# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Gerald Kehr' _publ_contact_author_name 'Gerald Kehr' data_t1 _database_code_depnum_ccdc_archive 'CCDC 895193' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H27 B F15 O2 P S' _chemical_formula_weight 778.36 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4942(4) _cell_length_b 29.0008(13) _cell_length_c 11.5368(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.018(2) _cell_angle_gamma 90.00 _cell_volume 3176.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9379 _exptl_absorpt_correction_T_max 0.9504 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30506 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.70 _diffrn_reflns_theta_max 29.13 _reflns_number_total 8222 _reflns_number_gt 6900 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0379P)^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 8222 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 P1 P 0.01641(5) 0.155603(15) -0.03917(4) 0.01905(10) Uani 1 1 d . . . S1 S 0.00605(5) 0.144841(14) 0.15599(4) 0.01993(9) Uani 1 1 d . . . O1 O 0.15937(13) 0.12586(4) 0.17539(10) 0.0195(3) Uani 1 1 d . . . B1 B 0.1933(2) 0.10149(7) 0.29320(18) 0.0187(4) Uani 1 1 d . . . F1 F 0.25999(13) 0.08341(4) 0.52983(9) 0.0336(3) Uani 1 1 d . . . C1 C 0.1763(2) 0.18965(7) -0.08348(17) 0.0247(4) Uani 1 1 d . . . O2 O -0.00733(16) 0.19097(4) 0.20673(11) 0.0301(3) Uani 1 1 d . . . F2 F 0.43049(14) 0.13178(5) 0.66886(10) 0.0415(3) Uani 1 1 d . . . C3 C 0.3073(2) 0.15827(7) -0.07876(19) 0.0313(5) Uani 1 1 d . . . H3B H 0.3907 0.1760 -0.1015 0.047 Uiso 1 1 calc R . . H3C H 0.2946 0.1323 -0.1320 0.047 Uiso 1 1 calc R . . H3D H 0.3197 0.1466 0.0003 0.047 Uiso 1 1 calc R . . F3 F 0.56303(14) 0.20862(5) 0.58911(11) 0.0447(3) Uani 1 1 d . . . C4 C 0.1627(2) 0.20899(7) -0.20753(18) 0.0343(5) Uani 1 1 d . . . H4A H 0.2478 0.2264 -0.2272 0.051 Uiso 1 1 calc R . . H4B H 0.0805 0.2294 -0.2119 0.051 Uiso 1 1 calc R . . H4C H 0.1512 0.1835 -0.2623 0.051 Uiso 1 1 calc R . . F4 F 0.52654(13) 0.23480(4) 0.36440(12) 0.0424(3) Uani 1 1 d . . . C2 C 0.1983(2) 0.22909(7) 0.00296(18) 0.0329(5) Uani 1 1 d . . . H2A H 0.2816 0.2470 -0.0194 0.049 Uiso 1 1 calc R . . H2B H 0.2121 0.2164 0.0808 0.049 Uiso 1 1 calc R . . H2C H 0.1154 0.2492 0.0028 0.049 Uiso 1 1 calc R . . F5 F 0.35679(12) 0.18945(4) 0.22646(10) 0.0316(3) Uani 1 1 d . . . C5 C -0.1528(2) 0.18832(7) -0.06382(19) 0.0284(4) Uani 1 1 d . . . F6 F 0.03612(12) 0.15316(4) 0.48352(9) 0.0282(3) Uani 1 1 d . . . C6 C -0.1298(2) 0.24011(7) -0.0344(2) 0.0387(5) Uani 1 1 d . . . H6A H -0.2178 0.2571 -0.0467 0.058 Uiso 1 1 calc R . . H6B H -0.0563 0.2528 -0.0847 0.058 Uiso 1 1 calc R . . H6C H -0.1009 0.2431 0.0468 0.058 Uiso 1 1 calc R . . F7 F -0.22739(12) 0.13950(4) 0.54475(11) 0.0347(3) Uani 1 1 d . . . C8 C -0.2706(2) 0.17131(8) 0.0174(2) 0.0383(5) Uani 1 1 d . . . H8A H -0.3570 0.1888 0.0023 0.057 Uiso 1 1 calc R . . H8B H -0.2418 0.1758 0.0982 0.057 Uiso 1 1 calc R . . H8C H -0.2881 0.1385 0.0034 0.057 Uiso 1 1 calc R . . F8 F -0.38012(12) 0.06844(5) 0.45109(12) 0.0421(3) Uani 1 1 d . . . C7 C -0.2014(3) 0.18427(8) -0.19046(19) 0.0412(6) Uani 1 1 d . . . H7A H -0.2898 0.2013 -0.2007 0.062 Uiso 1 1 calc R . . H7B H -0.2162 0.1517 -0.2098 0.062 Uiso 1 1 calc R . . H7C H -0.1292 0.1972 -0.2416 0.062 Uiso 1 1 calc R . . F9 F -0.25579(12) 0.01151(4) 0.29426(11) 0.0345(3) Uani 1 1 d . . . C9 C 0.0110(2) 0.09515(6) -0.10033(15) 0.0232(4) Uani 1 1 d . . . F10 F 0.00141(11) 0.02857(3) 0.21833(9) 0.0257(2) Uani 1 1 d . . . C12 C 0.1234(2) 0.06403(6) -0.04420(18) 0.0277(4) Uani 1 1 d . . . H12A H 0.1164 0.0329 -0.0766 0.042 Uiso 1 1 calc R . . H12B H 0.1079 0.0628 0.0397 0.042 Uiso 1 1 calc R . . H12C H 0.2172 0.0766 -0.0599 0.042 Uiso 1 1 calc R . . F11 F 0.43581(12) 0.10224(4) 0.14095(10) 0.0282(3) Uani 1 1 d . . . C11 C -0.1318(2) 0.07319(7) -0.07167(19) 0.0332(5) Uani 1 1 d . . . H11A H -0.1357 0.0420 -0.1044 0.050 Uiso 1 1 calc R . . H11B H -0.2075 0.0920 -0.1049 0.050 Uiso 1 1 calc R . . H11C H -0.1433 0.0715 0.0126 0.050 Uiso 1 1 calc R . . F12 F 0.59444(12) 0.03163(4) 0.07472(10) 0.0352(3) Uani 1 1 d . . . C10 C 0.0349(3) 0.09557(7) -0.23253(16) 0.0347(5) Uani 1 1 d . . . H10A H 0.0280 0.0640 -0.2626 0.052 Uiso 1 1 calc R . . H10B H 0.1287 0.1080 -0.2494 0.052 Uiso 1 1 calc R . . H10C H -0.0367 0.1149 -0.2696 0.052 Uiso 1 1 calc R . . F13 F 0.54259(13) -0.05459(4) 0.15793(11) 0.0408(3) Uani 1 1 d . . . C13 C 0.29439(19) 0.13421(6) 0.37223(16) 0.0203(4) Uani 1 1 d . . . C14 C 0.3224(2) 0.12162(7) 0.48633(16) 0.0235(4) Uani 1 1 d . . . F14 F 0.33116(13) -0.06769(4) 0.31384(10) 0.0337(3) Uani 1 1 d . . . F15 F 0.17598(12) 0.00215(4) 0.38646(10) 0.0283(3) Uani 1 1 d . . . C15 C 0.4109(2) 0.14570(7) 0.55877(17) 0.0285(4) Uani 1 1 d . . . C16 C 0.4803(2) 0.18381(7) 0.51839(18) 0.0309(5) Uani 1 1 d . . . C17 C 0.4611(2) 0.19686(7) 0.40595(19) 0.0287(4) Uani 1 1 d . . . C18 C 0.3695(2) 0.17267(6) 0.33586(17) 0.0236(4) Uani 1 1 d . . . C19 C 0.03808(18) 0.09008(6) 0.35136(15) 0.0195(4) Uani 1 1 d . . . C20 C -0.0296(2) 0.11689(6) 0.43363(16) 0.0218(4) Uani 1 1 d . . . C21 C -0.1681(2) 0.11056(7) 0.46766(16) 0.0250(4) Uani 1 1 d . . . C22 C -0.2460(2) 0.07535(7) 0.42127(17) 0.0269(4) Uani 1 1 d . . . C23 C -0.1830(2) 0.04667(7) 0.33998(17) 0.0240(4) Uani 1 1 d . . . C24 C -0.04689(19) 0.05519(6) 0.30644(16) 0.0212(4) Uani 1 1 d . . . C25 C 0.28951(19) 0.05588(6) 0.26053(15) 0.0191(4) Uani 1 1 d . . . C26 C 0.40272(19) 0.06039(6) 0.18478(16) 0.0210(4) Uani 1 1 d . . . C27 C 0.4883(2) 0.02457(6) 0.14946(15) 0.0248(4) Uani 1 1 d . . . C28 C 0.4636(2) -0.01893(7) 0.19302(17) 0.0264(4) Uani 1 1 d . . . C29 C 0.3577(2) -0.02513(6) 0.27193(17) 0.0231(4) Uani 1 1 d . . . C30 C 0.27560(19) 0.01175(6) 0.30576(16) 0.0200(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0237(2) 0.0161(2) 0.0174(2) -0.00065(17) -0.0021(2) 0.00199(19) S1 0.0205(2) 0.02023(19) 0.0191(2) -0.00069(16) 0.0006(2) 0.00119(19) O1 0.0203(6) 0.0210(6) 0.0173(6) 0.0019(5) 0.0002(5) 0.0009(5) B1 0.0214(10) 0.0170(9) 0.0178(10) 0.0004(8) 0.0020(8) 0.0009(8) F1 0.0387(7) 0.0378(7) 0.0244(6) 0.0093(5) -0.0006(6) -0.0015(5) C1 0.0276(10) 0.0213(9) 0.0252(11) 0.0055(8) 0.0021(8) -0.0031(8) O2 0.0394(8) 0.0260(7) 0.0250(7) -0.0053(5) 0.0010(7) 0.0081(7) F2 0.0432(7) 0.0599(9) 0.0213(6) 0.0001(6) -0.0083(6) 0.0107(6) C3 0.0268(10) 0.0351(11) 0.0321(12) 0.0078(9) 0.0038(9) 0.0002(9) F3 0.0411(7) 0.0486(8) 0.0445(8) -0.0203(7) -0.0183(6) 0.0000(6) C4 0.0448(13) 0.0311(11) 0.0271(11) 0.0102(9) 0.0012(10) -0.0002(10) F4 0.0387(7) 0.0332(7) 0.0554(8) -0.0012(6) -0.0099(7) -0.0150(6) C2 0.0377(12) 0.0266(11) 0.0344(12) 0.0022(9) -0.0039(10) -0.0112(9) F5 0.0376(7) 0.0290(6) 0.0282(6) 0.0071(5) -0.0055(5) -0.0087(5) C5 0.0274(10) 0.0309(11) 0.0268(11) -0.0013(9) -0.0073(9) 0.0083(9) F6 0.0334(6) 0.0232(5) 0.0279(6) -0.0095(5) 0.0034(5) -0.0012(5) C6 0.0449(13) 0.0283(11) 0.0427(14) -0.0042(10) -0.0071(11) 0.0161(10) F7 0.0308(6) 0.0399(7) 0.0335(6) -0.0102(6) 0.0093(6) 0.0056(5) C8 0.0249(11) 0.0467(13) 0.0432(13) -0.0041(11) -0.0021(10) 0.0110(10) F8 0.0206(6) 0.0614(9) 0.0442(8) -0.0095(7) 0.0069(6) -0.0043(6) C7 0.0430(13) 0.0459(14) 0.0348(13) -0.0028(11) -0.0139(11) 0.0160(11) F9 0.0275(6) 0.0387(7) 0.0374(7) -0.0079(6) -0.0015(6) -0.0125(5) C9 0.0331(10) 0.0180(8) 0.0185(9) -0.0047(7) 0.0001(9) -0.0013(8) F10 0.0266(6) 0.0263(5) 0.0242(5) -0.0083(4) 0.0037(5) -0.0022(5) C12 0.0372(11) 0.0199(9) 0.0261(10) -0.0021(8) 0.0039(9) 0.0025(8) F11 0.0274(6) 0.0256(6) 0.0316(6) 0.0075(5) 0.0067(5) -0.0002(5) C11 0.0354(11) 0.0280(11) 0.0360(13) -0.0078(9) -0.0063(10) -0.0070(9) F12 0.0303(6) 0.0441(7) 0.0313(7) 0.0037(6) 0.0108(5) 0.0090(5) C10 0.0576(15) 0.0283(10) 0.0180(10) -0.0041(8) -0.0031(10) 0.0031(10) F13 0.0446(7) 0.0326(7) 0.0452(8) -0.0029(6) 0.0088(6) 0.0185(6) C13 0.0202(9) 0.0209(9) 0.0198(9) -0.0028(7) 0.0009(7) 0.0047(7) C14 0.0221(9) 0.0266(10) 0.0219(10) 0.0013(8) 0.0017(8) 0.0041(8) F14 0.0412(7) 0.0193(5) 0.0405(7) 0.0037(5) 0.0013(6) 0.0048(5) F15 0.0318(6) 0.0246(6) 0.0284(6) 0.0067(5) 0.0088(5) 0.0020(5) C15 0.0263(10) 0.0400(12) 0.0192(10) -0.0063(9) -0.0036(9) 0.0114(9) C16 0.0236(10) 0.0345(10) 0.0346(11) -0.0138(9) -0.0067(9) 0.0029(9) C17 0.0252(10) 0.0246(10) 0.0365(12) -0.0037(9) -0.0028(9) -0.0019(8) C18 0.0245(9) 0.0227(9) 0.0236(10) 0.0016(8) -0.0020(8) 0.0015(8) C19 0.0222(9) 0.0191(8) 0.0174(9) 0.0029(7) 0.0021(7) 0.0029(7) C20 0.0267(10) 0.0192(8) 0.0196(9) 0.0020(7) -0.0025(8) 0.0012(7) C21 0.0242(9) 0.0304(10) 0.0204(10) -0.0017(8) 0.0038(8) 0.0061(8) C22 0.0186(9) 0.0368(12) 0.0254(10) 0.0019(9) 0.0005(8) 0.0013(8) C23 0.0236(9) 0.0265(9) 0.0220(10) 0.0016(8) -0.0048(9) -0.0023(8) C24 0.0267(10) 0.0186(9) 0.0184(9) -0.0001(7) 0.0025(7) 0.0039(7) C25 0.0225(9) 0.0195(9) 0.0154(9) 0.0007(7) -0.0016(7) 0.0010(7) C26 0.0230(9) 0.0210(9) 0.0189(9) 0.0019(7) -0.0014(8) 0.0005(7) C27 0.0211(9) 0.0340(10) 0.0192(9) 0.0003(7) 0.0034(8) 0.0057(8) C28 0.0285(11) 0.0267(10) 0.0239(10) -0.0035(8) -0.0021(8) 0.0106(8) C29 0.0266(10) 0.0189(9) 0.0238(10) 0.0014(8) -0.0047(8) 0.0017(8) C30 0.0192(9) 0.0222(9) 0.0186(10) 0.0001(7) -0.0002(7) -0.0003(7) _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 P1 C1 1.882(2) . ? P1 C5 1.887(2) . ? P1 C9 1.8904(18) . ? P1 S1 2.2753(6) . ? S1 O2 1.4657(13) . ? S1 O1 1.5722(13) . ? O1 B1 1.565(2) . ? B1 C13 1.629(3) . ? B1 C25 1.651(3) . ? B1 C19 1.652(3) . ? F1 C14 1.353(2) . ? C1 C2 1.532(3) . ? C1 C3 1.542(3) . ? C1 C4 1.543(3) . ? F2 C15 1.346(2) . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? F3 C16 1.342(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? F4 C17 1.352(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? F5 C18 1.358(2) . ? C5 C7 1.537(3) . ? C5 C8 1.541(3) . ? C5 C6 1.555(3) . ? F6 C20 1.352(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? F7 C21 1.346(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? F8 C22 1.334(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? F9 C23 1.340(2) . ? C9 C11 1.534(3) . ? C9 C12 1.540(3) . ? C9 C10 1.542(3) . ? F10 C24 1.356(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? F11 C26 1.352(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? F12 C27 1.342(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? F13 C28 1.340(2) . ? C13 C18 1.389(3) . ? C13 C14 1.392(3) . ? C14 C15 1.375(3) . ? F14 C29 1.349(2) . ? F15 C30 1.356(2) . ? C15 C16 1.369(3) . ? C16 C17 1.363(3) . ? C17 C18 1.379(3) . ? C19 C20 1.385(2) . ? C19 C24 1.394(3) . ? C20 C21 1.385(3) . ? C21 C22 1.370(3) . ? C22 C23 1.389(3) . ? C23 C24 1.372(3) . ? C25 C30 1.388(2) . ? C25 C26 1.392(3) . ? C26 C27 1.381(2) . ? C27 C28 1.378(3) . ? C28 C29 1.369(3) . ? C29 C30 1.380(3) . ? 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 C1 P1 C5 112.45(9) . . ? C1 P1 C9 114.01(9) . . ? C5 P1 C9 112.78(9) . . ? C1 P1 S1 112.08(6) . . ? C5 P1 S1 100.43(7) . . ? C9 P1 S1 103.94(6) . . ? O2 S1 O1 110.07(8) . . ? O2 S1 P1 105.89(6) . . ? O1 S1 P1 98.54(5) . . ? B1 O1 S1 118.14(11) . . ? O1 B1 C13 110.12(14) . . ? O1 B1 C25 106.08(14) . . ? C13 B1 C25 105.55(15) . . ? O1 B1 C19 105.07(14) . . ? C13 B1 C19 114.51(15) . . ? C25 B1 C19 115.21(15) . . ? C2 C1 C3 107.93(17) . . ? C2 C1 C4 110.12(16) . . ? C3 C1 C4 108.34(17) . . ? C2 C1 P1 108.96(13) . . ? C3 C1 P1 109.34(13) . . ? C4 C1 P1 112.05(15) . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C7 C5 C8 109.63(18) . . ? C7 C5 C6 108.88(18) . . ? C8 C5 C6 106.14(18) . . ? C7 C5 P1 111.11(15) . . ? C8 C5 P1 111.44(14) . . ? C6 C5 P1 109.48(14) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C9 C12 106.14(15) . . ? C11 C9 C10 110.29(17) . . ? C12 C9 C10 108.56(17) . . ? C11 C9 P1 109.17(14) . . ? C12 C9 P1 111.59(13) . . ? C10 C9 P1 110.97(13) . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C18 C13 C14 113.48(17) . . ? C18 C13 B1 126.97(17) . . ? C14 C13 B1 119.28(17) . . ? F1 C14 C15 117.25(17) . . ? F1 C14 C13 118.82(17) . . ? C15 C14 C13 123.92(19) . . ? F2 C15 C16 119.81(18) . . ? F2 C15 C14 120.37(19) . . ? C16 C15 C14 119.82(19) . . ? F3 C16 C17 120.53(19) . . ? F3 C16 C15 120.5(2) . . ? C17 C16 C15 118.92(19) . . ? F4 C17 C16 120.12(18) . . ? F4 C17 C18 119.75(19) . . ? C16 C17 C18 120.07(19) . . ? F5 C18 C17 114.74(17) . . ? F5 C18 C13 121.54(16) . . ? C17 C18 C13 123.72(19) . . ? C20 C19 C24 113.19(16) . . ? C20 C19 B1 125.42(16) . . ? C24 C19 B1 120.68(16) . . ? F6 C20 C21 114.87(16) . . ? F6 C20 C19 120.97(16) . . ? C21 C20 C19 124.10(17) . . ? F7 C21 C22 119.81(17) . . ? F7 C21 C20 120.13(18) . . ? C22 C21 C20 120.04(18) . . ? F8 C22 C21 121.76(18) . . ? F8 C22 C23 119.67(18) . . ? C21 C22 C23 118.56(18) . . ? F9 C23 C24 120.79(18) . . ? F9 C23 C22 119.98(17) . . ? C24 C23 C22 119.22(18) . . ? F10 C24 C23 115.31(16) . . ? F10 C24 C19 119.74(16) . . ? C23 C24 C19 124.83(17) . . ? C30 C25 C26 113.34(16) . . ? C30 C25 B1 126.85(16) . . ? C26 C25 B1 119.72(16) . . ? F11 C26 C27 115.35(16) . . ? F11 C26 C25 119.92(16) . . ? C27 C26 C25 124.72(17) . . ? F12 C27 C28 120.12(17) . . ? F12 C27 C26 121.14(17) . . ? C28 C27 C26 118.75(17) . . ? F13 C28 C29 120.72(17) . . ? F13 C28 C27 120.08(17) . . ? C29 C28 C27 119.20(17) . . ? F14 C29 C28 119.72(17) . . ? F14 C29 C30 120.16(17) . . ? C28 C29 C30 120.10(17) . . ? F15 C30 C29 115.39(16) . . ? F15 C30 C25 120.92(16) . . ? C29 C30 C25 123.68(17) . . ? 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 C1 P1 S1 O2 63.10(9) . . . . ? C5 P1 S1 O2 -56.49(9) . . . . ? C9 P1 S1 O2 -173.32(9) . . . . ? C1 P1 S1 O1 -50.70(8) . . . . ? C5 P1 S1 O1 -170.29(8) . . . . ? C9 P1 S1 O1 72.88(8) . . . . ? O2 S1 O1 B1 84.54(13) . . . . ? P1 S1 O1 B1 -164.99(11) . . . . ? S1 O1 B1 C13 -108.23(14) . . . . ? S1 O1 B1 C25 138.01(12) . . . . ? S1 O1 B1 C19 15.56(17) . . . . ? C5 P1 C1 C2 70.94(16) . . . . ? C9 P1 C1 C2 -159.07(13) . . . . ? S1 P1 C1 C2 -41.33(15) . . . . ? C5 P1 C1 C3 -171.31(14) . . . . ? C9 P1 C1 C3 -41.32(16) . . . . ? S1 P1 C1 C3 76.42(14) . . . . ? C5 P1 C1 C4 -51.17(16) . . . . ? C9 P1 C1 C4 78.82(16) . . . . ? S1 P1 C1 C4 -163.45(12) . . . . ? C1 P1 C5 C7 82.43(17) . . . . ? C9 P1 C5 C7 -48.19(18) . . . . ? S1 P1 C5 C7 -158.26(15) . . . . ? C1 P1 C5 C8 -154.99(15) . . . . ? C9 P1 C5 C8 74.39(17) . . . . ? S1 P1 C5 C8 -35.67(15) . . . . ? C1 P1 C5 C6 -37.87(17) . . . . ? C9 P1 C5 C6 -168.50(14) . . . . ? S1 P1 C5 C6 81.44(15) . . . . ? C1 P1 C9 C11 -172.71(13) . . . . ? C5 P1 C9 C11 -42.88(16) . . . . ? S1 P1 C9 C11 64.97(14) . . . . ? C1 P1 C9 C12 70.28(16) . . . . ? C5 P1 C9 C12 -159.89(14) . . . . ? S1 P1 C9 C12 -52.04(14) . . . . ? C1 P1 C9 C10 -50.94(18) . . . . ? C5 P1 C9 C10 78.89(17) . . . . ? S1 P1 C9 C10 -173.26(14) . . . . ? O1 B1 C13 C18 -14.5(3) . . . . ? C25 B1 C13 C18 99.6(2) . . . . ? C19 B1 C13 C18 -132.58(19) . . . . ? O1 B1 C13 C14 171.87(15) . . . . ? C25 B1 C13 C14 -74.0(2) . . . . ? C19 B1 C13 C14 53.7(2) . . . . ? C18 C13 C14 F1 -177.13(16) . . . . ? B1 C13 C14 F1 -2.6(3) . . . . ? C18 C13 C14 C15 2.7(3) . . . . ? B1 C13 C14 C15 177.17(18) . . . . ? F1 C14 C15 F2 -1.5(3) . . . . ? C13 C14 C15 F2 178.73(17) . . . . ? F1 C14 C15 C16 177.99(17) . . . . ? C13 C14 C15 C16 -1.8(3) . . . . ? F2 C15 C16 F3 -2.9(3) . . . . ? C14 C15 C16 F3 177.62(17) . . . . ? F2 C15 C16 C17 178.77(18) . . . . ? C14 C15 C16 C17 -0.7(3) . . . . ? F3 C16 C17 F4 0.6(3) . . . . ? C15 C16 C17 F4 178.90(18) . . . . ? F3 C16 C17 C18 -176.26(18) . . . . ? C15 C16 C17 C18 2.0(3) . . . . ? F4 C17 C18 F5 1.8(3) . . . . ? C16 C17 C18 F5 178.66(18) . . . . ? F4 C17 C18 C13 -177.93(17) . . . . ? C16 C17 C18 C13 -1.0(3) . . . . ? C14 C13 C18 F5 179.07(16) . . . . ? B1 C13 C18 F5 5.1(3) . . . . ? C14 C13 C18 C17 -1.2(3) . . . . ? B1 C13 C18 C17 -175.23(18) . . . . ? O1 B1 C19 C20 -96.99(19) . . . . ? C13 B1 C19 C20 24.0(2) . . . . ? C25 B1 C19 C20 146.67(18) . . . . ? O1 B1 C19 C24 72.7(2) . . . . ? C13 B1 C19 C24 -166.32(16) . . . . ? C25 B1 C19 C24 -43.6(2) . . . . ? C24 C19 C20 F6 -177.98(16) . . . . ? B1 C19 C20 F6 -7.6(3) . . . . ? C24 C19 C20 C21 -0.8(3) . . . . ? B1 C19 C20 C21 169.54(17) . . . . ? F6 C20 C21 F7 0.1(3) . . . . ? C19 C20 C21 F7 -177.16(17) . . . . ? F6 C20 C21 C22 178.89(17) . . . . ? C19 C20 C21 C22 1.6(3) . . . . ? F7 C21 C22 F8 -0.6(3) . . . . ? C20 C21 C22 F8 -179.35(18) . . . . ? F7 C21 C22 C23 178.56(17) . . . . ? C20 C21 C22 C23 -0.2(3) . . . . ? F8 C22 C23 F9 -1.8(3) . . . . ? C21 C22 C23 F9 179.04(17) . . . . ? F8 C22 C23 C24 177.38(17) . . . . ? C21 C22 C23 C24 -1.8(3) . . . . ? F9 C23 C24 F10 5.7(3) . . . . ? C22 C23 C24 F10 -173.48(16) . . . . ? F9 C23 C24 C19 -178.17(17) . . . . ? C22 C23 C24 C19 2.6(3) . . . . ? C20 C19 C24 F10 174.66(15) . . . . ? B1 C19 C24 F10 3.8(3) . . . . ? C20 C19 C24 C23 -1.3(3) . . . . ? B1 C19 C24 C23 -172.20(17) . . . . ? O1 B1 C25 C30 -136.40(18) . . . . ? C13 B1 C25 C30 106.7(2) . . . . ? C19 B1 C25 C30 -20.6(3) . . . . ? O1 B1 C25 C26 47.2(2) . . . . ? C13 B1 C25 C26 -69.6(2) . . . . ? C19 B1 C25 C26 163.01(16) . . . . ? C30 C25 C26 F11 -174.93(16) . . . . ? B1 C25 C26 F11 1.9(2) . . . . ? C30 C25 C26 C27 4.6(3) . . . . ? B1 C25 C26 C27 -178.56(17) . . . . ? F11 C26 C27 F12 -1.4(3) . . . . ? C25 C26 C27 F12 179.04(17) . . . . ? F11 C26 C27 C28 178.21(17) . . . . ? C25 C26 C27 C28 -1.4(3) . . . . ? F12 C27 C28 F13 -2.2(3) . . . . ? C26 C27 C28 F13 178.20(17) . . . . ? F12 C27 C28 C29 177.96(17) . . . . ? C26 C27 C28 C29 -1.6(3) . . . . ? F13 C28 C29 F14 -0.8(3) . . . . ? C27 C28 C29 F14 179.00(18) . . . . ? F13 C28 C29 C30 -178.86(17) . . . . ? C27 C28 C29 C30 1.0(3) . . . . ? F14 C29 C30 F15 3.6(3) . . . . ? C28 C29 C30 F15 -178.38(17) . . . . ? F14 C29 C30 C25 -175.25(17) . . . . ? C28 C29 C30 C25 2.8(3) . . . . ? C26 C25 C30 F15 175.92(16) . . . . ? B1 C25 C30 F15 -0.6(3) . . . . ? C26 C25 C30 C29 -5.3(3) . . . . ? B1 C25 C30 C29 178.16(17) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.370 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.054 # Attachment '- 4b.cif' data_erk6550 _database_code_depnum_ccdc_archive 'CCDC 895194' #TrackingRef '- 4b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H28 B F10 O2 P S' _chemical_formula_weight 720.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' B B 0.0090 0.0039 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2898(3) _cell_length_b 13.3521(6) _cell_length_c 22.5790(9) _cell_angle_alpha 73.392(3) _cell_angle_beta 73.073(3) _cell_angle_gamma 83.328(4) _cell_volume 3670.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11732 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7021 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53257 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 67.20 _reflns_number_total 12647 _reflns_number_gt 10730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. An unidentified disordered solvent molecule was found in the asymmetrical unit and could not be satisfactorily refined. The program SQUEEZE was therefore used to remove mathematically the effect of the solvent. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 705 208 ' ' _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^)+(0.0836P)^2^+1.4720P] 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 12647 _refine_ls_number_parameters 877 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1A P 0.66952(4) 0.44632(4) 0.10664(3) 0.04078(14) Uani 1 1 d . . . S1A S 0.60313(5) 0.39771(4) 0.03420(3) 0.04640(15) Uani 1 1 d . . . O1A O 0.60570(12) 0.27830(11) 0.05683(8) 0.0445(3) Uani 1 1 d . . . O2A O 0.69262(15) 0.43623(13) -0.02087(8) 0.0598(4) Uani 1 1 d . . . C1A C 0.78220(17) 0.35085(17) 0.10424(11) 0.0432(5) Uani 1 1 d . . . H1A H 0.8257 0.3624 0.0592 0.052 Uiso 1 1 calc R . . C2A C 0.73416(18) 0.24117(17) 0.12609(11) 0.0432(5) Uani 1 1 d . . . H2A1 H 0.6726 0.2405 0.1629 0.052 Uiso 1 1 calc R . . H2A2 H 0.7859 0.1897 0.1415 0.052 Uiso 1 1 calc R . . C3A C 0.8533(2) 0.35471(19) 0.14621(13) 0.0539(6) Uani 1 1 d . . . H3A1 H 0.8122 0.3416 0.1907 0.081 Uiso 1 1 calc R . . H3A2 H 0.8833 0.4232 0.1323 0.081 Uiso 1 1 calc R . . H3A3 H 0.9095 0.3017 0.1421 0.081 Uiso 1 1 calc R . . C11A C 0.60253(18) 0.43716(17) 0.19063(11) 0.0455(5) Uani 1 1 d . . . C12A C 0.6441(2) 0.49010(19) 0.22397(12) 0.0531(6) Uani 1 1 d . . . C13A C 0.5957(3) 0.4768(2) 0.28924(14) 0.0670(7) Uani 1 1 d . . . H13A H 0.6232 0.5108 0.3119 0.080 Uiso 1 1 calc R . . C14A C 0.5092(3) 0.4160(2) 0.32220(15) 0.0741(8) Uani 1 1 d . . . C15A C 0.4677(2) 0.3690(2) 0.28779(14) 0.0651(7) Uani 1 1 d . . . H15A H 0.4074 0.3293 0.3093 0.078 Uiso 1 1 calc R . . C16A C 0.51166(19) 0.37824(18) 0.22258(12) 0.0514(6) Uani 1 1 d . . . C17A C 0.7337(2) 0.5640(2) 0.19441(15) 0.0629(7) Uani 1 1 d . . . H17A H 0.7612 0.5674 0.1491 0.094 Uiso 1 1 calc R . . H17B H 0.7890 0.5391 0.2158 0.094 Uiso 1 1 calc R . . H17C H 0.7086 0.6332 0.1993 0.094 Uiso 1 1 calc R . . C18A C 0.4592(4) 0.4038(4) 0.39322(17) 0.1151(16) Uani 1 1 d . . . H18A H 0.5139 0.3976 0.4148 0.173 Uiso 1 1 calc R . . H18B H 0.4180 0.3414 0.4112 0.173 Uiso 1 1 calc R . . H18C H 0.4138 0.4645 0.3992 0.173 Uiso 1 1 calc R . . C19A C 0.4557(2) 0.3277(2) 0.18984(14) 0.0584(6) Uani 1 1 d . . . H19A H 0.4390 0.3799 0.1538 0.088 Uiso 1 1 calc R . . H19B H 0.3912 0.2982 0.2201 0.088 Uiso 1 1 calc R . . H19C H 0.5008 0.2727 0.1746 0.088 Uiso 1 1 calc R . . C21A C 0.68702(17) 0.58377(17) 0.06347(11) 0.0427(5) Uani 1 1 d . . . C22A C 0.78318(18) 0.62861(18) 0.02391(12) 0.0469(5) Uani 1 1 d . . . C23A C 0.7862(2) 0.73602(18) -0.00137(12) 0.0496(5) Uani 1 1 d . . . H23A H 0.8507 0.7656 -0.0269 0.059 Uiso 1 1 calc R . . C24A C 0.6982(2) 0.80149(18) 0.00953(12) 0.0498(5) Uani 1 1 d . . . C25A C 0.60302(19) 0.75643(17) 0.04423(12) 0.0488(5) Uani 1 1 d . . . H25A H 0.5418 0.7997 0.0495 0.059 Uiso 1 1 calc R . . C26A C 0.59442(18) 0.64888(17) 0.07174(11) 0.0454(5) Uani 1 1 d . . . C27A C 0.88482(19) 0.5668(2) 0.00725(14) 0.0602(7) Uani 1 1 d . . . H27A H 0.9387 0.6133 -0.0230 0.090 Uiso 1 1 calc R . . H27B H 0.8745 0.5137 -0.0119 0.090 Uiso 1 1 calc R . . H27C H 0.9067 0.5335 0.0459 0.090 Uiso 1 1 calc R . . C28A C 0.7056(3) 0.91883(19) -0.01765(14) 0.0647(7) Uani 1 1 d . . . H28A H 0.6958 0.9386 -0.0605 0.097 Uiso 1 1 calc R . . H28B H 0.7744 0.9396 -0.0197 0.097 Uiso 1 1 calc R . . H28C H 0.6515 0.9534 0.0098 0.097 Uiso 1 1 calc R . . C29A C 0.48566(18) 0.60980(19) 0.10854(14) 0.0557(6) Uani 1 1 d . . . H29A H 0.4766 0.5987 0.1541 0.083 Uiso 1 1 calc R . . H29B H 0.4772 0.5444 0.1001 0.083 Uiso 1 1 calc R . . H29C H 0.4334 0.6612 0.0950 0.083 Uiso 1 1 calc R . . C31A C 0.64780(17) 0.08500(17) 0.10741(11) 0.0424(5) Uani 1 1 d . . . F32A F 0.81254(11) 0.01785(10) 0.12539(8) 0.0577(4) Uani 1 1 d . . . C32A C 0.71031(18) 0.00189(18) 0.13186(11) 0.0466(5) Uani 1 1 d . . . F33A F 0.74373(14) -0.17411(11) 0.18483(9) 0.0732(4) Uani 1 1 d . . . C33A C 0.6781(2) -0.09890(18) 0.16167(12) 0.0532(6) Uani 1 1 d . . . F34A F 0.54279(14) -0.21958(12) 0.19622(8) 0.0740(5) Uani 1 1 d . . . C34A C 0.5770(2) -0.12226(18) 0.16745(12) 0.0548(6) Uani 1 1 d . . . F35A F 0.41305(12) -0.06602(13) 0.14719(9) 0.0756(5) Uani 1 1 d . . . C35A C 0.51171(19) -0.0442(2) 0.14306(13) 0.0537(6) Uani 1 1 d . . . F36A F 0.47726(11) 0.12664(12) 0.09069(8) 0.0653(4) Uani 1 1 d . . . C36A C 0.54740(18) 0.05640(19) 0.11387(12) 0.0490(5) Uani 1 1 d . . . C41A C 0.78790(17) 0.19505(16) 0.00796(11) 0.0424(5) Uani 1 1 d . . . F42A F 0.93799(11) 0.20490(13) 0.04340(7) 0.0620(4) Uani 1 1 d . . . C42A C 0.89635(19) 0.19298(19) -0.00236(12) 0.0490(5) Uani 1 1 d . . . F43A F 1.07241(12) 0.17925(17) -0.06366(9) 0.0841(5) Uani 1 1 d . . . C43A C 0.96815(19) 0.1788(2) -0.05711(14) 0.0577(6) Uani 1 1 d . . . F44A F 1.00397(13) 0.15401(15) -0.16042(8) 0.0800(5) Uani 1 1 d . . . C44A C 0.9346(2) 0.1656(2) -0.10633(13) 0.0555(6) Uani 1 1 d . . . F45A F 0.79337(13) 0.15129(14) -0.14612(7) 0.0695(4) Uani 1 1 d . . . C45A C 0.8284(2) 0.16609(19) -0.09905(12) 0.0517(6) Uani 1 1 d . . . F46A F 0.65555(10) 0.17536(11) -0.03857(7) 0.0534(3) Uani 1 1 d . . . C46A C 0.75875(17) 0.17976(17) -0.04322(11) 0.0435(5) Uani 1 1 d . . . B1A B 0.69816(19) 0.20161(19) 0.07449(13) 0.0419(5) Uani 1 1 d . . . P1B P 0.11449(5) 0.10385(5) 0.29561(3) 0.04651(15) Uani 1 1 d . . . S1B S 0.16137(5) 0.14706(5) 0.37756(3) 0.05061(16) Uani 1 1 d . . . O1B O 0.22420(12) 0.04585(13) 0.39939(8) 0.0499(4) Uani 1 1 d . . . O2B O 0.22943(15) 0.23315(14) 0.33826(9) 0.0630(5) Uani 1 1 d . . . B1B B 0.3310(2) 0.0078(2) 0.35952(14) 0.0495(6) Uani 1 1 d . . . C1B C 0.22694(19) 0.0140(2) 0.27064(13) 0.0537(6) Uani 1 1 d . . . H1B H 0.2429 0.0276 0.2234 0.064 Uiso 1 1 calc R . . C2B C 0.32791(18) 0.0365(2) 0.28539(12) 0.0506(5) Uani 1 1 d . . . H2B1 H 0.3408 0.1112 0.2667 0.061 Uiso 1 1 calc R . . H2B2 H 0.3870 -0.0015 0.2626 0.061 Uiso 1 1 calc R . . C3B C 0.1949(2) -0.0977(2) 0.29930(16) 0.0677(7) Uani 1 1 d . . . H3B1 H 0.2548 -0.1440 0.2880 0.102 Uiso 1 1 calc R . . H3B2 H 0.1389 -0.1096 0.2828 0.102 Uiso 1 1 calc R . . H3B3 H 0.1701 -0.1115 0.3456 0.102 Uiso 1 1 calc R . . C11B C 0.10453(18) 0.23530(19) 0.24426(11) 0.0477(5) Uani 1 1 d . . . C12B C 0.17729(19) 0.2785(2) 0.18468(11) 0.0502(5) Uani 1 1 d . . . C13B C 0.1636(2) 0.3830(2) 0.15364(13) 0.0559(6) Uani 1 1 d . . . H13B H 0.2122 0.4119 0.1143 0.067 Uiso 1 1 calc R . . C14B C 0.0814(2) 0.4465(2) 0.17815(13) 0.0585(6) Uani 1 1 d . . . C15B C 0.0100(2) 0.4020(2) 0.23585(13) 0.0574(6) Uani 1 1 d . . . H15B H -0.0472 0.4436 0.2526 0.069 Uiso 1 1 calc R . . C16B C 0.01958(19) 0.2986(2) 0.26989(12) 0.0523(6) Uani 1 1 d . . . C17B C 0.2680(2) 0.2188(2) 0.15077(12) 0.0569(6) Uani 1 1 d . . . H17D H 0.3135 0.1887 0.1786 0.085 Uiso 1 1 calc R . . H17E H 0.3077 0.2658 0.1117 0.085 Uiso 1 1 calc R . . H17F H 0.2413 0.1634 0.1402 0.085 Uiso 1 1 calc R . . C18B C 0.0696(3) 0.5605(2) 0.14352(16) 0.0772(8) Uani 1 1 d . . . H18D H 0.1262 0.5779 0.1042 0.116 Uiso 1 1 calc R . . H18E H 0.0727 0.6038 0.1709 0.116 Uiso 1 1 calc R . . H18F H 0.0025 0.5731 0.1333 0.116 Uiso 1 1 calc R . . C19B C -0.0638(2) 0.2617(2) 0.33244(14) 0.0672(7) Uani 1 1 d . . . H19D H -0.1062 0.3213 0.3435 0.101 Uiso 1 1 calc R . . H19E H -0.0303 0.2266 0.3661 0.101 Uiso 1 1 calc R . . H19F H -0.1084 0.2134 0.3278 0.101 Uiso 1 1 calc R . . C21B C -0.00580(19) 0.03689(19) 0.31121(12) 0.0501(5) Uani 1 1 d . . . C22B C -0.0382(2) 0.0300(2) 0.25826(13) 0.0540(6) Uani 1 1 d . . . C23B C -0.1292(2) -0.0226(2) 0.27032(15) 0.0637(7) Uani 1 1 d . . . H23B H -0.1513 -0.0276 0.2354 0.076 Uiso 1 1 calc R . . C24B C -0.1888(2) -0.0680(3) 0.33203(16) 0.0685(8) Uani 1 1 d . . . C25B C -0.1546(2) -0.0620(2) 0.38268(15) 0.0673(7) Uani 1 1 d . . . H25B H -0.1942 -0.0933 0.4247 0.081 Uiso 1 1 calc R . . C26B C -0.0636(2) -0.0114(2) 0.37433(13) 0.0573(6) Uani 1 1 d . . . C27B C 0.0224(2) 0.0735(2) 0.18924(13) 0.0633(7) Uani 1 1 d . . . H27D H -0.0135 0.0586 0.1612 0.095 Uiso 1 1 calc R . . H27E H 0.0927 0.0413 0.1818 0.095 Uiso 1 1 calc R . . H27F H 0.0272 0.1486 0.1804 0.095 Uiso 1 1 calc R . . C28B C -0.2876(3) -0.1244(3) 0.3435(2) 0.0965(12) Uani 1 1 d . . . H28D H -0.2774 -0.1982 0.3633 0.145 Uiso 1 1 calc R . . H28E H -0.3031 -0.1159 0.3029 0.145 Uiso 1 1 calc R . . H28F H -0.3459 -0.0954 0.3718 0.145 Uiso 1 1 calc R . . C29B C -0.0318(2) -0.0122(3) 0.43325(13) 0.0670(7) Uani 1 1 d . . . H29D H -0.0803 -0.0534 0.4711 0.101 Uiso 1 1 calc R . . H29E H -0.0335 0.0589 0.4365 0.101 Uiso 1 1 calc R . . H29F H 0.0389 -0.0425 0.4301 0.101 Uiso 1 1 calc R . . C31B C 0.34432(19) -0.11769(19) 0.39541(12) 0.0505(6) Uani 1 1 d . . . F32B F 0.49845(12) -0.12892(13) 0.31252(8) 0.0657(4) Uani 1 1 d . . . C32B C 0.4314(2) -0.1745(2) 0.36935(13) 0.0538(6) Uani 1 1 d . . . F33B F 0.54430(15) -0.32553(15) 0.36967(11) 0.0904(6) Uani 1 1 d . . . C33B C 0.4569(2) -0.2771(2) 0.39820(15) 0.0645(7) Uani 1 1 d . . . F34B F 0.41581(18) -0.42729(13) 0.48513(10) 0.0937(6) Uani 1 1 d . . . C34B C 0.3934(3) -0.3278(2) 0.45602(15) 0.0671(7) Uani 1 1 d . . . F35B F 0.24026(17) -0.32675(14) 0.53965(9) 0.0901(6) Uani 1 1 d . . . C35B C 0.3047(3) -0.2766(2) 0.48367(13) 0.0658(7) Uani 1 1 d . . . F36B F 0.19315(14) -0.13214(13) 0.48563(8) 0.0835(5) Uani 1 1 d . . . C36B C 0.2823(2) -0.1742(2) 0.45360(13) 0.0583(6) Uani 1 1 d . . . C41B C 0.42554(19) 0.06516(19) 0.37023(11) 0.0493(5) Uani 1 1 d . . . F42B F 0.53712(12) 0.09018(14) 0.26322(7) 0.0658(4) Uani 1 1 d . . . C42B C 0.5191(2) 0.0991(2) 0.32385(12) 0.0540(6) Uani 1 1 d . . . F43B F 0.68643(13) 0.17410(16) 0.28716(8) 0.0786(5) Uani 1 1 d . . . C43B C 0.5990(2) 0.1424(2) 0.33484(13) 0.0589(6) Uani 1 1 d . . . F44B F 0.66525(15) 0.19839(17) 0.40545(9) 0.0884(6) Uani 1 1 d . . . C44B C 0.5894(2) 0.1546(2) 0.39398(14) 0.0643(7) Uani 1 1 d . . . F45B F 0.48715(15) 0.13591(16) 0.50092(8) 0.0826(5) Uani 1 1 d . . . C45B C 0.4987(2) 0.1229(2) 0.44238(13) 0.0616(7) Uani 1 1 d . . . F46B F 0.33730(12) 0.04541(14) 0.48029(7) 0.0699(4) Uani 1 1 d . . . C46B C 0.4213(2) 0.0788(2) 0.42960(12) 0.0549(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1A 0.0408(3) 0.0363(3) 0.0478(3) -0.0130(2) -0.0153(2) 0.0016(2) S1A 0.0509(3) 0.0413(3) 0.0522(3) -0.0141(2) -0.0231(3) 0.0059(2) O1A 0.0441(8) 0.0392(8) 0.0557(9) -0.0159(7) -0.0205(7) 0.0039(6) O2A 0.0759(12) 0.0519(10) 0.0478(9) -0.0086(8) -0.0139(8) -0.0061(8) C1A 0.0423(11) 0.0401(11) 0.0498(13) -0.0140(10) -0.0152(10) 0.0011(9) C2A 0.0462(12) 0.0388(11) 0.0477(12) -0.0130(9) -0.0179(10) 0.0043(9) C3A 0.0529(14) 0.0486(13) 0.0695(16) -0.0188(12) -0.0298(12) 0.0037(11) C11A 0.0471(12) 0.0391(11) 0.0510(13) -0.0128(10) -0.0157(10) 0.0041(9) C12A 0.0621(15) 0.0444(12) 0.0576(14) -0.0192(11) -0.0205(12) 0.0042(11) C13A 0.090(2) 0.0606(16) 0.0578(16) -0.0274(13) -0.0219(15) 0.0028(15) C14A 0.098(2) 0.0609(17) 0.0577(17) -0.0222(14) -0.0079(16) 0.0005(16) C15A 0.0702(17) 0.0546(15) 0.0591(16) -0.0166(13) 0.0026(13) -0.0053(13) C16A 0.0535(13) 0.0397(12) 0.0586(14) -0.0141(10) -0.0114(11) 0.0013(10) C17A 0.0663(16) 0.0605(16) 0.0757(18) -0.0304(14) -0.0278(14) -0.0032(13) C18A 0.169(4) 0.105(3) 0.060(2) -0.035(2) 0.006(2) -0.019(3) C19A 0.0496(14) 0.0543(14) 0.0678(16) -0.0167(12) -0.0069(12) -0.0102(11) C21A 0.0413(11) 0.0396(11) 0.0496(12) -0.0136(9) -0.0156(10) 0.0019(9) C22A 0.0450(12) 0.0462(12) 0.0519(13) -0.0134(10) -0.0172(10) 0.0000(10) C23A 0.0552(14) 0.0445(12) 0.0491(13) -0.0091(10) -0.0147(11) -0.0094(10) C24A 0.0646(15) 0.0406(12) 0.0482(13) -0.0120(10) -0.0215(11) -0.0015(11) C25A 0.0555(14) 0.0378(11) 0.0555(14) -0.0144(10) -0.0206(11) 0.0081(10) C26A 0.0461(12) 0.0428(12) 0.0499(13) -0.0131(10) -0.0175(10) 0.0021(9) C27A 0.0437(13) 0.0546(14) 0.0694(17) -0.0071(12) -0.0048(12) -0.0019(11) C28A 0.091(2) 0.0401(13) 0.0640(16) -0.0107(12) -0.0233(15) -0.0059(13) C29A 0.0420(12) 0.0480(13) 0.0716(17) -0.0111(12) -0.0149(11) 0.0060(10) C31A 0.0434(11) 0.0408(11) 0.0449(12) -0.0161(9) -0.0108(9) 0.0000(9) F32A 0.0532(8) 0.0444(7) 0.0807(10) -0.0131(7) -0.0315(7) 0.0034(6) C32A 0.0486(13) 0.0435(12) 0.0507(13) -0.0145(10) -0.0160(10) -0.0014(10) F33A 0.0881(11) 0.0428(8) 0.0887(12) -0.0054(7) -0.0383(9) 0.0046(7) C33A 0.0655(16) 0.0396(12) 0.0549(14) -0.0116(10) -0.0192(12) 0.0011(11) F34A 0.0929(12) 0.0492(8) 0.0737(10) -0.0100(7) -0.0116(9) -0.0223(8) C34A 0.0691(16) 0.0414(12) 0.0516(14) -0.0133(10) -0.0086(12) -0.0115(11) F35A 0.0547(9) 0.0738(10) 0.0983(13) -0.0253(9) -0.0112(8) -0.0205(8) C35A 0.0465(13) 0.0561(14) 0.0581(14) -0.0220(12) -0.0027(11) -0.0127(11) F36A 0.0441(7) 0.0584(8) 0.0968(12) -0.0202(8) -0.0262(8) 0.0023(6) C36A 0.0468(13) 0.0495(13) 0.0525(13) -0.0188(11) -0.0124(10) 0.0017(10) C41A 0.0446(12) 0.0349(10) 0.0495(12) -0.0116(9) -0.0158(10) 0.0001(9) F42A 0.0460(7) 0.0835(10) 0.0705(9) -0.0382(8) -0.0217(7) 0.0036(7) C42A 0.0482(13) 0.0495(13) 0.0556(14) -0.0214(11) -0.0174(11) 0.0018(10) F43A 0.0403(8) 0.1244(15) 0.0996(13) -0.0619(12) -0.0067(8) 0.0002(9) C43A 0.0426(13) 0.0640(16) 0.0706(17) -0.0290(13) -0.0115(12) -0.0001(11) F44A 0.0688(10) 0.1027(13) 0.0696(10) -0.0466(10) 0.0031(8) -0.0040(9) C44A 0.0532(14) 0.0562(14) 0.0560(15) -0.0251(12) -0.0031(11) -0.0019(11) F45A 0.0771(10) 0.0865(11) 0.0557(9) -0.0319(8) -0.0227(8) -0.0004(8) C45A 0.0643(15) 0.0476(13) 0.0487(13) -0.0188(11) -0.0183(11) -0.0001(11) F46A 0.0492(7) 0.0597(8) 0.0590(8) -0.0208(7) -0.0229(6) 0.0023(6) C46A 0.0439(12) 0.0379(11) 0.0500(13) -0.0118(9) -0.0155(10) 0.0008(9) B1A 0.0378(12) 0.0388(12) 0.0513(14) -0.0140(11) -0.0149(11) 0.0031(10) P1B 0.0467(3) 0.0499(3) 0.0474(3) -0.0166(3) -0.0177(3) 0.0031(2) S1B 0.0524(3) 0.0519(3) 0.0526(3) -0.0189(3) -0.0192(3) 0.0040(3) O1B 0.0478(9) 0.0530(9) 0.0471(9) -0.0120(7) -0.0141(7) 0.0045(7) O2B 0.0701(11) 0.0544(10) 0.0692(12) -0.0120(9) -0.0277(9) -0.0094(9) B1B 0.0474(14) 0.0507(15) 0.0500(15) -0.0141(12) -0.0137(12) 0.0033(12) C1B 0.0512(13) 0.0589(14) 0.0579(15) -0.0225(12) -0.0209(11) 0.0049(11) C2B 0.0458(12) 0.0587(14) 0.0504(13) -0.0186(11) -0.0160(10) 0.0034(10) C3B 0.0647(17) 0.0606(16) 0.088(2) -0.0275(15) -0.0313(15) 0.0058(13) C11B 0.0467(12) 0.0537(13) 0.0481(13) -0.0188(10) -0.0173(10) 0.0018(10) C12B 0.0486(13) 0.0622(15) 0.0451(13) -0.0184(11) -0.0171(10) -0.0006(11) C13B 0.0580(15) 0.0583(15) 0.0504(14) -0.0104(11) -0.0161(11) -0.0046(12) C14B 0.0647(16) 0.0538(14) 0.0594(15) -0.0139(12) -0.0225(13) 0.0006(12) C15B 0.0578(15) 0.0551(14) 0.0603(15) -0.0200(12) -0.0171(12) 0.0089(12) C16B 0.0501(13) 0.0566(14) 0.0521(14) -0.0172(11) -0.0155(11) 0.0020(11) C17B 0.0546(14) 0.0679(16) 0.0451(13) -0.0149(12) -0.0119(11) 0.0056(12) C18B 0.089(2) 0.0550(16) 0.078(2) -0.0091(14) -0.0179(17) -0.0011(15) C19B 0.0578(16) 0.0657(17) 0.0653(17) -0.0171(14) -0.0029(13) 0.0121(13) C21B 0.0471(13) 0.0535(13) 0.0534(14) -0.0185(11) -0.0179(11) 0.0056(10) C22B 0.0540(14) 0.0548(14) 0.0617(15) -0.0212(12) -0.0275(12) 0.0093(11) C23B 0.0522(15) 0.0754(18) 0.0781(19) -0.0319(15) -0.0305(14) 0.0040(13) C24B 0.0463(14) 0.0812(19) 0.088(2) -0.0370(17) -0.0196(14) -0.0019(13) C25B 0.0538(15) 0.0805(19) 0.0682(18) -0.0277(15) -0.0072(13) -0.0084(13) C26B 0.0501(14) 0.0655(16) 0.0586(15) -0.0223(12) -0.0133(12) 0.0001(12) C27B 0.0742(18) 0.0677(17) 0.0577(16) -0.0168(13) -0.0332(14) -0.0003(14) C28B 0.0551(18) 0.123(3) 0.123(3) -0.048(3) -0.0210(19) -0.0181(19) C29B 0.0656(17) 0.083(2) 0.0505(15) -0.0156(14) -0.0085(13) -0.0195(14) C31B 0.0483(13) 0.0532(13) 0.0546(14) -0.0177(11) -0.0194(11) 0.0026(10) F32B 0.0528(8) 0.0704(10) 0.0711(10) -0.0233(8) -0.0109(7) 0.0049(7) C32B 0.0507(13) 0.0593(15) 0.0572(15) -0.0217(12) -0.0199(12) 0.0041(11) F33B 0.0800(12) 0.0728(11) 0.1158(15) -0.0369(11) -0.0223(11) 0.0267(9) C33B 0.0611(16) 0.0615(16) 0.081(2) -0.0318(15) -0.0289(15) 0.0175(13) F34B 0.1296(17) 0.0551(10) 0.0959(14) -0.0146(9) -0.0454(12) 0.0237(10) C34B 0.088(2) 0.0474(14) 0.0740(19) -0.0164(13) -0.0388(17) 0.0114(14) F35B 0.1212(15) 0.0639(10) 0.0648(11) -0.0027(8) -0.0086(10) -0.0026(10) C35B 0.085(2) 0.0568(15) 0.0530(15) -0.0101(12) -0.0212(14) 0.0011(14) F36B 0.0811(11) 0.0673(10) 0.0700(11) -0.0045(8) 0.0085(9) 0.0138(8) C36B 0.0621(15) 0.0562(15) 0.0558(15) -0.0156(12) -0.0172(12) 0.0064(12) C41B 0.0488(13) 0.0528(13) 0.0449(13) -0.0099(10) -0.0157(10) 0.0036(10) F42B 0.0616(9) 0.0899(11) 0.0471(8) -0.0200(7) -0.0115(7) -0.0112(8) C42B 0.0570(14) 0.0602(15) 0.0461(13) -0.0126(11) -0.0188(11) 0.0009(11) F43B 0.0612(9) 0.1032(13) 0.0669(10) -0.0133(9) -0.0107(8) -0.0258(9) C43B 0.0538(14) 0.0669(16) 0.0539(15) -0.0109(12) -0.0135(12) -0.0097(12) F44B 0.0816(12) 0.1149(15) 0.0822(12) -0.0241(11) -0.0328(10) -0.0347(11) C44B 0.0631(16) 0.0726(18) 0.0636(17) -0.0140(14) -0.0265(14) -0.0142(14) F45B 0.0892(12) 0.1126(14) 0.0580(10) -0.0299(9) -0.0259(9) -0.0175(10) C45B 0.0673(17) 0.0745(18) 0.0503(14) -0.0176(13) -0.0250(13) -0.0054(14) F46B 0.0625(9) 0.0982(12) 0.0494(8) -0.0211(8) -0.0110(7) -0.0116(8) C46B 0.0540(14) 0.0646(15) 0.0441(13) -0.0129(11) -0.0114(11) -0.0032(12) _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 P1A C11A 1.820(2) . ? P1A C21A 1.821(2) . ? P1A C1A 1.849(2) . ? P1A S1A 2.3356(8) . ? S1A O2A 1.4631(19) . ? S1A O1A 1.5284(16) . ? O1A B1A 1.574(3) . ? C1A C3A 1.535(3) . ? C1A C2A 1.554(3) . ? C1A H1A 0.9900 . ? C2A B1A 1.613(3) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C3A H3A3 0.9700 . ? C11A C16A 1.410(3) . ? C11A C12A 1.417(3) . ? C12A C13A 1.394(4) . ? C12A C17A 1.507(4) . ? C13A C14A 1.381(5) . ? C13A H13A 0.9400 . ? C14A C15A 1.382(5) . ? C14A C18A 1.515(4) . ? C15A C16A 1.392(4) . ? C15A H15A 0.9400 . ? C16A C19A 1.509(4) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C17A H17C 0.9700 . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C18A H18C 0.9700 . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C19A H19C 0.9700 . ? C21A C22A 1.413(3) . ? C21A C26A 1.420(3) . ? C22A C23A 1.384(3) . ? C22A C27A 1.507(3) . ? C23A C24A 1.382(3) . ? C23A H23A 0.9400 . ? C24A C25A 1.380(4) . ? C24A C28A 1.514(3) . ? C25A C26A 1.396(3) . ? C25A H25A 0.9400 . ? C26A C29A 1.510(3) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C27A H27C 0.9700 . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C28A H28C 0.9700 . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C29A H29C 0.9700 . ? C31A C36A 1.386(3) . ? C31A C32A 1.389(3) . ? C31A B1A 1.648(3) . ? F32A C32A 1.359(3) . ? C32A C33A 1.377(3) . ? F33A C33A 1.343(3) . ? C33A C34A 1.376(4) . ? F34A C34A 1.342(3) . ? C34A C35A 1.372(4) . ? F35A C35A 1.347(3) . ? C35A C36A 1.386(3) . ? F36A C36A 1.350(3) . ? C41A C42A 1.390(3) . ? C41A C46A 1.393(3) . ? C41A B1A 1.641(3) . ? F42A C42A 1.359(3) . ? C42A C43A 1.371(4) . ? F43A C43A 1.351(3) . ? C43A C44A 1.373(4) . ? F44A C44A 1.336(3) . ? C44A C45A 1.371(4) . ? F45A C45A 1.347(3) . ? C45A C46A 1.376(3) . ? F46A C46A 1.352(3) . ? P1B C21B 1.817(3) . ? P1B C11B 1.821(3) . ? P1B C1B 1.863(2) . ? P1B S1B 2.3471(8) . ? S1B O2B 1.4554(19) . ? S1B O1B 1.5372(17) . ? O1B B1B 1.560(3) . ? B1B C2B 1.619(4) . ? B1B C41B 1.652(4) . ? B1B C31B 1.653(4) . ? C1B C3B 1.503(4) . ? C1B C2B 1.553(3) . ? C1B H1B 0.9900 . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C3B H3B3 0.9700 . ? C11B C16B 1.415(3) . ? C11B C12B 1.416(3) . ? C12B C13B 1.388(4) . ? C12B C17B 1.504(3) . ? C13B C14B 1.385(4) . ? C13B H13B 0.9400 . ? C14B C15B 1.385(4) . ? C14B C18B 1.513(4) . ? C15B C16B 1.386(4) . ? C15B H15B 0.9400 . ? C16B C19B 1.511(4) . ? C17B H17D 0.9700 . ? C17B H17E 0.9700 . ? C17B H17F 0.9700 . ? C18B H18D 0.9700 . ? C18B H18E 0.9700 . ? C18B H18F 0.9700 . ? C19B H19D 0.9700 . ? C19B H19E 0.9700 . ? C19B H19F 0.9700 . ? C21B C26B 1.410(4) . ? C21B C22B 1.413(4) . ? C22B C23B 1.387(4) . ? C22B C27B 1.509(4) . ? C23B C24B 1.386(4) . ? C23B H23B 0.9400 . ? C24B C25B 1.373(4) . ? C24B C28B 1.510(4) . ? C25B C26B 1.393(4) . ? C25B H25B 0.9400 . ? C26B C29B 1.505(4) . ? C27B H27D 0.9700 . ? C27B H27E 0.9700 . ? C27B H27F 0.9700 . ? C28B H28D 0.9700 . ? C28B H28E 0.9700 . ? C28B H28F 0.9700 . ? C29B H29D 0.9700 . ? C29B H29E 0.9700 . ? C29B H29F 0.9700 . ? C31B C32B 1.384(3) . ? C31B C36B 1.386(4) . ? F32B C32B 1.351(3) . ? C32B C33B 1.388(4) . ? F33B C33B 1.345(3) . ? C33B C34B 1.364(4) . ? F34B C34B 1.345(3) . ? C34B C35B 1.369(4) . ? F35B C35B 1.341(3) . ? C35B C36B 1.382(4) . ? F36B C36B 1.350(3) . ? C41B C46B 1.388(4) . ? C41B C42B 1.396(4) . ? F42B C42B 1.357(3) . ? C42B C43B 1.379(4) . ? F43B C43B 1.347(3) . ? C43B C44B 1.359(4) . ? F44B C44B 1.342(3) . ? C44B C45B 1.383(4) . ? F45B C45B 1.345(3) . ? C45B C46B 1.377(4) . ? F46B C46B 1.355(3) . ? 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 C11A P1A C21A 108.70(10) . . ? C11A P1A C1A 107.60(10) . . ? C21A P1A C1A 121.42(10) . . ? C11A P1A S1A 126.27(8) . . ? C21A P1A S1A 97.37(8) . . ? C1A P1A S1A 96.39(7) . . ? O2A S1A O1A 111.70(10) . . ? O2A S1A P1A 94.22(8) . . ? O1A S1A P1A 103.49(6) . . ? S1A O1A B1A 128.65(14) . . ? C3A C1A C2A 109.75(18) . . ? C3A C1A P1A 115.46(16) . . ? C2A C1A P1A 105.99(14) . . ? C3A C1A H1A 108.5 . . ? C2A C1A H1A 108.5 . . ? P1A C1A H1A 108.5 . . ? C1A C2A B1A 118.23(19) . . ? C1A C2A H2A1 107.8 . . ? B1A C2A H2A1 107.8 . . ? C1A C2A H2A2 107.8 . . ? B1A C2A H2A2 107.8 . . ? H2A1 C2A H2A2 107.1 . . ? C1A C3A H3A1 109.5 . . ? C1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C16A C11A C12A 120.1(2) . . ? C16A C11A P1A 121.29(18) . . ? C12A C11A P1A 118.61(18) . . ? C13A C12A C11A 117.8(2) . . ? C13A C12A C17A 116.5(2) . . ? C11A C12A C17A 125.7(2) . . ? C14A C13A C12A 123.2(3) . . ? C14A C13A H13A 118.4 . . ? C12A C13A H13A 118.4 . . ? C13A C14A C15A 117.7(3) . . ? C13A C14A C18A 121.3(3) . . ? C15A C14A C18A 121.0(3) . . ? C14A C15A C16A 122.6(3) . . ? C14A C15A H15A 118.7 . . ? C16A C15A H15A 118.7 . . ? C15A C16A C11A 118.6(2) . . ? C15A C16A C19A 117.4(2) . . ? C11A C16A C19A 124.0(2) . . ? C12A C17A H17A 109.5 . . ? C12A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C12A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C14A C18A H18A 109.5 . . ? C14A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C14A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C16A C19A H19A 109.5 . . ? C16A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C16A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C22A C21A C26A 119.1(2) . . ? C22A C21A P1A 125.57(16) . . ? C26A C21A P1A 115.33(17) . . ? C23A C22A C21A 119.0(2) . . ? C23A C22A C27A 116.8(2) . . ? C21A C22A C27A 124.1(2) . . ? C24A C23A C22A 122.6(2) . . ? C24A C23A H23A 118.7 . . ? C22A C23A H23A 118.7 . . ? C25A C24A C23A 118.0(2) . . ? C25A C24A C28A 121.1(2) . . ? C23A C24A C28A 120.8(2) . . ? C24A C25A C26A 122.3(2) . . ? C24A C25A H25A 118.8 . . ? C26A C25A H25A 118.8 . . ? C25A C26A C21A 118.6(2) . . ? C25A C26A C29A 117.0(2) . . ? C21A C26A C29A 124.4(2) . . ? C22A C27A H27A 109.5 . . ? C22A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C22A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C24A C28A H28A 109.5 . . ? C24A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C24A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C26A C29A H29A 109.5 . . ? C26A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C26A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C36A C31A C32A 113.1(2) . . ? C36A C31A B1A 127.9(2) . . ? C32A C31A B1A 118.99(19) . . ? F32A C32A C33A 115.6(2) . . ? F32A C32A C31A 119.2(2) . . ? C33A C32A C31A 125.2(2) . . ? F33A C33A C34A 119.9(2) . . ? F33A C33A C32A 121.1(2) . . ? C34A C33A C32A 119.0(2) . . ? F34A C34A C35A 120.6(2) . . ? F34A C34A C33A 120.7(2) . . ? C35A C34A C33A 118.8(2) . . ? F35A C35A C34A 119.6(2) . . ? F35A C35A C36A 120.2(2) . . ? C34A C35A C36A 120.2(2) . . ? F36A C36A C31A 121.1(2) . . ? F36A C36A C35A 115.2(2) . . ? C31A C36A C35A 123.7(2) . . ? C42A C41A C46A 112.9(2) . . ? C42A C41A B1A 126.6(2) . . ? C46A C41A B1A 120.25(19) . . ? F42A C42A C43A 115.4(2) . . ? F42A C42A C41A 120.4(2) . . ? C43A C42A C41A 124.3(2) . . ? F43A C43A C42A 120.5(2) . . ? F43A C43A C44A 119.3(2) . . ? C42A C43A C44A 120.2(2) . . ? F44A C44A C45A 120.9(2) . . ? F44A C44A C43A 120.6(2) . . ? C45A C44A C43A 118.5(2) . . ? F45A C45A C44A 119.7(2) . . ? F45A C45A C46A 120.6(2) . . ? C44A C45A C46A 119.6(2) . . ? F46A C46A C45A 116.2(2) . . ? F46A C46A C41A 119.24(19) . . ? C45A C46A C41A 124.5(2) . . ? O1A B1A C2A 106.51(17) . . ? O1A B1A C41A 108.80(18) . . ? C2A B1A C41A 117.40(19) . . ? O1A B1A C31A 106.10(17) . . ? C2A B1A C31A 110.57(19) . . ? C41A B1A C31A 106.91(17) . . ? C21B P1B C11B 109.03(11) . . ? C21B P1B C1B 107.33(11) . . ? C11B P1B C1B 119.97(12) . . ? C21B P1B S1B 121.74(8) . . ? C11B P1B S1B 98.64(8) . . ? C1B P1B S1B 100.75(8) . . ? O2B S1B O1B 112.25(10) . . ? O2B S1B P1B 98.70(8) . . ? O1B S1B P1B 98.24(7) . . ? S1B O1B B1B 126.23(15) . . ? O1B B1B C2B 108.04(19) . . ? O1B B1B C41B 107.30(19) . . ? C2B B1B C41B 113.5(2) . . ? O1B B1B C31B 105.46(19) . . ? C2B B1B C31B 116.5(2) . . ? C41B B1B C31B 105.38(19) . . ? C3B C1B C2B 113.4(2) . . ? C3B C1B P1B 109.99(19) . . ? C2B C1B P1B 112.02(17) . . ? C3B C1B H1B 107.0 . . ? C2B C1B H1B 107.0 . . ? P1B C1B H1B 107.0 . . ? C1B C2B B1B 118.6(2) . . ? C1B C2B H2B1 107.7 . . ? B1B C2B H2B1 107.7 . . ? C1B C2B H2B2 107.7 . . ? B1B C2B H2B2 107.7 . . ? H2B1 C2B H2B2 107.1 . . ? C1B C3B H3B1 109.5 . . ? C1B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C1B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C16B C11B C12B 119.5(2) . . ? C16B C11B P1B 114.98(18) . . ? C12B C11B P1B 125.35(18) . . ? C13B C12B C11B 118.5(2) . . ? C13B C12B C17B 116.6(2) . . ? C11B C12B C17B 124.9(2) . . ? C14B C13B C12B 122.9(2) . . ? C14B C13B H13B 118.6 . . ? C12B C13B H13B 118.6 . . ? C13B C14B C15B 117.6(2) . . ? C13B C14B C18B 121.5(3) . . ? C15B C14B C18B 120.9(2) . . ? C14B C15B C16B 122.6(2) . . ? C14B C15B H15B 118.7 . . ? C16B C15B H15B 118.7 . . ? C15B C16B C11B 118.8(2) . . ? C15B C16B C19B 116.5(2) . . ? C11B C16B C19B 124.7(2) . . ? C12B C17B H17D 109.5 . . ? C12B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C12B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C14B C18B H18D 109.5 . . ? C14B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C14B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C16B C19B H19D 109.5 . . ? C16B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C16B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C26B C21B C22B 120.2(2) . . ? C26B C21B P1B 121.37(19) . . ? C22B C21B P1B 118.38(19) . . ? C23B C22B C21B 118.2(3) . . ? C23B C22B C27B 118.0(2) . . ? C21B C22B C27B 123.7(2) . . ? C24B C23B C22B 122.5(3) . . ? C24B C23B H23B 118.8 . . ? C22B C23B H23B 118.8 . . ? C25B C24B C23B 118.2(3) . . ? C25B C24B C28B 120.6(3) . . ? C23B C24B C28B 121.1(3) . . ? C24B C25B C26B 122.6(3) . . ? C24B C25B H25B 118.7 . . ? C26B C25B H25B 118.7 . . ? C25B C26B C21B 118.3(3) . . ? C25B C26B C29B 118.1(2) . . ? C21B C26B C29B 123.6(2) . . ? C22B C27B H27D 109.5 . . ? C22B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C22B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C24B C28B H28D 109.5 . . ? C24B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C24B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C26B C29B H29D 109.5 . . ? C26B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C26B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C32B C31B C36B 113.2(2) . . ? C32B C31B B1B 118.9(2) . . ? C36B C31B B1B 127.6(2) . . ? F32B C32B C31B 119.4(2) . . ? F32B C32B C33B 116.2(2) . . ? C31B C32B C33B 124.4(3) . . ? F33B C33B C34B 120.4(3) . . ? F33B C33B C32B 120.2(3) . . ? C34B C33B C32B 119.4(2) . . ? F34B C34B C33B 120.9(3) . . ? F34B C34B C35B 120.1(3) . . ? C33B C34B C35B 119.0(3) . . ? F35B C35B C34B 119.4(3) . . ? F35B C35B C36B 120.8(3) . . ? C34B C35B C36B 119.8(3) . . ? F36B C36B C35B 114.3(2) . . ? F36B C36B C31B 121.6(2) . . ? C35B C36B C31B 124.1(2) . . ? C46B C41B C42B 112.6(2) . . ? C46B C41B B1B 121.8(2) . . ? C42B C41B B1B 125.5(2) . . ? F42B C42B C43B 115.1(2) . . ? F42B C42B C41B 120.5(2) . . ? C43B C42B C41B 124.4(2) . . ? F43B C43B C44B 119.4(2) . . ? F43B C43B C42B 120.6(2) . . ? C44B C43B C42B 120.1(2) . . ? F44B C44B C43B 121.1(3) . . ? F44B C44B C45B 120.0(3) . . ? C43B C44B C45B 118.9(3) . . ? F45B C45B C46B 121.1(2) . . ? F45B C45B C44B 119.7(2) . . ? C46B C45B C44B 119.3(2) . . ? F46B C46B C45B 115.6(2) . . ? F46B C46B C41B 119.6(2) . . ? C45B C46B C41B 124.8(2) . . ? 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 C11A P1A S1A O2A 174.82(11) . . . . ? C21A P1A S1A O2A 55.09(10) . . . . ? C1A P1A S1A O2A -67.82(10) . . . . ? C11A P1A S1A O1A -71.66(11) . . . . ? C21A P1A S1A O1A 168.61(9) . . . . ? C1A P1A S1A O1A 45.69(10) . . . . ? O2A S1A O1A B1A 52.5(2) . . . . ? P1A S1A O1A B1A -47.73(18) . . . . ? C11A P1A C1A C3A -49.4(2) . . . . ? C21A P1A C1A C3A 76.6(2) . . . . ? S1A P1A C1A C3A 179.30(17) . . . . ? C11A P1A C1A C2A 72.31(17) . . . . ? C21A P1A C1A C2A -161.68(14) . . . . ? S1A P1A C1A C2A -58.99(14) . . . . ? C3A C1A C2A B1A -155.1(2) . . . . ? P1A C1A C2A B1A 79.6(2) . . . . ? C21A P1A C11A C16A 128.38(19) . . . . ? C1A P1A C11A C16A -98.4(2) . . . . ? S1A P1A C11A C16A 13.8(2) . . . . ? C21A P1A C11A C12A -52.1(2) . . . . ? C1A P1A C11A C12A 81.1(2) . . . . ? S1A P1A C11A C12A -166.74(15) . . . . ? C16A C11A C12A C13A 3.5(3) . . . . ? P1A C11A C12A C13A -176.03(19) . . . . ? C16A C11A C12A C17A -173.6(2) . . . . ? P1A C11A C12A C17A 6.9(3) . . . . ? C11A C12A C13A C14A -0.8(4) . . . . ? C17A C12A C13A C14A 176.5(3) . . . . ? C12A C13A C14A C15A -1.9(5) . . . . ? C12A C13A C14A C18A 179.9(3) . . . . ? C13A C14A C15A C16A 2.1(5) . . . . ? C18A C14A C15A C16A -179.8(3) . . . . ? C14A C15A C16A C11A 0.5(4) . . . . ? C14A C15A C16A C19A -177.0(3) . . . . ? C12A C11A C16A C15A -3.3(3) . . . . ? P1A C11A C16A C15A 176.15(19) . . . . ? C12A C11A C16A C19A 174.0(2) . . . . ? P1A C11A C16A C19A -6.6(3) . . . . ? C11A P1A C21A C22A 127.7(2) . . . . ? C1A P1A C21A C22A 2.2(3) . . . . ? S1A P1A C21A C22A -100.0(2) . . . . ? C11A P1A C21A C26A -52.0(2) . . . . ? C1A P1A C21A C26A -177.50(16) . . . . ? S1A P1A C21A C26A 80.35(17) . . . . ? C26A C21A C22A C23A 5.3(3) . . . . ? P1A C21A C22A C23A -174.36(18) . . . . ? C26A C21A C22A C27A -175.1(2) . . . . ? P1A C21A C22A C27A 5.2(4) . . . . ? C21A C22A C23A C24A -1.3(4) . . . . ? C27A C22A C23A C24A 179.1(2) . . . . ? C22A C23A C24A C25A -3.5(4) . . . . ? C22A C23A C24A C28A 178.4(2) . . . . ? C23A C24A C25A C26A 4.2(4) . . . . ? C28A C24A C25A C26A -177.7(2) . . . . ? C24A C25A C26A C21A -0.2(4) . . . . ? C24A C25A C26A C29A 179.9(2) . . . . ? C22A C21A C26A C25A -4.6(3) . . . . ? P1A C21A C26A C25A 175.09(18) . . . . ? C22A C21A C26A C29A 175.2(2) . . . . ? P1A C21A C26A C29A -5.0(3) . . . . ? C36A C31A C32A F32A 176.3(2) . . . . ? B1A C31A C32A F32A -3.0(3) . . . . ? C36A C31A C32A C33A -2.0(3) . . . . ? B1A C31A C32A C33A 178.7(2) . . . . ? F32A C32A C33A F33A 2.7(3) . . . . ? C31A C32A C33A F33A -178.9(2) . . . . ? F32A C32A C33A C34A -177.1(2) . . . . ? C31A C32A C33A C34A 1.3(4) . . . . ? F33A C33A C34A F34A 0.2(4) . . . . ? C32A C33A C34A F34A -180.0(2) . . . . ? F33A C33A C34A C35A -179.6(2) . . . . ? C32A C33A C34A C35A 0.2(4) . . . . ? F34A C34A C35A F35A -1.1(4) . . . . ? C33A C34A C35A F35A 178.8(2) . . . . ? F34A C34A C35A C36A 179.5(2) . . . . ? C33A C34A C35A C36A -0.7(4) . . . . ? C32A C31A C36A F36A -177.7(2) . . . . ? B1A C31A C36A F36A 1.6(4) . . . . ? C32A C31A C36A C35A 1.5(3) . . . . ? B1A C31A C36A C35A -179.3(2) . . . . ? F35A C35A C36A F36A -0.5(3) . . . . ? C34A C35A C36A F36A 179.0(2) . . . . ? F35A C35A C36A C31A -179.6(2) . . . . ? C34A C35A C36A C31A -0.2(4) . . . . ? C46A C41A C42A F42A -178.9(2) . . . . ? B1A C41A C42A F42A -5.3(3) . . . . ? C46A C41A C42A C43A 0.8(3) . . . . ? B1A C41A C42A C43A 174.4(2) . . . . ? F42A C42A C43A F43A -1.2(4) . . . . ? C41A C42A C43A F43A 179.1(2) . . . . ? F42A C42A C43A C44A 179.8(2) . . . . ? C41A C42A C43A C44A 0.1(4) . . . . ? F43A C43A C44A F44A -0.5(4) . . . . ? C42A C43A C44A F44A 178.6(2) . . . . ? F43A C43A C44A C45A -179.6(2) . . . . ? C42A C43A C44A C45A -0.5(4) . . . . ? F44A C44A C45A F45A 2.2(4) . . . . ? C43A C44A C45A F45A -178.7(2) . . . . ? F44A C44A C45A C46A -179.0(2) . . . . ? C43A C44A C45A C46A 0.1(4) . . . . ? F45A C45A C46A F46A 1.2(3) . . . . ? C44A C45A C46A F46A -177.6(2) . . . . ? F45A C45A C46A C41A 179.7(2) . . . . ? C44A C45A C46A C41A 0.9(4) . . . . ? C42A C41A C46A F46A 177.16(19) . . . . ? B1A C41A C46A F46A 3.1(3) . . . . ? C42A C41A C46A C45A -1.3(3) . . . . ? B1A C41A C46A C45A -175.3(2) . . . . ? S1A O1A B1A C2A 52.4(2) . . . . ? S1A O1A B1A C41A -75.0(2) . . . . ? S1A O1A B1A C31A 170.26(14) . . . . ? C1A C2A B1A O1A -64.2(2) . . . . ? C1A C2A B1A C41A 57.9(3) . . . . ? C1A C2A B1A C31A -179.07(18) . . . . ? C42A C41A B1A O1A 139.3(2) . . . . ? C46A C41A B1A O1A -47.6(3) . . . . ? C42A C41A B1A C2A 18.3(3) . . . . ? C46A C41A B1A C2A -168.53(19) . . . . ? C42A C41A B1A C31A -106.5(2) . . . . ? C46A C41A B1A C31A 66.6(2) . . . . ? C36A C31A B1A O1A 5.0(3) . . . . ? C32A C31A B1A O1A -175.81(19) . . . . ? C36A C31A B1A C2A 120.1(2) . . . . ? C32A C31A B1A C2A -60.7(3) . . . . ? C36A C31A B1A C41A -111.0(2) . . . . ? C32A C31A B1A C41A 68.2(3) . . . . ? C21B P1B S1B O2B -156.23(12) . . . . ? C11B P1B S1B O2B -37.42(11) . . . . ? C1B P1B S1B O2B 85.48(12) . . . . ? C21B P1B S1B O1B 89.61(11) . . . . ? C11B P1B S1B O1B -151.58(10) . . . . ? C1B P1B S1B O1B -28.68(11) . . . . ? O2B S1B O1B B1B -36.0(2) . . . . ? P1B S1B O1B B1B 67.02(19) . . . . ? S1B O1B B1B C2B -38.1(3) . . . . ? S1B O1B B1B C41B 84.6(2) . . . . ? S1B O1B B1B C31B -163.39(15) . . . . ? C21B P1B C1B C3B -27.1(2) . . . . ? C11B P1B C1B C3B -152.15(18) . . . . ? S1B P1B C1B C3B 101.23(18) . . . . ? C21B P1B C1B C2B -154.15(18) . . . . ? C11B P1B C1B C2B 80.8(2) . . . . ? S1B P1B C1B C2B -25.82(19) . . . . ? C3B C1B C2B B1B -54.9(3) . . . . ? P1B C1B C2B B1B 70.3(3) . . . . ? O1B B1B C2B C1B -44.5(3) . . . . ? C41B B1B C2B C1B -163.3(2) . . . . ? C31B B1B C2B C1B 74.0(3) . . . . ? C21B P1B C11B C16B 59.5(2) . . . . ? C1B P1B C11B C16B -176.28(17) . . . . ? S1B P1B C11B C16B -68.49(18) . . . . ? C21B P1B C11B C12B -124.7(2) . . . . ? C1B P1B C11B C12B -0.5(3) . . . . ? S1B P1B C11B C12B 107.3(2) . . . . ? C16B C11B C12B C13B 1.0(3) . . . . ? P1B C11B C12B C13B -174.64(19) . . . . ? C16B C11B C12B C17B -177.2(2) . . . . ? P1B C11B C12B C17B 7.2(4) . . . . ? C11B C12B C13B C14B -0.6(4) . . . . ? C17B C12B C13B C14B 177.8(2) . . . . ? C12B C13B C14B C15B -0.7(4) . . . . ? C12B C13B C14B C18B 179.1(3) . . . . ? C13B C14B C15B C16B 1.5(4) . . . . ? C18B C14B C15B C16B -178.2(3) . . . . ? C14B C15B C16B C11B -1.1(4) . . . . ? C14B C15B C16B C19B 179.3(3) . . . . ? C12B C11B C16B C15B -0.2(4) . . . . ? P1B C11B C16B C15B 175.9(2) . . . . ? C12B C11B C16B C19B 179.3(3) . . . . ? P1B C11B C16B C19B -4.6(3) . . . . ? C11B P1B C21B C26B -127.4(2) . . . . ? C1B P1B C21B C26B 101.2(2) . . . . ? S1B P1B C21B C26B -13.8(2) . . . . ? C11B P1B C21B C22B 55.3(2) . . . . ? C1B P1B C21B C22B -76.1(2) . . . . ? S1B P1B C21B C22B 168.92(15) . . . . ? C26B C21B C22B C23B 1.7(4) . . . . ? P1B C21B C22B C23B 179.00(19) . . . . ? C26B C21B C22B C27B -176.1(2) . . . . ? P1B C21B C22B C27B 1.2(3) . . . . ? C21B C22B C23B C24B 0.1(4) . . . . ? C27B C22B C23B C24B 178.1(3) . . . . ? C22B C23B C24B C25B -1.3(4) . . . . ? C22B C23B C24B C28B 179.8(3) . . . . ? C23B C24B C25B C26B 0.7(5) . . . . ? C28B C24B C25B C26B 179.6(3) . . . . ? C24B C25B C26B C21B 1.1(4) . . . . ? C24B C25B C26B C29B -178.3(3) . . . . ? C22B C21B C26B C25B -2.3(4) . . . . ? P1B C21B C26B C25B -179.5(2) . . . . ? C22B C21B C26B C29B 177.0(3) . . . . ? P1B C21B C26B C29B -0.1(4) . . . . ? O1B B1B C31B C32B 177.9(2) . . . . ? C2B B1B C31B C32B 58.1(3) . . . . ? C41B B1B C31B C32B -68.7(3) . . . . ? O1B B1B C31B C36B -8.4(3) . . . . ? C2B B1B C31B C36B -128.3(3) . . . . ? C41B B1B C31B C36B 104.9(3) . . . . ? C36B C31B C32B F32B 179.8(2) . . . . ? B1B C31B C32B F32B -5.7(3) . . . . ? C36B C31B C32B C33B -1.2(4) . . . . ? B1B C31B C32B C33B 173.3(2) . . . . ? F32B C32B C33B F33B 0.1(4) . . . . ? C31B C32B C33B F33B -178.9(2) . . . . ? F32B C32B C33B C34B 179.3(2) . . . . ? C31B C32B C33B C34B 0.3(4) . . . . ? F33B C33B C34B F34B -1.0(4) . . . . ? C32B C33B C34B F34B 179.8(3) . . . . ? F33B C33B C34B C35B -179.6(3) . . . . ? C32B C33B C34B C35B 1.1(4) . . . . ? F34B C34B C35B F35B -0.5(4) . . . . ? C33B C34B C35B F35B 178.2(3) . . . . ? F34B C34B C35B C36B 179.8(3) . . . . ? C33B C34B C35B C36B -1.6(5) . . . . ? F35B C35B C36B F36B 0.5(4) . . . . ? C34B C35B C36B F36B -179.7(3) . . . . ? F35B C35B C36B C31B -179.2(3) . . . . ? C34B C35B C36B C31B 0.6(5) . . . . ? C32B C31B C36B F36B -178.9(2) . . . . ? B1B C31B C36B F36B 7.2(4) . . . . ? C32B C31B C36B C35B 0.8(4) . . . . ? B1B C31B C36B C35B -173.1(3) . . . . ? O1B B1B C41B C46B 39.4(3) . . . . ? C2B B1B C41B C46B 158.7(2) . . . . ? C31B B1B C41B C46B -72.6(3) . . . . ? O1B B1B C41B C42B -144.6(2) . . . . ? C2B B1B C41B C42B -25.3(3) . . . . ? C31B B1B C41B C42B 103.4(3) . . . . ? C46B C41B C42B F42B 179.1(2) . . . . ? B1B C41B C42B F42B 2.8(4) . . . . ? C46B C41B C42B C43B -0.6(4) . . . . ? B1B C41B C42B C43B -176.9(2) . . . . ? F42B C42B C43B F43B 1.0(4) . . . . ? C41B C42B C43B F43B -179.3(2) . . . . ? F42B C42B C43B C44B -179.7(2) . . . . ? C41B C42B C43B C44B -0.1(4) . . . . ? F43B C43B C44B F44B 0.6(4) . . . . ? C42B C43B C44B F44B -178.7(3) . . . . ? F43B C43B C44B C45B 179.2(3) . . . . ? C42B C43B C44B C45B -0.1(4) . . . . ? F44B C44B C45B F45B -0.2(4) . . . . ? C43B C44B C45B F45B -178.9(3) . . . . ? F44B C44B C45B C46B 179.5(3) . . . . ? C43B C44B C45B C46B 0.8(4) . . . . ? F45B C45B C46B F46B -3.3(4) . . . . ? C44B C45B C46B F46B 177.0(3) . . . . ? F45B C45B C46B C41B 178.2(2) . . . . ? C44B C45B C46B C41B -1.6(5) . . . . ? C42B C41B C46B F46B -177.1(2) . . . . ? B1B C41B C46B F46B -0.7(4) . . . . ? C42B C41B C46B C45B 1.4(4) . . . . ? B1B C41B C46B C45B 177.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 67.20 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.358 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.049 # Attachment '- 6.cif' data_erk6341 _database_code_depnum_ccdc_archive 'CCDC 895195' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 B F10 O2 P S' _chemical_formula_weight 760.46 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' B B 0.0090 0.0039 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5993(4) _cell_length_b 11.8650(4) _cell_length_c 14.4165(9) _cell_angle_alpha 92.700(3) _cell_angle_beta 95.322(2) _cell_angle_gamma 111.030(4) _cell_volume 1678.66(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5136 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 2.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5891 _exptl_absorpt_correction_T_max 0.8837 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19387 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 66.65 _reflns_number_total 5692 _reflns_number_gt 4822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The O2 atom was found in the asymmetric unit disordered over two positions. Several restraints (SADI, SAME and SIMU) were used in order to improve refinement stability. ; _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^)+(0.0518P)^2^+1.3013P] 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 5692 _refine_ls_number_parameters 476 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.031 _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 P1 P 0.18422(6) 0.89909(5) 0.25401(4) 0.03134(15) Uani 1 1 d . A . B1 B 0.2934(3) 0.6582(2) 0.27524(19) 0.0355(6) Uani 1 1 d . . . O1 O 0.34311(15) 0.76159(14) 0.20820(11) 0.0361(4) Uani 1 1 d . A . S1 S 0.24419(7) 0.78997(6) 0.13556(4) 0.04162(17) Uani 1 1 d D . . O2A O 0.1356(3) 0.6898(2) 0.08959(17) 0.0518(8) Uani 0.744(5) 1 d PD A 1 O2B O 0.3035(7) 0.8558(6) 0.0698(4) 0.044(2) Uani 0.256(5) 1 d PD A 2 C1 C 0.2165(2) 0.8272(2) 0.36116(15) 0.0338(5) Uani 1 1 d . . . H1 H 0.3129 0.8702 0.3871 0.041 Uiso 1 1 calc R A . C6 C 0.1268(3) 0.8495(2) 0.43322(17) 0.0424(6) Uani 1 1 d . A . H6A H 0.1492 0.9369 0.4453 0.051 Uiso 1 1 calc R . . H6B H 0.0309 0.8128 0.4072 0.051 Uiso 1 1 calc R . . C5 C 0.1475(3) 0.7963(3) 0.52502(18) 0.0539(7) Uani 1 1 d . . . H5A H 0.2417 0.8372 0.5537 0.065 Uiso 1 1 calc R A . H5B H 0.0873 0.8099 0.5682 0.065 Uiso 1 1 calc R . . C4 C 0.1171(3) 0.6617(3) 0.5083(2) 0.0551(7) Uani 1 1 d . A . H4A H 0.0210 0.6199 0.4842 0.066 Uiso 1 1 calc R . . H4B H 0.1342 0.6294 0.5675 0.066 Uiso 1 1 calc R . . C3 C 0.2060(3) 0.6386(3) 0.43850(18) 0.0450(6) Uani 1 1 d . . . H3A H 0.1826 0.5509 0.4277 0.054 Uiso 1 1 calc R A . H3B H 0.3013 0.6740 0.4662 0.054 Uiso 1 1 calc R . . C2 C 0.1930(2) 0.6902(2) 0.34309(16) 0.0354(5) Uani 1 1 d . A . H2 H 0.0983 0.6483 0.3135 0.042 Uiso 1 1 calc R . . C11 C 0.3148(2) 1.0412(2) 0.23232(17) 0.0349(5) Uani 1 1 d . . . C12 C 0.4263(2) 1.1130(2) 0.29681(18) 0.0390(5) Uani 1 1 d . A . C13 C 0.5251(3) 1.2125(2) 0.2655(2) 0.0500(7) Uani 1 1 d . . . H13 H 0.6008 1.2597 0.3078 0.060 Uiso 1 1 calc R A . C14 C 0.5166(3) 1.2447(3) 0.1752(2) 0.0581(8) Uani 1 1 d . A . C15 C 0.4035(3) 1.1774(2) 0.1145(2) 0.0519(7) Uani 1 1 d . . . H15 H 0.3954 1.2003 0.0534 0.062 Uiso 1 1 calc R A . C16 C 0.3006(3) 1.0764(2) 0.14031(18) 0.0411(6) Uani 1 1 d . A . C17 C 0.4432(3) 1.0966(2) 0.39990(19) 0.0485(6) Uani 1 1 d . . . H17A H 0.4900 1.0407 0.4100 0.073 Uiso 1 1 calc R A . H17B H 0.3543 1.0645 0.4218 0.073 Uiso 1 1 calc R . . H17C H 0.4960 1.1743 0.4341 0.073 Uiso 1 1 calc R . . C18 C 0.6266(4) 1.3541(3) 0.1444(3) 0.0921(13) Uani 1 1 d . . . H18A H 0.5926 1.4194 0.1375 0.138 Uiso 1 1 calc R A . H18B H 0.6517 1.3324 0.0850 0.138 Uiso 1 1 calc R . . H18C H 0.7058 1.3804 0.1910 0.138 Uiso 1 1 calc R . . C19 C 0.1764(3) 1.0188(3) 0.06998(19) 0.0512(7) Uani 1 1 d . . . H19A H 0.1056 1.0479 0.0853 0.077 Uiso 1 1 calc R A . H19B H 0.1440 0.9314 0.0714 0.077 Uiso 1 1 calc R . . H19C H 0.1996 1.0399 0.0079 0.077 Uiso 1 1 calc R . . C21 C 0.0198(2) 0.9182(2) 0.24442(16) 0.0351(5) Uani 1 1 d . . . C22 C 0.0117(2) 1.0334(2) 0.26292(17) 0.0387(5) Uani 1 1 d . A . C23 C -0.1118(3) 1.0463(2) 0.23655(18) 0.0439(6) Uani 1 1 d . . . H23 H -0.1182 1.1224 0.2490 0.053 Uiso 1 1 calc R A . C24 C -0.2254(3) 0.9527(3) 0.19299(18) 0.0447(6) Uani 1 1 d . A . C25 C -0.2184(2) 0.8389(2) 0.18348(17) 0.0428(6) Uani 1 1 d . . . H25 H -0.2968 0.7729 0.1587 0.051 Uiso 1 1 calc R A . C26 C -0.0986(2) 0.8187(2) 0.20946(16) 0.0374(5) Uani 1 1 d . A . C27 C 0.1252(3) 1.1444(2) 0.3109(2) 0.0532(7) Uani 1 1 d . . . H27A H 0.1763 1.1205 0.3603 0.080 Uiso 1 1 calc R A . H27B H 0.0868 1.1999 0.3374 0.080 Uiso 1 1 calc R . . H27C H 0.1852 1.1841 0.2657 0.080 Uiso 1 1 calc R . . C28 C -0.3522(3) 0.9754(3) 0.1571(2) 0.0608(8) Uani 1 1 d . . . H28A H -0.3354 1.0208 0.1024 0.091 Uiso 1 1 calc R A . H28B H -0.3759 1.0213 0.2054 0.091 Uiso 1 1 calc R . . H28C H -0.4267 0.8984 0.1404 0.091 Uiso 1 1 calc R . . C29 C -0.1048(3) 0.6900(2) 0.2028(2) 0.0478(6) Uani 1 1 d . . . H29A H -0.1141 0.6591 0.2639 0.072 Uiso 1 1 calc R A . H29B H -0.0219 0.6873 0.1811 0.072 Uiso 1 1 calc R . . H29C H -0.1824 0.6406 0.1590 0.072 Uiso 1 1 calc R . . C31 C 0.4371(2) 0.6600(2) 0.33229(16) 0.0350(5) Uani 1 1 d . . . C32 C 0.5490(2) 0.7642(2) 0.36008(16) 0.0377(5) Uani 1 1 d . . . F32 F 0.54287(14) 0.87455(12) 0.34646(11) 0.0487(4) Uani 1 1 d . . . C33 C 0.6710(2) 0.7662(2) 0.40454(17) 0.0431(6) Uani 1 1 d . . . F33 F 0.77541(15) 0.87219(15) 0.42909(12) 0.0603(4) Uani 1 1 d . . . C34 C 0.6848(3) 0.6594(3) 0.42484(18) 0.0475(6) Uani 1 1 d . . . F34 F 0.80210(16) 0.65938(18) 0.46925(13) 0.0712(5) Uani 1 1 d . . . C35 C 0.5770(3) 0.5533(2) 0.40070(18) 0.0460(6) Uani 1 1 d . . . F35 F 0.58857(18) 0.44742(16) 0.42127(13) 0.0671(5) Uani 1 1 d . . . C36 C 0.4570(2) 0.5555(2) 0.35701(17) 0.0408(6) Uani 1 1 d . . . F36 F 0.35444(16) 0.44590(13) 0.33995(12) 0.0576(4) Uani 1 1 d . . . C41 C 0.2267(2) 0.5331(2) 0.20384(17) 0.0387(5) Uani 1 1 d . . . C42 C 0.3033(3) 0.5111(2) 0.13679(18) 0.0443(6) Uani 1 1 d . . . F42 F 0.43295(15) 0.58745(15) 0.13473(11) 0.0567(4) Uani 1 1 d . . . C43 C 0.2569(3) 0.4144(3) 0.06954(19) 0.0501(7) Uani 1 1 d . . . F43 F 0.33859(19) 0.39982(16) 0.00742(12) 0.0672(5) Uani 1 1 d . . . C44 C 0.1272(3) 0.3335(2) 0.0668(2) 0.0529(7) Uani 1 1 d . . . F44 F 0.0806(2) 0.23722(15) 0.00230(13) 0.0738(5) Uani 1 1 d . . . C45 C 0.0459(3) 0.3495(2) 0.1295(2) 0.0512(7) Uani 1 1 d . . . F45 F -0.08363(18) 0.27191(15) 0.12644(14) 0.0727(5) Uani 1 1 d . . . C46 C 0.0970(3) 0.4468(2) 0.19753(19) 0.0457(6) Uani 1 1 d . . . F46 F 0.00942(16) 0.45257(14) 0.25888(12) 0.0604(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0298(3) 0.0319(3) 0.0322(3) 0.0010(2) 0.0010(2) 0.0119(2) B1 0.0309(13) 0.0347(14) 0.0400(14) 0.0050(11) -0.0001(11) 0.0119(11) O1 0.0342(8) 0.0387(9) 0.0366(9) 0.0059(7) 0.0025(7) 0.0149(7) S1 0.0516(4) 0.0462(4) 0.0330(3) -0.0004(3) -0.0003(3) 0.0268(3) O2A 0.0618(17) 0.0509(15) 0.0435(14) -0.0116(11) -0.0168(12) 0.0291(13) O2B 0.051(4) 0.051(4) 0.033(4) 0.018(3) 0.016(3) 0.020(3) C1 0.0301(12) 0.0411(13) 0.0305(11) 0.0025(10) 0.0016(9) 0.0139(10) C6 0.0385(13) 0.0525(15) 0.0383(13) 0.0032(11) 0.0067(11) 0.0186(12) C5 0.0472(16) 0.086(2) 0.0333(13) 0.0062(13) 0.0092(12) 0.0289(15) C4 0.0449(15) 0.080(2) 0.0501(16) 0.0281(15) 0.0136(13) 0.0298(15) C3 0.0389(14) 0.0573(16) 0.0443(14) 0.0174(12) 0.0065(11) 0.0223(12) C2 0.0294(12) 0.0383(13) 0.0373(12) 0.0078(10) -0.0009(10) 0.0116(10) C11 0.0320(12) 0.0319(12) 0.0415(13) 0.0006(10) 0.0062(10) 0.0124(10) C12 0.0319(12) 0.0362(13) 0.0492(14) -0.0056(11) 0.0032(11) 0.0142(10) C13 0.0346(14) 0.0390(14) 0.0711(19) -0.0046(13) 0.0045(13) 0.0088(11) C14 0.0471(16) 0.0404(15) 0.085(2) 0.0112(15) 0.0189(15) 0.0099(13) C15 0.0539(17) 0.0441(15) 0.0604(17) 0.0159(13) 0.0187(14) 0.0169(13) C16 0.0441(14) 0.0376(13) 0.0446(14) 0.0047(11) 0.0072(11) 0.0180(11) C17 0.0440(15) 0.0445(15) 0.0499(15) -0.0123(12) -0.0077(12) 0.0129(12) C18 0.068(2) 0.059(2) 0.133(4) 0.032(2) 0.023(2) -0.0029(18) C19 0.0569(17) 0.0528(16) 0.0425(15) 0.0128(12) 0.0002(13) 0.0186(14) C21 0.0320(12) 0.0400(13) 0.0347(12) 0.0052(10) 0.0029(10) 0.0147(10) C22 0.0388(13) 0.0404(13) 0.0400(13) 0.0034(10) 0.0092(10) 0.0170(11) C23 0.0481(15) 0.0496(15) 0.0443(14) 0.0084(12) 0.0126(12) 0.0280(13) C24 0.0383(14) 0.0653(17) 0.0398(13) 0.0157(12) 0.0121(11) 0.0267(13) C25 0.0320(13) 0.0537(16) 0.0398(13) 0.0084(11) 0.0024(10) 0.0121(11) C26 0.0327(12) 0.0424(13) 0.0366(12) 0.0063(10) 0.0021(10) 0.0134(11) C27 0.0498(16) 0.0427(15) 0.0690(19) -0.0085(13) 0.0082(14) 0.0206(13) C28 0.0465(16) 0.088(2) 0.0627(18) 0.0187(16) 0.0097(14) 0.0402(16) C29 0.0392(14) 0.0416(14) 0.0558(16) 0.0053(12) -0.0082(12) 0.0096(11) C31 0.0306(12) 0.0404(13) 0.0350(12) 0.0016(10) 0.0020(10) 0.0148(10) C32 0.0365(13) 0.0429(14) 0.0366(12) -0.0003(10) 0.0037(10) 0.0183(11) F32 0.0434(8) 0.0384(8) 0.0610(9) 0.0001(7) -0.0011(7) 0.0133(6) C33 0.0299(13) 0.0570(16) 0.0389(13) -0.0053(12) 0.0011(10) 0.0133(12) F33 0.0360(8) 0.0681(11) 0.0629(10) -0.0055(8) -0.0062(7) 0.0065(7) C34 0.0347(13) 0.0720(19) 0.0425(14) 0.0035(13) -0.0006(11) 0.0291(14) F34 0.0430(9) 0.1025(14) 0.0766(12) 0.0098(10) -0.0084(8) 0.0402(9) C35 0.0512(16) 0.0549(16) 0.0438(14) 0.0056(12) 0.0021(12) 0.0341(14) F35 0.0759(12) 0.0676(11) 0.0749(11) 0.0125(9) -0.0044(9) 0.0493(10) C36 0.0398(13) 0.0423(14) 0.0417(13) 0.0020(11) 0.0002(11) 0.0181(11) F36 0.0571(9) 0.0378(8) 0.0727(11) 0.0087(7) -0.0126(8) 0.0154(7) C41 0.0381(13) 0.0367(13) 0.0399(13) 0.0053(10) -0.0040(10) 0.0140(11) C42 0.0446(15) 0.0431(14) 0.0446(14) -0.0004(11) -0.0038(11) 0.0181(12) F42 0.0441(9) 0.0632(10) 0.0589(10) -0.0115(8) 0.0082(7) 0.0165(8) C43 0.0612(18) 0.0494(16) 0.0440(15) -0.0030(12) -0.0043(13) 0.0286(14) F43 0.0838(12) 0.0702(11) 0.0545(10) -0.0145(8) 0.0030(9) 0.0403(10) C44 0.070(2) 0.0369(14) 0.0472(16) -0.0046(12) -0.0154(14) 0.0204(14) F44 0.0956(14) 0.0473(10) 0.0663(11) -0.0164(8) -0.0218(10) 0.0216(9) C45 0.0507(16) 0.0339(14) 0.0557(17) 0.0069(12) -0.0145(14) 0.0041(12) F45 0.0634(11) 0.0468(9) 0.0825(13) 0.0050(9) -0.0106(9) -0.0055(8) C46 0.0443(15) 0.0409(14) 0.0508(15) 0.0076(12) 0.0007(12) 0.0148(12) F46 0.0470(9) 0.0514(9) 0.0714(11) 0.0030(8) 0.0111(8) 0.0036(7) _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 P1 C11 1.820(2) . ? P1 C21 1.830(2) . ? P1 C1 1.862(2) . ? P1 S1 2.3622(8) . ? B1 O1 1.568(3) . ? B1 C2 1.637(4) . ? B1 C41 1.652(4) . ? B1 C31 1.655(3) . ? O1 S1 1.5467(16) . ? S1 O2B 1.316(6) . ? S1 O2A 1.407(2) . ? C1 C6 1.546(3) . ? C1 C2 1.559(3) . ? C1 H1 0.9900 . ? C6 C5 1.524(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C5 C4 1.514(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C4 C3 1.521(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C3 C2 1.546(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C2 H2 0.9900 . ? C11 C12 1.409(3) . ? C11 C16 1.420(3) . ? C12 C13 1.395(4) . ? C12 C17 1.510(4) . ? C13 C14 1.378(4) . ? C13 H13 0.9400 . ? C14 C15 1.376(4) . ? C14 C18 1.518(4) . ? C15 C16 1.393(4) . ? C15 H15 0.9400 . ? C16 C19 1.507(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C21 C26 1.409(3) . ? C21 C22 1.415(3) . ? C22 C23 1.392(3) . ? C22 C27 1.511(4) . ? C23 C24 1.382(4) . ? C23 H23 0.9400 . ? C24 C25 1.380(4) . ? C24 C28 1.514(3) . ? C25 C26 1.396(3) . ? C25 H25 0.9400 . ? C26 C29 1.502(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C31 C32 1.381(3) . ? C31 C36 1.387(3) . ? C32 F32 1.356(3) . ? C32 C33 1.380(3) . ? C33 F33 1.348(3) . ? C33 C34 1.369(4) . ? C34 F34 1.344(3) . ? C34 C35 1.365(4) . ? C35 F35 1.349(3) . ? C35 C36 1.376(3) . ? C36 F36 1.356(3) . ? C41 C46 1.381(4) . ? C41 C42 1.391(4) . ? C42 F42 1.352(3) . ? C42 C43 1.378(4) . ? C43 F43 1.349(3) . ? C43 C44 1.361(4) . ? C44 F44 1.350(3) . ? C44 C45 1.356(4) . ? C45 F45 1.346(3) . ? C45 C46 1.391(4) . ? C46 F46 1.357(3) . ? 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 C11 P1 C21 108.63(11) . . ? C11 P1 C1 117.31(11) . . ? C21 P1 C1 113.01(10) . . ? C11 P1 S1 92.09(8) . . ? C21 P1 S1 121.90(8) . . ? C1 P1 S1 102.80(7) . . ? O1 B1 C2 108.79(18) . . ? O1 B1 C41 104.01(19) . . ? C2 B1 C41 117.3(2) . . ? O1 B1 C31 103.17(18) . . ? C2 B1 C31 113.5(2) . . ? C41 B1 C31 108.77(19) . . ? S1 O1 B1 122.51(14) . . ? O2B S1 O2A 106.4(3) . . ? O2B S1 O1 114.3(3) . . ? O2A S1 O1 116.45(12) . . ? O2B S1 P1 114.3(3) . . ? O2A S1 P1 114.82(11) . . ? O1 S1 P1 90.30(7) . . ? C6 C1 C2 112.20(19) . . ? C6 C1 P1 107.32(15) . . ? C2 C1 P1 113.86(15) . . ? C6 C1 H1 107.7 . . ? C2 C1 H1 107.7 . . ? P1 C1 H1 107.7 . . ? C5 C6 C1 111.8(2) . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C1 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C4 C5 C6 110.5(2) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C4 C3 110.3(2) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C3 C2 114.7(2) . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C2 C1 108.4(2) . . ? C3 C2 B1 109.39(19) . . ? C1 C2 B1 115.95(19) . . ? C3 C2 H2 107.6 . . ? C1 C2 H2 107.6 . . ? B1 C2 H2 107.6 . . ? C12 C11 C16 119.8(2) . . ? C12 C11 P1 125.71(19) . . ? C16 C11 P1 114.50(17) . . ? C13 C12 C11 118.2(2) . . ? C13 C12 C17 116.5(2) . . ? C11 C12 C17 125.2(2) . . ? C14 C13 C12 122.8(3) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C15 C14 C13 118.2(3) . . ? C15 C14 C18 120.8(3) . . ? C13 C14 C18 120.9(3) . . ? C14 C15 C16 122.4(3) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C15 C16 C11 118.4(2) . . ? C15 C16 C19 116.7(2) . . ? C11 C16 C19 124.7(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 119.7(2) . . ? C26 C21 P1 119.07(18) . . ? C22 C21 P1 120.96(18) . . ? C23 C22 C21 117.8(2) . . ? C23 C22 C27 116.5(2) . . ? C21 C22 C27 125.7(2) . . ? C24 C23 C22 123.3(2) . . ? C24 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C25 C24 C23 117.6(2) . . ? C25 C24 C28 121.6(3) . . ? C23 C24 C28 120.8(3) . . ? C24 C25 C26 122.1(2) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 118.9(2) . . ? C25 C26 C29 117.7(2) . . ? C21 C26 C29 123.3(2) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 113.1(2) . . ? C32 C31 B1 124.1(2) . . ? C36 C31 B1 122.8(2) . . ? F32 C32 C33 115.2(2) . . ? F32 C32 C31 120.3(2) . . ? C33 C32 C31 124.5(2) . . ? F33 C33 C34 119.9(2) . . ? F33 C33 C32 120.7(2) . . ? C34 C33 C32 119.4(2) . . ? F34 C34 C35 120.6(3) . . ? F34 C34 C33 120.4(3) . . ? C35 C34 C33 119.0(2) . . ? F35 C35 C34 119.6(2) . . ? F35 C35 C36 120.6(2) . . ? C34 C35 C36 119.7(2) . . ? F36 C36 C35 115.0(2) . . ? F36 C36 C31 120.7(2) . . ? C35 C36 C31 124.3(2) . . ? C46 C41 C42 113.1(2) . . ? C46 C41 B1 127.9(2) . . ? C42 C41 B1 118.9(2) . . ? F42 C42 C43 115.4(2) . . ? F42 C42 C41 119.9(2) . . ? C43 C42 C41 124.7(3) . . ? F43 C43 C44 120.4(2) . . ? F43 C43 C42 120.7(3) . . ? C44 C43 C42 119.0(3) . . ? F44 C44 C45 120.4(3) . . ? F44 C44 C43 119.8(3) . . ? C45 C44 C43 119.8(2) . . ? F45 C45 C44 120.6(3) . . ? F45 C45 C46 119.7(3) . . ? C44 C45 C46 119.7(3) . . ? F46 C46 C41 121.1(2) . . ? F46 C46 C45 115.3(2) . . ? C41 C46 C45 123.7(3) . . ? 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 C2 B1 O1 S1 -62.8(2) . . . . ? C41 B1 O1 S1 62.9(2) . . . . ? C31 B1 O1 S1 176.40(14) . . . . ? B1 O1 S1 O2B -163.2(4) . . . . ? B1 O1 S1 O2A -38.3(2) . . . . ? B1 O1 S1 P1 79.80(16) . . . . ? C11 P1 S1 O2B -24.9(3) . . . . ? C21 P1 S1 O2B 88.6(3) . . . . ? C1 P1 S1 O2B -143.5(3) . . . . ? C11 P1 S1 O2A -148.37(14) . . . . ? C21 P1 S1 O2A -34.84(15) . . . . ? C1 P1 S1 O2A 93.01(14) . . . . ? C11 P1 S1 O1 92.09(10) . . . . ? C21 P1 S1 O1 -154.39(11) . . . . ? C1 P1 S1 O1 -26.54(10) . . . . ? C11 P1 C1 C6 104.72(18) . . . . ? C21 P1 C1 C6 -22.9(2) . . . . ? S1 P1 C1 C6 -156.11(15) . . . . ? C11 P1 C1 C2 -130.47(16) . . . . ? C21 P1 C1 C2 101.95(17) . . . . ? S1 P1 C1 C2 -31.31(17) . . . . ? C2 C1 C6 C5 55.4(3) . . . . ? P1 C1 C6 C5 -178.83(19) . . . . ? C1 C6 C5 C4 -57.5(3) . . . . ? C6 C5 C4 C3 57.1(3) . . . . ? C5 C4 C3 C2 -56.8(3) . . . . ? C4 C3 C2 C1 52.9(3) . . . . ? C4 C3 C2 B1 -179.8(2) . . . . ? C6 C1 C2 C3 -51.0(2) . . . . ? P1 C1 C2 C3 -173.19(15) . . . . ? C6 C1 C2 B1 -174.50(19) . . . . ? P1 C1 C2 B1 63.3(2) . . . . ? O1 B1 C2 C3 -149.01(19) . . . . ? C41 B1 C2 C3 93.4(2) . . . . ? C31 B1 C2 C3 -34.8(3) . . . . ? O1 B1 C2 C1 -26.0(3) . . . . ? C41 B1 C2 C1 -143.6(2) . . . . ? C31 B1 C2 C1 88.2(2) . . . . ? C21 P1 C11 C12 117.5(2) . . . . ? C1 P1 C11 C12 -12.2(2) . . . . ? S1 P1 C11 C12 -117.7(2) . . . . ? C21 P1 C11 C16 -64.7(2) . . . . ? C1 P1 C11 C16 165.66(16) . . . . ? S1 P1 C11 C16 60.10(17) . . . . ? C16 C11 C12 C13 -4.6(3) . . . . ? P1 C11 C12 C13 173.11(18) . . . . ? C16 C11 C12 C17 170.7(2) . . . . ? P1 C11 C12 C17 -11.6(3) . . . . ? C11 C12 C13 C14 1.4(4) . . . . ? C17 C12 C13 C14 -174.3(3) . . . . ? C12 C13 C14 C15 1.9(4) . . . . ? C12 C13 C14 C18 179.9(3) . . . . ? C13 C14 C15 C16 -2.1(4) . . . . ? C18 C14 C15 C16 179.9(3) . . . . ? C14 C15 C16 C11 -1.0(4) . . . . ? C14 C15 C16 C19 174.1(3) . . . . ? C12 C11 C16 C15 4.4(3) . . . . ? P1 C11 C16 C15 -173.53(19) . . . . ? C12 C11 C16 C19 -170.3(2) . . . . ? P1 C11 C16 C19 11.8(3) . . . . ? C11 P1 C21 C26 146.70(18) . . . . ? C1 P1 C21 C26 -81.3(2) . . . . ? S1 P1 C21 C26 41.9(2) . . . . ? C11 P1 C21 C22 -27.2(2) . . . . ? C1 P1 C21 C22 104.8(2) . . . . ? S1 P1 C21 C22 -131.94(17) . . . . ? C26 C21 C22 C23 -6.4(3) . . . . ? P1 C21 C22 C23 167.38(18) . . . . ? C26 C21 C22 C27 172.3(2) . . . . ? P1 C21 C22 C27 -13.9(3) . . . . ? C21 C22 C23 C24 -0.5(4) . . . . ? C27 C22 C23 C24 -179.3(2) . . . . ? C22 C23 C24 C25 6.2(4) . . . . ? C22 C23 C24 C28 -173.7(2) . . . . ? C23 C24 C25 C26 -5.1(4) . . . . ? C28 C24 C25 C26 174.7(2) . . . . ? C24 C25 C26 C21 -1.6(4) . . . . ? C24 C25 C26 C29 175.6(2) . . . . ? C22 C21 C26 C25 7.4(3) . . . . ? P1 C21 C26 C25 -166.50(18) . . . . ? C22 C21 C26 C29 -169.5(2) . . . . ? P1 C21 C26 C29 16.5(3) . . . . ? O1 B1 C31 C32 37.0(3) . . . . ? C2 B1 C31 C32 -80.5(3) . . . . ? C41 B1 C31 C32 147.0(2) . . . . ? O1 B1 C31 C36 -142.9(2) . . . . ? C2 B1 C31 C36 99.5(3) . . . . ? C41 B1 C31 C36 -32.9(3) . . . . ? C36 C31 C32 F32 -175.8(2) . . . . ? B1 C31 C32 F32 4.3(3) . . . . ? C36 C31 C32 C33 2.5(4) . . . . ? B1 C31 C32 C33 -177.4(2) . . . . ? F32 C32 C33 F33 -1.8(3) . . . . ? C31 C32 C33 F33 179.8(2) . . . . ? F32 C32 C33 C34 177.3(2) . . . . ? C31 C32 C33 C34 -1.1(4) . . . . ? F33 C33 C34 F34 0.0(4) . . . . ? C32 C33 C34 F34 -179.1(2) . . . . ? F33 C33 C34 C35 179.0(2) . . . . ? C32 C33 C34 C35 -0.2(4) . . . . ? F34 C34 C35 F35 -0.3(4) . . . . ? C33 C34 C35 F35 -179.2(2) . . . . ? F34 C34 C35 C36 178.7(2) . . . . ? C33 C34 C35 C36 -0.2(4) . . . . ? F35 C35 C36 F36 1.9(4) . . . . ? C34 C35 C36 F36 -177.1(2) . . . . ? F35 C35 C36 C31 -179.1(2) . . . . ? C34 C35 C36 C31 2.0(4) . . . . ? C32 C31 C36 F36 176.1(2) . . . . ? B1 C31 C36 F36 -4.0(4) . . . . ? C32 C31 C36 C35 -2.9(4) . . . . ? B1 C31 C36 C35 177.0(2) . . . . ? O1 B1 C41 C46 -124.2(2) . . . . ? C2 B1 C41 C46 -4.1(4) . . . . ? C31 B1 C41 C46 126.3(3) . . . . ? O1 B1 C41 C42 51.5(3) . . . . ? C2 B1 C41 C42 171.7(2) . . . . ? C31 B1 C41 C42 -57.9(3) . . . . ? C46 C41 C42 F42 -179.4(2) . . . . ? B1 C41 C42 F42 4.2(3) . . . . ? C46 C41 C42 C43 0.5(4) . . . . ? B1 C41 C42 C43 -175.9(2) . . . . ? F42 C42 C43 F43 0.3(4) . . . . ? C41 C42 C43 F43 -179.7(2) . . . . ? F42 C42 C43 C44 -179.9(2) . . . . ? C41 C42 C43 C44 0.2(4) . . . . ? F43 C43 C44 F44 0.8(4) . . . . ? C42 C43 C44 F44 -179.0(2) . . . . ? F43 C43 C44 C45 -179.8(2) . . . . ? C42 C43 C44 C45 0.4(4) . . . . ? F44 C44 C45 F45 -2.2(4) . . . . ? C43 C44 C45 F45 178.4(2) . . . . ? F44 C44 C45 C46 177.8(2) . . . . ? C43 C44 C45 C46 -1.6(4) . . . . ? C42 C41 C46 F46 178.5(2) . . . . ? B1 C41 C46 F46 -5.6(4) . . . . ? C42 C41 C46 C45 -1.8(4) . . . . ? B1 C41 C46 C45 174.2(2) . . . . ? F45 C45 C46 F46 2.2(4) . . . . ? C44 C45 C46 F46 -177.8(2) . . . . ? F45 C45 C46 C41 -177.6(2) . . . . ? C44 C45 C46 C41 2.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 66.65 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.241 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.049