0.043 Uiso 0.55 1 d PR D 1 H548 H 0.9320 0.6845 1.1375 0.043 Uiso 0.55 1 d PR D 1 C53E C 0.9663(11) 0.6404(13) 1.1927(7) 0.028(6) Uiso 0.45 1 d PD D 2 H539 H 0.9586 0.6918 1.1921 0.034 Uiso 0.45 1 d PR D 2 H540 H 1.0123 0.6300 1.2174 0.034 Uiso 0.45 1 d PR D 2 C54E C 0.9746(13) 0.6148(14) 1.1459(8) 0.043(8) Uiso 0.45 1 d PD D 2 H549 H 0.9290 0.6260 1.1210 0.051 Uiso 0.45 1 d PR D 2 H550 H 0.9819 0.5634 1.1462 0.051 Uiso 0.45 1 d PR D 2 C55D C 1.0402(9) 0.6543(10) 1.1368(6) 0.092(6) Uiso 1 1 d D . . H557 H 1.0757 0.6255 1.1603 0.110 Uiso 0.55 1 d PR D 1 H558 H 1.0537 0.7023 1.1296 0.110 Uiso 0.55 1 d PR D 1 H559 H 1.0861 0.6410 1.1608 0.110 Uiso 0.45 1 d PR D 2 H560 H 1.0283 0.7043 1.1298 0.110 Uiso 0.45 1 d PR D 2 C56D C 1.0402(12) 0.6163(12) 1.0925(7) 0.128(9) Uiso 1 1 d D D . H56F H 1.0462 0.5659 1.0990 0.191 Uiso 1 1 d R . . H56G H 0.9922 0.6250 1.0700 0.191 Uiso 1 1 d R . . H56H H 1.0795 0.6329 1.0796 0.191 Uiso 1 1 d R . . C57D C 0.8339(7) 0.4237(7) 1.2421(4) 0.042(3) Uiso 1 1 d . . . H577 H 0.8354 0.4019 1.2122 0.051 Uiso 1 1 d R . . H578 H 0.8803 0.4111 1.2658 0.051 Uiso 1 1 d R . . C58D C 0.7715(8) 0.3918(8) 1.2566(5) 0.059(4) Uiso 1 1 d . . . H587 H 0.7244 0.4045 1.2336 0.071 Uiso 1 1 d R . . H588 H 0.7708 0.4109 1.2874 0.071 Uiso 1 1 d R . . C59D C 0.7776(7) 0.3118(7) 1.2601(5) 0.049(4) Uiso 1 1 d . . . H597 H 0.7273 0.2927 1.2549 0.058 Uiso 1 1 d R . . H598 H 0.7957 0.2956 1.2337 0.058 Uiso 1 1 d R . . C60D C 0.8253(9) 0.2795(9) 1.3038(5) 0.074(5) Uiso 1 1 d . . . H607 H 0.8332 0.2295 1.2974 0.089 Uiso 1 1 d R . . H608 H 0.8740 0.3029 1.3121 0.089 Uiso 1 1 d R . . C61D C 0.7953(9) 0.2828(9) 1.3444(5) 0.071(5) Uiso 1 1 d . . . H617 H 0.7468 0.2592 1.3363 0.086 Uiso 1 1 d R . . H618 H 0.7875 0.3326 1.3509 0.086 Uiso 1 1 d R . . C62D C 0.8461(8) 0.2492(8) 1.3890(5) 0.063(4) Uiso 1 1 d . . . H62F H 0.8515 0.1991 1.3835 0.095 Uiso 1 1 d R . . H62G H 0.8242 0.2552 1.4150 0.095 Uiso 1 1 d R . . H62H H 0.8947 0.2717 1.3969 0.095 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1A 0.0446(19) 0.0068(15) 0.0241(16) -0.0046(12) 0.0051(14) -0.0065(14) S1B 0.0495(19) 0.0089(16) 0.0221(16) 0.0040(12) 0.0070(14) 0.0069(14) S1C 0.0343(17) 0.0049(15) 0.0394(18) 0.0016(13) 0.0047(15) -0.0021(13) S1D 0.0435(19) 0.0132(16) 0.0298(17) 0.0014(14) 0.0023(15) 0.0006(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1A O1A 1.428(8) . ? S1A O2A 1.438(8) . ? S1A C9A 1.749(11) . ? S1A C12A 1.775(11) . ? F1A C3A 1.369(12) . ? F2A C6A 1.360(12) . ? C1A C12A 1.360(15) . ? C1A C2A 1.393(16) . ? C2A C3A 1.392(15) . ? C2A C13A 1.497(14) . ? C3A C4A 1.353(15) . ? C4A C11A 1.400(15) . ? C5A C6A 1.348(14) . ? C5A C10A 1.354(15) . ? C6A C7A 1.393(15) . ? C7A C8A 1.402(15) . ? C7A C38A 1.510(15) . ? C8A C9A 1.357(15) . ? C9A C10A 1.407(16) . ? C10A C11A 1.498(14) . ? C11A C12A 1.376(14) . ? C13A C25A 1.380(15) . ? C13A C14A 1.405(16) . ? C14A C15A 1.376(15) . ? C15A C16A 1.401(15) . ? C16A C24A 1.392(16) . ? C16A C17A 1.441(16) . ? C17A C22A 1.362(16) . ? C17A C18A 1.400(17) . ? C18A C19A 1.420(16) . ? C19A C20A 1.402(17) . ? C20A C21A 1.370(17) . ? C21A C22A 1.414(16) . ? C22A C23A 1.543(16) . ? C23A C26A 1.493(16) . ? C23A C32A 1.522(17) . ? C23A C24A 1.569(15) . ? C24A C25A 1.404(15) . ? C26A C27A 1.527(18) . ? C27A C28A 1.547(17) . ? C28A C29A 1.542(19) . ? C29A C30A 1.500(18) . ? C30A C31A 1.575(19) . ? C32A C33A 1.525(17) . ? C33A C34A 1.553(17) . ? C34A C35A 1.536(17) . ? C35A C36A 1.555(17) . ? C36A C37A 1.509(18) . ? C38A C50A 1.313(15) . ? C38A C39A 1.446(15) . ? C39A C40A 1.385(15) . ? C40A C41A 1.361(15) . ? C41A C49A 1.421(15) . ? C41A C42A 1.488(15) . ? C42A C47A 1.364(15) . ? C42A C43A 1.412(16) . ? C43A C44A 1.388(17) . ? C44A C45A 1.374(18) . ? C45A C46A 1.418(18) . ? C46A C47A 1.412(16) . ? C47A C48A 1.531(16) . ? C48A C49A 1.482(15) . ? C48A C51A 1.543(17) . ? C48A C57A 1.558(15) . ? C49A C50A 1.401(14) . ? C51A C52A 1.552(17) . ? C52A C53A 1.522(18) . ? C53A C54A 1.480(17) . ? C54A C55A 1.532(18) . ? C55A C56A 1.53(2) . ? C57A C58A 1.523(16) . ? C58A C59A 1.548(17) . ? C59A C60A 1.487(18) . ? C60A C61A 1.579(19) . ? C61A C62A 1.45(2) . ? S1B O1B 1.414(8) . ? S1B O2B 1.437(8) . ? S1B C9B 1.757(11) . ? S1B C12B 1.782(11) . ? F1B C3B 1.351(14) . ? F2B C6B 1.368(12) . ? C1B C12B 1.356(15) . ? C1B C2B 1.433(16) . ? C2B C3B 1.391(16) . ? C2B C13B 1.463(15) . ? C3B C4B 1.355(16) . ? C4B C11B 1.376(16) . ? C5B C6B 1.325(15) . ? C5B C10B 1.422(16) . ? C6B C7B 1.434(15) . ? C7B C8B 1.375(15) . ? C7B C38B 1.484(15) . ? C8B C9B 1.393(15) . ? C9B C10B 1.392(15) . ? C10B C11B 1.449(15) . ? C11B C12B 1.433(16) . ? C13B C14B 1.406(15) . ? C13B C25B 1.410(15) . ? C14B C15B 1.370(15) . ? C15B C16B 1.386(15) . ? C16B C24B 1.386(15) . ? C16B C17B 1.499(15) . ? C17B C18B 1.377(15) . ? C17B C22B 1.392(15) . ? C18B C19B 1.387(16) . ? C19B C20B 1.404(17) . ? C20B C21B 1.361(17) . ? C21B C22B 1.385(16) . ? C22B C23B 1.528(16) . ? C23B C32B 1.527(16) . ? C23B C24B 1.540(15) . ? C23B C26B 1.549(16) . ? C24B C25B 1.380(15) . ? C26B C27B 1.491(16) . ? C27B C28B 1.531(16) . ? C28B C29B 1.518(18) . ? C29B C30B 1.510(18) . ? C30B C31B 1.53(2) . ? C32B C33B 1.478(16) . ? C33B C34B 1.533(17) . ? C34B C35B 1.537(18) . ? C35B C36B 1.548(19) . ? C36B C37B 1.49(2) . ? C38B C39B 1.364(16) . ? C38B C50B 1.392(15) . ? C39B C40B 1.418(15) . ? C40B C41B 1.376(14) . ? C41B C49B 1.393(15) . ? C41B C42B 1.474(15) . ? C42B C47B 1.378(16) . ? C42B C43B 1.395(16) . ? C43B C44B 1.396(16) . ? C44B C45B 1.375(17) . ? C45B C46B 1.374(17) . ? C46B C47B 1.412(16) . ? C47B C48B 1.540(16) . ? C48B C57B 1.526(15) . ? C48B C49B 1.543(15) . ? C48B C51B 1.547(16) . ? C49B C50B 1.367(14) . ? C51B C52B 1.497(15) . ? C52B C53B 1.523(16) . ? C53B C54B 1.543(17) . ? C54B C55B 1.510(19) . ? C55B C56B 1.496(18) . ? C57B C58B 1.527(16) . ? C58B C59B 1.525(15) . ? C59B C60B 1.486(16) . ? C60B C61B 1.503(17) . ? C61B C62B 1.529(19) . ? S1C O1C 1.412(8) . ? S1C O2C 1.445(9) . ? S1C C9C 1.765(12) . ? S1C C12C 1.803(12) . ? F1C C3C 1.387(13) . ? F2C C6C 1.364(13) . ? C1C C12C 1.332(15) . ? C1C C2C 1.396(16) . ? C2C C3C 1.353(16) . ? C2C C13C 1.494(15) . ? C3C C4C 1.349(15) . ? C4C C11C 1.396(15) . ? C5C C10C 1.383(16) . ? C5C C6C 1.389(15) . ? C6C C7C 1.378(16) . ? C7C C8C 1.407(15) . ? C7C C38C 1.483(15) . ? C8C C9C 1.353(15) . ? C9C C10C 1.445(16) . ? C10C C11C 1.415(15) . ? C11C C12C 1.405(15) . ? C13C C14C 1.386(16) . ? C13C C25C 1.427(16) . ? C14C C15C 1.355(16) . ? C15C C16C 1.367(16) . ? C16C C24C 1.415(16) . ? C16C C17C 1.469(17) . ? C17C C18C 1.410(18) . ? C17C C22C 1.406(18) . ? C18C C19C 1.376(18) . ? C19C C20C 1.367(19) . ? C20C C21C 1.410(18) . ? C21C C22C 1.384(17) . ? C22C C23C 1.485(17) . ? C23C C26C 1.523(17) . ? C23C C24C 1.535(16) . ? C23C C32C 1.590(19) . ? C24C C25C 1.380(15) . ? C26C C27C 1.547(18) . ? C27C C28C 1.515(18) . ? C28C C29C 1.502(18) . ? C29C C30C 1.565(19) . ? C30C C31C 1.538(19) . ? C32C C33C 1.48(2) . ? C33C C34C 1.60(2) . ? C34C C35C 1.473(17) . ? C35C C36C 1.527(17) . ? C36C C37C 1.466(17) . ? C38C C39C 1.360(15) . ? C38C C50C 1.429(15) . ? C39C C40C 1.364(15) . ? C40C C41C 1.369(16) . ? C41C C49C 1.369(16) . ? C41C C42C 1.468(16) . ? C42C C47C 1.390(16) . ? C42C C43C 1.403(17) . ? C43C C44C 1.352(17) . ? C44C C45C 1.372(18) . ? C45C C46C 1.409(17) . ? C46C C47C 1.389(16) . ? C47C C48C 1.529(17) . ? C48C C51C 1.530(16) . ? C48C C49C 1.550(16) . ? C48C C57C 1.559(17) . ? C49C C50C 1.402(16) . ? C51C C52C 1.551(17) . ? C52C C53C 1.496(15) . ? C53C C54C 1.502(16) . ? C54C C55C 1.507(18) . ? C55C C56C 1.502(18) . ? C57C C58C 1.509(15) . ? C58C C59C 1.568(16) . ? C59C C60C 1.514(16) . ? C60C C61C 1.539(18) . ? C61C C62C 1.51(2) . ? S1D O1D 1.433(9) . ? S1D O2D 1.455(9) . ? S1D C9D 1.752(11) . ? S1D C12D 1.779(12) . ? F1D C3D 1.365(13) . ? F2D C6D 1.382(13) . ? C1D C12D 1.341(15) . ? C1D C2D 1.408(15) . ? C2D C3D 1.393(16) . ? C2D C13D 1.477(15) . ? C3D C4D 1.368(15) . ? C4D C11D 1.386(15) . ? C5D C6D 1.347(15) . ? C5D C10D 1.418(15) . ? C6D C7D 1.402(16) . ? C7D C8D 1.412(15) . ? C7D C38D 1.445(15) . ? C8D C9D 1.385(15) . ? C9D C10D 1.389(15) . ? C10D C11D 1.408(15) . ? C11D C12D 1.420(16) . ? C13D C14D 1.402(15) . ? C13D C25D 1.401(15) . ? C14D C15D 1.360(15) . ? C15D C16D 1.389(15) . ? C16D C24D 1.384(15) . ? C16D C17D 1.493(15) . ? C17D C22D 1.378(15) . ? C17D C18D 1.381(16) . ? C18D C19D 1.368(16) . ? C19D C20D 1.360(17) . ? C20D C21D 1.399(17) . ? C21D C22D 1.379(16) . ? C22D C23D 1.534(15) . ? C23D C26D 1.522(15) . ? C23D C24D 1.523(15) . ? C23D C32D 1.536(15) . ? C24D C25D 1.394(15) . ? C26D C27D 1.542(16) . ? C27D C28D 1.520(15) . ? C27D C28E 1.555(16) . ? C28D C29D 1.551(15) . ? C29D C30D 1.498(16) . ? C28E C29E 1.563(17) . ? C29E C30D 1.560(16) . ? C30D C31D 1.53(2) . ? C32D C33D 1.501(14) . ? C33D C34D 1.550(16) . ? C34D C35D 1.517(16) . ? C35D C36D 1.548(17) . ? C36D C37D 1.515(17) . ? C38D C50D 1.393(15) . ? C38D C39D 1.405(15) . ? C39D C40D 1.349(15) . ? C40D C41D 1.412(15) . ? C41D C49D 1.420(16) . ? C41D C42D 1.451(15) . ? C42D C47D 1.394(15) . ? C42D C43D 1.415(16) . ? C43D C44D 1.394(16) . ? C44D C45D 1.369(17) . ? C45D C46D 1.398(16) . ? C46D C47D 1.379(15) . ? C47D C48D 1.515(16) . ? C48D C49D 1.507(16) . ? C48D C51D 1.511(17) . ? C48D C57D 1.569(17) . ? C49D C50D 1.419(16) . ? C51D C52D 1.561(19) . ? C52D C53E 1.521(16) . ? C52D C53D 1.544(15) . ? C53D C54D 1.511(15) . ? C54D C55D 1.548(15) . ? C53E C54E 1.525(16) . ? C54E C55D 1.539(16) . ? C55D C56D 1.504(15) . ? C57D C58D 1.495(18) . ? C58D C59D 1.531(19) . ? C59D C60D 1.494(19) . ? C60D C61D 1.48(2) . ? C61D C62D 1.544(19) . ? 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 O1A S1A O2A 117.3(5) . . ? O1A S1A C9A 111.1(5) . . ? O2A S1A C9A 110.6(5) . . ? O1A S1A C12A 111.9(5) . . ? O2A S1A C12A 110.2(5) . . ? C9A S1A C12A 93.1(5) . . ? C12A C1A C2A 119.5(11) . . ? C3A C2A C1A 115.2(10) . . ? C3A C2A C13A 123.4(10) . . ? C1A C2A C13A 121.4(10) . . ? C4A C3A F1A 115.9(10) . . ? C4A C3A C2A 125.9(11) . . ? F1A C3A C2A 118.2(9) . . ? C3A C4A C11A 118.0(11) . . ? C6A C5A C10A 120.2(11) . . ? C5A C6A F2A 117.9(10) . . ? C5A C6A C7A 123.2(10) . . ? F2A C6A C7A 118.9(9) . . ? C6A C7A C8A 116.2(10) . . ? C6A C7A C38A 121.5(10) . . ? C8A C7A C38A 122.2(10) . . ? C9A C8A C7A 120.8(11) . . ? C8A C9A C10A 120.6(11) . . ? C8A C9A S1A 127.0(9) . . ? C10A C9A S1A 112.2(8) . . ? C5A C10A C9A 118.9(10) . . ? C5A C10A C11A 131.2(10) . . ? C9A C10A C11A 109.9(9) . . ? C12A C11A C4A 116.7(9) . . ? C12A C11A C10A 114.9(9) . . ? C4A C11A C10A 128.3(10) . . ? C1A C12A C11A 124.6(10) . . ? C1A C12A S1A 125.4(9) . . ? C11A C12A S1A 109.8(7) . . ? C25A C13A C14A 119.9(10) . . ? C25A C13A C2A 122.8(10) . . ? C14A C13A C2A 117.2(10) . . ? C15A C14A C13A 120.5(11) . . ? C14A C15A C16A 121.0(11) . . ? C24A C16A C15A 117.4(10) . . ? C24A C16A C17A 110.4(10) . . ? C15A C16A C17A 132.2(11) . . ? C22A C17A C18A 122.1(11) . . ? C22A C17A C16A 108.1(10) . . ? C18A C17A C16A 129.8(11) . . ? C17A C18A C19A 116.2(12) . . ? C20A C19A C18A 122.0(12) . . ? C21A C20A C19A 119.4(11) . . ? C20A C21A C22A 119.5(12) . . ? C17A C22A C21A 120.6(11) . . ? C17A C22A C23A 113.6(10) . . ? C21A C22A C23A 125.8(11) . . ? C26A C23A C32A 111.4(10) . . ? C26A C23A C22A 110.7(9) . . ? C32A C23A C22A 110.7(10) . . ? C26A C23A C24A 111.9(10) . . ? C32A C23A C24A 113.4(9) . . ? C22A C23A C24A 98.0(9) . . ? C16A C24A C25A 122.5(10) . . ? C16A C24A C23A 109.9(9) . . ? C25A C24A C23A 127.5(10) . . ? C13A C25A C24A 118.5(11) . . ? C23A C26A C27A 116.7(11) . . ? C26A C27A C28A 113.1(11) . . ? C29A C28A C27A 116.8(12) . . ? C30A C29A C28A 110.9(12) . . ? C29A C30A C31A 113.0(12) . . ? C23A C32A C33A 117.4(10) . . ? C32A C33A C34A 113.1(11) . . ? C35A C34A C33A 109.7(10) . . ? C36A C35A C34A 111.1(10) . . ? C35A C36A C37A 111.0(11) . . ? C50A C38A C39A 118.7(11) . . ? C50A C38A C7A 125.1(11) . . ? C39A C38A C7A 115.8(9) . . ? C40A C39A C38A 120.5(10) . . ? C41A C40A C39A 117.9(11) . . ? C40A C41A C49A 123.3(10) . . ? C40A C41A C42A 132.0(11) . . ? C49A C41A C42A 104.8(9) . . ? C47A C42A C43A 120.5(10) . . ? C47A C42A C41A 110.5(10) . . ? C43A C42A C41A 128.9(11) . . ? C44A C43A C42A 119.3(12) . . ? C45A C44A C43A 119.6(13) . . ? C44A C45A C46A 122.5(13) . . ? C47A C46A C45A 116.2(12) . . ? C42A C47A C46A 121.6(11) . . ? C42A C47A C48A 110.5(9) . . ? C46A C47A C48A 127.9(11) . . ? C49A C48A C47A 101.2(9) . . ? C49A C48A C51A 113.6(10) . . ? C47A C48A C51A 110.4(9) . . ? C49A C48A C57A 112.1(9) . . ? C47A C48A C57A 111.1(9) . . ? C51A C48A C57A 108.3(10) . . ? C50A C49A C41A 115.7(10) . . ? C50A C49A C48A 131.3(11) . . ? C41A C49A C48A 113.0(9) . . ? C38A C50A C49A 123.9(12) . . ? C48A C51A C52A 113.6(10) . . ? C53A C52A C51A 115.4(11) . . ? C54A C53A C52A 117.1(11) . . ? C53A C54A C55A 110.8(10) . . ? C56A C55A C54A 114.0(12) . . ? C58A C57A C48A 115.0(10) . . ? C57A C58A C59A 113.3(10) . . ? C60A C59A C58A 113.1(11) . . ? C59A C60A C61A 112.9(12) . . ? C62A C61A C60A 112.4(13) . . ? O1B S1B O2B 119.0(5) . . ? O1B S1B C9B 110.4(5) . . ? O2B S1B C9B 110.3(5) . . ? O1B S1B C12B 111.9(5) . . ? O2B S1B C12B 109.0(5) . . ? C9B S1B C12B 93.2(5) . . ? C12B C1B C2B 119.3(11) . . ? C3B C2B C1B 114.6(10) . . ? C3B C2B C13B 123.9(11) . . ? C1B C2B C13B 121.2(10) . . ? F1B C3B C4B 116.6(11) . . ? F1B C3B C2B 116.7(10) . . ? C4B C3B C2B 126.7(12) . . ? C3B C4B C11B 118.9(12) . . ? C6B C5B C10B 119.6(11) . . ? C5B C6B F2B 118.3(10) . . ? C5B C6B C7B 124.5(11) . . ? F2B C6B C7B 117.2(9) . . ? C8B C7B C6B 115.4(10) . . ? C8B C7B C38B 121.6(10) . . ? C6B C7B C38B 123.0(10) . . ? C7B C8B C9B 121.2(11) . . ? C10B C9B C8B 121.9(11) . . ? C10B C9B S1B 110.3(8) . . ? C8B C9B S1B 127.7(9) . . ? C9B C10B C5B 117.1(10) . . ? C9B C10B C11B 115.1(10) . . ? C5B C10B C11B 127.7(11) . . ? C4B C11B C12B 116.8(10) . . ? C4B C11B C10B 131.4(11) . . ? C12B C11B C10B 111.7(10) . . ? C1B C12B C11B 123.7(11) . . ? C1B C12B S1B 126.5(9) . . ? C11B C12B S1B 109.7(8) . . ? C14B C13B C25B 118.5(10) . . ? C14B C13B C2B 120.0(10) . . ? C25B C13B C2B 121.5(10) . . ? C15B C14B C13B 122.2(11) . . ? C14B C15B C16B 117.6(11) . . ? C24B C16B C15B 122.2(10) . . ? C24B C16B C17B 108.7(10) . . ? C15B C16B C17B 129.1(11) . . ? C18B C17B C22B 121.3(10) . . ? C18B C17B C16B 131.5(10) . . ? C22B C17B C16B 107.2(10) . . ? C17B C18B C19B 118.0(11) . . ? C18B C19B C20B 120.6(12) . . ? C21B C20B C19B 121.0(12) . . ? C20B C21B C22B 118.8(12) . . ? C21B C22B C17B 120.5(11) . . ? C21B C22B C23B 127.1(11) . . ? C17B C22B C23B 112.5(9) . . ? C22B C23B C32B 112.9(10) . . ? C22B C23B C24B 100.2(9) . . ? C32B C23B C24B 113.8(9) . . ? C22B C23B C26B 112.2(9) . . ? C32B C23B C26B 108.7(9) . . ? C24B C23B C26B 108.8(9) . . ? C25B C24B C16B 119.8(10) . . ? C25B C24B C23B 128.8(10) . . ? C16B C24B C23B 111.4(9) . . ? C24B C25B C13B 119.5(11) . . ? C27B C26B C23B 115.6(10) . . ? C26B C27B C28B 112.5(10) . . ? C29B C28B C27B 115.3(11) . . ? C30B C29B C28B 113.6(12) . . ? C29B C30B C31B 112.9(12) . . ? C33B C32B C23B 116.9(10) . . ? C32B C33B C34B 114.6(10) . . ? C33B C34B C35B 114.2(11) . . ? C34B C35B C36B 116.3(12) . . ? C37B C36B C35B 110.8(12) . . ? C39B C38B C50B 119.5(11) . . ? C39B C38B C7B 119.6(10) . . ? C50B C38B C7B 121.0(10) . . ? C38B C39B C40B 120.9(11) . . ? C41B C40B C39B 118.8(11) . . ? C40B C41B C49B 119.6(10) . . ? C40B C41B C42B 131.6(10) . . ? C49B C41B C42B 108.8(9) . . ? C47B C42B C43B 120.2(10) . . ? C47B C42B C41B 108.8(10) . . ? C43B C42B C41B 131.0(11) . . ? C44B C43B C42B 118.0(12) . . ? C45B C44B C43B 122.1(13) . . ? C44B C45B C46B 120.1(12) . . ? C45B C46B C47B 118.8(12) . . ? C42B C47B C46B 120.9(11) . . ? C42B C47B C48B 111.4(10) . . ? C46B C47B C48B 127.7(11) . . ? C57B C48B C47B 114.1(9) . . ? C57B C48B C49B 113.6(9) . . ? C47B C48B C49B 100.3(9) . . ? C57B C48B C51B 107.4(10) . . ? C47B C48B C51B 110.8(9) . . ? C49B C48B C51B 110.6(9) . . ? C50B C49B C41B 121.0(10) . . ? C50B C49B C48B 128.4(10) . . ? C41B C49B C48B 110.5(9) . . ? C49B C50B C38B 120.1(11) . . ? C52B C51B C48B 115.0(10) . . ? C51B C52B C53B 113.9(10) . . ? C52B C53B C54B 114.5(10) . . ? C55B C54B C53B 114.4(11) . . ? C56B C55B C54B 114.7(12) . . ? C48B C57B C58B 117.1(10) . . ? C59B C58B C57B 111.2(10) . . ? C60B C59B C58B 114.7(10) . . ? C61B C60B C59B 114.5(11) . . ? C60B C61B C62B 112.8(12) . . ? O1C S1C O2C 116.7(5) . . ? O1C S1C C9C 110.0(5) . . ? O2C S1C C9C 110.8(5) . . ? O1C S1C C12C 109.9(5) . . ? O2C S1C C12C 113.0(5) . . ? C9C S1C C12C 94.2(5) . . ? C12C C1C C2C 119.7(11) . . ? C3C C2C C1C 114.9(10) . . ? C3C C2C C13C 126.0(11) . . ? C1C C2C C13C 119.1(10) . . ? C4C C3C C2C 126.8(12) . . ? C4C C3C F1C 116.6(11) . . ? C2C C3C F1C 116.5(10) . . ? C3C C4C C11C 118.9(11) . . ? C10C C5C C6C 119.1(11) . . ? F2C C6C C7C 117.4(9) . . ? F2C C6C C5C 117.1(10) . . ? C7C C6C C5C 125.4(11) . . ? C6C C7C C8C 115.7(10) . . ? C6C C7C C38C 125.8(10) . . ? C8C C7C C38C 118.5(10) . . ? C9C C8C C7C 120.3(11) . . ? C8C C9C C10C 123.6(11) . . ? C8C C9C S1C 128.3(9) . . ? C10C C9C S1C 107.9(8) . . ? C5C C10C C11C 129.8(11) . . ? C5C C10C C9C 115.7(10) . . ? C11C C10C C9C 114.5(10) . . ? C4C C11C C12C 114.2(10) . . ? C4C C11C C10C 130.4(11) . . ? C12C C11C C10C 115.3(10) . . ? C1C C12C C11C 125.4(11) . . ? C1C C12C S1C 126.6(10) . . ? C11C C12C S1C 108.0(8) . . ? C14C C13C C25C 117.8(10) . . ? C14C C13C C2C 120.9(10) . . ? C25C C13C C2C 121.3(10) . . ? C15C C14C C13C 122.6(12) . . ? C16C C15C C14C 120.5(13) . . ? C15C C16C C24C 119.0(11) . . ? C15C C16C C17C 134.3(12) . . ? C24C C16C C17C 106.5(10) . . ? C18C C17C C22C 122.5(12) . . ? C18C C17C C16C 127.5(12) . . ? C22C C17C C16C 110.0(11) . . ? C19C C18C C17C 118.1(14) . . ? C20C C19C C18C 121.1(14) . . ? C19C C20C C21C 120.5(13) . . ? C22C C21C C20C 120.8(13) . . ? C21C C22C C17C 117.1(12) . . ? C21C C22C C23C 132.2(12) . . ? C17C C22C C23C 110.3(11) . . ? C22C C23C C26C 110.8(10) . . ? C22C C23C C24C 102.4(10) . . ? C26C C23C C24C 110.6(10) . . ? C22C C23C C32C 112.0(11) . . ? C26C C23C C32C 113.0(11) . . ? C24C C23C C32C 107.6(10) . . ? C25C C24C C16C 120.9(11) . . ? C25C C24C C23C 128.6(11) . . ? C16C C24C C23C 110.5(10) . . ? C24C C25C C13C 119.0(11) . . ? C23C C26C C27C 113.9(11) . . ? C28C C27C C26C 114.0(11) . . ? C29C C28C C27C 110.9(12) . . ? C28C C29C C30C 114.9(12) . . ? C31C C30C C29C 113.9(13) . . ? C33C C32C C23C 115.8(12) . . ? C32C C33C C34C 111.1(15) . . ? C35C C34C C33C 115.1(19) . . ? C34C C35C C36C 129(2) . . ? C37C C36C C35C 100.7(19) . . ? C39C C38C C50C 116.4(10) . . ? C39C C38C C7C 123.6(10) . . ? C50C C38C C7C 119.9(10) . . ? C38C C39C C40C 124.8(11) . . ? C39C C40C C41C 119.0(12) . . ? C49C C41C C40C 119.5(11) . . ? C49C C41C C42C 108.6(10) . . ? C40C C41C C42C 131.8(12) . . ? C47C C42C C43C 121.8(11) . . ? C47C C42C C41C 107.8(11) . . ? C43C C42C C41C 130.5(12) . . ? C44C C43C C42C 116.5(13) . . ? C43C C44C C45C 122.6(13) . . ? C44C C45C C46C 121.9(12) . . ? C47C C46C C45C 115.8(12) . . ? C42C C47C C46C 121.1(12) . . ? C42C C47C C48C 112.8(10) . . ? C46C C47C C48C 126.1(11) . . ? C51C C48C C47C 112.0(10) . . ? C51C C48C C49C 113.4(10) . . ? C47C C48C C49C 98.3(10) . . ? C51C C48C C57C 109.3(10) . . ? C47C C48C C57C 113.9(10) . . ? C49C C48C C57C 109.8(10) . . ? C41C C49C C50C 121.7(11) . . ? C41C C49C C48C 112.6(10) . . ? C50C C49C C48C 125.7(11) . . ? C49C C50C C38C 118.5(11) . . ? C48C C51C C52C 114.6(10) . . ? C53C C52C C51C 113.7(10) . . ? C52C C53C C54C 117.6(10) . . ? C53C C54C C55C 113.9(11) . . ? C56C C55C C54C 113.7(12) . . ? C58C C57C C48C 113.5(10) . . ? C57C C58C C59C 114.8(10) . . ? C60C C59C C58C 112.7(10) . . ? C59C C60C C61C 109.8(10) . . ? C62C C61C C60C 114.1(12) . . ? O1D S1D O2D 117.3(5) . . ? O1D S1D C9D 110.6(5) . . ? O2D S1D C9D 110.6(5) . . ? O1D S1D C12D 111.5(5) . . ? O2D S1D C12D 111.1(5) . . ? C9D S1D C12D 93.2(6) . . ? C12D C1D C2D 119.5(11) . . ? C3D C2D C1D 115.4(10) . . ? C3D C2D C13D 123.0(10) . . ? C1D C2D C13D 121.5(10) . . ? F1D C3D C4D 117.9(10) . . ? F1D C3D C2D 116.8(9) . . ? C4D C3D C2D 125.3(11) . . ? C3D C4D C11D 119.1(11) . . ? C6D C5D C10D 118.6(11) . . ? C5D C6D F2D 116.9(11) . . ? C5D C6D C7D 127.0(11) . . ? F2D C6D C7D 116.1(10) . . ? C6D C7D C8D 113.5(10) . . ? C6D C7D C38D 125.2(10) . . ? C8D C7D C38D 121.2(10) . . ? C9D C8D C7D 121.0(11) . . ? C8D C9D C10D 123.2(10) . . ? C8D C9D S1D 127.1(9) . . ? C10D C9D S1D 109.8(8) . . ? C9D C10D C11D 114.8(10) . . ? C9D C10D C5D 116.7(10) . . ? C11D C10D C5D 128.3(11) . . ? C4D C11D C10D 130.5(11) . . ? C4D C11D C12D 115.6(10) . . ? C10D C11D C12D 113.9(10) . . ? C1D C12D C11D 124.9(11) . . ? C1D C12D S1D 126.9(10) . . ? C11D C12D S1D 108.2(8) . . ? C14D C13D C25D 119.2(10) . . ? C14D C13D C2D 119.2(10) . . ? C25D C13D C2D 121.7(10) . . ? C15D C14D C13D 121.7(11) . . ? C14D C15D C16D 118.6(11) . . ? C24D C16D C15D 121.4(10) . . ? C24D C16D C17D 107.5(9) . . ? C15D C16D C17D 131.1(10) . . ? C22D C17D C18D 121.1(10) . . ? C22D C17D C16D 108.3(10) . . ? C18D C17D C16D 130.6(10) . . ? C19D C18D C17D 118.6(12) . . ? C20D C19D C18D 120.9(12) . . ? C19D C20D C21D 121.1(12) . . ? C22D C21D C20D 117.9(12) . . ? C17D C22D C21D 120.3(11) . . ? C17D C22D C23D 111.6(9) . . ? C21D C22D C23D 128.0(11) . . ? C26D C23D C24D 112.1(9) . . ? C26D C23D C32D 108.2(9) . . ? C24D C23D C32D 111.1(9) . . ? C26D C23D C22D 112.7(9) . . ? C24D C23D C22D 100.0(9) . . ? C32D C23D C22D 112.7(9) . . ? C16D C24D C25D 119.8(10) . . ? C16D C24D C23D 112.2(9) . . ? C25D C24D C23D 128.0(10) . . ? C24D C25D C13D 119.2(10) . . ? C23D C26D C27D 116.0(10) . . ? C28D C27D C26D 116.0(11) . . ? C26D C27D C28E 107.4(13) . . ? C27D C28D C29D 114.3(14) . . ? C30D C29D C28D 109.9(15) . . ? C27D C28E C29E 109.0(19) . . ? C30D C29E C28E 125(2) . . ? C29D C30D C31D 102.5(17) . . ? C31D C30D C29E 124.9(19) . . ? C33D C32D C23D 114.8(9) . . ? C32D C33D C34D 110.8(9) . . ? C35D C34D C33D 112.9(10) . . ? C34D C35D C36D 114.1(11) . . ? C37D C36D C35D 112.7(11) . . ? C50D C38D C39D 118.4(10) . . ? C50D C38D C7D 122.5(11) . . ? C39D C38D C7D 119.1(10) . . ? C40D C39D C38D 124.6(11) . . ? C39D C40D C41D 117.6(11) . . ? C40D C41D C49D 120.2(10) . . ? C40D C41D C42D 133.2(11) . . ? C49D C41D C42D 106.6(10) . . ? C47D C42D C43D 120.1(10) . . ? C47D C42D C41D 110.1(10) . . ? C43D C42D C41D 129.8(11) . . ? C44D C43D C42D 118.0(11) . . ? C45D C44D C43D 121.4(12) . . ? C44D C45D C46D 120.5(12) . . ? C47D C46D C45D 119.3(11) . . ? C46D C47D C42D 120.6(11) . . ? C46D C47D C48D 128.9(11) . . ? C42D C47D C48D 110.4(9) . . ? C49D C48D C51D 113.2(10) . . ? C49D C48D C47D 101.3(9) . . ? C51D C48D C47D 111.3(10) . . ? C49D C48D C57D 111.7(10) . . ? C51D C48D C57D 106.2(10) . . ? C47D C48D C57D 113.3(10) . . ? C41D C49D C50D 119.8(10) . . ? C41D C49D C48D 111.6(10) . . ? C50D C49D C48D 128.4(11) . . ? C38D C50D C49D 119.2(11) . . ? C48D C51D C52D 115.6(11) . . ? C53E C52D C51D 130.0(15) . . ? C51D C52D C53D 101.3(12) . . ? C54D C53D C52D 111.8(15) . . ? C53D C54D C55D 103.7(14) . . ? C52D C53E C54E 109.3(15) . . ? C53E C54E C55D 107.4(16) . . ? C56D C55D C54E 96.7(17) . . ? C56D C55D C54D 132.0(17) . . ? C58D C57D C48D 116.9(11) . . ? C57D C58D C59D 112.0(12) . . ? C60D C59D C58D 119.1(13) . . ? C61D C60D C59D 114.9(14) . . ? C60D C61D C62D 113.6(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.847 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.096 #===================END data_4 _database_code_depnum_ccdc_archive 'CCDC 768386' #TrackingRef '- Li.cif' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C76 H96 O4 S' _chemical_formula_sum 'C76 H96 O4 S' _chemical_formula_weight 1105.59 _chemical_melting_point 452.8(6) _chemical_name_common ? _chemical_name_systematic ; 3,7-Bis(9,9-dihexylfluorene-2-yl)-2,8-di(cyclohexylmethoxy)dibenzothiophene-S,S-dioxide ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 32.509(3) _cell_length_b 32.509(3) _cell_length_c 12.3994(15) _cell_measurement_reflns_used 7739 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 21.62 _cell_measurement_theta_min 2.16 _cell_volume 13104(2) _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_F_000 4800 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of 3 runs of narrow-frame \w-scans (scan width 0.3\% \w, 45s exposure), every run at a different \f angle. Crystal to detector distance 4.83 cm. Weak diffraction: mean I/\s(I)=3.4. 6299 unique reflections after merging Friedel equivalents. ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 1.00 0.00 0.0300 -1.00 -1.00 0.00 0.0300 1.00 -1.00 0.00 0.0250 -1.00 1.00 0.00 0.0250 0.00 0.00 1.00 0.2150 0.00 0.00 -1.00 0.2150 _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 5.6 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2021 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 121430 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 1.25 _diffrn_source_current 35.0 _diffrn_source_power 1.75 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.84 _reflns_number_gt 7076 _reflns_number_total 11571 _reflns_threshold_expression I>2\s(I) _computing_cell_refinement 'SAINT version 7.46A (Bruker, 2007)' _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 7.46A (Bruker, 2007)' _computing_molecular_graphics ; Olex2, Durham University (compiled Nov 21 2008 17:47:00) ; _computing_publication_material ; Olex2, Durham University (compiled Nov 21 2008 17:47:00) ; _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)/Bruker' _refine_diff_density_max 0.481 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.053 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0615 _refine_ls_abs_structure_Flack 0.10(11) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_extinction_coef 0.0024(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 748 _refine_ls_number_reflns 11571 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.1388 _refine_ls_wR_factor_ref 0.1603 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. The C(75)H~2~C(76)H~2~C(77)H~3~ chain is disordered equally between two positions (unprimed and primed labels). The C(77) atom nearly overlaps with the C(77 ) of another molecule, related to the first by the symmetry operation 3/2-y, 3/2-x, 1/2+z (interatomic distances 0.51 \%A), hence these two positions cannot be occupied simultaneously. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.78749(3) 0.61773(3) 0.23662(8) 0.0290(2) Uani 1 1 d . . . O1 O 0.78640(8) 0.57337(7) 0.2434(2) 0.0364(7) Uani 1 1 d . . . O2 O 0.77107(8) 0.63529(8) 0.1394(2) 0.0319(7) Uani 1 1 d . . . O3 O 0.73193(8) 0.70247(9) 0.6263(2) 0.0377(7) Uani 1 1 d . . . O4 O 0.94479(8) 0.69174(9) 0.3639(2) 0.0364(7) Uani 1 1 d . . . C1 C 0.72438(12) 0.64388(12) 0.3802(3) 0.0315(10) Uani 1 1 d . . . H1 H 0.7040 0.6309 0.3372 0.038 Uiso 1 1 d R . . C2 C 0.71340(12) 0.66568(12) 0.4712(3) 0.0314(9) Uani 1 1 d . . . C3 C 0.74442(12) 0.68310(12) 0.5361(3) 0.0301(10) Uani 1 1 d . . . C4 C 0.78588(12) 0.67999(12) 0.5068(3) 0.0299(9) Uani 1 1 d . . . H4 H 0.8067 0.6916 0.5513 0.036 Uiso 1 1 d R . . C5 C 0.87339(12) 0.67614(12) 0.3987(3) 0.0298(10) Uani 1 1 d . . . H5 H 0.8741 0.6900 0.4661 0.036 Uiso 1 1 d R . . C6 C 0.90846(12) 0.67363(12) 0.3344(3) 0.0305(10) Uani 1 1 d . . . C7 C 0.90798(12) 0.65405(12) 0.2334(3) 0.0315(9) Uani 1 1 d . . . C8 C 0.87166(11) 0.63494(12) 0.1995(3) 0.0296(10) Uani 1 1 d . . . H8 H 0.8705 0.6209 0.1325 0.036 Uiso 1 1 d R . . C9 C 0.83679(11) 0.63701(11) 0.2660(3) 0.0282(9) Uani 1 1 d . . . C10 C 0.83740(11) 0.65788(12) 0.3618(3) 0.0288(9) Uani 1 1 d . . . C11 C 0.79615(12) 0.66011(12) 0.4133(3) 0.0286(9) Uani 1 1 d . . . C12 C 0.76596(12) 0.64101(12) 0.3522(3) 0.0289(9) Uani 1 1 d . . . C13 C 0.76280(12) 0.71900(14) 0.6969(3) 0.0384(11) Uani 1 1 d . . . H13B H 0.7792 0.7400 0.6582 0.046 Uiso 1 1 d R . . H13A H 0.7816 0.6969 0.7211 0.046 Uiso 1 1 d R . . C14 C 0.74168(13) 0.73847(14) 0.7927(4) 0.0397(11) Uani 1 1 d . . . H14 H 0.7635 0.7523 0.8365 0.048 Uiso 1 1 calc R . . C15 C 0.72141(16) 0.70772(17) 0.8640(4) 0.0586(14) Uani 1 1 d . . . H15B H 0.7419 0.6871 0.8875 0.070 Uiso 1 1 d R . . H15A H 0.6995 0.6932 0.8236 0.070 Uiso 1 1 d R . . C16 C 0.7028(2) 0.7285(2) 0.9633(5) 0.0821(19) Uani 1 1 d . . . H16A H 0.6897 0.7076 1.0101 0.098 Uiso 1 1 d R . . H16B H 0.7248 0.7422 1.0054 0.098 Uiso 1 1 d R . . C17 C 0.67109(17) 0.7599(2) 0.9277(5) 0.0732(18) Uani 1 1 d . . . H17B H 0.6593 0.7737 0.9919 0.088 Uiso 1 1 d R . . H17A H 0.6485 0.7460 0.8888 0.088 Uiso 1 1 d R . . C18 C 0.69082(15) 0.79170(18) 0.8546(4) 0.0608(15) Uani 1 1 d . . . H18B H 0.6696 0.8114 0.8299 0.073 Uiso 1 1 d R . . H18A H 0.7118 0.8072 0.8958 0.073 Uiso 1 1 d R . . C19 C 0.71107(14) 0.77178(14) 0.7582(4) 0.0458(11) Uani 1 1 d . . . H19B H 0.7256 0.7930 0.7155 0.055 Uiso 1 1 d R . . H19A H 0.6897 0.7593 0.7118 0.055 Uiso 1 1 d R . . C20 C 0.94403(12) 0.71827(14) 0.4561(4) 0.0395(11) Uani 1 1 d . . . H20A H 0.9352 0.7026 0.5205 0.047 Uiso 1 1 d R . . H20B H 0.9242 0.7409 0.4441 0.047 Uiso 1 1 d R . . C21 C 0.98637(12) 0.73563(14) 0.4741(3) 0.0383(11) Uani 1 1 d . . . H21 H 0.9968 0.7467 0.4040 0.046 Uiso 1 1 calc R . . C22 C 1.01587(13) 0.70358(16) 0.5130(4) 0.0510(13) Uani 1 1 d . . . H22A H 1.0189 0.6821 0.4570 0.061 Uiso 1 1 d R . . H22B H 1.0046 0.6904 0.5786 0.061 Uiso 1 1 d R . . C23 C 1.05797(15) 0.7215(2) 0.5392(5) 0.0697(17) Uani 1 1 d . . . H23A H 1.0761 0.6997 0.5686 0.084 Uiso 1 1 d R . . H23B H 1.0706 0.7320 0.4721 0.084 Uiso 1 1 d R . . C24 C 1.05440(16) 0.75591(19) 0.6197(5) 0.0686(17) Uani 1 1 d . . . H24B H 1.0820 0.7678 0.6331 0.082 Uiso 1 1 d R . . H24A H 1.0440 0.7448 0.6888 0.082 Uiso 1 1 d R . . C25 C 1.02588(15) 0.78946(17) 0.5803(5) 0.0605(15) Uani 1 1 d . . . H25A H 1.0374 0.8024 0.5147 0.073 Uiso 1 1 d R . . H25B H 1.0231 0.8109 0.6365 0.073 Uiso 1 1 d R . . C26 C 0.98333(14) 0.77117(14) 0.5545(4) 0.0487(13) Uani 1 1 d . . . H26A H 0.9706 0.7612 0.6221 0.058 Uiso 1 1 d R . . H26B H 0.9653 0.7929 0.5243 0.058 Uiso 1 1 d R . . C27 C 0.66933(12) 0.67250(13) 0.4992(3) 0.0329(10) Uani 1 1 d . . . C28 C 0.65452(12) 0.71239(13) 0.5122(3) 0.0321(10) Uani 1 1 d . . . H28 H 0.6727 0.7350 0.5032 0.038 Uiso 1 1 d R . . C29 C 0.61378(12) 0.71950(13) 0.5377(3) 0.0346(10) Uani 1 1 d . . . H29 H 0.6038 0.7469 0.5443 0.042 Uiso 1 1 d R . . C30 C 0.58755(12) 0.68651(12) 0.5542(3) 0.0300(9) Uani 1 1 d . . . C31 C 0.54432(12) 0.68425(13) 0.5901(3) 0.0343(10) Uani 1 1 d . . . C32 C 0.51540(13) 0.71580(14) 0.6056(4) 0.0407(11) Uani 1 1 d . . . H32 H 0.5222 0.7437 0.5921 0.049 Uiso 1 1 d R . . C33 C 0.47682(13) 0.70466(15) 0.6412(4) 0.0464(12) Uani 1 1 d . . . H33 H 0.4565 0.7252 0.6516 0.056 Uiso 1 1 d R . . C34 C 0.46729(13) 0.66439(16) 0.6618(4) 0.0518(13) Uani 1 1 d . . . H34 H 0.4406 0.6574 0.6873 0.062 Uiso 1 1 d R . . C35 C 0.49601(13) 0.63364(15) 0.6460(4) 0.0496(13) Uani 1 1 d . . . H35 H 0.4893 0.6058 0.6614 0.060 Uiso 1 1 d R . . C36 C 0.53452(13) 0.64392(14) 0.6077(4) 0.0397(11) Uani 1 1 d . . . C37 C 0.56970(13) 0.61546(13) 0.5784(4) 0.0434(12) Uani 1 1 d . . . C38 C 0.60238(12) 0.64698(13) 0.5434(4) 0.0360(11) Uani 1 1 d . . . C39 C 0.64266(12) 0.63919(13) 0.5133(4) 0.0379(11) Uani 1 1 d . . . H39 H 0.6519 0.6118 0.5023 0.045 Uiso 1 1 d R . . C40 C 0.58592(15) 0.59107(15) 0.6767(5) 0.0564(14) Uani 1 1 d . . . H40A H 0.5631 0.5741 0.7052 0.068 Uiso 1 1 d R . . H40B H 0.6077 0.5720 0.6516 0.068 Uiso 1 1 d R . . C41 C 0.60295(15) 0.61637(16) 0.7671(4) 0.0579(14) Uani 1 1 d . . . H41A H 0.5798 0.6296 0.8058 0.069 Uiso 1 1 d R . . H41B H 0.6203 0.6385 0.7365 0.069 Uiso 1 1 d R . . C42 C 0.6287(2) 0.5915(2) 0.8468(6) 0.097(2) Uani 1 1 d . . . H42A H 0.6110 0.5704 0.8810 0.116 Uiso 1 1 d R . . H42B H 0.6386 0.6102 0.9042 0.116 Uiso 1 1 d R . . C43 C 0.66764(18) 0.5694(2) 0.7928(6) 0.083(2) Uani 1 1 d . . . H43B H 0.6811 0.5518 0.8475 0.099 Uiso 1 1 d R . . H43A H 0.6577 0.5512 0.7343 0.099 Uiso 1 1 d R . . C44 C 0.69955(19) 0.5988(2) 0.7466(6) 0.092(2) Uani 1 1 d . . . H44B H 0.7144 0.6128 0.8059 0.110 Uiso 1 1 d R . . H44A H 0.6857 0.6201 0.7024 0.110 Uiso 1 1 d R . . C45 C 0.7300(2) 0.5751(3) 0.6794(7) 0.128(3) Uani 1 1 d . . . H45C H 0.7510 0.5938 0.6510 0.192 Uiso 1 1 d R . . H45A H 0.7153 0.5622 0.6193 0.192 Uiso 1 1 d R . . H45B H 0.7433 0.5538 0.7232 0.192 Uiso 1 1 d R . . C46 C 0.55804(13) 0.58583(15) 0.4848(5) 0.0598(16) Uani 1 1 d . . . H46B H 0.5827 0.5696 0.4649 0.072 Uiso 1 1 d R . . H46A H 0.5370 0.5663 0.5118 0.072 Uiso 1 1 d R . . C47 C 0.54139(16) 0.60654(17) 0.3835(5) 0.0608(15) Uani 1 1 d . . . H47B H 0.5604 0.6290 0.3626 0.073 Uiso 1 1 d R . . H47A H 0.5144 0.6191 0.4005 0.073 Uiso 1 1 d R . . C48 C 0.53626(19) 0.57760(19) 0.2878(5) 0.0753(18) Uani 1 1 d . . . H48A H 0.5154 0.5566 0.3063 0.090 Uiso 1 1 d R . . H48B H 0.5626 0.5632 0.2748 0.090 Uiso 1 1 d R . . C49 C 0.5230(2) 0.5993(2) 0.1848(5) 0.0813(19) Uani 1 1 d . . . H49A H 0.4947 0.6099 0.1944 0.098 Uiso 1 1 d R . . H49B H 0.5413 0.6232 0.1731 0.098 Uiso 1 1 d R . . C50 C 0.5237(3) 0.5721(3) 0.0857(6) 0.122(3) Uani 1 1 d . . . H50B H 0.5515 0.5601 0.0781 0.146 Uiso 1 1 d R . . H50A H 0.5040 0.5492 0.0951 0.146 Uiso 1 1 d R . . C51 C 0.5133(3) 0.5958(3) -0.0202(7) 0.135(3) Uani 1 1 d . . . H51A H 0.5142 0.5768 -0.0814 0.202 Uiso 1 1 d R . . H51C H 0.5331 0.6181 -0.0315 0.202 Uiso 1 1 d R . . H51B H 0.4856 0.6075 -0.0139 0.202 Uiso 1 1 d R . . C53 C 0.94341(12) 0.65563(12) 0.1570(4) 0.0341(10) Uani 1 1 d . . . C54 C 0.93669(13) 0.66693(14) 0.0521(4) 0.0402(11) Uani 1 1 d . . . H54 H 0.9094 0.6731 0.0303 0.048 Uiso 1 1 d R . . C55 C 0.96810(12) 0.66987(14) -0.0241(4) 0.0402(11) Uani 1 1 d . . . H55 H 0.9627 0.6777 -0.0966 0.048 Uiso 1 1 d R . . C56 C 1.00771(12) 0.66098(12) 0.0109(3) 0.0334(10) Uani 1 1 d . . . C57 C 1.04701(12) 0.66283(13) -0.0479(3) 0.0347(10) Uani 1 1 d . . . C58 C 1.05601(14) 0.67414(14) -0.1521(4) 0.0431(11) Uani 1 1 d . . . H58 H 1.0345 0.6810 -0.2008 0.052 Uiso 1 1 d R . . C59 C 1.09697(14) 0.67545(14) -0.1858(4) 0.0460(12) Uani 1 1 d . . . H59 H 1.1036 0.6835 -0.2574 0.055 Uiso 1 1 d R . . C60 C 1.12781(13) 0.66491(15) -0.1143(4) 0.0460(13) Uani 1 1 d . . . H60 H 1.1557 0.6664 -0.1369 0.055 Uiso 1 1 d R . . C61 C 1.11887(13) 0.65211(14) -0.0088(4) 0.0448(12) Uani 1 1 d . . . H61 H 1.1402 0.6439 0.0390 0.054 Uiso 1 1 d R . . C62 C 1.07788(12) 0.65177(12) 0.0239(4) 0.0364(11) Uani 1 1 d . . . C63 C 1.06098(12) 0.64144(12) 0.1357(4) 0.0346(10) Uani 1 1 d . . . C64 C 1.01500(12) 0.64856(12) 0.1161(4) 0.0342(10) Uani 1 1 d . . . C65 C 0.98365(12) 0.64575(12) 0.1905(4) 0.0332(10) Uani 1 1 d . . . H65 H 0.9890 0.6375 0.2626 0.040 Uiso 1 1 d R . . C66 C 1.07869(14) 0.66994(13) 0.2210(4) 0.0430(11) Uani 1 1 d . . . H66B H 1.1088 0.6657 0.2235 0.052 Uiso 1 1 d R . . H66A H 1.0675 0.6617 0.2920 0.052 Uiso 1 1 d R . . C67 C 1.07041(13) 0.71598(13) 0.2056(4) 0.0416(11) Uani 1 1 d . . . H67A H 1.0441 0.7234 0.2406 0.050 Uiso 1 1 d R . . H67B H 1.0680 0.7222 0.1277 0.050 Uiso 1 1 d R . . C68 C 1.10539(17) 0.74161(15) 0.2543(5) 0.0626(14) Uani 1 1 d . . . H68A H 1.1110 0.7311 0.3278 0.075 Uiso 1 1 d R . . H68B H 1.1305 0.7371 0.2107 0.075 Uiso 1 1 d R . . C69 C 1.0976(2) 0.78717(17) 0.2619(5) 0.0771(17) Uani 1 1 d . . . H69A H 1.0738 0.7922 0.3098 0.092 Uiso 1 1 d R . . H69B H 1.0907 0.7979 0.1895 0.092 Uiso 1 1 d R . . C70 C 1.1369(3) 0.8111(2) 0.3063(6) 0.111(3) Uani 1 1 d . . . H70A H 1.1440 0.7992 0.3773 0.133 Uiso 1 1 d R . . H70B H 1.1603 0.8058 0.2572 0.133 Uiso 1 1 d R . . C71 C 1.1331(2) 0.8538(2) 0.3187(7) 0.099(2) Uani 1 1 d . . . H71C H 1.1592 0.8653 0.3450 0.148 Uiso 1 1 d R . . H71A H 1.1113 0.8597 0.3708 0.148 Uiso 1 1 d R . . H71B H 1.1262 0.8663 0.2491 0.148 Uiso 1 1 d R . . C72 C 1.07026(13) 0.59619(13) 0.1668(4) 0.0482(13) Uani 1 1 d . . . H72B H 1.1004 0.5930 0.1746 0.058 Uiso 1 1 d R . . H72A H 1.0577 0.5905 0.2380 0.058 Uiso 1 1 d R . . C73 C 1.05521(16) 0.56424(14) 0.0881(5) 0.0618(16) Uani 1 1 d . C . H73B H 1.0646 0.5718 0.0148 0.074 Uiso 1 1 d R . . H73A H 1.0248 0.5645 0.0879 0.074 Uiso 1 1 d R . . C74 C 1.0705(2) 0.52067(18) 0.1140(7) 0.100(3) Uani 1 1 d D . . H74A H 1.1013 0.5222 0.1124 0.119 Uiso 1 1 d R C . H74B H 1.0606 0.5014 0.0614 0.119 Uiso 0.50 1 d PR A 1 H74C H 1.0597 0.5099 0.1803 0.119 Uiso 0.50 1 d PR B 2 C75 C 1.0584(4) 0.5059(3) 0.2370(9) 0.065(3) Uani 0.50 1 d PD C 1 H75B H 1.0710 0.5252 0.2891 0.078 Uiso 0.50 1 d PR C 1 H75A H 1.0282 0.5072 0.2465 0.078 Uiso 0.50 1 d PR C 1 C76 C 1.0739(4) 0.4605(3) 0.2620(9) 0.063(3) Uani 0.50 1 d PD C 1 H76A H 1.0578 0.4413 0.2164 0.075 Uiso 0.50 1 d PR C 1 H76B H 1.1029 0.4586 0.2382 0.075 Uiso 0.50 1 d PR C 1 C77 C 1.0711(5) 0.4439(5) 0.3860(11) 0.082(5) Uiso 0.50 1 d PD C 1 H77A H 1.0817 0.4165 0.3920 0.122 Uiso 0.50 1 d PR C 1 H77B H 1.0843 0.4613 0.4383 0.122 Uiso 0.50 1 d PR C 1 H77C H 1.0420 0.4436 0.3988 0.122 Uiso 0.50 1 d PR C 1 C75' C 1.0557(4) 0.4941(3) 0.0035(14) 0.142(8) Uani 0.50 1 d PD C 2 H75C H 1.0253 0.4933 -0.0008 0.171 Uiso 0.50 1 d PR C 2 H75D H 1.0656 0.5100 -0.0593 0.171 Uiso 0.50 1 d PR C 2 C76' C 1.0718(5) 0.4498(4) -0.0171(12) 0.120(6) Uani 0.50 1 d PD C 2 H76C H 1.0615 0.4330 0.0404 0.144 Uiso 0.50 1 d PR C 2 H76D H 1.1013 0.4494 -0.0149 0.144 Uiso 0.50 1 d PR C 2 C77' C 1.0553(5) 0.4421(5) -0.1376(13) 0.086(5) Uiso 0.50 1 d PD C 2 H77D H 1.0631 0.4148 -0.1586 0.129 Uiso 0.50 1 d PR C 2 H77E H 1.0258 0.4446 -0.1401 0.129 Uiso 0.50 1 d PR C 2 H77F H 1.0673 0.4617 -0.1862 0.129 Uiso 0.50 1 d PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S 0.0260(5) 0.0268(5) 0.0343(6) -0.0013(5) 0.0025(5) -0.0019(4) O1 0.0399(16) 0.0229(14) 0.0464(17) -0.0017(13) 0.0017(15) -0.0054(12) O2 0.0265(15) 0.0305(16) 0.0387(17) -0.0024(13) 0.0048(13) -0.0048(12) O3 0.0245(15) 0.0500(19) 0.0386(18) -0.0122(15) 0.0012(13) 0.0010(13) O4 0.0239(15) 0.0456(17) 0.0396(17) -0.0124(15) 0.0031(13) -0.0072(13) C1 0.028(2) 0.032(2) 0.034(2) 0.0030(19) 0.0003(19) -0.0078(17) C2 0.024(2) 0.036(2) 0.034(2) 0.002(2) 0.0092(19) -0.0009(18) C3 0.026(2) 0.034(2) 0.031(2) -0.0073(19) 0.0014(19) 0.0004(18) C4 0.023(2) 0.032(2) 0.034(2) -0.0007(19) -0.0005(19) -0.0027(18) C5 0.031(2) 0.029(2) 0.030(2) -0.0024(18) 0.0013(19) 0.0022(18) C6 0.028(2) 0.032(2) 0.032(2) 0.0021(19) -0.0007(19) 0.0018(18) C7 0.026(2) 0.035(2) 0.033(2) 0.001(2) 0.0020(19) 0.0051(17) C8 0.028(2) 0.028(2) 0.033(2) -0.0016(18) 0.0010(18) 0.0061(17) C9 0.024(2) 0.025(2) 0.035(2) 0.0019(19) -0.0008(19) 0.0015(16) C10 0.022(2) 0.030(2) 0.034(2) 0.005(2) 0.0026(18) 0.0033(17) C11 0.025(2) 0.028(2) 0.033(2) 0.0027(19) 0.0015(19) 0.0013(17) C12 0.024(2) 0.029(2) 0.034(2) -0.0003(19) 0.0038(19) -0.0025(17) C13 0.032(2) 0.048(3) 0.035(2) -0.007(2) -0.007(2) 0.004(2) C14 0.031(2) 0.050(3) 0.038(3) -0.007(2) -0.005(2) 0.006(2) C15 0.058(3) 0.072(4) 0.046(3) 0.008(3) 0.013(3) 0.011(3) C16 0.088(5) 0.101(5) 0.057(4) 0.005(4) 0.029(3) 0.007(4) C17 0.049(3) 0.106(5) 0.064(4) -0.015(4) 0.013(3) 0.023(3) C18 0.046(3) 0.081(4) 0.054(3) -0.026(3) -0.016(3) 0.025(3) C19 0.044(3) 0.052(3) 0.041(3) -0.015(2) -0.009(2) 0.011(2) C20 0.028(2) 0.049(3) 0.041(3) -0.007(2) 0.004(2) -0.003(2) C21 0.030(2) 0.054(3) 0.031(2) -0.004(2) 0.006(2) -0.010(2) C22 0.040(3) 0.069(3) 0.044(3) -0.016(3) -0.004(2) 0.003(2) C23 0.040(3) 0.107(5) 0.063(4) -0.022(4) -0.011(3) -0.001(3) C24 0.038(3) 0.109(5) 0.058(4) -0.029(4) -0.001(3) -0.017(3) C25 0.054(3) 0.068(4) 0.059(3) -0.014(3) 0.010(3) -0.029(3) C26 0.045(3) 0.047(3) 0.054(3) -0.002(2) -0.001(2) -0.015(2) C27 0.024(2) 0.040(3) 0.035(2) -0.007(2) 0.0012(19) -0.0024(19) C28 0.025(2) 0.036(2) 0.035(2) 0.000(2) 0.0029(18) -0.0039(19) C29 0.032(2) 0.034(2) 0.038(3) -0.003(2) -0.001(2) 0.0027(19) C30 0.026(2) 0.032(2) 0.033(2) -0.0055(18) 0.0031(18) -0.0009(18) C31 0.025(2) 0.040(3) 0.038(3) -0.009(2) 0.0019(19) 0.0005(19) C32 0.033(3) 0.039(3) 0.050(3) -0.011(2) 0.001(2) 0.001(2) C33 0.032(3) 0.047(3) 0.061(3) -0.013(3) 0.006(2) 0.010(2) C34 0.023(2) 0.066(4) 0.066(3) -0.014(3) 0.008(2) -0.002(2) C35 0.028(2) 0.044(3) 0.076(4) -0.009(3) 0.009(2) -0.009(2) C36 0.029(2) 0.040(3) 0.050(3) -0.008(2) 0.010(2) -0.004(2) C37 0.028(2) 0.034(2) 0.068(3) -0.010(2) 0.016(2) -0.002(2) C38 0.027(2) 0.037(3) 0.044(3) -0.010(2) 0.002(2) -0.0026(19) C39 0.032(2) 0.029(2) 0.053(3) -0.014(2) 0.008(2) 0.0012(19) C40 0.041(3) 0.037(3) 0.092(4) 0.011(3) 0.012(3) -0.001(2) C41 0.051(3) 0.064(3) 0.059(3) 0.022(3) 0.000(3) 0.011(3) C42 0.102(5) 0.095(5) 0.094(5) 0.033(4) -0.017(4) 0.009(4) C43 0.065(4) 0.089(5) 0.095(5) 0.015(4) -0.007(4) 0.018(4) C44 0.066(4) 0.104(5) 0.105(5) 0.040(5) -0.009(4) 0.002(4) C45 0.059(4) 0.180(8) 0.145(7) 0.043(7) -0.010(5) 0.042(5) C46 0.021(2) 0.042(3) 0.116(5) -0.026(3) 0.017(3) -0.005(2) C47 0.045(3) 0.064(4) 0.073(4) -0.026(3) 0.003(3) -0.007(3) C48 0.066(4) 0.072(4) 0.087(5) -0.016(4) -0.005(3) 0.014(3) C49 0.074(4) 0.087(5) 0.083(5) -0.023(4) 0.005(4) -0.016(4) C50 0.167(8) 0.118(7) 0.080(5) -0.040(5) -0.008(5) 0.000(6) C51 0.132(7) 0.184(9) 0.089(6) -0.022(6) 0.040(5) -0.047(7) C53 0.025(2) 0.034(2) 0.044(3) -0.002(2) 0.001(2) -0.0005(18) C54 0.026(2) 0.046(3) 0.049(3) 0.001(2) -0.003(2) 0.005(2) C55 0.030(2) 0.053(3) 0.037(3) 0.005(2) 0.003(2) 0.008(2) C56 0.027(2) 0.033(2) 0.039(3) -0.003(2) 0.005(2) -0.0006(18) C57 0.027(2) 0.039(3) 0.038(3) -0.010(2) 0.007(2) -0.0036(19) C58 0.035(3) 0.050(3) 0.044(3) -0.012(2) 0.002(2) 0.001(2) C59 0.042(3) 0.056(3) 0.040(3) -0.014(2) 0.015(2) -0.004(2) C60 0.028(2) 0.058(3) 0.052(3) -0.018(3) 0.017(2) -0.006(2) C61 0.031(2) 0.048(3) 0.055(3) -0.017(2) 0.002(2) -0.003(2) C62 0.027(2) 0.033(2) 0.049(3) -0.011(2) 0.006(2) -0.0014(19) C63 0.025(2) 0.034(2) 0.045(3) -0.001(2) 0.001(2) 0.0007(18) C64 0.027(2) 0.030(2) 0.045(3) -0.009(2) 0.003(2) 0.0011(18) C65 0.028(2) 0.034(2) 0.038(3) -0.001(2) 0.001(2) 0.0013(18) C66 0.037(3) 0.047(3) 0.045(3) 0.004(2) -0.002(2) -0.002(2) C67 0.041(3) 0.042(3) 0.042(3) -0.008(2) 0.005(2) -0.002(2) C68 0.077(4) 0.060(3) 0.051(3) 0.002(3) -0.004(3) -0.015(3) C69 0.107(5) 0.067(4) 0.057(4) -0.001(3) -0.010(4) -0.018(3) C70 0.140(7) 0.098(6) 0.094(6) 0.004(5) -0.063(5) -0.017(5) C71 0.103(6) 0.087(5) 0.107(6) 0.022(5) 0.000(5) -0.032(4) C72 0.023(2) 0.044(3) 0.078(4) 0.009(3) 0.005(2) 0.005(2) C73 0.047(3) 0.038(3) 0.100(5) -0.011(3) 0.006(3) 0.003(2) C74 0.068(4) 0.050(4) 0.180(8) -0.006(5) 0.017(5) 0.009(3) C75 0.070(7) 0.052(6) 0.072(8) 0.006(6) 0.011(7) 0.002(5) C76 0.080(8) 0.047(6) 0.061(7) -0.008(6) -0.003(6) 0.011(5) C75' 0.066(9) 0.036(7) 0.33(3) -0.018(12) 0.000(13) -0.005(6) C76' 0.136(14) 0.098(11) 0.127(14) 0.014(11) 0.044(12) 0.033(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 S O2 1.437(3) . ? S O1 1.445(3) . ? S C9 1.759(4) . ? S C12 1.766(4) . ? O3 C3 1.346(5) . ? O3 C13 1.436(5) . ? O4 C6 1.370(5) . ? O4 C20 1.432(5) . ? C1 C2 1.380(5) . ? C1 C12 1.399(5) . ? C2 C3 1.409(6) . ? C2 C27 1.490(5) . ? C3 C4 1.400(5) . ? C4 C11 1.368(5) . ? C5 C10 1.389(5) . ? C5 C6 1.393(5) . ? C6 C7 1.404(6) . ? C7 C8 1.399(5) . ? C7 C53 1.492(6) . ? C8 C9 1.403(5) . ? C9 C10 1.368(6) . ? C10 C11 1.487(5) . ? C11 C12 1.386(5) . ? C13 C14 1.511(6) . ? C14 C15 1.489(6) . ? C14 C19 1.532(6) . ? C15 C16 1.528(7) . ? C16 C17 1.519(8) . ? C17 C18 1.516(8) . ? C18 C19 1.510(6) . ? C20 C21 1.504(6) . ? C21 C22 1.496(6) . ? C21 C26 1.529(6) . ? C22 C23 1.522(6) . ? C23 C24 1.504(7) . ? C24 C25 1.512(8) . ? C25 C26 1.539(6) . ? C27 C28 1.393(6) . ? C27 C39 1.398(5) . ? C28 C29 1.381(5) . ? C29 C30 1.386(5) . ? C30 C38 1.379(6) . ? C30 C31 1.476(6) . ? C31 C36 1.367(6) . ? C31 C32 1.405(6) . ? C32 C33 1.378(6) . ? C33 C34 1.369(7) . ? C34 C35 1.382(6) . ? C35 C36 1.380(6) . ? C36 C37 1.515(6) . ? C37 C38 1.538(6) . ? C37 C40 1.547(7) . ? C37 C46 1.555(7) . ? C38 C39 1.385(6) . ? C40 C41 1.496(7) . ? C41 C42 1.528(7) . ? C42 C43 1.602(9) . ? C43 C44 1.523(8) . ? C44 C45 1.508(10) . ? C46 C47 1.524(8) . ? C47 C48 1.523(7) . ? C48 C49 1.521(9) . ? C49 C50 1.513(9) . ? C50 C51 1.560(11) . ? C53 C54 1.369(6) . ? C53 C65 1.409(6) . ? C54 C55 1.395(6) . ? C55 C56 1.390(6) . ? C56 C64 1.386(6) . ? C56 C57 1.473(6) . ? C57 C58 1.374(6) . ? C57 C62 1.389(6) . ? C58 C59 1.397(6) . ? C59 C60 1.382(6) . ? C60 C61 1.403(7) . ? C61 C62 1.393(6) . ? C62 C63 1.529(6) . ? C63 C66 1.519(6) . ? C63 C64 1.532(6) . ? C63 C72 1.550(6) . ? C64 C65 1.378(6) . ? C66 C67 1.533(6) . ? C67 C68 1.533(6) . ? C68 C69 1.506(7) . ? C69 C70 1.593(9) . ? C70 C71 1.403(9) . ? C72 C73 1.507(7) . ? C73 C74 1.536(8) . ? C74 C75 1.648(10) . ? C74 C75' 1.690(12) . ? C75 C76 1.589(10) . ? C76 C77 1.631(13) . ? C75' C76' 1.551(12) . ? C76' C77' 1.607(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 S O1 115.84(17) . . ? O2 S C9 111.75(17) . . ? O1 S C9 111.46(17) . . ? O2 S C12 111.34(17) . . ? O1 S C12 111.78(18) . . ? C9 S C12 92.32(19) . . ? C3 O3 C13 118.1(3) . . ? C6 O4 C20 117.2(3) . . ? C2 C1 C12 119.2(4) . . ? C1 C2 C3 119.2(4) . . ? C1 C2 C27 121.0(4) . . ? C3 C2 C27 119.7(4) . . ? O3 C3 C4 122.7(4) . . ? O3 C3 C2 116.5(3) . . ? C4 C3 C2 120.8(4) . . ? C11 C4 C3 119.3(4) . . ? C10 C5 C6 118.4(4) . . ? O4 C6 C5 121.8(4) . . ? O4 C6 C7 116.3(3) . . ? C5 C6 C7 121.8(4) . . ? C8 C7 C6 118.6(4) . . ? C8 C7 C53 118.4(4) . . ? C6 C7 C53 122.8(3) . . ? C7 C8 C9 119.0(4) . . ? C10 C9 C8 121.5(4) . . ? C10 C9 S 111.7(3) . . ? C8 C9 S 126.7(3) . . ? C9 C10 C5 120.7(4) . . ? C9 C10 C11 112.6(3) . . ? C5 C10 C11 126.7(4) . . ? C4 C11 C12 120.1(4) . . ? C4 C11 C10 127.4(4) . . ? C12 C11 C10 112.4(3) . . ? C11 C12 C1 121.3(4) . . ? C11 C12 S 110.8(3) . . ? C1 C12 S 127.8(3) . . ? O3 C13 C14 108.6(3) . . ? C15 C14 C13 112.8(4) . . ? C15 C14 C19 110.7(4) . . ? C13 C14 C19 111.8(4) . . ? C14 C15 C16 110.9(5) . . ? C17 C16 C15 109.3(5) . . ? C18 C17 C16 110.2(5) . . ? C19 C18 C17 111.4(5) . . ? C18 C19 C14 111.4(4) . . ? O4 C20 C21 109.2(3) . . ? C22 C21 C20 111.9(4) . . ? C22 C21 C26 110.9(4) . . ? C20 C21 C26 108.7(3) . . ? C21 C22 C23 112.3(4) . . ? C24 C23 C22 110.9(4) . . ? C23 C24 C25 111.7(5) . . ? C24 C25 C26 109.8(4) . . ? C21 C26 C25 111.7(4) . . ? C28 C27 C39 119.5(4) . . ? C28 C27 C2 119.9(4) . . ? C39 C27 C2 120.7(4) . . ? C29 C28 C27 120.9(4) . . ? C28 C29 C30 119.6(4) . . ? C38 C30 C29 119.5(4) . . ? C38 C30 C31 108.4(4) . . ? C29 C30 C31 132.0(4) . . ? C36 C31 C32 121.5(4) . . ? C36 C31 C30 108.5(4) . . ? C32 C31 C30 130.0(4) . . ? C33 C32 C31 117.5(4) . . ? C34 C33 C32 121.1(4) . . ? C33 C34 C35 120.8(4) . . ? C36 C35 C34 119.1(4) . . ? C31 C36 C35 119.9(4) . . ? C31 C36 C37 111.8(4) . . ? C35 C36 C37 128.3(4) . . ? C36 C37 C38 100.5(3) . . ? C36 C37 C40 112.4(4) . . ? C38 C37 C40 109.2(4) . . ? C36 C37 C46 111.9(4) . . ? C38 C37 C46 111.8(4) . . ? C40 C37 C46 110.7(4) . . ? C30 C38 C39 121.8(4) . . ? C30 C38 C37 110.6(4) . . ? C39 C38 C37 127.4(4) . . ? C38 C39 C27 118.6(4) . . ? C41 C40 C37 115.7(4) . . ? C40 C41 C42 113.3(5) . . ? C41 C42 C43 113.6(6) . . ? C44 C43 C42 114.4(6) . . ? C45 C44 C43 109.5(6) . . ? C47 C46 C37 115.3(4) . . ? C48 C47 C46 114.1(5) . . ? C49 C48 C47 113.5(5) . . ? C50 C49 C48 114.0(6) . . ? C49 C50 C51 113.1(7) . . ? C54 C53 C65 119.3(4) . . ? C54 C53 C7 119.3(4) . . ? C65 C53 C7 121.4(4) . . ? C53 C54 C55 123.1(4) . . ? C56 C55 C54 116.9(4) . . ? C64 C56 C55 120.9(4) . . ? C64 C56 C57 109.3(4) . . ? C55 C56 C57 129.8(4) . . ? C58 C57 C62 121.2(4) . . ? C58 C57 C56 131.4(4) . . ? C62 C57 C56 107.3(4) . . ? C57 C58 C59 119.5(4) . . ? C60 C59 C58 119.5(4) . . ? C59 C60 C61 121.5(4) . . ? C62 C61 C60 118.2(5) . . ? C57 C62 C61 120.1(4) . . ? C57 C62 C63 112.3(4) . . ? C61 C62 C63 127.6(4) . . ? C66 C63 C62 111.2(3) . . ? C66 C63 C64 112.8(3) . . ? C62 C63 C64 100.0(3) . . ? C66 C63 C72 109.4(4) . . ? C62 C63 C72 111.3(4) . . ? C64 C63 C72 111.9(3) . . ? C65 C64 C56 121.5(4) . . ? C65 C64 C63 127.3(4) . . ? C56 C64 C63 111.1(4) . . ? C64 C65 C53 118.3(4) . . ? C63 C66 C67 116.3(4) . . ? C66 C67 C68 110.6(4) . . ? C69 C68 C67 115.8(5) . . ? C68 C69 C70 111.6(5) . . ? C71 C70 C69 116.9(6) . . ? C73 C72 C63 115.5(4) . . ? C72 C73 C74 113.3(5) . . ? C73 C74 C75 112.6(6) . . ? C73 C74 C75' 102.1(6) . . ? C75 C74 C75' 122.2(8) . . ? C76 C75 C74 112.1(8) . . ? C75 C76 C77 118.3(10) . . ? C76' C75' C74 120.7(12) . . ? C75' C76' C77' 100.6(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 C1 C2 C3 -2.5(6) . . . . ? C12 C1 C2 C27 174.9(4) . . . . ? C13 O3 C3 C4 -2.6(6) . . . . ? C13 O3 C3 C2 177.3(4) . . . . ? C1 C2 C3 O3 -177.2(4) . . . . ? C27 C2 C3 O3 5.4(6) . . . . ? C1 C2 C3 C4 2.7(6) . . . . ? C27 C2 C3 C4 -174.8(4) . . . . ? O3 C3 C4 C11 -179.4(4) . . . . ? C2 C3 C4 C11 0.7(6) . . . . ? C20 O4 C6 C5 -8.5(5) . . . . ? C20 O4 C6 C7 168.6(4) . . . . ? C10 C5 C6 O4 178.3(3) . . . . ? C10 C5 C6 C7 1.3(6) . . . . ? O4 C6 C7 C8 179.8(3) . . . . ? C5 C6 C7 C8 -3.1(6) . . . . ? O4 C6 C7 C53 -5.3(6) . . . . ? C5 C6 C7 C53 171.9(4) . . . . ? C6 C7 C8 C9 1.8(6) . . . . ? C53 C7 C8 C9 -173.4(3) . . . . ? C7 C8 C9 C10 1.2(6) . . . . ? C7 C8 C9 S 176.4(3) . . . . ? O2 S C9 C10 117.6(3) . . . . ? O1 S C9 C10 -111.0(3) . . . . ? C12 S C9 C10 3.5(3) . . . . ? O2 S C9 C8 -58.0(4) . . . . ? O1 S C9 C8 73.4(4) . . . . ? C12 S C9 C8 -172.1(4) . . . . ? C8 C9 C10 C5 -3.0(6) . . . . ? S C9 C10 C5 -178.9(3) . . . . ? C8 C9 C10 C11 173.7(3) . . . . ? S C9 C10 C11 -2.2(4) . . . . ? C6 C5 C10 C9 1.7(6) . . . . ? C6 C5 C10 C11 -174.4(4) . . . . ? C3 C4 C11 C12 -4.2(6) . . . . ? C3 C4 C11 C10 172.0(4) . . . . ? C9 C10 C11 C4 -177.3(4) . . . . ? C5 C10 C11 C4 -0.8(7) . . . . ? C9 C10 C11 C12 -0.8(5) . . . . ? C5 C10 C11 C12 175.6(4) . . . . ? C4 C11 C12 C1 4.4(6) . . . . ? C10 C11 C12 C1 -172.4(4) . . . . ? C4 C11 C12 S -179.8(3) . . . . ? C10 C11 C12 S 3.4(4) . . . . ? C2 C1 C12 C11 -0.9(6) . . . . ? C2 C1 C12 S -175.9(3) . . . . ? O2 S C12 C11 -118.4(3) . . . . ? O1 S C12 C11 110.3(3) . . . . ? C9 S C12 C11 -4.0(3) . . . . ? O2 S C12 C1 57.0(4) . . . . ? O1 S C12 C1 -74.3(4) . . . . ? C9 S C12 C1 171.5(4) . . . . ? C3 O3 C13 C14 -179.1(3) . . . . ? O3 C13 C14 C15 68.4(5) . . . . ? O3 C13 C14 C19 -57.1(5) . . . . ? C13 C14 C15 C16 176.4(4) . . . . ? C19 C14 C15 C16 -57.5(6) . . . . ? C14 C15 C16 C17 59.8(6) . . . . ? C15 C16 C17 C18 -58.5(7) . . . . ? C16 C17 C18 C19 56.6(6) . . . . ? C17 C18 C19 C14 -54.2(5) . . . . ? C15 C14 C19 C18 54.6(5) . . . . ? C13 C14 C19 C18 -178.7(4) . . . . ? C6 O4 C20 C21 -178.9(3) . . . . ? O4 C20 C21 C22 -70.3(5) . . . . ? O4 C20 C21 C26 166.8(4) . . . . ? C20 C21 C22 C23 -175.8(4) . . . . ? C26 C21 C22 C23 -54.2(5) . . . . ? C21 C22 C23 C24 55.5(6) . . . . ? C22 C23 C24 C25 -56.7(6) . . . . ? C23 C24 C25 C26 56.5(6) . . . . ? C22 C21 C26 C25 54.3(5) . . . . ? C20 C21 C26 C25 177.8(4) . . . . ? C24 C25 C26 C21 -55.2(6) . . . . ? C1 C2 C27 C28 -123.1(4) . . . . ? C3 C2 C27 C28 54.3(6) . . . . ? C1 C2 C27 C39 57.4(6) . . . . ? C3 C2 C27 C39 -125.2(5) . . . . ? C39 C27 C28 C29 -0.7(6) . . . . ? C2 C27 C28 C29 179.7(4) . . . . ? C28 C29 C30 C31 174.4(4) . . . . ? C38 C30 C31 C36 4.1(5) . . . . ? C29 C30 C31 C36 -171.6(5) . . . . ? C38 C30 C31 C32 -175.4(4) . . . . ? C29 C30 C31 C32 8.9(8) . . . . ? C32 C31 C36 C37 176.1(4) . . . . ? C30 C31 C36 C37 -3.5(5) . . . . ? C34 C35 C36 C31 2.7(8) . . . . ? C34 C35 C36 C37 -176.1(5) . . . . ? C31 C36 C37 C38 1.6(5) . . . . ? C35 C36 C37 C38 -179.6(5) . . . . ? C31 C36 C37 C40 117.5(4) . . . . ? C35 C36 C37 C40 -63.6(6) . . . . ? C31 C36 C37 C46 -117.1(5) . . . . ? C35 C36 C37 C46 61.7(7) . . . . ? C29 C30 C38 C39 -2.0(7) . . . . ? C31 C30 C38 C39 -178.3(4) . . . . ? C29 C30 C38 C37 173.2(4) . . . . ? C31 C30 C38 C37 -3.1(5) . . . . ? C36 C37 C38 C30 1.1(5) . . . . ? C40 C37 C38 C30 -117.3(4) . . . . ? C46 C37 C38 C30 119.9(4) . . . . ? C36 C37 C38 C39 175.9(5) . . . . ? C40 C37 C38 C39 57.6(6) . . . . ? C46 C37 C38 C39 -65.2(6) . . . . ? C30 C38 C39 C27 3.4(7) . . . . ? C37 C38 C39 C27 -170.9(5) . . . . ? C28 C27 C39 C38 -2.1(7) . . . . ? C2 C27 C39 C38 177.5(4) . . . . ? C36 C37 C40 C41 -61.2(5) . . . . ? C38 C37 C40 C41 49.4(5) . . . . ? C46 C37 C40 C41 172.9(4) . . . . ? C37 C40 C41 C42 -164.3(5) . . . . ? C40 C41 C42 C43 59.6(7) . . . . ? C41 C42 C43 C44 63.9(8) . . . . ? C42 C43 C44 C45 -168.8(6) . . . . ? C36 C37 C46 C47 53.4(5) . . . . ? C38 C37 C46 C47 -58.4(5) . . . . ? C40 C37 C46 C47 179.7(4) . . . . ? C37 C46 C47 C48 171.4(4) . . . . ? C46 C47 C48 C49 -175.3(5) . . . . ? C47 C48 C49 C50 171.6(6) . . . . ? C48 C49 C50 C51 -175.5(7) . . . . ? C8 C7 C53 C54 45.9(6) . . . . ? C6 C7 C53 C54 -129.0(4) . . . . ? C8 C7 C53 C65 -134.1(4) . . . . ? C6 C7 C53 C65 50.9(6) . . . . ? C56 C57 C58 C59 176.1(4) . . . . ? C60 C61 C62 C63 -176.3(4) . . . . ? C57 C62 C63 C66 -119.5(4) . . . . ? C61 C62 C63 C66 58.7(6) . . . . ? C57 C62 C63 C64 -0.2(4) . . . . ? C61 C62 C63 C64 178.0(4) . . . . ? C57 C62 C63 C72 118.2(4) . . . . ? C61 C62 C63 C72 -63.6(5) . . . . ? C55 C56 C64 C65 -2.0(6) . . . . ? C57 C56 C64 C65 177.4(4) . . . . ? C55 C56 C64 C63 -178.9(4) . . . . ? C57 C56 C64 C63 0.5(5) . . . . ? C66 C63 C64 C65 -58.8(6) . . . . ? C62 C63 C64 C65 -176.9(4) . . . . ? C72 C63 C64 C65 65.1(6) . . . . ? C66 C63 C64 C56 117.9(4) . . . . ? C62 C63 C64 C56 -0.3(4) . . . . ? C72 C63 C64 C56 -118.2(4) . . . . ? C56 C64 C65 C53 0.4(6) . . . . ? C63 C64 C65 C53 176.8(4) . . . . ? C54 C53 C65 C64 1.1(6) . . . . ? C7 C53 C65 C64 -178.9(4) . . . . ? C62 C63 C66 C67 59.5(5) . . . . ? C64 C63 C66 C67 -51.8(5) . . . . ? C72 C63 C66 C67 -177.1(4) . . . . ? C63 C66 C67 C68 -150.5(4) . . . . ? C66 C67 C68 C69 -169.8(4) . . . . ? C67 C68 C69 C70 -176.3(5) . . . . ? C68 C69 C70 C71 -178.9(7) . . . . ? C66 C63 C72 C73 -178.8(4) . . . . ? C62 C63 C72 C73 -55.6(5) . . . . ? C64 C63 C72 C73 55.4(5) . . . . ? C63 C72 C73 C74 171.6(4) . . . . ? C72 C73 C74 C75 56.1(8) . . . . ? C72 C73 C74 C75' -171.1(6) . . . . ? C73 C74 C75 C76 179.2(7) . . . . ? C75' C74 C75 C76 57.1(12) . . . . ? C74 C75 C76 C77 170.1(10) . . . . ? C73 C74 C75' C76' 168.3(12) . . . . ? C75 C74 C75' C76' -64.8(15) . . . . ? C74 C75' C76' C77' -170.9(12) . . . . ? #===================END data_6 _database_code_depnum_ccdc_archive 'CCDC 768387' #TrackingRef '- Li.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,7-Bis(2-hexyloxy-S,S-dioxide-dibenzothiophene-3-yl)-2,8-di(cyclohexylmethoxy) dibenzothiophene-S,S-dioxide ; _chemical_name_common ? _chemical_melting_point 504.3(7) _chemical_formula_moiety 'C62 H68 O10 S3,C H4 O' _chemical_formula_sum 'C63 H72 O11 S3' _chemical_formula_weight 1101.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 21.067(2) _cell_length_b 9.5370(10) _cell_length_c 29.216(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.936(3) _cell_angle_gamma 90.00 _cell_volume 5552.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3115 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.47 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 3 runs of narrow-frame \w-scans (scan width 0.3\% \w, 20s exposure), every run at a different \f angle. Crystal to detector distance 4.84 cm. Weak diffraction at high 2\q, mean I/\s(I)=3.0. ; _diffrn_ambient_temperature 120(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 6K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 45282 _diffrn_reflns_av_R_equivalents 0.2217 _diffrn_reflns_av_sigmaI/netI 0.1708 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9777 _reflns_number_gt 4314 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT version 7.46A (Bruker, 2007)' _computing_data_reduction 'SAINT version 7.46A (Bruker, 2007)' _computing_structure_solution 'SHELXTL version 6.14 (Bruker, 2003)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. Methyl groups were refined as rigid bodies rotating around C---C bonds (with a common refined U for three H atoms), methanol OH group as rotating around the C---O bond. Other H atoms: riding model. Methylene groups C(58)H~2~C(59)H~2~ are disordered between positions A and B with estimated occupancies of 0.85 and 0.15. ; _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^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9777 _refine_ls_number_parameters 710 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1267 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.06954(6) 0.51511(16) 0.11320(5) 0.0545(4) Uani 1 1 d . . . S2 S 0.33706(5) 0.81292(14) 0.13132(4) 0.0363(3) Uani 1 1 d . . . S3 S 0.74410(5) 0.95740(14) 0.28441(4) 0.0407(3) Uani 1 1 d . . . O1 O -0.09758(16) 0.5937(4) 0.14357(13) 0.0664(11) Uani 1 1 d . . . O2 O -0.03765(16) 0.3840(4) 0.13173(14) 0.0688(11) Uani 1 1 d . . . O3 O 0.34765(13) 0.9040(3) 0.09541(10) 0.0428(8) Uani 1 1 d . . . O4 O 0.34505(12) 0.6653(3) 0.12571(10) 0.0413(8) Uani 1 1 d . . . O5 O 0.74324(14) 0.9061(3) 0.23782(11) 0.0483(9) Uani 1 1 d . . . O6 O 0.75912(14) 1.1024(3) 0.29409(12) 0.0525(9) Uani 1 1 d . . . O7 O 0.08769(13) 0.8629(3) 0.02478(10) 0.0433(8) Uani 1 1 d . . . O8 O 0.09410(12) 0.9136(3) 0.18079(10) 0.0455(9) Uani 1 1 d . . . O9 O 0.47379(12) 1.0467(3) 0.32235(10) 0.0392(8) Uani 1 1 d . . . O10 O 0.51399(12) 0.7381(3) 0.33224(10) 0.0443(8) Uani 1 1 d . A . C1 C -0.1276(2) 0.4896(5) 0.05531(19) 0.0495(13) Uani 1 1 d . . . C2 C -0.1889(2) 0.4205(6) 0.0442(2) 0.0642(16) Uani 1 1 d . . . H2 H -0.2034 0.3793 0.0687 0.077 Uiso 1 1 d R . . C3 C -0.2277(2) 0.4147(6) -0.0041(3) 0.0696(18) Uani 1 1 d . . . H3 H -0.2698 0.3681 -0.0127 0.083 Uiso 1 1 d R . . C4 C -0.2075(2) 0.4739(6) -0.0398(2) 0.0642(16) Uani 1 1 d . . . H4 H -0.2361 0.4697 -0.0724 0.077 Uiso 1 1 d R . . C5 C -0.1448(2) 0.5404(5) -0.02837(19) 0.0528(14) Uani 1 1 d . . . H5 H -0.1296 0.5773 -0.0532 0.063 Uiso 1 1 d R . . C6 C -0.1055(2) 0.5506(5) 0.02007(18) 0.0468(13) Uani 1 1 d . . . C7 C -0.03995(19) 0.6255(5) 0.04149(18) 0.0449(13) Uani 1 1 d . . . C8 C -0.00532(19) 0.7031(5) 0.01724(16) 0.0426(12) Uani 1 1 d . . . H8 H -0.0204 0.7074 -0.0171 0.051 Uiso 1 1 d R . . C9 C 0.05313(19) 0.7763(5) 0.04499(16) 0.0405(12) Uani 1 1 d . . . C10 C 0.07678(19) 0.7651(5) 0.09537(16) 0.0383(11) Uani 1 1 d . . . C11 C 0.04163(19) 0.6843(5) 0.11857(17) 0.0455(13) Uani 1 1 d . . . H11 H 0.0573 0.6746 0.1528 0.055 Uiso 1 1 d R . . C12 C -0.0170(2) 0.6172(5) 0.09082(17) 0.0453(12) Uani 1 1 d . . . C13 C 0.0644(2) 0.8866(5) -0.02638(15) 0.0457(13) Uani 1 1 d . . . H131 H 0.0160 0.9096 -0.0377 0.055 Uiso 1 1 d R . . H132 H 0.0715 0.8019 -0.0437 0.055 Uiso 1 1 d R . . C14 C 0.1044(2) 1.0066(5) -0.03554(17) 0.0475(13) Uani 1 1 d . . . H141 H 0.0974 1.0881 -0.0167 0.057 Uiso 1 1 d R . . H142 H 0.0861 1.0319 -0.0702 0.057 Uiso 1 1 d R . . C15 C 0.1793(2) 0.9830(6) -0.02301(19) 0.0555(14) Uani 1 1 d . . . H151 H 0.1876 0.9150 -0.0460 0.067 Uiso 1 1 d R . . H152 H 0.1972 0.9425 0.0099 0.067 Uiso 1 1 d R . . C16 C 0.2163(2) 1.1191(6) -0.02487(19) 0.0641(16) Uani 1 1 d . . . H161 H 0.1987 1.1570 -0.0582 0.077 Uiso 1 1 d R . . H162 H 0.2055 1.1877 -0.0031 0.077 Uiso 1 1 d R . . C17 C 0.2906(3) 1.1080(7) -0.0109(2) 0.0730(18) Uani 1 1 d . . . H171 H 0.3020 1.0531 -0.0360 0.088 Uiso 1 1 d R . . H172 H 0.3079 1.0561 0.0200 0.088 Uiso 1 1 d R . . C18 C 0.3249(3) 1.2487(7) -0.0055(2) 0.0813(19) Uani 1 1 d . . . H181 H 0.3728 1.2348 -0.0006 0.140(16) Uiso 1 1 d R . . H182 H 0.3196 1.2982 0.0224 0.140(16) Uiso 1 1 d R . . H183 H 0.3049 1.3047 -0.0348 0.140(16) Uiso 1 1 d R . . C19 C 0.26069(18) 0.8490(5) 0.14058(15) 0.0337(11) Uani 1 1 d . . . C20 C 0.19844(18) 0.8088(5) 0.11028(15) 0.0351(11) Uani 1 1 d . . . H20 H 0.1937 0.7682 0.0796 0.042 Uiso 1 1 d R . . C21 C 0.14261(19) 0.8282(5) 0.12524(15) 0.0399(12) Uani 1 1 d . . . C22 C 0.1508(2) 0.8971(5) 0.16922(16) 0.0393(12) Uani 1 1 d . . . C23 C 0.21456(19) 0.9397(5) 0.19942(15) 0.0378(11) Uani 1 1 d . . . H23 H 0.2197 0.9858 0.2292 0.045 Uiso 1 1 d R . . C24 C 0.26976(18) 0.9142(5) 0.18496(15) 0.0332(11) Uani 1 1 d . . . C25 C 0.34220(18) 0.9311(4) 0.21263(14) 0.0317(10) Uani 1 1 d . . . C26 C 0.37031(18) 0.9927(4) 0.25801(14) 0.0316(10) Uani 1 1 d . . . H26 H 0.3430 1.0368 0.2740 0.038 Uiso 1 1 d R . . C27 C 0.44024(18) 0.9877(5) 0.27911(14) 0.0326(11) Uani 1 1 d . . . C28 C 0.48085(19) 0.9192(5) 0.25715(14) 0.0357(11) Uani 1 1 d . . . C29 C 0.45219(19) 0.8633(5) 0.21129(15) 0.0365(11) Uani 1 1 d . . . H29 H 0.4793 0.8189 0.1952 0.044 Uiso 1 1 d R . . C30 C 0.38389(18) 0.8737(5) 0.18938(14) 0.0317(11) Uani 1 1 d . . . C31 C 0.09561(19) 0.9912(5) 0.22309(16) 0.0442(13) Uani 1 1 d . . . H311 H 0.1155 1.0850 0.2227 0.053 Uiso 1 1 d R . . H312 H 0.1230 0.9411 0.2526 0.053 Uiso 1 1 d R . . C32 C 0.0233(2) 1.0052(5) 0.22281(17) 0.0439(12) Uani 1 1 d . . . H32 H 0.0241 1.0652 0.2511 0.053 Uiso 1 1 d R . . C33 C -0.01937(19) 1.0806(6) 0.17734(17) 0.0488(13) Uani 1 1 d . . . H331 H -0.0178 1.0279 0.1485 0.059 Uiso 1 1 d R . . H332 H -0.0001 1.1747 0.1763 0.059 Uiso 1 1 d R . . C34 C -0.0932(2) 1.0970(6) 0.1754(2) 0.0588(15) Uani 1 1 d . . . H341 H -0.0956 1.1589 0.2020 0.071 Uiso 1 1 d R . . H342 H -0.1193 1.1413 0.1444 0.071 Uiso 1 1 d R . . C35 C -0.1227(2) 0.9573(6) 0.17959(19) 0.0593(15) Uani 1 1 d . . . H351 H -0.1696 0.9694 0.1790 0.071 Uiso 1 1 d R . . H352 H -0.1230 0.8972 0.1519 0.071 Uiso 1 1 d R . . C36 C -0.0820(2) 0.8887(6) 0.2262(2) 0.0640(16) Uani 1 1 d . . . H361 H -0.1014 0.7957 0.2288 0.077 Uiso 1 1 d R . . H362 H -0.0838 0.9466 0.2539 0.077 Uiso 1 1 d R . . C37 C -0.0087(2) 0.8697(6) 0.22810(19) 0.0580(15) Uani 1 1 d . . . H371 H 0.0171 0.8263 0.2594 0.070 Uiso 1 1 d R . . H372 H -0.0071 0.8052 0.2020 0.070 Uiso 1 1 d R . . C38 C 0.43636(19) 1.1104(5) 0.34982(15) 0.0398(12) Uani 1 1 d . . . H381 H 0.4078 1.0393 0.3584 0.048 Uiso 1 1 d R . . H382 H 0.4070 1.1853 0.3307 0.048 Uiso 1 1 d R . . C39 C 0.48679(19) 1.1719(5) 0.39563(15) 0.0389(11) Uani 1 1 d . . . H39 H 0.5128 1.2464 0.3854 0.047 Uiso 1 1 d R . . C40 C 0.5365(2) 1.0626(5) 0.42424(16) 0.0462(13) Uani 1 1 d . . . H401 H 0.5120 0.9846 0.4333 0.055 Uiso 1 1 d R . . H402 H 0.5616 1.0238 0.4037 0.055 Uiso 1 1 d R . . C41 C 0.5857(2) 1.1256(6) 0.46968(16) 0.0538(14) Uani 1 1 d . . . H41A H 0.6147 1.0503 0.4889 0.065 Uiso 1 1 d R . . H41B H 0.6149 1.1936 0.4604 0.065 Uiso 1 1 d R . . C42 C 0.5510(3) 1.1985(6) 0.50036(18) 0.0678(17) Uani 1 1 d . . . H421 H 0.5272 1.1283 0.5137 0.081 Uiso 1 1 d R . . H422 H 0.5848 1.2452 0.5279 0.081 Uiso 1 1 d R . . C43 C 0.5016(2) 1.3065(6) 0.47193(18) 0.0620(15) Uani 1 1 d . . . H431 H 0.5261 1.3830 0.4620 0.074 Uiso 1 1 d R . . H432 H 0.4772 1.3475 0.4926 0.074 Uiso 1 1 d R . . C44 C 0.4508(2) 1.2407(6) 0.42667(17) 0.0521(14) Uani 1 1 d . . . H441 H 0.4234 1.1700 0.4366 0.063 Uiso 1 1 d R . . H442 H 0.4203 1.3142 0.4077 0.063 Uiso 1 1 d R . . C45 C 0.79568(19) 0.8490(5) 0.33081(15) 0.0382(12) Uani 1 1 d . . . C46 C 0.8649(2) 0.8310(5) 0.34233(16) 0.0475(13) Uani 1 1 d . . . H46 H 0.8898 0.8813 0.3258 0.057 Uiso 1 1 d R . . C47 C 0.8958(2) 0.7367(5) 0.37923(16) 0.0479(13) Uani 1 1 d . . . H47 H 0.9428 0.7213 0.3880 0.057 Uiso 1 1 d R . . C48 C 0.85908(19) 0.6653(5) 0.40303(16) 0.0446(13) Uani 1 1 d . . . H48 H 0.8812 0.6012 0.4280 0.053 Uiso 1 1 d R . . C49 C 0.78951(19) 0.6854(5) 0.39118(15) 0.0408(12) Uani 1 1 d . . . H49 H 0.7646 0.6363 0.4080 0.049 Uiso 1 1 d R . . C50 C 0.75836(18) 0.7789(5) 0.35433(15) 0.0361(11) Uani 1 1 d . . . C51 C 0.68551(18) 0.8110(5) 0.33452(14) 0.0333(11) Uani 1 1 d . . . C52 C 0.63452(19) 0.7551(5) 0.34899(15) 0.0370(11) Uani 1 1 d . . . H52 H 0.6442 0.6922 0.3756 0.044 Uiso 1 1 d R . . C53 C 0.56803(19) 0.7927(5) 0.32322(15) 0.0361(11) Uani 1 1 d . . . C54 C 0.55347(18) 0.8894(5) 0.28441(14) 0.0338(11) Uani 1 1 d . . . C55 C 0.60490(19) 0.9453(5) 0.27095(15) 0.0356(11) Uani 1 1 d . . . H55 H 0.5958 1.0099 0.2449 0.043 Uiso 1 1 d R . . C56 C 0.67094(18) 0.9058(5) 0.29646(15) 0.0328(11) Uani 1 1 d . . . C57 C 0.52428(19) 0.6567(5) 0.37470(16) 0.0439(12) Uani 1 1 d D . . H571 H 0.5418 0.7173 0.4036 0.053 Uiso 1 1 d R A . H572 H 0.5574 0.5815 0.3765 0.053 Uiso 1 1 d R . . C58A C 0.4579(2) 0.5884(6) 0.3727(2) 0.0413(14) Uani 0.85 1 d PD A 1 H581 H 0.4455 0.5167 0.3468 0.050 Uiso 0.85 1 d PR A 1 H582 H 0.4646 0.5392 0.4038 0.050 Uiso 0.85 1 d PR A 1 C59A C 0.4011(2) 0.6916(6) 0.3661(2) 0.0398(14) Uani 0.85 1 d PD A 1 H591 H 0.3885 0.7290 0.3327 0.048 Uiso 0.85 1 d PR A 1 H592 H 0.4149 0.7717 0.3887 0.048 Uiso 0.85 1 d PR A 1 C58B C 0.4582(10) 0.664(4) 0.3868(10) 0.033(8) Uiso 0.15 1 d PD A 2 H583 H 0.4631 0.6128 0.4172 0.039 Uiso 0.15 1 d PR A 2 H584 H 0.4471 0.7629 0.3908 0.039 Uiso 0.15 1 d PR A 2 C59B C 0.3970(11) 0.603(4) 0.3484(10) 0.057(10) Uiso 0.15 1 d PD A 2 H593 H 0.4063 0.5037 0.3431 0.068 Uiso 0.15 1 d PR A 2 H594 H 0.3871 0.6569 0.3179 0.068 Uiso 0.15 1 d PR A 2 C60 C 0.3393(2) 0.6176(6) 0.37282(18) 0.0538(14) Uani 1 1 d D . . H601 H 0.3213 0.5473 0.3469 0.065 Uiso 1 1 d R A . H602 H 0.3536 0.5671 0.4041 0.065 Uiso 1 1 d R . . C61 C 0.2835(2) 0.7192(6) 0.37256(19) 0.0634(16) Uani 1 1 d . A . H611 H 0.2494 0.6688 0.3829 0.076 Uiso 1 1 d R . . H612 H 0.3025 0.7942 0.3965 0.076 Uiso 1 1 d R . . C62 C 0.2496(3) 0.7853(6) 0.3245(2) 0.0752(18) Uani 1 1 d . . . H621 H 0.2116 0.8419 0.3261 0.109(13) Uiso 1 1 d R A . H622 H 0.2335 0.7119 0.2999 0.109(13) Uiso 1 1 d R . . H623 H 0.2817 0.8455 0.3158 0.109(13) Uiso 1 1 d R . . O11 O 0.74134(19) 0.6422(4) 0.19663(13) 0.0625(10) Uani 1 1 d . . . H0 H 0.7465 0.7198 0.2110 0.10(3) Uiso 1 1 calc R . . C63 C 0.7430(3) 0.6618(6) 0.14891(19) 0.0664(16) Uani 1 1 d . . . H631 H 0.7177 0.7463 0.1348 0.122(14) Uiso 1 1 d R . . H632 H 0.7227 0.5801 0.1292 0.122(14) Uiso 1 1 d R . . H633 H 0.7896 0.6718 0.1497 0.122(14) Uiso 1 1 d 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 0.0334(7) 0.0639(10) 0.0644(9) -0.0005(8) 0.0136(6) -0.0052(7) S2 0.0189(5) 0.0549(8) 0.0281(6) -0.0053(6) -0.0019(5) 0.0008(5) S3 0.0242(6) 0.0556(9) 0.0385(7) 0.0033(6) 0.0051(5) 0.0018(6) O1 0.048(2) 0.085(3) 0.073(3) -0.019(2) 0.0295(19) -0.010(2) O2 0.053(2) 0.060(3) 0.092(3) 0.020(2) 0.022(2) -0.001(2) O3 0.0259(15) 0.064(2) 0.0316(17) 0.0018(16) 0.0002(13) -0.0095(15) O4 0.0255(15) 0.051(2) 0.0393(18) -0.0114(16) -0.0004(13) 0.0031(14) O5 0.0378(17) 0.070(2) 0.0357(18) 0.0014(17) 0.0096(15) 0.0071(16) O6 0.0400(18) 0.049(2) 0.064(2) 0.0053(18) 0.0097(17) -0.0026(17) O7 0.0238(15) 0.065(2) 0.0307(17) -0.0004(16) -0.0058(13) -0.0109(15) O8 0.0197(15) 0.071(2) 0.0428(19) -0.0159(18) 0.0067(14) 0.0013(15) O9 0.0225(15) 0.063(2) 0.0266(16) -0.0098(16) 0.0004(13) 0.0018(15) O10 0.0206(15) 0.071(2) 0.0375(18) 0.0161(17) 0.0045(13) -0.0015(15) C1 0.031(3) 0.048(3) 0.068(3) -0.005(3) 0.014(2) -0.005(2) C2 0.039(3) 0.058(4) 0.095(5) -0.015(3) 0.021(3) -0.006(3) C3 0.028(3) 0.061(4) 0.114(6) -0.018(4) 0.016(3) -0.014(3) C4 0.030(3) 0.061(4) 0.088(4) -0.021(3) -0.001(3) -0.007(3) C5 0.028(2) 0.054(3) 0.062(3) -0.007(3) -0.005(2) -0.004(2) C6 0.025(2) 0.045(3) 0.061(3) -0.010(3) 0.001(2) 0.000(2) C7 0.019(2) 0.052(3) 0.055(3) -0.011(3) -0.001(2) 0.002(2) C8 0.028(2) 0.053(3) 0.035(3) -0.007(2) -0.007(2) 0.001(2) C9 0.021(2) 0.054(3) 0.036(3) -0.003(2) -0.004(2) 0.002(2) C10 0.022(2) 0.048(3) 0.039(3) -0.004(2) 0.002(2) 0.002(2) C11 0.023(2) 0.063(3) 0.043(3) -0.005(3) 0.000(2) 0.004(2) C12 0.031(2) 0.056(3) 0.044(3) -0.001(3) 0.006(2) 0.006(2) C13 0.026(2) 0.070(4) 0.030(3) -0.003(3) -0.006(2) -0.001(2) C14 0.042(3) 0.061(4) 0.035(3) 0.001(3) 0.005(2) -0.003(3) C15 0.041(3) 0.074(4) 0.049(3) 0.003(3) 0.011(2) 0.001(3) C16 0.047(3) 0.087(5) 0.051(3) 0.014(3) 0.006(3) -0.005(3) C17 0.053(3) 0.096(5) 0.064(4) 0.014(4) 0.011(3) -0.006(3) C18 0.056(3) 0.110(6) 0.075(4) 0.016(4) 0.018(3) -0.009(4) C19 0.021(2) 0.043(3) 0.032(2) -0.001(2) 0.0019(19) 0.0028(19) C20 0.023(2) 0.049(3) 0.027(2) -0.007(2) -0.0014(18) -0.001(2) C21 0.024(2) 0.055(3) 0.032(3) -0.002(2) -0.003(2) 0.001(2) C22 0.026(2) 0.054(3) 0.036(3) -0.002(2) 0.008(2) 0.000(2) C23 0.025(2) 0.050(3) 0.032(2) -0.006(2) -0.0007(19) 0.002(2) C24 0.020(2) 0.043(3) 0.031(2) 0.001(2) 0.0004(19) -0.002(2) C25 0.023(2) 0.039(3) 0.028(2) 0.002(2) -0.0005(19) 0.0014(19) C26 0.020(2) 0.044(3) 0.025(2) -0.005(2) 0.0001(18) 0.0008(19) C27 0.018(2) 0.049(3) 0.024(2) -0.003(2) -0.0015(18) 0.000(2) C28 0.021(2) 0.055(3) 0.024(2) 0.005(2) -0.0032(19) 0.001(2) C29 0.024(2) 0.052(3) 0.030(2) 0.002(2) 0.0038(19) -0.001(2) C30 0.021(2) 0.043(3) 0.024(2) -0.002(2) -0.0022(18) 0.001(2) C31 0.027(2) 0.066(4) 0.034(3) -0.006(3) 0.002(2) 0.011(2) C32 0.029(2) 0.060(4) 0.041(3) 0.003(3) 0.010(2) 0.001(2) C33 0.027(2) 0.070(4) 0.050(3) 0.004(3) 0.012(2) 0.005(2) C34 0.027(2) 0.079(4) 0.063(3) 0.013(3) 0.004(2) 0.003(3) C35 0.031(3) 0.080(4) 0.063(4) 0.007(3) 0.010(3) 0.002(3) C36 0.048(3) 0.083(4) 0.071(4) 0.012(3) 0.033(3) 0.004(3) C37 0.043(3) 0.075(4) 0.058(3) 0.015(3) 0.019(3) 0.013(3) C38 0.024(2) 0.055(3) 0.035(3) -0.009(2) 0.002(2) 0.001(2) C39 0.028(2) 0.055(3) 0.030(2) -0.004(2) 0.004(2) -0.004(2) C40 0.039(3) 0.060(4) 0.033(3) 0.001(2) 0.004(2) -0.003(2) C41 0.046(3) 0.067(4) 0.034(3) 0.007(3) -0.007(2) -0.008(3) C42 0.070(4) 0.086(5) 0.032(3) -0.004(3) -0.003(3) -0.028(4) C43 0.058(3) 0.076(4) 0.049(3) -0.025(3) 0.013(3) -0.016(3) C44 0.042(3) 0.065(4) 0.049(3) -0.016(3) 0.014(2) -0.005(3) C45 0.022(2) 0.058(3) 0.031(2) 0.002(2) 0.0021(19) 0.001(2) C46 0.026(2) 0.072(4) 0.039(3) 0.001(3) 0.003(2) -0.003(2) C47 0.020(2) 0.076(4) 0.040(3) 0.002(3) -0.002(2) 0.007(2) C48 0.023(2) 0.068(4) 0.034(3) 0.000(3) -0.003(2) 0.005(2) C49 0.026(2) 0.059(3) 0.032(2) 0.000(2) 0.001(2) 0.001(2) C50 0.019(2) 0.051(3) 0.029(2) -0.002(2) -0.0042(19) 0.006(2) C51 0.021(2) 0.046(3) 0.026(2) -0.006(2) -0.0010(18) -0.001(2) C52 0.027(2) 0.054(3) 0.024(2) 0.005(2) 0.0003(19) 0.001(2) C53 0.026(2) 0.051(3) 0.029(2) -0.001(2) 0.0059(19) -0.003(2) C54 0.019(2) 0.050(3) 0.028(2) -0.006(2) 0.0021(19) -0.001(2) C55 0.030(2) 0.045(3) 0.027(2) 0.000(2) 0.002(2) 0.001(2) C56 0.020(2) 0.046(3) 0.029(2) -0.005(2) 0.0034(18) 0.001(2) C57 0.027(2) 0.066(4) 0.038(3) 0.010(3) 0.010(2) 0.003(2) C58A 0.036(3) 0.048(4) 0.037(3) -0.003(3) 0.008(3) -0.004(3) C59A 0.031(3) 0.051(4) 0.037(3) -0.002(3) 0.010(2) -0.004(3) C60 0.028(2) 0.082(4) 0.048(3) 0.007(3) 0.007(2) -0.004(3) C61 0.039(3) 0.083(4) 0.061(4) -0.004(3) 0.006(3) -0.011(3) C62 0.055(3) 0.094(5) 0.062(4) 0.001(4) -0.002(3) 0.007(3) O11 0.063(2) 0.068(3) 0.054(2) 0.001(2) 0.016(2) -0.012(2) C63 0.058(3) 0.089(5) 0.056(3) 0.008(3) 0.024(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O1 1.428(3) . ? S1 O2 1.439(4) . ? S1 C1 1.753(5) . ? S1 C12 1.753(5) . ? S2 O3 1.434(3) . ? S2 O4 1.434(3) . ? S2 C19 1.750(4) . ? S2 C30 1.761(4) . ? S3 O6 1.426(3) . ? S3 O5 1.441(3) . ? S3 C56 1.759(4) . ? S3 C45 1.770(4) . ? O7 C9 1.356(5) . ? O7 C13 1.432(5) . ? O8 C22 1.351(5) . ? O8 C31 1.432(5) . ? O9 C27 1.354(5) . ? O9 C38 1.430(5) . ? O10 C53 1.353(5) . ? O10 C57 1.419(5) . ? C1 C6 1.387(7) . ? C1 C2 1.391(6) . ? C2 C3 1.384(8) . ? C2 H2 0.9501 . ? C3 C4 1.370(8) . ? C3 H3 0.9500 . ? C4 C5 1.404(6) . ? C4 H4 0.9499 . ? C5 C6 1.392(6) . ? C5 H5 0.9502 . ? C6 C7 1.500(6) . ? C7 C12 1.366(6) . ? C7 C8 1.385(6) . ? C8 C9 1.419(6) . ? C8 H8 0.9499 . ? C9 C10 1.396(6) . ? C10 C11 1.388(6) . ? C10 C21 1.504(5) . ? C11 C12 1.393(6) . ? C11 H11 0.9501 . ? C13 C14 1.495(6) . ? C13 H131 0.9900 . ? C13 H132 0.9901 . ? C14 C15 1.517(6) . ? C14 H141 0.9901 . ? C14 H142 0.9899 . ? C15 C16 1.524(7) . ? C15 H151 0.9900 . ? C15 H152 0.9901 . ? C16 C17 1.487(7) . ? C16 H161 0.9901 . ? C16 H162 0.9900 . ? C17 C18 1.509(8) . ? C17 H171 0.9903 . ? C17 H172 0.9901 . ? C18 H181 0.9807 . ? C18 H182 0.9807 . ? C18 H183 0.9803 . ? C19 C20 1.377(5) . ? C19 C24 1.394(6) . ? C20 C21 1.394(5) . ? C20 H20 0.9500 . ? C21 C22 1.403(6) . ? C22 C23 1.407(5) . ? C23 C24 1.381(5) . ? C23 H23 0.9499 . ? C24 C25 1.486(5) . ? C25 C30 1.386(5) . ? C25 C26 1.395(5) . ? C26 C27 1.401(5) . ? C26 H26 0.9499 . ? C27 C28 1.388(6) . ? C28 C29 1.385(6) . ? C28 C54 1.505(5) . ? C29 C30 1.376(5) . ? C29 H29 0.9500 . ? C31 C32 1.527(5) . ? C31 H311 0.9900 . ? C31 H312 0.9900 . ? C32 C37 1.489(7) . ? C32 C33 1.521(6) . ? C32 H32 0.9998 . ? C33 C34 1.545(6) . ? C33 H331 0.9900 . ? C33 H332 0.9900 . ? C34 C35 1.493(7) . ? C34 H341 0.9900 . ? C34 H342 0.9902 . ? C35 C36 1.503(7) . ? C35 H351 0.9901 . ? C35 H352 0.9899 . ? C36 C37 1.537(6) . ? C36 H361 0.9900 . ? C36 H362 0.9902 . ? C37 H371 0.9898 . ? C37 H372 0.9902 . ? C38 C39 1.530(5) . ? C38 H381 0.9901 . ? C38 H382 0.9901 . ? C39 C44 1.508(6) . ? C39 C40 1.522(6) . ? C39 H39 0.9999 . ? C40 C41 1.518(6) . ? C40 H401 0.9899 . ? C40 H402 0.9902 . ? C41 C42 1.498(7) . ? C41 H41A 0.9901 . ? C41 H41B 0.9902 . ? C42 C43 1.508(7) . ? C42 H421 0.9900 . ? C42 H422 0.9901 . ? C43 C44 1.539(6) . ? C43 H431 0.9899 . ? C43 H432 0.9900 . ? C44 H441 0.9900 . ? C44 H442 0.9900 . ? C45 C50 1.374(6) . ? C45 C46 1.397(5) . ? C46 C47 1.393(6) . ? C46 H46 0.9499 . ? C47 C48 1.376(6) . ? C47 H47 0.9500 . ? C48 C49 1.405(5) . ? C48 H48 0.9499 . ? C49 C50 1.388(6) . ? C49 H49 0.9500 . ? C50 C51 1.486(5) . ? C51 C52 1.383(5) . ? C51 C56 1.388(6) . ? C52 C53 1.404(5) . ? C52 H52 0.9502 . ? C53 C54 1.416(6) . ? C54 C55 1.375(6) . ? C55 C56 1.400(5) . ? C55 H55 0.9501 . ? C57 C58A 1.527(6) . ? C57 C58B 1.544(17) . ? C57 H571 0.9899 . ? C57 H572 0.9900 . ? C58A C59A 1.512(6) . ? C58A H581 0.9899 . ? C58A H582 0.9901 . ? C59A C60 1.549(6) . ? C59A H591 0.9899 . ? C59A H592 0.9900 . ? C58B C59B 1.523(19) . ? C58B H583 0.9901 . ? C58B H584 0.9900 . ? C59B C60 1.603(18) . ? C59B H593 0.9900 . ? C59B H594 0.9899 . ? C60 C61 1.521(6) . ? C60 H601 0.9900 . ? C60 H602 0.9899 . ? C61 C62 1.493(7) . ? C61 H611 0.9900 . ? C61 H612 0.9900 . ? C62 H621 0.9803 . ? C62 H622 0.9803 . ? C62 H623 0.9801 . ? O11 C63 1.418(6) . ? O11 H0 0.8400 . ? C63 H631 0.9800 . ? C63 H632 0.9800 . ? C63 H633 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 S1 O2 117.3(2) . . ? O1 S1 C1 111.9(2) . . ? O2 S1 C1 109.7(2) . . ? O1 S1 C12 112.3(2) . . ? O2 S1 C12 110.4(2) . . ? C1 S1 C12 92.6(2) . . ? O3 S2 O4 117.34(19) . . ? O3 S2 C19 111.30(19) . . ? O4 S2 C19 111.0(2) . . ? O3 S2 C30 109.48(19) . . ? O4 S2 C30 112.56(19) . . ? C19 S2 C30 92.42(19) . . ? O6 S3 O5 116.8(2) . . ? O6 S3 C56 112.6(2) . . ? O5 S3 C56 110.54(19) . . ? O6 S3 C45 111.9(2) . . ? O5 S3 C45 110.0(2) . . ? C56 S3 C45 92.5(2) . . ? C9 O7 C13 120.0(3) . . ? C22 O8 C31 120.1(3) . . ? C27 O9 C38 119.0(3) . . ? C53 O10 C57 118.8(3) . . ? C6 C1 C2 122.3(5) . . ? C6 C1 S1 111.2(3) . . ? C2 C1 S1 126.5(4) . . ? C3 C2 C1 117.0(6) . . ? C3 C2 H2 121.5 . . ? C1 C2 H2 121.5 . . ? C4 C3 C2 122.2(5) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 118.4(5) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 120.6 . . ? C1 C6 C5 119.6(4) . . ? C1 C6 C7 112.0(4) . . ? C5 C6 C7 128.3(5) . . ? C12 C7 C8 120.4(4) . . ? C12 C7 C6 112.1(4) . . ? C8 C7 C6 127.5(4) . . ? C7 C8 C9 118.3(4) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.9 . . ? O7 C9 C10 116.6(4) . . ? O7 C9 C8 122.7(4) . . ? C10 C9 C8 120.7(4) . . ? C11 C10 C9 119.5(4) . . ? C11 C10 C21 118.4(4) . . ? C9 C10 C21 121.8(4) . . ? C10 C11 C12 118.9(4) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.5 . . ? C7 C12 C11 122.1(4) . . ? C7 C12 S1 112.0(3) . . ? C11 C12 S1 125.9(4) . . ? O7 C13 C14 106.6(3) . . ? O7 C13 H131 110.6 . . ? C14 C13 H131 110.4 . . ? O7 C13 H132 110.4 . . ? C14 C13 H132 110.2 . . ? H131 C13 H132 108.7 . . ? C13 C14 C15 116.5(4) . . ? C13 C14 H141 107.9 . . ? C15 C14 H141 108.3 . . ? C13 C14 H142 108.4 . . ? C15 C14 H142 108.1 . . ? H141 C14 H142 107.3 . . ? C14 C15 C16 111.7(4) . . ? C14 C15 H151 109.4 . . ? C16 C15 H151 109.2 . . ? C14 C15 H152 109.3 . . ? C16 C15 H152 109.2 . . ? H151 C15 H152 107.9 . . ? C17 C16 C15 115.7(5) . . ? C17 C16 H161 108.6 . . ? C15 C16 H161 108.3 . . ? C17 C16 H162 108.2 . . ? C15 C16 H162 108.2 . . ? H161 C16 H162 107.4 . . ? C16 C17 C18 113.0(5) . . ? C16 C17 H171 108.7 . . ? C18 C17 H171 108.9 . . ? C16 C17 H172 109.2 . . ? C18 C17 H172 109.1 . . ? H171 C17 H172 107.7 . . ? C17 C18 H181 109.3 . . ? C17 C18 H182 109.5 . . ? H181 C18 H182 109.4 . . ? C17 C18 H183 109.7 . . ? H181 C18 H183 109.4 . . ? H182 C18 H183 109.4 . . ? C20 C19 C24 122.4(4) . . ? C20 C19 S2 125.3(3) . . ? C24 C19 S2 112.1(3) . . ? C19 C20 C21 119.1(4) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.5 . . ? C20 C21 C22 119.0(4) . . ? C20 C21 C10 118.6(4) . . ? C22 C21 C10 122.3(4) . . ? O8 C22 C21 115.3(4) . . ? O8 C22 C23 123.4(4) . . ? C21 C22 C23 121.2(4) . . ? C24 C23 C22 119.0(4) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.6 . . ? C23 C24 C19 119.2(4) . . ? C23 C24 C25 129.2(4) . . ? C19 C24 C25 111.1(3) . . ? C30 C25 C26 119.4(3) . . ? C30 C25 C24 113.1(4) . . ? C26 C25 C24 127.4(4) . . ? C25 C26 C27 117.7(4) . . ? C25 C26 H26 121.1 . . ? C27 C26 H26 121.1 . . ? O9 C27 C28 114.4(3) . . ? O9 C27 C26 123.5(4) . . ? C28 C27 C26 122.0(4) . . ? C29 C28 C27 119.2(4) . . ? C29 C28 C54 119.2(4) . . ? C27 C28 C54 121.2(4) . . ? C30 C29 C28 118.9(4) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.5 . . ? C29 C30 C25 122.3(4) . . ? C29 C30 S2 126.8(3) . . ? C25 C30 S2 110.9(3) . . ? O8 C31 C32 107.3(3) . . ? O8 C31 H311 110.3 . . ? C32 C31 H311 110.3 . . ? O8 C31 H312 110.2 . . ? C32 C31 H312 110.2 . . ? H311 C31 H312 108.5 . . ? C37 C32 C33 110.0(4) . . ? C37 C32 C31 114.1(4) . . ? C33 C32 C31 110.6(4) . . ? C37 C32 H32 107.3 . . ? C33 C32 H32 107.4 . . ? C31 C32 H32 107.2 . . ? C32 C33 C34 112.4(4) . . ? C32 C33 H331 109.2 . . ? C34 C33 H331 109.4 . . ? C32 C33 H332 108.9 . . ? C34 C33 H332 109.0 . . ? H331 C33 H332 107.8 . . ? C35 C34 C33 110.3(4) . . ? C35 C34 H341 109.8 . . ? C33 C34 H341 109.9 . . ? C35 C34 H342 109.5 . . ? C33 C34 H342 109.2 . . ? H341 C34 H342 108.1 . . ? C34 C35 C36 109.4(4) . . ? C34 C35 H351 109.5 . . ? C36 C35 H351 109.9 . . ? C34 C35 H352 110.0 . . ? C36 C35 H352 109.8 . . ? H351 C35 H352 108.2 . . ? C35 C36 C37 110.8(4) . . ? C35 C36 H361 109.3 . . ? C37 C36 H361 109.1 . . ? C35 C36 H362 109.6 . . ? C37 C36 H362 109.8 . . ? H361 C36 H362 108.1 . . ? C32 C37 C36 112.1(4) . . ? C32 C37 H371 109.0 . . ? C36 C37 H371 109.2 . . ? C32 C37 H372 109.2 . . ? C36 C37 H372 109.4 . . ? H371 C37 H372 107.8 . . ? O9 C38 C39 107.5(3) . . ? O9 C38 H381 110.0 . . ? C39 C38 H381 110.3 . . ? O9 C38 H382 110.3 . . ? C39 C38 H382 110.2 . . ? H381 C38 H382 108.5 . . ? C44 C39 C40 111.0(4) . . ? C44 C39 C38 110.5(3) . . ? C40 C39 C38 112.1(4) . . ? C44 C39 H39 107.5 . . ? C40 C39 H39 107.7 . . ? C38 C39 H39 107.7 . . ? C41 C40 C39 111.2(4) . . ? C41 C40 H401 109.4 . . ? C39 C40 H401 109.5 . . ? C41 C40 H402 109.4 . . ? C39 C40 H402 109.3 . . ? H401 C40 H402 108.0 . . ? C42 C41 C40 112.4(4) . . ? C42 C41 H41A 109.1 . . ? C40 C41 H41A 109.2 . . ? C42 C41 H41B 109.1 . . ? C40 C41 H41B 109.1 . . ? H41A C41 H41B 107.9 . . ? C41 C42 C43 111.8(4) . . ? C41 C42 H421 109.2 . . ? C43 C42 H421 109.3 . . ? C41 C42 H422 109.5 . . ? C43 C42 H422 109.1 . . ? H421 C42 H422 108.0 . . ? C42 C43 C44 111.0(4) . . ? C42 C43 H431 109.4 . . ? C44 C43 H431 109.4 . . ? C42 C43 H432 109.6 . . ? C44 C43 H432 109.3 . . ? H431 C43 H432 108.0 . . ? C39 C44 C43 110.4(4) . . ? C39 C44 H441 109.5 . . ? C43 C44 H441 109.6 . . ? C39 C44 H442 109.5 . . ? C43 C44 H442 109.6 . . ? H441 C44 H442 108.1 . . ? C50 C45 C46 122.8(4) . . ? C50 C45 S3 111.0(3) . . ? C46 C45 S3 126.1(4) . . ? C47 C46 C45 117.0(4) . . ? C47 C46 H46 121.5 . . ? C45 C46 H46 121.5 . . ? C48 C47 C46 120.9(4) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.5 . . ? C47 C48 C49 121.3(4) . . ? C47 C48 H48 119.3 . . ? C49 C48 H48 119.4 . . ? C50 C49 C48 118.1(4) . . ? C50 C49 H49 121.1 . . ? C48 C49 H49 120.8 . . ? C45 C50 C49 119.8(4) . . ? C45 C50 C51 113.1(4) . . ? C49 C50 C51 127.1(4) . . ? C52 C51 C56 120.3(4) . . ? C52 C51 C50 127.5(4) . . ? C56 C51 C50 112.2(4) . . ? C51 C52 C53 118.5(4) . . ? C51 C52 H52 120.8 . . ? C53 C52 H52 120.8 . . ? O10 C53 C52 123.6(4) . . ? O10 C53 C54 115.4(3) . . ? C52 C53 C54 121.0(4) . . ? C55 C54 C53 119.7(4) . . ? C55 C54 C28 122.4(4) . . ? C53 C54 C28 117.8(4) . . ? C54 C55 C56 118.9(4) . . ? C54 C55 H55 120.6 . . ? C56 C55 H55 120.5 . . ? C51 C56 C55 121.7(4) . . ? C51 C56 S3 111.2(3) . . ? C55 C56 S3 127.0(3) . . ? O10 C57 C58A 108.8(3) . . ? O10 C57 C58B 106.4(13) . . ? O10 C57 H571 109.5 . . ? C58A C57 H571 111.4 . . ? O10 C57 H572 110.4 . . ? C58A C57 H572 108.4 . . ? H571 C57 H572 108.4 . . ? C59A C58A C57 113.9(5) . . ? C59A C58A H581 110.5 . . ? C57 C58A H581 109.6 . . ? C59A C58A H582 107.4 . . ? C57 C58A H582 108.1 . . ? H581 C58A H582 107.2 . . ? C58A C59A C60 110.5(4) . . ? C58A C59A H591 108.0 . . ? C60 C59A H591 108.8 . . ? C58A C59A H592 111.6 . . ? C60 C59A H592 110.1 . . ? H591 C59A H592 107.8 . . ? C59B C58B C57 115.2(17) . . ? C59B C58B H583 106.9 . . ? C57 C58B H583 110.2 . . ? C59B C58B H584 105.9 . . ? C57 C58B H584 109.6 . . ? H583 C58B H584 108.8 . . ? C58B C59B C60 102.8(14) . . ? C58B C59B H581 77.5 . . ? C58B C59B H593 108.4 . . ? C60 C59B H593 111.8 . . ? C58B C59B H594 110.2 . . ? C60 C59B H594 112.8 . . ? H593 C59B H594 110.5 . . ? C61 C60 C59A 112.8(4) . . ? C61 C60 H601 108.9 . . ? C59A C60 H601 109.9 . . ? C61 C60 H602 108.6 . . ? C59A C60 H602 108.8 . . ? C59B C60 H602 108.7 . . ? H601 C60 H602 107.7 . . ? C62 C61 C60 114.0(5) . . ? C62 C61 H611 108.6 . . ? C60 C61 H611 108.9 . . ? C62 C61 H612 108.7 . . ? C60 C61 H612 108.8 . . ? H611 C61 H612 107.6 . . ? C61 C62 H621 109.6 . . ? C61 C62 H622 109.5 . . ? H621 C62 H622 109.5 . . ? C61 C62 H623 109.3 . . ? H621 C62 H623 109.5 . . ? H622 C62 H623 109.5 . . ? C63 O11 H0 109.5 . . ? O11 C63 H631 109.8 . . ? O11 C63 H632 109.1 . . ? H631 C63 H632 109.5 . . ? O11 C63 H633 109.6 . . ? H631 C63 H633 109.5 . . ? H632 C63 H633 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H0 O5 0.84 1.95 2.784(5) 170.6 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.420 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.066 #===================END