Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Douglas W Stephan' _publ_contact_author_email DSTEPHAN@CHEM.UTORONTO.CA _publ_section_title ; Reactions of Phosphines with Electron Deficient Boranes ; loop_ _publ_author_name 'Douglas W Stephan' 'Meghan A Dureen' 'Thorsten Holtrichter-Rossmann' 'Shamola Labeodan' ; A.J.Lough ; 'Roberto Prieto' 'Gregory C Welch' # Attachment 'CIF-revised-2.txt' data_Et2PHB(C6F5)3 _database_code_depnum_ccdc_archive 'CCDC 698991' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C22 H11 B F15 P' _chemical_formula_weight 602.09 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.2030(16) _cell_length_b 16.295(3) _cell_length_c 8.4244(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.57(3) _cell_angle_gamma 90.00 _cell_volume 1116.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 6659 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3553 _reflns_number_gt 3288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0673P)^2^+0.3298P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(12) _refine_ls_number_reflns 3553 _refine_ls_number_parameters 356 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 P1 P 0.19315(9) 0.50385(5) 0.56797(9) 0.02542(19) Uani 1 1 d . . . B1 B 0.3389(4) 0.5853(2) 0.7042(4) 0.0245(7) Uani 1 1 d . . . F1 F 0.6733(3) 0.63733(14) 0.8325(3) 0.0448(6) Uani 1 1 d . . . F2 F 0.8971(2) 0.55157(16) 1.0182(2) 0.0449(6) Uani 1 1 d . . . F3 F 0.8223(3) 0.40321(15) 1.1348(3) 0.0526(6) Uani 1 1 d . . . F4 F 0.5139(3) 0.33944(15) 1.0512(3) 0.0578(7) Uani 1 1 d . . . F5 F 0.2878(2) 0.42364(13) 0.8616(2) 0.0373(5) Uani 1 1 d . . . F6 F 0.5586(2) 0.50828(13) 0.5110(2) 0.0342(4) Uani 1 1 d . . . F7 F 0.7351(3) 0.57764(15) 0.3044(2) 0.0435(5) Uani 1 1 d . . . F8 F 0.7080(3) 0.74246(16) 0.2431(3) 0.0538(6) Uani 1 1 d . . . F9 F 0.5028(3) 0.83439(14) 0.3995(3) 0.0487(6) Uani 1 1 d . . . F10 F 0.3362(2) 0.76855(12) 0.6140(3) 0.0380(5) Uani 1 1 d . . . F11 F 0.3745(2) 0.63600(14) 1.0547(2) 0.0386(5) Uani 1 1 d . . . F12 F 0.1730(3) 0.73383(15) 1.1842(2) 0.0477(6) Uani 1 1 d . . . F13 F -0.0954(3) 0.80028(14) 1.0062(3) 0.0433(5) Uani 1 1 d . . . F14 F -0.1569(2) 0.76442(14) 0.6865(2) 0.0377(5) Uani 1 1 d . . . F15 F 0.0436(2) 0.66586(12) 0.5510(2) 0.0333(5) Uani 1 1 d . . . C1 C 0.4714(4) 0.5326(2) 0.8279(4) 0.0254(7) Uani 1 1 d . . . C2 C 0.6293(4) 0.5621(2) 0.8767(4) 0.0302(7) Uani 1 1 d . . . C3 C 0.7466(4) 0.5192(2) 0.9755(4) 0.0327(8) Uani 1 1 d . . . C4 C 0.7092(5) 0.4438(2) 1.0348(4) 0.0385(9) Uani 1 1 d . . . C5 C 0.5536(4) 0.4120(2) 0.9938(4) 0.0342(8) Uani 1 1 d . . . C6 C 0.4394(4) 0.4578(2) 0.8919(4) 0.0306(7) Uani 1 1 d . . . C7 C 0.4358(4) 0.6338(2) 0.5733(4) 0.0249(7) Uani 1 1 d . . . C8 C 0.5422(4) 0.5901(2) 0.4890(4) 0.0278(7) Uani 1 1 d . . . C9 C 0.6339(4) 0.6248(2) 0.3804(4) 0.0309(8) Uani 1 1 d . . . C10 C 0.6219(4) 0.7072(3) 0.3493(4) 0.0354(8) Uani 1 1 d . . . C11 C 0.5174(4) 0.7537(2) 0.4281(4) 0.0334(8) Uani 1 1 d . . . C12 C 0.4294(4) 0.7167(2) 0.5390(4) 0.0294(7) Uani 1 1 d . . . C13 C 0.2177(4) 0.6435(2) 0.7945(4) 0.0250(7) Uani 1 1 d . . . C14 C 0.2425(4) 0.6645(2) 0.9561(4) 0.0293(7) Uani 1 1 d . . . C15 C 0.1388(5) 0.7159(2) 1.0283(4) 0.0316(8) Uani 1 1 d . . . C16 C 0.0032(4) 0.7495(2) 0.9386(4) 0.0320(8) Uani 1 1 d . . . C17 C -0.0265(4) 0.7310(2) 0.7776(4) 0.0280(7) Uani 1 1 d . . . C18 C 0.0785(4) 0.6799(2) 0.7114(4) 0.0272(7) Uani 1 1 d . . . C19 C -0.0017(4) 0.4802(2) 0.6396(4) 0.0327(8) Uani 1 1 d . . . H19A H 0.0145 0.4796 0.7558 0.039 Uiso 1 1 calc R . . H19B H -0.0805 0.5231 0.6052 0.039 Uiso 1 1 calc R . . C20 C -0.0721(5) 0.3977(3) 0.5786(5) 0.0476(10) Uani 1 1 d . . . H20A H -0.1745 0.3882 0.6192 0.071 Uiso 1 1 calc R . . H20B H 0.0041 0.3548 0.6146 0.071 Uiso 1 1 calc R . . H20C H -0.0903 0.3983 0.4637 0.071 Uiso 1 1 calc R . . C21 C 0.1479(4) 0.5291(2) 0.3548(4) 0.0319(8) Uani 1 1 d . . . H21A H 0.0299 0.5266 0.3238 0.038 Uiso 1 1 calc R . . H21B H 0.1826 0.5850 0.3389 0.038 Uiso 1 1 calc R . . C22 C 0.2302(5) 0.4731(3) 0.2455(4) 0.0398(9) Uani 1 1 d . . . H22A H 0.2010 0.4900 0.1363 0.060 Uiso 1 1 calc R . . H22B H 0.1943 0.4176 0.2578 0.060 Uiso 1 1 calc R . . H22C H 0.3474 0.4761 0.2732 0.060 Uiso 1 1 calc R . . H1 H 0.262(4) 0.437(2) 0.561(4) 0.017(8) 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 0.0211(4) 0.0278(4) 0.0272(4) -0.0006(3) 0.0025(3) 0.0006(3) B1 0.0208(17) 0.024(2) 0.0285(18) -0.0003(15) 0.0038(13) 0.0011(14) F1 0.0343(11) 0.0492(14) 0.0470(12) 0.0181(10) -0.0085(9) -0.0169(10) F2 0.0217(10) 0.0713(17) 0.0394(11) -0.0004(11) -0.0050(8) -0.0004(10) F3 0.0526(14) 0.0500(15) 0.0484(12) 0.0022(11) -0.0185(10) 0.0210(11) F4 0.0796(17) 0.0306(13) 0.0568(15) 0.0155(11) -0.0151(12) -0.0045(12) F5 0.0363(11) 0.0395(12) 0.0349(11) 0.0045(9) 0.0005(8) -0.0118(9) F6 0.0326(10) 0.0308(11) 0.0404(10) -0.0008(9) 0.0088(8) 0.0039(9) F7 0.0335(11) 0.0598(15) 0.0401(11) -0.0057(10) 0.0162(9) 0.0005(10) F8 0.0490(14) 0.0638(16) 0.0530(13) 0.0163(12) 0.0229(11) -0.0116(12) F9 0.0444(13) 0.0348(13) 0.0688(16) 0.0173(11) 0.0144(11) -0.0024(10) F10 0.0349(11) 0.0278(11) 0.0535(12) 0.0038(9) 0.0145(9) 0.0031(9) F11 0.0366(11) 0.0472(13) 0.0296(10) -0.0047(9) -0.0048(8) 0.0112(9) F12 0.0607(15) 0.0511(14) 0.0316(11) -0.0102(10) 0.0072(9) 0.0124(11) F13 0.0443(12) 0.0421(13) 0.0473(12) -0.0036(10) 0.0199(10) 0.0142(10) F14 0.0260(10) 0.0404(13) 0.0460(11) -0.0003(9) 0.0018(8) 0.0097(9) F15 0.0308(10) 0.0364(12) 0.0307(10) -0.0033(8) -0.0031(7) 0.0081(9) C1 0.0203(15) 0.0304(18) 0.0264(16) -0.0003(13) 0.0064(12) 0.0032(12) C2 0.0237(17) 0.036(2) 0.0313(17) 0.0015(15) 0.0052(13) 0.0003(14) C3 0.0225(16) 0.046(2) 0.0286(17) -0.0038(15) -0.0001(13) 0.0058(14) C4 0.039(2) 0.042(2) 0.0320(17) -0.0043(16) -0.0053(15) 0.0176(16) C5 0.043(2) 0.025(2) 0.0331(18) 0.0042(15) -0.0026(15) 0.0039(15) C6 0.0269(17) 0.036(2) 0.0282(16) -0.0034(15) 0.0025(13) -0.0004(15) C7 0.0177(15) 0.0308(19) 0.0251(15) 0.0029(13) -0.0012(11) -0.0026(13) C8 0.0227(16) 0.0337(19) 0.0261(16) -0.0008(14) 0.0004(12) -0.0027(14) C9 0.0208(16) 0.048(2) 0.0244(16) -0.0017(15) 0.0052(12) -0.0012(14) C10 0.0267(17) 0.046(2) 0.0335(18) 0.0087(16) 0.0049(14) -0.0114(15) C11 0.0281(17) 0.032(2) 0.0389(18) 0.0102(15) -0.0014(14) -0.0049(14) C12 0.0204(16) 0.034(2) 0.0327(17) 0.0030(14) 0.0008(12) 0.0006(13) C13 0.0222(15) 0.0236(17) 0.0293(17) 0.0017(13) 0.0033(12) -0.0033(12) C14 0.0281(17) 0.0320(19) 0.0274(16) -0.0002(14) 0.0025(13) -0.0004(14) C15 0.0385(19) 0.030(2) 0.0278(17) -0.0029(14) 0.0088(14) 0.0007(15) C16 0.0300(17) 0.0293(19) 0.0400(18) 0.0013(15) 0.0168(14) 0.0008(14) C17 0.0205(15) 0.0269(18) 0.0363(17) 0.0011(14) 0.0023(12) 0.0008(13) C18 0.0238(16) 0.0290(18) 0.0289(16) -0.0020(14) 0.0040(12) -0.0029(13) C19 0.0216(16) 0.039(2) 0.0383(18) -0.0015(15) 0.0054(13) -0.0060(14) C20 0.038(2) 0.042(2) 0.064(3) -0.004(2) 0.0074(18) -0.0152(18) C21 0.0294(17) 0.037(2) 0.0281(17) -0.0004(14) 0.0012(13) 0.0016(14) C22 0.040(2) 0.048(2) 0.0317(19) -0.0021(16) 0.0025(15) 0.0055(17) _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 C19 1.823(3) . ? P1 C21 1.832(3) . ? P1 B1 2.036(4) . ? P1 H1 1.23(3) . ? B1 C13 1.633(5) . ? B1 C7 1.644(5) . ? B1 C1 1.645(5) . ? F1 C2 1.345(4) . ? F2 C3 1.348(4) . ? F3 C4 1.343(4) . ? F4 C5 1.334(5) . ? F5 C6 1.355(4) . ? F6 C8 1.350(4) . ? F7 C9 1.353(4) . ? F8 C10 1.340(4) . ? F9 C11 1.339(5) . ? F10 C12 1.350(4) . ? F11 C14 1.357(4) . ? F12 C15 1.338(4) . ? F13 C16 1.336(4) . ? F14 C17 1.346(4) . ? F15 C18 1.363(4) . ? C1 C6 1.373(5) . ? C1 C2 1.391(5) . ? C2 C3 1.377(5) . ? C3 C4 1.376(6) . ? C4 C5 1.378(5) . ? C5 C6 1.400(5) . ? C7 C12 1.381(5) . ? C7 C8 1.391(5) . ? C8 C9 1.380(5) . ? C9 C10 1.368(5) . ? C10 C11 1.379(6) . ? C11 C12 1.392(5) . ? C13 C18 1.390(5) . ? C13 C14 1.393(4) . ? C14 C15 1.390(5) . ? C15 C16 1.373(5) . ? C16 C17 1.379(5) . ? C17 C18 1.370(5) . ? C19 C20 1.524(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.516(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 P1 C21 107.40(17) . . ? C19 P1 B1 115.27(15) . . ? C21 P1 B1 115.73(16) . . ? C19 P1 H1 105.0(14) . . ? C21 P1 H1 100.6(14) . . ? B1 P1 H1 111.3(15) . . ? C13 B1 C7 114.3(3) . . ? C13 B1 C1 113.6(3) . . ? C7 B1 C1 109.8(2) . . ? C13 B1 P1 107.0(2) . . ? C7 B1 P1 103.6(2) . . ? C1 B1 P1 107.9(2) . . ? C6 C1 C2 114.1(3) . . ? C6 C1 B1 124.6(3) . . ? C2 C1 B1 121.3(3) . . ? F1 C2 C3 116.0(3) . . ? F1 C2 C1 120.4(3) . . ? C3 C2 C1 123.6(3) . . ? F2 C3 C4 119.6(3) . . ? F2 C3 C2 120.4(3) . . ? C4 C3 C2 120.1(3) . . ? F3 C4 C3 119.9(3) . . ? F3 C4 C5 120.8(4) . . ? C3 C4 C5 119.3(3) . . ? F4 C5 C4 120.4(3) . . ? F4 C5 C6 121.2(3) . . ? C4 C5 C6 118.4(3) . . ? F5 C6 C1 120.6(3) . . ? F5 C6 C5 114.9(3) . . ? C1 C6 C5 124.6(3) . . ? C12 C7 C8 113.8(3) . . ? C12 C7 B1 127.0(3) . . ? C8 C7 B1 119.2(3) . . ? F6 C8 C9 116.3(3) . . ? F6 C8 C7 119.6(3) . . ? C9 C8 C7 124.1(3) . . ? F7 C9 C10 120.0(3) . . ? F7 C9 C8 120.1(3) . . ? C10 C9 C8 119.9(3) . . ? F8 C10 C9 121.2(3) . . ? F8 C10 C11 120.1(3) . . ? C9 C10 C11 118.7(3) . . ? F9 C11 C10 120.0(3) . . ? F9 C11 C12 120.3(3) . . ? C10 C11 C12 119.7(3) . . ? F10 C12 C7 121.5(3) . . ? F10 C12 C11 114.7(3) . . ? C7 C12 C11 123.7(3) . . ? C18 C13 C14 113.1(3) . . ? C18 C13 B1 121.5(3) . . ? C14 C13 B1 125.4(3) . . ? F11 C14 C15 115.1(3) . . ? F11 C14 C13 121.1(3) . . ? C15 C14 C13 123.8(3) . . ? F12 C15 C16 120.2(3) . . ? F12 C15 C14 120.0(3) . . ? C16 C15 C14 119.8(3) . . ? F13 C16 C15 120.3(3) . . ? F13 C16 C17 121.0(3) . . ? C15 C16 C17 118.7(3) . . ? F14 C17 C18 120.6(3) . . ? F14 C17 C16 119.8(3) . . ? C18 C17 C16 119.6(3) . . ? F15 C18 C17 116.4(3) . . ? F15 C18 C13 118.6(3) . . ? C17 C18 C13 125.0(3) . . ? C20 C19 P1 112.6(3) . . ? C20 C19 H19A 109.1 . . ? P1 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? P1 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P1 114.3(2) . . ? C22 C21 H21A 108.7 . . ? P1 C21 H21A 108.7 . . ? C22 C21 H21B 108.7 . . ? P1 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 C19 P1 B1 C13 -27.0(3) . . . . ? C21 P1 B1 C13 99.5(2) . . . . ? C19 P1 B1 C7 -148.1(2) . . . . ? C21 P1 B1 C7 -21.6(3) . . . . ? C19 P1 B1 C1 95.6(2) . . . . ? C21 P1 B1 C1 -137.9(2) . . . . ? C13 B1 C1 C6 85.9(4) . . . . ? C7 B1 C1 C6 -144.8(3) . . . . ? P1 B1 C1 C6 -32.5(4) . . . . ? C13 B1 C1 C2 -94.0(4) . . . . ? C7 B1 C1 C2 35.3(4) . . . . ? P1 B1 C1 C2 147.5(3) . . . . ? C6 C1 C2 F1 -175.1(3) . . . . ? B1 C1 C2 F1 4.8(5) . . . . ? C6 C1 C2 C3 2.4(5) . . . . ? B1 C1 C2 C3 -177.7(3) . . . . ? F1 C2 C3 F2 -2.3(5) . . . . ? C1 C2 C3 F2 -179.9(3) . . . . ? F1 C2 C3 C4 176.0(3) . . . . ? C1 C2 C3 C4 -1.6(5) . . . . ? F2 C3 C4 F3 0.2(5) . . . . ? C2 C3 C4 F3 -178.1(3) . . . . ? F2 C3 C4 C5 178.4(3) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? F3 C4 C5 F4 -1.0(5) . . . . ? C3 C4 C5 F4 -179.2(3) . . . . ? F3 C4 C5 C6 178.6(3) . . . . ? C3 C4 C5 C6 0.4(5) . . . . ? C2 C1 C6 F5 176.5(3) . . . . ? B1 C1 C6 F5 -3.4(5) . . . . ? C2 C1 C6 C5 -1.9(5) . . . . ? B1 C1 C6 C5 178.2(3) . . . . ? F4 C5 C6 F5 1.7(5) . . . . ? C4 C5 C6 F5 -177.9(3) . . . . ? F4 C5 C6 C1 -179.8(3) . . . . ? C4 C5 C6 C1 0.6(5) . . . . ? C13 B1 C7 C12 2.8(4) . . . . ? C1 B1 C7 C12 -126.1(3) . . . . ? P1 B1 C7 C12 118.9(3) . . . . ? C13 B1 C7 C8 -179.9(3) . . . . ? C1 B1 C7 C8 51.2(4) . . . . ? P1 B1 C7 C8 -63.8(3) . . . . ? C12 C7 C8 F6 -179.5(3) . . . . ? B1 C7 C8 F6 2.8(4) . . . . ? C12 C7 C8 C9 -0.1(4) . . . . ? B1 C7 C8 C9 -177.8(3) . . . . ? F6 C8 C9 F7 -1.0(4) . . . . ? C7 C8 C9 F7 179.6(3) . . . . ? F6 C8 C9 C10 178.8(3) . . . . ? C7 C8 C9 C10 -0.6(5) . . . . ? F7 C9 C10 F8 0.6(5) . . . . ? C8 C9 C10 F8 -179.3(3) . . . . ? F7 C9 C10 C11 179.8(3) . . . . ? C8 C9 C10 C11 0.0(5) . . . . ? F8 C10 C11 F9 -0.4(5) . . . . ? C9 C10 C11 F9 -179.7(3) . . . . ? F8 C10 C11 C12 -179.5(3) . . . . ? C9 C10 C11 C12 1.2(5) . . . . ? C8 C7 C12 F10 -177.9(3) . . . . ? B1 C7 C12 F10 -0.5(5) . . . . ? C8 C7 C12 C11 1.4(5) . . . . ? B1 C7 C12 C11 178.9(3) . . . . ? F9 C11 C12 F10 -1.7(5) . . . . ? C10 C11 C12 F10 177.4(3) . . . . ? F9 C11 C12 C7 178.9(3) . . . . ? C10 C11 C12 C7 -2.0(5) . . . . ? C7 B1 C13 C18 65.7(4) . . . . ? C1 B1 C13 C18 -167.3(3) . . . . ? P1 B1 C13 C18 -48.4(4) . . . . ? C7 B1 C13 C14 -112.0(3) . . . . ? C1 B1 C13 C14 15.0(5) . . . . ? P1 B1 C13 C14 133.9(3) . . . . ? C18 C13 C14 F11 -178.5(3) . . . . ? B1 C13 C14 F11 -0.7(5) . . . . ? C18 C13 C14 C15 0.4(5) . . . . ? B1 C13 C14 C15 178.3(3) . . . . ? F11 C14 C15 F12 -0.1(5) . . . . ? C13 C14 C15 F12 -179.1(3) . . . . ? F11 C14 C15 C16 178.7(3) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? F12 C15 C16 F13 0.0(5) . . . . ? C14 C15 C16 F13 -178.8(3) . . . . ? F12 C15 C16 C17 178.8(3) . . . . ? C14 C15 C16 C17 0.0(5) . . . . ? F13 C16 C17 F14 0.0(5) . . . . ? C15 C16 C17 F14 -178.8(3) . . . . ? F13 C16 C17 C18 178.9(3) . . . . ? C15 C16 C17 C18 0.2(5) . . . . ? F14 C17 C18 F15 0.4(5) . . . . ? C16 C17 C18 F15 -178.5(3) . . . . ? F14 C17 C18 C13 178.9(3) . . . . ? C16 C17 C18 C13 0.0(5) . . . . ? C14 C13 C18 F15 178.2(3) . . . . ? B1 C13 C18 F15 0.3(5) . . . . ? C14 C13 C18 C17 -0.3(5) . . . . ? B1 C13 C18 C17 -178.2(3) . . . . ? C21 P1 C19 C20 72.4(3) . . . . ? B1 P1 C19 C20 -157.0(3) . . . . ? C19 P1 C21 C22 -119.7(3) . . . . ? B1 P1 C21 C22 110.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.241 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.052 #===end data_(tBu2PH)B(C6F5)3.0.5(C7H8) _database_code_depnum_ccdc_archive 'CCDC 698992' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C29.5 H23 B F15 P' _chemical_formula_weight 704.26 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' 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' _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 9.3182(19) _cell_length_b 10.374(2) _cell_length_c 15.635(3) _cell_angle_alpha 88.96(3) _cell_angle_beta 85.90(3) _cell_angle_gamma 78.03(3) _cell_volume 1474.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 1.046 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART system' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 13213 _diffrn_reflns_av_R_equivalents 0.1255 _diffrn_reflns_av_sigmaI/netI 0.1568 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 24.69 _reflns_number_total 4977 _reflns_number_gt 2218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. Refinement employed data to 24.69deg to to small crystal. The toluene solvate was refined with contrainted C-C distances. Due to the disorder H atoms for this fragment were not included in the model. ; _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^)+(0.1108P)^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_number_reflns 4977 _refine_ls_number_parameters 412 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1857 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.988 _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 0.09817(19) 0.55363(16) 0.29732(11) 0.0490(5) Uani 1 1 d . . . B1 B 0.1750(7) 0.7270(7) 0.2703(4) 0.0392(17) Uani 1 1 d . . . F1 F 0.0259(3) 0.7749(3) 0.4386(2) 0.0509(9) Uani 1 1 d . . . F2 F -0.1627(4) 0.9894(4) 0.4946(2) 0.0621(11) Uani 1 1 d . . . F3 F -0.2693(4) 1.1851(4) 0.3828(3) 0.0711(12) Uani 1 1 d . . . F4 F -0.1636(4) 1.1679(4) 0.2163(3) 0.0643(11) Uani 1 1 d . . . F5 F 0.0409(4) 0.9664(3) 0.1608(2) 0.0540(10) Uani 1 1 d . . . F6 F -0.0084(4) 0.7296(4) 0.1287(2) 0.0544(10) Uani 1 1 d . . . F7 F 0.0740(4) 0.7026(4) -0.0373(2) 0.0706(12) Uani 1 1 d . . . F8 F 0.3652(4) 0.6591(4) -0.0917(2) 0.0697(12) Uani 1 1 d . . . F9 F 0.5678(4) 0.6505(4) 0.0265(2) 0.0624(11) Uani 1 1 d . . . F10 F 0.4898(3) 0.6835(4) 0.1898(2) 0.0538(10) Uani 1 1 d . . . F11 F 0.3187(4) 0.9368(3) 0.2483(2) 0.0534(10) Uani 1 1 d . . . F12 F 0.5142(4) 1.0100(4) 0.3413(3) 0.0772(13) Uani 1 1 d . . . F13 F 0.6075(4) 0.8678(5) 0.4829(3) 0.0985(17) Uani 1 1 d . . . F14 F 0.4968(5) 0.6507(4) 0.5267(3) 0.0865(15) Uani 1 1 d . . . F15 F 0.2996(4) 0.5786(4) 0.4375(2) 0.0637(11) Uani 1 1 d . . . C1 C -0.1023(7) 0.5473(7) 0.2912(4) 0.0555(19) Uani 1 1 d . . . C2 C -0.1320(8) 0.4825(7) 0.2074(5) 0.073(2) Uani 1 1 d . . . H2A H -0.2348 0.4816 0.2074 0.110 Uiso 1 1 calc R . . H2B H -0.0758 0.3938 0.2041 0.110 Uiso 1 1 calc R . . H2C H -0.1038 0.5321 0.1590 0.110 Uiso 1 1 calc R . . C3 C -0.2031(7) 0.6836(7) 0.2985(5) 0.062(2) Uani 1 1 d . . . H3A H -0.3032 0.6756 0.2948 0.094 Uiso 1 1 calc R . . H3B H -0.1763 0.7388 0.2526 0.094 Uiso 1 1 calc R . . H3C H -0.1929 0.7222 0.3525 0.094 Uiso 1 1 calc R . . C4 C -0.1458(9) 0.4674(9) 0.3693(5) 0.093(3) Uani 1 1 d . . . H4A H -0.2472 0.4619 0.3682 0.139 Uiso 1 1 calc R . . H4D H -0.1318 0.5103 0.4211 0.139 Uiso 1 1 calc R . . H4B H -0.0854 0.3803 0.3674 0.139 Uiso 1 1 calc R . . C5 C 0.2242(7) 0.4026(6) 0.2537(4) 0.0531(17) Uani 1 1 d . . . C6 C 0.2298(8) 0.3905(7) 0.1548(4) 0.064(2) Uani 1 1 d . . . H6A H 0.2980 0.3113 0.1369 0.095 Uiso 1 1 calc R . . H6B H 0.2612 0.4653 0.1286 0.095 Uiso 1 1 calc R . . H6C H 0.1338 0.3872 0.1376 0.095 Uiso 1 1 calc R . . C7 C 0.3814(7) 0.4073(7) 0.2777(4) 0.0622(19) Uani 1 1 d . . . H7A H 0.4492 0.3306 0.2555 0.093 Uiso 1 1 calc R . . H7B H 0.3833 0.4092 0.3390 0.093 Uiso 1 1 calc R . . H7C H 0.4091 0.4850 0.2534 0.093 Uiso 1 1 calc R . . C8 C 0.1821(10) 0.2787(7) 0.2962(6) 0.091(3) Uani 1 1 d . . . H8A H 0.2482 0.2013 0.2737 0.137 Uiso 1 1 calc R . . H8B H 0.0833 0.2755 0.2844 0.137 Uiso 1 1 calc R . . H8D H 0.1888 0.2824 0.3571 0.137 Uiso 1 1 calc R . . C9 C 0.0414(6) 0.8557(6) 0.2953(4) 0.0373(15) Uani 1 1 d . . . C10 C -0.0169(6) 0.8715(6) 0.3804(4) 0.0413(15) Uani 1 1 d . . . C11 C -0.1166(7) 0.9809(7) 0.4110(4) 0.0458(16) Uani 1 1 d . . . C12 C -0.1672(6) 1.0790(7) 0.3551(5) 0.0518(18) Uani 1 1 d . . . C13 C -0.1162(7) 1.0696(6) 0.2711(5) 0.0464(16) Uani 1 1 d . . . C14 C -0.0114(6) 0.9608(6) 0.2441(4) 0.0433(16) Uani 1 1 d . . . C15 C 0.2342(6) 0.7129(6) 0.1702(4) 0.0397(15) Uani 1 1 d . . . C16 C 0.1376(6) 0.7148(6) 0.1057(4) 0.0442(16) Uani 1 1 d . . . C17 C 0.1767(7) 0.6993(7) 0.0202(4) 0.0527(18) Uani 1 1 d . . . C18 C 0.3221(7) 0.6789(6) -0.0076(4) 0.0490(17) Uani 1 1 d . . . C19 C 0.4234(7) 0.6730(6) 0.0514(4) 0.0424(15) Uani 1 1 d . . . C20 C 0.3789(6) 0.6920(6) 0.1367(4) 0.0416(15) Uani 1 1 d . . . C21 C 0.3013(6) 0.7499(6) 0.3348(4) 0.0405(15) Uani 1 1 d . . . C22 C 0.3599(7) 0.8601(7) 0.3172(4) 0.0491(17) Uani 1 1 d . . . C23 C 0.4608(7) 0.9038(7) 0.3651(5) 0.0565(19) Uani 1 1 d . . . C24 C 0.5067(7) 0.8305(9) 0.4360(5) 0.067(2) Uani 1 1 d . . . C25 C 0.4516(8) 0.7207(9) 0.4579(4) 0.064(2) Uani 1 1 d . . . C26 C 0.3505(7) 0.6844(7) 0.4074(4) 0.0518(17) Uani 1 1 d . . . C51 C -0.5597(9) 1.0279(8) 0.0709(5) 0.082(2) Uiso 1 1 d D . . C52 C -0.2856(10) 0.9662(10) 0.0543(6) 0.110(3) Uiso 1 1 d D . . C54 C -0.4218(11) 1.0050(17) 0.1036(9) 0.087(5) Uiso 0.50 1 d PD . . C55 C -0.315(2) 0.9529(19) -0.0319(9) 0.098(6) Uiso 0.50 1 d PD . . C56 C -0.4295(14) 0.9881(16) 0.0123(11) 0.081(5) Uiso 0.50 1 d PD . . H1 H 0.097(4) 0.535(4) 0.389(3) 0.025(12) 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 0.0572(11) 0.0406(11) 0.0479(11) -0.0091(9) 0.0058(8) -0.0097(8) B1 0.043(4) 0.037(4) 0.037(4) -0.010(3) 0.000(3) -0.008(3) F1 0.054(2) 0.052(2) 0.044(2) -0.0104(19) 0.0056(17) -0.0072(18) F2 0.063(2) 0.068(3) 0.054(3) -0.030(2) 0.0148(19) -0.015(2) F3 0.062(2) 0.049(2) 0.097(3) -0.025(2) 0.012(2) -0.001(2) F4 0.071(3) 0.039(2) 0.078(3) 0.000(2) -0.005(2) 0.0003(19) F5 0.057(2) 0.048(2) 0.052(3) -0.0016(18) 0.0004(19) -0.0033(18) F6 0.046(2) 0.066(2) 0.051(2) -0.0128(19) -0.0033(17) -0.0089(18) F7 0.077(3) 0.093(3) 0.039(2) -0.020(2) -0.012(2) -0.006(2) F8 0.085(3) 0.082(3) 0.036(2) -0.012(2) 0.007(2) -0.007(2) F9 0.057(2) 0.071(3) 0.055(3) -0.012(2) 0.0179(19) -0.012(2) F10 0.045(2) 0.068(3) 0.046(2) -0.0183(19) -0.0025(17) -0.0032(18) F11 0.057(2) 0.047(2) 0.059(3) -0.004(2) -0.0001(19) -0.0189(18) F12 0.063(2) 0.093(3) 0.085(3) -0.038(3) 0.012(2) -0.040(2) F13 0.055(2) 0.146(4) 0.090(3) -0.071(3) -0.020(2) 0.000(3) F14 0.094(3) 0.091(3) 0.055(3) -0.023(2) -0.031(2) 0.038(3) F15 0.090(3) 0.050(3) 0.043(2) -0.002(2) -0.008(2) 0.004(2) C1 0.049(4) 0.054(5) 0.064(5) -0.016(4) 0.010(3) -0.015(3) C2 0.076(5) 0.070(5) 0.075(6) -0.035(4) 0.009(4) -0.021(4) C3 0.048(4) 0.070(5) 0.070(5) -0.018(4) 0.012(4) -0.017(4) C4 0.098(6) 0.087(6) 0.097(7) -0.006(6) 0.027(5) -0.041(5) C5 0.066(4) 0.040(4) 0.049(4) -0.012(3) 0.008(3) -0.006(3) C6 0.072(5) 0.056(5) 0.058(5) -0.017(4) 0.001(4) -0.003(4) C7 0.068(5) 0.047(4) 0.060(5) -0.013(4) -0.002(4) 0.015(4) C8 0.120(7) 0.041(5) 0.104(7) -0.006(5) 0.028(6) -0.006(5) C9 0.041(3) 0.033(4) 0.039(4) -0.004(3) -0.008(3) -0.010(3) C10 0.044(4) 0.034(4) 0.046(4) -0.006(3) -0.007(3) -0.008(3) C11 0.048(4) 0.045(4) 0.043(4) -0.019(4) 0.006(3) -0.008(3) C12 0.036(4) 0.039(4) 0.077(6) -0.025(4) 0.006(4) -0.002(3) C13 0.046(4) 0.034(4) 0.056(5) -0.008(4) 0.000(3) -0.001(3) C14 0.041(4) 0.052(4) 0.036(4) -0.013(3) 0.010(3) -0.011(3) C15 0.041(4) 0.044(4) 0.034(4) -0.006(3) 0.001(3) -0.008(3) C16 0.044(4) 0.044(4) 0.044(4) -0.010(3) 0.003(3) -0.008(3) C17 0.057(4) 0.061(5) 0.039(4) -0.017(4) -0.011(4) -0.006(4) C18 0.066(5) 0.044(4) 0.030(4) -0.011(3) 0.003(4) 0.004(3) C19 0.046(4) 0.037(4) 0.040(4) -0.006(3) 0.019(3) -0.005(3) C20 0.041(4) 0.046(4) 0.035(4) -0.003(3) 0.001(3) -0.004(3) C21 0.043(3) 0.040(4) 0.034(4) -0.009(3) -0.001(3) 0.001(3) C22 0.051(4) 0.050(4) 0.042(4) -0.009(4) -0.004(3) -0.001(3) C23 0.049(4) 0.066(5) 0.053(5) -0.034(4) 0.010(4) -0.012(4) C24 0.044(4) 0.097(7) 0.055(5) -0.045(5) -0.004(4) 0.003(4) C25 0.056(4) 0.083(6) 0.040(5) -0.026(4) -0.011(4) 0.023(4) C26 0.052(4) 0.049(5) 0.046(4) -0.016(4) -0.008(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C5 1.861(6) . ? P1 C1 1.892(6) . ? P1 B1 2.094(7) . ? B1 C15 1.622(9) . ? B1 C9 1.656(9) . ? B1 C21 1.659(8) . ? F1 C10 1.358(7) . ? F2 C11 1.344(7) . ? F3 C12 1.352(7) . ? F4 C13 1.344(7) . ? F5 C14 1.362(7) . ? F6 C16 1.360(7) . ? F7 C17 1.353(6) . ? F8 C18 1.354(7) . ? F9 C19 1.347(6) . ? F10 C20 1.359(6) . ? F11 C22 1.358(7) . ? F12 C23 1.336(8) . ? F13 C24 1.353(7) . ? F14 C25 1.331(8) . ? F15 C26 1.348(8) . ? C1 C3 1.528(9) . ? C1 C4 1.540(10) . ? C1 C2 1.551(9) . ? C5 C8 1.545(9) . ? C5 C7 1.549(9) . ? C5 C6 1.550(8) . ? C9 C14 1.368(8) . ? C9 C10 1.400(8) . ? C10 C11 1.379(8) . ? C11 C12 1.360(9) . ? C12 C13 1.362(9) . ? C13 C14 1.381(8) . ? C15 C20 1.386(8) . ? C15 C16 1.396(8) . ? C16 C17 1.364(8) . ? C17 C18 1.367(9) . ? C18 C19 1.358(8) . ? C19 C20 1.373(8) . ? C21 C26 1.371(9) . ? C21 C22 1.381(8) . ? C22 C23 1.393(9) . ? C23 C24 1.375(10) . ? C24 C25 1.371(11) . ? C25 C26 1.385(9) . ? C51 C56 1.329(16) 2_475 ? C51 C55 1.336(17) 2_475 ? C51 C54 1.389(9) . ? C51 C56 1.459(18) . ? C52 C55 1.408(9) . ? C52 C54 1.423(9) . ? C52 C56 1.508(9) . ? C54 C56 1.45(2) . ? C55 C56 1.22(2) . ? C55 C51 1.336(17) 2_475 ? C56 C51 1.329(16) 2_475 ? C56 C56 1.37(2) 2_475 ? 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 C5 P1 C1 112.5(3) . . ? C5 P1 B1 113.7(3) . . ? C1 P1 B1 121.5(3) . . ? C15 B1 C9 116.2(5) . . ? C15 B1 C21 113.5(5) . . ? C9 B1 C21 100.9(4) . . ? C15 B1 P1 104.2(4) . . ? C9 B1 P1 109.2(4) . . ? C21 B1 P1 113.2(4) . . ? C3 C1 C4 106.5(6) . . ? C3 C1 C2 108.2(6) . . ? C4 C1 C2 109.8(6) . . ? C3 C1 P1 112.4(4) . . ? C4 C1 P1 107.2(5) . . ? C2 C1 P1 112.6(5) . . ? C8 C5 C7 107.8(6) . . ? C8 C5 C6 109.8(6) . . ? C7 C5 C6 107.2(5) . . ? C8 C5 P1 110.0(5) . . ? C7 C5 P1 107.6(4) . . ? C6 C5 P1 114.1(5) . . ? C14 C9 C10 113.0(5) . . ? C14 C9 B1 127.7(5) . . ? C10 C9 B1 118.9(5) . . ? F1 C10 C11 116.1(6) . . ? F1 C10 C9 119.5(5) . . ? C11 C10 C9 124.4(6) . . ? F2 C11 C12 121.1(6) . . ? F2 C11 C10 120.2(6) . . ? C12 C11 C10 118.7(6) . . ? F3 C12 C11 119.9(7) . . ? F3 C12 C13 120.1(7) . . ? C11 C12 C13 120.0(6) . . ? F4 C13 C12 120.0(6) . . ? F4 C13 C14 120.7(6) . . ? C12 C13 C14 119.3(6) . . ? F5 C14 C9 121.0(5) . . ? F5 C14 C13 114.4(6) . . ? C9 C14 C13 124.5(6) . . ? C20 C15 C16 111.3(5) . . ? C20 C15 B1 127.4(5) . . ? C16 C15 B1 121.2(5) . . ? F6 C16 C17 115.9(5) . . ? F6 C16 C15 118.4(5) . . ? C17 C16 C15 125.7(6) . . ? F7 C17 C16 121.0(6) . . ? F7 C17 C18 119.7(6) . . ? C16 C17 C18 119.3(6) . . ? F8 C18 C19 120.4(6) . . ? F8 C18 C17 120.8(6) . . ? C19 C18 C17 118.6(6) . . ? F9 C19 C18 120.2(6) . . ? F9 C19 C20 119.7(5) . . ? C18 C19 C20 120.1(6) . . ? F10 C20 C19 114.9(5) . . ? F10 C20 C15 120.2(5) . . ? C19 C20 C15 124.9(5) . . ? C26 C21 C22 113.2(6) . . ? C26 C21 B1 131.3(6) . . ? C22 C21 B1 115.3(5) . . ? F11 C22 C21 119.9(5) . . ? F11 C22 C23 114.3(6) . . ? C21 C22 C23 125.8(7) . . ? F12 C23 C24 121.7(6) . . ? F12 C23 C22 121.1(7) . . ? C24 C23 C22 117.2(7) . . ? F13 C24 C25 120.8(8) . . ? F13 C24 C23 118.9(8) . . ? C25 C24 C23 120.2(6) . . ? F14 C25 C24 119.6(7) . . ? F14 C25 C26 121.2(8) . . ? C24 C25 C26 119.1(7) . . ? F15 C26 C21 121.8(6) . . ? F15 C26 C25 113.6(7) . . ? C21 C26 C25 124.5(7) . . ? C56 C51 C55 54.7(9) 2_475 2_475 ? C56 C51 C54 119.6(10) 2_475 . ? C55 C51 C54 174.3(11) 2_475 . ? C56 C51 C56 58.5(9) 2_475 . ? C55 C51 C56 113.2(10) 2_475 . ? C54 C51 C56 61.1(8) . . ? C55 C52 C54 108.6(11) . . ? C55 C52 C56 49.5(10) . . ? C54 C52 C56 59.2(9) . . ? C51 C54 C52 125.2(11) . . ? C51 C54 C56 61.8(8) . . ? C52 C54 C56 63.3(7) . . ? C56 C55 C51 62.4(12) . 2_475 ? C56 C55 C52 69.5(8) . . ? C51 C55 C52 131.9(15) 2_475 . ? C55 C56 C51 63.0(12) . 2_475 ? C55 C56 C56 128(2) . 2_475 ? C51 C56 C56 65.5(12) 2_475 2_475 ? C55 C56 C54 118.5(9) . . ? C51 C56 C54 178.4(12) 2_475 . ? C56 C56 C54 113.1(19) 2_475 . ? C55 C56 C51 175.5(13) . . ? C51 C56 C51 121.5(9) 2_475 . ? C56 C56 C51 56.0(12) 2_475 . ? C54 C56 C51 57.1(8) . . ? C55 C56 C52 61.0(6) . . ? C51 C56 C52 123.9(13) 2_475 . ? C56 C56 C52 171(2) 2_475 . ? C54 C56 C52 57.5(6) . . ? C51 C56 C52 114.6(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.531 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.077 #===end data_Ph2PH(B(C6F5)3) _database_code_depnum_ccdc_archive 'CCDC 698993' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C30 H11 B F15 P' _chemical_formula_weight 698.17 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 16.064(2) _cell_length_b 8.3163(11) _cell_length_c 21.102(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.364(2) _cell_angle_gamma 90.00 _cell_volume 2753.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6400 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 24.63 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.948 _exptl_absorpt_correction_T_max 0.978 _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 25561 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4837 _reflns_number_gt 3586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0475P)^2^+0.5727P] 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_number_reflns 4837 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0997 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 P1 P 0.22343(3) 0.63473(7) 0.41143(3) 0.04842(16) Uani 1 1 d . . . B1 B 0.21582(15) 0.3855(3) 0.42449(11) 0.0463(5) Uani 1 1 d . . . F1 F 0.19309(8) 0.05594(16) 0.38427(8) 0.0761(4) Uani 1 1 d . . . F2 F 0.05461(10) -0.08456(19) 0.31762(8) 0.0882(5) Uani 1 1 d . . . F3 F -0.09051(9) 0.0878(2) 0.27456(8) 0.0911(5) Uani 1 1 d . . . F4 F -0.09428(8) 0.4021(2) 0.30723(9) 0.0920(5) Uani 1 1 d . . . F5 F 0.04230(8) 0.54433(18) 0.37634(9) 0.0903(5) Uani 1 1 d . . . F6 F 0.23749(8) 0.43608(17) 0.29562(6) 0.0626(3) Uani 1 1 d . . . F7 F 0.37200(9) 0.3635(2) 0.24584(7) 0.0807(4) Uani 1 1 d . . . F8 F 0.50615(9) 0.2001(2) 0.31870(8) 0.0934(5) Uani 1 1 d . . . F9 F 0.50044(8) 0.10908(19) 0.44086(7) 0.0824(5) Uani 1 1 d . . . F10 F 0.36685(8) 0.17586(16) 0.49055(6) 0.0628(4) Uani 1 1 d . . . F11 F 0.35495(8) 0.48510(15) 0.52806(6) 0.0595(3) Uani 1 1 d . . . F12 F 0.36311(10) 0.4767(2) 0.65455(6) 0.0853(5) Uani 1 1 d . . . F13 F 0.22990(10) 0.3580(2) 0.70175(6) 0.0933(5) Uani 1 1 d . . . F14 F 0.09195(10) 0.2388(2) 0.61750(8) 0.0882(5) Uani 1 1 d . . . F15 F 0.08164(9) 0.2467(2) 0.49235(7) 0.0828(5) Uani 1 1 d . . . C1 C 0.12792(13) 0.3120(3) 0.37984(10) 0.0481(5) Uani 1 1 d . . . C2 C 0.12449(13) 0.1503(3) 0.36344(10) 0.0518(5) Uani 1 1 d . . . C3 C 0.05317(15) 0.0742(3) 0.32941(11) 0.0589(6) Uani 1 1 d . . . C4 C -0.02011(14) 0.1591(3) 0.30860(11) 0.0631(6) Uani 1 1 d . . . C5 C -0.02173(14) 0.3177(3) 0.32417(12) 0.0624(6) Uani 1 1 d . . . C6 C 0.05111(14) 0.3891(3) 0.35944(11) 0.0572(6) Uani 1 1 d . . . C7 C 0.29735(12) 0.3203(2) 0.39707(10) 0.0460(5) Uani 1 1 d . . . C8 C 0.30253(13) 0.3555(3) 0.33371(10) 0.0510(5) Uani 1 1 d . . . C9 C 0.37057(15) 0.3189(3) 0.30687(11) 0.0586(6) Uani 1 1 d . . . C10 C 0.43831(15) 0.2376(3) 0.34319(13) 0.0639(6) Uani 1 1 d . . . C11 C 0.43542(14) 0.1916(3) 0.40525(12) 0.0591(6) Uani 1 1 d . . . C12 C 0.36582(13) 0.2318(3) 0.43039(10) 0.0504(5) Uani 1 1 d . . . C13 C 0.21882(13) 0.3657(3) 0.50211(10) 0.0488(5) Uani 1 1 d . . . C14 C 0.28736(13) 0.4215(3) 0.54820(10) 0.0510(5) Uani 1 1 d . . . C15 C 0.29313(16) 0.4191(3) 0.61405(11) 0.0610(6) Uani 1 1 d . . . C16 C 0.22697(17) 0.3593(3) 0.63792(11) 0.0667(7) Uani 1 1 d . . . C17 C 0.15695(16) 0.3016(3) 0.59518(12) 0.0632(6) Uani 1 1 d . . . C18 C 0.15407(14) 0.3061(3) 0.52947(11) 0.0573(6) Uani 1 1 d . . . C19 C 0.21465(14) 0.7503(3) 0.48242(11) 0.0516(5) Uani 1 1 d . . . C20 C 0.28457(16) 0.8248(3) 0.52089(13) 0.0672(7) Uani 1 1 d . . . H20A H 0.3367 0.8243 0.5083 0.081 Uiso 1 1 calc R . . C21 C 0.27741(19) 0.8996(3) 0.57756(14) 0.0799(8) Uani 1 1 d . . . H21A H 0.3250 0.9475 0.6036 0.096 Uiso 1 1 calc R . . C22 C 0.2010(2) 0.9042(4) 0.59597(14) 0.0833(8) Uani 1 1 d . . . H22A H 0.1967 0.9532 0.6348 0.100 Uiso 1 1 calc R . . C23 C 0.1309(2) 0.8364(4) 0.55693(16) 0.0921(10) Uani 1 1 d . . . H23A H 0.0783 0.8427 0.5686 0.110 Uiso 1 1 calc R . . C24 C 0.13739(17) 0.7587(3) 0.50044(13) 0.0741(7) Uani 1 1 d . . . H24A H 0.0894 0.7118 0.4745 0.089 Uiso 1 1 calc R . . C25 C 0.31432(14) 0.7054(3) 0.38135(10) 0.0506(5) Uani 1 1 d . . . C26 C 0.29828(17) 0.7872(3) 0.32298(12) 0.0687(7) Uani 1 1 d . . . H26A H 0.2425 0.8094 0.3019 0.082 Uiso 1 1 calc R . . C27 C 0.3650(2) 0.8357(4) 0.29598(14) 0.0887(9) Uani 1 1 d . . . H27A H 0.3540 0.8904 0.2566 0.106 Uiso 1 1 calc R . . C28 C 0.44749(19) 0.8037(4) 0.32691(15) 0.0836(8) Uani 1 1 d . . . H28A H 0.4922 0.8359 0.3083 0.100 Uiso 1 1 calc R . . C29 C 0.46403(16) 0.7250(3) 0.38470(13) 0.0721(7) Uani 1 1 d . . . H29A H 0.5201 0.7050 0.4058 0.087 Uiso 1 1 calc R . . C30 C 0.39775(14) 0.6748(3) 0.41199(12) 0.0610(6) Uani 1 1 d . . . H30A H 0.4093 0.6200 0.4513 0.073 Uiso 1 1 calc R . . H1 H 0.1603(13) 0.684(2) 0.3674(10) 0.056(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 0.0427(3) 0.0545(3) 0.0485(3) 0.0032(3) 0.0109(2) 0.0050(3) B1 0.0419(12) 0.0508(14) 0.0453(13) 0.0009(11) 0.0071(10) 0.0048(11) F1 0.0590(8) 0.0568(8) 0.1047(11) 0.0023(8) 0.0000(8) 0.0067(7) F2 0.0824(10) 0.0685(10) 0.1089(12) -0.0236(9) 0.0099(9) -0.0110(8) F3 0.0601(9) 0.1147(13) 0.0889(11) -0.0253(10) -0.0059(8) -0.0196(9) F4 0.0446(8) 0.1043(12) 0.1181(13) -0.0033(10) -0.0026(8) 0.0135(8) F5 0.0496(8) 0.0699(10) 0.1467(15) -0.0245(10) 0.0107(9) 0.0109(7) F6 0.0594(8) 0.0794(9) 0.0465(7) 0.0048(6) 0.0055(6) 0.0135(7) F7 0.0840(10) 0.1074(12) 0.0583(9) 0.0020(8) 0.0325(7) 0.0020(9) F8 0.0626(9) 0.1244(13) 0.1050(12) 0.0003(10) 0.0443(9) 0.0167(9) F9 0.0526(8) 0.0971(11) 0.0942(11) 0.0060(9) 0.0084(7) 0.0263(8) F10 0.0623(8) 0.0686(9) 0.0561(8) 0.0089(6) 0.0094(6) 0.0144(6) F11 0.0557(7) 0.0676(8) 0.0537(7) -0.0019(6) 0.0082(6) -0.0054(6) F12 0.0823(10) 0.1190(13) 0.0491(8) -0.0144(8) 0.0019(7) 0.0036(9) F13 0.1032(12) 0.1356(15) 0.0465(8) 0.0148(8) 0.0278(8) 0.0353(11) F14 0.0799(10) 0.1142(13) 0.0830(10) 0.0227(9) 0.0451(9) 0.0125(9) F15 0.0604(9) 0.1209(13) 0.0706(9) 0.0019(9) 0.0217(7) -0.0198(8) C1 0.0437(12) 0.0561(13) 0.0451(11) 0.0008(10) 0.0107(9) 0.0006(10) C2 0.0485(12) 0.0567(14) 0.0495(12) 0.0011(10) 0.0088(10) 0.0044(10) C3 0.0596(14) 0.0603(15) 0.0566(14) -0.0106(11) 0.0119(11) -0.0053(12) C4 0.0478(13) 0.0861(19) 0.0524(13) -0.0117(12) 0.0044(11) -0.0120(13) C5 0.0400(12) 0.0813(18) 0.0637(15) 0.0036(13) 0.0060(10) 0.0060(12) C6 0.0470(13) 0.0593(14) 0.0652(14) -0.0048(11) 0.0116(11) 0.0041(11) C7 0.0406(11) 0.0515(12) 0.0447(11) -0.0037(9) 0.0064(9) 0.0004(9) C8 0.0454(12) 0.0572(13) 0.0483(12) -0.0046(10) 0.0058(10) 0.0025(10) C9 0.0587(14) 0.0706(15) 0.0503(13) -0.0054(11) 0.0202(11) -0.0012(12) C10 0.0483(13) 0.0753(17) 0.0740(17) -0.0079(13) 0.0259(12) 0.0035(12) C11 0.0419(12) 0.0636(14) 0.0694(16) -0.0030(12) 0.0065(11) 0.0089(11) C12 0.0466(12) 0.0546(13) 0.0487(12) -0.0032(10) 0.0070(10) 0.0013(10) C13 0.0489(12) 0.0504(12) 0.0482(12) 0.0019(10) 0.0127(10) 0.0080(10) C14 0.0517(13) 0.0522(12) 0.0499(13) 0.0011(10) 0.0123(10) 0.0063(10) C15 0.0631(15) 0.0727(16) 0.0451(13) -0.0032(11) 0.0072(11) 0.0157(12) C16 0.0778(17) 0.0813(17) 0.0449(13) 0.0095(12) 0.0214(13) 0.0289(14) C17 0.0623(15) 0.0735(16) 0.0625(15) 0.0132(12) 0.0323(13) 0.0167(13) C18 0.0488(13) 0.0658(15) 0.0586(14) 0.0038(11) 0.0145(11) 0.0051(11) C19 0.0538(13) 0.0477(12) 0.0570(13) 0.0034(10) 0.0199(11) 0.0044(10) C20 0.0598(15) 0.0676(16) 0.0776(17) -0.0122(13) 0.0224(13) -0.0008(12) C21 0.0837(19) 0.0747(18) 0.0800(19) -0.0207(15) 0.0147(15) -0.0049(15) C22 0.109(2) 0.0775(19) 0.0736(18) -0.0141(15) 0.0424(18) 0.0006(17) C23 0.087(2) 0.109(2) 0.095(2) -0.0268(19) 0.0516(18) -0.0113(18) C24 0.0649(16) 0.0845(19) 0.0790(18) -0.0142(15) 0.0292(14) -0.0089(14) C25 0.0524(13) 0.0533(12) 0.0486(12) -0.0015(10) 0.0163(10) 0.0008(10) C26 0.0693(16) 0.0809(18) 0.0589(15) 0.0141(13) 0.0203(12) 0.0061(13) C27 0.096(2) 0.109(2) 0.0680(18) 0.0255(16) 0.0333(17) -0.0007(18) C28 0.077(2) 0.103(2) 0.082(2) -0.0012(17) 0.0432(16) -0.0145(17) C29 0.0561(15) 0.0884(19) 0.0756(18) -0.0060(15) 0.0222(13) -0.0048(13) C30 0.0538(14) 0.0736(16) 0.0572(14) 0.0071(12) 0.0154(11) 0.0013(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 P1 C25 1.810(2) . ? P1 C19 1.811(2) . ? P1 B1 2.098(3) . ? P1 H1 1.29(2) . ? B1 C7 1.634(3) . ? B1 C13 1.637(3) . ? B1 C1 1.639(3) . ? F1 C2 1.348(2) . ? F2 C3 1.345(3) . ? F3 C4 1.341(3) . ? F4 C5 1.341(3) . ? F5 C6 1.355(3) . ? F6 C8 1.352(2) . ? F7 C9 1.345(3) . ? F8 C10 1.339(3) . ? F9 C11 1.338(3) . ? F10 C12 1.349(2) . ? F11 C14 1.355(2) . ? F12 C15 1.346(3) . ? F13 C16 1.338(3) . ? F14 C17 1.340(3) . ? F15 C18 1.350(3) . ? C1 C6 1.375(3) . ? C1 C2 1.386(3) . ? C2 C3 1.370(3) . ? C3 C4 1.362(3) . ? C4 C5 1.361(4) . ? C5 C6 1.379(3) . ? C7 C12 1.384(3) . ? C7 C8 1.389(3) . ? C8 C9 1.369(3) . ? C9 C10 1.368(3) . ? C10 C11 1.375(3) . ? C11 C12 1.377(3) . ? C13 C14 1.384(3) . ? C13 C18 1.385(3) . ? C14 C15 1.373(3) . ? C15 C16 1.364(4) . ? C16 C17 1.369(4) . ? C17 C18 1.378(3) . ? C19 C24 1.375(3) . ? C19 C20 1.383(3) . ? C20 C21 1.375(4) . ? C20 H20A 0.9300 . ? C21 C22 1.365(4) . ? C21 H21A 0.9300 . ? C22 C23 1.367(4) . ? C22 H22A 0.9300 . ? C23 C24 1.380(4) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C30 1.381(3) . ? C25 C26 1.382(3) . ? C26 C27 1.377(4) . ? C26 H26A 0.9300 . ? C27 C28 1.373(4) . ? C27 H27A 0.9300 . ? C28 C29 1.359(4) . ? C28 H28A 0.9300 . ? C29 C30 1.379(3) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? 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 C25 P1 C19 109.23(10) . . ? C25 P1 B1 116.16(10) . . ? C19 P1 B1 113.51(10) . . ? C25 P1 H1 102.4(9) . . ? C19 P1 H1 103.9(9) . . ? B1 P1 H1 110.4(9) . . ? C7 B1 C13 117.83(17) . . ? C7 B1 C1 109.26(17) . . ? C13 B1 C1 112.02(17) . . ? C7 B1 P1 101.99(14) . . ? C13 B1 P1 103.94(14) . . ? C1 B1 P1 111.13(14) . . ? C6 C1 C2 112.90(19) . . ? C6 C1 B1 127.6(2) . . ? C2 C1 B1 119.26(18) . . ? F1 C2 C3 115.8(2) . . ? F1 C2 C1 119.83(19) . . ? C3 C2 C1 124.3(2) . . ? F2 C3 C4 119.8(2) . . ? F2 C3 C2 120.3(2) . . ? C4 C3 C2 119.9(2) . . ? F3 C4 C5 120.0(2) . . ? F3 C4 C3 121.0(2) . . ? C5 C4 C3 119.0(2) . . ? F4 C5 C4 120.2(2) . . ? F4 C5 C6 120.5(2) . . ? C4 C5 C6 119.3(2) . . ? F5 C6 C1 120.0(2) . . ? F5 C6 C5 115.3(2) . . ? C1 C6 C5 124.7(2) . . ? C12 C7 C8 113.35(18) . . ? C12 C7 B1 127.37(19) . . ? C8 C7 B1 119.27(18) . . ? F6 C8 C9 116.63(19) . . ? F6 C8 C7 118.62(18) . . ? C9 C8 C7 124.7(2) . . ? F7 C9 C10 119.9(2) . . ? F7 C9 C8 120.9(2) . . ? C10 C9 C8 119.2(2) . . ? F8 C10 C9 121.0(2) . . ? F8 C10 C11 119.9(2) . . ? C9 C10 C11 119.1(2) . . ? F9 C11 C10 119.8(2) . . ? F9 C11 C12 120.6(2) . . ? C10 C11 C12 119.7(2) . . ? F10 C12 C11 115.57(19) . . ? F10 C12 C7 120.65(18) . . ? C11 C12 C7 123.8(2) . . ? C14 C13 C18 112.5(2) . . ? C14 C13 B1 121.21(19) . . ? C18 C13 B1 126.12(19) . . ? F11 C14 C15 116.0(2) . . ? F11 C14 C13 118.74(18) . . ? C15 C14 C13 125.3(2) . . ? F12 C15 C16 120.4(2) . . ? F12 C15 C14 120.2(2) . . ? C16 C15 C14 119.4(2) . . ? F13 C16 C15 120.8(2) . . ? F13 C16 C17 120.5(2) . . ? C15 C16 C17 118.7(2) . . ? F14 C17 C16 119.8(2) . . ? F14 C17 C18 120.2(2) . . ? C16 C17 C18 120.0(2) . . ? F15 C18 C17 114.4(2) . . ? F15 C18 C13 121.3(2) . . ? C17 C18 C13 124.3(2) . . ? C24 C19 C20 118.9(2) . . ? C24 C19 P1 119.35(18) . . ? C20 C19 P1 121.73(17) . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C23 119.5(3) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C19 C24 C23 120.1(3) . . ? C19 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C30 C25 C26 119.0(2) . . ? C30 C25 P1 123.41(17) . . ? C26 C25 P1 117.51(17) . . ? C27 C26 C25 120.0(3) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 120.2(2) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C28 C29 C30 120.0(3) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 C25 120.5(2) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? 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 C25 P1 B1 C7 -3.84(17) . . . . ? C19 P1 B1 C7 -131.71(13) . . . . ? C25 P1 B1 C13 119.15(14) . . . . ? C19 P1 B1 C13 -8.72(17) . . . . ? C25 P1 B1 C1 -120.18(15) . . . . ? C19 P1 B1 C1 111.96(15) . . . . ? C7 B1 C1 C6 -140.4(2) . . . . ? C13 B1 C1 C6 87.2(3) . . . . ? P1 B1 C1 C6 -28.6(3) . . . . ? C7 B1 C1 C2 45.3(3) . . . . ? C13 B1 C1 C2 -87.2(2) . . . . ? P1 B1 C1 C2 157.05(16) . . . . ? C6 C1 C2 F1 -175.12(19) . . . . ? B1 C1 C2 F1 0.0(3) . . . . ? C6 C1 C2 C3 1.2(3) . . . . ? B1 C1 C2 C3 176.4(2) . . . . ? F1 C2 C3 F2 -1.1(3) . . . . ? C1 C2 C3 F2 -177.6(2) . . . . ? F1 C2 C3 C4 177.5(2) . . . . ? C1 C2 C3 C4 1.0(4) . . . . ? F2 C3 C4 F3 -2.2(4) . . . . ? C2 C3 C4 F3 179.2(2) . . . . ? F2 C3 C4 C5 176.3(2) . . . . ? C2 C3 C4 C5 -2.3(4) . . . . ? F3 C4 C5 F4 2.0(4) . . . . ? C3 C4 C5 F4 -176.5(2) . . . . ? F3 C4 C5 C6 179.7(2) . . . . ? C3 C4 C5 C6 1.2(4) . . . . ? C2 C1 C6 F5 174.6(2) . . . . ? B1 C1 C6 F5 0.0(3) . . . . ? C2 C1 C6 C5 -2.4(3) . . . . ? B1 C1 C6 C5 -177.0(2) . . . . ? F4 C5 C6 F5 1.8(3) . . . . ? C4 C5 C6 F5 -175.9(2) . . . . ? F4 C5 C6 C1 179.0(2) . . . . ? C4 C5 C6 C1 1.2(4) . . . . ? C13 B1 C7 C12 8.3(3) . . . . ? C1 B1 C7 C12 -121.0(2) . . . . ? P1 B1 C7 C12 121.3(2) . . . . ? C13 B1 C7 C8 -170.88(19) . . . . ? C1 B1 C7 C8 59.8(2) . . . . ? P1 B1 C7 C8 -57.9(2) . . . . ? C12 C7 C8 F6 177.40(18) . . . . ? B1 C7 C8 F6 -3.3(3) . . . . ? C12 C7 C8 C9 -4.7(3) . . . . ? B1 C7 C8 C9 174.6(2) . . . . ? F6 C8 C9 F7 0.8(3) . . . . ? C7 C8 C9 F7 -177.1(2) . . . . ? F6 C8 C9 C10 179.9(2) . . . . ? C7 C8 C9 C10 2.0(4) . . . . ? F7 C9 C10 F8 -0.7(4) . . . . ? C8 C9 C10 F8 -179.8(2) . . . . ? F7 C9 C10 C11 -179.4(2) . . . . ? C8 C9 C10 C11 1.5(4) . . . . ? F8 C10 C11 F9 -0.2(4) . . . . ? C9 C10 C11 F9 178.6(2) . . . . ? F8 C10 C11 C12 179.4(2) . . . . ? C9 C10 C11 C12 -1.8(4) . . . . ? F9 C11 C12 F10 -3.1(3) . . . . ? C10 C11 C12 F10 177.3(2) . . . . ? F9 C11 C12 C7 178.3(2) . . . . ? C10 C11 C12 C7 -1.3(4) . . . . ? C8 C7 C12 F10 -174.20(18) . . . . ? B1 C7 C12 F10 6.6(3) . . . . ? C8 C7 C12 C11 4.3(3) . . . . ? B1 C7 C12 C11 -174.9(2) . . . . ? C7 B1 C13 C14 52.6(3) . . . . ? C1 B1 C13 C14 -179.36(19) . . . . ? P1 B1 C13 C14 -59.3(2) . . . . ? C7 B1 C13 C18 -132.7(2) . . . . ? C1 B1 C13 C18 -4.7(3) . . . . ? P1 B1 C13 C18 115.4(2) . . . . ? C18 C13 C14 F11 -179.19(18) . . . . ? B1 C13 C14 F11 -3.8(3) . . . . ? C18 C13 C14 C15 0.4(3) . . . . ? B1 C13 C14 C15 175.8(2) . . . . ? F11 C14 C15 F12 -0.4(3) . . . . ? C13 C14 C15 F12 179.9(2) . . . . ? F11 C14 C15 C16 178.9(2) . . . . ? C13 C14 C15 C16 -0.7(4) . . . . ? F12 C15 C16 F13 0.6(4) . . . . ? C14 C15 C16 F13 -178.7(2) . . . . ? F12 C15 C16 C17 -179.9(2) . . . . ? C14 C15 C16 C17 0.7(4) . . . . ? F13 C16 C17 F14 -2.1(4) . . . . ? C15 C16 C17 F14 178.5(2) . . . . ? F13 C16 C17 C18 178.9(2) . . . . ? C15 C16 C17 C18 -0.6(4) . . . . ? F14 C17 C18 F15 1.3(3) . . . . ? C16 C17 C18 F15 -179.7(2) . . . . ? F14 C17 C18 C13 -178.7(2) . . . . ? C16 C17 C18 C13 0.4(4) . . . . ? C14 C13 C18 F15 179.8(2) . . . . ? B1 C13 C18 F15 4.7(4) . . . . ? C14 C13 C18 C17 -0.3(3) . . . . ? B1 C13 C18 C17 -175.4(2) . . . . ? C25 P1 C19 C24 157.88(19) . . . . ? B1 P1 C19 C24 -70.7(2) . . . . ? C25 P1 C19 C20 -25.1(2) . . . . ? B1 P1 C19 C20 106.3(2) . . . . ? C24 C19 C20 C21 2.8(4) . . . . ? P1 C19 C20 C21 -174.2(2) . . . . ? C19 C20 C21 C22 -1.3(4) . . . . ? C20 C21 C22 C23 -1.2(5) . . . . ? C21 C22 C23 C24 2.3(5) . . . . ? C20 C19 C24 C23 -1.8(4) . . . . ? P1 C19 C24 C23 175.3(2) . . . . ? C22 C23 C24 C19 -0.8(5) . . . . ? C19 P1 C25 C30 72.9(2) . . . . ? B1 P1 C25 C30 -57.0(2) . . . . ? C19 P1 C25 C26 -110.4(2) . . . . ? B1 P1 C25 C26 119.71(19) . . . . ? C30 C25 C26 C27 0.5(4) . . . . ? P1 C25 C26 C27 -176.3(2) . . . . ? C25 C26 C27 C28 -0.2(5) . . . . ? C26 C27 C28 C29 -0.6(5) . . . . ? C27 C28 C29 C30 1.0(5) . . . . ? C28 C29 C30 C25 -0.7(4) . . . . ? C26 C25 C30 C29 -0.1(4) . . . . ? P1 C25 C30 C29 176.59(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.292 _refine_diff_density_min -0.157 _refine_diff_density_rms 0.038 #===end data_Et3PB(C6F5)3 _database_code_depnum_ccdc_archive 'CCDC 698994' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H15 B F15 P' _chemical_formula_weight 630.14 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.197(2) _cell_length_b 10.5908(18) _cell_length_c 18.211(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.850(2) _cell_angle_gamma 90.00 _cell_volume 2539.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4868 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.18 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.946 _exptl_absorpt_correction_T_max 0.977 _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 23727 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4463 _reflns_number_gt 2363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0484P)^2^+0.6880P] 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_number_reflns 4463 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 P1 P 0.05658(7) 0.34273(9) 0.23512(5) 0.0473(3) Uani 1 1 d . . . B1 B 0.0355(3) 0.4010(4) 0.3422(2) 0.0434(10) Uani 1 1 d . . . F1 F 0.06344(17) 0.2587(2) 0.48755(11) 0.0710(7) Uani 1 1 d . . . F2 F -0.06238(18) 0.0954(2) 0.53844(13) 0.0824(7) Uani 1 1 d . . . F3 F -0.2396(2) 0.0382(3) 0.46258(14) 0.1096(10) Uani 1 1 d . . . F4 F -0.28853(19) 0.1550(3) 0.33203(15) 0.1101(10) Uani 1 1 d . . . F5 F -0.16240(15) 0.3219(2) 0.27839(12) 0.0727(7) Uani 1 1 d . . . F6 F 0.17787(16) 0.19261(19) 0.35073(12) 0.0678(6) Uani 1 1 d . . . F7 F 0.36265(18) 0.1869(2) 0.41868(14) 0.0933(8) Uani 1 1 d . . . F8 F 0.43449(18) 0.3898(2) 0.49733(15) 0.1005(9) Uani 1 1 d . . . F9 F 0.31643(18) 0.5987(2) 0.50530(13) 0.0814(7) Uani 1 1 d . . . F10 F 0.13538(16) 0.6086(2) 0.43694(11) 0.0699(6) Uani 1 1 d . . . F11 F -0.16224(17) 0.5023(2) 0.39892(12) 0.0762(7) Uani 1 1 d . . . F12 F -0.2330(2) 0.7316(3) 0.38067(14) 0.1007(9) Uani 1 1 d . . . F13 F -0.1294(2) 0.9089(2) 0.30845(17) 0.1127(10) Uani 1 1 d . . . F14 F 0.0510(2) 0.8456(2) 0.25440(16) 0.1041(9) Uani 1 1 d . . . F15 F 0.12452(17) 0.61482(19) 0.27137(13) 0.0725(7) Uani 1 1 d . . . C1 C -0.0396(3) 0.2972(3) 0.37755(19) 0.0447(9) Uani 1 1 d . . . C2 C -0.0214(3) 0.2354(4) 0.4439(2) 0.0518(10) Uani 1 1 d . . . C3 C -0.0867(3) 0.1490(4) 0.4727(2) 0.0586(10) Uani 1 1 d . . . C4 C -0.1761(3) 0.1206(4) 0.4353(3) 0.0703(12) Uani 1 1 d . . . C5 C -0.2000(3) 0.1800(4) 0.3696(2) 0.0680(12) Uani 1 1 d . . . C6 C -0.1332(3) 0.2642(4) 0.3428(2) 0.0540(10) Uani 1 1 d . . . C7 C 0.1480(3) 0.4024(3) 0.38558(18) 0.0440(9) Uani 1 1 d . . . C8 C 0.2111(3) 0.2985(4) 0.38641(19) 0.0522(10) Uani 1 1 d . . . C9 C 0.3052(3) 0.2916(4) 0.4223(2) 0.0623(11) Uani 1 1 d . . . C10 C 0.3417(3) 0.3932(5) 0.4619(2) 0.0650(12) Uani 1 1 d . . . C11 C 0.2827(3) 0.4982(4) 0.4658(2) 0.0583(11) Uani 1 1 d . . . C12 C 0.1884(3) 0.5011(4) 0.42809(19) 0.0513(9) Uani 1 1 d . . . C13 C -0.0163(3) 0.5424(3) 0.33323(18) 0.0456(9) Uani 1 1 d . . . C14 C -0.1061(3) 0.5818(4) 0.3603(2) 0.0528(10) Uani 1 1 d . . . C15 C -0.1446(3) 0.7023(4) 0.3521(2) 0.0652(11) Uani 1 1 d . . . C16 C -0.0926(4) 0.7913(4) 0.3167(2) 0.0707(13) Uani 1 1 d . . . C17 C -0.0027(4) 0.7594(4) 0.2897(2) 0.0667(11) Uani 1 1 d . . . C18 C 0.0326(3) 0.6391(4) 0.2984(2) 0.0541(10) Uani 1 1 d . . . C19 C 0.0188(3) 0.1792(4) 0.2200(2) 0.0640(11) Uani 1 1 d . . . H19A H 0.0274 0.1356 0.2669 0.077 Uiso 1 1 calc R . . H19B H -0.0532 0.1782 0.2052 0.077 Uiso 1 1 calc R . . C20 C 0.0721(4) 0.1041(4) 0.1650(2) 0.0995(17) Uani 1 1 d . . . H20A H 0.0449 0.0200 0.1626 0.149 Uiso 1 1 calc R . . H20B H 0.1433 0.1007 0.1795 0.149 Uiso 1 1 calc R . . H20C H 0.0623 0.1433 0.1175 0.149 Uiso 1 1 calc R . . C21 C -0.0173(4) 0.4392(4) 0.1682(2) 0.0605(12) Uani 1 1 d . . . C22 C -0.0398(3) 0.3871(4) 0.0917(2) 0.0820(14) Uani 1 1 d . . . H22A H -0.0793 0.4472 0.0625 0.123 Uiso 1 1 calc R . . H22B H -0.0772 0.3097 0.0944 0.123 Uiso 1 1 calc R . . H22C H 0.0228 0.3712 0.0693 0.123 Uiso 1 1 calc R . . C23 C 0.1903(3) 0.3578(6) 0.2143(2) 0.0656(12) Uani 1 1 d . . . C24 C 0.2174(3) 0.3766(5) 0.1363(2) 0.0919(16) Uani 1 1 d . . . H24A H 0.2898 0.3825 0.1350 0.138 Uiso 1 1 calc R . . H24B H 0.1866 0.4530 0.1172 0.138 Uiso 1 1 calc R . . H24C H 0.1930 0.3063 0.1069 0.138 Uiso 1 1 calc R . . H21A H -0.077(3) 0.449(3) 0.1882(18) 0.054(11) Uiso 1 1 d . . . H23A H 0.218(3) 0.281(4) 0.230(2) 0.106(18) Uiso 1 1 d . . . H21B H 0.021(3) 0.524(4) 0.164(2) 0.102(16) Uiso 1 1 d . . . H23B H 0.216(4) 0.425(5) 0.245(3) 0.12(2) 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 0.0493(6) 0.0512(6) 0.0418(5) -0.0008(5) 0.0056(4) 0.0069(5) B1 0.045(2) 0.049(2) 0.036(2) -0.0052(19) 0.0054(19) 0.001(2) F1 0.0697(15) 0.0935(17) 0.0486(13) 0.0141(12) -0.0056(11) -0.0146(13) F2 0.1008(19) 0.0838(17) 0.0645(16) 0.0186(13) 0.0195(14) -0.0074(14) F3 0.114(2) 0.112(2) 0.106(2) 0.0060(17) 0.0281(17) -0.0601(18) F4 0.0737(18) 0.154(3) 0.101(2) -0.0004(19) -0.0089(15) -0.0580(18) F5 0.0582(14) 0.1020(18) 0.0563(14) 0.0054(13) -0.0077(11) -0.0103(13) F6 0.0737(15) 0.0523(13) 0.0751(15) -0.0061(12) -0.0114(12) 0.0102(11) F7 0.0767(17) 0.0853(18) 0.114(2) 0.0100(16) -0.0200(15) 0.0273(14) F8 0.0643(16) 0.107(2) 0.124(2) 0.0260(17) -0.0369(15) -0.0145(15) F9 0.0823(17) 0.0831(17) 0.0760(16) -0.0050(14) -0.0160(13) -0.0303(14) F10 0.0712(15) 0.0654(15) 0.0718(15) -0.0198(12) -0.0040(12) 0.0015(12) F11 0.0713(16) 0.0822(17) 0.0789(16) 0.0048(13) 0.0332(13) 0.0165(13) F12 0.090(2) 0.107(2) 0.107(2) -0.0126(16) 0.0189(16) 0.0475(16) F13 0.131(2) 0.0613(17) 0.142(3) -0.0050(16) -0.0179(19) 0.0382(16) F14 0.115(2) 0.0591(16) 0.137(2) 0.0317(16) 0.0031(18) -0.0099(16) F15 0.0654(15) 0.0635(14) 0.0907(17) 0.0086(13) 0.0209(13) -0.0086(12) C1 0.047(2) 0.047(2) 0.040(2) -0.0061(17) 0.0024(17) 0.0018(17) C2 0.058(3) 0.054(2) 0.044(2) -0.0079(19) 0.005(2) -0.004(2) C3 0.076(3) 0.055(3) 0.046(2) 0.002(2) 0.015(2) -0.004(2) C4 0.076(3) 0.066(3) 0.071(3) -0.002(2) 0.022(3) -0.033(2) C5 0.058(3) 0.079(3) 0.067(3) -0.009(3) 0.006(2) -0.026(2) C6 0.059(3) 0.061(3) 0.043(2) -0.004(2) 0.006(2) -0.005(2) C7 0.047(2) 0.046(2) 0.039(2) -0.0024(17) 0.0061(17) -0.0050(18) C8 0.059(3) 0.051(2) 0.046(2) 0.0015(19) -0.0019(19) 0.001(2) C9 0.056(3) 0.063(3) 0.067(3) 0.016(2) -0.004(2) 0.008(2) C10 0.046(3) 0.081(3) 0.067(3) 0.020(3) -0.011(2) -0.009(2) C11 0.060(3) 0.067(3) 0.047(2) 0.004(2) -0.003(2) -0.018(2) C12 0.052(2) 0.055(3) 0.047(2) 0.0029(19) 0.0052(19) -0.001(2) C13 0.047(2) 0.050(2) 0.040(2) -0.0068(17) 0.0037(17) -0.0027(18) C14 0.058(3) 0.057(3) 0.044(2) -0.003(2) 0.0077(19) 0.002(2) C15 0.065(3) 0.070(3) 0.061(3) -0.012(2) 0.000(2) 0.025(2) C16 0.090(4) 0.046(3) 0.074(3) -0.008(2) -0.015(3) 0.019(3) C17 0.080(3) 0.045(3) 0.074(3) 0.002(2) -0.002(2) 0.002(3) C18 0.053(2) 0.054(3) 0.055(2) -0.004(2) 0.0037(19) 0.001(2) C19 0.077(3) 0.058(3) 0.056(3) -0.008(2) 0.000(2) -0.001(2) C20 0.164(5) 0.063(3) 0.074(3) -0.009(3) 0.020(3) 0.019(3) C21 0.057(3) 0.075(3) 0.050(3) 0.001(2) 0.007(2) 0.015(2) C22 0.087(3) 0.101(4) 0.056(3) 0.000(3) -0.008(2) 0.016(3) C23 0.059(3) 0.077(3) 0.063(3) -0.007(3) 0.018(2) 0.010(3) C24 0.069(3) 0.130(4) 0.079(3) 0.016(3) 0.029(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C19 1.818(4) . ? P1 C21 1.822(4) . ? P1 C23 1.837(4) . ? P1 B1 2.081(4) . ? B1 C7 1.634(5) . ? B1 C1 1.641(5) . ? B1 C13 1.650(5) . ? F1 C2 1.351(4) . ? F2 C3 1.345(4) . ? F3 C4 1.330(4) . ? F4 C5 1.340(4) . ? F5 C6 1.355(4) . ? F6 C8 1.354(4) . ? F7 C9 1.347(4) . ? F8 C10 1.345(4) . ? F9 C11 1.344(4) . ? F10 C12 1.352(4) . ? F11 C14 1.350(4) . ? F12 C15 1.345(4) . ? F13 C16 1.342(4) . ? F14 C17 1.345(5) . ? F15 C18 1.364(4) . ? C1 C2 1.382(5) . ? C1 C6 1.394(5) . ? C2 C3 1.384(5) . ? C3 C4 1.355(5) . ? C4 C5 1.369(6) . ? C5 C6 1.367(5) . ? C7 C8 1.380(5) . ? C7 C12 1.386(5) . ? C8 C9 1.366(5) . ? C9 C10 1.364(5) . ? C10 C11 1.363(5) . ? C11 C12 1.380(5) . ? C13 C14 1.378(5) . ? C13 C18 1.387(5) . ? C14 C15 1.378(5) . ? C15 C16 1.354(6) . ? C16 C17 1.358(6) . ? C17 C18 1.362(5) . ? C19 C20 1.492(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.509(5) . ? C21 H21A 0.89(3) . ? C21 H21B 1.04(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.502(6) . ? C23 H23A 0.93(4) . ? C23 H23B 0.95(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 P1 C21 107.7(2) . . ? C19 P1 C23 108.0(2) . . ? C21 P1 C23 107.0(2) . . ? C19 P1 B1 111.80(17) . . ? C21 P1 B1 111.19(18) . . ? C23 P1 B1 110.97(19) . . ? C7 B1 C1 111.7(3) . . ? C7 B1 C13 113.4(3) . . ? C1 B1 C13 112.9(3) . . ? C7 B1 P1 106.4(2) . . ? C1 B1 P1 107.0(2) . . ? C13 B1 P1 104.9(2) . . ? C2 C1 C6 112.0(3) . . ? C2 C1 B1 126.0(3) . . ? C6 C1 B1 122.0(3) . . ? F1 C2 C1 121.1(3) . . ? F1 C2 C3 114.3(3) . . ? C1 C2 C3 124.6(4) . . ? F2 C3 C4 120.1(4) . . ? F2 C3 C2 119.9(4) . . ? C4 C3 C2 120.0(4) . . ? F3 C4 C3 120.5(4) . . ? F3 C4 C5 120.9(4) . . ? C3 C4 C5 118.6(4) . . ? F4 C5 C6 120.5(4) . . ? F4 C5 C4 119.8(4) . . ? C6 C5 C4 119.7(4) . . ? F5 C6 C5 116.7(4) . . ? F5 C6 C1 118.2(3) . . ? C5 C6 C1 125.1(4) . . ? C8 C7 C12 112.7(3) . . ? C8 C7 B1 121.8(3) . . ? C12 C7 B1 125.5(3) . . ? F6 C8 C9 116.2(4) . . ? F6 C8 C7 118.6(3) . . ? C9 C8 C7 125.2(4) . . ? F7 C9 C10 119.7(4) . . ? F7 C9 C8 121.1(4) . . ? C10 C9 C8 119.2(4) . . ? F8 C10 C11 120.1(4) . . ? F8 C10 C9 120.7(4) . . ? C11 C10 C9 119.2(4) . . ? F9 C11 C10 120.3(4) . . ? F9 C11 C12 120.3(4) . . ? C10 C11 C12 119.4(4) . . ? F10 C12 C11 114.6(3) . . ? F10 C12 C7 121.2(3) . . ? C11 C12 C7 124.2(4) . . ? C14 C13 C18 112.2(3) . . ? C14 C13 B1 126.9(3) . . ? C18 C13 B1 120.8(3) . . ? F11 C14 C15 115.0(4) . . ? F11 C14 C13 120.8(3) . . ? C15 C14 C13 124.2(4) . . ? F12 C15 C16 120.3(4) . . ? F12 C15 C14 119.7(4) . . ? C16 C15 C14 120.1(4) . . ? F13 C16 C15 120.6(5) . . ? F13 C16 C17 120.5(5) . . ? C15 C16 C17 118.9(4) . . ? F14 C17 C16 120.4(4) . . ? F14 C17 C18 120.2(4) . . ? C16 C17 C18 119.3(4) . . ? C17 C18 F15 116.1(4) . . ? C17 C18 C13 125.3(4) . . ? F15 C18 C13 118.6(3) . . ? C20 C19 P1 118.2(3) . . ? C20 C19 H19A 107.8 . . ? P1 C19 H19A 107.8 . . ? C20 C19 H19B 107.8 . . ? P1 C19 H19B 107.8 . . ? H19A C19 H19B 107.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P1 118.4(3) . . ? C22 C21 H21A 107(2) . . ? P1 C21 H21A 104(2) . . ? C22 C21 H21B 109(2) . . ? P1 C21 H21B 107(2) . . ? H21A C21 H21B 112(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P1 120.0(3) . . ? C24 C23 H23A 108(3) . . ? P1 C23 H23A 103(3) . . ? C24 C23 H23B 111(3) . . ? P1 C23 H23B 105(3) . . ? H23A C23 H23B 111(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 C19 P1 B1 C7 103.5(3) . . . . ? C21 P1 B1 C7 -136.1(3) . . . . ? C23 P1 B1 C7 -17.1(3) . . . . ? C19 P1 B1 C1 -15.9(3) . . . . ? C21 P1 B1 C1 104.5(3) . . . . ? C23 P1 B1 C1 -136.6(3) . . . . ? C19 P1 B1 C13 -136.1(2) . . . . ? C21 P1 B1 C13 -15.7(3) . . . . ? C23 P1 B1 C13 103.3(3) . . . . ? C7 B1 C1 C2 12.5(5) . . . . ? C13 B1 C1 C2 -116.6(4) . . . . ? P1 B1 C1 C2 128.5(3) . . . . ? C7 B1 C1 C6 -169.4(3) . . . . ? C13 B1 C1 C6 61.5(4) . . . . ? P1 B1 C1 C6 -53.4(4) . . . . ? C6 C1 C2 F1 -177.1(3) . . . . ? B1 C1 C2 F1 1.2(5) . . . . ? C6 C1 C2 C3 1.1(5) . . . . ? B1 C1 C2 C3 179.4(3) . . . . ? F1 C2 C3 F2 -0.8(5) . . . . ? C1 C2 C3 F2 -179.0(3) . . . . ? F1 C2 C3 C4 177.8(4) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? F2 C3 C4 F3 -1.1(6) . . . . ? C2 C3 C4 F3 -179.7(4) . . . . ? F2 C3 C4 C5 177.9(4) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? F3 C4 C5 F4 0.0(6) . . . . ? C3 C4 C5 F4 -179.0(4) . . . . ? F3 C4 C5 C6 -179.9(4) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? F4 C5 C6 F5 1.6(6) . . . . ? C4 C5 C6 F5 -178.5(4) . . . . ? F4 C5 C6 C1 179.7(4) . . . . ? C4 C5 C6 C1 -0.4(6) . . . . ? C2 C1 C6 F5 177.5(3) . . . . ? B1 C1 C6 F5 -0.9(5) . . . . ? C2 C1 C6 C5 -0.7(5) . . . . ? B1 C1 C6 C5 -179.0(4) . . . . ? C1 B1 C7 C8 63.5(4) . . . . ? C13 B1 C7 C8 -167.6(3) . . . . ? P1 B1 C7 C8 -52.8(4) . . . . ? C1 B1 C7 C12 -112.7(4) . . . . ? C13 B1 C7 C12 16.2(5) . . . . ? P1 B1 C7 C12 131.0(3) . . . . ? C12 C7 C8 F6 176.0(3) . . . . ? B1 C7 C8 F6 -0.7(5) . . . . ? C12 C7 C8 C9 -2.2(5) . . . . ? B1 C7 C8 C9 -178.9(4) . . . . ? F6 C8 C9 F7 3.3(5) . . . . ? C7 C8 C9 F7 -178.5(3) . . . . ? F6 C8 C9 C10 -177.4(3) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? F7 C9 C10 F8 -0.1(6) . . . . ? C8 C9 C10 F8 -179.4(3) . . . . ? F7 C9 C10 C11 -179.4(4) . . . . ? C8 C9 C10 C11 1.3(6) . . . . ? F8 C10 C11 F9 -0.3(6) . . . . ? C9 C10 C11 F9 179.0(3) . . . . ? F8 C10 C11 C12 178.9(3) . . . . ? C9 C10 C11 C12 -1.8(6) . . . . ? F9 C11 C12 F10 -2.1(5) . . . . ? C10 C11 C12 F10 178.7(3) . . . . ? F9 C11 C12 C7 179.4(3) . . . . ? C10 C11 C12 C7 0.3(6) . . . . ? C8 C7 C12 F10 -176.7(3) . . . . ? B1 C7 C12 F10 -0.2(5) . . . . ? C8 C7 C12 C11 1.6(5) . . . . ? B1 C7 C12 C11 178.1(3) . . . . ? C7 B1 C13 C14 -119.4(4) . . . . ? C1 B1 C13 C14 8.8(5) . . . . ? P1 B1 C13 C14 124.9(3) . . . . ? C7 B1 C13 C18 57.5(4) . . . . ? C1 B1 C13 C18 -174.3(3) . . . . ? P1 B1 C13 C18 -58.2(4) . . . . ? C18 C13 C14 F11 -177.0(3) . . . . ? B1 C13 C14 F11 0.2(5) . . . . ? C18 C13 C14 C15 1.6(5) . . . . ? B1 C13 C14 C15 178.8(4) . . . . ? F11 C14 C15 F12 -1.2(5) . . . . ? C13 C14 C15 F12 -179.8(3) . . . . ? F11 C14 C15 C16 177.4(3) . . . . ? C13 C14 C15 C16 -1.3(6) . . . . ? F12 C15 C16 F13 -1.4(6) . . . . ? C14 C15 C16 F13 180.0(4) . . . . ? F12 C15 C16 C17 178.7(4) . . . . ? C14 C15 C16 C17 0.2(6) . . . . ? F13 C16 C17 F14 0.3(6) . . . . ? C15 C16 C17 F14 -179.9(4) . . . . ? F13 C16 C17 C18 -179.5(4) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? F14 C17 C18 F15 1.8(6) . . . . ? C16 C17 C18 F15 -178.5(3) . . . . ? F14 C17 C18 C13 -179.6(3) . . . . ? C16 C17 C18 C13 0.2(6) . . . . ? C14 C13 C18 C17 -1.1(5) . . . . ? B1 C13 C18 C17 -178.5(4) . . . . ? C14 C13 C18 F15 177.5(3) . . . . ? B1 C13 C18 F15 0.2(5) . . . . ? C21 P1 C19 C20 87.3(4) . . . . ? C23 P1 C19 C20 -27.9(4) . . . . ? B1 P1 C19 C20 -150.2(3) . . . . ? C19 P1 C21 C22 -37.2(4) . . . . ? C23 P1 C21 C22 78.7(4) . . . . ? B1 P1 C21 C22 -160.0(3) . . . . ? C19 P1 C23 C24 83.7(5) . . . . ? C21 P1 C23 C24 -32.0(5) . . . . ? B1 P1 C23 C24 -153.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.330 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.045 #===end data_Et3P-C4H8O-B(C6F5)3 _database_code_depnum_ccdc_archive 'CCDC 698995' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H23 B F15 O P' _chemical_formula_weight 702.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.3288(17) _cell_length_b 12.082(2) _cell_length_c 13.083(2) _cell_angle_alpha 94.234(2) _cell_angle_beta 105.527(2) _cell_angle_gamma 106.696(2) _cell_volume 1486.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3597 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.14 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9209 _exptl_absorpt_correction_T_max 0.9593 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 14171 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5216 _reflns_number_gt 2245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.1173P)^2^+1.0096P] 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 5216 _refine_ls_number_parameters 409 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1615 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2591 _refine_ls_wR_factor_gt 0.1973 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.011 _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 0.3143(2) 0.72348(16) 0.24329(14) 0.0903(6) Uani 1 1 d . . . F1 F 0.6177(4) 0.5920(3) 0.7910(4) 0.1152(13) Uani 1 1 d . . . F2 F 0.8485(5) 0.6670(4) 0.9577(4) 0.1446(18) Uani 1 1 d . . . F3 F 0.9204(5) 0.8788(5) 1.0790(4) 0.170(2) Uani 1 1 d . . . F4 F 0.7460(5) 1.0123(5) 1.0313(4) 0.156(2) Uani 1 1 d . . . F5 F 0.5140(4) 0.9385(3) 0.8698(3) 0.0999(11) Uani 1 1 d . . . F6 F 0.2306(4) 0.7018(3) 0.8377(3) 0.1062(12) Uani 1 1 d . . . F7 F 0.0255(5) 0.7963(4) 0.8226(4) 0.1426(18) Uani 1 1 d . . . F8 F -0.0113(4) 0.9480(4) 0.6842(4) 0.1484(18) Uani 1 1 d . . . F9 F 0.1624(5) 1.0006(4) 0.5596(4) 0.1489(18) Uani 1 1 d . . . F10 F 0.3604(4) 0.9040(3) 0.5688(3) 0.1137(13) Uani 1 1 d . . . F11 F 0.3830(4) 0.5365(3) 0.8602(3) 0.1004(11) Uani 1 1 d . . . F12 F 0.2122(5) 0.3183(4) 0.8042(4) 0.1407(17) Uani 1 1 d . . . F13 F 0.0483(5) 0.2326(4) 0.5994(4) 0.1505(19) Uani 1 1 d . . . F14 F 0.0535(4) 0.3771(4) 0.4497(4) 0.1316(16) Uani 1 1 d . . . F15 F 0.2168(4) 0.5961(3) 0.5039(3) 0.0970(11) Uani 1 1 d . . . B1 B 0.4180(7) 0.7190(5) 0.7052(5) 0.0634(16) Uani 1 1 d . . . C1 C 0.5489(6) 0.7588(5) 0.8203(4) 0.0670(14) Uani 1 1 d . . . C2 C 0.6422(7) 0.6958(6) 0.8498(5) 0.0816(17) Uani 1 1 d . . . C3 C 0.7641(8) 0.7336(8) 0.9340(7) 0.101(2) Uani 1 1 d . . . C4 C 0.8019(8) 0.8380(10) 0.9957(6) 0.113(3) Uani 1 1 d . . . C5 C 0.7128(9) 0.9067(7) 0.9721(6) 0.104(2) Uani 1 1 d . . . C6 C 0.5903(6) 0.8645(6) 0.8863(5) 0.0754(16) Uani 1 1 d . . . C7 C 0.3042(5) 0.7922(4) 0.7009(4) 0.0632(14) Uani 1 1 d . . . C8 C 0.2151(6) 0.7738(5) 0.7642(5) 0.0759(16) Uani 1 1 d . . . C9 C 0.1095(7) 0.8237(6) 0.7593(6) 0.091(2) Uani 1 1 d . . . C10 C 0.0912(7) 0.8991(7) 0.6905(7) 0.097(2) Uani 1 1 d . . . C11 C 0.1773(8) 0.9244(6) 0.6276(6) 0.095(2) Uani 1 1 d . . . C12 C 0.2801(6) 0.8716(5) 0.6338(5) 0.0784(16) Uani 1 1 d . . . C13 C 0.3163(6) 0.5789(5) 0.6833(5) 0.0660(14) Uani 1 1 d . . . C14 C 0.3062(7) 0.5020(6) 0.7555(6) 0.0783(16) Uani 1 1 d . . . C15 C 0.2173(8) 0.3866(6) 0.7293(7) 0.091(2) Uani 1 1 d . . . C16 C 0.1331(8) 0.3453(6) 0.6254(9) 0.102(2) Uani 1 1 d . . . C17 C 0.1362(7) 0.4175(7) 0.5517(7) 0.0887(19) Uani 1 1 d . . . C18 C 0.2242(6) 0.5302(5) 0.5808(5) 0.0710(15) Uani 1 1 d . . . C19A C 0.5856(14) 0.7065(12) 0.6106(9) 0.089(4) Uiso 0.50 1 d PD . . C19B C 0.5968(13) 0.7950(10) 0.6083(8) 0.076(3) Uiso 0.50 1 d PD . . C20 C 0.6429(7) 0.7451(7) 0.5189(5) 0.100(2) Uani 1 1 d D . . C21 C 0.5257(12) 0.6909(10) 0.4100(7) 0.175(4) Uani 1 1 d D . . H21A H 0.5685 0.6700 0.3570 0.210 Uiso 1 1 calc R . . H21B H 0.4589 0.6199 0.4186 0.210 Uiso 1 1 calc R . . C22 C 0.4505(10) 0.7716(8) 0.3714(8) 0.151(3) Uiso 1 1 d D . . H22A H 0.5196 0.8435 0.3671 0.181 Uiso 1 1 calc R . . H22B H 0.4074 0.7906 0.4249 0.181 Uiso 1 1 calc R . . C23 C 0.3812(13) 0.6829(12) 0.1366(8) 0.188(5) Uani 1 1 d . . . H23A H 0.4066 0.6131 0.1514 0.225 Uiso 1 1 calc R . . H23B H 0.3024 0.6601 0.0708 0.225 Uiso 1 1 calc R . . C24 C 0.4882(15) 0.7555(14) 0.1158(10) 0.229(7) Uani 1 1 d . . . H24A H 0.5078 0.7185 0.0567 0.344 Uiso 1 1 calc R . . H24B H 0.5701 0.7769 0.1781 0.344 Uiso 1 1 calc R . . H24C H 0.4653 0.8244 0.0971 0.344 Uiso 1 1 calc R . . C25 C 0.2606(14) 0.8450(10) 0.2137(11) 0.196(5) Uani 1 1 d . . . H25A H 0.3415 0.9038 0.2046 0.235 Uiso 1 1 calc R . . H25B H 0.1888 0.8213 0.1440 0.235 Uiso 1 1 calc R . . C26 C 0.1722(11) 0.5968(11) 0.2477(8) 0.174(4) Uani 1 1 d . . . H26A H 0.2108 0.5333 0.2629 0.209 Uiso 1 1 calc R . . H26B H 0.1387 0.6154 0.3073 0.209 Uiso 1 1 calc R . . C27 C 0.2094(14) 0.8990(12) 0.2791(10) 0.223(7) Uani 1 1 d . . . H27A H 0.1852 0.9629 0.2485 0.334 Uiso 1 1 calc R . . H27B H 0.2800 0.9284 0.3479 0.334 Uiso 1 1 calc R . . H27C H 0.1264 0.8443 0.2877 0.334 Uiso 1 1 calc R . . C28 C 0.0546(12) 0.5562(11) 0.1538(10) 0.210(5) Uani 1 1 d . . . H28A H -0.0143 0.4890 0.1643 0.315 Uiso 1 1 calc R . . H28B H 0.0853 0.5349 0.0943 0.315 Uiso 1 1 calc R . . H28C H 0.0129 0.6170 0.1389 0.315 Uiso 1 1 calc R . . O1 O 0.4774(4) 0.7355(4) 0.6183(3) 0.0839(12) Uani 1 1 d . . . H19A H 0.6635 0.7397 0.6786 0.101 Uiso 0.50 1 d P . . H19B H 0.5649 0.6233 0.6050 0.101 Uiso 0.50 1 d P . . H19C H 0.5953 0.8730 0.5979 0.101 Uiso 0.50 1 d P . . H19D H 0.6706 0.8054 0.6766 0.101 Uiso 0.50 1 d P . . H20A H 0.7274 0.7220 0.5217 0.101 Uiso 0.50 1 d P . . H20B H 0.6753 0.8303 0.5272 0.101 Uiso 0.50 1 d P . . H20C H 0.6874 0.6879 0.5451 0.101 Uiso 0.50 1 d P . . H20D H 0.7194 0.8082 0.5067 0.101 Uiso 0.50 1 d P . . 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 0.0882(13) 0.1010(13) 0.0836(12) 0.0146(10) 0.0217(10) 0.0371(11) F1 0.092(3) 0.092(3) 0.164(4) 0.016(3) 0.024(3) 0.047(2) F2 0.105(3) 0.181(4) 0.162(4) 0.071(4) 0.019(3) 0.075(3) F3 0.119(4) 0.224(5) 0.114(3) 0.034(3) -0.029(3) 0.031(4) F4 0.154(4) 0.151(4) 0.101(3) -0.042(3) -0.015(3) 0.020(3) F5 0.097(3) 0.082(2) 0.102(3) -0.0166(19) 0.007(2) 0.030(2) F6 0.129(3) 0.099(3) 0.120(3) 0.028(2) 0.080(3) 0.039(2) F7 0.115(3) 0.127(3) 0.207(5) -0.012(3) 0.107(3) 0.027(3) F8 0.089(3) 0.140(4) 0.218(5) -0.019(3) 0.028(3) 0.068(3) F9 0.155(4) 0.142(4) 0.185(5) 0.063(4) 0.043(3) 0.100(3) F10 0.132(3) 0.126(3) 0.132(3) 0.070(3) 0.069(3) 0.076(3) F11 0.113(3) 0.095(2) 0.097(3) 0.038(2) 0.038(2) 0.028(2) F12 0.143(4) 0.096(3) 0.206(5) 0.071(3) 0.086(4) 0.030(3) F13 0.120(3) 0.076(3) 0.229(5) -0.015(3) 0.062(4) -0.007(2) F14 0.101(3) 0.120(3) 0.134(4) -0.043(3) 0.011(3) 0.014(2) F15 0.096(3) 0.104(3) 0.077(2) 0.003(2) 0.0151(19) 0.024(2) B1 0.065(4) 0.058(4) 0.072(4) 0.013(3) 0.026(3) 0.020(3) C1 0.067(4) 0.059(3) 0.074(4) 0.013(3) 0.024(3) 0.014(3) C2 0.072(4) 0.077(4) 0.092(5) 0.021(4) 0.019(4) 0.022(4) C3 0.079(5) 0.122(6) 0.102(6) 0.044(5) 0.015(5) 0.037(5) C4 0.079(5) 0.147(8) 0.078(5) 0.033(5) -0.006(4) 0.010(6) C5 0.101(6) 0.109(6) 0.070(5) -0.004(4) 0.007(4) 0.009(5) C6 0.068(4) 0.086(4) 0.069(4) 0.013(4) 0.017(3) 0.023(4) C7 0.055(3) 0.056(3) 0.072(4) -0.002(3) 0.018(3) 0.012(3) C8 0.075(4) 0.064(4) 0.093(4) 0.003(3) 0.038(4) 0.020(3) C9 0.061(4) 0.081(5) 0.119(6) -0.024(4) 0.037(4) 0.006(4) C10 0.061(4) 0.085(5) 0.132(7) -0.013(5) 0.010(4) 0.027(4) C11 0.087(5) 0.081(5) 0.114(6) 0.014(4) 0.013(4) 0.039(4) C12 0.071(4) 0.077(4) 0.091(5) 0.011(4) 0.022(4) 0.032(3) C13 0.066(4) 0.058(3) 0.078(4) 0.005(3) 0.028(3) 0.021(3) C14 0.079(4) 0.075(4) 0.084(5) 0.010(4) 0.029(4) 0.026(4) C15 0.085(5) 0.064(5) 0.143(7) 0.035(5) 0.056(5) 0.026(4) C16 0.078(5) 0.062(5) 0.162(8) -0.008(5) 0.053(6) 0.008(4) C17 0.072(4) 0.079(5) 0.102(6) -0.018(5) 0.023(4) 0.016(4) C18 0.071(4) 0.065(4) 0.079(4) 0.003(3) 0.025(3) 0.025(3) C20 0.073(4) 0.159(7) 0.066(4) 0.012(4) 0.022(3) 0.037(4) C21 0.234(12) 0.252(12) 0.117(7) 0.038(8) 0.105(8) 0.145(11) C23 0.181(11) 0.250(14) 0.137(8) 0.053(8) 0.075(8) 0.045(10) C24 0.223(14) 0.35(2) 0.202(12) 0.152(13) 0.134(12) 0.131(14) C25 0.191(11) 0.173(10) 0.259(14) 0.054(10) 0.083(11) 0.095(9) C26 0.141(9) 0.243(13) 0.119(7) 0.041(8) 0.016(7) 0.051(9) C27 0.225(13) 0.301(17) 0.215(13) 0.019(11) 0.073(10) 0.193(13) C28 0.137(9) 0.225(12) 0.216(13) -0.043(10) 0.044(9) 0.009(9) O1 0.060(2) 0.130(3) 0.078(3) 0.035(2) 0.033(2) 0.040(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C25 1.746(11) . ? P1 C22 1.803(9) . ? P1 C26 1.808(11) . ? P1 C23 1.810(11) . ? F1 C2 1.341(7) . ? F2 C3 1.341(8) . ? F3 C4 1.337(8) . ? F4 C5 1.344(8) . ? F5 C6 1.345(7) . ? F6 C8 1.352(7) . ? F7 C9 1.345(7) . ? F8 C10 1.340(7) . ? F9 C11 1.338(8) . ? F10 C12 1.344(7) . ? F11 C14 1.351(7) . ? F12 C15 1.329(7) . ? F13 C16 1.350(7) . ? F14 C17 1.342(8) . ? F15 C18 1.328(6) . ? B1 O1 1.431(7) . ? B1 C7 1.655(8) . ? B1 C1 1.659(8) . ? B1 C13 1.673(8) . ? C1 C6 1.374(8) . ? C1 C2 1.387(8) . ? C2 C3 1.364(9) . ? C3 C4 1.339(11) . ? C4 C5 1.398(11) . ? C5 C6 1.380(9) . ? C7 C8 1.377(8) . ? C7 C12 1.378(8) . ? C8 C9 1.379(9) . ? C9 C10 1.344(10) . ? C10 C11 1.354(10) . ? C11 C12 1.376(8) . ? C13 C14 1.375(8) . ? C13 C18 1.389(8) . ? C14 C15 1.389(9) . ? C15 C16 1.368(10) . ? C16 C17 1.349(10) . ? C17 C18 1.360(9) . ? C19A C19B 1.046(14) . ? C19A O1 1.289(13) . ? C19A C20 1.521(8) . ? C19A H19A 0.990(13) . ? C19A H19B 0.959(13) . ? C19A H19D 1.335(13) . ? C19A H20C 1.575(11) . ? C19B O1 1.283(12) . ? C19B C20 1.523(8) . ? C19B H19A 1.336(12) . ? C19B H19C 0.966(12) . ? C19B H19D 0.979(11) . ? C19B H20B 1.514(10) . ? C20 C21 1.552(12) . ? C20 H20A 0.982(6) . ? C20 H20B 0.975(8) . ? C20 H20C 0.969(7) . ? C20 H20D 0.985(7) . ? C21 C22 1.452(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.305(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C27 1.340(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C28 1.413(12) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C25 P1 C22 105.6(6) . . ? C25 P1 C26 113.8(6) . . ? C22 P1 C26 111.0(5) . . ? C25 P1 C23 107.1(6) . . ? C22 P1 C23 112.2(5) . . ? C26 P1 C23 107.1(6) . . ? O1 B1 C7 110.9(5) . . ? O1 B1 C1 108.9(4) . . ? C7 B1 C1 112.1(4) . . ? O1 B1 C13 107.2(4) . . ? C7 B1 C13 103.5(4) . . ? C1 B1 C13 114.2(4) . . ? C6 C1 C2 112.9(6) . . ? C6 C1 B1 124.2(5) . . ? C2 C1 B1 122.1(5) . . ? F1 C2 C3 115.6(7) . . ? F1 C2 C1 119.7(6) . . ? C3 C2 C1 124.6(7) . . ? C4 C3 F2 118.3(8) . . ? C4 C3 C2 120.7(7) . . ? F2 C3 C2 121.0(8) . . ? F3 C4 C3 122.8(9) . . ? F3 C4 C5 118.8(9) . . ? C3 C4 C5 118.4(7) . . ? F4 C5 C6 120.4(8) . . ? F4 C5 C4 120.7(8) . . ? C6 C5 C4 118.8(7) . . ? F5 C6 C1 121.6(5) . . ? F5 C6 C5 113.8(6) . . ? C1 C6 C5 124.6(7) . . ? C8 C7 C12 111.9(5) . . ? C8 C7 B1 121.5(5) . . ? C12 C7 B1 126.6(5) . . ? F6 C8 C7 118.6(5) . . ? F6 C8 C9 116.2(6) . . ? C7 C8 C9 125.2(6) . . ? C10 C9 F7 120.6(7) . . ? C10 C9 C8 119.4(7) . . ? F7 C9 C8 120.1(8) . . ? F8 C10 C9 120.2(8) . . ? F8 C10 C11 120.7(8) . . ? C9 C10 C11 119.1(7) . . ? F9 C11 C10 120.1(7) . . ? F9 C11 C12 120.1(8) . . ? C10 C11 C12 119.8(7) . . ? F10 C12 C11 114.8(6) . . ? F10 C12 C7 120.5(5) . . ? C11 C12 C7 124.7(7) . . ? C14 C13 C18 112.8(6) . . ? C14 C13 B1 128.6(5) . . ? C18 C13 B1 118.5(5) . . ? F11 C14 C13 120.8(6) . . ? F11 C14 C15 114.9(6) . . ? C13 C14 C15 124.3(7) . . ? F12 C15 C16 120.6(7) . . ? F12 C15 C14 120.6(8) . . ? C16 C15 C14 118.8(7) . . ? C17 C16 F13 121.6(9) . . ? C17 C16 C15 119.5(7) . . ? F13 C16 C15 118.9(9) . . ? F14 C17 C16 119.6(7) . . ? F14 C17 C18 120.5(8) . . ? C16 C17 C18 119.9(7) . . ? F15 C18 C17 115.8(6) . . ? F15 C18 C13 119.5(5) . . ? C17 C18 C13 124.7(6) . . ? C19B C19A O1 65.7(10) . . ? C19B C19A C20 70.0(7) . . ? O1 C19A C20 116.5(9) . . ? C19B C19A H19A 82.0(12) . . ? O1 C19A H19A 108.4(10) . . ? C20 C19A H19A 107.8(9) . . ? C19B C19A H19B 172.8(17) . . ? O1 C19A H19B 110.3(10) . . ? C20 C19A H19B 108.0(10) . . ? H19A C19A H19B 105.2(12) . . ? C19B C19A H19D 46.6(9) . . ? O1 C19A H19D 89.2(9) . . ? C20 C19A H19D 91.6(7) . . ? H19A C19A H19D 35.4(5) . . ? H19B C19A H19D 140.5(12) . . ? C19B C19A H20C 100.7(9) . . ? O1 C19A H20C 151.2(9) . . ? C20 C19A H20C 36.4(4) . . ? H19A C19A H20C 93.8(9) . . ? H19B C19A H20C 80.0(8) . . ? H19D C19A H20C 99.3(7) . . ? C19A C19B O1 66.3(10) . . ? C19A C19B C20 69.8(7) . . ? O1 C19B C20 116.8(8) . . ? C19A C19B H19A 47.2(9) . . ? O1 C19B H19A 90.2(8) . . ? C20 C19B H19A 91.5(6) . . ? C19A C19B H19C 172.1(16) . . ? O1 C19B H19C 109.1(9) . . ? C20 C19B H19C 108.3(9) . . ? H19A C19B H19C 140.6(11) . . ? C19A C19B H19D 82.4(12) . . ? O1 C19B H19D 108.4(9) . . ? C20 C19B H19D 108.3(9) . . ? H19A C19B H19D 35.3(4) . . ? H19C C19B H19D 105.4(11) . . ? C19A C19B H20B 106.2(8) . . ? O1 C19B H20B 143.7(9) . . ? C20 C19B H20B 37.5(4) . . ? H19A C19B H20B 110.8(7) . . ? H19C C19B H20B 73.4(7) . . ? H19D C19B H20B 105.5(9) . . ? C19A C20 C19B 40.2(6) . . ? C19A C20 C21 109.5(8) . . ? C19B C20 C21 116.3(7) . . ? C19A C20 H20A 110.4(8) . . ? C19B C20 H20A 130.7(7) . . ? C21 C20 H20A 110.8(6) . . ? C19A C20 H20B 109.9(7) . . ? C19B C20 H20B 70.8(6) . . ? C21 C20 H20B 110.8(7) . . ? H20A C20 H20B 105.4(6) . . ? C19A C20 H20C 74.8(7) . . ? C19B C20 H20C 108.3(7) . . ? C21 C20 H20C 110.1(7) . . ? H20A C20 H20C 38.9(3) . . ? H20B C20 H20C 133.9(7) . . ? C19A C20 H20D 139.0(8) . . ? C19B C20 H20D 107.9(7) . . ? C21 C20 H20D 108.8(6) . . ? H20A C20 H20D 67.8(4) . . ? H20B C20 H20D 41.2(3) . . ? H20C C20 H20D 104.7(6) . . ? C22 C21 C20 111.7(8) . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? C21 C22 P1 117.2(8) . . ? C21 C22 H22A 108.0 . . ? P1 C22 H22A 108.0 . . ? C21 C22 H22B 108.0 . . ? P1 C22 H22B 108.0 . . ? H22A C22 H22B 107.2 . . ? C24 C23 P1 121.7(11) . . ? C24 C23 H23A 106.9 . . ? P1 C23 H23A 106.9 . . ? C24 C23 H23B 106.9 . . ? P1 C23 H23B 106.9 . . ? H23A C23 H23B 106.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 P1 122.1(11) . . ? C27 C25 H25A 106.8 . . ? P1 C25 H25A 106.8 . . ? C27 C25 H25B 106.8 . . ? P1 C25 H25B 106.8 . . ? H25A C25 H25B 106.6 . . ? C28 C26 P1 116.0(8) . . ? C28 C26 H26A 108.3 . . ? P1 C26 H26A 108.3 . . ? C28 C26 H26B 108.3 . . ? P1 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19B O1 C19A 48.0(6) . . ? C19B O1 B1 135.5(6) . . ? C19A O1 B1 125.0(6) . . ? 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 O1 B1 C1 C6 100.4(6) . . . . ? C7 B1 C1 C6 -22.7(7) . . . . ? C13 B1 C1 C6 -139.9(5) . . . . ? O1 B1 C1 C2 -68.6(6) . . . . ? C7 B1 C1 C2 168.4(5) . . . . ? C13 B1 C1 C2 51.1(7) . . . . ? C6 C1 C2 F1 -178.2(5) . . . . ? B1 C1 C2 F1 -8.1(8) . . . . ? C6 C1 C2 C3 -1.0(9) . . . . ? B1 C1 C2 C3 169.0(6) . . . . ? F1 C2 C3 C4 177.4(7) . . . . ? C1 C2 C3 C4 0.2(11) . . . . ? F1 C2 C3 F2 -3.1(9) . . . . ? C1 C2 C3 F2 179.6(6) . . . . ? F2 C3 C4 F3 0.6(12) . . . . ? C2 C3 C4 F3 -179.9(6) . . . . ? F2 C3 C4 C5 -179.0(6) . . . . ? C2 C3 C4 C5 0.5(12) . . . . ? F3 C4 C5 F4 0.6(11) . . . . ? C3 C4 C5 F4 -179.8(7) . . . . ? F3 C4 C5 C6 -179.8(6) . . . . ? C3 C4 C5 C6 -0.3(11) . . . . ? C2 C1 C6 F5 179.3(5) . . . . ? B1 C1 C6 F5 9.4(8) . . . . ? C2 C1 C6 C5 1.3(9) . . . . ? B1 C1 C6 C5 -168.5(6) . . . . ? F4 C5 C6 F5 0.7(9) . . . . ? C4 C5 C6 F5 -178.8(6) . . . . ? F4 C5 C6 C1 178.8(6) . . . . ? C4 C5 C6 C1 -0.7(10) . . . . ? O1 B1 C7 C8 168.3(5) . . . . ? C1 B1 C7 C8 -69.8(6) . . . . ? C13 B1 C7 C8 53.7(6) . . . . ? O1 B1 C7 C12 -8.3(8) . . . . ? C1 B1 C7 C12 113.6(6) . . . . ? C13 B1 C7 C12 -122.9(6) . . . . ? C12 C7 C8 F6 -177.1(5) . . . . ? B1 C7 C8 F6 5.8(8) . . . . ? C12 C7 C8 C9 2.7(8) . . . . ? B1 C7 C8 C9 -174.4(5) . . . . ? F6 C8 C9 C10 177.9(6) . . . . ? C7 C8 C9 C10 -1.9(10) . . . . ? F6 C8 C9 F7 -2.5(8) . . . . ? C7 C8 C9 F7 177.7(5) . . . . ? F7 C9 C10 F8 0.0(10) . . . . ? C8 C9 C10 F8 179.7(5) . . . . ? F7 C9 C10 C11 -179.8(6) . . . . ? C8 C9 C10 C11 -0.1(10) . . . . ? F8 C10 C11 F9 1.2(10) . . . . ? C9 C10 C11 F9 -179.0(6) . . . . ? F8 C10 C11 C12 -178.8(6) . . . . ? C9 C10 C11 C12 1.0(10) . . . . ? F9 C11 C12 F10 0.7(9) . . . . ? C10 C11 C12 F10 -179.4(6) . . . . ? F9 C11 C12 C7 180.0(6) . . . . ? C10 C11 C12 C7 0.0(10) . . . . ? C8 C7 C12 F10 177.6(5) . . . . ? B1 C7 C12 F10 -5.5(9) . . . . ? C8 C7 C12 C11 -1.7(9) . . . . ? B1 C7 C12 C11 175.2(6) . . . . ? O1 B1 C13 C14 136.7(6) . . . . ? C7 B1 C13 C14 -106.1(6) . . . . ? C1 B1 C13 C14 16.0(8) . . . . ? O1 B1 C13 C18 -45.7(6) . . . . ? C7 B1 C13 C18 71.6(6) . . . . ? C1 B1 C13 C18 -166.3(5) . . . . ? C18 C13 C14 F11 -176.7(5) . . . . ? B1 C13 C14 F11 1.1(9) . . . . ? C18 C13 C14 C15 1.9(8) . . . . ? B1 C13 C14 C15 179.6(5) . . . . ? F11 C14 C15 F12 -0.3(8) . . . . ? C13 C14 C15 F12 -179.0(5) . . . . ? F11 C14 C15 C16 178.4(6) . . . . ? C13 C14 C15 C16 -0.3(9) . . . . ? F12 C15 C16 C17 177.5(6) . . . . ? C14 C15 C16 C17 -1.2(10) . . . . ? F12 C15 C16 F13 -2.4(10) . . . . ? C14 C15 C16 F13 178.9(5) . . . . ? F13 C16 C17 F14 -0.1(10) . . . . ? C15 C16 C17 F14 -179.9(6) . . . . ? F13 C16 C17 C18 -179.3(5) . . . . ? C15 C16 C17 C18 0.9(10) . . . . ? F14 C17 C18 F15 3.0(8) . . . . ? C16 C17 C18 F15 -177.8(6) . . . . ? F14 C17 C18 C13 -178.2(5) . . . . ? C16 C17 C18 C13 1.0(9) . . . . ? C14 C13 C18 F15 176.4(5) . . . . ? B1 C13 C18 F15 -1.6(7) . . . . ? C14 C13 C18 C17 -2.3(8) . . . . ? B1 C13 C18 C17 179.7(5) . . . . ? C20 C19A C19B O1 133.3(7) . . . . ? O1 C19A C19B C20 -133.3(7) . . . . ? O1 C19A C20 C19B 47.8(10) . . . . ? C19B C19A C20 C21 -108.0(11) . . . . ? O1 C19A C20 C21 -60.2(12) . . . . ? O1 C19B C20 C19A -48.3(10) . . . . ? C19A C19B C20 C21 89.6(12) . . . . ? O1 C19B C20 C21 41.3(13) . . . . ? C19A C20 C21 C22 95.9(10) . . . . ? C19B C20 C21 C22 52.7(11) . . . . ? C20 C21 C22 P1 178.1(6) . . . . ? C25 P1 C22 C21 -173.2(9) . . . . ? C26 P1 C22 C21 63.0(9) . . . . ? C23 P1 C22 C21 -56.8(10) . . . . ? C25 P1 C23 C24 59.7(13) . . . . ? C22 P1 C23 C24 -55.7(13) . . . . ? C26 P1 C23 C24 -177.8(11) . . . . ? C22 P1 C25 C27 -58.2(13) . . . . ? C26 P1 C25 C27 63.8(14) . . . . ? C23 P1 C25 C27 -178.0(12) . . . . ? C25 P1 C26 C28 56.8(12) . . . . ? C22 P1 C26 C28 175.8(9) . . . . ? C23 P1 C26 C28 -61.4(11) . . . . ? C20 C19B O1 C19A 49.9(9) . . . . ? C19A C19B O1 B1 100.6(10) . . . . ? C20 C19B O1 B1 150.5(7) . . . . ? C20 C19A O1 C19B -49.8(9) . . . . ? C19B C19A O1 B1 -122.8(9) . . . . ? C20 C19A O1 B1 -172.7(7) . . . . ? C7 B1 O1 C19B 104.5(9) . . . . ? C1 B1 O1 C19B -19.3(11) . . . . ? C13 B1 O1 C19B -143.2(9) . . . . ? C7 B1 O1 C19A 167.6(8) . . . . ? C1 B1 O1 C19A 43.8(10) . . . . ? C13 B1 O1 C19A -80.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.605 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.053 #===end data_Cy3PC4H8OB(C6F5)3 _database_code_depnum_ccdc_archive 'CCDC 698996' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C40 H41 B F15 O P' _chemical_formula_weight 864.51 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.267(4) _cell_length_b 13.076(4) _cell_length_c 24.449(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3922(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3611 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 18.66 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37516 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6900 _reflns_number_gt 3723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.19(14) _refine_ls_number_reflns 6900 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 P1 P 0.71314(9) 0.57877(8) 0.86979(4) 0.0445(3) Uani 1 1 d . . . O1 O 0.6171(2) 0.3598(2) 1.00734(10) 0.0471(7) Uani 1 1 d . . . B1 B 0.6297(4) 0.3449(4) 1.0655(2) 0.0474(13) Uani 1 1 d . . . F1 F 0.6433(2) 0.5012(2) 1.16090(10) 0.0799(8) Uani 1 1 d . . . F2 F 0.8095(3) 0.6219(2) 1.18101(11) 0.0967(10) Uani 1 1 d . . . F3 F 0.9956(2) 0.6095(2) 1.12062(12) 0.1009(10) Uani 1 1 d . . . F4 F 1.0054(2) 0.4751(2) 1.03630(14) 0.0986(10) Uani 1 1 d . . . F5 F 0.83790(19) 0.3568(2) 1.01290(11) 0.0714(8) Uani 1 1 d . . . F6 F 0.7012(2) 0.16659(18) 0.99167(10) 0.0735(8) Uani 1 1 d . . . F7 F 0.7848(3) -0.0074(2) 1.02464(12) 0.1003(10) Uani 1 1 d . . . F8 F 0.8135(2) -0.04847(19) 1.13226(14) 0.1012(10) Uani 1 1 d . . . F9 F 0.7571(2) 0.0953(2) 1.20744(12) 0.0911(9) Uani 1 1 d . . . F10 F 0.6716(2) 0.27214(19) 1.17616(10) 0.0723(8) Uani 1 1 d . . . F11 F 0.46721(19) 0.20442(17) 1.12827(11) 0.0725(7) Uani 1 1 d . . . F12 F 0.2779(2) 0.26115(19) 1.16836(11) 0.0853(9) Uani 1 1 d . . . F13 F 0.2046(3) 0.4554(2) 1.15515(13) 0.1070(10) Uani 1 1 d . . . F14 F 0.3298(2) 0.5930(2) 1.10248(12) 0.0967(10) Uani 1 1 d . . . F15 F 0.5239(2) 0.54092(18) 1.06368(10) 0.0730(8) Uani 1 1 d . . . C1 C 0.7297(4) 0.4224(3) 1.08515(16) 0.0484(11) Uani 1 1 d . . . C2 C 0.7304(4) 0.4909(3) 1.1274(2) 0.0581(12) Uani 1 1 d . . . C3 C 0.8166(5) 0.5543(4) 1.1395(2) 0.0645(14) Uani 1 1 d . . . C4 C 0.9099(5) 0.5489(4) 1.1092(2) 0.0687(15) Uani 1 1 d . . . C5 C 0.9164(4) 0.4812(4) 1.0672(2) 0.0659(14) Uani 1 1 d . . . C6 C 0.8266(4) 0.4208(3) 1.05607(18) 0.0536(12) Uani 1 1 d . . . C7 C 0.6775(3) 0.2294(3) 1.08244(18) 0.0507(12) Uani 1 1 d . . . C8 C 0.7092(4) 0.1533(3) 1.04612(19) 0.0539(12) Uani 1 1 d . . . C9 C 0.7544(4) 0.0618(3) 1.0632(3) 0.0688(15) Uani 1 1 d . . . C10 C 0.7690(4) 0.0410(4) 1.1164(3) 0.0704(16) Uani 1 1 d . . . C11 C 0.7423(4) 0.1137(4) 1.1538(2) 0.0600(13) Uani 1 1 d . . . C12 C 0.6970(3) 0.2041(3) 1.1362(2) 0.0551(12) Uani 1 1 d . . . C13 C 0.5107(3) 0.3709(3) 1.09568(15) 0.0453(11) Uani 1 1 d . . . C14 C 0.4401(4) 0.3041(3) 1.12134(18) 0.0540(12) Uani 1 1 d . . . C15 C 0.3405(4) 0.3311(3) 1.14205(19) 0.0592(13) Uani 1 1 d . . . C16 C 0.3020(4) 0.4271(4) 1.1359(2) 0.0675(13) Uani 1 1 d . . . C17 C 0.3674(4) 0.4966(3) 1.1094(2) 0.0628(13) Uani 1 1 d . . . C18 C 0.4651(4) 0.4677(3) 1.09011(17) 0.0543(12) Uani 1 1 d . . . C19 C 0.5247(3) 0.3164(3) 0.98179(15) 0.0529(12) Uani 1 1 d . . . H19A H 0.4599 0.3537 0.9927 0.063 Uiso 1 1 calc R . . H19B H 0.5164 0.2460 0.9936 0.063 Uiso 1 1 calc R . . C20 C 0.5357(4) 0.3197(3) 0.92146(16) 0.0527(12) Uani 1 1 d . . . H20A H 0.4697 0.2923 0.9052 0.063 Uiso 1 1 calc R . . H20B H 0.5956 0.2756 0.9107 0.063 Uiso 1 1 calc R . . C21 C 0.5557(3) 0.4256(3) 0.89853(18) 0.0583(12) Uani 1 1 d . . . H21A H 0.5201 0.4754 0.9219 0.070 Uiso 1 1 calc R . . H21B H 0.5225 0.4301 0.8626 0.070 Uiso 1 1 calc R . . C22 C 0.6766(3) 0.4533(3) 0.89372(16) 0.0507(12) Uani 1 1 d . . . H22A H 0.7103 0.4038 0.8694 0.061 Uiso 1 1 calc R . . H22B H 0.7093 0.4441 0.9295 0.061 Uiso 1 1 calc R . . C23 C 0.8536(4) 0.5720(3) 0.84578(16) 0.0546(12) Uani 1 1 d . . . H23A H 0.8940 0.5377 0.8751 0.065 Uiso 1 1 calc R . . C24 C 0.9100(4) 0.6768(4) 0.8385(2) 0.0769(15) Uani 1 1 d . . . H24A H 0.8753 0.7141 0.8089 0.092 Uiso 1 1 calc R . . H24B H 0.9022 0.7167 0.8717 0.092 Uiso 1 1 calc R . . C25 C 1.0307(4) 0.6620(5) 0.8257(2) 0.0997(19) Uani 1 1 d . . . H25A H 1.0643 0.7282 0.8197 0.120 Uiso 1 1 calc R . . H25B H 1.0663 0.6304 0.8568 0.120 Uiso 1 1 calc R . . C26 C 1.0473(4) 0.5966(5) 0.7762(2) 0.0951(19) Uani 1 1 d . . . H26A H 1.1248 0.5869 0.7702 0.114 Uiso 1 1 calc R . . H26B H 1.0173 0.6307 0.7444 0.114 Uiso 1 1 calc R . . C27 C 0.9930(4) 0.4935(4) 0.7832(2) 0.0853(17) Uani 1 1 d . . . H27A H 1.0275 0.4567 0.8130 0.102 Uiso 1 1 calc R . . H27B H 1.0020 0.4537 0.7501 0.102 Uiso 1 1 calc R . . C28 C 0.8708(4) 0.5065(4) 0.79550(19) 0.0719(15) Uani 1 1 d . . . H28A H 0.8352 0.5381 0.7644 0.086 Uiso 1 1 calc R . . H28B H 0.8381 0.4398 0.8013 0.086 Uiso 1 1 calc R . . C29 C 0.6158(3) 0.6189(3) 0.81858(16) 0.0481(11) Uani 1 1 d . . . H29A H 0.5453 0.6205 0.8375 0.058 Uiso 1 1 calc R . . C30 C 0.6319(4) 0.7267(3) 0.79636(17) 0.0577(13) Uani 1 1 d . . . H30A H 0.6982 0.7293 0.7748 0.069 Uiso 1 1 calc R . . H30B H 0.6395 0.7743 0.8265 0.069 Uiso 1 1 calc R . . C31 C 0.5351(4) 0.7577(4) 0.76098(19) 0.0743(15) Uani 1 1 d . . . H31A H 0.4705 0.7620 0.7837 0.089 Uiso 1 1 calc R . . H31B H 0.5486 0.8250 0.7457 0.089 Uiso 1 1 calc R . . C32 C 0.5146(4) 0.6840(4) 0.71537(18) 0.0742(15) Uani 1 1 d . . . H32A H 0.5751 0.6861 0.6898 0.089 Uiso 1 1 calc R . . H32B H 0.4492 0.7040 0.6959 0.089 Uiso 1 1 calc R . . C33 C 0.5012(4) 0.5758(4) 0.73697(18) 0.0689(14) Uani 1 1 d . . . H33A H 0.4364 0.5718 0.7596 0.083 Uiso 1 1 calc R . . H33B H 0.4926 0.5287 0.7066 0.083 Uiso 1 1 calc R . . C34 C 0.5995(4) 0.5462(3) 0.77017(16) 0.0592(13) Uani 1 1 d . . . H34A H 0.6638 0.5476 0.7471 0.071 Uiso 1 1 calc R . . H34B H 0.5905 0.4769 0.7836 0.071 Uiso 1 1 calc R . . C35 C 0.7087(3) 0.6694(3) 0.92581(14) 0.0422(10) Uani 1 1 d . . . H35A H 0.7310 0.7356 0.9107 0.051 Uiso 1 1 calc R . . C36 C 0.5966(3) 0.6852(3) 0.95106(18) 0.0624(14) Uani 1 1 d . . . H36A H 0.5450 0.7041 0.9228 0.075 Uiso 1 1 calc R . . H36B H 0.5719 0.6219 0.9676 0.075 Uiso 1 1 calc R . . C37 C 0.6012(4) 0.7687(4) 0.9941(2) 0.0731(16) Uani 1 1 d . . . H37A H 0.6185 0.8331 0.9764 0.088 Uiso 1 1 calc R . . H37B H 0.5299 0.7755 1.0108 0.088 Uiso 1 1 calc R . . C38 C 0.6842(4) 0.7481(4) 1.03803(17) 0.0663(14) Uani 1 1 d . . . H38A H 0.6624 0.6886 1.0590 0.080 Uiso 1 1 calc R . . H38B H 0.6876 0.8061 1.0627 0.080 Uiso 1 1 calc R . . C39 C 0.7955(4) 0.7299(3) 1.01307(16) 0.0584(12) Uani 1 1 d . . . H39A H 0.8470 0.7122 1.0417 0.070 Uiso 1 1 calc R . . H39B H 0.8208 0.7920 0.9955 0.070 Uiso 1 1 calc R . . C40 C 0.7908(4) 0.6433(3) 0.97091(15) 0.0574(12) Uani 1 1 d . . . H40A H 0.8624 0.6332 0.9549 0.069 Uiso 1 1 calc R . . H40B H 0.7694 0.5802 0.9888 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0447(7) 0.0446(6) 0.0441(6) 0.0007(5) -0.0004(6) 0.0008(6) O1 0.0440(19) 0.0527(18) 0.0445(18) 0.0003(14) -0.0089(14) -0.0080(14) B1 0.045(3) 0.052(3) 0.045(3) 0.001(3) 0.002(3) -0.006(3) F1 0.089(2) 0.095(2) 0.0560(17) -0.0144(15) 0.0084(16) -0.0244(18) F2 0.126(3) 0.088(2) 0.0754(19) -0.0140(17) -0.0197(19) -0.036(2) F3 0.085(2) 0.099(2) 0.119(2) 0.0093(19) -0.024(2) -0.0488(19) F4 0.052(2) 0.100(2) 0.144(3) -0.002(2) 0.010(2) -0.0121(17) F5 0.0469(17) 0.0750(19) 0.092(2) -0.0109(16) 0.0087(15) 0.0021(14) F6 0.089(2) 0.0637(17) 0.0682(18) -0.0110(14) 0.0060(17) 0.0042(16) F7 0.106(3) 0.0599(18) 0.135(3) -0.0141(18) 0.018(2) 0.0103(18) F8 0.084(2) 0.0592(18) 0.161(3) 0.0246(19) -0.017(2) 0.0058(15) F9 0.092(2) 0.089(2) 0.092(2) 0.0318(17) -0.0316(17) -0.0091(16) F10 0.081(2) 0.0748(19) 0.0614(17) 0.0026(15) -0.0090(15) 0.0034(15) F11 0.0614(17) 0.0495(15) 0.107(2) 0.0156(15) 0.0099(17) -0.0022(13) F12 0.0645(18) 0.0691(17) 0.122(2) 0.0082(17) 0.0305(18) -0.0153(16) F13 0.073(2) 0.091(2) 0.157(3) -0.0006(19) 0.046(2) 0.0097(18) F14 0.092(2) 0.0592(18) 0.139(3) 0.0077(17) 0.0195(19) 0.0264(16) F15 0.0738(19) 0.0500(15) 0.095(2) 0.0180(14) 0.0181(16) -0.0005(14) C1 0.052(3) 0.049(3) 0.044(3) 0.006(2) -0.006(2) -0.004(2) C2 0.060(3) 0.065(3) 0.050(3) 0.004(3) -0.001(3) -0.012(3) C3 0.074(4) 0.061(3) 0.059(3) 0.001(3) -0.020(3) -0.013(3) C4 0.064(4) 0.062(4) 0.080(4) 0.014(3) -0.022(3) -0.025(3) C5 0.045(4) 0.071(4) 0.082(4) 0.012(3) -0.005(3) -0.006(3) C6 0.047(3) 0.054(3) 0.060(3) -0.004(3) -0.002(3) 0.003(3) C7 0.043(3) 0.054(3) 0.055(3) 0.005(2) -0.002(2) -0.012(2) C8 0.053(3) 0.051(3) 0.057(3) -0.003(3) 0.004(3) -0.010(3) C9 0.056(4) 0.038(3) 0.112(5) -0.004(3) 0.010(3) 0.000(2) C10 0.053(3) 0.045(3) 0.114(5) 0.027(3) -0.004(3) 0.001(3) C11 0.051(3) 0.062(3) 0.067(3) 0.022(3) -0.014(3) -0.011(3) C12 0.049(3) 0.050(3) 0.066(3) -0.001(3) 0.001(3) -0.005(2) C13 0.044(3) 0.047(3) 0.045(3) 0.002(2) -0.001(2) -0.005(2) C14 0.054(3) 0.042(3) 0.066(3) 0.005(2) -0.005(3) 0.000(2) C15 0.053(3) 0.054(3) 0.071(4) 0.004(3) 0.011(3) -0.013(3) C16 0.050(3) 0.063(3) 0.089(4) -0.012(3) 0.023(3) 0.004(3) C17 0.059(3) 0.041(3) 0.088(4) 0.002(3) 0.002(3) 0.008(3) C18 0.060(3) 0.042(3) 0.061(3) 0.011(2) 0.003(3) -0.003(3) C19 0.048(3) 0.057(3) 0.054(3) 0.001(2) -0.004(2) -0.005(2) C20 0.050(3) 0.056(3) 0.052(3) -0.007(2) -0.007(2) -0.008(2) C21 0.056(3) 0.058(3) 0.060(3) 0.005(2) -0.005(2) -0.010(2) C22 0.054(3) 0.042(2) 0.056(3) 0.004(2) -0.003(2) -0.004(2) C23 0.049(3) 0.063(3) 0.052(3) -0.007(2) 0.011(2) 0.000(2) C24 0.061(4) 0.067(3) 0.102(4) -0.003(3) 0.028(3) -0.009(3) C25 0.064(4) 0.121(5) 0.114(5) -0.007(4) 0.033(4) -0.022(4) C26 0.054(4) 0.146(6) 0.086(4) 0.026(4) 0.024(3) 0.016(4) C27 0.063(4) 0.109(5) 0.084(4) -0.007(3) 0.018(3) 0.009(4) C28 0.057(4) 0.090(4) 0.068(3) -0.006(3) 0.013(3) 0.011(3) C29 0.050(3) 0.055(3) 0.039(2) -0.002(2) -0.001(2) 0.005(2) C30 0.065(3) 0.050(3) 0.058(3) 0.010(2) -0.007(3) 0.002(2) C31 0.072(4) 0.073(3) 0.079(4) 0.018(3) -0.011(3) 0.010(3) C32 0.065(4) 0.107(4) 0.051(3) 0.012(3) -0.008(3) 0.012(3) C33 0.056(3) 0.099(4) 0.051(3) 0.006(3) -0.012(3) 0.006(3) C34 0.069(4) 0.060(3) 0.048(3) -0.004(2) -0.008(3) -0.003(3) C35 0.041(3) 0.041(2) 0.045(2) -0.0014(19) -0.002(2) -0.003(2) C36 0.047(3) 0.069(3) 0.071(3) -0.014(3) -0.002(3) 0.000(2) C37 0.052(3) 0.093(4) 0.075(3) -0.041(3) 0.005(3) 0.003(3) C38 0.078(4) 0.069(3) 0.052(3) -0.008(2) 0.005(3) -0.018(3) C39 0.057(3) 0.063(3) 0.055(3) -0.001(2) -0.007(3) 0.004(3) C40 0.060(3) 0.059(3) 0.053(3) -0.010(2) -0.011(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C22 1.799(4) . ? P1 C29 1.808(4) . ? P1 C35 1.812(4) . ? P1 C23 1.823(4) . ? O1 C19 1.414(4) . ? O1 B1 1.444(5) . ? B1 C1 1.661(6) . ? B1 C13 1.670(6) . ? B1 C7 1.672(6) . ? F1 C2 1.354(5) . ? F2 C3 1.350(5) . ? F3 C4 1.346(5) . ? F4 C5 1.330(5) . ? F5 C6 1.355(5) . ? F6 C8 1.346(4) . ? F7 C9 1.360(5) . ? F8 C10 1.348(5) . ? F9 C11 1.345(5) . ? F10 C12 1.358(5) . ? F11 C14 1.356(4) . ? F12 C15 1.356(5) . ? F13 C16 1.336(5) . ? F14 C17 1.352(5) . ? F15 C18 1.362(4) . ? C1 C2 1.367(5) . ? C1 C6 1.385(6) . ? C2 C3 1.375(6) . ? C3 C4 1.365(7) . ? C4 C5 1.359(6) . ? C5 C6 1.383(6) . ? C7 C12 1.375(5) . ? C7 C8 1.389(5) . ? C8 C9 1.384(6) . ? C9 C10 1.340(7) . ? C10 C11 1.359(6) . ? C11 C12 1.376(6) . ? C13 C14 1.380(5) . ? C13 C18 1.391(6) . ? C14 C15 1.369(6) . ? C15 C16 1.351(6) . ? C16 C17 1.375(6) . ? C17 C18 1.343(6) . ? C19 C20 1.482(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.515(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.531(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C28 1.513(5) . ? C23 C24 1.545(6) . ? C23 H23A 0.9800 . ? C24 C25 1.526(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.495(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.513(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.537(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.523(5) . ? C29 C34 1.531(5) . ? C29 H29A 0.9800 . ? C30 C31 1.524(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.495(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.519(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.504(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.521(5) . ? C35 C40 1.532(5) . ? C35 H35A 0.9800 . ? C36 C37 1.516(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.504(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.515(6) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.532(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? 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 C22 P1 C29 109.0(2) . . ? C22 P1 C35 110.07(19) . . ? C29 P1 C35 108.29(18) . . ? C22 P1 C23 107.2(2) . . ? C29 P1 C23 114.6(2) . . ? C35 P1 C23 107.7(2) . . ? C19 O1 B1 117.8(3) . . ? O1 B1 C1 106.3(3) . . ? O1 B1 C13 108.3(4) . . ? C1 B1 C13 113.2(4) . . ? O1 B1 C7 113.7(4) . . ? C1 B1 C7 102.7(3) . . ? C13 B1 C7 112.4(3) . . ? C2 C1 C6 113.0(4) . . ? C2 C1 B1 128.5(4) . . ? C6 C1 B1 118.5(4) . . ? F1 C2 C1 121.1(4) . . ? F1 C2 C3 114.6(5) . . ? C1 C2 C3 124.3(5) . . ? F2 C3 C4 119.7(5) . . ? F2 C3 C2 120.5(5) . . ? C4 C3 C2 119.8(5) . . ? F3 C4 C5 119.6(6) . . ? F3 C4 C3 120.8(5) . . ? C5 C4 C3 119.5(5) . . ? F4 C5 C4 121.1(5) . . ? F4 C5 C6 120.6(5) . . ? C4 C5 C6 118.2(5) . . ? F5 C6 C5 115.1(4) . . ? F5 C6 C1 119.8(4) . . ? C5 C6 C1 125.1(5) . . ? C12 C7 C8 112.9(4) . . ? C12 C7 B1 121.0(4) . . ? C8 C7 B1 126.0(4) . . ? F6 C8 C9 116.1(4) . . ? F6 C8 C7 121.3(4) . . ? C9 C8 C7 122.6(4) . . ? C10 C9 F7 120.1(5) . . ? C10 C9 C8 121.5(5) . . ? F7 C9 C8 118.4(5) . . ? C9 C10 F8 120.6(5) . . ? C9 C10 C11 118.6(5) . . ? F8 C10 C11 120.7(5) . . ? F9 C11 C10 119.9(5) . . ? F9 C11 C12 121.0(5) . . ? C10 C11 C12 119.1(5) . . ? F10 C12 C7 119.3(4) . . ? F10 C12 C11 115.4(4) . . ? C7 C12 C11 125.2(5) . . ? C14 C13 C18 111.6(4) . . ? C14 C13 B1 128.4(4) . . ? C18 C13 B1 119.6(4) . . ? F11 C14 C15 114.8(4) . . ? F11 C14 C13 120.7(4) . . ? C15 C14 C13 124.4(4) . . ? C16 C15 F12 118.8(4) . . ? C16 C15 C14 120.7(4) . . ? F12 C15 C14 120.5(4) . . ? F13 C16 C15 122.1(5) . . ? F13 C16 C17 120.3(5) . . ? C15 C16 C17 117.6(4) . . ? C18 C17 F14 121.5(5) . . ? C18 C17 C16 120.0(4) . . ? F14 C17 C16 118.4(5) . . ? C17 C18 F15 116.2(4) . . ? C17 C18 C13 125.6(4) . . ? F15 C18 C13 118.2(4) . . ? O1 C19 C20 110.8(3) . . ? O1 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? O1 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C19 C20 C21 114.2(3) . . ? C19 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? C19 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 113.7(3) . . ? C20 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? C20 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 P1 118.8(3) . . ? C21 C22 H22A 107.6 . . ? P1 C22 H22A 107.6 . . ? C21 C22 H22B 107.6 . . ? P1 C22 H22B 107.6 . . ? H22A C22 H22B 107.0 . . ? C28 C23 C24 110.3(4) . . ? C28 C23 P1 114.9(3) . . ? C24 C23 P1 114.6(3) . . ? C28 C23 H23A 105.3 . . ? C24 C23 H23A 105.3 . . ? P1 C23 H23A 105.3 . . ? C25 C24 C23 110.2(4) . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 111.8(5) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C25 C26 C27 111.0(4) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 110.7(4) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C23 C28 C27 110.9(4) . . ? C23 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C34 108.4(3) . . ? C30 C29 P1 115.4(3) . . ? C34 C29 P1 116.2(3) . . ? C30 C29 H29A 105.2 . . ? C34 C29 H29A 105.2 . . ? P1 C29 H29A 105.2 . . ? C29 C30 C31 110.3(4) . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 112.5(4) . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? C30 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 C33 111.0(4) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 109.9(4) . . ? C34 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? C34 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C33 C34 C29 111.2(4) . . ? C33 C34 H34A 109.4 . . ? C29 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C29 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C40 109.4(3) . . ? C36 C35 P1 115.0(3) . . ? C40 C35 P1 112.2(3) . . ? C36 C35 H35A 106.5 . . ? C40 C35 H35A 106.5 . . ? P1 C35 H35A 106.5 . . ? C37 C36 C35 110.2(4) . . ? C37 C36 H36A 109.6 . . ? C35 C36 H36A 109.6 . . ? C37 C36 H36B 109.6 . . ? C35 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C36 113.1(4) . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 C39 110.5(4) . . ? C37 C38 H38A 109.6 . . ? C39 C38 H38A 109.6 . . ? C37 C38 H38B 109.6 . . ? C39 C38 H38B 109.6 . . ? H38A C38 H38B 108.1 . . ? C38 C39 C40 110.7(4) . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? C35 C40 C39 110.1(3) . . ? C35 C40 H40A 109.6 . . ? C39 C40 H40A 109.6 . . ? C35 C40 H40B 109.6 . . ? C39 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? 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 C19 O1 B1 C1 -169.1(3) . . . . ? C19 O1 B1 C13 -47.1(5) . . . . ? C19 O1 B1 C7 78.6(4) . . . . ? O1 B1 C1 C2 129.9(4) . . . . ? C13 B1 C1 C2 11.0(6) . . . . ? C7 B1 C1 C2 -110.4(5) . . . . ? O1 B1 C1 C6 -49.6(5) . . . . ? C13 B1 C1 C6 -168.5(4) . . . . ? C7 B1 C1 C6 70.1(5) . . . . ? C6 C1 C2 F1 -178.7(4) . . . . ? B1 C1 C2 F1 1.8(7) . . . . ? C6 C1 C2 C3 1.6(6) . . . . ? B1 C1 C2 C3 -177.9(4) . . . . ? F1 C2 C3 F2 -1.6(6) . . . . ? C1 C2 C3 F2 178.1(4) . . . . ? F1 C2 C3 C4 178.5(4) . . . . ? C1 C2 C3 C4 -1.8(7) . . . . ? F2 C3 C4 F3 0.7(7) . . . . ? C2 C3 C4 F3 -179.4(4) . . . . ? F2 C3 C4 C5 -179.5(4) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? F3 C4 C5 F4 -1.3(7) . . . . ? C3 C4 C5 F4 178.9(4) . . . . ? F3 C4 C5 C6 -179.3(4) . . . . ? C3 C4 C5 C6 1.0(7) . . . . ? F4 C5 C6 F5 0.6(7) . . . . ? C4 C5 C6 F5 178.6(4) . . . . ? F4 C5 C6 C1 -179.1(4) . . . . ? C4 C5 C6 C1 -1.1(7) . . . . ? C2 C1 C6 F5 -179.8(4) . . . . ? B1 C1 C6 F5 -0.2(6) . . . . ? C2 C1 C6 C5 -0.2(6) . . . . ? B1 C1 C6 C5 179.4(4) . . . . ? O1 B1 C7 C12 178.1(4) . . . . ? C1 B1 C7 C12 63.6(5) . . . . ? C13 B1 C7 C12 -58.4(5) . . . . ? O1 B1 C7 C8 3.3(6) . . . . ? C1 B1 C7 C8 -111.2(5) . . . . ? C13 B1 C7 C8 126.8(4) . . . . ? C12 C7 C8 F6 -176.7(4) . . . . ? B1 C7 C8 F6 -1.6(7) . . . . ? C12 C7 C8 C9 0.6(6) . . . . ? B1 C7 C8 C9 175.8(4) . . . . ? F6 C8 C9 C10 178.3(4) . . . . ? C7 C8 C9 C10 0.8(7) . . . . ? F6 C8 C9 F7 -1.3(6) . . . . ? C7 C8 C9 F7 -178.8(4) . . . . ? F7 C9 C10 F8 -0.2(7) . . . . ? C8 C9 C10 F8 -179.8(4) . . . . ? F7 C9 C10 C11 177.0(4) . . . . ? C8 C9 C10 C11 -2.6(7) . . . . ? C9 C10 C11 F9 -179.4(4) . . . . ? F8 C10 C11 F9 -2.1(7) . . . . ? C9 C10 C11 C12 2.8(7) . . . . ? F8 C10 C11 C12 -180.0(4) . . . . ? C8 C7 C12 F10 179.0(4) . . . . ? B1 C7 C12 F10 3.6(6) . . . . ? C8 C7 C12 C11 -0.4(7) . . . . ? B1 C7 C12 C11 -175.8(4) . . . . ? F9 C11 C12 F10 1.5(6) . . . . ? C10 C11 C12 F10 179.3(4) . . . . ? F9 C11 C12 C7 -179.1(4) . . . . ? C10 C11 C12 C7 -1.3(7) . . . . ? O1 B1 C13 C14 111.3(5) . . . . ? C1 B1 C13 C14 -131.0(4) . . . . ? C7 B1 C13 C14 -15.1(6) . . . . ? O1 B1 C13 C18 -59.7(5) . . . . ? C1 B1 C13 C18 58.0(5) . . . . ? C7 B1 C13 C18 173.8(4) . . . . ? C18 C13 C14 F11 176.7(4) . . . . ? B1 C13 C14 F11 5.1(7) . . . . ? C18 C13 C14 C15 -4.0(6) . . . . ? B1 C13 C14 C15 -175.6(4) . . . . ? F11 C14 C15 C16 -177.4(4) . . . . ? C13 C14 C15 C16 3.4(8) . . . . ? F11 C14 C15 F12 1.6(6) . . . . ? C13 C14 C15 F12 -177.7(4) . . . . ? F12 C15 C16 F13 0.3(8) . . . . ? C14 C15 C16 F13 179.3(4) . . . . ? F12 C15 C16 C17 179.6(4) . . . . ? C14 C15 C16 C17 -1.4(8) . . . . ? F13 C16 C17 C18 -179.9(4) . . . . ? C15 C16 C17 C18 0.8(8) . . . . ? F13 C16 C17 F14 -1.2(7) . . . . ? C15 C16 C17 F14 179.5(4) . . . . ? F14 C17 C18 F15 0.4(7) . . . . ? C16 C17 C18 F15 179.1(4) . . . . ? F14 C17 C18 C13 179.4(4) . . . . ? C16 C17 C18 C13 -2.0(8) . . . . ? C14 C13 C18 C17 3.4(6) . . . . ? B1 C13 C18 C17 175.8(4) . . . . ? C14 C13 C18 F15 -177.7(4) . . . . ? B1 C13 C18 F15 -5.2(6) . . . . ? B1 O1 C19 C20 -168.2(4) . . . . ? O1 C19 C20 C21 -55.8(5) . . . . ? C19 C20 C21 C22 90.5(4) . . . . ? C20 C21 C22 P1 -177.4(3) . . . . ? C29 P1 C22 C21 -35.5(4) . . . . ? C35 P1 C22 C21 83.1(4) . . . . ? C23 P1 C22 C21 -160.0(3) . . . . ? C22 P1 C23 C28 66.7(4) . . . . ? C29 P1 C23 C28 -54.3(4) . . . . ? C35 P1 C23 C28 -174.9(3) . . . . ? C22 P1 C23 C24 -164.0(3) . . . . ? C29 P1 C23 C24 74.9(4) . . . . ? C35 P1 C23 C24 -45.6(4) . . . . ? C28 C23 C24 C25 -55.9(5) . . . . ? P1 C23 C24 C25 172.6(4) . . . . ? C23 C24 C25 C26 56.5(6) . . . . ? C24 C25 C26 C27 -57.1(6) . . . . ? C25 C26 C27 C28 56.6(6) . . . . ? C24 C23 C28 C27 56.5(5) . . . . ? P1 C23 C28 C27 -172.1(4) . . . . ? C26 C27 C28 C23 -56.9(6) . . . . ? C22 P1 C29 C30 176.8(3) . . . . ? C35 P1 C29 C30 57.1(4) . . . . ? C23 P1 C29 C30 -63.1(4) . . . . ? C22 P1 C29 C34 -54.7(4) . . . . ? C35 P1 C29 C34 -174.4(3) . . . . ? C23 P1 C29 C34 65.4(4) . . . . ? C34 C29 C30 C31 57.0(5) . . . . ? P1 C29 C30 C31 -170.7(3) . . . . ? C29 C30 C31 C32 -55.9(5) . . . . ? C30 C31 C32 C33 54.7(6) . . . . ? C31 C32 C33 C34 -55.7(5) . . . . ? C32 C33 C34 C29 59.4(5) . . . . ? C30 C29 C34 C33 -60.1(5) . . . . ? P1 C29 C34 C33 168.0(3) . . . . ? C22 P1 C35 C36 -63.6(4) . . . . ? C29 P1 C35 C36 55.4(4) . . . . ? C23 P1 C35 C36 179.8(3) . . . . ? C22 P1 C35 C40 62.4(3) . . . . ? C29 P1 C35 C40 -178.6(3) . . . . ? C23 P1 C35 C40 -54.2(3) . . . . ? C40 C35 C36 C37 57.3(5) . . . . ? P1 C35 C36 C37 -175.3(3) . . . . ? C35 C36 C37 C38 -56.1(5) . . . . ? C36 C37 C38 C39 54.8(5) . . . . ? C37 C38 C39 C40 -55.3(5) . . . . ? C36 C35 C40 C39 -59.2(5) . . . . ? P1 C35 C40 C39 171.9(3) . . . . ? C38 C39 C40 C35 58.4(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.177 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.040 #===end data_PhtBu2PHC6F4BF(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 698997' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H15 B F15 P' _chemical_formula_weight 678.18 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.155(5) _cell_length_b 10.399(2) _cell_length_c 23.014(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.67(3) _cell_angle_gamma 90.00 _cell_volume 5530.4(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40995 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.220 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 25443 _diffrn_reflns_av_R_equivalents 0.1158 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4840 _reflns_number_gt 2289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0756P)^2^+10.6626P] 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 4840 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1717 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1961 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.10651(6) 0.23735(13) 0.07135(7) 0.0582(4) Uani 1 1 d . . . B1 B -0.1251(2) -0.0501(6) 0.1228(3) 0.0550(16) Uani 1 1 d . . . F1 F -0.14193(12) -0.1096(3) 0.06795(13) 0.0712(9) Uani 1 1 d . . . F2 F -0.16702(15) 0.1576(4) 0.05147(16) 0.0970(12) Uani 1 1 d . . . F3 F -0.25887(17) 0.3080(4) 0.06584(19) 0.1149(14) Uani 1 1 d . . . F4 F -0.32287(14) 0.2770(3) 0.15992(16) 0.0911(11) Uani 1 1 d . . . F5 F -0.29236(14) 0.0943(3) 0.24009(16) 0.0898(11) Uani 1 1 d . . . F6 F -0.20285(13) -0.0569(3) 0.22702(14) 0.0783(9) Uani 1 1 d . . . F7 F -0.14531(17) -0.3370(3) 0.1156(2) 0.1055(13) Uani 1 1 d . . . F8 F -0.1045(2) -0.5089(4) 0.1933(2) 0.150(2) Uani 1 1 d . . . F9 F -0.0509(2) -0.4320(5) 0.2959(2) 0.151(2) Uani 1 1 d . . . F10 F -0.04155(16) -0.1767(4) 0.31998(19) 0.1091(13) Uani 1 1 d . . . F11 F -0.07579(13) -0.0035(3) 0.24000(13) 0.0772(9) Uani 1 1 d . . . F12 F -0.08733(12) 0.2177(3) 0.16730(14) 0.0705(9) Uani 1 1 d . . . F13 F 0.01138(13) 0.3307(3) 0.14793(14) 0.0737(9) Uani 1 1 d . . . F14 F 0.06873(11) -0.0295(2) 0.04179(13) 0.0597(8) Uani 1 1 d . . . F15 F -0.02841(11) -0.1464(3) 0.06191(12) 0.0588(8) Uani 1 1 d . . . C1 C -0.1793(2) 0.0434(5) 0.1384(2) 0.0566(14) Uani 1 1 d . . . C2 C -0.1974(2) 0.1379(6) 0.0992(3) 0.0708(16) Uani 1 1 d . . . C3 C -0.2444(3) 0.2179(6) 0.1059(3) 0.0789(18) Uani 1 1 d . . . C4 C -0.2767(3) 0.2027(6) 0.1531(3) 0.0685(16) Uani 1 1 d . . . C5 C -0.2602(2) 0.1101(6) 0.1934(3) 0.0659(15) Uani 1 1 d . . . C6 C -0.2131(2) 0.0326(5) 0.1853(2) 0.0579(14) Uani 1 1 d . . . C7 C -0.1096(2) -0.1605(5) 0.1721(3) 0.0564(14) Uani 1 1 d . . . C8 C -0.1165(3) -0.2916(6) 0.1653(3) 0.0767(18) Uani 1 1 d . . . C9 C -0.0966(3) -0.3839(6) 0.2061(5) 0.093(2) Uani 1 1 d . . . C10 C -0.0706(3) -0.3429(9) 0.2571(5) 0.099(2) Uani 1 1 d . . . C11 C -0.0647(3) -0.2173(8) 0.2679(3) 0.0777(18) Uani 1 1 d . . . C12 C -0.0833(2) -0.1280(6) 0.2260(3) 0.0625(15) Uani 1 1 d . . . C13 C -0.0646(2) 0.0306(5) 0.1139(2) 0.0494(13) Uani 1 1 d . . . C14 C -0.0501(2) 0.1523(5) 0.1353(2) 0.0562(14) Uani 1 1 d . . . C15 C 0.0011(2) 0.2123(5) 0.1256(2) 0.0549(14) Uani 1 1 d . . . C16 C 0.0421(2) 0.1574(4) 0.0930(2) 0.0498(13) Uani 1 1 d . . . C17 C 0.0296(2) 0.0334(5) 0.0727(2) 0.0504(13) Uani 1 1 d . . . C18 C -0.0214(2) -0.0251(4) 0.0833(2) 0.0493(13) Uani 1 1 d . . . C19 C 0.0929(2) 0.3999(5) 0.0479(2) 0.0579(14) Uani 1 1 d . . . C20 C 0.0919(3) 0.5048(5) 0.0845(3) 0.0729(17) Uani 1 1 d . . . H20A H 0.0976 0.4932 0.1245 0.088 Uiso 1 1 calc R . . C21 C 0.0828(3) 0.6252(6) 0.0625(3) 0.0787(18) Uani 1 1 d . . . H21A H 0.0815 0.6950 0.0876 0.094 Uiso 1 1 calc R . . C22 C 0.0754(3) 0.6441(6) 0.0037(3) 0.0818(19) Uani 1 1 d . . . H22A H 0.0700 0.7266 -0.0112 0.098 Uiso 1 1 calc R . . C23 C 0.0761(4) 0.5395(7) -0.0334(3) 0.108(3) Uani 1 1 d . . . H23A H 0.0708 0.5517 -0.0734 0.129 Uiso 1 1 calc R . . C24 C 0.0847(3) 0.4173(5) -0.0112(3) 0.085(2) Uani 1 1 d . . . H24A H 0.0849 0.3470 -0.0362 0.102 Uiso 1 1 calc R . . C25 C 0.1669(2) 0.2158(5) 0.1251(3) 0.0739(17) Uani 1 1 d . . . C26 C 0.1539(3) 0.2684(6) 0.1838(3) 0.099(2) Uani 1 1 d . . . H26A H 0.1866 0.2551 0.2109 0.148 Uiso 1 1 calc R . . H26B H 0.1208 0.2249 0.1975 0.148 Uiso 1 1 calc R . . H26C H 0.1459 0.3588 0.1805 0.148 Uiso 1 1 calc R . . C27 C 0.1769(3) 0.0699(6) 0.1303(3) 0.097(2) Uani 1 1 d . . . H27A H 0.2085 0.0533 0.1583 0.145 Uiso 1 1 calc R . . H27B H 0.1858 0.0359 0.0932 0.145 Uiso 1 1 calc R . . H27C H 0.1425 0.0293 0.1428 0.145 Uiso 1 1 calc R . . C28 C 0.2193(3) 0.2830(7) 0.1003(4) 0.118(3) Uani 1 1 d . . . H28A H 0.2525 0.2741 0.1272 0.177 Uiso 1 1 calc R . . H28B H 0.2108 0.3726 0.0944 0.177 Uiso 1 1 calc R . . H28C H 0.2272 0.2442 0.0638 0.177 Uiso 1 1 calc R . . H1 H 0.1281(14) 0.172(3) 0.0254(14) 0.026(9) 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 0.0539(9) 0.0463(8) 0.0761(10) -0.0063(7) 0.0168(7) -0.0056(6) B1 0.048(4) 0.056(4) 0.062(4) -0.014(3) 0.012(3) -0.006(3) F1 0.0560(18) 0.086(2) 0.072(2) -0.0252(18) 0.0092(15) -0.0092(16) F2 0.084(2) 0.115(3) 0.096(3) 0.031(2) 0.034(2) 0.026(2) F3 0.104(3) 0.115(3) 0.128(3) 0.037(3) 0.024(2) 0.044(2) F4 0.065(2) 0.081(2) 0.129(3) -0.013(2) 0.017(2) 0.0211(18) F5 0.067(2) 0.106(3) 0.100(3) -0.004(2) 0.032(2) 0.0180(19) F6 0.067(2) 0.088(2) 0.082(2) 0.011(2) 0.0231(17) 0.0132(18) F7 0.105(3) 0.069(2) 0.148(4) -0.038(2) 0.050(3) -0.027(2) F8 0.183(5) 0.050(3) 0.229(6) 0.011(3) 0.119(4) 0.003(2) F9 0.149(4) 0.132(4) 0.182(5) 0.096(4) 0.086(3) 0.055(3) F10 0.084(3) 0.162(4) 0.082(3) 0.039(3) 0.015(2) 0.000(2) F11 0.081(2) 0.077(2) 0.074(2) -0.0028(17) 0.0068(18) -0.0193(18) F12 0.0648(19) 0.0575(18) 0.093(2) -0.0195(16) 0.0306(17) -0.0021(15) F13 0.078(2) 0.0504(18) 0.096(2) -0.0192(17) 0.0311(17) -0.0092(15) F14 0.0530(17) 0.0469(17) 0.082(2) -0.0094(15) 0.0234(16) -0.0041(13) F15 0.0562(18) 0.0484(18) 0.073(2) -0.0123(14) 0.0158(15) -0.0042(13) C1 0.050(3) 0.059(3) 0.061(4) -0.006(3) 0.011(3) -0.001(3) C2 0.058(4) 0.082(4) 0.075(4) 0.005(4) 0.019(3) -0.001(3) C3 0.066(4) 0.068(4) 0.102(5) 0.019(4) -0.003(4) 0.021(3) C4 0.052(4) 0.072(4) 0.083(5) -0.014(4) 0.017(3) 0.004(3) C5 0.058(4) 0.072(4) 0.070(4) -0.007(3) 0.021(3) -0.005(3) C6 0.043(3) 0.061(3) 0.071(4) -0.003(3) 0.014(3) 0.006(3) C7 0.043(3) 0.051(4) 0.077(4) -0.004(3) 0.022(3) -0.002(3) C8 0.062(4) 0.062(4) 0.110(6) -0.016(4) 0.035(4) -0.008(3) C9 0.096(6) 0.041(4) 0.151(8) 0.003(5) 0.072(5) 0.003(4) C10 0.081(5) 0.080(6) 0.141(8) 0.033(6) 0.059(5) 0.013(4) C11 0.058(4) 0.096(6) 0.082(5) 0.015(5) 0.027(4) -0.008(4) C12 0.046(3) 0.059(4) 0.084(5) 0.012(4) 0.020(3) -0.003(3) C13 0.046(3) 0.045(3) 0.057(3) -0.003(3) 0.004(3) -0.003(2) C14 0.055(3) 0.052(3) 0.064(4) -0.006(3) 0.020(3) 0.003(3) C15 0.061(4) 0.042(3) 0.064(4) -0.010(3) 0.019(3) -0.004(3) C16 0.049(3) 0.041(3) 0.059(3) -0.001(3) 0.006(3) -0.004(2) C17 0.048(3) 0.050(3) 0.053(3) -0.003(3) 0.009(3) 0.000(3) C18 0.052(3) 0.038(3) 0.058(3) -0.007(2) 0.007(3) -0.001(2) C19 0.060(3) 0.053(3) 0.062(4) 0.002(3) 0.015(3) -0.008(3) C20 0.095(5) 0.054(4) 0.070(4) -0.002(3) 0.010(3) -0.002(3) C21 0.102(5) 0.051(4) 0.083(5) -0.004(3) 0.012(4) 0.003(3) C22 0.111(5) 0.057(4) 0.079(5) 0.001(4) 0.020(4) -0.005(3) C23 0.183(8) 0.069(5) 0.072(5) 0.004(4) 0.015(5) -0.007(5) C24 0.136(6) 0.042(4) 0.080(5) -0.003(3) 0.018(4) -0.005(3) C25 0.059(4) 0.056(4) 0.105(5) -0.006(3) -0.005(3) -0.010(3) C26 0.117(6) 0.075(5) 0.099(5) -0.005(4) -0.030(5) 0.003(4) C27 0.082(5) 0.060(4) 0.144(6) -0.011(4) -0.022(4) 0.009(3) C28 0.065(4) 0.097(5) 0.192(8) -0.005(5) 0.011(5) -0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C19 1.796(5) . ? P1 C16 1.805(5) . ? P1 C25 1.821(6) . ? P1 H1 1.38(3) . ? B1 F1 1.436(6) . ? B1 C7 1.638(8) . ? B1 C1 1.645(8) . ? B1 C13 1.657(7) . ? F2 C2 1.358(6) . ? F3 C3 1.342(7) . ? F4 C4 1.336(6) . ? F5 C5 1.357(6) . ? F6 C6 1.347(6) . ? F7 C8 1.371(7) . ? F8 C9 1.343(7) . ? F9 C10 1.347(8) . ? F10 C11 1.350(7) . ? F11 C12 1.343(6) . ? F12 C14 1.352(5) . ? F13 C15 1.349(5) . ? F14 C17 1.355(5) . ? F15 C18 1.359(5) . ? C1 C6 1.378(7) . ? C1 C2 1.381(8) . ? C2 C3 1.385(8) . ? C3 C4 1.368(8) . ? C4 C5 1.373(8) . ? C5 C6 1.378(7) . ? C7 C8 1.380(8) . ? C7 C12 1.388(8) . ? C8 C9 1.400(10) . ? C9 C10 1.353(10) . ? C10 C11 1.335(10) . ? C11 C12 1.387(8) . ? C13 C18 1.386(6) . ? C13 C14 1.392(7) . ? C14 C15 1.371(7) . ? C15 C16 1.372(6) . ? C16 C17 1.396(6) . ? C17 C18 1.365(6) . ? C19 C24 1.373(8) . ? C19 C20 1.380(7) . ? C20 C21 1.362(8) . ? C20 H20A 0.9300 . ? C21 C22 1.367(8) . ? C21 H21A 0.9300 . ? C22 C23 1.383(8) . ? C22 H22A 0.9300 . ? C23 C24 1.379(8) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.506(8) . ? C25 C27 1.539(8) . ? C25 C28 1.541(9) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 P1 C16 112.6(2) . . ? C19 P1 C25 115.6(3) . . ? C16 P1 C25 111.6(3) . . ? C19 P1 H1 107.3(14) . . ? C16 P1 H1 109.4(14) . . ? C25 P1 H1 99.3(14) . . ? F1 B1 C7 110.0(4) . . ? F1 B1 C1 106.2(4) . . ? C7 B1 C1 113.5(4) . . ? F1 B1 C13 107.1(4) . . ? C7 B1 C13 106.9(4) . . ? C1 B1 C13 112.9(4) . . ? C6 C1 C2 113.9(5) . . ? C6 C1 B1 127.0(5) . . ? C2 C1 B1 118.9(5) . . ? F2 C2 C1 118.9(5) . . ? F2 C2 C3 116.8(6) . . ? C1 C2 C3 124.3(6) . . ? F3 C3 C4 120.1(6) . . ? F3 C3 C2 120.4(6) . . ? C4 C3 C2 119.5(6) . . ? F4 C4 C3 120.6(6) . . ? F4 C4 C5 121.2(6) . . ? C3 C4 C5 118.3(5) . . ? F5 C5 C4 118.4(5) . . ? F5 C5 C6 121.0(6) . . ? C4 C5 C6 120.5(5) . . ? F6 C6 C5 114.4(5) . . ? F6 C6 C1 122.1(5) . . ? C5 C6 C1 123.5(6) . . ? C8 C7 C12 112.5(6) . . ? C8 C7 B1 126.5(6) . . ? C12 C7 B1 120.8(5) . . ? F7 C8 C7 118.8(6) . . ? F7 C8 C9 116.4(7) . . ? C7 C8 C9 124.8(7) . . ? F8 C9 C10 122.8(9) . . ? F8 C9 C8 118.8(9) . . ? C10 C9 C8 118.4(7) . . ? C11 C10 F9 121.5(10) . . ? C11 C10 C9 120.3(8) . . ? F9 C10 C9 118.2(9) . . ? C10 C11 F10 120.1(8) . . ? C10 C11 C12 120.1(8) . . ? F10 C11 C12 119.7(7) . . ? F11 C12 C11 116.7(6) . . ? F11 C12 C7 119.5(5) . . ? C11 C12 C7 123.8(6) . . ? C18 C13 C14 113.3(4) . . ? C18 C13 B1 119.6(4) . . ? C14 C13 B1 127.1(4) . . ? F12 C14 C15 116.6(4) . . ? F12 C14 C13 120.2(4) . . ? C15 C14 C13 123.2(5) . . ? F13 C15 C14 119.1(4) . . ? F13 C15 C16 118.5(4) . . ? C14 C15 C16 122.4(5) . . ? C15 C16 C17 115.6(4) . . ? C15 C16 P1 124.9(4) . . ? C17 C16 P1 119.4(4) . . ? F14 C17 C18 119.6(4) . . ? F14 C17 C16 119.4(4) . . ? C18 C17 C16 121.0(4) . . ? F15 C18 C17 115.6(4) . . ? F15 C18 C13 119.9(4) . . ? C17 C18 C13 124.4(5) . . ? C24 C19 C20 119.6(5) . . ? C24 C19 P1 115.6(4) . . ? C20 C19 P1 124.7(5) . . ? C21 C20 C19 120.5(6) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 120.5(6) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C22 C23 119.4(6) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C24 C23 C22 120.3(6) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C19 C24 C23 119.7(6) . . ? C19 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C26 C25 C27 109.0(6) . . ? C26 C25 C28 112.1(5) . . ? C27 C25 C28 111.0(5) . . ? C26 C25 P1 112.1(4) . . ? C27 C25 P1 106.2(4) . . ? C28 C25 P1 106.3(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 F1 B1 C1 C6 117.1(6) . . . . ? C7 B1 C1 C6 -3.9(7) . . . . ? C13 B1 C1 C6 -125.9(6) . . . . ? F1 B1 C1 C2 -57.2(6) . . . . ? C7 B1 C1 C2 -178.1(5) . . . . ? C13 B1 C1 C2 59.9(6) . . . . ? C6 C1 C2 F2 179.6(5) . . . . ? B1 C1 C2 F2 -5.5(8) . . . . ? C6 C1 C2 C3 1.4(9) . . . . ? B1 C1 C2 C3 176.4(5) . . . . ? F2 C2 C3 F3 1.4(9) . . . . ? C1 C2 C3 F3 179.5(5) . . . . ? F2 C2 C3 C4 180.0(5) . . . . ? C1 C2 C3 C4 -1.8(10) . . . . ? F3 C3 C4 F4 0.0(9) . . . . ? C2 C3 C4 F4 -178.6(5) . . . . ? F3 C3 C4 C5 -179.5(5) . . . . ? C2 C3 C4 C5 1.9(9) . . . . ? F4 C4 C5 F5 0.9(8) . . . . ? C3 C4 C5 F5 -179.6(5) . . . . ? F4 C4 C5 C6 178.8(5) . . . . ? C3 C4 C5 C6 -1.7(9) . . . . ? F5 C5 C6 F6 0.0(8) . . . . ? C4 C5 C6 F6 -177.9(5) . . . . ? F5 C5 C6 C1 179.3(5) . . . . ? C4 C5 C6 C1 1.4(9) . . . . ? C2 C1 C6 F6 178.0(5) . . . . ? B1 C1 C6 F6 3.6(8) . . . . ? C2 C1 C6 C5 -1.2(8) . . . . ? B1 C1 C6 C5 -175.7(5) . . . . ? F1 B1 C7 C8 -5.9(7) . . . . ? C1 B1 C7 C8 112.9(6) . . . . ? C13 B1 C7 C8 -121.9(5) . . . . ? F1 B1 C7 C12 169.6(4) . . . . ? C1 B1 C7 C12 -71.6(6) . . . . ? C13 B1 C7 C12 53.6(6) . . . . ? C12 C7 C8 F7 175.7(4) . . . . ? B1 C7 C8 F7 -8.5(8) . . . . ? C12 C7 C8 C9 -3.6(8) . . . . ? B1 C7 C8 C9 172.2(5) . . . . ? F7 C8 C9 F8 2.8(8) . . . . ? C7 C8 C9 F8 -177.9(5) . . . . ? F7 C8 C9 C10 -176.6(6) . . . . ? C7 C8 C9 C10 2.7(9) . . . . ? F8 C9 C10 C11 -178.9(5) . . . . ? C8 C9 C10 C11 0.5(10) . . . . ? F8 C9 C10 F9 1.5(10) . . . . ? C8 C9 C10 F9 -179.1(5) . . . . ? F9 C10 C11 F10 -3.9(9) . . . . ? C9 C10 C11 F10 176.5(6) . . . . ? F9 C10 C11 C12 177.3(5) . . . . ? C9 C10 C11 C12 -2.3(10) . . . . ? C10 C11 C12 F11 -179.8(5) . . . . ? F10 C11 C12 F11 1.4(7) . . . . ? C10 C11 C12 C7 1.2(9) . . . . ? F10 C11 C12 C7 -177.6(5) . . . . ? C8 C7 C12 F11 -177.3(4) . . . . ? B1 C7 C12 F11 6.6(7) . . . . ? C8 C7 C12 C11 1.6(7) . . . . ? B1 C7 C12 C11 -174.4(5) . . . . ? F1 B1 C13 C18 -43.1(6) . . . . ? C7 B1 C13 C18 74.8(6) . . . . ? C1 B1 C13 C18 -159.6(5) . . . . ? F1 B1 C13 C14 138.5(5) . . . . ? C7 B1 C13 C14 -103.6(6) . . . . ? C1 B1 C13 C14 22.0(7) . . . . ? C18 C13 C14 F12 -178.4(4) . . . . ? B1 C13 C14 F12 0.1(8) . . . . ? C18 C13 C14 C15 1.7(7) . . . . ? B1 C13 C14 C15 -179.8(5) . . . . ? F12 C14 C15 F13 -0.1(7) . . . . ? C13 C14 C15 F13 179.8(5) . . . . ? F12 C14 C15 C16 -178.9(5) . . . . ? C13 C14 C15 C16 1.0(8) . . . . ? F13 C15 C16 C17 178.2(4) . . . . ? C14 C15 C16 C17 -3.0(7) . . . . ? F13 C15 C16 P1 -6.3(7) . . . . ? C14 C15 C16 P1 172.4(4) . . . . ? C19 P1 C16 C15 -42.1(5) . . . . ? C25 P1 C16 C15 89.8(5) . . . . ? C19 P1 C16 C17 133.2(4) . . . . ? C25 P1 C16 C17 -94.8(5) . . . . ? C15 C16 C17 F14 -177.8(4) . . . . ? P1 C16 C17 F14 6.5(6) . . . . ? C15 C16 C17 C18 2.4(7) . . . . ? P1 C16 C17 C18 -173.4(4) . . . . ? F14 C17 C18 F15 1.0(7) . . . . ? C16 C17 C18 F15 -179.2(4) . . . . ? F14 C17 C18 C13 -179.5(5) . . . . ? C16 C17 C18 C13 0.4(8) . . . . ? C14 C13 C18 F15 177.2(4) . . . . ? B1 C13 C18 F15 -1.5(7) . . . . ? C14 C13 C18 C17 -2.4(7) . . . . ? B1 C13 C18 C17 179.0(5) . . . . ? C16 P1 C19 C24 -97.2(5) . . . . ? C25 P1 C19 C24 132.9(5) . . . . ? C16 P1 C19 C20 84.8(5) . . . . ? C25 P1 C19 C20 -45.1(6) . . . . ? C24 C19 C20 C21 0.2(9) . . . . ? P1 C19 C20 C21 178.2(5) . . . . ? C19 C20 C21 C22 -1.2(10) . . . . ? C20 C21 C22 C23 1.4(10) . . . . ? C21 C22 C23 C24 -0.6(11) . . . . ? C20 C19 C24 C23 0.5(10) . . . . ? P1 C19 C24 C23 -177.6(6) . . . . ? C22 C23 C24 C19 -0.4(11) . . . . ? C19 P1 C25 C26 70.7(5) . . . . ? C16 P1 C25 C26 -59.7(5) . . . . ? C19 P1 C25 C27 -170.3(4) . . . . ? C16 P1 C25 C27 59.3(5) . . . . ? C19 P1 C25 C28 -52.1(5) . . . . ? C16 P1 C25 C28 177.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.306 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.059 #===end data_tBuMesPH-C6F4-BF(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 698998' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C31 H21 B F15 P' _chemical_formula_weight 720.26 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' 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' _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 11.819(5) _cell_length_b 12.003(6) _cell_length_c 14.694(7) _cell_angle_alpha 66.442(5) _cell_angle_beta 69.594(5) _cell_angle_gamma 74.705(6) _cell_volume 1772.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4391 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.00 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.939 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 16879 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6209 _reflns_number_gt 3569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0592P)^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 6209 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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 0.92026(6) 0.47787(7) 0.27390(5) 0.0463(2) Uani 1 1 d . . . B1 B 0.7164(3) 0.4050(3) 0.7515(2) 0.0513(8) Uani 1 1 d . . . F1 F 0.81786(13) 0.41796(14) 0.77698(11) 0.0617(4) Uani 1 1 d . . . F2 F 0.71426(15) 0.66451(15) 0.66642(13) 0.0772(5) Uani 1 1 d . . . F3 F 0.5597(2) 0.8353(2) 0.73878(17) 0.1119(7) Uani 1 1 d . . . F4 F 0.35858(19) 0.7744(2) 0.89992(17) 0.1112(7) Uani 1 1 d . . . F5 F 0.31718(16) 0.5372(2) 0.98777(14) 0.1008(7) Uani 1 1 d . . . F6 F 0.47337(15) 0.36388(18) 0.92327(13) 0.0789(5) Uani 1 1 d . . . F7 F 0.82674(17) 0.19320(17) 0.91014(14) 0.0872(6) Uani 1 1 d . . . F8 F 0.7734(2) -0.03333(19) 0.99364(17) 0.1229(8) Uani 1 1 d . . . F9 F 0.6088(2) -0.0968(2) 0.93966(19) 0.1342(9) Uani 1 1 d . . . F10 F 0.4921(2) 0.0773(2) 0.8014(2) 0.1300(9) Uani 1 1 d . . . F11 F 0.54345(17) 0.30659(19) 0.71663(15) 0.0916(6) Uani 1 1 d . . . F12 F 0.94763(14) 0.30355(16) 0.63974(12) 0.0750(5) Uani 1 1 d . . . F13 F 1.02971(13) 0.33795(15) 0.44139(11) 0.0685(5) Uani 1 1 d . . . F14 F 0.66230(14) 0.59338(15) 0.38982(12) 0.0689(5) Uani 1 1 d . . . F15 F 0.58045(13) 0.56094(16) 0.58649(12) 0.0721(5) Uani 1 1 d . . . C1 C 0.6033(2) 0.5045(3) 0.79017(19) 0.0503(7) Uani 1 1 d . . . C2 C 0.6165(3) 0.6272(3) 0.7485(2) 0.0606(8) Uani 1 1 d . . . C3 C 0.5381(3) 0.7181(3) 0.7834(3) 0.0713(9) Uani 1 1 d . . . C4 C 0.4375(3) 0.6870(4) 0.8649(3) 0.0752(10) Uani 1 1 d . . . C5 C 0.4170(3) 0.5680(4) 0.9083(2) 0.0691(9) Uani 1 1 d . . . C6 C 0.4994(2) 0.4799(3) 0.8717(2) 0.0560(7) Uani 1 1 d . . . C7 C 0.6887(2) 0.2627(3) 0.8072(2) 0.0554(7) Uani 1 1 d . . . C8 C 0.7428(3) 0.1702(3) 0.8791(2) 0.0653(8) Uani 1 1 d . . . C9 C 0.7176(4) 0.0525(4) 0.9227(3) 0.0845(11) Uani 1 1 d . . . C10 C 0.6345(4) 0.0189(4) 0.8980(3) 0.0904(12) Uani 1 1 d . . . C11 C 0.5766(3) 0.1050(4) 0.8282(3) 0.0848(11) Uani 1 1 d . . . C12 C 0.6045(3) 0.2232(3) 0.7851(2) 0.0691(8) Uani 1 1 d . . . C13 C 0.7603(2) 0.4329(2) 0.62472(19) 0.0485(7) Uani 1 1 d . . . C14 C 0.8737(2) 0.3790(2) 0.5801(2) 0.0508(7) Uani 1 1 d . . . C15 C 0.9181(2) 0.3953(2) 0.4763(2) 0.0500(7) Uani 1 1 d . . . C16 C 0.8499(2) 0.4677(2) 0.40708(19) 0.0449(6) Uani 1 1 d . . . C17 C 0.7360(2) 0.5221(2) 0.4500(2) 0.0495(7) Uani 1 1 d . . . C18 C 0.6943(2) 0.5035(3) 0.5545(2) 0.0524(7) Uani 1 1 d . . . C19 C 0.8809(3) 0.6226(2) 0.1732(2) 0.0555(7) Uani 1 1 d . . . C20 C 0.8778(3) 0.7306(3) 0.2054(2) 0.0697(8) Uani 1 1 d . . . H20A H 0.8566 0.8065 0.1542 0.105 Uiso 1 1 calc R . . H20B H 0.9566 0.7287 0.2114 0.105 Uiso 1 1 calc R . . H20C H 0.8181 0.7240 0.2707 0.105 Uiso 1 1 calc R . . C21 C 0.9900(3) 0.6227(3) 0.0769(2) 0.0741(9) Uani 1 1 d . . . H21A H 0.9771 0.6952 0.0197 0.111 Uiso 1 1 calc R . . H21B H 0.9968 0.5512 0.0602 0.111 Uiso 1 1 calc R . . H21C H 1.0637 0.6217 0.0911 0.111 Uiso 1 1 calc R . . C22 C 0.7635(3) 0.6301(3) 0.1483(2) 0.0753(9) Uani 1 1 d . . . H22A H 0.7491 0.7075 0.0959 0.113 Uiso 1 1 calc R . . H22B H 0.6964 0.6229 0.2094 0.113 Uiso 1 1 calc R . . H22C H 0.7713 0.5645 0.1238 0.113 Uiso 1 1 calc R . . C23 C 0.9177(2) 0.3410(2) 0.25295(18) 0.0479(6) Uani 1 1 d . . . C24 C 0.8070(2) 0.2964(2) 0.2812(2) 0.0534(7) Uani 1 1 d . . . C25 C 0.8104(3) 0.1929(3) 0.2593(2) 0.0706(9) Uani 1 1 d . . . H25A H 0.7378 0.1626 0.2779 0.085 Uiso 1 1 calc R . . C26 C 0.9168(3) 0.1334(3) 0.2111(3) 0.0728(9) Uani 1 1 d . . . C27 C 1.0239(3) 0.1768(3) 0.1870(2) 0.0677(8) Uani 1 1 d . . . H27A H 1.0964 0.1356 0.1565 0.081 Uiso 1 1 calc R . . C28 C 1.0285(2) 0.2794(3) 0.2063(2) 0.0532(7) Uani 1 1 d . . . C29 C 0.6866(2) 0.3507(3) 0.3372(2) 0.0709(9) Uani 1 1 d . . . H29A H 0.6972 0.4207 0.3480 0.106 Uiso 1 1 calc R . . H29B H 0.6556 0.2904 0.4027 0.106 Uiso 1 1 calc R . . H29C H 0.6299 0.3759 0.2967 0.106 Uiso 1 1 calc R . . C30 C 0.9157(4) 0.0221(4) 0.1874(4) 0.1254(16) Uani 1 1 d . . . H30A H 0.8335 0.0054 0.2092 0.188 Uiso 1 1 calc R . . H30B H 0.9648 -0.0476 0.2235 0.188 Uiso 1 1 calc R . . H30C H 0.9483 0.0379 0.1144 0.188 Uiso 1 1 calc R . . C31 C 1.1526(3) 0.3160(3) 0.1768(3) 0.0788(10) Uani 1 1 d . . . H31A H 1.2134 0.2607 0.1462 0.118 Uiso 1 1 calc R . . H31B H 1.1694 0.3124 0.2374 0.118 Uiso 1 1 calc R . . H31C H 1.1538 0.3982 0.1281 0.118 Uiso 1 1 calc R . . H1 H 1.0280(19) 0.4840(18) 0.2660(15) 0.038(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 0.0481(4) 0.0529(4) 0.0407(4) -0.0208(3) -0.0111(3) -0.0057(3) B1 0.0446(18) 0.067(2) 0.0422(17) -0.0205(16) -0.0113(14) -0.0050(16) F1 0.0500(9) 0.0856(12) 0.0552(9) -0.0264(9) -0.0175(7) -0.0106(8) F2 0.0781(12) 0.0756(12) 0.0700(11) -0.0286(10) 0.0000(10) -0.0207(10) F3 0.1357(19) 0.0781(15) 0.1147(17) -0.0477(13) -0.0162(14) -0.0051(13) F4 0.1010(15) 0.1267(17) 0.1146(17) -0.0846(15) -0.0182(13) 0.0233(13) F5 0.0615(11) 0.1520(19) 0.0818(13) -0.0630(13) 0.0119(10) -0.0100(12) F6 0.0678(11) 0.0948(14) 0.0641(11) -0.0301(10) 0.0034(9) -0.0204(10) F7 0.0825(13) 0.0962(14) 0.0719(12) -0.0166(10) -0.0337(10) 0.0027(11) F8 0.1275(18) 0.0846(15) 0.0944(16) -0.0003(12) -0.0149(14) 0.0145(14) F9 0.150(2) 0.0700(15) 0.134(2) -0.0323(14) 0.0284(16) -0.0345(14) F10 0.1292(19) 0.131(2) 0.156(2) -0.0675(17) -0.0156(17) -0.0636(16) F11 0.0828(13) 0.1112(16) 0.0944(14) -0.0299(13) -0.0354(12) -0.0290(12) F12 0.0592(10) 0.1011(13) 0.0509(10) -0.0253(9) -0.0221(8) 0.0192(9) F13 0.0472(9) 0.0895(12) 0.0535(10) -0.0292(9) -0.0093(7) 0.0161(8) F14 0.0630(10) 0.0847(12) 0.0594(10) -0.0316(9) -0.0313(8) 0.0195(9) F15 0.0504(10) 0.1031(13) 0.0600(10) -0.0428(10) -0.0165(8) 0.0192(9) C1 0.0477(16) 0.065(2) 0.0418(15) -0.0235(14) -0.0103(13) -0.0079(14) C2 0.0516(18) 0.080(2) 0.0500(17) -0.0308(17) -0.0043(14) -0.0092(17) C3 0.081(2) 0.067(2) 0.070(2) -0.0341(19) -0.0167(19) -0.0045(19) C4 0.068(2) 0.100(3) 0.071(2) -0.058(2) -0.0197(19) 0.014(2) C5 0.0467(18) 0.109(3) 0.0577(19) -0.046(2) -0.0033(15) -0.0082(19) C6 0.0493(17) 0.074(2) 0.0478(17) -0.0261(16) -0.0104(14) -0.0090(16) C7 0.0471(16) 0.072(2) 0.0469(16) -0.0288(16) -0.0029(13) -0.0076(15) C8 0.059(2) 0.067(2) 0.0574(19) -0.0246(18) -0.0037(16) -0.0001(17) C9 0.079(3) 0.073(3) 0.068(2) -0.020(2) -0.001(2) 0.008(2) C10 0.097(3) 0.063(3) 0.082(3) -0.027(2) 0.014(2) -0.013(2) C11 0.080(3) 0.090(3) 0.090(3) -0.047(3) 0.004(2) -0.034(2) C12 0.066(2) 0.080(2) 0.061(2) -0.0287(19) -0.0113(17) -0.0104(19) C13 0.0426(15) 0.0586(18) 0.0459(15) -0.0223(14) -0.0116(13) -0.0036(13) C14 0.0487(16) 0.0590(18) 0.0419(15) -0.0144(13) -0.0185(13) 0.0005(14) C15 0.0399(15) 0.0556(17) 0.0534(17) -0.0241(14) -0.0103(13) 0.0006(13) C16 0.0467(15) 0.0484(16) 0.0412(14) -0.0186(13) -0.0133(12) -0.0023(13) C17 0.0487(16) 0.0570(18) 0.0477(16) -0.0249(14) -0.0204(13) 0.0053(14) C18 0.0413(16) 0.0648(19) 0.0530(17) -0.0311(15) -0.0108(13) 0.0038(14) C19 0.0697(19) 0.0557(18) 0.0477(16) -0.0178(14) -0.0239(15) -0.0088(15) C20 0.092(2) 0.0513(19) 0.072(2) -0.0219(16) -0.0334(18) -0.0051(16) C21 0.096(2) 0.078(2) 0.0454(17) -0.0157(16) -0.0163(17) -0.0211(19) C22 0.091(2) 0.071(2) 0.071(2) -0.0156(17) -0.0463(19) -0.0059(18) C23 0.0546(17) 0.0476(16) 0.0407(15) -0.0158(13) -0.0118(13) -0.0067(13) C24 0.0519(17) 0.0518(18) 0.0571(17) -0.0196(14) -0.0144(14) -0.0079(14) C25 0.067(2) 0.064(2) 0.090(2) -0.0319(19) -0.0217(18) -0.0160(17) C26 0.081(2) 0.056(2) 0.091(2) -0.0393(19) -0.023(2) -0.0040(18) C27 0.075(2) 0.061(2) 0.069(2) -0.0355(17) -0.0161(17) 0.0032(17) C28 0.0546(18) 0.0580(18) 0.0465(16) -0.0229(14) -0.0108(13) -0.0037(14) C29 0.0481(17) 0.082(2) 0.087(2) -0.0403(19) -0.0098(16) -0.0122(16) C30 0.124(3) 0.094(3) 0.191(5) -0.094(3) -0.030(3) -0.013(3) C31 0.0583(19) 0.092(2) 0.091(2) -0.053(2) -0.0011(17) -0.0089(18) _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 C23 1.798(3) . ? P1 C16 1.807(3) . ? P1 C19 1.850(3) . ? P1 H1 1.26(2) . ? B1 F1 1.436(3) . ? B1 C7 1.638(4) . ? B1 C1 1.646(4) . ? B1 C13 1.664(4) . ? F2 C2 1.364(3) . ? F3 C3 1.345(4) . ? F4 C4 1.348(3) . ? F5 C5 1.348(3) . ? F6 C6 1.352(3) . ? F7 C8 1.352(4) . ? F8 C9 1.358(4) . ? F9 C10 1.345(4) . ? F10 C11 1.349(4) . ? F11 C12 1.362(4) . ? F12 C14 1.354(3) . ? F13 C15 1.345(3) . ? F14 C17 1.346(3) . ? F15 C18 1.355(3) . ? C1 C2 1.379(4) . ? C1 C6 1.383(4) . ? C2 C3 1.376(4) . ? C3 C4 1.368(4) . ? C4 C5 1.362(4) . ? C5 C6 1.379(4) . ? C7 C8 1.385(4) . ? C7 C12 1.386(4) . ? C8 C9 1.365(5) . ? C9 C10 1.353(5) . ? C10 C11 1.363(5) . ? C11 C12 1.379(5) . ? C13 C18 1.379(3) . ? C13 C14 1.384(3) . ? C14 C15 1.379(3) . ? C15 C16 1.391(3) . ? C16 C17 1.382(3) . ? C17 C18 1.381(3) . ? C19 C22 1.526(4) . ? C19 C20 1.535(4) . ? C19 C21 1.547(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.409(4) . ? C23 C28 1.414(3) . ? C24 C25 1.389(4) . ? C24 C29 1.501(4) . ? C25 C26 1.379(4) . ? C25 H25A 0.9300 . ? C26 C27 1.374(4) . ? C26 C30 1.513(4) . ? C27 C28 1.388(4) . ? C27 H27A 0.9300 . ? C28 C31 1.508(4) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 P1 C16 112.02(12) . . ? C23 P1 C19 114.40(12) . . ? C16 P1 C19 117.51(12) . . ? C23 P1 H1 109.2(9) . . ? C16 P1 H1 99.8(9) . . ? C19 P1 H1 101.9(9) . . ? F1 B1 C7 110.1(2) . . ? F1 B1 C1 104.8(2) . . ? C7 B1 C1 113.7(2) . . ? F1 B1 C13 106.4(2) . . ? C7 B1 C13 106.8(2) . . ? C1 B1 C13 114.8(2) . . ? C2 C1 C6 113.0(3) . . ? C2 C1 B1 118.8(2) . . ? C6 C1 B1 127.6(3) . . ? F2 C2 C3 115.8(3) . . ? F2 C2 C1 119.1(2) . . ? C3 C2 C1 125.2(3) . . ? F3 C3 C4 120.4(3) . . ? F3 C3 C2 120.9(3) . . ? C4 C3 C2 118.7(3) . . ? F4 C4 C5 120.7(3) . . ? F4 C4 C3 119.9(4) . . ? C5 C4 C3 119.3(3) . . ? F5 C5 C4 119.5(3) . . ? F5 C5 C6 120.7(3) . . ? C4 C5 C6 119.8(3) . . ? F6 C6 C5 115.0(3) . . ? F6 C6 C1 121.0(3) . . ? C5 C6 C1 124.0(3) . . ? C8 C7 C12 112.6(3) . . ? C8 C7 B1 126.1(3) . . ? C12 C7 B1 121.3(3) . . ? F7 C8 C9 115.6(3) . . ? F7 C8 C7 120.4(3) . . ? C9 C8 C7 124.0(3) . . ? C10 C9 F8 118.3(4) . . ? C10 C9 C8 120.9(4) . . ? F8 C9 C8 120.8(4) . . ? F9 C10 C9 121.8(5) . . ? F9 C10 C11 119.5(5) . . ? C9 C10 C11 118.7(4) . . ? F10 C11 C10 121.3(4) . . ? F10 C11 C12 119.5(4) . . ? C10 C11 C12 119.1(4) . . ? F11 C12 C11 117.2(3) . . ? F11 C12 C7 118.1(3) . . ? C11 C12 C7 124.8(3) . . ? C18 C13 C14 112.9(2) . . ? C18 C13 B1 127.6(2) . . ? C14 C13 B1 119.5(2) . . ? F12 C14 C15 116.0(2) . . ? F12 C14 C13 119.9(2) . . ? C15 C14 C13 124.0(2) . . ? F13 C15 C14 118.9(2) . . ? F13 C15 C16 119.3(2) . . ? C14 C15 C16 121.8(2) . . ? C17 C16 C15 115.2(2) . . ? C17 C16 P1 128.45(19) . . ? C15 C16 P1 116.37(19) . . ? F14 C17 C18 118.6(2) . . ? F14 C17 C16 119.9(2) . . ? C18 C17 C16 121.4(2) . . ? F15 C18 C13 120.1(2) . . ? F15 C18 C17 115.3(2) . . ? C13 C18 C17 124.6(2) . . ? C22 C19 C20 112.0(2) . . ? C22 C19 C21 109.1(2) . . ? C20 C19 C21 109.1(2) . . ? C22 C19 P1 114.3(2) . . ? C20 C19 P1 108.42(18) . . ? C21 C19 P1 103.47(19) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 120.3(2) . . ? C24 C23 P1 120.7(2) . . ? C28 C23 P1 119.0(2) . . ? C25 C24 C23 118.0(3) . . ? C25 C24 C29 118.0(3) . . ? C23 C24 C29 124.0(2) . . ? C26 C25 C24 122.8(3) . . ? C26 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? C27 C26 C25 118.0(3) . . ? C27 C26 C30 121.0(3) . . ? C25 C26 C30 121.0(3) . . ? C26 C27 C28 122.8(3) . . ? C26 C27 H27A 118.6 . . ? C28 C27 H27A 118.6 . . ? C27 C28 C23 118.1(3) . . ? C27 C28 C31 117.1(3) . . ? C23 C28 C31 124.8(2) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 F1 B1 C1 C2 59.6(3) . . . . ? C7 B1 C1 C2 179.9(2) . . . . ? C13 B1 C1 C2 -56.7(3) . . . . ? F1 B1 C1 C6 -110.6(3) . . . . ? C7 B1 C1 C6 9.7(4) . . . . ? C13 B1 C1 C6 133.1(3) . . . . ? C6 C1 C2 F2 -179.0(2) . . . . ? B1 C1 C2 F2 9.5(4) . . . . ? C6 C1 C2 C3 1.3(4) . . . . ? B1 C1 C2 C3 -170.3(3) . . . . ? F2 C2 C3 F3 -0.9(4) . . . . ? C1 C2 C3 F3 178.8(3) . . . . ? F2 C2 C3 C4 179.3(3) . . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? F3 C3 C4 F4 0.9(5) . . . . ? C2 C3 C4 F4 -179.4(3) . . . . ? F3 C3 C4 C5 179.5(3) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? F4 C4 C5 F5 -0.5(5) . . . . ? C3 C4 C5 F5 -179.2(3) . . . . ? F4 C4 C5 C6 -179.5(2) . . . . ? C3 C4 C5 C6 1.8(5) . . . . ? F5 C5 C6 F6 -1.9(4) . . . . ? C4 C5 C6 F6 177.1(3) . . . . ? F5 C5 C6 C1 179.6(2) . . . . ? C4 C5 C6 C1 -1.4(5) . . . . ? C2 C1 C6 F6 -178.5(2) . . . . ? B1 C1 C6 F6 -7.8(4) . . . . ? C2 C1 C6 C5 -0.1(4) . . . . ? B1 C1 C6 C5 170.5(3) . . . . ? F1 B1 C7 C8 7.8(4) . . . . ? C1 B1 C7 C8 -109.4(3) . . . . ? C13 B1 C7 C8 122.9(3) . . . . ? F1 B1 C7 C12 -172.4(2) . . . . ? C1 B1 C7 C12 70.4(3) . . . . ? C13 B1 C7 C12 -57.2(3) . . . . ? C12 C7 C8 F7 -179.5(2) . . . . ? B1 C7 C8 F7 0.3(4) . . . . ? C12 C7 C8 C9 0.8(4) . . . . ? B1 C7 C8 C9 -179.3(3) . . . . ? F7 C8 C9 C10 179.6(3) . . . . ? C7 C8 C9 C10 -0.7(5) . . . . ? F7 C8 C9 F8 0.9(4) . . . . ? C7 C8 C9 F8 -179.4(3) . . . . ? F8 C9 C10 F9 -1.7(5) . . . . ? C8 C9 C10 F9 179.6(3) . . . . ? F8 C9 C10 C11 178.9(3) . . . . ? C8 C9 C10 C11 0.2(5) . . . . ? F9 C10 C11 F10 1.3(5) . . . . ? C9 C10 C11 F10 -179.3(3) . . . . ? F9 C10 C11 C12 -179.3(3) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? F10 C11 C12 F11 0.1(4) . . . . ? C10 C11 C12 F11 -179.2(3) . . . . ? F10 C11 C12 C7 179.5(3) . . . . ? C10 C11 C12 C7 0.1(5) . . . . ? C8 C7 C12 F11 178.8(2) . . . . ? B1 C7 C12 F11 -1.0(4) . . . . ? C8 C7 C12 C11 -0.5(4) . . . . ? B1 C7 C12 C11 179.6(3) . . . . ? F1 B1 C13 C18 -136.0(3) . . . . ? C7 B1 C13 C18 106.4(3) . . . . ? C1 B1 C13 C18 -20.6(4) . . . . ? F1 B1 C13 C14 46.1(3) . . . . ? C7 B1 C13 C14 -71.6(3) . . . . ? C1 B1 C13 C14 161.4(2) . . . . ? C18 C13 C14 F12 -177.8(2) . . . . ? B1 C13 C14 F12 0.5(4) . . . . ? C18 C13 C14 C15 1.1(4) . . . . ? B1 C13 C14 C15 179.3(3) . . . . ? F12 C14 C15 F13 -0.9(4) . . . . ? C13 C14 C15 F13 -179.8(2) . . . . ? F12 C14 C15 C16 178.2(2) . . . . ? C13 C14 C15 C16 -0.7(4) . . . . ? F13 C15 C16 C17 179.4(2) . . . . ? C14 C15 C16 C17 0.4(4) . . . . ? F13 C15 C16 P1 -0.1(3) . . . . ? C14 C15 C16 P1 -179.1(2) . . . . ? C23 P1 C16 C17 -103.6(3) . . . . ? C19 P1 C16 C17 31.9(3) . . . . ? C23 P1 C16 C15 75.8(2) . . . . ? C19 P1 C16 C15 -148.7(2) . . . . ? C15 C16 C17 F14 -179.5(2) . . . . ? P1 C16 C17 F14 -0.1(4) . . . . ? C15 C16 C17 C18 -0.5(4) . . . . ? P1 C16 C17 C18 178.9(2) . . . . ? C14 C13 C18 F15 179.0(2) . . . . ? B1 C13 C18 F15 0.9(4) . . . . ? C14 C13 C18 C17 -1.3(4) . . . . ? B1 C13 C18 C17 -179.3(3) . . . . ? F14 C17 C18 F15 -0.1(4) . . . . ? C16 C17 C18 F15 -179.2(2) . . . . ? F14 C17 C18 C13 -179.9(2) . . . . ? C16 C17 C18 C13 1.0(4) . . . . ? C23 P1 C19 C22 50.2(2) . . . . ? C16 P1 C19 C22 -84.3(2) . . . . ? C23 P1 C19 C20 175.95(19) . . . . ? C16 P1 C19 C20 41.5(2) . . . . ? C23 P1 C19 C21 -68.3(2) . . . . ? C16 P1 C19 C21 157.25(17) . . . . ? C16 P1 C23 C24 55.2(2) . . . . ? C19 P1 C23 C24 -81.8(2) . . . . ? C16 P1 C23 C28 -125.7(2) . . . . ? C19 P1 C23 C28 97.4(2) . . . . ? C28 C23 C24 C25 -1.6(4) . . . . ? P1 C23 C24 C25 177.5(2) . . . . ? C28 C23 C24 C29 175.8(3) . . . . ? P1 C23 C24 C29 -5.0(4) . . . . ? C23 C24 C25 C26 -0.3(5) . . . . ? C29 C24 C25 C26 -177.9(3) . . . . ? C24 C25 C26 C27 2.1(5) . . . . ? C24 C25 C26 C30 -179.1(3) . . . . ? C25 C26 C27 C28 -2.0(5) . . . . ? C30 C26 C27 C28 179.2(3) . . . . ? C26 C27 C28 C23 0.2(4) . . . . ? C26 C27 C28 C31 179.4(3) . . . . ? C24 C23 C28 C27 1.7(4) . . . . ? P1 C23 C28 C27 -177.4(2) . . . . ? C24 C23 C28 C31 -177.5(3) . . . . ? P1 C23 C28 C31 3.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.291 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.039 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 1 -0.071 0.000 0.500 365.0 76.5 _platon_squeeze_details ; ; #===end data_nBu3P-C6F4-BF(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 698999' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C30 H27 B F15 P' _chemical_formula_weight 714.30 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.2247(16) _cell_length_b 16.029(3) _cell_length_c 21.638(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.781(2) _cell_angle_gamma 90.00 _cell_volume 3143.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 296(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 29420 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5502 _reflns_number_gt 3934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0838P)^2^+1.4688P] 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 5502 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1678 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.45710(8) 0.37009(5) 0.16143(4) 0.0634(3) Uani 1 1 d . . . B1 B 1.0226(3) 0.6036(2) 0.21570(16) 0.0573(8) Uani 1 1 d . . . F1 F 1.14782(18) 0.56737(11) 0.19753(9) 0.0730(5) Uani 1 1 d . . . F2 F 1.1842(2) 0.76104(13) 0.24232(10) 0.0928(7) Uani 1 1 d . . . F3 F 1.1568(3) 0.89855(14) 0.17281(13) 0.1116(8) Uani 1 1 d . . . F4 F 0.9656(3) 0.90411(15) 0.06182(12) 0.1153(8) Uani 1 1 d . . . F5 F 0.7896(3) 0.76978(19) 0.02481(11) 0.1297(9) Uani 1 1 d . . . F6 F 0.8043(3) 0.63547(15) 0.09513(10) 0.1083(8) Uani 1 1 d . . . F7 F 0.9330(2) 0.74555(11) 0.29638(9) 0.0744(5) Uani 1 1 d . . . F8 F 1.0050(3) 0.75665(16) 0.42009(11) 0.1100(8) Uani 1 1 d . . . F9 F 1.1837(3) 0.6415(2) 0.48720(11) 0.1469(12) Uani 1 1 d . . . F10 F 1.2743(3) 0.5074(2) 0.42711(13) 0.1354(10) Uani 1 1 d . . . F11 F 1.1842(3) 0.48745(14) 0.30464(12) 0.1052(7) Uani 1 1 d . . . F12 F 0.72808(19) 0.63599(11) 0.24046(10) 0.0833(6) Uani 1 1 d . . . F13 F 0.49579(19) 0.53884(12) 0.21988(11) 0.0866(6) Uani 1 1 d . . . F14 F 0.7694(2) 0.33907(11) 0.12985(11) 0.0849(6) Uani 1 1 d . . . F15 F 1.0002(2) 0.43276(12) 0.15380(12) 0.0919(7) Uani 1 1 d . . . C1 C 0.9926(3) 0.69028(19) 0.17406(14) 0.0603(7) Uani 1 1 d . . . C2 C 1.0801(4) 0.7607(2) 0.18913(16) 0.0678(8) Uani 1 1 d . . . C3 C 1.0720(4) 0.8318(2) 0.15373(18) 0.0775(9) Uani 1 1 d . . . C4 C 0.9743(4) 0.8353(2) 0.09803(18) 0.0811(10) Uani 1 1 d . . . C5 C 0.8870(4) 0.7684(3) 0.07957(16) 0.0825(10) Uani 1 1 d . . . C6 C 0.8972(4) 0.6987(2) 0.11768(15) 0.0722(8) Uani 1 1 d . . . C7 C 1.0585(3) 0.61728(18) 0.29273(14) 0.0602(7) Uani 1 1 d . . . C8 C 1.0162(3) 0.6829(2) 0.32667(15) 0.0636(8) Uani 1 1 d . . . C9 C 1.0527(4) 0.6912(3) 0.39072(17) 0.0804(10) Uani 1 1 d . . . C10 C 1.1422(5) 0.6322(3) 0.42493(18) 0.0951(13) Uani 1 1 d . . . C11 C 1.1863(4) 0.5653(3) 0.3942(2) 0.0935(12) Uani 1 1 d . . . C12 C 1.1423(4) 0.5579(2) 0.33059(17) 0.0756(9) Uani 1 1 d . . . C13 C 0.8792(3) 0.53962(17) 0.20060(13) 0.0547(7) Uani 1 1 d . . . C14 C 0.7439(3) 0.56029(17) 0.21522(14) 0.0581(7) Uani 1 1 d . . . C15 C 0.6218(3) 0.51077(18) 0.20410(14) 0.0585(7) Uani 1 1 d . . . C16 C 0.6226(3) 0.43292(17) 0.17601(13) 0.0550(7) Uani 1 1 d . . . C17 C 0.7569(3) 0.41154(17) 0.16014(14) 0.0588(7) Uani 1 1 d . . . C18 C 0.8788(3) 0.46224(18) 0.17253(14) 0.0594(7) Uani 1 1 d . . . C19 C 0.3846(4) 0.3609(2) 0.23214(18) 0.0796(10) Uani 1 1 d . . . H19A H 0.3592 0.4162 0.2450 0.096 Uiso 1 1 calc R . . H19B H 0.2944 0.3284 0.2233 0.096 Uiso 1 1 calc R . . C20 C 0.4876(5) 0.3212(3) 0.28544(19) 0.0998(12) Uani 1 1 d . . . H20A H 0.5793 0.3524 0.2934 0.120 Uiso 1 1 calc R . . H20B H 0.5100 0.2650 0.2733 0.120 Uiso 1 1 calc R . . C21 C 0.4262(6) 0.3170(4) 0.3456(2) 0.1234(17) Uani 1 1 d . . . H21A H 0.4063 0.3732 0.3584 0.148 Uiso 1 1 calc R . . H21B H 0.3332 0.2870 0.3374 0.148 Uiso 1 1 calc R . . C22 C 0.5260(9) 0.2759(6) 0.3975(3) 0.202(4) Uani 1 1 d . . . H22A H 0.4814 0.2752 0.4342 0.303 Uiso 1 1 calc R . . H22B H 0.6176 0.3059 0.4065 0.303 Uiso 1 1 calc R . . H22C H 0.5442 0.2197 0.3857 0.303 Uiso 1 1 calc R . . C23 C 0.4986(4) 0.2686(2) 0.13368(16) 0.0709(8) Uani 1 1 d . . . H23A H 0.5299 0.2751 0.0936 0.085 Uiso 1 1 calc R . . H23B H 0.5810 0.2453 0.1631 0.085 Uiso 1 1 calc R . . C24 C 0.3713(4) 0.2069(2) 0.12552(16) 0.0726(9) Uani 1 1 d . . . H24A H 0.3367 0.2015 0.1650 0.087 Uiso 1 1 calc R . . H24B H 0.2904 0.2281 0.0943 0.087 Uiso 1 1 calc R . . C25 C 0.4164(5) 0.1224(2) 0.1053(2) 0.0941(12) Uani 1 1 d . . . H25A H 0.4974 0.1015 0.1366 0.113 Uiso 1 1 calc R . . H25B H 0.4518 0.1282 0.0660 0.113 Uiso 1 1 calc R . . C26 C 0.2913(6) 0.0593(3) 0.0964(2) 0.1165(15) Uani 1 1 d . . . H26A H 0.3262 0.0067 0.0839 0.175 Uiso 1 1 calc R . . H26B H 0.2119 0.0788 0.0644 0.175 Uiso 1 1 calc R . . H26C H 0.2566 0.0526 0.1353 0.175 Uiso 1 1 calc R . . C27 C 0.3190(4) 0.4239(3) 0.1061(2) 0.1009(13) Uani 1 1 d . . . H27A H 0.2390 0.3850 0.0923 0.121 Uiso 1 1 calc R . . H27B H 0.2798 0.4682 0.1287 0.121 Uiso 1 1 calc R . . C28 C 0.3577(6) 0.4592(5) 0.0521(3) 0.159(3) Uani 1 1 d . . . H28A H 0.3848 0.4146 0.0262 0.191 Uiso 1 1 calc R . . H28B H 0.4443 0.4939 0.0650 0.191 Uiso 1 1 calc R . . C29 C 0.2364(8) 0.5125(4) 0.0115(3) 0.152(2) Uani 1 1 d . . . H29A H 0.2599 0.5162 -0.0303 0.182 Uiso 1 1 calc R . . H29B H 0.1444 0.4820 0.0074 0.182 Uiso 1 1 calc R . . C30 C 0.2101(12) 0.5943(5) 0.0307(4) 0.217(4) Uani 1 1 d . . . H30A H 0.1298 0.6184 0.0016 0.326 Uiso 1 1 calc R . . H30B H 0.2972 0.6275 0.0319 0.326 Uiso 1 1 calc R . . H30C H 0.1855 0.5927 0.0719 0.326 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0515(4) 0.0624(5) 0.0761(5) -0.0011(4) 0.0115(4) -0.0093(3) B1 0.0475(17) 0.0570(19) 0.069(2) -0.0069(15) 0.0160(15) -0.0019(14) F1 0.0519(9) 0.0763(11) 0.0944(13) -0.0099(9) 0.0232(9) -0.0010(8) F2 0.0749(12) 0.0976(15) 0.0978(15) 0.0169(11) -0.0045(11) -0.0348(11) F3 0.1119(17) 0.0805(14) 0.142(2) 0.0197(14) 0.0231(15) -0.0300(13) F4 0.132(2) 0.1007(16) 0.1215(19) 0.0482(15) 0.0451(15) 0.0208(15) F5 0.145(2) 0.153(2) 0.0800(15) 0.0321(15) -0.0085(15) -0.0021(18) F6 0.1312(19) 0.1052(16) 0.0749(13) 0.0001(11) -0.0154(13) -0.0321(14) F7 0.0682(11) 0.0663(11) 0.0911(13) -0.0115(9) 0.0209(9) -0.0016(9) F8 0.1106(17) 0.135(2) 0.0937(15) -0.0455(14) 0.0427(13) -0.0435(15) F9 0.142(2) 0.227(3) 0.0651(14) 0.0091(17) 0.0015(14) -0.057(2) F10 0.1092(18) 0.161(2) 0.124(2) 0.0685(18) -0.0105(16) -0.0018(17) F11 0.1053(16) 0.0810(14) 0.1275(19) 0.0193(13) 0.0169(14) 0.0255(12) F12 0.0596(10) 0.0739(12) 0.1203(16) -0.0406(11) 0.0274(10) -0.0072(9) F13 0.0525(10) 0.0873(13) 0.1265(16) -0.0391(12) 0.0333(10) -0.0061(9) F14 0.0679(11) 0.0588(10) 0.1343(17) -0.0270(11) 0.0353(11) -0.0043(8) F15 0.0583(10) 0.0715(12) 0.1554(19) -0.0314(12) 0.0445(12) -0.0038(9) C1 0.0545(16) 0.0666(18) 0.0623(18) -0.0026(14) 0.0169(14) -0.0018(14) C2 0.0601(18) 0.070(2) 0.075(2) 0.0071(16) 0.0169(16) -0.0077(15) C3 0.072(2) 0.072(2) 0.092(3) 0.0106(18) 0.0233(19) -0.0054(17) C4 0.086(2) 0.075(2) 0.090(3) 0.022(2) 0.038(2) 0.012(2) C5 0.084(2) 0.105(3) 0.058(2) 0.0102(19) 0.0110(17) 0.010(2) C6 0.076(2) 0.077(2) 0.0638(19) -0.0038(17) 0.0134(16) -0.0061(17) C7 0.0482(15) 0.0617(18) 0.0699(18) 0.0043(14) 0.0092(13) -0.0095(13) C8 0.0522(16) 0.0667(19) 0.073(2) -0.0029(15) 0.0145(14) -0.0137(14) C9 0.072(2) 0.099(3) 0.075(2) -0.018(2) 0.0246(18) -0.034(2) C10 0.083(3) 0.136(4) 0.064(2) 0.008(3) 0.006(2) -0.037(3) C11 0.074(2) 0.116(3) 0.085(3) 0.036(3) -0.001(2) -0.015(2) C12 0.0634(19) 0.075(2) 0.087(2) 0.0113(18) 0.0108(17) -0.0040(16) C13 0.0484(15) 0.0566(16) 0.0598(16) -0.0014(13) 0.0119(12) 0.0001(12) C14 0.0517(16) 0.0569(16) 0.0666(18) -0.0136(14) 0.0128(13) 0.0003(13) C15 0.0464(15) 0.0659(18) 0.0660(18) -0.0087(14) 0.0172(13) 0.0006(13) C16 0.0484(15) 0.0531(16) 0.0638(17) -0.0003(13) 0.0110(12) -0.0019(12) C17 0.0553(16) 0.0468(15) 0.0760(19) -0.0046(14) 0.0165(14) 0.0019(12) C18 0.0481(16) 0.0547(16) 0.078(2) -0.0010(14) 0.0196(14) 0.0037(13) C19 0.065(2) 0.080(2) 0.100(3) -0.0109(19) 0.0315(19) -0.0166(17) C20 0.086(3) 0.121(3) 0.097(3) 0.008(2) 0.028(2) -0.015(2) C21 0.125(4) 0.155(5) 0.100(3) 0.010(3) 0.045(3) -0.017(3) C22 0.185(7) 0.306(10) 0.113(5) 0.065(6) 0.024(5) -0.006(7) C23 0.070(2) 0.069(2) 0.077(2) -0.0075(16) 0.0201(16) -0.0136(16) C24 0.070(2) 0.072(2) 0.077(2) -0.0033(16) 0.0159(16) -0.0153(16) C25 0.094(3) 0.067(2) 0.125(3) -0.014(2) 0.029(2) -0.0089(19) C26 0.127(4) 0.081(3) 0.144(4) -0.019(3) 0.030(3) -0.028(3) C27 0.065(2) 0.095(3) 0.132(4) 0.016(3) -0.009(2) -0.016(2) C28 0.101(4) 0.222(7) 0.137(5) 0.073(5) -0.020(3) -0.021(4) C29 0.169(5) 0.125(4) 0.135(5) 0.020(4) -0.038(4) 0.006(4) C30 0.334(13) 0.146(6) 0.166(7) -0.004(5) 0.032(7) 0.014(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 C19 1.787(4) . ? P1 C27 1.797(4) . ? P1 C23 1.800(3) . ? P1 C16 1.807(3) . ? B1 F1 1.413(4) . ? B1 C1 1.650(5) . ? B1 C7 1.652(5) . ? B1 C13 1.658(4) . ? F2 C2 1.354(4) . ? F3 C3 1.344(4) . ? F4 C4 1.346(4) . ? F5 C5 1.346(4) . ? F6 C6 1.357(4) . ? F7 C8 1.357(4) . ? F8 C9 1.343(4) . ? F9 C10 1.338(5) . ? F10 C11 1.346(5) . ? F11 C12 1.349(4) . ? F12 C14 1.350(3) . ? F13 C15 1.349(3) . ? F14 C17 1.349(3) . ? F15 C18 1.346(3) . ? C1 C6 1.371(4) . ? C1 C2 1.390(4) . ? C2 C3 1.368(5) . ? C3 C4 1.365(5) . ? C4 C5 1.357(5) . ? C5 C6 1.381(5) . ? C7 C8 1.379(4) . ? C7 C12 1.392(4) . ? C8 C9 1.370(5) . ? C9 C10 1.376(6) . ? C10 C11 1.364(6) . ? C11 C12 1.365(5) . ? C13 C18 1.381(4) . ? C13 C14 1.383(4) . ? C14 C15 1.362(4) . ? C15 C16 1.389(4) . ? C16 C17 1.388(4) . ? C17 C18 1.373(4) . ? C19 C20 1.493(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.516(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.468(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.520(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.507(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.520(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.403(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.545(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.410(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 P1 C27 106.1(2) . . ? C19 P1 C23 110.40(16) . . ? C27 P1 C23 112.4(2) . . ? C19 P1 C16 109.62(15) . . ? C27 P1 C16 108.62(16) . . ? C23 P1 C16 109.65(14) . . ? F1 B1 C1 104.9(2) . . ? F1 B1 C7 108.4(2) . . ? C1 B1 C7 114.9(2) . . ? F1 B1 C13 110.8(2) . . ? C1 B1 C13 111.6(2) . . ? C7 B1 C13 106.4(2) . . ? C6 C1 C2 112.2(3) . . ? C6 C1 B1 125.6(3) . . ? C2 C1 B1 121.6(3) . . ? F2 C2 C3 115.3(3) . . ? F2 C2 C1 119.4(3) . . ? C3 C2 C1 125.2(3) . . ? F3 C3 C4 119.2(3) . . ? F3 C3 C2 121.6(3) . . ? C4 C3 C2 119.2(3) . . ? F4 C4 C5 120.6(4) . . ? F4 C4 C3 120.4(4) . . ? C5 C4 C3 119.0(3) . . ? F5 C5 C4 120.5(4) . . ? F5 C5 C6 119.9(4) . . ? C4 C5 C6 119.6(3) . . ? F6 C6 C1 120.3(3) . . ? F6 C6 C5 114.9(3) . . ? C1 C6 C5 124.8(3) . . ? C8 C7 C12 112.9(3) . . ? C8 C7 B1 127.9(3) . . ? C12 C7 B1 119.2(3) . . ? F7 C8 C9 115.2(3) . . ? F7 C8 C7 119.9(3) . . ? C9 C8 C7 124.9(3) . . ? F8 C9 C8 121.0(4) . . ? F8 C9 C10 119.9(4) . . ? C8 C9 C10 119.1(4) . . ? F9 C10 C11 121.6(5) . . ? F9 C10 C9 119.6(5) . . ? C11 C10 C9 118.8(4) . . ? F10 C11 C10 119.3(4) . . ? F10 C11 C12 120.7(5) . . ? C10 C11 C12 120.0(4) . . ? F11 C12 C11 116.0(3) . . ? F11 C12 C7 119.9(3) . . ? C11 C12 C7 124.2(4) . . ? C18 C13 C14 112.8(3) . . ? C18 C13 B1 125.4(2) . . ? C14 C13 B1 121.8(2) . . ? F12 C14 C15 116.5(2) . . ? F12 C14 C13 118.6(2) . . ? C15 C14 C13 124.8(3) . . ? F13 C15 C14 119.0(2) . . ? F13 C15 C16 119.1(2) . . ? C14 C15 C16 121.9(3) . . ? C17 C16 C15 114.1(2) . . ? C17 C16 P1 125.7(2) . . ? C15 C16 P1 120.2(2) . . ? F14 C17 C18 117.6(2) . . ? F14 C17 C16 119.6(2) . . ? C18 C17 C16 122.8(3) . . ? F15 C18 C17 115.5(3) . . ? F15 C18 C13 120.9(2) . . ? C17 C18 C13 123.5(3) . . ? C20 C19 P1 114.2(3) . . ? C20 C19 H19A 108.7 . . ? P1 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? P1 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 C21 113.3(4) . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 113.2(5) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P1 114.7(2) . . ? C24 C23 H23A 108.6 . . ? P1 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? P1 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C23 111.7(3) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 113.0(3) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 P1 119.3(4) . . ? C28 C27 H27A 107.5 . . ? P1 C27 H27A 107.5 . . ? C28 C27 H27B 107.5 . . ? P1 C27 H27B 107.5 . . ? H27A C27 H27B 107.0 . . ? C27 C28 C29 115.3(5) . . ? C27 C28 H28A 108.4 . . ? C29 C28 H28A 108.4 . . ? C27 C28 H28B 108.4 . . ? C29 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? C30 C29 C28 119.4(6) . . ? C30 C29 H29A 107.5 . . ? C28 C29 H29A 107.5 . . ? C30 C29 H29B 107.5 . . ? C28 C29 H29B 107.5 . . ? H29A C29 H29B 107.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 F1 B1 C1 C6 94.8(3) . . . . ? C7 B1 C1 C6 -146.4(3) . . . . ? C13 B1 C1 C6 -25.1(4) . . . . ? F1 B1 C1 C2 -75.6(3) . . . . ? C7 B1 C1 C2 43.2(4) . . . . ? C13 B1 C1 C2 164.5(3) . . . . ? C6 C1 C2 F2 -177.5(3) . . . . ? B1 C1 C2 F2 -5.9(4) . . . . ? C6 C1 C2 C3 1.7(5) . . . . ? B1 C1 C2 C3 173.2(3) . . . . ? F2 C2 C3 F3 -3.5(5) . . . . ? C1 C2 C3 F3 177.3(3) . . . . ? F2 C2 C3 C4 177.3(3) . . . . ? C1 C2 C3 C4 -1.9(5) . . . . ? F3 C3 C4 F4 1.7(5) . . . . ? C2 C3 C4 F4 -179.0(3) . . . . ? F3 C3 C4 C5 -178.7(3) . . . . ? C2 C3 C4 C5 0.5(5) . . . . ? F4 C4 C5 F5 -0.3(5) . . . . ? C3 C4 C5 F5 -179.8(3) . . . . ? F4 C4 C5 C6 -179.6(3) . . . . ? C3 C4 C5 C6 0.8(5) . . . . ? C2 C1 C6 F6 179.3(3) . . . . ? B1 C1 C6 F6 8.1(5) . . . . ? C2 C1 C6 C5 -0.2(5) . . . . ? B1 C1 C6 C5 -171.3(3) . . . . ? F5 C5 C6 F6 0.2(5) . . . . ? C4 C5 C6 F6 179.5(3) . . . . ? F5 C5 C6 C1 179.6(3) . . . . ? C4 C5 C6 C1 -1.0(6) . . . . ? F1 B1 C7 C8 142.6(3) . . . . ? C1 B1 C7 C8 25.7(4) . . . . ? C13 B1 C7 C8 -98.2(3) . . . . ? F1 B1 C7 C12 -36.7(4) . . . . ? C1 B1 C7 C12 -153.6(3) . . . . ? C13 B1 C7 C12 82.4(3) . . . . ? C12 C7 C8 F7 -179.6(2) . . . . ? B1 C7 C8 F7 1.1(4) . . . . ? C12 C7 C8 C9 0.9(4) . . . . ? B1 C7 C8 C9 -178.5(3) . . . . ? F7 C8 C9 F8 1.3(4) . . . . ? C7 C8 C9 F8 -179.1(3) . . . . ? F7 C8 C9 C10 -177.2(3) . . . . ? C7 C8 C9 C10 2.4(5) . . . . ? F8 C9 C10 F9 -1.4(5) . . . . ? C8 C9 C10 F9 177.2(3) . . . . ? F8 C9 C10 C11 178.4(3) . . . . ? C8 C9 C10 C11 -3.0(5) . . . . ? F9 C10 C11 F10 -0.4(6) . . . . ? C9 C10 C11 F10 179.8(3) . . . . ? F9 C10 C11 C12 -179.8(3) . . . . ? C9 C10 C11 C12 0.4(6) . . . . ? F10 C11 C12 F11 4.2(5) . . . . ? C10 C11 C12 F11 -176.4(3) . . . . ? F10 C11 C12 C7 -176.2(3) . . . . ? C10 C11 C12 C7 3.2(6) . . . . ? C8 C7 C12 F11 175.9(3) . . . . ? B1 C7 C12 F11 -4.6(4) . . . . ? C8 C7 C12 C11 -3.7(5) . . . . ? B1 C7 C12 C11 175.8(3) . . . . ? F1 B1 C13 C18 -1.7(4) . . . . ? C1 B1 C13 C18 114.7(3) . . . . ? C7 B1 C13 C18 -119.3(3) . . . . ? F1 B1 C13 C14 178.8(3) . . . . ? C1 B1 C13 C14 -64.8(4) . . . . ? C7 B1 C13 C14 61.2(4) . . . . ? C18 C13 C14 F12 -177.2(3) . . . . ? B1 C13 C14 F12 2.3(4) . . . . ? C18 C13 C14 C15 0.4(4) . . . . ? B1 C13 C14 C15 180.0(3) . . . . ? F12 C14 C15 F13 -1.4(4) . . . . ? C13 C14 C15 F13 -179.1(3) . . . . ? F12 C14 C15 C16 177.4(3) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? F13 C15 C16 C17 178.2(3) . . . . ? C14 C15 C16 C17 -0.7(4) . . . . ? F13 C15 C16 P1 -0.4(4) . . . . ? C14 C15 C16 P1 -179.3(2) . . . . ? C19 P1 C16 C17 129.8(3) . . . . ? C27 P1 C16 C17 -114.7(3) . . . . ? C23 P1 C16 C17 8.5(3) . . . . ? C19 P1 C16 C15 -51.8(3) . . . . ? C27 P1 C16 C15 63.8(3) . . . . ? C23 P1 C16 C15 -173.1(2) . . . . ? C15 C16 C17 F14 -176.9(3) . . . . ? P1 C16 C17 F14 1.6(4) . . . . ? C15 C16 C17 C18 1.4(4) . . . . ? P1 C16 C17 C18 180.0(2) . . . . ? F14 C17 C18 F15 -1.2(4) . . . . ? C16 C17 C18 F15 -179.6(3) . . . . ? F14 C17 C18 C13 177.0(3) . . . . ? C16 C17 C18 C13 -1.4(5) . . . . ? C14 C13 C18 F15 178.5(3) . . . . ? B1 C13 C18 F15 -1.0(5) . . . . ? C14 C13 C18 C17 0.4(4) . . . . ? B1 C13 C18 C17 -179.2(3) . . . . ? C27 P1 C19 C20 -177.1(3) . . . . ? C23 P1 C19 C20 60.9(3) . . . . ? C16 P1 C19 C20 -60.0(3) . . . . ? P1 C19 C20 C21 177.8(3) . . . . ? C19 C20 C21 C22 178.5(5) . . . . ? C19 P1 C23 C24 53.6(3) . . . . ? C27 P1 C23 C24 -64.6(3) . . . . ? C16 P1 C23 C24 174.5(2) . . . . ? P1 C23 C24 C25 -177.2(3) . . . . ? C23 C24 C25 C26 -179.7(4) . . . . ? C19 P1 C27 C28 163.8(5) . . . . ? C23 P1 C27 C28 -75.5(5) . . . . ? C16 P1 C27 C28 46.0(5) . . . . ? P1 C27 C28 C29 -173.4(4) . . . . ? C27 C28 C29 C30 77.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.663 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.047 #===end data_Ph3P-C6F4-BF(C6F5)2.C6H5Br _database_code_depnum_ccdc_archive 'CCDC 699000' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C42 H20 B Br F15 P' _chemical_formula_weight 931.27 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' 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' Br Br -0.2901 2.4595 '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 12.9407(16) _cell_length_b 13.0760(16) _cell_length_c 13.2779(16) _cell_angle_alpha 68.326(2) _cell_angle_beta 65.310(2) _cell_angle_gamma 72.050(2) _cell_volume 1865.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7351 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.59 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 1.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.606 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 18019 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6552 _reflns_number_gt 5088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0631P)^2^+1.8249P] 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_number_reflns 6552 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 Br1 Br 0.81052(5) 0.14917(5) 0.45965(5) 0.1146(2) Uani 1 1 d . . . P1 P 0.80513(6) 0.71893(6) -0.10507(6) 0.04103(18) Uani 1 1 d . . . B1 B 0.5100(3) 0.3533(3) 0.2620(3) 0.0454(7) Uani 1 1 d . . . F1 F 0.41333(15) 0.37952(15) 0.22588(15) 0.0592(5) Uani 1 1 d . . . F2 F 0.57176(18) 0.12779(15) 0.43227(16) 0.0689(5) Uani 1 1 d . . . F3 F 0.6725(2) -0.06300(17) 0.3799(2) 0.0949(7) Uani 1 1 d . . . F4 F 0.7364(2) -0.0740(2) 0.1602(3) 0.1091(9) Uani 1 1 d . . . F5 F 0.7034(2) 0.1151(2) -0.0074(2) 0.1009(8) Uani 1 1 d . . . F6 F 0.6053(2) 0.31024(18) 0.04263(17) 0.0824(6) Uani 1 1 d . . . F7 F 0.63608(17) 0.39392(18) 0.38263(17) 0.0725(5) Uani 1 1 d . . . F8 F 0.5659(2) 0.3739(2) 0.6067(2) 0.0878(7) Uani 1 1 d . . . F9 F 0.3547(2) 0.3232(2) 0.74839(18) 0.0965(8) Uani 1 1 d . . . F10 F 0.21479(18) 0.2917(2) 0.66065(18) 0.0843(6) Uani 1 1 d . . . F11 F 0.28617(17) 0.30176(19) 0.44064(17) 0.0750(6) Uani 1 1 d . . . F12 F 0.42199(13) 0.59319(14) 0.18563(15) 0.0564(4) Uani 1 1 d . . . F13 F 0.53898(14) 0.74945(13) 0.03483(16) 0.0575(4) Uani 1 1 d . . . F14 F 0.88721(13) 0.48759(14) 0.01428(15) 0.0554(4) Uani 1 1 d . . . F15 F 0.77068(14) 0.33113(13) 0.16620(16) 0.0594(5) Uani 1 1 d . . . C1 C 0.5805(2) 0.2300(2) 0.2398(2) 0.0469(6) Uani 1 1 d . . . C2 C 0.6030(3) 0.1312(3) 0.3206(3) 0.0520(7) Uani 1 1 d . . . C3 C 0.6556(3) 0.0299(3) 0.2958(3) 0.0631(8) Uani 1 1 d . . . C4 C 0.6885(3) 0.0245(3) 0.1856(4) 0.0706(10) Uani 1 1 d . . . C5 C 0.6697(3) 0.1195(3) 0.1022(3) 0.0680(9) Uani 1 1 d . . . C6 C 0.6179(3) 0.2190(3) 0.1298(3) 0.0580(8) Uani 1 1 d . . . C7 C 0.4649(2) 0.3505(2) 0.3979(2) 0.0451(6) Uani 1 1 d . . . C8 C 0.5302(3) 0.3677(2) 0.4484(3) 0.0522(7) Uani 1 1 d . . . C9 C 0.4961(3) 0.3583(3) 0.5636(3) 0.0615(8) Uani 1 1 d . . . C10 C 0.3897(3) 0.3327(3) 0.6352(3) 0.0643(9) Uani 1 1 d . . . C11 C 0.3198(3) 0.3172(3) 0.5909(3) 0.0602(8) Uani 1 1 d . . . C12 C 0.3581(3) 0.3249(2) 0.4754(3) 0.0509(7) Uani 1 1 d . . . C13 C 0.5889(2) 0.4514(2) 0.1782(2) 0.0419(6) Uani 1 1 d . . . C14 C 0.5372(2) 0.5619(2) 0.1418(2) 0.0424(6) Uani 1 1 d . . . C15 C 0.5983(2) 0.6453(2) 0.0622(2) 0.0414(6) Uani 1 1 d . . . C16 C 0.7178(2) 0.6237(2) 0.0132(2) 0.0402(6) Uani 1 1 d . . . C17 C 0.7708(2) 0.5144(2) 0.0540(2) 0.0428(6) Uani 1 1 d . . . C18 C 0.7085(2) 0.4332(2) 0.1332(2) 0.0438(6) Uani 1 1 d . . . C19 C 0.7178(2) 0.8415(2) -0.1677(2) 0.0465(6) Uani 1 1 d . . . C20 C 0.6716(3) 0.9300(3) -0.1182(3) 0.0621(8) Uani 1 1 d . . . H20A H 0.6860 0.9257 -0.0536 0.075 Uiso 1 1 calc R . . C21 C 0.6042(3) 1.0241(3) -0.1658(4) 0.0753(11) Uani 1 1 d . . . H21A H 0.5717 1.0831 -0.1325 0.090 Uiso 1 1 calc R . . C22 C 0.5848(3) 1.0309(3) -0.2622(4) 0.0748(11) Uani 1 1 d . . . H22A H 0.5396 1.0948 -0.2940 0.090 Uiso 1 1 calc R . . C23 C 0.6308(3) 0.9455(3) -0.3116(3) 0.0675(9) Uani 1 1 d . . . H23A H 0.6175 0.9517 -0.3774 0.081 Uiso 1 1 calc R . . C24 C 0.6970(3) 0.8494(3) -0.2650(3) 0.0536(7) Uani 1 1 d . . . H24A H 0.7275 0.7905 -0.2984 0.064 Uiso 1 1 calc R . . C25 C 0.8917(2) 0.7639(2) -0.0589(2) 0.0465(6) Uani 1 1 d . . . C26 C 0.9451(3) 0.8555(3) -0.1327(3) 0.0664(9) Uani 1 1 d . . . H26A H 0.9334 0.8934 -0.2028 0.080 Uiso 1 1 calc R . . C27 C 1.0152(3) 0.8892(3) -0.1010(4) 0.0782(11) Uani 1 1 d . . . H27A H 1.0511 0.9500 -0.1500 0.094 Uiso 1 1 calc R . . C28 C 1.0320(3) 0.8341(4) 0.0018(4) 0.0744(10) Uani 1 1 d . . . H28A H 1.0791 0.8577 0.0227 0.089 Uiso 1 1 calc R . . C29 C 0.9801(3) 0.7440(3) 0.0746(3) 0.0666(9) Uani 1 1 d . . . H29A H 0.9927 0.7064 0.1443 0.080 Uiso 1 1 calc R . . C30 C 0.9091(3) 0.7090(3) 0.0451(3) 0.0522(7) Uani 1 1 d . . . H30A H 0.8731 0.6484 0.0951 0.063 Uiso 1 1 calc R . . C31 C 0.8949(2) 0.6418(2) -0.2082(2) 0.0439(6) Uani 1 1 d . . . C32 C 0.8434(3) 0.5843(3) -0.2390(3) 0.0573(8) Uani 1 1 d . . . H32A H 0.7640 0.5857 -0.2060 0.069 Uiso 1 1 calc R . . C33 C 0.9112(4) 0.5251(3) -0.3190(3) 0.0710(10) Uani 1 1 d . . . H33A H 0.8773 0.4871 -0.3405 0.085 Uiso 1 1 calc R . . C34 C 1.0283(4) 0.5220(3) -0.3668(3) 0.0754(11) Uani 1 1 d . . . H34A H 1.0732 0.4828 -0.4214 0.091 Uiso 1 1 calc R . . C35 C 1.0796(3) 0.5761(3) -0.3347(3) 0.0709(10) Uani 1 1 d . . . H35A H 1.1594 0.5721 -0.3663 0.085 Uiso 1 1 calc R . . C36 C 1.0137(3) 0.6369(3) -0.2555(3) 0.0561(8) Uani 1 1 d . . . H36A H 1.0486 0.6741 -0.2343 0.067 Uiso 1 1 calc R . . C100 C 0.8854(4) 0.1669(4) 0.5461(4) 0.0851(12) Uani 1 1 d . . . C101 C 1.0031(4) 0.1401(4) 0.5136(4) 0.0891(12) Uani 1 1 d . . . H10A H 1.0465 0.1115 0.4506 0.107 Uiso 1 1 calc R . . C102 C 1.0559(5) 0.1560(5) 0.5754(5) 0.1103(16) Uani 1 1 d . . . H10B H 1.1361 0.1384 0.5537 0.132 Uiso 1 1 calc R . . C103 C 0.9940(7) 0.1966(6) 0.6670(6) 0.127(2) Uani 1 1 d . . . H10C H 1.0322 0.2064 0.7077 0.153 Uiso 1 1 calc R . . C104 C 0.8762(7) 0.2239(6) 0.7014(5) 0.131(2) Uani 1 1 d . . . H10D H 0.8345 0.2522 0.7649 0.157 Uiso 1 1 calc R . . C105 C 0.8199(5) 0.2091(5) 0.6414(5) 0.1113(17) Uani 1 1 d . . . H10E H 0.7397 0.2268 0.6638 0.134 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.1115(4) 0.1108(4) 0.1326(5) 0.0041(3) -0.0663(4) -0.0471(3) P1 0.0403(4) 0.0393(4) 0.0439(4) -0.0104(3) -0.0135(3) -0.0104(3) B1 0.0442(17) 0.0459(17) 0.0488(18) -0.0061(14) -0.0208(14) -0.0137(14) F1 0.0514(10) 0.0664(11) 0.0651(11) -0.0036(9) -0.0293(8) -0.0225(8) F2 0.0923(14) 0.0529(11) 0.0546(11) -0.0070(8) -0.0314(10) -0.0053(10) F3 0.1118(18) 0.0516(12) 0.1062(18) -0.0135(12) -0.0454(15) 0.0060(12) F4 0.113(2) 0.0810(16) 0.130(2) -0.0641(16) -0.0278(17) 0.0086(14) F5 0.122(2) 0.119(2) 0.0750(15) -0.0551(14) -0.0138(14) -0.0327(16) F6 0.1296(19) 0.0775(14) 0.0507(11) -0.0077(10) -0.0366(12) -0.0374(13) F7 0.0631(12) 0.0988(15) 0.0685(12) -0.0141(11) -0.0293(10) -0.0336(11) F8 0.1131(18) 0.0990(17) 0.0826(15) -0.0285(13) -0.0557(14) -0.0254(14) F9 0.124(2) 0.1123(19) 0.0550(12) -0.0362(12) -0.0193(12) -0.0237(15) F10 0.0657(13) 0.0977(16) 0.0630(12) -0.0207(11) 0.0026(10) -0.0166(11) F11 0.0598(11) 0.1075(16) 0.0632(12) -0.0139(11) -0.0175(9) -0.0401(11) F12 0.0356(8) 0.0562(10) 0.0623(10) -0.0115(8) -0.0086(7) -0.0062(7) F13 0.0456(9) 0.0386(9) 0.0726(11) -0.0093(8) -0.0153(8) -0.0013(7) F14 0.0348(8) 0.0495(9) 0.0701(11) -0.0096(8) -0.0152(8) -0.0050(7) F15 0.0482(9) 0.0398(9) 0.0819(12) -0.0016(8) -0.0300(9) -0.0052(7) C1 0.0465(15) 0.0495(16) 0.0498(16) -0.0113(13) -0.0158(13) -0.0196(13) C2 0.0502(17) 0.0515(17) 0.0568(18) -0.0131(14) -0.0191(14) -0.0139(13) C3 0.061(2) 0.0495(18) 0.077(2) -0.0149(17) -0.0246(17) -0.0085(15) C4 0.060(2) 0.064(2) 0.090(3) -0.040(2) -0.0147(19) -0.0074(17) C5 0.066(2) 0.085(3) 0.065(2) -0.038(2) -0.0099(17) -0.0262(19) C6 0.068(2) 0.061(2) 0.0541(18) -0.0143(16) -0.0198(15) -0.0271(16) C7 0.0482(16) 0.0380(14) 0.0500(16) -0.0098(12) -0.0201(13) -0.0075(12) C8 0.0553(18) 0.0475(16) 0.0573(18) -0.0116(14) -0.0235(15) -0.0120(13) C9 0.079(2) 0.0536(19) 0.066(2) -0.0210(16) -0.0377(19) -0.0079(16) C10 0.084(2) 0.0560(19) 0.0496(18) -0.0205(15) -0.0182(17) -0.0073(17) C11 0.0586(19) 0.0532(18) 0.0562(19) -0.0158(15) -0.0102(16) -0.0065(15) C12 0.0510(17) 0.0474(16) 0.0531(18) -0.0114(13) -0.0189(14) -0.0091(13) C13 0.0425(15) 0.0432(15) 0.0423(14) -0.0085(12) -0.0180(12) -0.0103(12) C14 0.0356(14) 0.0476(15) 0.0435(15) -0.0131(12) -0.0126(11) -0.0076(11) C15 0.0421(14) 0.0351(14) 0.0464(15) -0.0115(11) -0.0172(12) -0.0032(11) C16 0.0395(14) 0.0388(14) 0.0431(14) -0.0107(11) -0.0141(11) -0.0093(11) C17 0.0361(14) 0.0438(15) 0.0493(15) -0.0136(12) -0.0154(12) -0.0064(11) C18 0.0434(15) 0.0365(14) 0.0527(16) -0.0085(12) -0.0232(13) -0.0042(11) C19 0.0439(15) 0.0397(15) 0.0496(16) -0.0067(12) -0.0132(12) -0.0102(12) C20 0.069(2) 0.0473(18) 0.067(2) -0.0182(15) -0.0208(17) -0.0075(15) C21 0.074(2) 0.0437(18) 0.095(3) -0.0215(19) -0.022(2) -0.0011(16) C22 0.061(2) 0.048(2) 0.097(3) 0.0042(19) -0.034(2) -0.0073(16) C23 0.063(2) 0.066(2) 0.069(2) 0.0035(18) -0.0331(18) -0.0177(17) C24 0.0515(17) 0.0524(17) 0.0564(18) -0.0098(14) -0.0207(14) -0.0121(14) C25 0.0442(15) 0.0484(16) 0.0515(16) -0.0177(13) -0.0140(13) -0.0131(12) C26 0.075(2) 0.067(2) 0.066(2) -0.0088(17) -0.0257(18) -0.0328(18) C27 0.079(3) 0.082(3) 0.088(3) -0.022(2) -0.022(2) -0.045(2) C28 0.060(2) 0.097(3) 0.089(3) -0.045(2) -0.023(2) -0.025(2) C29 0.060(2) 0.087(3) 0.067(2) -0.0349(19) -0.0236(17) -0.0121(18) C30 0.0493(16) 0.0585(18) 0.0531(17) -0.0215(14) -0.0155(14) -0.0113(14) C31 0.0425(15) 0.0447(15) 0.0428(15) -0.0119(12) -0.0146(12) -0.0060(12) C32 0.0516(17) 0.0596(19) 0.068(2) -0.0263(16) -0.0252(15) -0.0027(14) C33 0.087(3) 0.068(2) 0.074(2) -0.0350(19) -0.040(2) 0.0018(19) C34 0.076(3) 0.078(3) 0.062(2) -0.0336(19) -0.0208(19) 0.012(2) C35 0.0498(19) 0.078(2) 0.067(2) -0.0242(19) -0.0086(16) 0.0000(17) C36 0.0468(17) 0.0585(19) 0.0571(18) -0.0142(15) -0.0136(14) -0.0102(14) C100 0.081(3) 0.075(3) 0.091(3) 0.003(2) -0.033(2) -0.030(2) C101 0.074(3) 0.100(3) 0.091(3) -0.019(2) -0.030(2) -0.020(2) C102 0.096(4) 0.136(5) 0.110(4) -0.024(4) -0.044(3) -0.037(3) C103 0.157(6) 0.149(5) 0.102(4) -0.026(4) -0.045(4) -0.073(5) C104 0.160(6) 0.138(5) 0.099(4) -0.036(4) -0.018(4) -0.066(5) C105 0.084(3) 0.105(4) 0.114(4) -0.021(3) -0.007(3) -0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C100 1.891(5) . ? P1 C31 1.793(3) . ? P1 C19 1.795(3) . ? P1 C25 1.795(3) . ? P1 C16 1.798(3) . ? B1 F1 1.424(4) . ? B1 C7 1.639(4) . ? B1 C13 1.652(4) . ? B1 C1 1.654(4) . ? F2 C2 1.351(4) . ? F3 C3 1.345(4) . ? F4 C4 1.345(4) . ? F5 C5 1.351(4) . ? F6 C6 1.344(4) . ? F7 C8 1.351(4) . ? F8 C9 1.348(4) . ? F9 C10 1.344(4) . ? F10 C11 1.348(4) . ? F11 C12 1.345(3) . ? F12 C14 1.343(3) . ? F13 C15 1.342(3) . ? F14 C17 1.348(3) . ? F15 C18 1.350(3) . ? C1 C6 1.382(4) . ? C1 C2 1.382(4) . ? C2 C3 1.381(5) . ? C3 C4 1.365(5) . ? C4 C5 1.361(6) . ? C5 C6 1.374(5) . ? C7 C8 1.384(4) . ? C7 C12 1.386(4) . ? C8 C9 1.372(5) . ? C9 C10 1.366(5) . ? C10 C11 1.360(5) . ? C11 C12 1.374(4) . ? C13 C18 1.384(4) . ? C13 C14 1.388(4) . ? C14 C15 1.383(4) . ? C15 C16 1.385(4) . ? C16 C17 1.393(4) . ? C17 C18 1.370(4) . ? C19 C24 1.388(4) . ? C19 C20 1.392(4) . ? C20 C21 1.378(5) . ? C20 H20A 0.9300 . ? C21 C22 1.370(6) . ? C21 H21A 0.9300 . ? C22 C23 1.355(5) . ? C22 H22A 0.9300 . ? C23 C24 1.379(5) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C30 1.378(4) . ? C25 C26 1.397(4) . ? C26 C27 1.378(5) . ? C26 H26A 0.9300 . ? C27 C28 1.362(6) . ? C27 H27A 0.9300 . ? C28 C29 1.370(5) . ? C28 H28A 0.9300 . ? C29 C30 1.379(4) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C36 1.387(4) . ? C31 C32 1.393(4) . ? C32 C33 1.381(5) . ? C32 H32A 0.9300 . ? C33 C34 1.370(6) . ? C33 H33A 0.9300 . ? C34 C35 1.369(6) . ? C34 H34A 0.9300 . ? C35 C36 1.384(5) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C100 C101 1.365(6) . ? C100 C105 1.398(7) . ? C101 C102 1.367(7) . ? C101 H10A 0.9300 . ? C102 C103 1.343(8) . ? C102 H10B 0.9300 . ? C103 C104 1.365(9) . ? C103 H10C 0.9300 . ? C104 C105 1.374(8) . ? C104 H10D 0.9300 . ? C105 H10E 0.9300 . ? 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 C31 P1 C19 110.42(13) . . ? C31 P1 C25 110.73(13) . . ? C19 P1 C25 107.74(13) . . ? C31 P1 C16 105.26(13) . . ? C19 P1 C16 111.55(13) . . ? C25 P1 C16 111.16(13) . . ? F1 B1 C7 109.7(2) . . ? F1 B1 C13 106.8(2) . . ? C7 B1 C13 111.3(2) . . ? F1 B1 C1 105.1(2) . . ? C7 B1 C1 112.5(2) . . ? C13 B1 C1 111.1(2) . . ? C6 C1 C2 113.6(3) . . ? C6 C1 B1 118.5(3) . . ? C2 C1 B1 127.7(3) . . ? F2 C2 C3 115.1(3) . . ? F2 C2 C1 121.0(3) . . ? C3 C2 C1 123.9(3) . . ? F3 C3 C4 120.3(3) . . ? F3 C3 C2 120.2(3) . . ? C4 C3 C2 119.5(3) . . ? F4 C4 C5 120.3(4) . . ? F4 C4 C3 120.5(4) . . ? C5 C4 C3 119.2(3) . . ? F5 C5 C4 119.6(3) . . ? F5 C5 C6 120.6(4) . . ? C4 C5 C6 119.8(3) . . ? F6 C6 C5 116.7(3) . . ? F6 C6 C1 119.3(3) . . ? C5 C6 C1 124.0(3) . . ? C8 C7 C12 113.3(3) . . ? C8 C7 B1 124.1(3) . . ? C12 C7 B1 122.6(2) . . ? F7 C8 C9 116.0(3) . . ? F7 C8 C7 119.6(3) . . ? C9 C8 C7 124.5(3) . . ? F8 C9 C10 119.8(3) . . ? F8 C9 C8 120.9(3) . . ? C10 C9 C8 119.2(3) . . ? F9 C10 C11 120.5(3) . . ? F9 C10 C9 120.1(3) . . ? C11 C10 C9 119.4(3) . . ? F10 C11 C10 120.0(3) . . ? F10 C11 C12 120.3(3) . . ? C10 C11 C12 119.7(3) . . ? F11 C12 C11 115.5(3) . . ? F11 C12 C7 120.5(3) . . ? C11 C12 C7 123.9(3) . . ? C18 C13 C14 113.7(2) . . ? C18 C13 B1 125.2(2) . . ? C14 C13 B1 121.0(2) . . ? F12 C14 C15 116.3(2) . . ? F12 C14 C13 120.1(2) . . ? C15 C14 C13 123.6(2) . . ? F13 C15 C14 118.2(2) . . ? F13 C15 C16 120.2(2) . . ? C14 C15 C16 121.6(2) . . ? C15 C16 C17 115.1(2) . . ? C15 C16 P1 125.8(2) . . ? C17 C16 P1 118.8(2) . . ? F14 C17 C18 118.9(2) . . ? F14 C17 C16 119.0(2) . . ? C18 C17 C16 122.2(2) . . ? F15 C18 C17 116.1(2) . . ? F15 C18 C13 120.3(2) . . ? C17 C18 C13 123.6(2) . . ? C24 C19 C20 119.9(3) . . ? C24 C19 P1 121.0(2) . . ? C20 C19 P1 119.1(2) . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C23 C22 C21 120.8(3) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 120.5(4) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C23 C24 C19 119.4(3) . . ? C23 C24 H24A 120.3 . . ? C19 C24 H24A 120.3 . . ? C30 C25 C26 119.6(3) . . ? C30 C25 P1 122.0(2) . . ? C26 C25 P1 118.4(2) . . ? C27 C26 C25 119.5(3) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C25 C30 C29 119.8(3) . . ? C25 C30 H30A 120.1 . . ? C29 C30 H30A 120.1 . . ? C36 C31 C32 120.1(3) . . ? C36 C31 P1 121.3(2) . . ? C32 C31 P1 118.7(2) . . ? C33 C32 C31 119.3(3) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? C34 C33 C32 120.3(3) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C35 C34 C33 120.5(3) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 120.5(3) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 C31 119.3(3) . . ? C35 C36 H36A 120.3 . . ? C31 C36 H36A 120.3 . . ? C101 C100 C105 120.7(5) . . ? C101 C100 Br1 119.5(4) . . ? C105 C100 Br1 119.7(4) . . ? C100 C101 C102 118.7(5) . . ? C100 C101 H10A 120.6 . . ? C102 C101 H10A 120.6 . . ? C103 C102 C101 121.1(6) . . ? C103 C102 H10B 119.4 . . ? C101 C102 H10B 119.4 . . ? C102 C103 C104 121.3(6) . . ? C102 C103 H10C 119.4 . . ? C104 C103 H10C 119.4 . . ? C103 C104 C105 119.3(6) . . ? C103 C104 H10D 120.3 . . ? C105 C104 H10D 120.3 . . ? C104 C105 C100 118.8(5) . . ? C104 C105 H10E 120.6 . . ? C100 C105 H10E 120.6 . . ? 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 F1 B1 C1 C6 57.3(3) . . . . ? C7 B1 C1 C6 176.6(2) . . . . ? C13 B1 C1 C6 -57.9(3) . . . . ? F1 B1 C1 C2 -119.2(3) . . . . ? C7 B1 C1 C2 0.1(4) . . . . ? C13 B1 C1 C2 125.7(3) . . . . ? C6 C1 C2 F2 180.0(3) . . . . ? B1 C1 C2 F2 -3.5(4) . . . . ? C6 C1 C2 C3 -1.3(4) . . . . ? B1 C1 C2 C3 175.3(3) . . . . ? F2 C2 C3 F3 0.0(4) . . . . ? C1 C2 C3 F3 -178.8(3) . . . . ? F2 C2 C3 C4 178.9(3) . . . . ? C1 C2 C3 C4 0.1(5) . . . . ? F3 C3 C4 F4 1.2(5) . . . . ? C2 C3 C4 F4 -177.7(3) . . . . ? F3 C3 C4 C5 179.5(3) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? F4 C4 C5 F5 -2.5(5) . . . . ? C3 C4 C5 F5 179.2(3) . . . . ? F4 C4 C5 C6 178.2(3) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? F5 C5 C6 F6 -1.4(5) . . . . ? C4 C5 C6 F6 177.9(3) . . . . ? F5 C5 C6 C1 179.5(3) . . . . ? C4 C5 C6 C1 -1.2(5) . . . . ? C2 C1 C6 F6 -177.3(3) . . . . ? B1 C1 C6 F6 5.8(4) . . . . ? C2 C1 C6 C5 1.8(5) . . . . ? B1 C1 C6 C5 -175.1(3) . . . . ? F1 B1 C7 C8 -155.8(3) . . . . ? C13 B1 C7 C8 -37.8(4) . . . . ? C1 B1 C7 C8 87.6(3) . . . . ? F1 B1 C7 C12 27.4(4) . . . . ? C13 B1 C7 C12 145.5(3) . . . . ? C1 B1 C7 C12 -89.2(3) . . . . ? C12 C7 C8 F7 -179.6(3) . . . . ? B1 C7 C8 F7 3.3(4) . . . . ? C12 C7 C8 C9 1.5(4) . . . . ? B1 C7 C8 C9 -175.5(3) . . . . ? F7 C8 C9 F8 -0.4(5) . . . . ? C7 C8 C9 F8 178.5(3) . . . . ? F7 C8 C9 C10 179.6(3) . . . . ? C7 C8 C9 C10 -1.5(5) . . . . ? F8 C9 C10 F9 0.1(5) . . . . ? C8 C9 C10 F9 -180.0(3) . . . . ? F8 C9 C10 C11 179.9(3) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? F9 C10 C11 F10 -0.3(5) . . . . ? C9 C10 C11 F10 179.9(3) . . . . ? F9 C10 C11 C12 -178.6(3) . . . . ? C9 C10 C11 C12 1.5(5) . . . . ? F10 C11 C12 F11 -2.2(4) . . . . ? C10 C11 C12 F11 176.1(3) . . . . ? F10 C11 C12 C7 -179.9(3) . . . . ? C10 C11 C12 C7 -1.5(5) . . . . ? C8 C7 C12 F11 -177.5(3) . . . . ? B1 C7 C12 F11 -0.4(4) . . . . ? C8 C7 C12 C11 0.0(4) . . . . ? B1 C7 C12 C11 177.1(3) . . . . ? F1 B1 C13 C18 -139.9(3) . . . . ? C7 B1 C13 C18 100.4(3) . . . . ? C1 B1 C13 C18 -25.8(4) . . . . ? F1 B1 C13 C14 36.8(4) . . . . ? C7 B1 C13 C14 -82.9(3) . . . . ? C1 B1 C13 C14 150.9(3) . . . . ? C18 C13 C14 F12 -174.9(2) . . . . ? B1 C13 C14 F12 8.1(4) . . . . ? C18 C13 C14 C15 4.1(4) . . . . ? B1 C13 C14 C15 -173.0(3) . . . . ? F12 C14 C15 F13 -0.2(4) . . . . ? C13 C14 C15 F13 -179.2(2) . . . . ? F12 C14 C15 C16 178.4(2) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? F13 C15 C16 C17 175.7(2) . . . . ? C14 C15 C16 C17 -2.9(4) . . . . ? F13 C15 C16 P1 -10.7(4) . . . . ? C14 C15 C16 P1 170.7(2) . . . . ? C31 P1 C16 C15 -127.9(2) . . . . ? C19 P1 C16 C15 -8.1(3) . . . . ? C25 P1 C16 C15 112.2(3) . . . . ? C31 P1 C16 C17 45.5(2) . . . . ? C19 P1 C16 C17 165.3(2) . . . . ? C25 P1 C16 C17 -74.4(2) . . . . ? C15 C16 C17 F14 -177.2(2) . . . . ? P1 C16 C17 F14 8.7(3) . . . . ? C15 C16 C17 C18 2.7(4) . . . . ? P1 C16 C17 C18 -171.4(2) . . . . ? F14 C17 C18 F15 0.5(4) . . . . ? C16 C17 C18 F15 -179.4(2) . . . . ? F14 C17 C18 C13 -179.0(3) . . . . ? C16 C17 C18 C13 1.0(4) . . . . ? C14 C13 C18 F15 176.1(2) . . . . ? B1 C13 C18 F15 -7.0(4) . . . . ? C14 C13 C18 C17 -4.3(4) . . . . ? B1 C13 C18 C17 172.6(3) . . . . ? C31 P1 C19 C24 20.1(3) . . . . ? C25 P1 C19 C24 141.2(2) . . . . ? C16 P1 C19 C24 -96.5(3) . . . . ? C31 P1 C19 C20 -159.2(2) . . . . ? C25 P1 C19 C20 -38.2(3) . . . . ? C16 P1 C19 C20 84.1(3) . . . . ? C24 C19 C20 C21 0.9(5) . . . . ? P1 C19 C20 C21 -179.8(3) . . . . ? C19 C20 C21 C22 -1.1(6) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C21 C22 C23 C24 0.7(6) . . . . ? C22 C23 C24 C19 -1.0(5) . . . . ? C20 C19 C24 C23 0.2(5) . . . . ? P1 C19 C24 C23 -179.2(2) . . . . ? C31 P1 C25 C30 -101.1(3) . . . . ? C19 P1 C25 C30 138.0(2) . . . . ? C16 P1 C25 C30 15.5(3) . . . . ? C31 P1 C25 C26 77.1(3) . . . . ? C19 P1 C25 C26 -43.8(3) . . . . ? C16 P1 C25 C26 -166.3(2) . . . . ? C30 C25 C26 C27 0.4(5) . . . . ? P1 C25 C26 C27 -177.8(3) . . . . ? C25 C26 C27 C28 -0.2(6) . . . . ? C26 C27 C28 C29 0.3(6) . . . . ? C27 C28 C29 C30 -0.7(6) . . . . ? C26 C25 C30 C29 -0.7(5) . . . . ? P1 C25 C30 C29 177.4(2) . . . . ? C28 C29 C30 C25 0.9(5) . . . . ? C19 P1 C31 C36 109.7(3) . . . . ? C25 P1 C31 C36 -9.5(3) . . . . ? C16 P1 C31 C36 -129.7(2) . . . . ? C19 P1 C31 C32 -71.5(3) . . . . ? C25 P1 C31 C32 169.3(2) . . . . ? C16 P1 C31 C32 49.0(3) . . . . ? C36 C31 C32 C33 -1.7(5) . . . . ? P1 C31 C32 C33 179.6(3) . . . . ? C31 C32 C33 C34 0.7(5) . . . . ? C32 C33 C34 C35 0.9(6) . . . . ? C33 C34 C35 C36 -1.5(6) . . . . ? C34 C35 C36 C31 0.5(5) . . . . ? C32 C31 C36 C35 1.1(5) . . . . ? P1 C31 C36 C35 179.9(3) . . . . ? C105 C100 C101 C102 -0.5(7) . . . . ? Br1 C100 C101 C102 178.4(4) . . . . ? C100 C101 C102 C103 0.4(8) . . . . ? C101 C102 C103 C104 -0.3(10) . . . . ? C102 C103 C104 C105 0.2(10) . . . . ? C103 C104 C105 C100 -0.3(9) . . . . ? C101 C100 C105 C104 0.5(7) . . . . ? Br1 C100 C105 C104 -178.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.417 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.052 #===end data_(F-Ph3)PC6F4B(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 699001' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C36 H12 B F18 P' _chemical_formula_weight 828.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _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 12.9545(15) _cell_length_b 13.2370(16) _cell_length_c 13.5614(16) _cell_angle_alpha 66.727(2) _cell_angle_beta 63.9130(10) _cell_angle_gamma 72.990(2) _cell_volume 1898.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5602 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 25.23 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_T_max 0.946 _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 18290 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6669 _reflns_number_gt 4590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0809P)^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 6669 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 P1 P 0.80383(5) 0.72125(4) 0.39482(5) 0.04945(17) Uani 1 1 d . . . B1 B 0.5109(2) 0.3367(2) 0.7660(2) 0.0550(6) Uani 1 1 d . . . F1 F 0.41302(11) 0.35821(11) 0.73482(11) 0.0683(4) Uani 1 1 d . . . F2 F 0.27602(13) 0.31019(16) 0.95121(13) 0.0964(5) Uani 1 1 d . . . F3 F 0.20978(16) 0.3236(2) 1.16040(15) 0.1323(8) Uani 1 1 d . . . F4 F 0.3602(2) 0.35615(18) 1.22979(15) 0.1290(7) Uani 1 1 d . . . F5 F 0.5825(2) 0.37423(16) 1.08328(16) 0.1171(7) Uani 1 1 d . . . F6 F 0.65243(14) 0.36237(16) 0.87165(14) 0.0992(5) Uani 1 1 d . . . F7 F 0.59446(17) 0.28755(16) 0.55532(14) 0.1028(5) Uani 1 1 d . . . F8 F 0.68697(18) 0.0917(2) 0.5171(2) 0.1362(8) Uani 1 1 d . . . F9 F 0.7351(2) -0.08793(18) 0.6854(3) 0.1577(10) Uani 1 1 d . . . F10 F 0.6808(2) -0.06931(15) 0.8960(2) 0.1398(8) Uani 1 1 d . . . F11 F 0.58189(16) 0.12134(12) 0.93831(14) 0.0968(5) Uani 1 1 d . . . F12 F 0.77421(11) 0.32275(10) 0.64772(13) 0.0745(4) Uani 1 1 d . . . F13 F 0.88913(10) 0.48728(10) 0.49879(13) 0.0723(4) Uani 1 1 d . . . F14 F 0.53944(10) 0.73706(10) 0.54797(11) 0.0673(4) Uani 1 1 d . . . F15 F 0.42320(10) 0.57238(11) 0.69610(12) 0.0712(4) Uani 1 1 d . . . F16 F 1.08518(18) 0.8669(2) 0.53928(19) 0.1335(8) Uani 1 1 d . . . F17 F 0.52149(18) 1.12502(14) 0.2098(2) 0.1295(8) Uani 1 1 d . . . F18 F 1.10656(17) 0.51872(18) 0.02992(17) 0.1213(7) Uani 1 1 d . . . C1 C 0.46780(19) 0.34046(16) 0.89751(19) 0.0538(5) Uani 1 1 d . . . C2 C 0.3561(2) 0.3299(2) 0.9768(2) 0.0652(6) Uani 1 1 d . . . C3 C 0.3190(3) 0.3355(2) 1.0876(2) 0.0830(8) Uani 1 1 d . . . C4 C 0.3947(3) 0.3515(2) 1.1219(2) 0.0836(8) Uani 1 1 d . . . C5 C 0.5066(3) 0.3608(2) 1.0484(2) 0.0771(8) Uani 1 1 d . . . C6 C 0.5392(2) 0.35589(19) 0.9397(2) 0.0644(6) Uani 1 1 d . . . C7 C 0.5803(2) 0.21462(19) 0.7495(2) 0.0600(6) Uani 1 1 d . . . C8 C 0.6116(2) 0.1999(2) 0.6435(3) 0.0763(7) Uani 1 1 d . . . C9 C 0.6614(3) 0.1009(3) 0.6212(3) 0.0942(10) Uani 1 1 d . . . C10 C 0.6857(3) 0.0104(3) 0.7046(4) 0.1037(11) Uani 1 1 d . . . C11 C 0.6592(3) 0.0193(2) 0.8107(4) 0.0968(10) Uani 1 1 d . . . C12 C 0.6065(2) 0.1206(2) 0.8309(2) 0.0719(7) Uani 1 1 d . . . C13 C 0.59056(18) 0.43686(17) 0.67543(18) 0.0513(5) Uani 1 1 d . . . C14 C 0.71081(18) 0.42380(17) 0.62265(19) 0.0539(5) Uani 1 1 d . . . C15 C 0.77219(17) 0.50899(17) 0.54389(19) 0.0535(5) Uani 1 1 d . . . C16 C 0.71843(17) 0.61805(16) 0.51071(17) 0.0486(5) Uani 1 1 d . . . C17 C 0.59834(17) 0.63388(16) 0.56727(18) 0.0499(5) Uani 1 1 d . . . C18 C 0.53881(17) 0.54707(18) 0.64476(17) 0.0514(5) Uani 1 1 d . . . C19 C 0.88715(18) 0.76420(18) 0.44292(19) 0.0553(5) Uani 1 1 d . . . C20 C 0.8998(2) 0.7068(2) 0.5478(2) 0.0641(6) Uani 1 1 d . . . H20A H 0.8631 0.6446 0.5966 0.077 Uiso 1 1 calc R . . C21 C 0.9668(2) 0.7420(3) 0.5797(2) 0.0801(8) Uani 1 1 d . . . H21A H 0.9755 0.7042 0.6504 0.096 Uiso 1 1 calc R . . C22 C 1.0200(2) 0.8319(3) 0.5075(3) 0.0824(8) Uani 1 1 d . . . C23 C 1.0100(3) 0.8909(3) 0.4035(3) 0.0892(9) Uani 1 1 d . . . H23A H 1.0480 0.9525 0.3556 0.107 Uiso 1 1 calc R . . C24 C 0.9424(2) 0.8574(2) 0.3710(2) 0.0751(7) Uani 1 1 d . . . H24A H 0.9335 0.8971 0.3007 0.090 Uiso 1 1 calc R . . C25 C 0.71572(18) 0.84334(17) 0.33799(19) 0.0543(5) Uani 1 1 d . . . C26 C 0.6699(2) 0.92553(19) 0.3916(2) 0.0721(7) Uani 1 1 d . . . H26A H 0.6841 0.9163 0.4564 0.087 Uiso 1 1 calc R . . C27 C 0.6034(3) 1.0205(2) 0.3486(3) 0.0849(8) Uani 1 1 d . . . H27A H 0.5711 1.0758 0.3841 0.102 Uiso 1 1 calc R . . C28 C 0.5861(2) 1.0315(2) 0.2518(3) 0.0868(9) Uani 1 1 d . . . C29 C 0.6290(2) 0.9527(2) 0.1977(3) 0.0808(8) Uani 1 1 d . . . H29A H 0.6144 0.9630 0.1329 0.097 Uiso 1 1 calc R . . C30 C 0.6947(2) 0.8573(2) 0.2412(2) 0.0666(6) Uani 1 1 d . . . H30A H 0.7251 0.8021 0.2057 0.080 Uiso 1 1 calc R . . C31 C 0.89761(18) 0.65801(18) 0.28487(18) 0.0530(5) Uani 1 1 d . . . C32 C 0.8501(2) 0.6046(2) 0.2480(2) 0.0667(6) Uani 1 1 d . . . H32A H 0.7708 0.6008 0.2812 0.080 Uiso 1 1 calc R . . C33 C 0.9213(3) 0.5575(2) 0.1618(3) 0.0822(8) Uani 1 1 d . . . H33A H 0.8908 0.5217 0.1360 0.099 Uiso 1 1 calc R . . C34 C 1.0367(3) 0.5641(2) 0.1152(2) 0.0808(8) Uani 1 1 d . . . C35 C 1.0868(2) 0.6122(3) 0.1514(2) 0.0832(8) Uani 1 1 d . . . H35A H 1.1666 0.6127 0.1192 0.100 Uiso 1 1 calc R . . C36 C 1.0164(2) 0.6605(2) 0.2371(2) 0.0694(6) Uani 1 1 d . . . H36A H 1.0485 0.6948 0.2629 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0484(3) 0.0473(3) 0.0522(3) -0.0182(2) -0.0168(2) -0.0054(2) B1 0.0543(14) 0.0557(14) 0.0601(15) -0.0132(12) -0.0273(12) -0.0116(11) F1 0.0597(8) 0.0833(9) 0.0705(8) -0.0177(7) -0.0321(7) -0.0181(7) F2 0.0633(9) 0.1413(15) 0.0770(10) -0.0205(10) -0.0211(8) -0.0308(9) F3 0.0849(12) 0.186(2) 0.0693(11) -0.0267(12) -0.0041(9) 0.0023(12) F4 0.181(2) 0.1329(16) 0.0729(11) -0.0491(11) -0.0504(12) 0.0071(14) F5 0.1732(19) 0.1183(14) 0.1068(13) -0.0209(11) -0.0892(14) -0.0455(13) F6 0.0850(11) 0.1451(15) 0.0831(10) -0.0155(10) -0.0421(9) -0.0482(10) F7 0.1327(15) 0.1221(14) 0.0760(10) -0.0389(11) -0.0419(10) -0.0322(11) F8 0.1192(15) 0.187(2) 0.1469(17) -0.1241(17) -0.0140(13) -0.0385(14) F9 0.1264(17) 0.1029(15) 0.234(3) -0.1127(18) -0.0164(17) 0.0017(12) F10 0.1433(18) 0.0637(11) 0.178(2) -0.0240(12) -0.0604(16) 0.0147(11) F11 0.1259(14) 0.0648(9) 0.0848(11) -0.0113(8) -0.0483(10) 0.0055(9) F12 0.0575(8) 0.0454(7) 0.1016(10) -0.0091(7) -0.0296(7) -0.0002(6) F13 0.0425(7) 0.0561(7) 0.0958(10) -0.0146(7) -0.0189(7) 0.0005(6) F14 0.0554(7) 0.0480(7) 0.0804(9) -0.0174(6) -0.0199(7) 0.0056(6) F15 0.0444(7) 0.0688(8) 0.0803(9) -0.0202(7) -0.0124(6) -0.0014(6) F16 0.1126(14) 0.201(2) 0.1466(17) -0.0955(17) -0.0401(13) -0.0598(14) F17 0.1298(16) 0.0629(10) 0.180(2) -0.0009(11) -0.0916(15) 0.0118(10) F18 0.1076(13) 0.1669(19) 0.1096(13) -0.1008(14) -0.0417(11) 0.0367(12) C1 0.0608(14) 0.0410(11) 0.0593(13) -0.0125(9) -0.0263(11) -0.0047(9) C2 0.0607(15) 0.0657(15) 0.0628(15) -0.0144(11) -0.0264(12) -0.0023(11) C3 0.0780(19) 0.0874(19) 0.0588(16) -0.0196(14) -0.0192(15) 0.0086(15) C4 0.120(3) 0.0679(17) 0.0594(16) -0.0244(13) -0.0400(18) 0.0092(16) C5 0.122(2) 0.0580(15) 0.0743(18) -0.0153(13) -0.0586(19) -0.0158(15) C6 0.0727(16) 0.0588(14) 0.0675(15) -0.0121(11) -0.0328(13) -0.0166(12) C7 0.0616(14) 0.0567(13) 0.0681(14) -0.0223(11) -0.0228(12) -0.0154(11) C8 0.0742(17) 0.0841(19) 0.0831(19) -0.0383(16) -0.0203(14) -0.0254(14) C9 0.082(2) 0.109(3) 0.110(2) -0.070(2) -0.0098(18) -0.0298(19) C10 0.076(2) 0.090(2) 0.148(3) -0.075(3) -0.008(2) -0.0144(18) C11 0.082(2) 0.0569(17) 0.134(3) -0.0280(19) -0.032(2) -0.0008(14) C12 0.0694(16) 0.0631(16) 0.0819(18) -0.0251(13) -0.0233(14) -0.0116(12) C13 0.0514(12) 0.0531(12) 0.0529(12) -0.0167(10) -0.0234(10) -0.0057(10) C14 0.0509(12) 0.0433(12) 0.0661(13) -0.0136(10) -0.0268(11) -0.0010(10) C15 0.0415(12) 0.0509(12) 0.0657(13) -0.0182(11) -0.0210(10) -0.0010(9) C16 0.0480(12) 0.0471(11) 0.0513(11) -0.0158(9) -0.0202(10) -0.0041(9) C17 0.0483(12) 0.0470(12) 0.0538(12) -0.0188(10) -0.0205(10) 0.0009(9) C18 0.0411(11) 0.0585(13) 0.0511(12) -0.0172(10) -0.0164(10) -0.0031(10) C19 0.0529(12) 0.0590(13) 0.0564(13) -0.0263(11) -0.0140(10) -0.0096(10) C20 0.0602(14) 0.0761(15) 0.0602(14) -0.0305(12) -0.0170(12) -0.0110(12) C21 0.0690(16) 0.118(2) 0.0677(16) -0.0445(17) -0.0242(14) -0.0131(16) C22 0.0659(16) 0.113(2) 0.091(2) -0.0582(19) -0.0169(15) -0.0264(16) C23 0.088(2) 0.089(2) 0.102(2) -0.0414(18) -0.0203(18) -0.0369(16) C24 0.0883(18) 0.0697(16) 0.0745(16) -0.0199(13) -0.0280(14) -0.0281(14) C25 0.0525(12) 0.0474(12) 0.0553(12) -0.0115(10) -0.0159(10) -0.0092(9) C26 0.0832(17) 0.0500(13) 0.0686(15) -0.0179(11) -0.0212(13) -0.0011(12) C27 0.0859(19) 0.0542(15) 0.095(2) -0.0215(14) -0.0264(17) 0.0031(13) C28 0.0753(18) 0.0514(16) 0.112(2) 0.0026(16) -0.0429(17) -0.0061(13) C29 0.0865(19) 0.0655(16) 0.0898(19) -0.0009(14) -0.0514(16) -0.0128(14) C30 0.0696(15) 0.0583(14) 0.0708(15) -0.0116(12) -0.0307(13) -0.0122(12) C31 0.0513(12) 0.0558(12) 0.0546(12) -0.0221(10) -0.0199(10) -0.0038(10) C32 0.0588(14) 0.0760(16) 0.0812(16) -0.0424(14) -0.0314(13) 0.0028(12) C33 0.091(2) 0.0910(19) 0.0950(19) -0.0559(16) -0.0532(17) 0.0132(15) C34 0.0774(19) 0.100(2) 0.0748(17) -0.0551(16) -0.0334(15) 0.0212(15) C35 0.0538(15) 0.121(2) 0.0767(17) -0.0516(17) -0.0147(13) 0.0001(15) C36 0.0567(14) 0.0893(17) 0.0711(15) -0.0382(14) -0.0216(12) -0.0073(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 P1 C19 1.785(2) . ? P1 C31 1.788(2) . ? P1 C16 1.794(2) . ? P1 C25 1.794(2) . ? B1 F1 1.425(3) . ? B1 C1 1.635(3) . ? B1 C7 1.651(3) . ? B1 C13 1.653(3) . ? F2 C2 1.347(3) . ? F3 C3 1.334(3) . ? F4 C4 1.350(3) . ? F5 C5 1.342(3) . ? F6 C6 1.353(3) . ? F7 C8 1.346(3) . ? F8 C9 1.348(4) . ? F9 C10 1.344(3) . ? F10 C11 1.346(4) . ? F11 C12 1.351(3) . ? F12 C14 1.350(2) . ? F13 C15 1.349(2) . ? F14 C17 1.341(2) . ? F15 C18 1.347(2) . ? F16 C22 1.350(3) . ? F17 C28 1.346(3) . ? F18 C34 1.351(3) . ? C1 C6 1.376(3) . ? C1 C2 1.378(3) . ? C2 C3 1.387(4) . ? C3 C4 1.351(4) . ? C4 C5 1.359(4) . ? C5 C6 1.366(4) . ? C7 C12 1.371(3) . ? C7 C8 1.391(4) . ? C8 C9 1.368(4) . ? C9 C10 1.355(5) . ? C10 C11 1.370(5) . ? C11 C12 1.389(4) . ? C13 C14 1.389(3) . ? C13 C18 1.394(3) . ? C14 C15 1.368(3) . ? C15 C16 1.395(3) . ? C16 C17 1.393(3) . ? C17 C18 1.368(3) . ? C19 C20 1.380(3) . ? C19 C24 1.392(3) . ? C20 C21 1.373(3) . ? C20 H20A 0.9300 . ? C21 C22 1.347(4) . ? C21 H21A 0.9300 . ? C22 C23 1.359(4) . ? C23 C24 1.369(4) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C30 1.387(3) . ? C25 C26 1.390(3) . ? C26 C27 1.376(4) . ? C26 H26A 0.9300 . ? C27 C28 1.372(4) . ? C27 H27A 0.9300 . ? C28 C29 1.357(4) . ? C29 C30 1.375(3) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C36 1.387(3) . ? C31 C32 1.391(3) . ? C32 C33 1.377(3) . ? C32 H32A 0.9300 . ? C33 C34 1.358(4) . ? C33 H33A 0.9300 . ? C34 C35 1.356(4) . ? C35 C36 1.381(3) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 P1 C31 110.34(10) . . ? C19 P1 C16 110.69(10) . . ? C31 P1 C16 106.45(10) . . ? C19 P1 C25 107.17(10) . . ? C31 P1 C25 109.99(10) . . ? C16 P1 C25 112.23(10) . . ? F1 B1 C1 109.95(19) . . ? F1 B1 C7 105.52(18) . . ? C1 B1 C7 113.73(18) . . ? F1 B1 C13 106.89(17) . . ? C1 B1 C13 109.01(17) . . ? C7 B1 C13 111.48(19) . . ? C6 C1 C2 113.2(2) . . ? C6 C1 B1 123.3(2) . . ? C2 C1 B1 123.5(2) . . ? F2 C2 C1 121.0(2) . . ? F2 C2 C3 115.5(2) . . ? C1 C2 C3 123.5(2) . . ? F3 C3 C4 120.1(3) . . ? F3 C3 C2 120.4(3) . . ? C4 C3 C2 119.5(3) . . ? F4 C4 C3 120.2(3) . . ? F4 C4 C5 119.9(3) . . ? C3 C4 C5 119.9(2) . . ? F5 C5 C4 119.9(3) . . ? F5 C5 C6 121.4(3) . . ? C4 C5 C6 118.7(3) . . ? F6 C6 C5 115.9(2) . . ? F6 C6 C1 118.8(2) . . ? C5 C6 C1 125.2(3) . . ? C12 C7 C8 113.8(2) . . ? C12 C7 B1 127.9(2) . . ? C8 C7 B1 118.2(2) . . ? F7 C8 C9 116.7(3) . . ? F7 C8 C7 119.2(2) . . ? C9 C8 C7 124.1(3) . . ? F8 C9 C10 119.2(3) . . ? F8 C9 C8 121.1(4) . . ? C10 C9 C8 119.8(3) . . ? F9 C10 C9 121.3(4) . . ? F9 C10 C11 119.4(4) . . ? C9 C10 C11 119.4(3) . . ? F10 C11 C10 120.9(3) . . ? F10 C11 C12 119.8(3) . . ? C10 C11 C12 119.2(3) . . ? F11 C12 C7 121.0(2) . . ? F11 C12 C11 115.3(3) . . ? C7 C12 C11 123.7(3) . . ? C14 C13 C18 113.05(19) . . ? C14 C13 B1 126.11(19) . . ? C18 C13 B1 120.84(18) . . ? F12 C14 C15 116.00(18) . . ? F12 C14 C13 120.29(18) . . ? C15 C14 C13 123.71(19) . . ? F13 C15 C14 118.84(18) . . ? F13 C15 C16 118.79(18) . . ? C14 C15 C16 122.35(19) . . ? C17 C16 C15 114.78(18) . . ? C17 C16 P1 125.81(15) . . ? C15 C16 P1 119.20(15) . . ? F14 C17 C18 118.86(17) . . ? F14 C17 C16 119.44(18) . . ? C18 C17 C16 121.68(18) . . ? F15 C18 C17 116.58(18) . . ? F15 C18 C13 119.10(18) . . ? C17 C18 C13 124.29(18) . . ? C20 C19 C24 119.4(2) . . ? C20 C19 P1 122.01(17) . . ? C24 C19 P1 118.60(18) . . ? C21 C20 C19 119.7(2) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C22 C21 C20 119.3(3) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 F16 119.2(3) . . ? C21 C22 C23 123.0(2) . . ? F16 C22 C23 117.8(3) . . ? C22 C23 C24 118.4(3) . . ? C22 C23 H23A 120.8 . . ? C24 C23 H23A 120.8 . . ? C23 C24 C19 120.3(3) . . ? C23 C24 H24A 119.9 . . ? C19 C24 H24A 119.9 . . ? C30 C25 C26 120.1(2) . . ? C30 C25 P1 121.15(17) . . ? C26 C25 P1 118.78(18) . . ? C27 C26 C25 119.8(3) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C28 C27 C26 118.2(3) . . ? C28 C27 H27A 120.9 . . ? C26 C27 H27A 120.9 . . ? F17 C28 C29 118.6(3) . . ? F17 C28 C27 117.9(3) . . ? C29 C28 C27 123.5(2) . . ? C28 C29 C30 118.4(3) . . ? C28 C29 H29A 120.8 . . ? C30 C29 H29A 120.8 . . ? C29 C30 C25 120.1(2) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? C36 C31 C32 119.9(2) . . ? C36 C31 P1 121.11(17) . . ? C32 C31 P1 119.04(17) . . ? C33 C32 C31 119.5(2) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? C34 C33 C32 119.0(2) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? F18 C34 C35 117.6(3) . . ? F18 C34 C33 119.1(3) . . ? C35 C34 C33 123.3(2) . . ? C34 C35 C36 118.4(2) . . ? C34 C35 H35A 120.8 . . ? C36 C35 H35A 120.8 . . ? C35 C36 C31 120.0(2) . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? 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 F1 B1 C1 C6 -160.02(19) . . . . ? C7 B1 C1 C6 81.9(3) . . . . ? C13 B1 C1 C6 -43.2(3) . . . . ? F1 B1 C1 C2 19.1(3) . . . . ? C7 B1 C1 C2 -98.9(2) . . . . ? C13 B1 C1 C2 136.0(2) . . . . ? C6 C1 C2 F2 -177.5(2) . . . . ? B1 C1 C2 F2 3.3(3) . . . . ? C6 C1 C2 C3 0.6(3) . . . . ? B1 C1 C2 C3 -178.6(2) . . . . ? F2 C2 C3 F3 -1.2(4) . . . . ? C1 C2 C3 F3 -179.4(2) . . . . ? F2 C2 C3 C4 177.9(2) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? F3 C3 C4 F4 -0.4(4) . . . . ? C2 C3 C4 F4 -179.5(2) . . . . ? F3 C3 C4 C5 178.3(3) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? F4 C4 C5 F5 0.2(4) . . . . ? C3 C4 C5 F5 -178.5(2) . . . . ? F4 C4 C5 C6 -179.9(2) . . . . ? C3 C4 C5 C6 1.3(4) . . . . ? F5 C5 C6 F6 1.7(4) . . . . ? C4 C5 C6 F6 -178.1(2) . . . . ? F5 C5 C6 C1 178.9(2) . . . . ? C4 C5 C6 C1 -1.0(4) . . . . ? C2 C1 C6 F6 177.1(2) . . . . ? B1 C1 C6 F6 -3.7(3) . . . . ? C2 C1 C6 C5 0.0(3) . . . . ? B1 C1 C6 C5 179.3(2) . . . . ? F1 B1 C7 C12 -122.0(2) . . . . ? C1 B1 C7 C12 -1.4(3) . . . . ? C13 B1 C7 C12 122.4(2) . . . . ? F1 B1 C7 C8 53.9(3) . . . . ? C1 B1 C7 C8 174.5(2) . . . . ? C13 B1 C7 C8 -61.7(3) . . . . ? C12 C7 C8 F7 -177.4(2) . . . . ? B1 C7 C8 F7 6.2(3) . . . . ? C12 C7 C8 C9 1.6(4) . . . . ? B1 C7 C8 C9 -174.9(2) . . . . ? F7 C8 C9 F8 -2.8(4) . . . . ? C7 C8 C9 F8 178.3(2) . . . . ? F7 C8 C9 C10 177.2(3) . . . . ? C7 C8 C9 C10 -1.8(4) . . . . ? F8 C9 C10 F9 0.3(5) . . . . ? C8 C9 C10 F9 -179.7(3) . . . . ? F8 C9 C10 C11 -179.6(3) . . . . ? C8 C9 C10 C11 0.5(5) . . . . ? F9 C10 C11 F10 -0.7(5) . . . . ? C9 C10 C11 F10 179.1(3) . . . . ? F9 C10 C11 C12 -179.0(3) . . . . ? C9 C10 C11 C12 0.9(5) . . . . ? C8 C7 C12 F11 179.8(2) . . . . ? B1 C7 C12 F11 -4.2(4) . . . . ? C8 C7 C12 C11 -0.2(4) . . . . ? B1 C7 C12 C11 175.9(2) . . . . ? F10 C11 C12 F11 0.8(4) . . . . ? C10 C11 C12 F11 179.1(3) . . . . ? F10 C11 C12 C7 -179.3(3) . . . . ? C10 C11 C12 C7 -1.0(4) . . . . ? F1 B1 C13 C14 -137.7(2) . . . . ? C1 B1 C13 C14 103.5(2) . . . . ? C7 B1 C13 C14 -22.8(3) . . . . ? F1 B1 C13 C18 42.4(3) . . . . ? C1 B1 C13 C18 -76.4(2) . . . . ? C7 B1 C13 C18 157.19(19) . . . . ? C18 C13 C14 F12 176.82(19) . . . . ? B1 C13 C14 F12 -3.2(3) . . . . ? C18 C13 C14 C15 -3.3(3) . . . . ? B1 C13 C14 C15 176.7(2) . . . . ? F12 C14 C15 F13 -0.9(3) . . . . ? C13 C14 C15 F13 179.3(2) . . . . ? F12 C14 C15 C16 -179.20(19) . . . . ? C13 C14 C15 C16 0.9(3) . . . . ? F13 C15 C16 C17 -175.93(19) . . . . ? C14 C15 C16 C17 2.4(3) . . . . ? F13 C15 C16 P1 8.9(3) . . . . ? C14 C15 C16 P1 -172.78(17) . . . . ? C19 P1 C16 C17 108.37(19) . . . . ? C31 P1 C16 C17 -131.69(18) . . . . ? C25 P1 C16 C17 -11.3(2) . . . . ? C19 P1 C16 C15 -77.04(19) . . . . ? C31 P1 C16 C15 42.89(19) . . . . ? C25 P1 C16 C15 163.27(16) . . . . ? C15 C16 C17 F14 175.02(18) . . . . ? P1 C16 C17 F14 -10.2(3) . . . . ? C15 C16 C17 C18 -3.1(3) . . . . ? P1 C16 C17 C18 171.65(16) . . . . ? F14 C17 C18 F15 0.5(3) . . . . ? C16 C17 C18 F15 178.63(19) . . . . ? F14 C17 C18 C13 -177.49(19) . . . . ? C16 C17 C18 C13 0.7(3) . . . . ? C14 C13 C18 F15 -175.36(18) . . . . ? B1 C13 C18 F15 4.6(3) . . . . ? C14 C13 C18 C17 2.5(3) . . . . ? B1 C13 C18 C17 -177.47(19) . . . . ? C31 P1 C19 C20 -105.1(2) . . . . ? C16 P1 C19 C20 12.5(2) . . . . ? C25 P1 C19 C20 135.15(19) . . . . ? C31 P1 C19 C24 73.8(2) . . . . ? C16 P1 C19 C24 -168.67(18) . . . . ? C25 P1 C19 C24 -46.0(2) . . . . ? C24 C19 C20 C21 -0.2(3) . . . . ? P1 C19 C20 C21 178.64(19) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C20 C21 C22 F16 179.5(2) . . . . ? C20 C21 C22 C23 0.5(4) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? F16 C22 C23 C24 -178.9(3) . . . . ? C22 C23 C24 C19 -0.9(4) . . . . ? C20 C19 C24 C23 0.9(4) . . . . ? P1 C19 C24 C23 -178.0(2) . . . . ? C19 P1 C25 C30 142.32(19) . . . . ? C31 P1 C25 C30 22.3(2) . . . . ? C16 P1 C25 C30 -96.0(2) . . . . ? C19 P1 C25 C26 -36.6(2) . . . . ? C31 P1 C25 C26 -156.57(18) . . . . ? C16 P1 C25 C26 85.1(2) . . . . ? C30 C25 C26 C27 0.2(4) . . . . ? P1 C25 C26 C27 179.1(2) . . . . ? C25 C26 C27 C28 -1.0(4) . . . . ? C26 C27 C28 F17 -179.6(2) . . . . ? C26 C27 C28 C29 1.4(5) . . . . ? F17 C28 C29 C30 -179.9(2) . . . . ? C27 C28 C29 C30 -0.9(4) . . . . ? C28 C29 C30 C25 0.0(4) . . . . ? C26 C25 C30 C29 0.3(3) . . . . ? P1 C25 C30 C29 -178.56(18) . . . . ? C19 P1 C31 C36 -8.6(2) . . . . ? C16 P1 C31 C36 -128.7(2) . . . . ? C25 P1 C31 C36 109.5(2) . . . . ? C19 P1 C31 C32 170.78(18) . . . . ? C16 P1 C31 C32 50.6(2) . . . . ? C25 P1 C31 C32 -71.2(2) . . . . ? C36 C31 C32 C33 -1.9(4) . . . . ? P1 C31 C32 C33 178.8(2) . . . . ? C31 C32 C33 C34 0.2(4) . . . . ? C32 C33 C34 F18 -179.4(3) . . . . ? C32 C33 C34 C35 2.0(5) . . . . ? F18 C34 C35 C36 179.0(3) . . . . ? C33 C34 C35 C36 -2.4(5) . . . . ? C34 C35 C36 C31 0.7(4) . . . . ? C32 C31 C36 C35 1.4(4) . . . . ? P1 C31 C36 C35 -179.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.247 _refine_diff_density_min -0.158 _refine_diff_density_rms 0.042 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 1 -0.071 0.000 0.500 365.0 76.5 _platon_squeeze_details ; ; #===end data_PhB(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 699002' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C18 H5 B F10' _chemical_formula_weight 422.03 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.6539(13) _cell_length_b 16.736(2) _cell_length_c 19.095(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3404.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5303 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 20.39 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 36577 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4098 _reflns_number_gt 2142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.0690P)^2^+0.5934P] 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 4098 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 B1 B 0.3753(2) 0.20002(16) 0.62948(13) 0.0583(6) Uani 1 1 d . . . F1 F 0.14599(12) 0.12244(9) 0.67752(8) 0.0850(4) Uani 1 1 d . . . F2 F 0.03539(15) -0.00153(10) 0.61570(11) 0.1226(7) Uani 1 1 d . . . F3 F 0.1372(2) -0.06607(11) 0.49813(12) 0.1465(9) Uani 1 1 d . . . F4 F 0.3504(2) -0.00251(12) 0.44338(10) 0.1363(8) Uani 1 1 d . . . F5 F 0.46250(13) 0.11934(11) 0.50564(7) 0.0974(5) Uani 1 1 d . . . F6 F 0.54729(15) 0.32442(10) 0.58470(11) 0.1238(7) Uani 1 1 d . . . F7 F 0.79667(16) 0.31867(12) 0.59620(13) 0.1390(8) Uani 1 1 d . . . F8 F 0.90933(13) 0.18844(11) 0.64985(11) 0.1163(6) Uani 1 1 d . . . F9 F 0.77091(13) 0.06478(9) 0.69564(9) 0.0953(5) Uani 1 1 d . . . F10 F 0.52045(12) 0.06985(7) 0.68691(8) 0.0796(4) Uani 1 1 d . . . C1 C 0.30171(19) 0.27325(14) 0.65627(12) 0.0628(6) Uani 1 1 d . . . C2 C 0.1839(2) 0.29406(15) 0.62961(13) 0.0723(6) Uani 1 1 d . . . H2A H 0.1476 0.2626 0.5949 0.087 Uiso 1 1 calc R . . C3 C 0.1204(2) 0.36047(16) 0.65393(16) 0.0809(7) Uani 1 1 d . . . H3A H 0.0431 0.3742 0.6348 0.097 Uiso 1 1 calc R . . C4 C 0.1710(2) 0.40605(16) 0.70608(17) 0.0855(8) Uani 1 1 d . . . H4A H 0.1272 0.4501 0.7229 0.103 Uiso 1 1 calc R . . C5 C 0.2865(3) 0.38713(16) 0.73386(15) 0.0869(8) Uani 1 1 d . . . H5A H 0.3206 0.4180 0.7697 0.104 Uiso 1 1 calc R . . C6 C 0.3512(2) 0.32223(14) 0.70823(14) 0.0743(7) Uani 1 1 d . . . H6A H 0.4303 0.3108 0.7262 0.089 Uiso 1 1 calc R . . C7 C 0.30828(19) 0.12722(13) 0.59390(11) 0.0609(6) Uani 1 1 d . . . C8 C 0.1981(2) 0.09355(14) 0.61901(13) 0.0669(6) Uani 1 1 d . . . C9 C 0.1405(3) 0.02951(17) 0.58887(16) 0.0841(8) Uani 1 1 d . . . C10 C 0.1915(3) -0.00334(16) 0.5298(2) 0.0984(10) Uani 1 1 d . . . C11 C 0.2999(3) 0.02752(18) 0.50217(15) 0.0923(9) Uani 1 1 d . . . C12 C 0.3567(2) 0.09057(16) 0.53492(13) 0.0730(6) Uani 1 1 d . . . C13 C 0.52233(18) 0.19768(12) 0.63651(11) 0.0569(5) Uani 1 1 d . . . C14 C 0.5988(2) 0.25960(15) 0.61429(14) 0.0764(7) Uani 1 1 d . . . C15 C 0.7268(2) 0.25678(16) 0.61808(16) 0.0854(8) Uani 1 1 d . . . C16 C 0.7843(2) 0.19120(16) 0.64538(14) 0.0755(7) Uani 1 1 d . . . C17 C 0.7139(2) 0.12904(13) 0.66897(12) 0.0631(6) Uani 1 1 d . . . C18 C 0.58567(19) 0.13271(12) 0.66353(11) 0.0562(5) 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 B1 0.0516(13) 0.0687(16) 0.0547(13) 0.0062(12) -0.0018(11) 0.0014(11) F1 0.0659(8) 0.1044(11) 0.0849(10) 0.0010(8) 0.0103(7) -0.0063(7) F2 0.0972(13) 0.1056(12) 0.1650(18) 0.0260(12) -0.0276(12) -0.0400(11) F3 0.1792(18) 0.0870(12) 0.173(2) -0.0352(12) -0.0776(16) -0.0098(12) F4 0.1590(18) 0.1470(17) 0.1029(13) -0.0619(13) -0.0266(12) 0.0485(14) F5 0.0738(9) 0.1446(14) 0.0739(9) -0.0137(9) 0.0080(7) 0.0172(9) F6 0.0881(11) 0.0923(11) 0.1909(19) 0.0714(12) 0.0056(11) 0.0088(9) F7 0.0824(11) 0.1196(15) 0.215(2) 0.0688(14) 0.0170(12) -0.0279(10) F8 0.0462(8) 0.1285(14) 0.1742(18) 0.0156(12) -0.0023(9) -0.0026(8) F9 0.0733(9) 0.0847(10) 0.1278(13) 0.0212(9) -0.0144(8) 0.0204(8) F10 0.0698(8) 0.0646(8) 0.1042(10) 0.0201(7) -0.0065(7) -0.0121(7) C1 0.0493(11) 0.0645(13) 0.0746(14) 0.0008(11) -0.0025(10) 0.0022(10) C2 0.0560(13) 0.0766(16) 0.0844(17) -0.0046(13) -0.0075(11) 0.0041(11) C3 0.0569(13) 0.0785(17) 0.107(2) 0.0069(15) -0.0053(13) 0.0140(12) C4 0.0736(16) 0.0642(15) 0.119(2) -0.0062(15) 0.0048(15) 0.0113(13) C5 0.0847(18) 0.0692(16) 0.107(2) -0.0216(15) -0.0101(15) 0.0036(14) C6 0.0592(13) 0.0697(15) 0.0940(18) -0.0099(13) -0.0118(12) 0.0026(12) C7 0.0513(11) 0.0692(14) 0.0622(13) -0.0020(11) -0.0071(10) 0.0070(10) C8 0.0616(13) 0.0697(14) 0.0693(14) 0.0021(12) -0.0109(11) 0.0040(12) C9 0.0766(17) 0.0755(17) 0.100(2) 0.0077(16) -0.0263(16) -0.0085(14) C10 0.110(2) 0.0696(17) 0.116(3) -0.0125(18) -0.052(2) 0.0010(17) C11 0.105(2) 0.093(2) 0.0785(18) -0.0301(16) -0.0298(17) 0.0303(18) C12 0.0639(13) 0.0907(17) 0.0644(14) -0.0064(13) -0.0073(12) 0.0155(13) C13 0.0483(11) 0.0598(12) 0.0626(13) 0.0039(10) -0.0005(9) 0.0004(9) C14 0.0642(13) 0.0659(15) 0.0990(18) 0.0237(14) 0.0009(13) 0.0064(12) C15 0.0583(13) 0.0790(17) 0.119(2) 0.0258(16) 0.0107(14) -0.0140(13) C16 0.0452(12) 0.0831(17) 0.0982(19) 0.0040(14) -0.0001(12) 0.0005(12) C17 0.0556(12) 0.0608(13) 0.0730(14) 0.0034(11) -0.0087(10) 0.0100(11) C18 0.0531(12) 0.0550(12) 0.0606(12) -0.0004(10) -0.0018(10) -0.0034(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 B1 C1 1.542(3) . ? B1 C7 1.567(3) . ? B1 C13 1.573(3) . ? F1 C8 1.338(3) . ? F2 C9 1.337(3) . ? F3 C10 1.343(3) . ? F4 C11 1.342(3) . ? F5 C12 1.347(3) . ? F6 C14 1.340(3) . ? F7 C15 1.342(3) . ? F8 C16 1.336(3) . ? F9 C17 1.336(2) . ? F10 C18 1.337(2) . ? C1 C6 1.391(3) . ? C1 C2 1.399(3) . ? C2 C3 1.381(3) . ? C2 H2A 0.9300 . ? C3 C4 1.365(4) . ? C3 H3A 0.9300 . ? C4 C5 1.377(4) . ? C4 H4A 0.9300 . ? C5 C6 1.376(3) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.382(3) . ? C7 C8 1.387(3) . ? C8 C9 1.363(4) . ? C9 C10 1.367(4) . ? C10 C11 1.371(4) . ? C11 C12 1.368(4) . ? C13 C18 1.380(3) . ? C13 C14 1.385(3) . ? C14 C15 1.366(3) . ? C15 C16 1.361(3) . ? C16 C17 1.359(3) . ? C17 C18 1.372(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 B1 C7 122.03(19) . . ? C1 B1 C13 119.8(2) . . ? C7 B1 C13 118.1(2) . . ? C6 C1 C2 116.9(2) . . ? C6 C1 B1 120.8(2) . . ? C2 C1 B1 122.2(2) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C4 C3 C2 120.1(2) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 120.4(2) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C1 121.9(2) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? C12 C7 C8 114.7(2) . . ? C12 C7 B1 121.9(2) . . ? C8 C7 B1 123.4(2) . . ? F1 C8 C9 116.7(2) . . ? F1 C8 C7 119.5(2) . . ? C9 C8 C7 123.7(2) . . ? F2 C9 C8 121.4(3) . . ? F2 C9 C10 119.5(3) . . ? C8 C9 C10 119.1(3) . . ? F3 C10 C9 121.0(3) . . ? F3 C10 C11 118.9(3) . . ? C9 C10 C11 120.1(3) . . ? F4 C11 C12 119.6(3) . . ? F4 C11 C10 121.2(3) . . ? C12 C11 C10 119.2(3) . . ? F5 C12 C11 117.2(2) . . ? F5 C12 C7 119.5(2) . . ? C11 C12 C7 123.3(3) . . ? C18 C13 C14 114.63(19) . . ? C18 C13 B1 122.58(19) . . ? C14 C13 B1 122.8(2) . . ? F6 C14 C15 117.3(2) . . ? F6 C14 C13 119.6(2) . . ? C15 C14 C13 123.0(2) . . ? F7 C15 C16 119.4(2) . . ? F7 C15 C14 120.7(2) . . ? C16 C15 C14 119.8(2) . . ? F8 C16 C17 120.2(2) . . ? F8 C16 C15 120.1(2) . . ? C17 C16 C15 119.7(2) . . ? F9 C17 C16 119.5(2) . . ? F9 C17 C18 121.2(2) . . ? C16 C17 C18 119.4(2) . . ? F10 C18 C17 117.20(19) . . ? F10 C18 C13 119.38(18) . . ? C17 C18 C13 123.4(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 C7 B1 C1 C6 156.7(2) . . . . ? C13 B1 C1 C6 -24.3(3) . . . . ? C7 B1 C1 C2 -23.9(3) . . . . ? C13 B1 C1 C2 155.2(2) . . . . ? C6 C1 C2 C3 0.2(4) . . . . ? B1 C1 C2 C3 -179.3(2) . . . . ? C1 C2 C3 C4 -1.6(4) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? C4 C5 C6 C1 -2.0(4) . . . . ? C2 C1 C6 C5 1.6(4) . . . . ? B1 C1 C6 C5 -178.9(2) . . . . ? C1 B1 C7 C12 137.7(2) . . . . ? C13 B1 C7 C12 -41.3(3) . . . . ? C1 B1 C7 C8 -43.4(3) . . . . ? C13 B1 C7 C8 137.6(2) . . . . ? C12 C7 C8 F1 177.34(19) . . . . ? B1 C7 C8 F1 -1.6(3) . . . . ? C12 C7 C8 C9 0.0(3) . . . . ? B1 C7 C8 C9 -179.0(2) . . . . ? F1 C8 C9 F2 1.6(4) . . . . ? C7 C8 C9 F2 179.0(2) . . . . ? F1 C8 C9 C10 -178.6(2) . . . . ? C7 C8 C9 C10 -1.2(4) . . . . ? F2 C9 C10 F3 0.3(4) . . . . ? C8 C9 C10 F3 -179.5(2) . . . . ? F2 C9 C10 C11 -179.4(2) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? F3 C10 C11 F4 1.7(4) . . . . ? C9 C10 C11 F4 -178.5(2) . . . . ? F3 C10 C11 C12 -178.9(2) . . . . ? C9 C10 C11 C12 0.9(4) . . . . ? F4 C11 C12 F5 -0.1(4) . . . . ? C10 C11 C12 F5 -179.5(2) . . . . ? F4 C11 C12 C7 177.2(2) . . . . ? C10 C11 C12 C7 -2.2(4) . . . . ? C8 C7 C12 F5 179.00(19) . . . . ? B1 C7 C12 F5 -2.0(3) . . . . ? C8 C7 C12 C11 1.8(3) . . . . ? B1 C7 C12 C11 -179.3(2) . . . . ? C1 B1 C13 C18 131.3(2) . . . . ? C7 B1 C13 C18 -49.6(3) . . . . ? C1 B1 C13 C14 -50.5(3) . . . . ? C7 B1 C13 C14 128.5(2) . . . . ? C18 C13 C14 F6 177.5(2) . . . . ? B1 C13 C14 F6 -0.8(4) . . . . ? C18 C13 C14 C15 0.5(4) . . . . ? B1 C13 C14 C15 -177.7(3) . . . . ? F6 C14 C15 F7 3.4(4) . . . . ? C13 C14 C15 F7 -179.6(3) . . . . ? F6 C14 C15 C16 -177.7(3) . . . . ? C13 C14 C15 C16 -0.7(5) . . . . ? F7 C15 C16 F8 -0.5(4) . . . . ? C14 C15 C16 F8 -179.3(3) . . . . ? F7 C15 C16 C17 178.6(3) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? F8 C16 C17 F9 -1.0(4) . . . . ? C15 C16 C17 F9 179.9(2) . . . . ? F8 C16 C17 C18 -179.6(2) . . . . ? C15 C16 C17 C18 1.3(4) . . . . ? F9 C17 C18 F10 0.9(3) . . . . ? C16 C17 C18 F10 179.5(2) . . . . ? F9 C17 C18 C13 179.9(2) . . . . ? C16 C17 C18 C13 -1.5(4) . . . . ? C14 C13 C18 F10 179.6(2) . . . . ? B1 C13 C18 F10 -2.2(3) . . . . ? C14 C13 C18 C17 0.6(3) . . . . ? B1 C13 C18 C17 178.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.250 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.033 #===end data_Cy3P-C6F4-BF(C6F5)Ph-CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 699003' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C37 H40 B Cl2 F10 P' _chemical_formula_weight 787.37 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' 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' Cl Cl 0.1484 0.1585 '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 11.635(3) _cell_length_b 12.659(3) _cell_length_c 13.371(3) _cell_angle_alpha 73.387(3) _cell_angle_beta 77.620(3) _cell_angle_gamma 82.653(3) _cell_volume 1838.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4767 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.00 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.942 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 17839 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6441 _reflns_number_gt 4731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics '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^)+(0.1244P)^2^+1.2066P] 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 6441 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.2180 _refine_ls_wR_factor_gt 0.1954 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 P1 P 0.71478(7) 0.79286(7) 0.27088(6) 0.0392(2) Uani 1 1 d . . . B1 B 0.6131(4) 0.8389(3) 0.7429(3) 0.0492(10) Uani 1 1 d . . . F1 F 0.5564(2) 0.94395(16) 0.75217(16) 0.0594(6) Uani 1 1 d . . . F2 F 0.4371(2) 0.7505(2) 0.65620(18) 0.0738(7) Uani 1 1 d . . . F3 F 0.2766(3) 0.6104(3) 0.7647(3) 0.0983(10) Uani 1 1 d . . . F4 F 0.2564(3) 0.5259(3) 0.9767(3) 0.1114(11) Uani 1 1 d . . . F5 F 0.3993(3) 0.5916(3) 1.0815(2) 0.1042(10) Uani 1 1 d . . . F6 F 0.5589(3) 0.7356(3) 0.97575(19) 0.0853(8) Uani 1 1 d . . . F7 F 0.6083(2) 1.02789(16) 0.54084(16) 0.0659(6) Uani 1 1 d . . . F8 F 0.6569(2) 1.01088(16) 0.34866(16) 0.0633(6) Uani 1 1 d . . . F9 F 0.75850(19) 0.62736(15) 0.47466(15) 0.0536(5) Uani 1 1 d . . . F10 F 0.7038(2) 0.64471(16) 0.66783(15) 0.0580(6) Uani 1 1 d . . . C1 C 0.7376(4) 0.8206(3) 0.7835(3) 0.0536(9) Uani 1 1 d . . . C2 C 0.7900(4) 0.7184(4) 0.8320(3) 0.0709(12) Uani 1 1 d . . . H2A H 0.7489 0.6553 0.8491 0.085 Uiso 1 1 calc R . . C3 C 0.9019(5) 0.7093(6) 0.8551(4) 0.0936(17) Uani 1 1 d . . . H3A H 0.9346 0.6401 0.8871 0.112 Uiso 1 1 calc R . . C4 C 0.9643(6) 0.7987(7) 0.8320(6) 0.111(2) Uani 1 1 d . . . H4A H 1.0399 0.7915 0.8468 0.134 Uiso 1 1 calc R . . C5 C 0.9145(5) 0.9003(7) 0.7864(6) 0.110(2) Uani 1 1 d . . . H5A H 0.9563 0.9625 0.7722 0.132 Uiso 1 1 calc R . . C6 C 0.8028(4) 0.9128(4) 0.7608(4) 0.0742(12) Uani 1 1 d . . . H6A H 0.7715 0.9825 0.7286 0.089 Uiso 1 1 calc R . . C7 C 0.5135(3) 0.7472(3) 0.8087(3) 0.0533(9) Uani 1 1 d . . . C8 C 0.4348(4) 0.7133(3) 0.7617(3) 0.0571(9) Uani 1 1 d . . . C9 C 0.3491(4) 0.6405(4) 0.8167(4) 0.0670(11) Uani 1 1 d . . . C10 C 0.3391(4) 0.5984(4) 0.9237(4) 0.0751(13) Uani 1 1 d . . . C11 C 0.4106(4) 0.6308(4) 0.9751(3) 0.0690(12) Uani 1 1 d . . . C12 C 0.4953(4) 0.7040(3) 0.9185(3) 0.0602(10) Uani 1 1 d . . . C13 C 0.6496(3) 0.8361(3) 0.6168(3) 0.0448(8) Uani 1 1 d . . . C14 C 0.6433(3) 0.9252(3) 0.5291(3) 0.0459(8) Uani 1 1 d . . . C15 C 0.6690(3) 0.9174(3) 0.4253(3) 0.0442(8) Uani 1 1 d . . . C16 C 0.7053(3) 0.8171(3) 0.4000(2) 0.0414(7) Uani 1 1 d . . . C17 C 0.7189(3) 0.7278(3) 0.4881(3) 0.0423(7) Uani 1 1 d . . . C18 C 0.6917(3) 0.7386(3) 0.5900(3) 0.0436(8) Uani 1 1 d . . . C19 C 0.8481(3) 0.7037(3) 0.2470(3) 0.0460(8) Uani 1 1 d . . . H19A H 0.8335 0.6326 0.2997 0.055 Uiso 1 1 calc R . . C20 C 0.9598(3) 0.7412(4) 0.2679(4) 0.0606(10) Uani 1 1 d . . . H20A H 0.9841 0.8080 0.2138 0.073 Uiso 1 1 calc R . . H20B H 0.9434 0.7570 0.3366 0.073 Uiso 1 1 calc R . . C21 C 1.0575(4) 0.6496(4) 0.2656(4) 0.0754(12) Uani 1 1 d . . . H21A H 1.1292 0.6746 0.2744 0.090 Uiso 1 1 calc R . . H21B H 1.0357 0.5861 0.3248 0.090 Uiso 1 1 calc R . . C22 C 1.0814(4) 0.6150(4) 0.1635(4) 0.0823(14) Uani 1 1 d . . . H22A H 1.1383 0.5516 0.1691 0.099 Uiso 1 1 calc R . . H22B H 1.1153 0.6748 0.1054 0.099 Uiso 1 1 calc R . . C23 C 0.9696(4) 0.5856(4) 0.1390(3) 0.0708(12) Uani 1 1 d . . . H23A H 0.9422 0.5190 0.1916 0.085 Uiso 1 1 calc R . . H23B H 0.9874 0.5705 0.0700 0.085 Uiso 1 1 calc R . . C24 C 0.8717(4) 0.6784(3) 0.1391(3) 0.0586(10) Uani 1 1 d . . . H24A H 0.8956 0.7438 0.0830 0.070 Uiso 1 1 calc R . . H24B H 0.8006 0.6557 0.1268 0.070 Uiso 1 1 calc R . . C25 C 0.5867(3) 0.7192(3) 0.2774(3) 0.0423(7) Uani 1 1 d . . . H25A H 0.5874 0.7164 0.2048 0.051 Uiso 1 1 calc R . . C26 C 0.4717(3) 0.7858(3) 0.3109(4) 0.0571(9) Uani 1 1 d . . . H26A H 0.4655 0.7893 0.3834 0.069 Uiso 1 1 calc R . . H26B H 0.4723 0.8607 0.2651 0.069 Uiso 1 1 calc R . . C27 C 0.3664(4) 0.7302(3) 0.3024(4) 0.0721(12) Uani 1 1 d . . . H27A H 0.2939 0.7704 0.3266 0.087 Uiso 1 1 calc R . . H27B H 0.3693 0.7331 0.2286 0.087 Uiso 1 1 calc R . . C28 C 0.3656(4) 0.6100(3) 0.3686(4) 0.0739(12) Uani 1 1 d . . . H28A H 0.3551 0.6072 0.4433 0.089 Uiso 1 1 calc R . . H28B H 0.3000 0.5763 0.3588 0.089 Uiso 1 1 calc R . . C29 C 0.4795(4) 0.5465(3) 0.3363(4) 0.0638(11) Uani 1 1 d . . . H29A H 0.4866 0.5440 0.2633 0.077 Uiso 1 1 calc R . . H29B H 0.4786 0.4711 0.3810 0.077 Uiso 1 1 calc R . . C30 C 0.5856(3) 0.5997(3) 0.3462(3) 0.0536(9) Uani 1 1 d . . . H30A H 0.6578 0.5583 0.3235 0.064 Uiso 1 1 calc R . . H30B H 0.5814 0.5982 0.4198 0.064 Uiso 1 1 calc R . . C31 C 0.7070(3) 0.9231(3) 0.1683(3) 0.0431(7) Uani 1 1 d . . . H31A H 0.6431 0.9700 0.1982 0.052 Uiso 1 1 calc R . . C32 C 0.6738(3) 0.9113(3) 0.0664(3) 0.0501(8) Uani 1 1 d . . . H32A H 0.7364 0.8683 0.0316 0.060 Uiso 1 1 calc R . . H32B H 0.6022 0.8727 0.0846 0.060 Uiso 1 1 calc R . . C33 C 0.6550(4) 1.0252(3) -0.0087(3) 0.0594(10) Uani 1 1 d . . . H33A H 0.6380 1.0169 -0.0739 0.071 Uiso 1 1 calc R . . H33B H 0.5874 1.0651 0.0239 0.071 Uiso 1 1 calc R . . C34 C 0.7627(4) 1.0918(4) -0.0351(3) 0.0701(12) Uani 1 1 d . . . H34A H 0.8278 1.0572 -0.0761 0.084 Uiso 1 1 calc R . . H34B H 0.7451 1.1657 -0.0781 0.084 Uiso 1 1 calc R . . C35 C 0.7987(4) 1.0992(3) 0.0654(3) 0.0676(11) Uani 1 1 d . . . H35A H 0.8705 1.1375 0.0463 0.081 Uiso 1 1 calc R . . H35B H 0.7375 1.1420 0.1017 0.081 Uiso 1 1 calc R . . C36 C 0.8188(3) 0.9865(3) 0.1399(3) 0.0523(9) Uani 1 1 d . . . H36A H 0.8385 0.9947 0.2041 0.063 Uiso 1 1 calc R . . H36B H 0.8843 0.9454 0.1062 0.063 Uiso 1 1 calc R . . C100 C 1.0486(18) 0.7652(15) 0.5758(11) 0.309(11) Uani 1 1 d . . . H10A H 1.0234 0.7523 0.6541 0.371 Uiso 0.50 1 d P . . H10B H 0.9789 0.8098 0.5501 0.371 Uiso 0.50 1 d P . . H10C H 1.1122 0.7691 0.6075 0.371 Uiso 0.50 1 d P . . H10D H 0.9755 0.7730 0.6309 0.371 Uiso 0.50 1 d P . . Cl1 Cl 1.0503(4) 0.6487(3) 0.5524(3) 0.2272(16) Uani 1 1 d . . . Cl2 Cl 1.1492(8) 0.8446(9) 0.5420(9) 0.312(6) Uani 0.50 1 d P . . Cl2A Cl 1.0419(8) 0.8691(7) 0.4749(7) 0.210(3) Uiso 0.50 1 d P . . 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 0.0430(5) 0.0402(5) 0.0358(4) -0.0122(3) -0.0067(3) -0.0050(3) B1 0.070(3) 0.040(2) 0.040(2) -0.0139(16) -0.0108(19) -0.0030(18) F1 0.0787(15) 0.0468(11) 0.0536(12) -0.0208(10) -0.0089(11) 0.0035(10) F2 0.0766(16) 0.0955(18) 0.0554(14) -0.0213(13) -0.0132(12) -0.0238(14) F3 0.0844(19) 0.120(2) 0.107(2) -0.0563(19) 0.0029(16) -0.0429(17) F4 0.117(2) 0.097(2) 0.104(2) -0.0241(18) 0.0360(19) -0.0472(19) F5 0.126(3) 0.113(2) 0.0522(16) -0.0059(15) 0.0123(15) -0.0163(19) F6 0.101(2) 0.112(2) 0.0494(14) -0.0303(14) -0.0112(13) -0.0176(16) F7 0.1101(19) 0.0386(11) 0.0489(12) -0.0169(9) -0.0133(12) 0.0046(11) F8 0.1043(18) 0.0396(11) 0.0433(11) -0.0082(9) -0.0164(11) 0.0018(11) F9 0.0749(14) 0.0409(11) 0.0464(11) -0.0163(9) -0.0136(10) 0.0056(9) F10 0.0897(16) 0.0416(11) 0.0414(11) -0.0088(9) -0.0162(10) 0.0020(10) C1 0.068(2) 0.055(2) 0.0433(19) -0.0227(17) -0.0097(17) -0.0042(18) C2 0.083(3) 0.085(3) 0.054(2) -0.031(2) -0.025(2) 0.010(2) C3 0.098(4) 0.122(5) 0.084(4) -0.058(3) -0.041(3) 0.022(4) C4 0.082(4) 0.167(7) 0.122(5) -0.090(5) -0.045(4) 0.020(4) C5 0.081(4) 0.148(6) 0.134(5) -0.085(5) -0.010(4) -0.035(4) C6 0.077(3) 0.076(3) 0.079(3) -0.032(2) -0.015(2) -0.014(2) C7 0.065(2) 0.048(2) 0.047(2) -0.0189(16) -0.0010(17) -0.0030(17) C8 0.067(2) 0.057(2) 0.048(2) -0.0206(17) 0.0005(18) -0.0077(19) C9 0.065(3) 0.066(3) 0.074(3) -0.032(2) 0.002(2) -0.014(2) C10 0.083(3) 0.062(3) 0.072(3) -0.023(2) 0.020(2) -0.020(2) C11 0.083(3) 0.064(3) 0.047(2) -0.0111(19) 0.010(2) -0.003(2) C12 0.074(3) 0.062(2) 0.045(2) -0.0210(18) -0.0052(19) -0.002(2) C13 0.053(2) 0.0430(18) 0.0406(18) -0.0142(15) -0.0088(15) -0.0061(15) C14 0.061(2) 0.0351(17) 0.0450(19) -0.0165(14) -0.0100(16) -0.0026(15) C15 0.056(2) 0.0345(16) 0.0419(18) -0.0070(14) -0.0118(15) -0.0044(14) C16 0.0456(18) 0.0430(18) 0.0380(17) -0.0132(14) -0.0074(14) -0.0063(14) C17 0.0492(19) 0.0356(16) 0.0445(18) -0.0139(14) -0.0106(15) -0.0017(14) C18 0.053(2) 0.0405(18) 0.0375(17) -0.0069(14) -0.0125(15) -0.0057(14) C19 0.0445(19) 0.0486(19) 0.0439(18) -0.0137(15) -0.0050(15) -0.0018(15) C20 0.045(2) 0.069(3) 0.071(3) -0.024(2) -0.0115(18) -0.0031(18) C21 0.050(2) 0.081(3) 0.094(3) -0.022(3) -0.016(2) 0.003(2) C22 0.069(3) 0.073(3) 0.087(3) -0.016(3) 0.005(2) 0.014(2) C23 0.082(3) 0.069(3) 0.056(2) -0.024(2) -0.001(2) 0.014(2) C24 0.068(2) 0.061(2) 0.047(2) -0.0212(18) -0.0059(18) 0.0009(19) C25 0.0456(18) 0.0403(17) 0.0427(18) -0.0107(14) -0.0093(14) -0.0080(14) C26 0.048(2) 0.0433(19) 0.079(3) -0.0166(18) -0.0084(18) -0.0039(16) C27 0.048(2) 0.058(2) 0.108(4) -0.013(2) -0.021(2) -0.0051(18) C28 0.057(2) 0.059(2) 0.100(4) -0.006(2) -0.016(2) -0.017(2) C29 0.068(3) 0.043(2) 0.080(3) -0.0031(19) -0.023(2) -0.0137(18) C30 0.055(2) 0.0407(19) 0.064(2) -0.0094(17) -0.0139(18) -0.0067(16) C31 0.0502(19) 0.0411(17) 0.0397(17) -0.0101(14) -0.0105(15) -0.0074(14) C32 0.060(2) 0.050(2) 0.0423(19) -0.0107(15) -0.0129(16) -0.0091(16) C33 0.072(3) 0.061(2) 0.047(2) -0.0070(17) -0.0214(19) -0.0106(19) C34 0.085(3) 0.063(3) 0.054(2) 0.0054(19) -0.018(2) -0.019(2) C35 0.081(3) 0.057(2) 0.064(3) 0.0020(19) -0.024(2) -0.028(2) C36 0.057(2) 0.052(2) 0.047(2) -0.0051(16) -0.0128(16) -0.0147(17) C100 0.47(3) 0.33(2) 0.156(11) -0.132(13) 0.075(13) -0.23(2) Cl1 0.317(5) 0.206(3) 0.155(2) -0.032(2) -0.027(3) -0.075(3) Cl2 0.224(8) 0.320(10) 0.386(13) -0.173(9) 0.150(9) -0.167(8) _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 C16 1.817(3) . ? P1 C19 1.824(3) . ? P1 C31 1.825(3) . ? P1 C25 1.831(3) . ? B1 F1 1.433(4) . ? B1 C1 1.620(6) . ? B1 C13 1.658(5) . ? B1 C7 1.670(6) . ? F2 C8 1.349(4) . ? F3 C9 1.351(5) . ? F4 C10 1.354(5) . ? F5 C11 1.349(5) . ? F6 C12 1.337(5) . ? F7 C14 1.355(4) . ? F8 C15 1.341(4) . ? F9 C17 1.344(4) . ? F10 C18 1.352(4) . ? C1 C2 1.398(6) . ? C1 C6 1.398(6) . ? C2 C3 1.384(7) . ? C2 H2A 0.9300 . ? C3 C4 1.349(9) . ? C3 H3A 0.9300 . ? C4 C5 1.368(9) . ? C4 H4A 0.9300 . ? C5 C6 1.392(8) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.385(5) . ? C7 C12 1.392(5) . ? C8 C9 1.384(6) . ? C9 C10 1.361(7) . ? C10 C11 1.352(7) . ? C11 C12 1.384(6) . ? C13 C14 1.383(5) . ? C13 C18 1.383(5) . ? C14 C15 1.384(5) . ? C15 C16 1.397(4) . ? C16 C17 1.401(5) . ? C17 C18 1.374(5) . ? C19 C24 1.527(5) . ? C19 C20 1.543(5) . ? C19 H19A 0.9800 . ? C20 C21 1.518(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.510(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.520(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.528(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C30 1.530(5) . ? C25 C26 1.540(5) . ? C25 H25A 0.9800 . ? C26 C27 1.528(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.526(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.507(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.526(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.537(5) . ? C31 C32 1.546(5) . ? C31 H31A 0.9800 . ? C32 C33 1.524(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.522(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.520(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.510(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C100 Cl2 1.550(15) . ? C100 Cl1 1.589(15) . ? C100 Cl2A 1.600(18) . ? C100 H10A 0.995(12) . ? C100 H10B 0.99(2) . ? C100 H10C 0.941(19) . ? C100 H10D 1.014(16) . ? Cl2 Cl2A 1.638(13) . ? Cl2 H10C 1.153(10) . ? Cl2A H10B 1.227(9) . ? 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 C16 P1 C19 107.47(16) . . ? C16 P1 C31 110.94(15) . . ? C19 P1 C31 114.52(16) . . ? C16 P1 C25 107.92(15) . . ? C19 P1 C25 108.68(16) . . ? C31 P1 C25 107.11(15) . . ? F1 B1 C1 109.4(3) . . ? F1 B1 C13 111.1(3) . . ? C1 B1 C13 104.6(3) . . ? F1 B1 C7 105.3(3) . . ? C1 B1 C7 116.6(3) . . ? C13 B1 C7 109.9(3) . . ? C2 C1 C6 116.9(4) . . ? C2 C1 B1 125.2(4) . . ? C6 C1 B1 117.7(4) . . ? C3 C2 C1 121.3(5) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C4 C3 C2 121.3(6) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C4 C5 C6 121.6(6) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C1 120.1(5) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C8 C7 C12 113.3(4) . . ? C8 C7 B1 123.9(3) . . ? C12 C7 B1 122.6(3) . . ? F2 C8 C9 114.9(4) . . ? F2 C8 C7 121.1(3) . . ? C9 C8 C7 124.1(4) . . ? F3 C9 C10 120.0(4) . . ? F3 C9 C8 120.5(4) . . ? C10 C9 C8 119.5(4) . . ? C11 C10 F4 121.3(4) . . ? C11 C10 C9 119.5(4) . . ? F4 C10 C9 119.2(5) . . ? F5 C11 C10 119.9(4) . . ? F5 C11 C12 120.1(4) . . ? C10 C11 C12 120.0(4) . . ? F6 C12 C11 116.2(4) . . ? F6 C12 C7 120.1(4) . . ? C11 C12 C7 123.7(4) . . ? C14 C13 C18 112.9(3) . . ? C14 C13 B1 126.3(3) . . ? C18 C13 B1 120.8(3) . . ? F7 C14 C13 120.6(3) . . ? F7 C14 C15 115.4(3) . . ? C13 C14 C15 124.0(3) . . ? F8 C15 C14 117.1(3) . . ? F8 C15 C16 120.6(3) . . ? C14 C15 C16 122.3(3) . . ? C15 C16 C17 113.9(3) . . ? C15 C16 P1 125.6(3) . . ? C17 C16 P1 119.8(2) . . ? F9 C17 C18 117.8(3) . . ? F9 C17 C16 120.2(3) . . ? C18 C17 C16 122.0(3) . . ? F10 C18 C17 115.8(3) . . ? F10 C18 C13 119.5(3) . . ? C17 C18 C13 124.7(3) . . ? C24 C19 C20 110.9(3) . . ? C24 C19 P1 114.2(3) . . ? C20 C19 P1 114.5(2) . . ? C24 C19 H19A 105.4 . . ? C20 C19 H19A 105.4 . . ? P1 C19 H19A 105.4 . . ? C21 C20 C19 108.8(3) . . ? C21 C20 H20A 109.9 . . ? C19 C20 H20A 109.9 . . ? C21 C20 H20B 109.9 . . ? C19 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C22 C21 C20 112.7(4) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 111.8(4) . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C22 C23 C24 112.1(4) . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C19 C24 C23 108.4(3) . . ? C19 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? C19 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? C30 C25 C26 110.6(3) . . ? C30 C25 P1 115.9(2) . . ? C26 C25 P1 110.3(2) . . ? C30 C25 H25A 106.5 . . ? C26 C25 H25A 106.5 . . ? P1 C25 H25A 106.5 . . ? C27 C26 C25 109.4(3) . . ? C27 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? C27 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C28 C27 C26 111.6(3) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C29 C28 C27 110.6(4) . . ? C29 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C28 C29 C30 111.2(3) . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C25 109.8(3) . . ? C29 C30 H30A 109.7 . . ? C25 C30 H30A 109.7 . . ? C29 C30 H30B 109.7 . . ? C25 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C36 C31 C32 110.1(3) . . ? C36 C31 P1 113.6(2) . . ? C32 C31 P1 113.7(2) . . ? C36 C31 H31A 106.3 . . ? C32 C31 H31A 106.3 . . ? P1 C31 H31A 106.3 . . ? C33 C32 C31 109.8(3) . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C32 111.8(3) . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 111.1(3) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 112.1(3) . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35B 109.2 . . ? C34 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C31 109.9(3) . . ? C35 C36 H36A 109.7 . . ? C31 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? C31 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? Cl2 C100 Cl1 128.0(13) . . ? Cl2 C100 Cl2A 62.7(8) . . ? Cl1 C100 Cl2A 114.4(8) . . ? Cl2 C100 H10A 106.1(12) . . ? Cl1 C100 H10A 106.2(13) . . ? Cl2A C100 H10A 135.1(17) . . ? Cl2 C100 H10B 106.0(15) . . ? Cl1 C100 H10B 106.3(11) . . ? Cl2A C100 H10B 50.0(9) . . ? H10A C100 H10B 101.3(16) . . ? Cl2 C100 H10C 47.9(9) . . ? Cl1 C100 H10C 112.0(19) . . ? Cl2A C100 H10C 110.2(12) . . ? H10A C100 H10C 69.0(10) . . ? H10B C100 H10C 141.7(17) . . ? Cl2 C100 H10D 123.1(11) . . ? Cl1 C100 H10D 107.8(11) . . ? Cl2A C100 H10D 106.8(19) . . ? H10A C100 H10D 39.7(5) . . ? H10B C100 H10D 62.5(13) . . ? H10C C100 H10D 104.9(11) . . ? C100 Cl2 Cl2A 60.2(8) . . ? C100 Cl2 H10C 37.3(8) . . ? Cl2A Cl2 H10C 97.2(6) . . ? C100 Cl2A Cl2 57.2(7) . . ? C100 Cl2A H10B 38.3(8) . . ? Cl2 Cl2A H10B 90.7(6) . . ? 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 F1 B1 C1 C2 148.8(4) . . . . ? C13 B1 C1 C2 -92.1(4) . . . . ? C7 B1 C1 C2 29.5(5) . . . . ? F1 B1 C1 C6 -36.7(5) . . . . ? C13 B1 C1 C6 82.4(4) . . . . ? C7 B1 C1 C6 -156.0(3) . . . . ? C6 C1 C2 C3 -0.8(6) . . . . ? B1 C1 C2 C3 173.8(4) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C2 C3 C4 C5 1.0(9) . . . . ? C3 C4 C5 C6 -1.8(9) . . . . ? C4 C5 C6 C1 1.3(8) . . . . ? C2 C1 C6 C5 0.0(6) . . . . ? B1 C1 C6 C5 -175.0(4) . . . . ? F1 B1 C7 C8 92.2(4) . . . . ? C1 B1 C7 C8 -146.3(4) . . . . ? C13 B1 C7 C8 -27.5(5) . . . . ? F1 B1 C7 C12 -82.4(4) . . . . ? C1 B1 C7 C12 39.1(5) . . . . ? C13 B1 C7 C12 158.0(3) . . . . ? C12 C7 C8 F2 177.5(3) . . . . ? B1 C7 C8 F2 2.5(6) . . . . ? C12 C7 C8 C9 -2.3(6) . . . . ? B1 C7 C8 C9 -177.4(4) . . . . ? F2 C8 C9 F3 0.9(6) . . . . ? C7 C8 C9 F3 -179.2(4) . . . . ? F2 C8 C9 C10 -179.7(4) . . . . ? C7 C8 C9 C10 0.2(7) . . . . ? F3 C9 C10 C11 -178.7(4) . . . . ? C8 C9 C10 C11 2.0(7) . . . . ? F3 C9 C10 F4 0.4(7) . . . . ? C8 C9 C10 F4 -178.9(4) . . . . ? F4 C10 C11 F5 -0.8(7) . . . . ? C9 C10 C11 F5 178.3(4) . . . . ? F4 C10 C11 C12 179.2(4) . . . . ? C9 C10 C11 C12 -1.7(7) . . . . ? F5 C11 C12 F6 -2.8(6) . . . . ? C10 C11 C12 F6 177.2(4) . . . . ? F5 C11 C12 C7 179.2(4) . . . . ? C10 C11 C12 C7 -0.7(7) . . . . ? C8 C7 C12 F6 -175.2(3) . . . . ? B1 C7 C12 F6 -0.1(6) . . . . ? C8 C7 C12 C11 2.6(6) . . . . ? B1 C7 C12 C11 177.7(4) . . . . ? F1 B1 C13 C14 8.6(5) . . . . ? C1 B1 C13 C14 -109.3(4) . . . . ? C7 B1 C13 C14 124.8(4) . . . . ? F1 B1 C13 C18 -171.8(3) . . . . ? C1 B1 C13 C18 70.3(4) . . . . ? C7 B1 C13 C18 -55.6(4) . . . . ? C18 C13 C14 F7 -177.4(3) . . . . ? B1 C13 C14 F7 2.2(6) . . . . ? C18 C13 C14 C15 3.9(5) . . . . ? B1 C13 C14 C15 -176.5(3) . . . . ? F7 C14 C15 F8 0.1(5) . . . . ? C13 C14 C15 F8 178.9(3) . . . . ? F7 C14 C15 C16 -179.5(3) . . . . ? C13 C14 C15 C16 -0.7(6) . . . . ? F8 C15 C16 C17 177.3(3) . . . . ? C14 C15 C16 C17 -3.1(5) . . . . ? F8 C15 C16 P1 -11.7(5) . . . . ? C14 C15 C16 P1 167.9(3) . . . . ? C19 P1 C16 C15 140.3(3) . . . . ? C31 P1 C16 C15 14.4(4) . . . . ? C25 P1 C16 C15 -102.6(3) . . . . ? C19 P1 C16 C17 -49.1(3) . . . . ? C31 P1 C16 C17 -175.0(3) . . . . ? C25 P1 C16 C17 67.9(3) . . . . ? C15 C16 C17 F9 -177.0(3) . . . . ? P1 C16 C17 F9 11.4(4) . . . . ? C15 C16 C17 C18 3.6(5) . . . . ? P1 C16 C17 C18 -168.0(3) . . . . ? F9 C17 C18 F10 -2.3(4) . . . . ? C16 C17 C18 F10 177.1(3) . . . . ? F9 C17 C18 C13 -179.7(3) . . . . ? C16 C17 C18 C13 -0.3(5) . . . . ? C14 C13 C18 F10 179.3(3) . . . . ? B1 C13 C18 F10 -0.4(5) . . . . ? C14 C13 C18 C17 -3.4(5) . . . . ? B1 C13 C18 C17 176.9(3) . . . . ? C16 P1 C19 C24 -178.0(3) . . . . ? C31 P1 C19 C24 -54.2(3) . . . . ? C25 P1 C19 C24 65.5(3) . . . . ? C16 P1 C19 C20 -48.5(3) . . . . ? C31 P1 C19 C20 75.2(3) . . . . ? C25 P1 C19 C20 -165.1(3) . . . . ? C24 C19 C20 C21 -59.6(4) . . . . ? P1 C19 C20 C21 169.3(3) . . . . ? C19 C20 C21 C22 55.4(5) . . . . ? C20 C21 C22 C23 -53.1(5) . . . . ? C21 C22 C23 C24 53.7(5) . . . . ? C20 C19 C24 C23 60.3(4) . . . . ? P1 C19 C24 C23 -168.5(3) . . . . ? C22 C23 C24 C19 -56.9(5) . . . . ? C16 P1 C25 C30 -69.7(3) . . . . ? C19 P1 C25 C30 46.6(3) . . . . ? C31 P1 C25 C30 170.8(3) . . . . ? C16 P1 C25 C26 56.9(3) . . . . ? C19 P1 C25 C26 173.2(2) . . . . ? C31 P1 C25 C26 -62.6(3) . . . . ? C30 C25 C26 C27 -57.5(4) . . . . ? P1 C25 C26 C27 173.0(3) . . . . ? C25 C26 C27 C28 56.4(5) . . . . ? C26 C27 C28 C29 -56.5(5) . . . . ? C27 C28 C29 C30 56.9(5) . . . . ? C28 C29 C30 C25 -58.1(5) . . . . ? C26 C25 C30 C29 58.3(4) . . . . ? P1 C25 C30 C29 -175.2(3) . . . . ? C16 P1 C31 C36 72.0(3) . . . . ? C19 P1 C31 C36 -49.9(3) . . . . ? C25 P1 C31 C36 -170.5(2) . . . . ? C16 P1 C31 C32 -161.1(2) . . . . ? C19 P1 C31 C32 77.0(3) . . . . ? C25 P1 C31 C32 -43.6(3) . . . . ? C36 C31 C32 C33 -58.0(4) . . . . ? P1 C31 C32 C33 173.2(3) . . . . ? C31 C32 C33 C34 56.2(4) . . . . ? C32 C33 C34 C35 -54.4(5) . . . . ? C33 C34 C35 C36 54.9(5) . . . . ? C34 C35 C36 C31 -57.1(5) . . . . ? C32 C31 C36 C35 58.5(4) . . . . ? P1 C31 C36 C35 -172.7(3) . . . . ? Cl1 C100 Cl2 Cl2A 100.7(15) . . . . ? Cl1 C100 Cl2A Cl2 -121.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.978 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.067 #===end