Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'D. W. Stephan' _publ_contact_author_address ; Dept of Chemistry & Biochemistry University of Windsor Windsor Ontario N9P 3P4 CANADA ; _publ_contact_author_email STEPHAN@UWINDSOR.CA _publ_section_title ; Tuning Lewis Acidity using The Reactivity of Frustrated Lewis Pairs: Facile Formation of Phosphine-Boranes and Cationic Phosphonium-Boranes ; loop_ _publ_author_name 'D. W. Stephan' 'Lourdes Cabrera' 'Preston A. Chase' 'Emily Hollink' 'Jason D. Masuda' 'Pingrong Wei' ; G.C.Welch ; data_i-Pr3P(C6F4)BF(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 636617' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C27 H21 B F15 P' _chemical_formula_weight 672.22 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 9.544(6) _cell_length_b 18.426(11) _cell_length_c 17.134(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.156(12) _cell_angle_gamma 90.00 _cell_volume 2908(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.345020 _exptl_absorpt_correction_T_max 0.488936 _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_reflns_number 12247 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 23.20 _reflns_number_total 4120 _reflns_number_gt 2650 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^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 SHELXL _refine_ls_extinction_coef 0.0039(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4120 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 -0.00290(7) 0.19791(4) 0.34455(5) 0.0574(2) Uani 1 1 d . . . F15 F 0.26287(17) 0.50535(8) 0.18859(10) 0.0764(5) Uani 1 1 d . . . B1 B 0.3565(3) 0.45029(16) 0.23198(19) 0.0580(8) Uani 1 1 d . . . C1 C 0.4485(3) 0.41724(16) 0.17010(16) 0.0601(7) Uani 1 1 d . . . C2 C 0.5217(3) 0.4646(2) 0.13258(18) 0.0784(9) Uani 1 1 d . . . C3 C 0.6059(4) 0.4443(3) 0.0809(2) 0.0979(12) Uani 1 1 d . . . C4 C 0.6151(4) 0.3718(4) 0.0643(2) 0.1067(13) Uani 1 1 d . . . C5 C 0.5452(4) 0.3220(3) 0.0978(2) 0.0922(11) Uani 1 1 d . . . C6 C 0.4630(3) 0.34501(19) 0.14962(18) 0.0707(8) Uani 1 1 d . . . C7 C 0.4638(3) 0.48962(14) 0.31299(16) 0.0619(8) Uani 1 1 d . . . C8 C 0.3982(4) 0.52830(16) 0.36452(19) 0.0780(9) Uani 1 1 d . . . C9 C 0.4708(7) 0.56683(19) 0.4301(2) 0.1043(13) Uani 1 1 d . . . C10 C 0.6187(7) 0.5689(2) 0.4501(2) 0.1108(16) Uani 1 1 d . . . C11 C 0.6928(5) 0.5298(2) 0.4041(2) 0.1049(13) Uani 1 1 d . . . C12 C 0.6138(4) 0.49105(17) 0.33717(18) 0.0729(9) Uani 1 1 d . . . C13 C 0.2599(3) 0.38794(13) 0.26249(15) 0.0501(6) Uani 1 1 d . . . C14 C 0.1102(3) 0.38091(14) 0.23718(17) 0.0601(7) Uani 1 1 d . . . C15 C 0.0335(3) 0.32746(15) 0.26409(18) 0.0624(8) Uani 1 1 d . . . C16 C 0.0987(3) 0.27487(14) 0.32043(16) 0.0539(7) Uani 1 1 d . . . C17 C 0.2494(3) 0.28149(13) 0.34661(16) 0.0513(6) Uani 1 1 d . . . C18 C 0.3225(2) 0.33526(13) 0.31896(16) 0.0503(6) Uani 1 1 d . . . C19 C -0.3076(3) 0.1954(2) 0.3015(3) 0.144(2) Uani 1 1 d . . . H19A H -0.3915 0.2136 0.3161 0.216 Uiso 1 1 calc R . . H19B H -0.3047 0.1434 0.3063 0.216 Uiso 1 1 calc R . . H19C H -0.3125 0.2088 0.2467 0.216 Uiso 1 1 calc R . . C20 C -0.1850(4) 0.29508(18) 0.3986(3) 0.1013(12) Uani 1 1 d . . . H20A H -0.2820 0.3046 0.4023 0.152 Uiso 1 1 calc R . . H20B H -0.1530 0.3342 0.3705 0.152 Uiso 1 1 calc R . . H20C H -0.1213 0.2909 0.4520 0.152 Uiso 1 1 calc R . . C21 C -0.1829(3) 0.2247(2) 0.3529(3) 0.1092(13) Uani 1 1 d . . . H21A H -0.1827 0.1929 0.3987 0.131 Uiso 1 1 calc R . . C22 C -0.0678(4) 0.1651(2) 0.17820(19) 0.1024(12) Uani 1 1 d . . . H22A H -0.0712 0.1284 0.1380 0.154 Uiso 1 1 calc R . . H22B H -0.0032 0.2032 0.1716 0.154 Uiso 1 1 calc R . . H22C H -0.1633 0.1847 0.1721 0.154 Uiso 1 1 calc R . . C23 C 0.1341(4) 0.0931(2) 0.2734(2) 0.1082(13) Uani 1 1 d . . . H23A H 0.1262 0.0584 0.2306 0.162 Uiso 1 1 calc R . . H23B H 0.1605 0.0685 0.3245 0.162 Uiso 1 1 calc R . . H23C H 0.2071 0.1283 0.2713 0.162 Uiso 1 1 calc R . . C24 C -0.0125(3) 0.13140(16) 0.26334(18) 0.0723(8) Uani 1 1 d . . . H24A H -0.0829 0.0942 0.2686 0.087 Uiso 1 1 calc R . . C25 C 0.1162(4) 0.2092(2) 0.5132(2) 0.0974(11) Uani 1 1 d . . . H25A H 0.1685 0.1848 0.5616 0.146 Uiso 1 1 calc R . . H25B H 0.0235 0.2247 0.5191 0.146 Uiso 1 1 calc R . . H25C H 0.1705 0.2507 0.5040 0.146 Uiso 1 1 calc R . . C26 C 0.0199(4) 0.08597(18) 0.4567(2) 0.0856(10) Uani 1 1 d . . . H26A H 0.0735 0.0655 0.5072 0.128 Uiso 1 1 calc R . . H26B H 0.0177 0.0521 0.4139 0.128 Uiso 1 1 calc R . . H26C H -0.0775 0.0963 0.4591 0.128 Uiso 1 1 calc R . . C27 C 0.0937(3) 0.15668(15) 0.44065(17) 0.0689(8) Uani 1 1 d . . . H27A H 0.1904 0.1434 0.4357 0.083 Uiso 1 1 calc R . . F1 F 0.5184(2) 0.53697(12) 0.14712(11) 0.1020(6) Uani 1 1 d . . . F2 F 0.6745(3) 0.49523(17) 0.04755(13) 0.1444(10) Uani 1 1 d . . . F3 F 0.6965(3) 0.3505(2) 0.01470(15) 0.1708(12) Uani 1 1 d . . . F4 F 0.5536(3) 0.25061(15) 0.08155(14) 0.1372(9) Uani 1 1 d . . . F5 F 0.39737(19) 0.29091(9) 0.18015(11) 0.0848(5) Uani 1 1 d . . . F6 F 0.2514(3) 0.52672(11) 0.34972(12) 0.1054(7) Uani 1 1 d . . . F7 F 0.4000(4) 0.60293(12) 0.47733(14) 0.1473(10) Uani 1 1 d . . . F8 F 0.6970(4) 0.60619(15) 0.51501(14) 0.1766(13) Uani 1 1 d . . . F9 F 0.8386(3) 0.52880(17) 0.42295(14) 0.1554(11) Uani 1 1 d . . . F10 F 0.69327(18) 0.45352(11) 0.29554(11) 0.0907(6) Uani 1 1 d . . . F11 F 0.03026(17) 0.42699(9) 0.18055(11) 0.0915(6) Uani 1 1 d . . . F12 F -0.11235(16) 0.32562(10) 0.23243(12) 0.0966(6) Uani 1 1 d . . . F13 F 0.32795(15) 0.23235(8) 0.39958(10) 0.0730(5) Uani 1 1 d . . . F14 F 0.46939(14) 0.33486(7) 0.34835(9) 0.0665(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0451(4) 0.0571(4) 0.0738(5) -0.0056(4) 0.0222(3) -0.0057(3) F15 0.0816(11) 0.0630(10) 0.0856(12) 0.0240(9) 0.0236(9) 0.0137(8) B1 0.0629(19) 0.0498(18) 0.062(2) 0.0070(16) 0.0177(16) 0.0100(15) C1 0.0541(16) 0.075(2) 0.0494(16) 0.0031(15) 0.0103(13) -0.0031(15) C2 0.076(2) 0.098(3) 0.0588(19) -0.0025(19) 0.0133(17) -0.0115(19) C3 0.074(2) 0.164(4) 0.060(2) 0.001(3) 0.0243(19) -0.019(3) C4 0.082(3) 0.176(5) 0.068(2) -0.023(3) 0.032(2) 0.006(3) C5 0.083(2) 0.120(3) 0.071(2) -0.022(2) 0.015(2) 0.019(2) C6 0.0612(18) 0.087(2) 0.0600(19) -0.0126(18) 0.0096(15) 0.0098(17) C7 0.085(2) 0.0450(15) 0.0581(18) 0.0036(14) 0.0235(16) -0.0088(14) C8 0.121(3) 0.0495(17) 0.064(2) 0.0039(17) 0.025(2) -0.0013(19) C9 0.193(5) 0.055(2) 0.077(3) 0.003(2) 0.056(3) -0.007(3) C10 0.196(5) 0.080(3) 0.058(2) -0.012(2) 0.036(3) -0.063(3) C11 0.119(3) 0.117(3) 0.069(2) 0.011(2) 0.008(2) -0.065(3) C12 0.096(2) 0.067(2) 0.0556(19) 0.0046(16) 0.0214(19) -0.0287(18) C13 0.0529(16) 0.0435(14) 0.0542(15) -0.0010(13) 0.0147(13) 0.0059(12) C14 0.0544(17) 0.0539(16) 0.0663(18) 0.0103(15) 0.0057(14) 0.0146(14) C15 0.0377(15) 0.0662(18) 0.079(2) -0.0013(16) 0.0065(14) 0.0033(13) C16 0.0428(14) 0.0503(15) 0.0681(17) -0.0009(14) 0.0136(13) 0.0029(12) C17 0.0440(14) 0.0450(15) 0.0631(16) 0.0063(13) 0.0106(13) 0.0055(12) C18 0.0355(14) 0.0491(15) 0.0660(17) -0.0014(14) 0.0125(12) 0.0006(11) C19 0.0420(19) 0.155(4) 0.223(5) -0.066(4) 0.013(3) -0.005(2) C20 0.077(2) 0.088(2) 0.148(3) -0.015(2) 0.045(2) 0.0177(18) C21 0.056(2) 0.107(3) 0.176(4) -0.044(3) 0.052(2) -0.0101(18) C22 0.140(3) 0.098(3) 0.074(2) -0.007(2) 0.035(2) -0.037(2) C23 0.107(3) 0.101(3) 0.135(3) -0.029(2) 0.064(3) 0.011(2) C24 0.079(2) 0.0645(18) 0.080(2) -0.0113(17) 0.0323(17) -0.0155(16) C25 0.099(3) 0.109(3) 0.074(2) -0.009(2) 0.0067(19) -0.006(2) C26 0.088(2) 0.081(2) 0.097(2) 0.0150(19) 0.0404(19) -0.0150(18) C27 0.0624(17) 0.0722(19) 0.077(2) 0.0058(17) 0.0272(15) -0.0056(15) F1 0.1190(16) 0.1019(15) 0.0922(13) 0.0158(12) 0.0402(12) -0.0293(12) F2 0.1238(17) 0.232(3) 0.0923(16) 0.0140(17) 0.0551(14) -0.0491(18) F3 0.134(2) 0.280(4) 0.1232(18) -0.046(2) 0.0787(17) 0.019(2) F4 0.148(2) 0.142(2) 0.1240(19) -0.0471(16) 0.0405(16) 0.0442(16) F5 0.0969(13) 0.0685(11) 0.0907(13) -0.0105(10) 0.0273(11) 0.0059(9) F6 0.1303(18) 0.0950(14) 0.1022(15) 0.0027(12) 0.0507(13) 0.0403(13) F7 0.282(3) 0.0819(14) 0.0959(15) -0.0125(12) 0.0816(19) 0.0206(17) F8 0.295(4) 0.145(2) 0.0807(15) -0.0369(15) 0.0321(19) -0.111(2) F9 0.130(2) 0.225(3) 0.0941(16) -0.0017(17) -0.0009(14) -0.096(2) F10 0.0688(11) 0.1252(15) 0.0773(12) 0.0002(12) 0.0177(9) -0.0176(10) F11 0.0694(11) 0.0922(12) 0.1004(13) 0.0354(11) 0.0000(10) 0.0168(9) F12 0.0427(9) 0.1158(15) 0.1190(15) 0.0162(12) -0.0008(9) 0.0037(9) F13 0.0499(8) 0.0647(9) 0.1005(12) 0.0320(9) 0.0125(8) 0.0032(7) F14 0.0409(8) 0.0621(9) 0.0930(11) 0.0179(8) 0.0111(8) -0.0009(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 C16 1.825(3) . ? P1 C21 1.828(3) . ? P1 C27 1.829(3) . ? P1 C24 1.839(3) . ? F15 B1 1.426(3) . ? B1 C13 1.642(4) . ? B1 C1 1.659(4) . ? B1 C7 1.661(4) . ? C1 C2 1.377(4) . ? C1 C6 1.393(4) . ? C2 F1 1.359(4) . ? C2 C3 1.393(5) . ? C3 F2 1.354(4) . ? C3 C4 1.374(6) . ? C4 C5 1.347(6) . ? C4 F3 1.350(4) . ? C5 F4 1.352(5) . ? C5 C6 1.395(5) . ? C6 F5 1.353(4) . ? C7 C12 1.382(4) . ? C7 C8 1.403(4) . ? C8 C9 1.356(5) . ? C8 F6 1.358(4) . ? C9 F7 1.357(4) . ? C9 C10 1.364(6) . ? C10 F8 1.354(4) . ? C10 C11 1.390(6) . ? C11 F9 1.343(5) . ? C11 C12 1.393(5) . ? C12 F10 1.359(4) . ? C13 C14 1.386(4) . ? C13 C18 1.390(3) . ? C14 F11 1.363(3) . ? C14 C15 1.377(4) . ? C15 F12 1.355(3) . ? C15 C16 1.394(4) . ? C16 C17 1.396(3) . ? C17 F13 1.360(3) . ? C17 C18 1.366(3) . ? C18 F14 1.360(3) . ? C19 C21 1.391(5) . ? C20 C21 1.518(5) . ? C22 C24 1.546(4) . ? C23 C24 1.536(4) . ? C25 C27 1.545(4) . ? C26 C27 1.539(4) . ? 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 C21 111.91(16) . . ? C16 P1 C27 110.75(13) . . ? C21 P1 C27 107.74(19) . . ? C16 P1 C24 105.70(13) . . ? C21 P1 C24 112.17(15) . . ? C27 P1 C24 108.55(14) . . ? F15 B1 C13 109.6(2) . . ? F15 B1 C1 107.0(2) . . ? C13 B1 C1 112.4(2) . . ? F15 B1 C7 106.9(2) . . ? C13 B1 C7 108.3(2) . . ? C1 B1 C7 112.4(2) . . ? C2 C1 C6 113.0(3) . . ? C2 C1 B1 118.9(3) . . ? C6 C1 B1 128.0(3) . . ? F1 C2 C1 119.8(3) . . ? F1 C2 C3 115.1(4) . . ? C1 C2 C3 125.0(4) . . ? F2 C3 C4 121.5(4) . . ? F2 C3 C2 120.3(5) . . ? C4 C3 C2 118.1(4) . . ? C5 C4 F3 120.1(5) . . ? C5 C4 C3 120.5(4) . . ? F3 C4 C3 119.4(5) . . ? C4 C5 F4 120.8(4) . . ? C4 C5 C6 119.2(4) . . ? F4 C5 C6 120.0(4) . . ? F5 C6 C1 121.3(3) . . ? F5 C6 C5 114.6(3) . . ? C1 C6 C5 124.0(4) . . ? C12 C7 C8 113.5(3) . . ? C12 C7 B1 128.5(3) . . ? C8 C7 B1 117.9(3) . . ? C9 C8 F6 116.4(4) . . ? C9 C8 C7 124.9(4) . . ? F6 C8 C7 118.7(3) . . ? C8 C9 F7 121.6(5) . . ? C8 C9 C10 119.6(4) . . ? F7 C9 C10 118.7(5) . . ? F8 C10 C9 122.2(5) . . ? F8 C10 C11 118.4(5) . . ? C9 C10 C11 119.3(4) . . ? F9 C11 C10 121.3(4) . . ? F9 C11 C12 119.7(4) . . ? C10 C11 C12 119.0(4) . . ? F10 C12 C7 120.6(3) . . ? F10 C12 C11 115.8(3) . . ? C7 C12 C11 123.5(4) . . ? C14 C13 C18 111.9(2) . . ? C14 C13 B1 125.8(2) . . ? C18 C13 B1 122.3(2) . . ? F11 C14 C15 115.9(2) . . ? F11 C14 C13 120.2(2) . . ? C15 C14 C13 123.8(2) . . ? F12 C15 C14 117.7(2) . . ? F12 C15 C16 119.0(2) . . ? C14 C15 C16 123.3(2) . . ? C15 C16 C17 113.4(2) . . ? C15 C16 P1 121.96(19) . . ? C17 C16 P1 123.99(19) . . ? F13 C17 C18 118.2(2) . . ? F13 C17 C16 119.9(2) . . ? C18 C17 C16 121.9(2) . . ? F14 C18 C17 116.0(2) . . ? F14 C18 C13 118.4(2) . . ? C17 C18 C13 125.6(2) . . ? C19 C21 C20 122.3(3) . . ? C19 C21 P1 120.7(3) . . ? C20 C21 P1 114.2(2) . . ? C23 C24 C22 111.5(3) . . ? C23 C24 P1 111.0(2) . . ? C22 C24 P1 112.5(2) . . ? C26 C27 C25 111.1(3) . . ? C26 C27 P1 111.5(2) . . ? C25 C27 P1 113.3(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.20 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.229 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.033 #===end data_Cy3P(C6F4)BF(C6F5)2.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 636618' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C37 H35 B Cl2 F15 P' _chemical_formula_weight 877.33 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 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 14.235(3) _cell_length_b 25.588(5) _cell_length_c 21.701(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.113(5) _cell_angle_gamma 90.00 _cell_volume 7756(2) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.481030 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 273(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 17798 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 23.41 _reflns_number_total 9885 _reflns_number_gt 4706 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 9885 _refine_ls_number_parameters 979 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1809 _refine_ls_R_factor_gt 0.1082 _refine_ls_wR_factor_ref 0.3517 _refine_ls_wR_factor_gt 0.2841 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.012 _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 0.89067(14) 0.14473(9) 0.68098(11) 0.0613(7) Uani 1 1 d . . . P2 P 0.40748(14) 0.37301(9) 0.67897(11) 0.0632(7) Uani 1 1 d . . . B1 B 0.4686(6) 0.0676(4) 0.6922(5) 0.056(2) Uani 1 1 d . . . B2 B -0.0135(6) 0.4494(4) 0.6960(5) 0.060(3) Uani 1 1 d . . . F1 F 0.4586(6) 0.0995(3) 0.8200(3) 0.131(2) Uani 1 1 d . . . F2 F 0.3310(8) 0.1641(3) 0.8542(4) 0.186(4) Uani 1 1 d . . . F3 F 0.2029(5) 0.2178(3) 0.7661(4) 0.161(3) Uani 1 1 d . . . F4 F 0.2088(4) 0.2049(2) 0.6438(4) 0.133(3) Uani 1 1 d . . . F5 F 0.3290(5) 0.1389(2) 0.6087(3) 0.116(2) Uani 1 1 d . . . F6 F 0.3307(3) -0.0193(2) 0.6668(3) 0.0944(17) Uani 1 1 d . . . F7 F 0.2595(4) -0.0623(2) 0.5571(3) 0.122(2) Uani 1 1 d . . . F8 F 0.3078(5) -0.0258(4) 0.4508(4) 0.161(3) Uani 1 1 d . . . F9 F 0.4287(5) 0.0571(4) 0.4571(3) 0.151(3) Uani 1 1 d . . . F10 F 0.5006(4) 0.1013(3) 0.5659(3) 0.1065(19) Uani 1 1 d . . . F11 F 0.6299(3) 0.00341(18) 0.6806(2) 0.0721(13) Uani 1 1 d . . . F12 F 0.8031(3) 0.03004(17) 0.6788(2) 0.0684(13) Uani 1 1 d . . . F13 F 0.7209(3) 0.20791(18) 0.6990(2) 0.0811(15) Uani 1 1 d . . . F14 F 0.5480(3) 0.18076(18) 0.7026(3) 0.0831(15) Uani 1 1 d . . . F15 F 0.4789(3) 0.0274(2) 0.7371(2) 0.0775(14) Uani 1 1 d . . . F16 F -0.1495(3) 0.5372(2) 0.6665(3) 0.0854(15) Uani 1 1 d . . . F17 F -0.2261(4) 0.5732(2) 0.5535(3) 0.116(2) Uani 1 1 d . . . F18 F -0.1922(5) 0.5254(4) 0.4496(3) 0.148(3) Uani 1 1 d . . . F19 F -0.0777(5) 0.4387(3) 0.4604(3) 0.149(3) Uani 1 1 d . . . F20 F 0.0035(4) 0.4036(3) 0.5733(3) 0.117(2) Uani 1 1 d . . . F21 F 0.0062(7) 0.4236(3) 0.8273(4) 0.151(3) Uani 1 1 d . . . F22 F -0.1058(9) 0.3634(4) 0.8812(5) 0.237(6) Uani 1 1 d . . . F23 F -0.2510(7) 0.3073(3) 0.8075(6) 0.243(6) Uani 1 1 d . . . F24 F -0.2793(5) 0.3145(3) 0.6808(6) 0.216(6) Uani 1 1 d . . . F25 F -0.1734(5) 0.3779(2) 0.6287(4) 0.129(3) Uani 1 1 d . . . F26 F 0.0642(3) 0.33672(19) 0.7015(3) 0.0923(17) Uani 1 1 d . . . F27 F 0.2359(3) 0.30889(19) 0.6929(3) 0.0955(17) Uani 1 1 d . . . F28 F 0.3212(3) 0.48776(17) 0.6812(2) 0.0707(13) Uani 1 1 d . . . F29 F 0.1485(3) 0.51391(18) 0.6840(2) 0.0695(13) Uani 1 1 d . . . F30 F -0.0015(3) 0.4930(2) 0.7377(2) 0.0789(14) Uani 1 1 d . . . C1 C 0.3971(6) 0.1124(3) 0.7120(5) 0.068(2) Uani 1 1 d . . . C2 C 0.3934(8) 0.1226(4) 0.7739(6) 0.090(3) Uani 1 1 d . . . C3 C 0.3270(11) 0.1578(5) 0.7917(7) 0.106(4) Uani 1 1 d . . . C4 C 0.2661(10) 0.1844(5) 0.7479(10) 0.113(5) Uani 1 1 d . . . C5 C 0.2688(7) 0.1785(4) 0.6875(7) 0.097(4) Uani 1 1 d . . . C6 C 0.3300(6) 0.1420(4) 0.6700(6) 0.081(3) Uani 1 1 d . . . C7 C 0.4233(5) 0.0426(3) 0.6240(4) 0.065(2) Uani 1 1 d . . . C8 C 0.3599(6) 0.0020(4) 0.6164(5) 0.067(2) Uani 1 1 d . . . C9 C 0.3208(6) -0.0213(4) 0.5594(6) 0.092(3) Uani 1 1 d . . . C10 C 0.3445(8) -0.0016(5) 0.5058(6) 0.099(4) Uani 1 1 d . . . C11 C 0.4038(8) 0.0375(5) 0.5096(6) 0.101(4) Uani 1 1 d . . . C12 C 0.4423(7) 0.0598(4) 0.5659(5) 0.077(3) Uani 1 1 d . . . C13 C 0.5784(5) 0.0902(3) 0.6923(4) 0.0539(19) Uani 1 1 d . . . C14 C 0.6496(5) 0.0550(3) 0.6865(4) 0.056(2) Uani 1 1 d . . . C15 C 0.7439(5) 0.0696(3) 0.6851(4) 0.055(2) Uani 1 1 d . . . C16 C 0.7725(5) 0.1205(3) 0.6876(3) 0.054(2) Uani 1 1 d . . . C17 C 0.7020(6) 0.1565(3) 0.6952(4) 0.063(2) Uani 1 1 d . . . C18 C 0.6093(5) 0.1416(3) 0.6964(4) 0.061(2) Uani 1 1 d . . . C19 C 0.8710(6) 0.1984(4) 0.6247(4) 0.075(3) Uani 1 1 d . . . H19A H 0.8473 0.2275 0.6468 0.090 Uiso 1 1 calc R . . C20 C 0.9668(6) 0.2179(4) 0.6078(4) 0.089(3) Uani 1 1 d . . . H20A H 1.0123 0.2264 0.6457 0.107 Uiso 1 1 calc R . . H20B H 0.9943 0.1907 0.5856 0.107 Uiso 1 1 calc R . . C21 C 0.9451(8) 0.2674(4) 0.5655(6) 0.116(4) Uani 1 1 d . . . H21A H 0.9246 0.2953 0.5901 0.139 Uiso 1 1 calc R . . H21B H 1.0038 0.2786 0.5530 0.139 Uiso 1 1 calc R . . C22 C 0.8731(9) 0.2597(6) 0.5099(6) 0.137(5) Uani 1 1 d . . . H22A H 0.8958 0.2348 0.4826 0.165 Uiso 1 1 calc R . . H22B H 0.8609 0.2926 0.4874 0.165 Uiso 1 1 calc R . . C23 C 0.7794(8) 0.2395(6) 0.5273(6) 0.134(5) Uani 1 1 d . . . H23A H 0.7535 0.2661 0.5511 0.160 Uiso 1 1 calc R . . H23B H 0.7328 0.2330 0.4891 0.160 Uiso 1 1 calc R . . C24 C 0.7953(7) 0.1894(4) 0.5659(5) 0.099(3) Uani 1 1 d . . . H24A H 0.7358 0.1787 0.5776 0.119 Uiso 1 1 calc R . . H24B H 0.8159 0.1617 0.5410 0.119 Uiso 1 1 calc R . . C25 C 0.9539(6) 0.1688(3) 0.7563(4) 0.068(2) Uani 1 1 d . . . H25A H 1.0196 0.1748 0.7506 0.081 Uiso 1 1 calc R . . C26 C 0.9621(6) 0.1265(3) 0.8065(4) 0.070(2) Uani 1 1 d . . . H26A H 0.9854 0.0944 0.7909 0.084 Uiso 1 1 calc R . . H26B H 0.8995 0.1196 0.8161 0.084 Uiso 1 1 calc R . . C27 C 1.0309(8) 0.1438(4) 0.8664(5) 0.093(3) Uani 1 1 d . . . H27A H 1.0314 0.1178 0.8989 0.112 Uiso 1 1 calc R . . H27B H 1.0953 0.1464 0.8580 0.112 Uiso 1 1 calc R . . C28 C 1.0035(9) 0.1936(5) 0.8885(5) 0.119(4) Uani 1 1 d . . . H28A H 1.0506 0.2040 0.9250 0.142 Uiso 1 1 calc R . . H28B H 0.9425 0.1898 0.9016 0.142 Uiso 1 1 calc R . . C29 C 0.9951(8) 0.2371(4) 0.8383(5) 0.100(4) Uani 1 1 d . . . H29A H 0.9734 0.2693 0.8545 0.120 Uiso 1 1 calc R . . H29B H 1.0570 0.2434 0.8272 0.120 Uiso 1 1 calc R . . C30 C 0.9235(8) 0.2193(4) 0.7807(5) 0.096(3) Uani 1 1 d . . . H30A H 0.8610 0.2151 0.7915 0.115 Uiso 1 1 calc R . . H30B H 0.9184 0.2457 0.7481 0.115 Uiso 1 1 calc R . . C31 C 0.9598(5) 0.0913(3) 0.6581(4) 0.063(2) Uani 1 1 d . . . H31A H 0.9485 0.0615 0.6841 0.075 Uiso 1 1 calc R . . C32 C 0.9253(6) 0.0741(4) 0.5907(4) 0.086(3) Uani 1 1 d . . . H32A H 0.8566 0.0685 0.5832 0.103 Uiso 1 1 calc R . . H32B H 0.9384 0.1014 0.5625 0.103 Uiso 1 1 calc R . . C33 C 0.9742(8) 0.0246(5) 0.5774(5) 0.118(4) Uani 1 1 d . . . H33A H 0.9526 0.0152 0.5336 0.142 Uiso 1 1 calc R . . H33B H 0.9560 -0.0033 0.6029 0.142 Uiso 1 1 calc R . . C34 C 1.0854(7) 0.0297(5) 0.5911(5) 0.118(4) Uani 1 1 d . . . H34A H 1.1141 -0.0041 0.5866 0.141 Uiso 1 1 calc R . . H34B H 1.1050 0.0536 0.5612 0.141 Uiso 1 1 calc R . . C35 C 1.1192(6) 0.0499(4) 0.6570(5) 0.088(3) Uani 1 1 d . . . H35A H 1.1876 0.0563 0.6633 0.106 Uiso 1 1 calc R . . H35B H 1.1088 0.0230 0.6865 0.106 Uiso 1 1 calc R . . C36 C 1.0697(5) 0.0998(4) 0.6717(4) 0.075(3) Uani 1 1 d . . . H36A H 1.0859 0.1282 0.6462 0.090 Uiso 1 1 calc R . . H36B H 1.0913 0.1090 0.7155 0.090 Uiso 1 1 calc R . . C37 C -0.0646(5) 0.4700(3) 0.6276(4) 0.064(2) Uani 1 1 d . . . C38 C -0.1249(6) 0.5123(3) 0.6180(4) 0.063(2) Uani 1 1 d . . . C39 C -0.1678(6) 0.5319(4) 0.5589(6) 0.086(3) Uani 1 1 d . . . C40 C -0.1501(7) 0.5060(5) 0.5069(6) 0.097(3) Uani 1 1 d . . . C41 C -0.0944(7) 0.4646(5) 0.5116(5) 0.096(3) Uani 1 1 d . . . C42 C -0.0518(7) 0.4466(4) 0.5704(5) 0.083(3) Uani 1 1 d . . . C43 C -0.0795(6) 0.4066(4) 0.7256(6) 0.079(3) Uani 1 1 d . . . C44 C -0.0668(10) 0.3996(5) 0.7902(7) 0.109(4) Uani 1 1 d . . . C45 C -0.1272(18) 0.3658(8) 0.8157(12) 0.188(11) Uani 1 1 d . . . C46 C -0.1981(17) 0.3379(8) 0.7792(19) 0.22(2) Uani 1 1 d . . . C47 C -0.2104(10) 0.3431(6) 0.7174(13) 0.163(9) Uani 1 1 d . . . C48 C -0.1527(7) 0.3761(4) 0.6919(8) 0.108(4) Uani 1 1 d . . . C49 C 0.0963(5) 0.4277(3) 0.6951(4) 0.060(2) Uani 1 1 d . . . C50 C 0.1261(5) 0.3753(3) 0.6969(4) 0.065(2) Uani 1 1 d . . . C51 C 0.2178(6) 0.3610(3) 0.6928(4) 0.069(2) Uani 1 1 d . . . C52 C 0.2890(5) 0.3967(3) 0.6865(4) 0.059(2) Uani 1 1 d . . . C53 C 0.2617(5) 0.4481(3) 0.6867(4) 0.055(2) Uani 1 1 d . . . C54 C 0.1679(6) 0.4626(3) 0.6897(4) 0.059(2) Uani 1 1 d . . . C55 C 0.4690(5) 0.3470(3) 0.7541(4) 0.064(2) Uani 1 1 d . . . H55A H 0.5349 0.3407 0.7488 0.077 Uiso 1 1 calc R . . C56 C 0.4771(6) 0.3869(3) 0.8058(4) 0.071(2) Uani 1 1 d . . . H56A H 0.4141 0.3941 0.8145 0.085 Uiso 1 1 calc R . . H56B H 0.5026 0.4192 0.7924 0.085 Uiso 1 1 calc R . . C57 C 0.5431(7) 0.3670(4) 0.8659(4) 0.088(3) Uani 1 1 d . . . H57A H 0.6079 0.3640 0.8585 0.106 Uiso 1 1 calc R . . H57B H 0.5436 0.3922 0.8994 0.106 Uiso 1 1 calc R . . C58 C 0.5116(8) 0.3152(5) 0.8862(5) 0.107(4) Uani 1 1 d . . . H58A H 0.4503 0.3192 0.8989 0.129 Uiso 1 1 calc R . . H58B H 0.5576 0.3030 0.9222 0.129 Uiso 1 1 calc R . . C59 C 0.5021(8) 0.2742(4) 0.8335(5) 0.103(4) Uani 1 1 d . . . H59A H 0.5645 0.2671 0.8237 0.124 Uiso 1 1 calc R . . H59B H 0.4773 0.2418 0.8474 0.124 Uiso 1 1 calc R . . C60 C 0.4341(7) 0.2946(4) 0.7748(5) 0.095(3) Uani 1 1 d . . . H60A H 0.4305 0.2694 0.7410 0.114 Uiso 1 1 calc R . . H60B H 0.3704 0.2988 0.7838 0.114 Uiso 1 1 calc R . . C61 C 0.4788(5) 0.4279(3) 0.6604(4) 0.064(2) Uani 1 1 d . . . H61A H 0.4688 0.4563 0.6886 0.077 Uiso 1 1 calc R . . C62 C 0.5885(5) 0.4179(4) 0.6725(4) 0.080(3) Uani 1 1 d . . . H62A H 0.6101 0.4050 0.7149 0.096 Uiso 1 1 calc R . . H62B H 0.6033 0.3918 0.6434 0.096 Uiso 1 1 calc R . . C63 C 0.6395(6) 0.4694(4) 0.6635(5) 0.085(3) Uani 1 1 d . . . H63A H 0.6292 0.4941 0.6955 0.102 Uiso 1 1 calc R . . H63B H 0.7078 0.4631 0.6691 0.102 Uiso 1 1 calc R . . C64 C 0.6044(7) 0.4931(4) 0.5995(5) 0.101(3) Uani 1 1 d . . . H64A H 0.6210 0.4702 0.5676 0.122 Uiso 1 1 calc R . . H64B H 0.6361 0.5264 0.5969 0.122 Uiso 1 1 calc R . . C65 C 0.4957(7) 0.5015(4) 0.5868(5) 0.090(3) Uani 1 1 d . . . H65A H 0.4745 0.5151 0.5447 0.109 Uiso 1 1 calc R . . H65B H 0.4791 0.5267 0.6164 0.109 Uiso 1 1 calc R . . C66 C 0.4450(6) 0.4483(4) 0.5938(4) 0.079(3) Uani 1 1 d . . . H66A H 0.3762 0.4531 0.5857 0.094 Uiso 1 1 calc R . . H66B H 0.4605 0.4233 0.5637 0.094 Uiso 1 1 calc R . . C67 C 0.3896(6) 0.3218(4) 0.6194(4) 0.077(3) Uani 1 1 d . . . H67A H 0.3625 0.2922 0.6387 0.092 Uiso 1 1 calc R . . C68 C 0.4847(7) 0.3018(4) 0.6049(5) 0.085(3) Uani 1 1 d . . . H68A H 0.5272 0.2915 0.6434 0.103 Uiso 1 1 calc R . . H68B H 0.5156 0.3292 0.5852 0.103 Uiso 1 1 calc R . . C69 C 0.4630(9) 0.2539(5) 0.5599(6) 0.118(4) Uani 1 1 d . . . H69A H 0.5224 0.2420 0.5491 0.141 Uiso 1 1 calc R . . H69B H 0.4380 0.2257 0.5819 0.141 Uiso 1 1 calc R . . C70 C 0.3943(9) 0.2651(5) 0.5018(6) 0.125(4) Uani 1 1 d . . . H70A H 0.3816 0.2335 0.4769 0.150 Uiso 1 1 calc R . . H70B H 0.4210 0.2909 0.4773 0.150 Uiso 1 1 calc R . . C71 C 0.3002(9) 0.2860(5) 0.5177(6) 0.129(5) Uani 1 1 d . . . H71A H 0.2564 0.2950 0.4791 0.155 Uiso 1 1 calc R . . H71B H 0.2706 0.2587 0.5385 0.155 Uiso 1 1 calc R . . C72 C 0.3176(7) 0.3341(4) 0.5602(5) 0.096(3) Uani 1 1 d . . . H72A H 0.3413 0.3626 0.5380 0.115 Uiso 1 1 calc R . . H72B H 0.2577 0.3451 0.5712 0.115 Uiso 1 1 calc R . . C73 C -0.3088(13) 0.3819(7) 0.3935(7) 0.187(7) Uiso 1 1 d D . . H73A H -0.3638 0.3995 0.3687 0.224 Uiso 1 1 calc R . . H73B H -0.2527 0.4026 0.3904 0.224 Uiso 1 1 calc R . . Cl1 Cl -0.2984(4) 0.32800(19) 0.3627(2) 0.1752(17) Uiso 1 1 d . . . Cl2 Cl -0.3223(6) 0.3825(3) 0.4730(4) 0.290(4) Uiso 1 1 d D . . C74 C 0.2203(18) 0.3874(11) 0.9132(11) 0.309(14) Uiso 1 1 d D . . H74A H 0.2856 0.3988 0.9287 0.370 Uiso 1 1 calc R . . H74B H 0.1823 0.4162 0.8927 0.370 Uiso 1 1 calc R . . Cl3 Cl 0.2139(5) 0.3312(3) 0.8651(3) 0.252(3) Uiso 1 1 d . . . Cl4 Cl 0.1688(10) 0.3577(5) 0.9712(7) 0.468(7) Uiso 1 1 d 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 0.0397(12) 0.0791(15) 0.0662(16) -0.0010(11) 0.0126(11) -0.0088(10) P2 0.0439(12) 0.0716(15) 0.0744(17) -0.0020(12) 0.0124(12) 0.0096(10) B1 0.037(5) 0.072(6) 0.059(7) 0.006(5) 0.010(5) -0.007(4) B2 0.039(5) 0.069(6) 0.071(7) -0.003(5) 0.008(5) 0.006(4) F1 0.169(7) 0.140(6) 0.077(5) -0.006(4) 0.010(5) 0.000(5) F2 0.288(11) 0.147(6) 0.166(7) -0.057(5) 0.154(8) -0.046(7) F3 0.128(5) 0.126(5) 0.265(9) -0.035(6) 0.131(6) 0.004(4) F4 0.068(4) 0.104(5) 0.218(8) -0.003(5) 0.002(5) 0.015(3) F5 0.119(5) 0.129(5) 0.092(5) -0.006(4) -0.002(4) 0.035(4) F6 0.057(3) 0.107(4) 0.118(5) 0.008(3) 0.015(3) -0.020(3) F7 0.076(4) 0.116(5) 0.163(6) -0.034(4) -0.009(4) -0.026(4) F8 0.114(5) 0.247(9) 0.115(6) -0.089(6) 0.007(5) -0.043(6) F9 0.114(5) 0.268(10) 0.069(4) 0.005(5) 0.013(4) -0.037(6) F10 0.093(4) 0.141(5) 0.085(4) 0.014(3) 0.015(3) -0.040(4) F11 0.049(3) 0.074(3) 0.096(4) -0.012(3) 0.022(3) -0.013(2) F12 0.044(2) 0.076(3) 0.089(4) -0.008(2) 0.021(2) 0.000(2) F13 0.056(3) 0.071(3) 0.117(4) -0.003(3) 0.019(3) -0.009(2) F14 0.046(3) 0.080(3) 0.129(4) -0.005(3) 0.028(3) 0.003(2) F15 0.056(3) 0.102(4) 0.078(4) 0.014(3) 0.021(3) 0.001(2) F16 0.065(3) 0.094(4) 0.099(4) 0.005(3) 0.020(3) 0.021(3) F17 0.077(4) 0.121(5) 0.144(6) 0.049(4) 0.005(4) 0.025(3) F18 0.091(5) 0.251(9) 0.098(5) 0.055(6) 0.004(4) 0.018(5) F19 0.106(5) 0.256(9) 0.080(5) -0.054(5) 0.006(4) 0.015(5) F20 0.092(4) 0.144(5) 0.109(5) -0.040(4) 0.005(4) 0.032(4) F21 0.189(8) 0.163(7) 0.101(6) 0.026(5) 0.031(6) 0.032(6) F22 0.354(16) 0.195(9) 0.219(10) 0.096(8) 0.201(12) 0.111(10) F23 0.194(9) 0.149(7) 0.458(17) 0.128(9) 0.239(11) 0.048(6) F24 0.062(4) 0.100(5) 0.474(19) 0.055(8) 0.024(7) -0.005(4) F25 0.090(5) 0.098(4) 0.180(7) 0.021(5) -0.020(5) -0.023(3) F26 0.050(3) 0.073(3) 0.155(5) -0.005(3) 0.023(3) -0.001(2) F27 0.060(3) 0.070(3) 0.157(5) 0.003(3) 0.024(3) 0.008(2) F28 0.048(2) 0.074(3) 0.094(4) 0.000(2) 0.022(2) 0.004(2) F29 0.052(3) 0.074(3) 0.084(3) 0.006(2) 0.017(2) 0.013(2) F30 0.056(3) 0.108(4) 0.074(3) -0.004(3) 0.016(3) 0.010(3) C1 0.043(5) 0.082(6) 0.083(7) -0.004(5) 0.023(5) -0.016(4) C2 0.081(7) 0.101(8) 0.094(9) -0.008(7) 0.035(7) -0.018(6) C3 0.133(11) 0.097(9) 0.113(11) -0.034(8) 0.083(9) -0.025(8) C4 0.088(9) 0.074(8) 0.200(18) -0.025(9) 0.082(11) -0.012(6) C5 0.055(6) 0.092(8) 0.144(12) -0.012(8) 0.019(8) -0.008(6) C6 0.052(5) 0.071(6) 0.127(10) -0.006(6) 0.030(7) 0.001(5) C7 0.040(4) 0.070(5) 0.084(7) -0.008(5) 0.008(5) 0.000(4) C8 0.041(5) 0.085(6) 0.076(7) -0.007(5) 0.011(5) -0.008(4) C9 0.039(5) 0.105(8) 0.123(11) -0.028(8) -0.003(7) -0.010(5) C10 0.078(8) 0.136(10) 0.082(9) -0.041(8) 0.009(7) -0.014(7) C11 0.066(7) 0.156(11) 0.078(9) -0.025(8) 0.007(7) -0.008(7) C12 0.063(6) 0.106(7) 0.064(7) -0.002(6) 0.016(6) -0.015(5) C13 0.046(4) 0.061(5) 0.056(5) -0.001(4) 0.016(4) -0.004(4) C14 0.045(4) 0.066(5) 0.057(5) -0.009(4) 0.008(4) -0.004(4) C15 0.041(4) 0.066(5) 0.059(6) 0.000(4) 0.012(4) -0.002(4) C16 0.033(4) 0.074(6) 0.054(5) -0.004(4) 0.004(4) -0.002(4) C17 0.053(5) 0.065(6) 0.071(6) -0.002(4) 0.009(4) -0.012(4) C18 0.048(5) 0.077(6) 0.062(6) 0.000(4) 0.017(4) 0.013(4) C19 0.049(5) 0.103(7) 0.072(7) 0.008(5) 0.008(5) -0.007(5) C20 0.066(6) 0.122(8) 0.085(7) 0.021(6) 0.027(5) -0.025(6) C21 0.091(8) 0.114(9) 0.155(12) 0.052(8) 0.055(9) 0.002(7) C22 0.109(10) 0.198(14) 0.102(10) 0.063(9) 0.013(9) 0.003(9) C23 0.097(9) 0.196(14) 0.106(9) 0.075(9) 0.014(7) -0.003(9) C24 0.081(7) 0.126(9) 0.085(8) 0.015(7) 0.002(7) -0.013(6) C25 0.055(5) 0.071(6) 0.076(6) -0.001(5) 0.009(5) -0.011(4) C26 0.068(6) 0.075(6) 0.069(6) -0.005(5) 0.016(5) -0.004(4) C27 0.104(8) 0.096(8) 0.078(8) -0.014(6) 0.012(7) 0.001(6) C28 0.112(9) 0.143(11) 0.097(9) -0.037(9) 0.012(7) 0.022(8) C29 0.108(8) 0.070(7) 0.109(9) -0.037(6) -0.012(7) 0.011(6) C30 0.099(8) 0.089(7) 0.093(8) -0.016(6) -0.001(7) 0.014(6) C31 0.039(4) 0.085(6) 0.066(6) -0.011(4) 0.014(4) -0.009(4) C32 0.058(5) 0.127(8) 0.079(7) -0.019(6) 0.026(5) -0.012(5) C33 0.099(8) 0.164(11) 0.096(9) -0.066(8) 0.030(7) -0.005(8) C34 0.078(7) 0.170(11) 0.118(10) -0.039(8) 0.052(7) -0.009(7) C35 0.050(5) 0.105(8) 0.115(9) -0.010(6) 0.028(6) -0.009(5) C36 0.047(5) 0.096(7) 0.086(7) -0.007(5) 0.025(5) -0.013(5) C37 0.037(4) 0.079(6) 0.075(7) 0.011(5) 0.007(5) 0.001(4) C38 0.042(5) 0.080(6) 0.067(7) 0.011(5) 0.014(5) 0.007(4) C39 0.049(6) 0.093(7) 0.114(10) 0.030(7) 0.013(7) 0.009(5) C40 0.052(6) 0.154(11) 0.080(9) 0.021(8) 0.001(7) 0.010(7) C41 0.058(6) 0.164(11) 0.065(8) -0.001(8) 0.005(6) 0.010(7) C42 0.060(6) 0.105(8) 0.087(9) -0.002(6) 0.017(6) 0.016(5) C43 0.051(6) 0.084(7) 0.109(9) 0.025(6) 0.030(6) 0.021(5) C44 0.102(9) 0.114(10) 0.122(13) 0.039(9) 0.045(9) 0.038(8) C45 0.24(2) 0.154(17) 0.23(2) 0.119(16) 0.20(2) 0.108(16) C46 0.15(2) 0.109(14) 0.46(6) 0.15(2) 0.21(3) 0.075(13) C47 0.072(9) 0.084(9) 0.35(3) 0.092(15) 0.067(14) 0.030(7) C48 0.045(6) 0.087(8) 0.193(15) 0.053(9) 0.026(9) 0.020(6) C49 0.042(4) 0.070(6) 0.067(6) 0.003(4) 0.008(4) 0.006(4) C50 0.043(5) 0.066(6) 0.087(7) 0.013(4) 0.016(5) 0.005(4) C51 0.053(5) 0.060(5) 0.090(7) 0.003(5) 0.003(5) 0.009(4) C52 0.037(4) 0.063(5) 0.074(6) -0.001(4) 0.005(4) 0.005(4) C53 0.038(4) 0.064(5) 0.062(6) 0.001(4) 0.010(4) 0.003(4) C54 0.057(5) 0.063(5) 0.058(6) 0.005(4) 0.014(4) 0.013(4) C55 0.046(5) 0.067(5) 0.079(6) 0.010(5) 0.010(5) 0.012(4) C56 0.058(5) 0.084(6) 0.073(7) -0.003(5) 0.017(5) 0.003(4) C57 0.081(7) 0.114(8) 0.070(7) 0.020(6) 0.014(6) 0.002(6) C58 0.094(8) 0.128(10) 0.100(9) 0.036(8) 0.018(7) 0.000(7) C59 0.093(8) 0.099(8) 0.104(9) 0.042(7) -0.017(7) -0.014(6) C60 0.084(7) 0.079(7) 0.116(9) 0.001(6) 0.008(7) -0.002(5) C61 0.048(5) 0.074(6) 0.074(6) 0.005(5) 0.018(5) 0.007(4) C62 0.042(5) 0.115(8) 0.086(7) 0.001(6) 0.021(5) 0.015(5) C63 0.053(5) 0.096(7) 0.114(9) 0.009(6) 0.038(6) 0.013(5) C64 0.084(7) 0.122(8) 0.115(9) 0.020(7) 0.062(7) 0.018(6) C65 0.078(7) 0.112(8) 0.084(7) 0.020(6) 0.023(6) 0.010(6) C66 0.057(5) 0.096(7) 0.084(7) 0.007(5) 0.015(5) 0.014(5) C67 0.062(6) 0.087(6) 0.078(7) -0.004(5) 0.005(6) 0.023(5) C68 0.075(6) 0.090(7) 0.097(7) -0.023(6) 0.030(6) 0.015(5) C69 0.109(9) 0.128(10) 0.122(11) -0.030(8) 0.039(9) 0.021(8) C70 0.118(10) 0.149(11) 0.108(10) -0.049(8) 0.022(9) 0.013(9) C71 0.127(11) 0.149(11) 0.101(9) -0.039(8) -0.004(8) 0.013(9) C72 0.083(7) 0.109(8) 0.090(8) -0.010(6) 0.004(7) 0.019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C31 1.809(8) . ? P1 C25 1.815(9) . ? P1 C19 1.822(9) . ? P1 C16 1.824(7) . ? P2 C55 1.821(8) . ? P2 C61 1.823(8) . ? P2 C67 1.823(9) . ? P2 C52 1.828(7) . ? B1 F15 1.405(10) . ? B1 C7 1.627(13) . ? B1 C1 1.644(12) . ? B1 C13 1.667(11) . ? B2 F30 1.427(11) . ? B2 C37 1.610(13) . ? B2 C43 1.649(13) . ? B2 C49 1.663(11) . ? F1 C2 1.360(12) . ? F2 C3 1.357(13) . ? F3 C4 1.353(13) . ? F4 C5 1.332(13) . ? F5 C6 1.330(12) . ? F6 C8 1.357(10) . ? F7 C9 1.360(11) . ? F8 C10 1.355(12) . ? F9 C11 1.353(13) . ? F10 C12 1.346(10) . ? F11 C14 1.352(8) . ? F12 C15 1.341(8) . ? F13 C17 1.342(9) . ? F14 C18 1.351(8) . ? F16 C38 1.333(9) . ? F17 C39 1.334(11) . ? F18 C40 1.364(12) . ? F19 C41 1.354(12) . ? F20 C42 1.347(11) . ? F21 C44 1.336(15) . ? F22 C45 1.40(3) . ? F23 C46 1.319(19) . ? F24 C47 1.35(2) . ? F25 C48 1.346(15) . ? F26 C50 1.341(9) . ? F27 C51 1.359(9) . ? F28 C53 1.343(8) . ? F29 C54 1.341(8) . ? C1 C2 1.381(13) . ? C1 C6 1.408(13) . ? C2 C3 1.412(16) . ? C3 C4 1.342(18) . ? C4 C5 1.328(17) . ? C5 C6 1.379(14) . ? C7 C8 1.366(11) . ? C7 C12 1.408(12) . ? C8 C9 1.389(13) . ? C9 C10 1.369(15) . ? C10 C11 1.302(15) . ? C11 C12 1.365(14) . ? C13 C14 1.378(10) . ? C13 C18 1.386(11) . ? C14 C15 1.400(10) . ? C15 C16 1.362(10) . ? C16 C17 1.395(10) . ? C17 C18 1.378(11) . ? C19 C24 1.521(12) . ? C19 C20 1.562(11) . ? C20 C21 1.559(13) . ? C21 C22 1.437(16) . ? C22 C23 1.544(16) . ? C23 C24 1.524(14) . ? C25 C30 1.491(12) . ? C25 C26 1.524(11) . ? C26 C27 1.535(12) . ? C27 C28 1.440(14) . ? C28 C29 1.547(15) . ? C29 C30 1.523(13) . ? C31 C32 1.515(11) . ? C31 C36 1.551(10) . ? C32 C33 1.500(14) . ? C33 C34 1.558(14) . ? C34 C35 1.509(13) . ? C35 C36 1.520(12) . ? C37 C38 1.373(11) . ? C37 C42 1.422(13) . ? C38 C39 1.404(12) . ? C39 C40 1.373(15) . ? C40 C41 1.315(15) . ? C41 C42 1.380(14) . ? C43 C44 1.391(15) . ? C43 C48 1.392(15) . ? C44 C45 1.40(2) . ? C45 C46 1.36(4) . ? C46 C47 1.32(4) . ? C47 C48 1.368(18) . ? C49 C54 1.377(11) . ? C49 C50 1.403(11) . ? C50 C51 1.376(11) . ? C51 C52 1.391(11) . ? C52 C53 1.371(10) . ? C53 C54 1.400(10) . ? C55 C56 1.504(11) . ? C55 C60 1.527(12) . ? C56 C57 1.540(12) . ? C57 C58 1.490(14) . ? C58 C59 1.538(15) . ? C59 C60 1.537(13) . ? C61 C66 1.524(11) . ? C61 C62 1.553(10) . ? C62 C63 1.536(12) . ? C63 C64 1.509(13) . ? C64 C65 1.534(12) . ? C65 C66 1.561(13) . ? C67 C72 1.514(12) . ? C67 C68 1.535(11) . ? C68 C69 1.560(13) . ? C69 C70 1.467(15) . ? C70 C71 1.541(16) . ? C71 C72 1.531(14) . ? C73 Cl1 1.553(17) . ? C73 Cl2 1.774(13) . ? C74 Cl4 1.748(16) . ? C74 Cl3 1.77(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 C31 P1 C25 107.6(4) . . ? C31 P1 C19 114.0(4) . . ? C25 P1 C19 109.5(4) . . ? C31 P1 C16 108.9(4) . . ? C25 P1 C16 110.4(4) . . ? C19 P1 C16 106.5(4) . . ? C55 P2 C61 106.7(4) . . ? C55 P2 C67 110.5(4) . . ? C61 P2 C67 113.8(4) . . ? C55 P2 C52 109.5(4) . . ? C61 P2 C52 109.1(4) . . ? C67 P2 C52 107.2(4) . . ? F15 B1 C7 108.3(7) . . ? F15 B1 C1 108.5(7) . . ? C7 B1 C1 110.8(7) . . ? F15 B1 C13 106.3(6) . . ? C7 B1 C13 110.2(6) . . ? C1 B1 C13 112.6(7) . . ? F30 B2 C37 107.8(7) . . ? F30 B2 C43 106.3(7) . . ? C37 B2 C43 112.7(7) . . ? F30 B2 C49 105.7(7) . . ? C37 B2 C49 110.9(7) . . ? C43 B2 C49 113.0(7) . . ? C2 C1 C6 112.3(10) . . ? C2 C1 B1 121.9(9) . . ? C6 C1 B1 125.7(8) . . ? F1 C2 C1 119.0(10) . . ? F1 C2 C3 118.3(11) . . ? C1 C2 C3 122.7(12) . . ? C4 C3 F2 123.0(14) . . ? C4 C3 C2 120.4(12) . . ? F2 C3 C2 116.6(15) . . ? C5 C4 C3 120.2(12) . . ? C5 C4 F3 120.5(17) . . ? C3 C4 F3 119.3(17) . . ? C4 C5 F4 120.5(13) . . ? C4 C5 C6 119.4(13) . . ? F4 C5 C6 120.0(13) . . ? F5 C6 C5 115.5(11) . . ? F5 C6 C1 119.4(8) . . ? C5 C6 C1 124.9(12) . . ? C8 C7 C12 111.6(8) . . ? C8 C7 B1 123.0(8) . . ? C12 C7 B1 125.5(8) . . ? F6 C8 C7 120.5(9) . . ? F6 C8 C9 114.5(9) . . ? C7 C8 C9 125.1(9) . . ? F7 C9 C10 121.0(11) . . ? F7 C9 C8 120.5(11) . . ? C10 C9 C8 118.6(10) . . ? C11 C10 F8 122.8(13) . . ? C11 C10 C9 119.4(11) . . ? F8 C10 C9 117.7(12) . . ? C10 C11 F9 120.2(12) . . ? C10 C11 C12 121.5(12) . . ? F9 C11 C12 118.4(11) . . ? F10 C12 C11 118.0(9) . . ? F10 C12 C7 118.2(8) . . ? C11 C12 C7 123.9(10) . . ? C14 C13 C18 113.3(7) . . ? C14 C13 B1 118.7(7) . . ? C18 C13 B1 128.0(7) . . ? F11 C14 C13 120.2(7) . . ? F11 C14 C15 116.2(7) . . ? C13 C14 C15 123.6(7) . . ? F12 C15 C16 122.5(6) . . ? F12 C15 C14 115.1(7) . . ? C16 C15 C14 122.3(7) . . ? C15 C16 C17 114.8(7) . . ? C15 C16 P1 126.4(6) . . ? C17 C16 P1 118.7(6) . . ? F13 C17 C18 116.8(7) . . ? F13 C17 C16 120.9(7) . . ? C18 C17 C16 122.2(7) . . ? F14 C18 C17 115.8(7) . . ? F14 C18 C13 120.5(7) . . ? C17 C18 C13 123.7(7) . . ? C24 C19 C20 111.1(8) . . ? C24 C19 P1 116.2(7) . . ? C20 C19 P1 111.7(6) . . ? C21 C20 C19 108.4(8) . . ? C22 C21 C20 114.3(10) . . ? C21 C22 C23 110.5(10) . . ? C24 C23 C22 111.9(10) . . ? C19 C24 C23 109.9(9) . . ? C30 C25 C26 110.5(8) . . ? C30 C25 P1 119.1(6) . . ? C26 C25 P1 111.1(6) . . ? C25 C26 C27 110.4(7) . . ? C28 C27 C26 111.6(9) . . ? C27 C28 C29 113.0(9) . . ? C30 C29 C28 108.2(9) . . ? C25 C30 C29 110.9(8) . . ? C32 C31 C36 110.6(6) . . ? C32 C31 P1 113.1(6) . . ? C36 C31 P1 115.1(6) . . ? C33 C32 C31 110.8(8) . . ? C32 C33 C34 112.6(9) . . ? C35 C34 C33 109.7(8) . . ? C34 C35 C36 114.2(9) . . ? C35 C36 C31 109.5(7) . . ? C38 C37 C42 112.4(8) . . ? C38 C37 B2 123.8(8) . . ? C42 C37 B2 123.9(8) . . ? F16 C38 C37 120.6(8) . . ? F16 C38 C39 114.6(8) . . ? C37 C38 C39 124.7(9) . . ? F17 C39 C40 121.4(11) . . ? F17 C39 C38 121.1(10) . . ? C40 C39 C38 117.5(10) . . ? C41 C40 F18 121.1(12) . . ? C41 C40 C39 121.9(11) . . ? F18 C40 C39 117.0(11) . . ? C40 C41 F19 121.8(12) . . ? C40 C41 C42 119.4(11) . . ? F19 C41 C42 118.7(11) . . ? F20 C42 C41 117.6(10) . . ? F20 C42 C37 118.3(9) . . ? C41 C42 C37 124.0(10) . . ? C44 C43 C48 113.3(12) . . ? C44 C43 B2 120.4(10) . . ? C48 C43 B2 126.3(10) . . ? F21 C44 C43 118.8(12) . . ? F21 C44 C45 120.7(18) . . ? C43 C44 C45 120.4(18) . . ? C46 C45 F22 124(2) . . ? C46 C45 C44 122(2) . . ? F22 C45 C44 113(3) . . ? F23 C46 C47 124(3) . . ? F23 C46 C45 118(3) . . ? C47 C46 C45 118.4(19) . . ? C46 C47 F24 118.7(19) . . ? C46 C47 C48 120(2) . . ? F24 C47 C48 121(2) . . ? F25 C48 C47 113.7(16) . . ? F25 C48 C43 120.8(10) . . ? C47 C48 C43 125.5(17) . . ? C54 C49 C50 113.5(7) . . ? C54 C49 B2 119.8(7) . . ? C50 C49 B2 126.7(7) . . ? F26 C50 C51 117.1(7) . . ? F26 C50 C49 120.4(7) . . ? C51 C50 C49 122.5(8) . . ? F27 C51 C50 116.3(7) . . ? F27 C51 C52 120.2(7) . . ? C50 C51 C52 123.4(8) . . ? C53 C52 C51 114.6(7) . . ? C53 C52 P2 125.9(6) . . ? C51 C52 P2 119.6(6) . . ? F28 C53 C52 122.7(6) . . ? F28 C53 C54 115.3(7) . . ? C52 C53 C54 122.0(7) . . ? F29 C54 C49 120.1(7) . . ? F29 C54 C53 115.9(7) . . ? C49 C54 C53 123.9(7) . . ? C56 C55 C60 111.0(8) . . ? C56 C55 P2 112.0(6) . . ? C60 C55 P2 117.1(6) . . ? C55 C56 C57 110.7(7) . . ? C58 C57 C56 112.0(8) . . ? C57 C58 C59 112.1(9) . . ? C60 C59 C58 109.6(9) . . ? C55 C60 C59 110.7(8) . . ? C66 C61 C62 109.9(7) . . ? C66 C61 P2 112.7(6) . . ? C62 C61 P2 114.9(6) . . ? C63 C62 C61 108.8(7) . . ? C64 C63 C62 112.4(8) . . ? C63 C64 C65 111.4(7) . . ? C64 C65 C66 109.2(8) . . ? C61 C66 C65 108.9(7) . . ? C72 C67 C68 112.0(8) . . ? C72 C67 P2 115.5(6) . . ? C68 C67 P2 112.2(6) . . ? C67 C68 C69 108.3(8) . . ? C70 C69 C68 113.8(10) . . ? C69 C70 C71 109.8(10) . . ? C72 C71 C70 111.5(10) . . ? C67 C72 C71 110.4(9) . . ? Cl1 C73 Cl2 117.6(11) . . ? Cl4 C74 Cl3 95.2(14) . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 23.41 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 1.833 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.105 #===end data_t-Bu2HP(C6F4)BF(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 636619' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C26 H19 B F15 P' _chemical_formula_weight 658.19 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 8.955(5) _cell_length_b 15.767(9) _cell_length_c 19.743(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.482(12) _cell_angle_gamma 90.00 _cell_volume 2788(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.215 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.520733 _exptl_absorpt_correction_T_max 0.800992 _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_reflns_number 11750 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3951 _reflns_number_gt 2152 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3951 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _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 0.28064(10) -0.03116(7) 0.18154(4) 0.0477(3) Uani 1 1 d . . . B1 B -0.0514(5) 0.2183(3) -0.02195(19) 0.0465(11) Uani 1 1 d . . . C1 C 0.0463(4) 0.1518(2) 0.02599(15) 0.0433(9) Uani 1 1 d . . . C2 C -0.0234(4) 0.0833(2) 0.05692(16) 0.0443(9) Uani 1 1 d . . . C3 C 0.0449(4) 0.0281(2) 0.10095(16) 0.0421(9) Uani 1 1 d . . . C4 C 0.1957(4) 0.0351(2) 0.11700(15) 0.0424(9) Uani 1 1 d . . . C5 C 0.2688(4) 0.1015(2) 0.08571(17) 0.0457(9) Uani 1 1 d . . . C6 C 0.1974(4) 0.1573(2) 0.04149(16) 0.0451(9) Uani 1 1 d . . . C7 C -0.1920(4) 0.2624(2) 0.01889(17) 0.0458(9) Uani 1 1 d . . . C8 C -0.2155(5) 0.2634(3) 0.0889(2) 0.0666(12) Uani 1 1 d . . . C9 C -0.3414(6) 0.3006(3) 0.1174(2) 0.0860(15) Uani 1 1 d . . . C10 C -0.4441(5) 0.3382(3) 0.0782(3) 0.0876(15) Uani 1 1 d . . . C11 C -0.4236(5) 0.3416(3) 0.0100(3) 0.0769(13) Uani 1 1 d . . . C12 C -0.2987(4) 0.3041(3) -0.0172(2) 0.0561(10) Uani 1 1 d . . . C13 C 0.0504(4) 0.2940(2) -0.05481(16) 0.0457(9) Uani 1 1 d . . . C14 C 0.0865(4) 0.3674(3) -0.02006(17) 0.0495(10) Uani 1 1 d . . . C15 C 0.1630(4) 0.4351(3) -0.0465(2) 0.0556(10) Uani 1 1 d . . . C16 C 0.2100(4) 0.4311(3) -0.1119(2) 0.0611(11) Uani 1 1 d . . . C17 C 0.1845(4) 0.3595(3) -0.14869(19) 0.0610(11) Uani 1 1 d . . . C18 C 0.1046(4) 0.2930(3) -0.12088(18) 0.0577(11) Uani 1 1 d . . . C19 C 0.2675(4) 0.0264(3) 0.26249(17) 0.0676(12) Uani 1 1 d . . . C20 C 0.3407(5) 0.1148(3) 0.2569(2) 0.0912(15) Uani 1 1 d . . . H20A H 0.3331 0.1438 0.2995 0.137 Uiso 1 1 calc R . . H20B H 0.2905 0.1472 0.2223 0.137 Uiso 1 1 calc R . . H20C H 0.4440 0.1085 0.2453 0.137 Uiso 1 1 calc R . . C21 C 0.3372(5) -0.0274(3) 0.32098(19) 0.0980(17) Uani 1 1 d . . . H21A H 0.3307 0.0035 0.3628 0.147 Uiso 1 1 calc R . . H21B H 0.4401 -0.0389 0.3112 0.147 Uiso 1 1 calc R . . H21C H 0.2838 -0.0800 0.3250 0.147 Uiso 1 1 calc R . . C22 C 0.0981(4) 0.0388(3) 0.27533(19) 0.0959(17) Uani 1 1 d . . . H22A H 0.0846 0.0691 0.3170 0.144 Uiso 1 1 calc R . . H22B H 0.0503 -0.0155 0.2782 0.144 Uiso 1 1 calc R . . H22C H 0.0547 0.0707 0.2387 0.144 Uiso 1 1 calc R . . C23 C 0.4621(4) -0.0797(3) 0.15844(18) 0.0564(10) Uani 1 1 d . . . C24 C 0.5993(4) -0.0272(3) 0.1801(2) 0.0771(13) Uani 1 1 d . . . H24A H 0.6887 -0.0560 0.1665 0.116 Uiso 1 1 calc R . . H24B H 0.5998 -0.0204 0.2285 0.116 Uiso 1 1 calc R . . H24C H 0.5951 0.0276 0.1589 0.116 Uiso 1 1 calc R . . C25 C 0.4613(4) -0.0916(3) 0.07998(19) 0.0772(13) Uani 1 1 d . . . H25A H 0.5540 -0.1167 0.0662 0.116 Uiso 1 1 calc R . . H25B H 0.4493 -0.0375 0.0584 0.116 Uiso 1 1 calc R . . H25C H 0.3801 -0.1281 0.0671 0.116 Uiso 1 1 calc R . . C26 C 0.4652(5) -0.1680(3) 0.1923(2) 0.0886(14) Uani 1 1 d . . . H26A H 0.5574 -0.1960 0.1819 0.133 Uiso 1 1 calc R . . H26B H 0.3831 -0.2013 0.1756 0.133 Uiso 1 1 calc R . . H26C H 0.4571 -0.1617 0.2405 0.133 Uiso 1 1 calc R . . F1 F -0.1178(2) 0.16752(13) -0.07492(8) 0.0575(6) Uani 1 1 d . . . F2 F -0.1718(2) 0.07079(13) 0.04545(9) 0.0605(6) Uani 1 1 d . . . F3 F -0.0377(2) -0.03248(13) 0.13146(9) 0.0586(6) Uani 1 1 d . . . F4 F 0.4164(2) 0.11378(14) 0.09864(10) 0.0644(6) Uani 1 1 d . . . F5 F 0.2824(2) 0.21912(14) 0.01599(10) 0.0652(6) Uani 1 1 d . . . F6 F -0.1145(3) 0.22964(18) 0.13206(10) 0.1068(10) Uani 1 1 d . . . F7 F -0.3576(4) 0.2980(2) 0.18500(14) 0.1505(14) Uani 1 1 d . . . F8 F -0.5663(3) 0.3746(2) 0.10423(17) 0.1459(14) Uani 1 1 d . . . F9 F -0.5222(3) 0.3824(2) -0.03144(17) 0.1292(11) Uani 1 1 d . . . F10 F -0.2856(3) 0.31176(16) -0.08626(11) 0.0815(7) Uani 1 1 d . . . F11 F 0.0505(2) 0.37320(15) 0.04635(10) 0.0764(7) Uani 1 1 d . . . F12 F 0.1959(3) 0.50363(16) -0.00833(13) 0.0901(8) Uani 1 1 d . . . F13 F 0.2855(3) 0.49636(17) -0.13983(13) 0.0934(8) Uani 1 1 d . . . F14 F 0.2330(3) 0.35372(18) -0.21360(11) 0.0974(9) Uani 1 1 d . . . F15 F 0.0832(3) 0.22419(16) -0.16126(10) 0.0900(8) Uani 1 1 d . . . H1 H 0.191(3) -0.0938(17) 0.1855(11) 0.032(7) 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 0.0386(6) 0.0618(7) 0.0427(5) 0.0094(5) 0.0013(4) -0.0028(5) B1 0.047(3) 0.057(3) 0.035(2) 0.000(2) -0.003(2) 0.005(2) C1 0.038(2) 0.052(3) 0.040(2) -0.0036(18) 0.0050(17) 0.0053(18) C2 0.030(2) 0.055(3) 0.048(2) 0.002(2) 0.0013(18) 0.000(2) C3 0.036(2) 0.045(3) 0.045(2) 0.0011(19) 0.0062(18) -0.0044(19) C4 0.039(2) 0.048(2) 0.0403(19) -0.0031(18) 0.0029(17) -0.0011(19) C5 0.027(2) 0.063(3) 0.047(2) -0.003(2) -0.0014(18) -0.0009(19) C6 0.042(2) 0.047(3) 0.046(2) 0.0082(19) 0.0063(19) -0.007(2) C7 0.044(2) 0.051(3) 0.043(2) 0.0058(18) 0.0001(18) 0.0001(19) C8 0.075(3) 0.070(3) 0.055(3) 0.008(2) 0.003(3) 0.014(2) C9 0.101(4) 0.090(4) 0.068(3) -0.005(3) 0.037(3) 0.012(3) C10 0.066(3) 0.089(4) 0.109(4) -0.019(3) 0.036(3) 0.010(3) C11 0.040(3) 0.067(3) 0.124(4) -0.007(3) -0.011(3) 0.009(2) C12 0.049(3) 0.055(3) 0.065(3) 0.008(2) 0.000(2) -0.002(2) C13 0.039(2) 0.054(3) 0.044(2) 0.0061(19) -0.0017(18) 0.0106(18) C14 0.045(2) 0.060(3) 0.043(2) -0.006(2) -0.0032(19) 0.004(2) C15 0.050(2) 0.051(3) 0.065(3) -0.007(2) -0.001(2) -0.002(2) C16 0.051(3) 0.050(3) 0.082(3) 0.016(3) 0.003(2) -0.006(2) C17 0.058(3) 0.080(4) 0.046(2) 0.018(2) 0.012(2) 0.007(2) C18 0.066(3) 0.062(3) 0.046(2) -0.006(2) 0.007(2) 0.004(2) C19 0.054(3) 0.103(4) 0.045(2) 0.000(2) -0.001(2) -0.006(3) C20 0.091(4) 0.118(5) 0.064(3) -0.024(3) -0.004(2) 0.003(3) C21 0.085(3) 0.159(5) 0.050(2) 0.022(3) -0.005(2) -0.006(3) C22 0.066(3) 0.164(5) 0.059(3) -0.021(3) 0.016(2) 0.008(3) C23 0.043(2) 0.067(3) 0.059(2) 0.006(2) -0.0073(19) 0.003(2) C24 0.038(2) 0.105(4) 0.088(3) 0.005(3) -0.005(2) -0.002(2) C25 0.058(3) 0.095(4) 0.079(3) -0.019(3) 0.006(2) 0.012(2) C26 0.071(3) 0.080(4) 0.114(3) 0.025(3) -0.006(3) 0.013(3) F1 0.0631(14) 0.0619(15) 0.0475(11) -0.0073(10) -0.0053(10) -0.0048(11) F2 0.0383(12) 0.0701(16) 0.0729(13) 0.0156(11) -0.0054(10) -0.0067(11) F3 0.0428(12) 0.0635(15) 0.0696(13) 0.0156(11) 0.0041(10) -0.0062(11) F4 0.0386(13) 0.0773(17) 0.0772(14) 0.0187(12) -0.0024(11) -0.0076(11) F5 0.0466(12) 0.0675(16) 0.0816(14) 0.0256(12) 0.0014(11) -0.0075(11) F6 0.148(2) 0.131(3) 0.0415(13) -0.0003(14) -0.0027(15) 0.059(2) F7 0.207(3) 0.158(3) 0.0870(19) -0.0048(19) 0.076(2) 0.048(3) F8 0.079(2) 0.156(3) 0.204(3) -0.046(3) 0.058(2) 0.0310(19) F9 0.0716(19) 0.138(3) 0.178(3) -0.005(2) -0.0289(19) 0.0459(19) F10 0.0865(17) 0.0926(19) 0.0652(15) 0.0148(13) -0.0209(13) 0.0194(14) F11 0.0843(17) 0.093(2) 0.0518(13) -0.0185(12) 0.0066(12) -0.0221(14) F12 0.0855(18) 0.0710(18) 0.1140(19) -0.0190(15) 0.0079(15) -0.0207(14) F13 0.0821(17) 0.0810(19) 0.1174(19) 0.0290(15) 0.0181(15) -0.0169(14) F14 0.111(2) 0.117(2) 0.0642(15) 0.0103(14) 0.0282(14) -0.0173(16) F15 0.131(2) 0.0793(19) 0.0601(13) -0.0183(13) 0.0327(14) -0.0170(16) _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 C4 1.810(4) . ? P1 C19 1.842(4) . ? P1 C23 1.856(4) . ? B1 F1 1.441(4) . ? B1 C13 1.639(5) . ? B1 C7 1.655(5) . ? B1 C1 1.657(5) . ? C1 C6 1.387(4) . ? C1 C2 1.391(5) . ? C2 F2 1.361(4) . ? C2 C3 1.371(4) . ? C3 F3 1.353(4) . ? C3 C4 1.389(4) . ? C4 C5 1.383(5) . ? C5 F4 1.358(4) . ? C5 C6 1.392(5) . ? C6 F5 1.338(4) . ? C7 C12 1.356(5) . ? C7 C8 1.400(5) . ? C8 F6 1.347(4) . ? C8 C9 1.393(6) . ? C9 C10 1.336(6) . ? C9 F7 1.344(5) . ? C10 F8 1.342(5) . ? C10 C11 1.363(6) . ? C11 F9 1.360(5) . ? C11 C12 1.377(5) . ? C12 F10 1.375(4) . ? C13 C14 1.382(5) . ? C13 C18 1.396(5) . ? C14 F11 1.356(4) . ? C14 C15 1.374(5) . ? C15 F12 1.349(4) . ? C15 C16 1.362(5) . ? C16 F13 1.351(4) . ? C16 C17 1.362(5) . ? C17 F14 1.360(4) . ? C17 C18 1.385(5) . ? C18 F15 1.359(4) . ? C19 C20 1.546(6) . ? C19 C22 1.552(5) . ? C19 C21 1.559(5) . ? C23 C24 1.539(5) . ? C23 C26 1.546(6) . ? C23 C25 1.560(5) . ? 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 C4 P1 C19 107.28(18) . . ? C4 P1 C23 115.36(16) . . ? C19 P1 C23 118.59(17) . . ? F1 B1 C13 110.2(3) . . ? F1 B1 C7 106.0(3) . . ? C13 B1 C7 108.3(3) . . ? F1 B1 C1 106.0(3) . . ? C13 B1 C1 113.2(3) . . ? C7 B1 C1 112.8(3) . . ? C6 C1 C2 113.1(3) . . ? C6 C1 B1 126.6(3) . . ? C2 C1 B1 120.3(3) . . ? F2 C2 C3 116.3(3) . . ? F2 C2 C1 118.8(3) . . ? C3 C2 C1 124.9(3) . . ? F3 C3 C2 119.2(3) . . ? F3 C3 C4 119.2(3) . . ? C2 C3 C4 121.5(3) . . ? C5 C4 C3 114.9(3) . . ? C5 C4 P1 123.6(3) . . ? C3 C4 P1 121.1(3) . . ? F4 C5 C4 119.2(3) . . ? F4 C5 C6 118.0(3) . . ? C4 C5 C6 122.8(3) . . ? F5 C6 C1 121.3(3) . . ? F5 C6 C5 115.9(3) . . ? C1 C6 C5 122.8(3) . . ? C12 C7 C8 113.7(3) . . ? C12 C7 B1 118.9(3) . . ? C8 C7 B1 127.4(3) . . ? F6 C8 C9 116.8(4) . . ? F6 C8 C7 121.0(4) . . ? C9 C8 C7 122.2(4) . . ? C10 C9 F7 120.5(5) . . ? C10 C9 C8 120.6(4) . . ? F7 C9 C8 118.9(5) . . ? C9 C10 F8 121.9(5) . . ? C9 C10 C11 119.4(4) . . ? F8 C10 C11 118.6(5) . . ? F9 C11 C10 121.4(5) . . ? F9 C11 C12 119.6(5) . . ? C10 C11 C12 119.0(4) . . ? C7 C12 F10 119.8(3) . . ? C7 C12 C11 125.0(4) . . ? F10 C12 C11 115.1(4) . . ? C14 C13 C18 113.1(3) . . ? C14 C13 B1 122.8(3) . . ? C18 C13 B1 124.1(4) . . ? F11 C14 C15 116.0(3) . . ? F11 C14 C13 118.7(3) . . ? C15 C14 C13 125.2(3) . . ? F12 C15 C16 119.9(4) . . ? F12 C15 C14 121.2(4) . . ? C16 C15 C14 118.9(4) . . ? F13 C16 C15 120.8(4) . . ? F13 C16 C17 119.7(4) . . ? C15 C16 C17 119.5(4) . . ? F14 C17 C16 120.3(4) . . ? F14 C17 C18 119.6(4) . . ? C16 C17 C18 120.1(4) . . ? F15 C18 C17 116.2(3) . . ? F15 C18 C13 120.6(4) . . ? C17 C18 C13 123.2(4) . . ? C20 C19 C22 108.3(4) . . ? C20 C19 C21 112.1(3) . . ? C22 C19 C21 109.5(3) . . ? C20 C19 P1 110.6(3) . . ? C22 C19 P1 105.9(3) . . ? C21 C19 P1 110.3(3) . . ? C24 C23 C26 110.6(3) . . ? C24 C23 C25 109.8(3) . . ? C26 C23 C25 108.7(3) . . ? C24 C23 P1 114.1(3) . . ? C26 C23 P1 106.1(3) . . ? C25 C23 P1 107.3(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.184 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.043 #===end data_iPr3PC6F4BH(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 636620' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C27 H22 B F14 P' _chemical_formula_weight 654.23 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 P21/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 9.3212(7) _cell_length_b 16.4421(13) _cell_length_c 17.8541(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.0440(10) _cell_angle_gamma 90.00 _cell_volume 2735.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.449990 _exptl_absorpt_correction_T_max 1.000000 _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 25837 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4817 _reflns_number_gt 3588 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+0.8248P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4817 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.14494(7) 0.03911(4) 0.17946(4) 0.0528(2) Uani 1 1 d . . . F1 F 0.6015(2) -0.18563(13) 0.14284(11) 0.0941(6) Uani 1 1 d . . . F2 F 0.8540(2) -0.23914(15) 0.19284(13) 0.1124(7) Uani 1 1 d . . . F3 F 1.0249(2) -0.33018(14) 0.10390(15) 0.1130(8) Uani 1 1 d . . . F4 F 0.9321(2) -0.36967(13) -0.03653(14) 0.1056(7) Uani 1 1 d . . . F5 F 0.67711(19) -0.31920(11) -0.08731(11) 0.0848(5) Uani 1 1 d . . . F6 F 0.4552(2) -0.38450(10) 0.06573(10) 0.0805(5) Uani 1 1 d . . . F7 F 0.3101(2) -0.51332(10) 0.01924(12) 0.0934(6) Uani 1 1 d . . . F8 F 0.1445(2) -0.50700(12) -0.10753(12) 0.0937(6) Uani 1 1 d . . . F9 F 0.1352(2) -0.36844(13) -0.18942(11) 0.0981(6) Uani 1 1 d . . . F10 F 0.2804(2) -0.23639(11) -0.14385(10) 0.0825(5) Uani 1 1 d . . . F11 F 0.3141(2) -0.25035(9) 0.12703(9) 0.0772(5) Uani 1 1 d . . . F12 F 0.1700(2) -0.14310(10) 0.20270(9) 0.0800(5) Uani 1 1 d . . . F13 F 0.27899(17) 0.05558(9) 0.01955(8) 0.0638(4) Uani 1 1 d . . . F14 F 0.41319(16) -0.05161(9) -0.05585(8) 0.0629(4) Uani 1 1 d . . . C1 C 0.6247(3) -0.24988(15) 0.02448(16) 0.0598(7) Uani 1 1 d . . . C2 C 0.6786(3) -0.23181(18) 0.09548(17) 0.0679(7) Uani 1 1 d . . . C3 C 0.8102(4) -0.2582(2) 0.12280(19) 0.0777(9) Uani 1 1 d . . . C4 C 0.8960(3) -0.3046(2) 0.0781(2) 0.0795(9) Uani 1 1 d . . . C5 C 0.8495(3) -0.32413(18) 0.0077(2) 0.0752(8) Uani 1 1 d . . . C6 C 0.7170(3) -0.29710(17) -0.01705(18) 0.0662(7) Uani 1 1 d . . . C7 C 0.3760(3) -0.30323(15) -0.03674(14) 0.0556(6) Uani 1 1 d . . . C8 C 0.3765(3) -0.37622(16) 0.00186(15) 0.0595(7) Uani 1 1 d . . . C9 C 0.3025(3) -0.44414(17) -0.02080(17) 0.0662(7) Uani 1 1 d . . . C10 C 0.2203(3) -0.44148(18) -0.08535(18) 0.0677(8) Uani 1 1 d . . . C11 C 0.2147(3) -0.37128(19) -0.12590(16) 0.0679(8) Uani 1 1 d . . . C12 C 0.2909(3) -0.30434(17) -0.10123(15) 0.0609(7) Uani 1 1 d . . . C13 C 0.3770(3) -0.15745(15) 0.03250(14) 0.0523(6) Uani 1 1 d . . . C14 C 0.3064(3) -0.17419(15) 0.09828(15) 0.0583(6) Uani 1 1 d . . . C15 C 0.2321(3) -0.11808(16) 0.13903(14) 0.0579(6) Uani 1 1 d . . . C16 C 0.2195(3) -0.03690(15) 0.11684(13) 0.0513(6) Uani 1 1 d . . . C17 C 0.2846(3) -0.01980(14) 0.04891(13) 0.0501(6) Uani 1 1 d . . . C18 C 0.3571(3) -0.07780(15) 0.00945(13) 0.0505(6) Uani 1 1 d . . . C19 C 0.1186(3) 0.13531(16) 0.12945(15) 0.0614(7) Uani 1 1 d . . . H19A H 0.2084 0.1465 0.1037 0.074 Uiso 1 1 calc R . . C20 C 0.0938(4) 0.20741(19) 0.18245(19) 0.0860(10) Uani 1 1 d . . . H20A H 0.0813 0.2563 0.1536 0.129 Uiso 1 1 calc R . . H20B H 0.1752 0.2134 0.2157 0.129 Uiso 1 1 calc R . . H20C H 0.0094 0.1976 0.2111 0.129 Uiso 1 1 calc R . . C21 C 0.0012(4) 0.13044(19) 0.06862(18) 0.0757(8) Uani 1 1 d . . . H21A H -0.0075 0.1821 0.0439 0.113 Uiso 1 1 calc R . . H21B H -0.0884 0.1166 0.0910 0.113 Uiso 1 1 calc R . . H21C H 0.0259 0.0895 0.0327 0.113 Uiso 1 1 calc R . . C22 C -0.0216(3) -0.00107(18) 0.21785(16) 0.0664(7) Uani 1 1 d . . . H22A H 0.0062 -0.0452 0.2521 0.080 Uiso 1 1 calc R . . C23 C -0.1215(4) -0.0386(2) 0.1588(2) 0.0885(10) Uani 1 1 d . . . H23A H -0.2063 -0.0586 0.1824 0.133 Uiso 1 1 calc R . . H23B H -0.0734 -0.0827 0.1346 0.133 Uiso 1 1 calc R . . H23C H -0.1478 0.0019 0.1224 0.133 Uiso 1 1 calc R . . C24 C -0.1005(4) 0.0623(3) 0.2651(2) 0.0982(11) Uani 1 1 d . . . H24A H -0.1866 0.0388 0.2842 0.147 Uiso 1 1 calc R . . H24B H -0.1245 0.1085 0.2345 0.147 Uiso 1 1 calc R . . H24C H -0.0395 0.0793 0.3061 0.147 Uiso 1 1 calc R . . C25 C 0.2777(3) 0.05683(19) 0.25435(15) 0.0673(7) Uani 1 1 d . . . H25A H 0.2412 0.1016 0.2849 0.081 Uiso 1 1 calc R . . C26 C 0.4188(4) 0.0859(3) 0.2211(2) 0.1068(14) Uani 1 1 d . . . H26A H 0.4876 0.0956 0.2608 0.160 Uiso 1 1 calc R . . H26B H 0.4025 0.1354 0.1938 0.160 Uiso 1 1 calc R . . H26C H 0.4549 0.0451 0.1880 0.160 Uiso 1 1 calc R . . C27 C 0.3004(4) -0.0148(3) 0.3063(2) 0.0986(12) Uani 1 1 d . . . H27A H 0.3706 -0.0009 0.3442 0.148 Uiso 1 1 calc R . . H27B H 0.3337 -0.0606 0.2782 0.148 Uiso 1 1 calc R . . H27C H 0.2115 -0.0283 0.3295 0.148 Uiso 1 1 calc R . . B1 B 0.4717(3) -0.22248(18) -0.01521(17) 0.0563(7) Uani 1 1 d . . . H1 H 0.515(3) -0.191(2) -0.0784(19) 0.096 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 0.0543(4) 0.0566(4) 0.0474(4) -0.0004(3) 0.0005(3) 0.0002(3) F1 0.0889(13) 0.1117(15) 0.0812(12) -0.0310(11) -0.0136(10) 0.0184(11) F2 0.1064(15) 0.1294(18) 0.0999(15) -0.0011(13) -0.0365(13) 0.0077(13) F3 0.0671(12) 0.1144(16) 0.157(2) 0.0282(15) -0.0177(12) 0.0110(11) F4 0.0742(12) 0.0998(15) 0.1439(19) -0.0053(13) 0.0314(12) 0.0198(11) F5 0.0793(11) 0.0899(13) 0.0856(12) -0.0210(10) 0.0128(9) 0.0058(9) F6 0.0997(13) 0.0669(10) 0.0743(11) 0.0122(8) -0.0169(9) -0.0106(9) F7 0.1153(15) 0.0569(10) 0.1080(15) 0.0097(10) 0.0035(12) -0.0166(10) F8 0.0854(12) 0.0799(12) 0.1157(15) -0.0295(11) 0.0002(11) -0.0231(10) F9 0.0960(14) 0.1104(15) 0.0868(13) -0.0186(11) -0.0306(11) -0.0011(11) F10 0.0954(13) 0.0762(11) 0.0753(11) 0.0062(9) -0.0152(9) 0.0073(9) F11 0.1027(13) 0.0521(9) 0.0774(11) 0.0134(8) 0.0175(9) 0.0045(8) F12 0.1033(13) 0.0693(10) 0.0684(10) 0.0163(8) 0.0287(9) 0.0052(9) F13 0.0803(10) 0.0514(8) 0.0600(9) 0.0091(7) 0.0110(7) 0.0051(7) F14 0.0729(10) 0.0609(9) 0.0554(8) 0.0062(7) 0.0134(7) 0.0021(7) C1 0.0596(16) 0.0467(14) 0.0733(18) -0.0005(12) 0.0049(13) -0.0064(12) C2 0.0687(18) 0.0606(17) 0.0743(19) -0.0031(14) 0.0007(15) 0.0004(14) C3 0.075(2) 0.071(2) 0.086(2) 0.0099(17) -0.0157(18) -0.0082(16) C4 0.0563(18) 0.0670(19) 0.115(3) 0.0171(19) -0.0038(18) -0.0002(14) C5 0.0592(18) 0.0622(18) 0.105(3) 0.0048(17) 0.0151(17) 0.0009(14) C6 0.0635(17) 0.0565(16) 0.0788(19) -0.0048(14) 0.0107(14) -0.0077(13) C7 0.0569(15) 0.0520(14) 0.0580(15) -0.0072(12) 0.0036(12) 0.0019(11) C8 0.0646(16) 0.0551(15) 0.0587(16) -0.0027(12) 0.0012(13) -0.0013(12) C9 0.0683(18) 0.0529(16) 0.0778(19) -0.0017(14) 0.0102(15) -0.0021(13) C10 0.0600(16) 0.0636(18) 0.080(2) -0.0190(15) 0.0069(14) -0.0075(13) C11 0.0594(17) 0.079(2) 0.0645(17) -0.0166(15) -0.0053(14) 0.0044(14) C12 0.0636(16) 0.0571(16) 0.0622(16) -0.0039(13) 0.0007(13) 0.0067(13) C13 0.0519(14) 0.0519(14) 0.0529(14) -0.0005(11) -0.0023(11) -0.0059(11) C14 0.0681(16) 0.0444(14) 0.0625(16) 0.0058(12) 0.0003(13) -0.0014(12) C15 0.0629(16) 0.0578(15) 0.0531(15) 0.0066(12) 0.0053(12) -0.0025(12) C16 0.0520(14) 0.0514(14) 0.0504(13) 0.0026(11) -0.0021(11) -0.0013(11) C17 0.0526(14) 0.0462(13) 0.0514(14) 0.0052(11) -0.0044(11) -0.0029(10) C18 0.0499(13) 0.0539(14) 0.0477(13) 0.0011(11) 0.0014(10) -0.0040(11) C19 0.0720(18) 0.0543(15) 0.0579(15) -0.0016(12) 0.0031(13) 0.0017(13) C20 0.113(3) 0.0621(19) 0.084(2) -0.0092(16) 0.0117(19) 0.0086(17) C21 0.084(2) 0.0705(19) 0.0725(19) 0.0102(15) -0.0127(16) 0.0062(15) C22 0.0577(16) 0.0768(19) 0.0649(17) 0.0070(14) 0.0108(13) -0.0008(14) C23 0.0674(19) 0.093(2) 0.105(3) 0.000(2) -0.0006(18) -0.0184(17) C24 0.085(2) 0.112(3) 0.098(3) -0.004(2) 0.035(2) 0.004(2) C25 0.0637(17) 0.087(2) 0.0506(14) -0.0050(14) -0.0054(12) -0.0012(14) C26 0.076(2) 0.168(4) 0.075(2) -0.003(2) -0.0113(18) -0.042(2) C27 0.091(2) 0.129(3) 0.075(2) 0.020(2) -0.0264(19) 0.002(2) B1 0.0631(18) 0.0482(16) 0.0576(17) -0.0006(13) 0.0035(14) -0.0019(13) _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 1.823(3) . ? P1 C25 1.828(3) . ? P1 C19 1.831(3) . ? P1 C22 1.832(3) . ? F1 C2 1.353(3) . ? F2 C3 1.346(4) . ? F3 C4 1.346(4) . ? F4 C5 1.342(4) . ? F5 C6 1.352(3) . ? F6 C8 1.352(3) . ? F7 C9 1.345(3) . ? F8 C10 1.344(3) . ? F9 C11 1.344(3) . ? F10 C12 1.354(3) . ? F11 C14 1.355(3) . ? F12 C15 1.349(3) . ? F13 C17 1.346(3) . ? F14 C18 1.356(3) . ? C1 C6 1.385(4) . ? C1 C2 1.388(4) . ? C1 B1 1.643(4) . ? C2 C3 1.382(4) . ? C3 C4 1.372(5) . ? C4 C5 1.360(5) . ? C5 C6 1.377(4) . ? C7 C8 1.384(4) . ? C7 C12 1.386(4) . ? C7 B1 1.642(4) . ? C8 C9 1.370(4) . ? C9 C10 1.373(4) . ? C10 C11 1.363(4) . ? C11 C12 1.378(4) . ? C13 C14 1.384(4) . ? C13 C18 1.384(3) . ? C13 B1 1.636(4) . ? C14 C15 1.371(4) . ? C15 C16 1.397(4) . ? C16 C17 1.395(3) . ? C17 C18 1.371(3) . ? C19 C21 1.530(4) . ? C19 C20 1.537(4) . ? C22 C23 1.524(4) . ? C22 C24 1.536(4) . ? C25 C27 1.511(5) . ? C25 C26 1.530(5) . ? 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 C25 107.30(13) . . ? C16 P1 C19 110.03(12) . . ? C25 P1 C19 107.57(13) . . ? C16 P1 C22 108.50(13) . . ? C25 P1 C22 110.53(13) . . ? C19 P1 C22 112.77(14) . . ? C6 C1 C2 113.0(3) . . ? C6 C1 B1 117.8(2) . . ? C2 C1 B1 129.2(3) . . ? F1 C2 C3 115.8(3) . . ? F1 C2 C1 120.2(3) . . ? C3 C2 C1 124.1(3) . . ? F2 C3 C4 120.0(3) . . ? F2 C3 C2 120.5(3) . . ? C4 C3 C2 119.5(3) . . ? F3 C4 C5 120.7(3) . . ? F3 C4 C3 120.0(3) . . ? C5 C4 C3 119.3(3) . . ? F4 C5 C4 119.9(3) . . ? F4 C5 C6 120.8(3) . . ? C4 C5 C6 119.3(3) . . ? F5 C6 C5 116.2(3) . . ? F5 C6 C1 119.0(3) . . ? C5 C6 C1 124.8(3) . . ? C8 C7 C12 113.5(2) . . ? C8 C7 B1 126.0(2) . . ? C12 C7 B1 120.4(2) . . ? F6 C8 C9 115.5(2) . . ? F6 C8 C7 120.3(2) . . ? C9 C8 C7 124.2(3) . . ? F7 C9 C8 120.7(3) . . ? F7 C9 C10 119.8(3) . . ? C8 C9 C10 119.5(3) . . ? F8 C10 C11 120.5(3) . . ? F8 C10 C9 120.3(3) . . ? C11 C10 C9 119.2(3) . . ? F9 C11 C10 119.5(3) . . ? F9 C11 C12 121.0(3) . . ? C10 C11 C12 119.5(3) . . ? F10 C12 C11 116.6(2) . . ? F10 C12 C7 119.4(2) . . ? C11 C12 C7 124.0(3) . . ? C14 C13 C18 112.2(2) . . ? C14 C13 B1 125.5(2) . . ? C18 C13 B1 122.3(2) . . ? F11 C14 C15 116.4(2) . . ? F11 C14 C13 118.9(2) . . ? C15 C14 C13 124.7(2) . . ? F12 C15 C14 118.1(2) . . ? F12 C15 C16 119.7(2) . . ? C14 C15 C16 122.2(2) . . ? C17 C16 C15 113.8(2) . . ? C17 C16 P1 124.88(19) . . ? C15 C16 P1 120.82(19) . . ? F13 C17 C18 117.1(2) . . ? F13 C17 C16 120.7(2) . . ? C18 C17 C16 122.2(2) . . ? F14 C18 C17 115.0(2) . . ? F14 C18 C13 120.3(2) . . ? C17 C18 C13 124.7(2) . . ? C21 C19 C20 111.3(2) . . ? C21 C19 P1 112.89(19) . . ? C20 C19 P1 112.7(2) . . ? C23 C22 C24 111.2(3) . . ? C23 C22 P1 113.5(2) . . ? C24 C22 P1 112.2(2) . . ? C27 C25 C26 111.7(3) . . ? C27 C25 P1 114.2(2) . . ? C26 C25 P1 110.0(2) . . ? C13 B1 C7 110.7(2) . . ? C13 B1 C1 115.3(2) . . ? C7 B1 C1 110.1(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.755 _refine_diff_density_min -0.174 _refine_diff_density_rms 0.045 #===end data_t-Bu2PHC6F4BH(C6F5)2 _database_code_depnum_ccdc_archive 'CCDC 636621' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C26 H20 B F14 P' _chemical_formula_weight 640.20 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 9.6218(12) _cell_length_b 17.225(2) _cell_length_c 18.468(2) _cell_angle_alpha 67.652(2) _cell_angle_beta 76.712(3) _cell_angle_gamma 88.612(2) _cell_volume 2748.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.211 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_number 13680 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0419 _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 -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 23.33 _reflns_number_total 7884 _reflns_number_gt 5320 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1026P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7884 _refine_ls_number_parameters 785 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1537 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.19061(9) 0.42814(6) 0.23242(6) 0.0458(3) Uani 1 1 d . . . P2 P -0.90300(10) -0.07490(6) 0.23558(6) 0.0510(3) Uani 1 1 d . . . H1A H -0.982(3) -0.012(2) 0.220(2) 0.062(10) Uiso 1 1 d . . . F1 F -0.1090(2) 0.34295(13) 0.28217(17) 0.0778(7) Uani 1 1 d . . . F2 F -0.3541(2) 0.41183(13) 0.28716(16) 0.0751(7) Uani 1 1 d . . . F3 F -0.1115(2) 0.68079(12) 0.17355(15) 0.0696(6) Uani 1 1 d . . . F4 F 0.1341(2) 0.61111(12) 0.17192(14) 0.0669(6) Uani 1 1 d . . . F5 F -0.2535(3) 0.6167(2) 0.35120(17) 0.1005(9) Uani 1 1 d . . . F6 F -0.3784(5) 0.6266(3) 0.4899(2) 0.1562(15) Uani 1 1 d . . . F7 F -0.6669(5) 0.6124(3) 0.5421(2) 0.1661(17) Uani 1 1 d . . . F8 F -0.8314(3) 0.5880(2) 0.4478(2) 0.1353(13) Uani 1 1 d . . . F9 F -0.7073(2) 0.58196(18) 0.30646(18) 0.0939(8) Uani 1 1 d . . . F10 F -0.4727(3) 0.60301(17) 0.08475(17) 0.1021(9) Uani 1 1 d . . . F11 F -0.5120(4) 0.7427(2) -0.03317(18) 0.1273(12) Uani 1 1 d . . . F12 F -0.4672(3) 0.89541(17) -0.02840(16) 0.1038(9) Uani 1 1 d . . . F13 F -0.3854(3) 0.90523(14) 0.09869(15) 0.0851(7) Uani 1 1 d . . . F14 F -0.3512(2) 0.76618(13) 0.21978(13) 0.0645(6) Uani 1 1 d . . . F15 F -0.8285(2) 0.10607(13) 0.20265(17) 0.0799(7) Uani 1 1 d . . . F16 F -0.5948(2) 0.17168(13) 0.21587(16) 0.0753(7) Uani 1 1 d . . . F17 F -0.3946(2) -0.09092(13) 0.27409(16) 0.0754(7) Uani 1 1 d . . . F18 F -0.6232(2) -0.15492(13) 0.25791(17) 0.0757(7) Uani 1 1 d . . . F19 F -0.6312(3) 0.0710(2) 0.38652(17) 0.0991(9) Uani 1 1 d . . . F20 F -0.6595(4) 0.1086(2) 0.51315(19) 0.1240(11) Uani 1 1 d . . . F21 F -0.4322(5) 0.1569(3) 0.5516(2) 0.1633(17) Uani 1 1 d . . . F22 F -0.1684(4) 0.1684(3) 0.4552(2) 0.181(2) Uani 1 1 d . . . F23 F -0.1331(3) 0.1331(2) 0.32440(17) 0.1163(11) Uani 1 1 d . . . F24 F -0.1543(4) 0.07601(17) 0.12101(19) 0.1218(12) Uani 1 1 d . . . F25 F 0.0038(4) 0.2032(2) -0.00189(19) 0.1465(15) Uani 1 1 d . . . F26 F -0.0230(3) 0.36325(18) -0.00937(15) 0.0999(9) Uani 1 1 d . . . F27 F -0.2088(3) 0.39234(14) 0.11059(15) 0.0849(7) Uani 1 1 d . . . F28 F -0.3618(2) 0.26678(13) 0.23517(14) 0.0671(6) Uani 1 1 d . . . C1 C 0.2595(4) 0.4036(2) 0.1425(2) 0.0542(9) Uani 1 1 d . . . C2 C 0.2514(5) 0.4839(3) 0.0699(3) 0.0837(13) Uani 1 1 d . . . H2C H 0.2902 0.4752 0.0210 0.126 Uiso 1 1 calc R . . H2D H 0.3056 0.5296 0.0706 0.126 Uiso 1 1 calc R . . H2E H 0.1533 0.4972 0.0726 0.126 Uiso 1 1 calc R . . C3 C 0.1713(5) 0.3309(3) 0.1423(3) 0.0840(14) Uani 1 1 d . . . H3A H 0.2072 0.3229 0.0929 0.126 Uiso 1 1 calc R . . H3B H 0.0729 0.3440 0.1469 0.126 Uiso 1 1 calc R . . H3C H 0.1785 0.2804 0.1870 0.126 Uiso 1 1 calc R . . C4 C 0.4153(4) 0.3833(3) 0.1395(3) 0.0702(11) Uani 1 1 d . . . H4A H 0.4578 0.3786 0.0891 0.105 Uiso 1 1 calc R . . H4B H 0.4196 0.3311 0.1831 0.105 Uiso 1 1 calc R . . H4C H 0.4665 0.4275 0.1444 0.105 Uiso 1 1 calc R . . C5 C 0.1926(4) 0.3496(2) 0.3334(2) 0.0560(9) Uani 1 1 d . . . C6 C 0.3462(4) 0.3540(3) 0.3435(3) 0.0709(11) Uani 1 1 d . . . H6A H 0.3517 0.3144 0.3958 0.106 Uiso 1 1 calc R . . H6B H 0.3714 0.4098 0.3383 0.106 Uiso 1 1 calc R . . H6C H 0.4112 0.3406 0.3027 0.106 Uiso 1 1 calc R . . C7 C 0.1521(5) 0.2586(3) 0.3458(3) 0.0833(13) Uani 1 1 d . . . H7A H 0.1601 0.2210 0.3983 0.125 Uiso 1 1 calc R . . H7B H 0.2155 0.2437 0.3055 0.125 Uiso 1 1 calc R . . H7C H 0.0554 0.2545 0.3412 0.125 Uiso 1 1 calc R . . C8 C 0.0924(5) 0.3774(3) 0.3954(3) 0.0835(13) Uani 1 1 d . . . H8A H 0.1071 0.3456 0.4481 0.125 Uiso 1 1 calc R . . H8B H -0.0052 0.3677 0.3950 0.125 Uiso 1 1 calc R . . H8C H 0.1126 0.4362 0.3818 0.125 Uiso 1 1 calc R . . C9 C 0.0216(3) 0.4738(2) 0.2289(2) 0.0466(8) Uani 1 1 d . . . C10 C -0.1085(3) 0.4275(2) 0.2558(2) 0.0526(9) Uani 1 1 d . . . C11 C -0.2358(3) 0.4646(2) 0.2571(2) 0.0514(9) Uani 1 1 d . . . C12 C -0.2474(3) 0.5509(2) 0.2303(2) 0.0455(8) Uani 1 1 d . . . C13 C -0.1168(4) 0.5960(2) 0.2014(2) 0.0493(9) Uani 1 1 d . . . C14 C 0.0130(3) 0.5603(2) 0.2007(2) 0.0491(9) Uani 1 1 d . . . C15 C -0.4733(4) 0.5970(2) 0.3219(2) 0.0552(9) Uani 1 1 d . . . C16 C -0.3972(5) 0.6084(3) 0.3723(3) 0.0722(12) Uani 1 1 d . . . C17 C -0.4600(7) 0.6144(3) 0.4449(3) 0.0979(16) Uani 1 1 d . . . C18 C -0.6061(8) 0.6088(4) 0.4702(3) 0.1023(18) Uani 1 1 d . . . C19 C -0.6865(6) 0.5959(3) 0.4234(3) 0.0927(16) Uani 1 1 d . . . C20 C -0.6189(4) 0.5923(3) 0.3505(3) 0.0672(11) Uani 1 1 d . . . C21 C -0.4113(3) 0.6767(2) 0.1601(2) 0.0483(9) Uani 1 1 d . . . C22 C -0.4508(4) 0.6770(3) 0.0919(3) 0.0652(11) Uani 1 1 d . . . C23 C -0.4704(5) 0.7479(3) 0.0294(3) 0.0769(12) Uani 1 1 d . . . C24 C -0.4472(5) 0.8255(3) 0.0316(2) 0.0682(11) Uani 1 1 d . . . C25 C -0.4068(4) 0.8293(2) 0.0958(3) 0.0601(10) Uani 1 1 d . . . C26 C -0.3913(3) 0.7569(2) 0.1574(2) 0.0505(9) Uani 1 1 d . . . C27 C -0.9836(5) -0.1440(3) 0.3399(3) 0.0957(17) Uani 1 1 d . . . C28 C -0.8939(7) -0.2071(5) 0.3795(4) 0.183(4) Uani 1 1 d . . . H28A H -0.9331 -0.2290 0.4367 0.274 Uiso 1 1 calc R . . H28B H -0.7990 -0.1821 0.3675 0.274 Uiso 1 1 calc R . . H28C H -0.8902 -0.2520 0.3605 0.274 Uiso 1 1 calc R . . C29 C -1.1356(5) -0.1722(4) 0.3465(3) 0.1024(17) Uani 1 1 d . . . H29A H -1.1802 -0.2056 0.4018 0.154 Uiso 1 1 calc R . . H29B H -1.1341 -0.2052 0.3145 0.154 Uiso 1 1 calc R . . H29C H -1.1888 -0.1238 0.3272 0.154 Uiso 1 1 calc R . . C30 C -0.9981(7) -0.0797(5) 0.3867(4) 0.155(3) Uani 1 1 d . . . H30A H -1.0395 -0.1100 0.4431 0.232 Uiso 1 1 calc R . . H30B H -1.0584 -0.0360 0.3647 0.232 Uiso 1 1 calc R . . H30C H -0.9050 -0.0551 0.3797 0.232 Uiso 1 1 calc R . . C31 C -0.8925(5) -0.1090(3) 0.1518(3) 0.0818(14) Uani 1 1 d . . . C32 C -0.8296(6) -0.1978(4) 0.1705(5) 0.155(3) Uani 1 1 d . . . H32A H -0.8299 -0.2157 0.1272 0.233 Uiso 1 1 calc R . . H32B H -0.8873 -0.2377 0.2199 0.233 Uiso 1 1 calc R . . H32C H -0.7332 -0.1941 0.1757 0.233 Uiso 1 1 calc R . . C33 C -1.0465(5) -0.1160(3) 0.1426(3) 0.0882(15) Uani 1 1 d . . . H33A H -1.0447 -0.1321 0.0980 0.132 Uiso 1 1 calc R . . H33B H -1.0874 -0.0627 0.1330 0.132 Uiso 1 1 calc R . . H33C H -1.1033 -0.1578 0.1911 0.132 Uiso 1 1 calc R . . C34 C -0.8054(8) -0.0431(6) 0.0793(3) 0.192(5) Uani 1 1 d . . . H34A H -0.8071 -0.0551 0.0328 0.288 Uiso 1 1 calc R . . H34B H -0.7085 -0.0415 0.0844 0.288 Uiso 1 1 calc R . . H34C H -0.8437 0.0104 0.0732 0.288 Uiso 1 1 calc R . . C35 C -0.7363(3) -0.0278(2) 0.2319(2) 0.0486(9) Uani 1 1 d . . . C36 C -0.7210(4) 0.0562(2) 0.2199(2) 0.0538(9) Uani 1 1 d . . . C37 C -0.5982(4) 0.0892(2) 0.2270(2) 0.0537(9) Uani 1 1 d . . . C38 C -0.4833(4) 0.0433(2) 0.2479(2) 0.0503(9) Uani 1 1 d . . . C39 C -0.4987(4) -0.0392(2) 0.2560(2) 0.0523(9) Uani 1 1 d . . . C40 C -0.6188(4) -0.0733(2) 0.2482(2) 0.0532(9) Uani 1 1 d . . . C41 C -0.3788(4) 0.1001(2) 0.3462(2) 0.0580(10) Uani 1 1 d . . . C42 C -0.5085(4) 0.0951(3) 0.3990(3) 0.0651(11) Uani 1 1 d . . . C43 C -0.5284(6) 0.1136(3) 0.4667(3) 0.0821(13) Uani 1 1 d . . . C44 C -0.4149(7) 0.1385(4) 0.4854(3) 0.1071(19) Uani 1 1 d . . . C45 C -0.2838(7) 0.1439(4) 0.4377(3) 0.113(2) Uani 1 1 d . . . C46 C -0.2677(5) 0.1247(3) 0.3708(3) 0.0827(14) Uani 1 1 d . . . C47 C -0.2671(4) 0.1637(2) 0.1861(2) 0.0527(9) Uani 1 1 d . . . C48 C -0.1721(5) 0.1544(3) 0.1208(3) 0.0746(12) Uani 1 1 d . . . C49 C -0.0906(5) 0.2196(3) 0.0564(3) 0.0825(13) Uani 1 1 d . . . C50 C -0.1032(5) 0.2997(3) 0.0522(2) 0.0695(11) Uani 1 1 d . . . C51 C -0.1967(4) 0.3132(2) 0.1136(2) 0.0574(10) Uani 1 1 d . . . C52 C -0.2743(4) 0.2469(2) 0.1774(2) 0.0494(9) Uani 1 1 d . . . B1 B -0.4057(4) 0.5892(3) 0.2351(3) 0.0495(10) Uani 1 1 d . . . H2B H -0.479(3) 0.5410(18) 0.2258(17) 0.039(8) Uiso 1 1 d . . . B2 B -0.3438(4) 0.0817(3) 0.2636(3) 0.0528(11) Uani 1 1 d . . . H1B H -0.261(4) 0.036(2) 0.272(2) 0.063(10) Uiso 1 1 d . . . H2A H 0.274(3) 0.4866(19) 0.2219(18) 0.048(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 0.0344(5) 0.0446(5) 0.0578(6) -0.0198(4) -0.0099(4) 0.0021(4) P2 0.0472(5) 0.0472(6) 0.0620(6) -0.0227(5) -0.0166(5) 0.0049(4) F1 0.0510(12) 0.0412(13) 0.136(2) -0.0266(13) -0.0247(13) 0.0029(9) F2 0.0405(11) 0.0517(13) 0.126(2) -0.0291(13) -0.0154(12) -0.0035(9) F3 0.0499(12) 0.0423(13) 0.1078(18) -0.0235(12) -0.0117(12) 0.0041(9) F4 0.0444(11) 0.0470(12) 0.0982(17) -0.0192(12) -0.0103(11) -0.0037(9) F5 0.0842(19) 0.150(3) 0.101(2) -0.077(2) -0.0366(16) 0.0081(17) F6 0.204(4) 0.209(4) 0.102(3) -0.097(3) -0.063(3) 0.030(3) F7 0.227(4) 0.185(4) 0.074(2) -0.066(2) 0.013(2) 0.049(3) F8 0.093(2) 0.153(3) 0.126(3) -0.050(2) 0.031(2) 0.0289(19) F9 0.0530(14) 0.118(2) 0.119(2) -0.0600(19) -0.0144(15) 0.0167(13) F10 0.161(3) 0.0830(18) 0.095(2) -0.0575(16) -0.0523(19) 0.0102(17) F11 0.204(4) 0.124(3) 0.083(2) -0.0505(19) -0.073(2) 0.027(2) F12 0.140(3) 0.0837(19) 0.0659(17) -0.0058(15) -0.0249(16) 0.0149(17) F13 0.1103(19) 0.0517(15) 0.0874(18) -0.0228(13) -0.0190(15) -0.0019(13) F14 0.0717(14) 0.0598(14) 0.0758(15) -0.0367(12) -0.0256(12) 0.0043(10) F15 0.0706(14) 0.0516(14) 0.131(2) -0.0328(14) -0.0550(15) 0.0177(11) F16 0.0725(14) 0.0431(13) 0.121(2) -0.0324(13) -0.0418(14) 0.0092(10) F17 0.0606(13) 0.0609(14) 0.129(2) -0.0515(14) -0.0455(14) 0.0233(11) F18 0.0659(13) 0.0506(13) 0.130(2) -0.0491(14) -0.0366(14) 0.0152(10) F19 0.0640(15) 0.154(3) 0.096(2) -0.067(2) -0.0159(14) -0.0003(15) F20 0.116(2) 0.169(3) 0.089(2) -0.066(2) 0.0003(19) 0.012(2) F21 0.204(4) 0.225(4) 0.079(2) -0.083(3) -0.018(2) -0.051(3) F22 0.155(3) 0.308(6) 0.090(2) -0.080(3) -0.031(2) -0.099(3) F23 0.0689(17) 0.195(3) 0.0861(19) -0.050(2) -0.0241(15) -0.0295(18) F24 0.179(3) 0.0786(19) 0.109(2) -0.0600(18) 0.006(2) 0.0106(18) F25 0.196(4) 0.134(3) 0.086(2) -0.059(2) 0.040(2) 0.008(2) F26 0.115(2) 0.095(2) 0.0633(16) -0.0074(15) -0.0084(15) -0.0127(16) F27 0.1106(19) 0.0523(15) 0.0880(18) -0.0220(13) -0.0248(15) 0.0041(13) F28 0.0684(13) 0.0634(14) 0.0736(15) -0.0353(12) -0.0101(12) 0.0146(11) C1 0.048(2) 0.059(2) 0.060(2) -0.027(2) -0.0141(18) 0.0115(17) C2 0.094(3) 0.097(4) 0.061(3) -0.031(3) -0.021(2) 0.030(3) C3 0.074(3) 0.097(4) 0.111(4) -0.067(3) -0.034(3) 0.009(2) C4 0.056(2) 0.080(3) 0.085(3) -0.046(3) -0.014(2) 0.017(2) C5 0.0439(19) 0.057(2) 0.058(2) -0.0145(19) -0.0091(18) 0.0039(16) C6 0.058(2) 0.080(3) 0.068(3) -0.018(2) -0.020(2) 0.003(2) C7 0.076(3) 0.056(3) 0.098(3) -0.002(2) -0.030(3) -0.001(2) C8 0.071(3) 0.107(4) 0.057(3) -0.023(3) -0.002(2) 0.012(2) C9 0.0386(18) 0.044(2) 0.058(2) -0.0213(17) -0.0115(16) 0.0056(15) C10 0.043(2) 0.040(2) 0.076(3) -0.0232(19) -0.0143(18) 0.0012(16) C11 0.0354(18) 0.050(2) 0.068(2) -0.0247(19) -0.0080(17) -0.0047(16) C12 0.0413(19) 0.045(2) 0.054(2) -0.0245(17) -0.0091(16) 0.0032(15) C13 0.050(2) 0.037(2) 0.062(2) -0.0225(17) -0.0103(17) 0.0030(15) C14 0.0369(18) 0.048(2) 0.063(2) -0.0246(18) -0.0063(16) -0.0038(16) C15 0.059(2) 0.051(2) 0.055(2) -0.0219(19) -0.0114(19) 0.0113(17) C16 0.078(3) 0.076(3) 0.065(3) -0.031(2) -0.013(2) 0.009(2) C17 0.138(5) 0.104(4) 0.069(3) -0.045(3) -0.036(4) 0.021(3) C18 0.128(5) 0.101(4) 0.067(4) -0.039(3) 0.007(4) 0.025(3) C19 0.086(4) 0.084(3) 0.086(4) -0.029(3) 0.013(3) 0.025(3) C20 0.062(3) 0.065(3) 0.068(3) -0.026(2) -0.003(2) 0.012(2) C21 0.0401(18) 0.055(2) 0.059(2) -0.0332(19) -0.0099(17) 0.0104(15) C22 0.079(3) 0.062(3) 0.070(3) -0.041(2) -0.021(2) 0.012(2) C23 0.102(3) 0.087(4) 0.054(3) -0.036(3) -0.029(2) 0.012(3) C24 0.080(3) 0.064(3) 0.051(3) -0.014(2) -0.012(2) 0.015(2) C25 0.058(2) 0.051(2) 0.067(3) -0.024(2) -0.004(2) 0.0061(18) C26 0.0412(19) 0.061(3) 0.056(2) -0.031(2) -0.0108(17) 0.0058(16) C27 0.051(2) 0.095(4) 0.096(4) 0.003(3) -0.002(2) 0.013(2) C28 0.115(5) 0.198(8) 0.114(5) 0.066(5) -0.016(4) 0.006(5) C29 0.068(3) 0.115(4) 0.099(4) -0.025(3) 0.003(3) -0.022(3) C30 0.126(6) 0.247(9) 0.106(5) -0.093(6) -0.009(4) -0.001(5) C31 0.066(3) 0.104(4) 0.101(4) -0.067(3) -0.021(3) -0.007(2) C32 0.106(4) 0.189(7) 0.293(10) -0.197(8) -0.104(6) 0.077(4) C33 0.083(3) 0.095(4) 0.121(4) -0.066(3) -0.048(3) 0.010(3) C34 0.165(7) 0.333(12) 0.075(4) -0.090(6) 0.015(4) -0.142(8) C35 0.050(2) 0.046(2) 0.054(2) -0.0232(18) -0.0156(17) 0.0058(16) C36 0.053(2) 0.049(2) 0.066(3) -0.0229(19) -0.0251(19) 0.0119(17) C37 0.060(2) 0.039(2) 0.066(3) -0.0214(18) -0.0216(19) 0.0053(17) C38 0.052(2) 0.051(2) 0.053(2) -0.0239(18) -0.0151(17) 0.0064(17) C39 0.052(2) 0.052(2) 0.065(2) -0.0302(19) -0.0228(18) 0.0147(17) C40 0.055(2) 0.044(2) 0.070(3) -0.0302(19) -0.0185(19) 0.0056(17) C41 0.060(2) 0.053(2) 0.060(2) -0.0151(19) -0.024(2) -0.0064(18) C42 0.064(3) 0.072(3) 0.063(3) -0.026(2) -0.020(2) 0.000(2) C43 0.089(3) 0.089(4) 0.060(3) -0.024(3) -0.009(3) -0.005(3) C44 0.134(5) 0.137(5) 0.050(3) -0.039(3) -0.013(3) -0.035(4) C45 0.110(4) 0.173(6) 0.061(3) -0.044(4) -0.028(3) -0.053(4) C46 0.067(3) 0.112(4) 0.062(3) -0.024(3) -0.014(2) -0.024(3) C47 0.053(2) 0.055(2) 0.063(2) -0.031(2) -0.0225(19) 0.0048(17) C48 0.102(3) 0.064(3) 0.071(3) -0.042(3) -0.019(3) 0.011(2) C49 0.103(4) 0.089(4) 0.053(3) -0.033(3) -0.002(3) 0.004(3) C50 0.082(3) 0.066(3) 0.050(3) -0.010(2) -0.015(2) -0.009(2) C51 0.067(2) 0.051(2) 0.060(3) -0.021(2) -0.027(2) 0.0060(19) C52 0.049(2) 0.056(2) 0.054(2) -0.028(2) -0.0201(18) 0.0109(17) B1 0.039(2) 0.050(2) 0.063(3) -0.027(2) -0.010(2) 0.0046(18) B2 0.052(2) 0.051(3) 0.065(3) -0.028(2) -0.021(2) 0.008(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 C9 1.793(3) . ? P1 C1 1.840(4) . ? P1 C5 1.846(4) . ? P2 C35 1.791(3) . ? P2 C27 1.829(5) . ? P2 C31 1.834(4) . ? F1 C10 1.348(4) . ? F2 C11 1.344(4) . ? F3 C13 1.349(4) . ? F4 C14 1.348(4) . ? F5 C16 1.343(5) . ? F6 C17 1.337(6) . ? F7 C18 1.347(6) . ? F8 C19 1.355(6) . ? F9 C20 1.361(5) . ? F10 C22 1.357(4) . ? F11 C23 1.340(5) . ? F12 C24 1.337(5) . ? F13 C25 1.351(4) . ? F14 C26 1.361(4) . ? F15 C36 1.345(4) . ? F16 C37 1.355(4) . ? F17 C39 1.339(4) . ? F18 C40 1.348(4) . ? F19 C42 1.357(5) . ? F20 C43 1.336(5) . ? F21 C44 1.348(5) . ? F22 C45 1.345(5) . ? F23 C46 1.355(5) . ? F24 C48 1.355(5) . ? F25 C49 1.354(5) . ? F26 C50 1.333(5) . ? F27 C51 1.346(4) . ? F28 C52 1.347(4) . ? C1 C4 1.524(5) . ? C1 C3 1.531(5) . ? C1 C2 1.533(6) . ? C5 C8 1.535(5) . ? C5 C6 1.539(5) . ? C5 C7 1.541(5) . ? C9 C10 1.382(4) . ? C9 C14 1.386(5) . ? C10 C11 1.367(5) . ? C11 C12 1.387(5) . ? C12 C13 1.376(5) . ? C12 B1 1.642(5) . ? C13 C14 1.379(5) . ? C15 C20 1.372(5) . ? C15 C16 1.378(6) . ? C15 B1 1.641(6) . ? C16 C17 1.381(6) . ? C17 C18 1.369(8) . ? C18 C19 1.363(8) . ? C19 C20 1.377(6) . ? C21 C26 1.380(5) . ? C21 C22 1.394(5) . ? C21 B1 1.624(6) . ? C22 C23 1.370(6) . ? C23 C24 1.377(6) . ? C24 C25 1.354(6) . ? C25 C26 1.365(5) . ? C27 C28 1.449(8) . ? C27 C29 1.516(6) . ? C27 C30 1.630(8) . ? C31 C34 1.469(8) . ? C31 C33 1.543(6) . ? C31 C32 1.573(7) . ? C35 C40 1.384(5) . ? C35 C36 1.384(5) . ? C36 C37 1.378(5) . ? C37 C38 1.385(5) . ? C38 C39 1.379(5) . ? C38 B2 1.640(5) . ? C39 C40 1.370(5) . ? C41 C42 1.378(5) . ? C41 C46 1.387(5) . ? C41 B2 1.632(6) . ? C42 C43 1.375(6) . ? C43 C44 1.343(7) . ? C44 C45 1.345(8) . ? C45 C46 1.370(7) . ? C47 C52 1.383(5) . ? C47 C48 1.396(5) . ? C47 B2 1.618(6) . ? C48 C49 1.375(6) . ? C49 C50 1.357(6) . ? C50 C51 1.368(6) . ? C51 C52 1.365(5) . ? 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 C9 P1 C1 110.37(16) . . ? C9 P1 C5 112.54(16) . . ? C1 P1 C5 120.07(17) . . ? C35 P2 C27 108.8(2) . . ? C35 P2 C31 112.63(18) . . ? C27 P2 C31 121.7(3) . . ? C4 C1 C3 111.0(3) . . ? C4 C1 C2 109.7(3) . . ? C3 C1 C2 109.6(4) . . ? C4 C1 P1 107.9(3) . . ? C3 C1 P1 112.4(3) . . ? C2 C1 P1 106.1(2) . . ? C8 C5 C6 108.4(3) . . ? C8 C5 C7 111.7(3) . . ? C6 C5 C7 108.5(3) . . ? C8 C5 P1 107.3(3) . . ? C6 C5 P1 106.7(3) . . ? C7 C5 P1 114.0(3) . . ? C10 C9 C14 114.9(3) . . ? C10 C9 P1 124.0(3) . . ? C14 C9 P1 121.1(2) . . ? F1 C10 C11 119.3(3) . . ? F1 C10 C9 118.5(3) . . ? C11 C10 C9 122.2(3) . . ? F2 C11 C10 115.8(3) . . ? F2 C11 C12 120.1(3) . . ? C10 C11 C12 124.0(3) . . ? C13 C12 C11 113.0(3) . . ? C13 C12 B1 126.7(3) . . ? C11 C12 B1 120.2(3) . . ? F3 C13 C12 119.6(3) . . ? F3 C13 C14 116.2(3) . . ? C12 C13 C14 124.2(3) . . ? F4 C14 C13 118.8(3) . . ? F4 C14 C9 119.6(3) . . ? C13 C14 C9 121.6(3) . . ? C20 C15 C16 113.6(4) . . ? C20 C15 B1 120.0(4) . . ? C16 C15 B1 126.3(3) . . ? F5 C16 C15 120.5(4) . . ? F5 C16 C17 115.7(4) . . ? C15 C16 C17 123.8(5) . . ? F6 C17 C18 120.3(5) . . ? F6 C17 C16 120.1(6) . . ? C18 C17 C16 119.6(5) . . ? F7 C18 C19 121.6(6) . . ? F7 C18 C17 119.4(7) . . ? C19 C18 C17 119.0(5) . . ? F8 C19 C18 120.3(5) . . ? F8 C19 C20 120.6(6) . . ? C18 C19 C20 119.2(5) . . ? F9 C20 C15 119.9(4) . . ? F9 C20 C19 115.4(4) . . ? C15 C20 C19 124.7(5) . . ? C26 C21 C22 112.2(3) . . ? C26 C21 B1 126.4(3) . . ? C22 C21 B1 121.1(3) . . ? F10 C22 C23 115.6(4) . . ? F10 C22 C21 119.6(4) . . ? C23 C22 C21 124.8(4) . . ? F11 C23 C22 121.1(4) . . ? F11 C23 C24 120.0(4) . . ? C22 C23 C24 119.0(4) . . ? F12 C24 C25 121.0(4) . . ? F12 C24 C23 119.9(4) . . ? C25 C24 C23 119.0(4) . . ? F13 C25 C24 119.3(4) . . ? F13 C25 C26 120.9(4) . . ? C24 C25 C26 119.8(4) . . ? F14 C26 C25 116.2(3) . . ? F14 C26 C21 118.6(3) . . ? C25 C26 C21 125.2(4) . . ? C28 C27 C29 117.8(5) . . ? C28 C27 C30 103.9(6) . . ? C29 C27 C30 105.7(4) . . ? C28 C27 P2 115.8(4) . . ? C29 C27 P2 109.3(4) . . ? C30 C27 P2 102.4(4) . . ? C34 C31 C33 110.2(5) . . ? C34 C31 C32 112.9(6) . . ? C33 C31 C32 108.6(4) . . ? C34 C31 P2 106.9(3) . . ? C33 C31 P2 107.2(3) . . ? C32 C31 P2 110.9(4) . . ? C40 C35 C36 115.1(3) . . ? C40 C35 P2 123.2(3) . . ? C36 C35 P2 121.4(3) . . ? F15 C36 C37 119.3(3) . . ? F15 C36 C35 119.8(3) . . ? C37 C36 C35 120.9(3) . . ? F16 C37 C36 116.5(3) . . ? F16 C37 C38 118.9(3) . . ? C36 C37 C38 124.5(3) . . ? C39 C38 C37 113.3(3) . . ? C39 C38 B2 122.8(3) . . ? C37 C38 B2 123.9(3) . . ? F17 C39 C40 116.5(3) . . ? F17 C39 C38 120.2(3) . . ? C40 C39 C38 123.3(3) . . ? F18 C40 C39 118.5(3) . . ? F18 C40 C35 118.8(3) . . ? C39 C40 C35 122.7(3) . . ? C42 C41 C46 111.1(4) . . ? C42 C41 B2 129.4(3) . . ? C46 C41 B2 119.5(4) . . ? F19 C42 C43 114.0(4) . . ? F19 C42 C41 120.6(4) . . ? C43 C42 C41 125.4(4) . . ? F20 C43 C44 119.7(5) . . ? F20 C43 C42 120.7(4) . . ? C44 C43 C42 119.5(5) . . ? C43 C44 C45 119.0(5) . . ? C43 C44 F21 120.4(6) . . ? C45 C44 F21 120.6(5) . . ? C44 C45 F22 120.1(5) . . ? C44 C45 C46 120.0(5) . . ? F22 C45 C46 119.9(5) . . ? F23 C46 C45 117.0(4) . . ? F23 C46 C41 118.1(4) . . ? C45 C46 C41 124.9(4) . . ? C52 C47 C48 112.3(3) . . ? C52 C47 B2 127.3(3) . . ? C48 C47 B2 120.2(3) . . ? F24 C48 C49 116.9(4) . . ? F24 C48 C47 118.8(4) . . ? C49 C48 C47 124.3(4) . . ? F25 C49 C50 120.4(4) . . ? F25 C49 C48 119.6(4) . . ? C50 C49 C48 120.0(4) . . ? F26 C50 C49 120.4(4) . . ? F26 C50 C51 121.1(4) . . ? C49 C50 C51 118.4(4) . . ? F27 C51 C52 120.9(4) . . ? F27 C51 C50 119.0(4) . . ? C52 C51 C50 120.1(4) . . ? F28 C52 C51 115.5(3) . . ? F28 C52 C47 119.7(3) . . ? C51 C52 C47 124.8(3) . . ? C21 B1 C15 111.3(3) . . ? C21 B1 C12 114.0(3) . . ? C15 B1 C12 112.7(3) . . ? C47 B2 C41 111.7(3) . . ? C47 B2 C38 111.4(3) . . ? C41 B2 C38 113.6(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.960 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.054 #===end