data_nb060137 _publ_section_references ; Bruker (2003). SAINT. Version 6.45. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2000). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997). SHELXL97 & SHELXS97. University of Gottingen, Germany. Sheldrick, G.M. (1997b). SADABS. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; Hydrogen atoms were found in Fourier difference maps and refined using a riding model. ; _publ_requested_journal J.Amer.Chem.Soc. _publ_contact_author_name 'Andreas Decken' _publ_contact_author_address ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 6E2 Canada ; _publ_contact_author_email adecken@unb.ca _publ_contact_author_phone '(506) 453-4875' _publ_contact_author_fax '(506) 453-4981' loop_ _publ_author_name _publ_author_address 'Andreas Decken' ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 6E2 Canada ; 'Neil Burford' ;Department of Chemistry Dalhousie University Halifax, NS B4H 4J3 Canada ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Cl F3 O3 P2 S' _chemical_formula_weight 554.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P n' _symmetry_int_tables_number 7 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 10.0707(16) _cell_length_b 8.8891(15) _cell_length_c 14.166(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.192(3) _cell_angle_gamma 90.00 _cell_volume 1229.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 4133 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.06 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997b)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker AXS SMART1000/P4' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8149 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4027 _reflns_number_gt 3720 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0349P)^2^+0.0883P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(5) _refine_ls_number_reflns 4027 _refine_ls_number_parameters 396 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.030 _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 0.06259(6) 0.06685(7) 0.50619(4) 0.01929(13) Uani 1 1 d . . . P2 P 0.02229(6) -0.06494(7) 0.36668(4) 0.02269(14) Uani 1 1 d . . . Cl Cl -0.18007(6) -0.10164(7) 0.36536(4) 0.03107(14) Uani 1 1 d . . . C1 C -0.0428(2) 0.2319(3) 0.49205(15) 0.0219(5) Uani 1 1 d . . . C2 C -0.0011(3) 0.3562(3) 0.44521(17) 0.0259(5) Uani 1 1 d . . . C3 C -0.0861(3) 0.4791(3) 0.42308(18) 0.0307(6) Uani 1 1 d . . . C4 C -0.2118(3) 0.4812(3) 0.4462(2) 0.0371(6) Uani 1 1 d . . . C5 C -0.2526(3) 0.3595(4) 0.4925(2) 0.0389(7) Uani 1 1 d . . . C6 C -0.1687(3) 0.2334(3) 0.51540(19) 0.0311(6) Uani 1 1 d . . . C7 C 0.0327(2) -0.0578(3) 0.59872(16) 0.0211(5) Uani 1 1 d . . . C8 C 0.0196(3) 0.0002(3) 0.68686(17) 0.0281(5) Uani 1 1 d . . . C9 C 0.0115(3) -0.0971(3) 0.76214(18) 0.0308(6) Uani 1 1 d . . . C10 C 0.0155(3) -0.2500(3) 0.74943(19) 0.0330(6) Uani 1 1 d . . . C11 C 0.0279(3) -0.3090(3) 0.6610(2) 0.0333(6) Uani 1 1 d . . . C12 C 0.0375(3) -0.2135(3) 0.58616(17) 0.0272(5) Uani 1 1 d . . . C13 C 0.2398(2) 0.1220(3) 0.54065(16) 0.0225(5) Uani 1 1 d . . . C14 C 0.2782(3) 0.2381(3) 0.60932(17) 0.0277(5) Uani 1 1 d . . . C15 C 0.4159(3) 0.2691(3) 0.64543(19) 0.0329(6) Uani 1 1 d . . . C16 C 0.5143(3) 0.1869(3) 0.61536(18) 0.0331(6) Uani 1 1 d . . . C17 C 0.4766(3) 0.0737(3) 0.54693(18) 0.0324(6) Uani 1 1 d . . . C18 C 0.3392(3) 0.0402(3) 0.50981(17) 0.0258(5) Uani 1 1 d . . . C19 C 0.0147(2) 0.0916(3) 0.28312(15) 0.0227(5) Uani 1 1 d . . . C20 C 0.1359(3) 0.1194(3) 0.25482(17) 0.0280(5) Uani 1 1 d . . . C21 C 0.1395(3) 0.2330(3) 0.18854(19) 0.0333(6) Uani 1 1 d . . . C22 C 0.0240(3) 0.3165(3) 0.15017(17) 0.0311(6) Uani 1 1 d . . . C23 C -0.0957(3) 0.2904(3) 0.17786(17) 0.0306(6) Uani 1 1 d . . . C24 C -0.1016(3) 0.1783(3) 0.24449(17) 0.0276(5) Uani 1 1 d . . . C25 C 0.3191(3) 0.5679(3) 0.38447(19) 0.0350(6) Uani 1 1 d . . . F1 F 0.2170(2) 0.5142(3) 0.31663(13) 0.0713(7) Uani 1 1 d . . . F2 F 0.26562(17) 0.6277(2) 0.45303(11) 0.0430(4) Uani 1 1 d . . . F3 F 0.3958(2) 0.4520(2) 0.42622(15) 0.0659(6) Uani 1 1 d . . . S S 0.41925(6) 0.70405(7) 0.33495(4) 0.02823(14) Uani 1 1 d . . . O1 O 0.5204(2) 0.7554(3) 0.41880(14) 0.0499(6) Uani 1 1 d . . . O2 O 0.4729(3) 0.6203(2) 0.26658(14) 0.0503(6) Uani 1 1 d . . . O3 O 0.3173(2) 0.8139(2) 0.29382(16) 0.0471(5) Uani 1 1 d . . . H2 H 0.081(3) 0.350(3) 0.4287(18) 0.024(7) Uiso 1 1 d . . . H3 H -0.061(3) 0.562(3) 0.393(2) 0.038(8) Uiso 1 1 d . . . H4 H -0.276(3) 0.568(3) 0.427(2) 0.039(8) Uiso 1 1 d . . . H5 H -0.330(3) 0.360(4) 0.507(2) 0.046(9) Uiso 1 1 d . . . H6 H -0.195(3) 0.141(4) 0.551(2) 0.042(8) Uiso 1 1 d . . . H8 H 0.025(3) 0.100(3) 0.6991(18) 0.023(7) Uiso 1 1 d . . . H9 H 0.003(3) -0.057(3) 0.821(2) 0.044(8) Uiso 1 1 d . . . H10 H 0.006(3) -0.321(3) 0.7983(18) 0.025(6) Uiso 1 1 d . . . H11 H 0.025(4) -0.413(4) 0.650(2) 0.058(10) Uiso 1 1 d . . . H12 H 0.046(3) -0.252(3) 0.523(2) 0.034(7) Uiso 1 1 d . . . H14 H 0.208(3) 0.291(3) 0.6330(16) 0.018(6) Uiso 1 1 d . . . H15 H 0.437(3) 0.330(4) 0.690(2) 0.038(8) Uiso 1 1 d . . . H16 H 0.603(3) 0.205(3) 0.6470(19) 0.030(7) Uiso 1 1 d . . . H17 H 0.545(3) 0.015(3) 0.5288(18) 0.024(7) Uiso 1 1 d . . . H18 H 0.319(3) -0.043(3) 0.467(2) 0.038(8) Uiso 1 1 d . . . H20 H 0.211(3) 0.062(3) 0.2794(18) 0.023(7) Uiso 1 1 d . . . H21 H 0.220(3) 0.250(3) 0.1676(18) 0.027(7) Uiso 1 1 d . . . H22 H 0.031(3) 0.402(3) 0.100(2) 0.043(8) Uiso 1 1 d . . . H23 H -0.176(3) 0.348(3) 0.153(2) 0.038(8) Uiso 1 1 d . . . H24 H -0.180(3) 0.159(3) 0.2659(17) 0.021(6) Uiso 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 0.0207(3) 0.0169(3) 0.0203(3) 0.0011(2) 0.0051(2) 0.0004(2) P2 0.0255(3) 0.0203(3) 0.0217(3) -0.0005(2) 0.0046(2) 0.0011(3) Cl 0.0269(3) 0.0311(3) 0.0328(3) 0.0015(3) 0.0026(2) -0.0060(3) C1 0.0212(12) 0.0209(12) 0.0224(10) -0.0004(9) 0.0033(9) 0.0011(10) C2 0.0314(14) 0.0202(13) 0.0267(11) 0.0000(10) 0.0081(10) -0.0021(10) C3 0.0391(16) 0.0209(13) 0.0303(12) 0.0031(11) 0.0049(11) -0.0009(11) C4 0.0374(16) 0.0292(14) 0.0421(14) 0.0026(12) 0.0046(12) 0.0108(13) C5 0.0260(15) 0.0390(18) 0.0545(17) 0.0087(14) 0.0154(14) 0.0109(12) C6 0.0294(14) 0.0271(14) 0.0386(13) 0.0057(11) 0.0114(11) 0.0044(11) C7 0.0164(11) 0.0232(12) 0.0236(10) 0.0034(9) 0.0045(9) 0.0002(9) C8 0.0316(14) 0.0251(14) 0.0286(12) 0.0004(11) 0.0094(10) 0.0009(11) C9 0.0298(14) 0.0401(16) 0.0238(12) 0.0022(11) 0.0090(10) 0.0000(12) C10 0.0301(14) 0.0359(16) 0.0326(12) 0.0129(12) 0.0068(11) -0.0055(12) C11 0.0365(15) 0.0232(14) 0.0387(13) 0.0076(11) 0.0061(12) -0.0017(12) C12 0.0314(14) 0.0254(13) 0.0250(11) 0.0015(10) 0.0072(10) 0.0000(11) C13 0.0218(12) 0.0208(12) 0.0235(10) 0.0045(9) 0.0029(9) -0.0022(10) C14 0.0303(14) 0.0246(13) 0.0272(11) 0.0000(10) 0.0052(10) -0.0007(11) C15 0.0404(16) 0.0271(14) 0.0268(12) 0.0001(11) -0.0001(11) -0.0092(13) C16 0.0255(14) 0.0417(16) 0.0296(12) 0.0106(12) 0.0019(11) -0.0074(12) C17 0.0254(14) 0.0418(17) 0.0305(12) 0.0082(12) 0.0077(11) 0.0024(12) C18 0.0288(13) 0.0247(13) 0.0236(11) 0.0029(10) 0.0059(10) 0.0005(11) C19 0.0281(13) 0.0193(12) 0.0198(10) -0.0017(9) 0.0042(9) 0.0000(10) C20 0.0291(14) 0.0277(14) 0.0262(11) 0.0017(10) 0.0050(10) 0.0029(11) C21 0.0336(15) 0.0362(15) 0.0317(12) 0.0017(11) 0.0110(11) -0.0070(12) C22 0.0377(15) 0.0290(14) 0.0239(11) 0.0022(11) 0.0026(10) -0.0052(12) C23 0.0329(15) 0.0263(14) 0.0284(12) 0.0056(10) -0.0007(11) 0.0033(11) C24 0.0254(13) 0.0312(14) 0.0248(10) 0.0018(10) 0.0035(10) 0.0005(11) C25 0.0479(17) 0.0282(15) 0.0301(12) -0.0024(11) 0.0120(12) -0.0035(13) F1 0.0887(16) 0.0749(15) 0.0478(11) -0.0155(10) 0.0116(10) -0.0526(13) F2 0.0439(10) 0.0502(11) 0.0417(8) -0.0015(8) 0.0235(7) 0.0002(8) F3 0.1016(17) 0.0377(11) 0.0733(12) 0.0259(10) 0.0503(12) 0.0264(11) S 0.0319(3) 0.0245(3) 0.0300(3) 0.0007(3) 0.0108(2) 0.0047(3) O1 0.0367(12) 0.0634(15) 0.0482(11) -0.0083(11) 0.0075(9) -0.0080(11) O2 0.0823(16) 0.0355(12) 0.0443(11) 0.0002(9) 0.0372(11) 0.0103(11) O3 0.0447(12) 0.0365(12) 0.0614(12) 0.0183(10) 0.0158(10) 0.0149(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.793(2) . ? P1 C7 1.797(2) . ? P1 C13 1.799(2) . ? P1 P2 2.2471(8) . ? P2 C19 1.816(2) . ? P2 Cl 2.0595(9) . ? C1 C6 1.387(4) . ? C1 C2 1.405(3) . ? C2 C3 1.376(4) . ? C2 H2 0.92(3) . ? C3 C4 1.383(4) . ? C3 H3 0.92(3) . ? C4 C5 1.379(4) . ? C4 H4 1.00(3) . ? C5 C6 1.393(4) . ? C5 H5 0.85(3) . ? C6 H6 1.03(3) . ? C7 C8 1.387(3) . ? C7 C12 1.398(3) . ? C8 C9 1.391(4) . ? C8 H8 0.91(3) . ? C9 C10 1.374(4) . ? C9 H9 0.93(3) . ? C10 C11 1.391(4) . ? C10 H10 0.96(3) . ? C11 C12 1.380(3) . ? C11 H11 0.94(3) . ? C12 H12 0.98(3) . ? C13 C18 1.391(3) . ? C13 C14 1.406(3) . ? C14 C15 1.384(4) . ? C14 H14 0.98(3) . ? C15 C16 1.379(4) . ? C15 H15 0.82(3) . ? C16 C17 1.384(4) . ? C16 H16 0.91(3) . ? C17 C18 1.387(4) . ? C17 H17 0.95(3) . ? C18 H18 0.95(3) . ? C19 C24 1.396(4) . ? C19 C20 1.397(3) . ? C20 C21 1.386(4) . ? C20 H20 0.91(3) . ? C21 C22 1.374(4) . ? C21 H21 0.94(3) . ? C22 C23 1.376(4) . ? C22 H22 1.05(3) . ? C23 C24 1.384(4) . ? C23 H23 0.96(3) . ? C24 H24 0.93(3) . ? C25 F1 1.313(3) . ? C25 F2 1.332(3) . ? C25 F3 1.335(3) . ? C25 S 1.822(3) . ? S O2 1.429(2) . ? S O3 1.433(2) . ? S O1 1.437(2) . ? 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 C7 112.68(11) . . ? C1 P1 C13 109.13(11) . . ? C7 P1 C13 107.60(10) . . ? C1 P1 P2 110.73(7) . . ? C7 P1 P2 107.09(8) . . ? C13 P1 P2 109.52(8) . . ? C19 P2 Cl 103.41(8) . . ? C19 P2 P1 98.24(8) . . ? Cl P2 P1 93.18(3) . . ? C6 C1 C2 120.1(2) . . ? C6 C1 P1 122.15(19) . . ? C2 C1 P1 117.36(19) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2 122.6(17) . . ? C1 C2 H2 117.9(17) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 121.0(19) . . ? C4 C3 H3 118.3(19) . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 119.0(17) . . ? C3 C4 H4 121.0(17) . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 120(2) . . ? C6 C5 H5 119(2) . . ? C1 C6 C5 119.4(3) . . ? C1 C6 H6 118.1(18) . . ? C5 C6 H6 122.6(18) . . ? C8 C7 C12 119.8(2) . . ? C8 C7 P1 119.85(19) . . ? C12 C7 P1 120.03(18) . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H8 121.5(16) . . ? C9 C8 H8 118.5(16) . . ? C10 C9 C8 120.4(2) . . ? C10 C9 H9 120.7(19) . . ? C8 C9 H9 118.9(19) . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10 123.2(15) . . ? C11 C10 H10 116.6(15) . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11 119(2) . . ? C10 C11 H11 121(2) . . ? C11 C12 C7 120.0(2) . . ? C11 C12 H12 121.6(17) . . ? C7 C12 H12 118.3(17) . . ? C18 C13 C14 120.3(2) . . ? C18 C13 P1 120.96(19) . . ? C14 C13 P1 118.29(19) . . ? C15 C14 C13 118.8(2) . . ? C15 C14 H14 121.7(14) . . ? C13 C14 H14 119.3(15) . . ? C16 C15 C14 120.8(2) . . ? C16 C15 H15 121(2) . . ? C14 C15 H15 118(2) . . ? C15 C16 C17 120.5(3) . . ? C15 C16 H16 116.4(17) . . ? C17 C16 H16 122.9(17) . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17 119.7(16) . . ? C18 C17 H17 120.3(16) . . ? C17 C18 C13 119.8(2) . . ? C17 C18 H18 116.6(18) . . ? C13 C18 H18 123.5(18) . . ? C24 C19 C20 119.9(2) . . ? C24 C19 P2 125.13(19) . . ? C20 C19 P2 114.96(18) . . ? C21 C20 C19 119.5(3) . . ? C21 C20 H20 120.7(17) . . ? C19 C20 H20 119.8(17) . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 119.8(16) . . ? C20 C21 H21 120.0(16) . . ? C21 C22 C23 120.8(2) . . ? C21 C22 H22 117.9(17) . . ? C23 C22 H22 121.3(17) . . ? C22 C23 C24 120.2(2) . . ? C22 C23 H23 121.8(18) . . ? C24 C23 H23 118.0(18) . . ? C23 C24 C19 119.5(2) . . ? C23 C24 H24 122.3(16) . . ? C19 C24 H24 118.2(16) . . ? F1 C25 F2 107.1(3) . . ? F1 C25 F3 108.0(2) . . ? F2 C25 F3 106.2(2) . . ? F1 C25 S 111.56(18) . . ? F2 C25 S 112.11(18) . . ? F3 C25 S 111.6(2) . . ? O2 S O3 115.58(13) . . ? O2 S O1 114.61(14) . . ? O3 S O1 114.33(14) . . ? O2 S C25 104.60(13) . . ? O3 S C25 101.56(14) . . ? O1 S C25 103.87(13) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.309 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.046