data_global _journal_coden_Cambridge 177 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'David Kingston' _publ_contact_author_name 'David Kingston' _publ_contact_author_email DKINGSTON@VT.EDU _publ_section_title ; Design, synthesis and biological evaluation of bridged epothilone D analogues ; # Attachment 'cs1165.cif' data_cs1165 _database_code_depnum_ccdc_archive 'CCDC 699878' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H47 N O8 S' _chemical_formula_sum 'C36 H47 N O8 S' _chemical_formula_weight 653.81 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.0080(11) _cell_length_b 17.848(2) _cell_length_c 30.989(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3323.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1295 _cell_measurement_theta_min 3.7929 _cell_measurement_theta_max 51.5277 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 1.305 _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.9 (release 17-07-2007 CrysAlis171 .NET) (compiled Aug 17 2007,17:36:27) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_detector CCD _diffrn_detector_type 'Oxford Diffraction Sapphire 3 CCD' _diffrn_source_voltage 45 _diffrn_source_current 45 _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.0355 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time . _diffrn_standards_decay_% <2% _diffrn_reflns_number 10746 _diffrn_reflns_av_R_equivalents 0.1684 _diffrn_reflns_av_sigmaI/netI 0.2356 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 52.68 _reflns_number_total 3558 _reflns_number_gt 1655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction)' _computing_structure_solution 'SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)' _computing_molecular_graphics 'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)' _computing_publication_material 'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_number_reflns 3558 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.804 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.0640(5) 0.11291(13) 0.29495(6) 0.0464(7) Uani 1 1 d . . . O1 O 1.0293(12) 0.2312(3) 0.51919(17) 0.0473(19) Uani 1 1 d . . . O2 O 0.5562(11) 0.0696(3) 0.56868(16) 0.0432(17) Uani 1 1 d . . . H2 H 0.5458 0.0861 0.5434 0.065 Uiso 1 1 calc R . . O3 O 0.2364(15) 0.0680(3) 0.6651(2) 0.055(2) Uani 1 1 d . . . O4 O 0.2588(12) -0.0764(3) 0.68809(17) 0.0455(18) Uani 1 1 d . . . H4 H 0.1709 -0.0400 0.6859 0.068 Uiso 1 1 calc R . . O5 O 0.7747(12) -0.0390(3) 0.50217(16) 0.0394(18) Uani 1 1 d . . . O6 O 0.9611(11) 0.1081(3) 0.52816(15) 0.0412(17) Uani 1 1 d . . . O7 O 0.7554(13) -0.1493(3) 0.43882(17) 0.0416(18) Uani 1 1 d . . . O8 O 0.3869(13) -0.1630(3) 0.4562(2) 0.054(2) Uani 1 1 d . . . N1 N 1.3749(13) 0.1312(4) 0.3496(2) 0.039(2) Uani 1 1 d . . . C1 C 0.9244(19) 0.1828(6) 0.5350(3) 0.040(3) Uani 1 1 d . . . C2 C 0.7440(18) 0.1912(4) 0.5697(3) 0.042(3) Uani 1 1 d . . . H2A H 0.7954 0.2296 0.5904 0.050 Uiso 1 1 calc R . . H2B H 0.6092 0.2114 0.5554 0.050 Uiso 1 1 calc R . . C3 C 0.6752(15) 0.1231(4) 0.5951(3) 0.036(2) Uani 1 1 d . . . H3 H 0.8126 0.0983 0.6065 0.044 Uiso 1 1 calc R . . C4 C 0.5254(17) 0.1417(4) 0.6331(2) 0.036(3) Uani 1 1 d . . . C5 C 0.424(2) 0.0681(5) 0.6527(3) 0.041(3) Uani 1 1 d . . . C6 C 0.5687(16) -0.0025(4) 0.6589(2) 0.034(2) Uani 1 1 d . . . H6 H 0.6849 -0.0039 0.6358 0.041 Uiso 1 1 calc R . . C7 C 0.4222(17) -0.0721(5) 0.6548(3) 0.034(2) Uani 1 1 d . . . H7 H 0.3419 -0.0688 0.6266 0.041 Uiso 1 1 calc R . . C8 C 0.5434(17) -0.1485(5) 0.6562(2) 0.038(2) Uani 1 1 d . . . H8 H 0.5909 -0.1567 0.6868 0.046 Uiso 1 1 calc R . . C9 C 0.7544(17) -0.1520(5) 0.6284(2) 0.039(3) Uani 1 1 d . . . H9A H 0.8238 -0.2019 0.6323 0.047 Uiso 1 1 calc R . . H9B H 0.8611 -0.1141 0.6392 0.047 Uiso 1 1 calc R . . C10 C 0.7166(18) -0.1385(4) 0.5796(2) 0.042(3) Uani 1 1 d . . . H10A H 0.6326 -0.1813 0.5673 0.051 Uiso 1 1 calc R . . H10B H 0.6258 -0.0928 0.5756 0.051 Uiso 1 1 calc R . . C11 C 0.9360(17) -0.1297(4) 0.5551(2) 0.040(3) Uani 1 1 d . . . H11A H 1.0262 -0.0901 0.5691 0.048 Uiso 1 1 calc R . . H11B H 1.0207 -0.1772 0.5568 0.048 Uiso 1 1 calc R . . C12 C 0.8986(16) -0.1094(5) 0.5080(2) 0.038(2) Uani 1 1 d . . . C13 C 1.0065(18) -0.0457(4) 0.4860(3) 0.038(3) Uani 1 1 d . . . H13 H 1.0177 -0.0517 0.4540 0.045 Uiso 1 1 calc R . . C14 C 1.1771(17) 0.0056(4) 0.5048(3) 0.040(3) Uani 1 1 d . . . H14A H 1.3244 -0.0071 0.4925 0.048 Uiso 1 1 calc R . . H14B H 1.1847 -0.0029 0.5364 0.048 Uiso 1 1 calc R . . C15 C 1.1285(18) 0.0891(4) 0.4964(3) 0.045(3) Uani 1 1 d . . . H15 H 1.2662 0.1190 0.5021 0.054 Uiso 1 1 calc R . . C16 C 1.052(2) 0.1029(4) 0.4502(3) 0.037(2) Uani 1 1 d . . . C17 C 1.2124(18) 0.1083(4) 0.4206(3) 0.041(3) Uani 1 1 d . . . H17 H 1.3610 0.1088 0.4311 0.049 Uiso 1 1 calc R . . C18 C 1.184(2) 0.1136(5) 0.3728(3) 0.044(3) Uani 1 1 d . . . C19 C 0.9979(18) 0.1024(5) 0.3476(3) 0.046(3) Uani 1 1 d . . . H19 H 0.8540 0.0904 0.3583 0.055 Uiso 1 1 calc R . . C20 C 1.3372(17) 0.1336(4) 0.3077(3) 0.040(3) Uani 1 1 d . . . C21 C 1.4989(19) 0.1531(5) 0.2745(3) 0.054(3) Uani 1 1 d . . . H21A H 1.5817 0.1978 0.2834 0.081 Uiso 1 1 calc R . . H21B H 1.4211 0.1632 0.2473 0.081 Uiso 1 1 calc R . . H21C H 1.6026 0.1113 0.2704 0.081 Uiso 1 1 calc R . . C22 C 0.3282(18) 0.1921(5) 0.6193(3) 0.051(3) Uani 1 1 d . . . H22A H 0.3835 0.2423 0.6122 0.077 Uiso 1 1 calc R . . H22B H 0.2211 0.1956 0.6431 0.077 Uiso 1 1 calc R . . H22C H 0.2550 0.1704 0.5940 0.077 Uiso 1 1 calc R . . C23 C 0.6627(19) 0.1812(4) 0.6689(3) 0.048(3) Uani 1 1 d . . . H23A H 0.7987 0.1513 0.6744 0.058 Uiso 1 1 calc R . . H23B H 0.7106 0.2308 0.6580 0.058 Uiso 1 1 calc R . . C24 C 0.544(2) 0.1925(4) 0.7111(3) 0.065(4) Uani 1 1 d . . . H24 H 0.3903 0.2046 0.7111 0.078 Uiso 1 1 calc R . . C25 C 0.652(3) 0.1858(5) 0.7486(3) 0.088(5) Uani 1 1 d . . . H25A H 0.8064 0.1737 0.7489 0.105 Uiso 1 1 calc R . . H25B H 0.5752 0.1932 0.7751 0.105 Uiso 1 1 calc R . . C26 C 0.6857(17) -0.0011(5) 0.7037(3) 0.047(3) Uani 1 1 d . . . H26A H 0.5731 0.0001 0.7265 0.070 Uiso 1 1 calc R . . H26B H 0.7798 0.0436 0.7057 0.070 Uiso 1 1 calc R . . H26C H 0.7779 -0.0460 0.7069 0.070 Uiso 1 1 calc R . . C27 C 0.3804(17) -0.2123(5) 0.6449(3) 0.046(3) Uani 1 1 d . . . H27A H 0.3345 -0.2076 0.6146 0.069 Uiso 1 1 calc R . . H27B H 0.2491 -0.2092 0.6635 0.069 Uiso 1 1 calc R . . H27C H 0.4540 -0.2607 0.6492 0.069 Uiso 1 1 calc R . . C28 C 0.8171(18) -0.1754(4) 0.4810(3) 0.040(3) Uani 1 1 d . . . H28A H 0.9364 -0.2134 0.4785 0.048 Uiso 1 1 calc R . . H28B H 0.6872 -0.1991 0.4951 0.048 Uiso 1 1 calc R . . C29 C 0.532(3) -0.1443(4) 0.4313(3) 0.044(3) Uani 1 1 d . . . C30 C 0.4889(18) -0.1115(5) 0.3871(3) 0.037(3) Uani 1 1 d . . . C31 C 0.2763(19) -0.1170(5) 0.3714(3) 0.045(3) Uani 1 1 d . . . H31 H 0.1615 -0.1380 0.3887 0.054 Uiso 1 1 calc R . . C32 C 0.230(2) -0.0912(5) 0.3293(3) 0.056(3) Uani 1 1 d . . . H32 H 0.0843 -0.0966 0.3177 0.067 Uiso 1 1 calc R . . C33 C 0.392(2) -0.0585(5) 0.3056(3) 0.046(3) Uani 1 1 d . . . H33 H 0.3590 -0.0400 0.2776 0.056 Uiso 1 1 calc R . . C34 C 0.601(2) -0.0520(5) 0.3213(3) 0.052(3) Uani 1 1 d . . . H34 H 0.7139 -0.0295 0.3040 0.063 Uiso 1 1 calc R . . C35 C 0.655(2) -0.0784(5) 0.3632(3) 0.048(3) Uani 1 1 d . . . H35 H 0.8011 -0.0734 0.3745 0.058 Uiso 1 1 calc R . . C36 C 0.8077(17) 0.1053(5) 0.4417(2) 0.040(2) Uani 1 1 d . . . H36A H 0.7752 0.1452 0.4209 0.060 Uiso 1 1 calc R . . H36B H 0.7283 0.1153 0.4687 0.060 Uiso 1 1 calc R . . H36C H 0.7592 0.0570 0.4299 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.054(2) 0.0547(14) 0.0309(13) -0.0006(11) -0.0015(13) -0.0055(15) O1 0.064(6) 0.038(4) 0.040(4) 0.009(3) 0.007(4) -0.008(4) O2 0.059(5) 0.047(3) 0.024(3) 0.003(3) -0.003(3) -0.009(4) O3 0.053(6) 0.041(4) 0.073(5) 0.016(3) 0.020(4) 0.001(4) O4 0.050(6) 0.048(4) 0.038(4) 0.005(3) 0.014(4) -0.002(4) O5 0.048(6) 0.037(3) 0.033(3) 0.005(2) -0.004(3) 0.008(4) O6 0.055(5) 0.040(4) 0.029(3) -0.001(3) 0.007(3) -0.005(4) O7 0.053(6) 0.047(4) 0.025(4) 0.003(3) -0.009(3) -0.002(4) O8 0.065(7) 0.053(4) 0.045(4) 0.007(3) 0.015(4) 0.008(4) N1 0.043(7) 0.043(5) 0.031(5) -0.004(3) 0.004(4) -0.002(4) C1 0.056(9) 0.039(7) 0.024(5) -0.004(5) -0.004(5) 0.005(6) C2 0.055(9) 0.028(5) 0.042(5) -0.002(4) -0.001(6) -0.009(5) C3 0.033(7) 0.039(5) 0.038(5) 0.003(5) -0.001(5) 0.000(5) C4 0.039(8) 0.038(5) 0.030(5) 0.000(4) -0.003(5) -0.006(5) C5 0.042(9) 0.052(7) 0.029(5) -0.011(4) 0.012(6) -0.016(7) C6 0.035(6) 0.036(5) 0.031(5) 0.001(4) 0.002(5) 0.006(6) C7 0.035(7) 0.040(6) 0.028(5) 0.000(4) -0.008(5) 0.003(6) C8 0.039(7) 0.049(6) 0.027(5) 0.007(4) 0.005(5) -0.005(6) C9 0.046(8) 0.029(5) 0.042(6) 0.001(4) 0.004(5) 0.000(5) C10 0.064(9) 0.033(5) 0.030(5) 0.001(4) -0.003(5) 0.006(5) C11 0.051(8) 0.035(5) 0.033(5) 0.004(4) -0.002(5) -0.001(6) C12 0.033(7) 0.041(5) 0.039(5) 0.003(5) 0.012(5) 0.003(6) C13 0.046(9) 0.026(5) 0.040(5) -0.007(4) 0.003(5) 0.001(5) C14 0.050(8) 0.042(5) 0.028(5) 0.004(4) 0.000(5) 0.018(6) C15 0.064(9) 0.047(6) 0.023(6) -0.002(4) -0.003(5) -0.007(6) C16 0.054(9) 0.027(5) 0.030(6) -0.006(4) -0.003(6) 0.004(6) C17 0.046(8) 0.045(6) 0.031(6) -0.002(4) -0.004(5) 0.011(6) C18 0.068(9) 0.030(5) 0.034(6) -0.002(4) 0.004(6) -0.001(6) C19 0.049(9) 0.062(6) 0.027(5) 0.001(4) -0.001(5) -0.004(6) C20 0.054(9) 0.039(6) 0.029(6) -0.004(4) 0.000(5) 0.003(5) C21 0.068(9) 0.066(6) 0.029(5) -0.008(4) 0.004(6) -0.002(6) C22 0.062(9) 0.049(6) 0.043(6) -0.005(4) -0.002(5) 0.015(6) C23 0.080(10) 0.037(5) 0.027(5) 0.004(4) -0.001(5) -0.008(5) C24 0.116(12) 0.039(5) 0.040(7) -0.004(5) 0.017(7) -0.011(6) C25 0.189(16) 0.047(6) 0.027(6) -0.002(5) 0.016(8) -0.009(8) C26 0.053(8) 0.048(5) 0.039(6) 0.003(5) -0.003(5) -0.002(6) C27 0.061(9) 0.038(5) 0.038(5) -0.005(4) -0.007(5) -0.009(6) C28 0.046(8) 0.040(5) 0.036(6) -0.003(4) -0.009(5) 0.002(5) C29 0.077(12) 0.030(5) 0.024(6) -0.004(4) -0.002(7) 0.010(6) C30 0.034(8) 0.035(5) 0.043(6) -0.006(5) 0.001(5) -0.006(6) C31 0.041(9) 0.052(6) 0.042(6) 0.001(5) -0.002(5) 0.002(6) C32 0.044(9) 0.069(7) 0.054(8) -0.003(6) -0.004(7) -0.006(7) C33 0.049(10) 0.053(6) 0.037(6) -0.001(5) -0.016(7) 0.005(7) C34 0.072(11) 0.047(6) 0.038(7) 0.005(5) 0.006(6) 0.001(6) C35 0.054(9) 0.046(6) 0.044(7) -0.001(5) -0.009(6) 0.013(6) C36 0.029(8) 0.059(6) 0.032(5) 0.001(4) 0.000(5) 0.008(6) _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 C19 1.691(8) . ? S1 C20 1.728(10) . ? O1 C1 1.177(10) . ? O2 C3 1.448(9) . ? O3 C5 1.194(11) . ? O4 C7 1.426(10) . ? O5 C12 1.471(10) . ? O5 C13 1.484(11) . ? O6 C1 1.368(10) . ? O6 C15 1.448(10) . ? O7 C29 1.367(14) . ? O7 C28 1.436(9) . ? O8 C29 1.210(12) . ? N1 C20 1.321(10) . ? N1 C18 1.386(12) . ? C1 C2 1.532(13) . ? C2 C3 1.507(10) . ? C3 C4 1.517(11) . ? C4 C22 1.548(12) . ? C4 C23 1.554(12) . ? C4 C5 1.568(12) . ? C5 C6 1.542(13) . ? C6 C7 1.527(12) . ? C6 C26 1.555(11) . ? C7 C8 1.547(12) . ? C8 C9 1.534(13) . ? C8 C27 1.543(12) . ? C9 C10 1.550(11) . ? C10 C11 1.528(13) . ? C11 C12 1.521(11) . ? C12 C13 1.475(12) . ? C12 C28 1.528(11) . ? C13 C14 1.492(12) . ? C14 C15 1.542(11) . ? C15 C16 1.525(12) . ? C16 C17 1.335(12) . ? C16 C36 1.490(13) . ? C17 C18 1.494(12) . ? C18 C19 1.379(13) . ? C20 C21 1.457(13) . ? C23 C24 1.502(13) . ? C24 C25 1.337(15) . ? C29 C30 1.512(13) . ? C30 C31 1.370(12) . ? C30 C35 1.374(12) . ? C31 C32 1.411(13) . ? C32 C33 1.355(14) . ? C33 C34 1.353(15) . ? C34 C35 1.419(12) . ? 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 C19 S1 C20 91.5(5) . . ? C12 O5 C13 59.9(5) . . ? C1 O6 C15 116.5(7) . . ? C29 O7 C28 115.4(7) . . ? C20 N1 C18 112.0(8) . . ? O1 C1 O6 124.3(9) . . ? O1 C1 C2 126.8(8) . . ? O6 C1 C2 108.6(9) . . ? C3 C2 C1 118.8(7) . . ? O2 C3 C2 111.8(6) . . ? O2 C3 C4 106.8(7) . . ? C2 C3 C4 113.1(7) . . ? C3 C4 C22 111.6(7) . . ? C3 C4 C23 109.8(8) . . ? C22 C4 C23 109.8(7) . . ? C3 C4 C5 110.3(7) . . ? C22 C4 C5 107.3(9) . . ? C23 C4 C5 107.9(6) . . ? O3 C5 C6 119.3(9) . . ? O3 C5 C4 119.5(10) . . ? C6 C5 C4 121.1(10) . . ? C7 C6 C5 109.3(8) . . ? C7 C6 C26 110.4(6) . . ? C5 C6 C26 110.6(6) . . ? O4 C7 C6 112.4(6) . . ? O4 C7 C8 104.8(6) . . ? C6 C7 C8 116.3(8) . . ? C9 C8 C27 111.5(7) . . ? C9 C8 C7 114.2(7) . . ? C27 C8 C7 110.2(8) . . ? C8 C9 C10 114.9(8) . . ? C11 C10 C9 111.9(8) . . ? C12 C11 C10 111.9(8) . . ? O5 C12 C13 60.5(5) . . ? O5 C12 C11 113.4(6) . . ? C13 C12 C11 124.2(8) . . ? O5 C12 C28 115.4(7) . . ? C13 C12 C28 118.8(7) . . ? C11 C12 C28 113.0(7) . . ? C12 C13 O5 59.6(6) . . ? C12 C13 C14 126.4(7) . . ? O5 C13 C14 117.6(7) . . ? C13 C14 C15 113.4(7) . . ? O6 C15 C16 113.0(8) . . ? O6 C15 C14 104.0(6) . . ? C16 C15 C14 111.9(6) . . ? C17 C16 C36 126.0(8) . . ? C17 C16 C15 115.9(10) . . ? C36 C16 C15 117.9(8) . . ? C16 C17 C18 127.1(10) . . ? C19 C18 N1 114.3(8) . . ? C19 C18 C17 130.0(10) . . ? N1 C18 C17 115.7(10) . . ? C18 C19 S1 109.8(8) . . ? N1 C20 C21 126.1(9) . . ? N1 C20 S1 112.4(7) . . ? C21 C20 S1 121.5(7) . . ? C24 C23 C4 115.6(9) . . ? C25 C24 C23 121.0(12) . . ? O7 C28 C12 109.4(6) . . ? O8 C29 O7 125.5(8) . . ? O8 C29 C30 124.2(12) . . ? O7 C29 C30 110.3(10) . . ? C31 C30 C35 121.0(9) . . ? C31 C30 C29 116.9(11) . . ? C35 C30 C29 122.1(10) . . ? C30 C31 C32 119.3(10) . . ? C33 C32 C31 119.9(11) . . ? C34 C33 C32 120.8(10) . . ? C33 C34 C35 120.6(11) . . ? C30 C35 C34 118.2(10) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 50.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.306 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.076