data_kt011_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 B F12 O P Si' _chemical_formula_weight 678.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 9.9406(8) _cell_length_b 11.7049(8) _cell_length_c 13.2536(10) _cell_angle_alpha 95.840(4) _cell_angle_beta 97.626(4) _cell_angle_gamma 102.456(4) _cell_volume 1478.89(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9550 _exptl_absorpt_correction_T_max 0.9772 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26289 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7239 _reflns_number_gt 5734 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7239 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.25710(4) 0.94331(3) 0.32539(3) 0.01713(11) Uani 1 1 d . . . H1 H 0.3380(17) 0.9782(15) 0.4118(13) 0.017(4) Uiso 1 1 d . . . H2 H 0.1670(18) 1.0049(15) 0.3398(13) 0.021(4) Uiso 1 1 d . . . B1 B 0.19133(17) 0.76392(14) 0.31250(13) 0.0162(3) Uani 1 1 d . . . O1 O 0.38063(12) 1.14585(9) 0.29058(8) 0.0220(2) Uani 1 1 d . . . Si1 Si 0.40267(5) 1.28033(4) 0.25497(4) 0.02222(12) Uani 1 1 d . . . C1 C 0.36049(16) 1.03081(13) 0.23620(12) 0.0198(3) Uani 1 1 d . . . C2 C 0.50165(16) 0.99986(13) 0.22883(12) 0.0213(3) Uani 1 1 d . . . H3 H 0.4842 0.9138 0.2070 0.026 Uiso 1 1 calc R . . H4 H 0.5421 1.0402 0.1739 0.026 Uiso 1 1 calc R . . C3 C 0.61063(17) 1.03129(14) 0.32601(13) 0.0248(3) Uani 1 1 d . . . H5 H 0.5752 0.9869 0.3804 0.030 Uiso 1 1 calc R . . H6 H 0.6273 1.1166 0.3507 0.030 Uiso 1 1 calc R . . C4 C 0.74795(18) 1.00180(16) 0.30543(15) 0.0328(4) Uani 1 1 d . . . H7 H 0.7292 0.9208 0.2703 0.049 Uiso 1 1 calc R . . H8 H 0.8102 1.0089 0.3708 0.049 Uiso 1 1 calc R . . H9 H 0.7924 1.0568 0.2620 0.049 Uiso 1 1 calc R . . C5 C 0.27229(17) 1.01869(13) 0.13017(12) 0.0231(3) Uani 1 1 d . . . H10 H 0.1802 1.0336 0.1399 0.028 Uiso 1 1 calc R . . H11 H 0.3179 1.0814 0.0928 0.028 Uiso 1 1 calc R . . C6 C 0.24775(18) 0.90031(14) 0.06204(13) 0.0262(3) Uani 1 1 d . . . H12 H 0.3373 0.8899 0.0421 0.031 Uiso 1 1 calc R . . H13 H 0.2132 0.8356 0.1014 0.031 Uiso 1 1 calc R . . C7 C 0.1427(2) 0.89270(17) -0.03426(15) 0.0430(5) Uani 1 1 d . . . H14 H 0.0526 0.8992 -0.0149 0.065 Uiso 1 1 calc R . . H15 H 0.1316 0.8168 -0.0769 0.065 Uiso 1 1 calc R . . H16 H 0.1762 0.9572 -0.0731 0.065 Uiso 1 1 calc R . . C8 C 0.4511(2) 1.38048(15) 0.37746(14) 0.0338(4) Uani 1 1 d . . . H17 H 0.3774 1.3622 0.4197 0.051 Uiso 1 1 calc R . . H18 H 0.4626 1.4624 0.3636 0.051 Uiso 1 1 calc R . . H19 H 0.5390 1.3701 0.4142 0.051 Uiso 1 1 calc R . . C9 C 0.5442(2) 1.30523(17) 0.17430(18) 0.0423(5) Uani 1 1 d . . . H20 H 0.6290 1.2890 0.2109 0.063 Uiso 1 1 calc R . . H21 H 0.5634 1.3874 0.1606 0.063 Uiso 1 1 calc R . . H22 H 0.5145 1.2523 0.1092 0.063 Uiso 1 1 calc R . . C10 C 0.2377(2) 1.30215(17) 0.18552(14) 0.0349(4) Uani 1 1 d . . . H23 H 0.2159 1.2545 0.1177 0.052 Uiso 1 1 calc R . . H24 H 0.2480 1.3857 0.1774 0.052 Uiso 1 1 calc R . . H25 H 0.1619 1.2777 0.2247 0.052 Uiso 1 1 calc R . . C11 C 0.05320(15) 0.70896(13) 0.22537(11) 0.0176(3) Uani 1 1 d . . . C12 C -0.03633(16) 0.76901(13) 0.17576(12) 0.0200(3) Uani 1 1 d . . . C13 C -0.15449(17) 0.71268(15) 0.10613(12) 0.0233(3) Uani 1 1 d . . . C14 C -0.19051(16) 0.59238(15) 0.08026(12) 0.0252(3) Uani 1 1 d . . . H26 H -0.2699 0.5542 0.0309 0.030 Uiso 1 1 calc R . . C15 C -0.10512(16) 0.52957(14) 0.12989(13) 0.0236(3) Uani 1 1 d . . . C16 C 0.01024(16) 0.58689(13) 0.20056(12) 0.0197(3) Uani 1 1 d . . . C17 C 0.14381(15) 0.73168(12) 0.42265(11) 0.0172(3) Uani 1 1 d . . . C18 C 0.05260(16) 0.78711(13) 0.46865(12) 0.0193(3) Uani 1 1 d . . . C19 C 0.00373(16) 0.75900(14) 0.55814(12) 0.0228(3) Uani 1 1 d . . . C20 C 0.04290(17) 0.67085(15) 0.60777(13) 0.0259(3) Uani 1 1 d . . . H27 H 0.0110 0.6517 0.6698 0.031 Uiso 1 1 calc R . . C21 C 0.13026(17) 0.61180(14) 0.56354(12) 0.0229(3) Uani 1 1 d . . . C22 C 0.17802(16) 0.64063(13) 0.47369(12) 0.0197(3) Uani 1 1 d . . . C23 C 0.33494(15) 0.72343(12) 0.29080(11) 0.0163(3) Uani 1 1 d . . . C24 C 0.45252(16) 0.75041(13) 0.36686(11) 0.0188(3) Uani 1 1 d . . . C25 C 0.57718(16) 0.72136(14) 0.35443(12) 0.0216(3) Uani 1 1 d . . . C26 C 0.59287(17) 0.66124(14) 0.26341(13) 0.0248(3) Uani 1 1 d . . . H28 H 0.6777 0.6396 0.2544 0.030 Uiso 1 1 calc R . . C27 C 0.47964(17) 0.63415(13) 0.18637(12) 0.0218(3) Uani 1 1 d . . . C28 C 0.35557(15) 0.66478(12) 0.19936(12) 0.0181(3) Uani 1 1 d . . . F1 F -0.00990(10) 0.88861(8) 0.19354(7) 0.0261(2) Uani 1 1 d . . . F2 F -0.23644(11) 0.78017(9) 0.06465(8) 0.0331(2) Uani 1 1 d . . . F3 F -0.13453(11) 0.41089(8) 0.10992(8) 0.0348(3) Uani 1 1 d . . . F4 F 0.08723(10) 0.51851(8) 0.24671(8) 0.0249(2) Uani 1 1 d . . . F5 F 0.00675(10) 0.87400(8) 0.42402(8) 0.0271(2) Uani 1 1 d . . . F6 F -0.08184(11) 0.82034(9) 0.59768(8) 0.0326(2) Uani 1 1 d . . . F7 F 0.17031(11) 0.52291(9) 0.60796(8) 0.0335(2) Uani 1 1 d . . . F8 F 0.26016(10) 0.57378(8) 0.43599(7) 0.0249(2) Uani 1 1 d . . . F9 F 0.44681(9) 0.80892(8) 0.45937(7) 0.0234(2) Uani 1 1 d . . . F10 F 0.68501(10) 0.75356(10) 0.43217(8) 0.0321(2) Uani 1 1 d . . . F11 F 0.48742(10) 0.57570(9) 0.09427(8) 0.0312(2) Uani 1 1 d . . . F12 F 0.25315(9) 0.63376(8) 0.11673(7) 0.0230(2) 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 0.0208(2) 0.01408(18) 0.0171(2) 0.00160(14) 0.00457(15) 0.00459(14) B1 0.0187(8) 0.0140(7) 0.0168(8) 0.0016(6) 0.0031(6) 0.0058(6) O1 0.0304(6) 0.0144(5) 0.0212(6) 0.0016(4) 0.0051(5) 0.0050(4) Si1 0.0277(2) 0.0156(2) 0.0254(2) 0.00510(17) 0.00837(18) 0.00574(17) C1 0.0263(8) 0.0141(7) 0.0189(7) 0.0026(5) 0.0056(6) 0.0030(6) C2 0.0241(8) 0.0180(7) 0.0223(8) 0.0014(6) 0.0076(6) 0.0045(6) C3 0.0243(8) 0.0215(8) 0.0276(9) 0.0010(6) 0.0056(7) 0.0034(6) C4 0.0233(9) 0.0314(9) 0.0416(11) 0.0000(8) 0.0058(8) 0.0037(7) C5 0.0308(9) 0.0197(7) 0.0194(8) 0.0047(6) 0.0037(7) 0.0061(6) C6 0.0352(9) 0.0220(8) 0.0214(8) 0.0024(6) 0.0043(7) 0.0074(7) C7 0.0649(14) 0.0320(10) 0.0264(10) -0.0013(8) -0.0086(9) 0.0107(9) C8 0.0450(11) 0.0189(8) 0.0344(10) 0.0009(7) 0.0022(8) 0.0045(7) C9 0.0464(12) 0.0311(10) 0.0553(13) 0.0125(9) 0.0286(10) 0.0065(8) C10 0.0472(11) 0.0330(10) 0.0296(10) 0.0062(7) 0.0057(8) 0.0198(8) C11 0.0184(7) 0.0198(7) 0.0151(7) 0.0026(5) 0.0040(6) 0.0047(6) C12 0.0221(8) 0.0196(7) 0.0202(8) 0.0045(6) 0.0067(6) 0.0062(6) C13 0.0212(8) 0.0336(9) 0.0178(8) 0.0063(6) 0.0033(6) 0.0106(7) C14 0.0185(8) 0.0322(9) 0.0215(8) -0.0017(6) 0.0032(6) 0.0014(6) C15 0.0219(8) 0.0210(8) 0.0251(8) -0.0014(6) 0.0063(6) -0.0006(6) C16 0.0203(7) 0.0190(7) 0.0212(8) 0.0044(6) 0.0057(6) 0.0056(6) C17 0.0169(7) 0.0160(7) 0.0178(7) 0.0025(5) 0.0025(6) 0.0017(5) C18 0.0196(7) 0.0181(7) 0.0210(8) 0.0034(6) 0.0037(6) 0.0055(6) C19 0.0226(8) 0.0218(8) 0.0245(8) 0.0003(6) 0.0089(6) 0.0046(6) C20 0.0299(9) 0.0279(8) 0.0199(8) 0.0059(6) 0.0098(7) 0.0018(7) C21 0.0248(8) 0.0214(7) 0.0233(8) 0.0089(6) 0.0038(6) 0.0043(6) C22 0.0183(7) 0.0180(7) 0.0230(8) 0.0026(6) 0.0042(6) 0.0045(6) C23 0.0179(7) 0.0136(6) 0.0179(7) 0.0034(5) 0.0044(6) 0.0031(5) C24 0.0221(7) 0.0183(7) 0.0159(7) 0.0025(5) 0.0050(6) 0.0034(6) C25 0.0172(7) 0.0232(8) 0.0236(8) 0.0063(6) 0.0015(6) 0.0029(6) C26 0.0196(8) 0.0261(8) 0.0322(9) 0.0065(7) 0.0102(7) 0.0078(6) C27 0.0260(8) 0.0188(7) 0.0219(8) 0.0004(6) 0.0108(6) 0.0049(6) C28 0.0199(7) 0.0149(7) 0.0193(7) 0.0026(5) 0.0033(6) 0.0034(5) F1 0.0279(5) 0.0193(5) 0.0318(5) 0.0046(4) 0.0000(4) 0.0093(4) F2 0.0289(5) 0.0406(6) 0.0312(6) 0.0060(5) -0.0039(4) 0.0160(4) F3 0.0339(6) 0.0197(5) 0.0435(6) -0.0056(4) 0.0008(5) -0.0019(4) F4 0.0259(5) 0.0170(4) 0.0320(5) 0.0048(4) 0.0024(4) 0.0063(4) F5 0.0311(5) 0.0277(5) 0.0312(5) 0.0115(4) 0.0134(4) 0.0172(4) F6 0.0349(6) 0.0352(6) 0.0344(6) 0.0040(4) 0.0201(5) 0.0140(4) F7 0.0416(6) 0.0316(6) 0.0338(6) 0.0197(4) 0.0105(5) 0.0130(5) F8 0.0295(5) 0.0215(5) 0.0292(5) 0.0081(4) 0.0100(4) 0.0127(4) F9 0.0249(5) 0.0270(5) 0.0171(5) -0.0010(4) 0.0022(4) 0.0063(4) F10 0.0186(5) 0.0465(6) 0.0288(6) 0.0041(4) -0.0016(4) 0.0064(4) F11 0.0299(5) 0.0359(6) 0.0285(5) -0.0072(4) 0.0121(4) 0.0104(4) F12 0.0238(5) 0.0257(5) 0.0184(5) -0.0028(4) 0.0021(4) 0.0070(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.9021(15) . ? P1 B1 2.0422(16) . ? P1 H1 1.281(17) . ? P1 H2 1.286(17) . ? B1 C11 1.637(2) . ? B1 C17 1.648(2) . ? B1 C23 1.649(2) . ? O1 C1 1.4216(17) . ? O1 Si1 1.6668(11) . ? Si1 C8 1.8448(18) . ? Si1 C10 1.8521(19) . ? Si1 C9 1.8690(19) . ? C1 C5 1.531(2) . ? C1 C2 1.536(2) . ? C2 C3 1.526(2) . ? C2 H3 0.9900 . ? C2 H4 0.9900 . ? C3 C4 1.530(2) . ? C3 H5 0.9900 . ? C3 H6 0.9900 . ? C4 H7 0.9800 . ? C4 H8 0.9800 . ? C4 H9 0.9800 . ? C5 C6 1.528(2) . ? C5 H10 0.9900 . ? C5 H11 0.9900 . ? C6 C7 1.520(2) . ? C6 H12 0.9900 . ? C6 H13 0.9900 . ? C7 H14 0.9800 . ? C7 H15 0.9800 . ? C7 H16 0.9800 . ? C8 H17 0.9800 . ? C8 H18 0.9800 . ? C8 H19 0.9800 . ? C9 H20 0.9800 . ? C9 H21 0.9800 . ? C9 H22 0.9800 . ? C10 H23 0.9800 . ? C10 H24 0.9800 . ? C10 H25 0.9800 . ? C11 C12 1.388(2) . ? C11 C16 1.391(2) . ? C12 F1 1.3572(17) . ? C12 C13 1.386(2) . ? C13 F2 1.3554(18) . ? C13 C14 1.371(2) . ? C14 C15 1.383(2) . ? C14 H26 0.9500 . ? C15 F3 1.3471(18) . ? C15 C16 1.378(2) . ? C16 F4 1.3565(17) . ? C17 C18 1.391(2) . ? C17 C22 1.397(2) . ? C18 F5 1.3575(17) . ? C18 C19 1.384(2) . ? C19 F6 1.3486(17) . ? C19 C20 1.376(2) . ? C20 C21 1.374(2) . ? C20 H27 0.9500 . ? C21 F7 1.3524(18) . ? C21 C22 1.386(2) . ? C22 F8 1.3539(17) . ? C23 C28 1.393(2) . ? C23 C24 1.395(2) . ? C24 F9 1.3565(16) . ? C24 C25 1.379(2) . ? C25 F10 1.3440(18) . ? C25 C26 1.378(2) . ? C26 C27 1.373(2) . ? C26 H28 0.9500 . ? C27 F11 1.3572(17) . ? C27 C28 1.383(2) . ? C28 F12 1.3533(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 B1 126.76(7) . . ? C1 P1 H1 101.3(7) . . ? B1 P1 H1 107.5(7) . . ? C1 P1 H2 101.1(8) . . ? B1 P1 H2 117.5(8) . . ? H1 P1 H2 98.0(10) . . ? C11 B1 C17 105.63(12) . . ? C11 B1 C23 115.78(12) . . ? C17 B1 C23 113.49(12) . . ? C11 B1 P1 113.70(10) . . ? C17 B1 P1 107.39(10) . . ? C23 B1 P1 100.75(10) . . ? C1 O1 Si1 133.55(10) . . ? O1 Si1 C8 104.02(7) . . ? O1 Si1 C10 110.99(8) . . ? C8 Si1 C10 109.07(9) . . ? O1 Si1 C9 110.38(7) . . ? C8 Si1 C9 111.40(10) . . ? C10 Si1 C9 110.80(10) . . ? O1 C1 C5 111.42(12) . . ? O1 C1 C2 110.40(12) . . ? C5 C1 C2 111.73(13) . . ? O1 C1 P1 98.72(9) . . ? C5 C1 P1 110.58(11) . . ? C2 C1 P1 113.34(11) . . ? C3 C2 C1 116.89(13) . . ? C3 C2 H3 108.1 . . ? C1 C2 H3 108.1 . . ? C3 C2 H4 108.1 . . ? C1 C2 H4 108.1 . . ? H3 C2 H4 107.3 . . ? C2 C3 C4 110.94(14) . . ? C2 C3 H5 109.5 . . ? C4 C3 H5 109.5 . . ? C2 C3 H6 109.5 . . ? C4 C3 H6 109.5 . . ? H5 C3 H6 108.0 . . ? C3 C4 H7 109.5 . . ? C3 C4 H8 109.5 . . ? H7 C4 H8 109.5 . . ? C3 C4 H9 109.5 . . ? H7 C4 H9 109.5 . . ? H8 C4 H9 109.5 . . ? C6 C5 C1 116.62(13) . . ? C6 C5 H10 108.1 . . ? C1 C5 H10 108.1 . . ? C6 C5 H11 108.1 . . ? C1 C5 H11 108.1 . . ? H10 C5 H11 107.3 . . ? C7 C6 C5 111.71(14) . . ? C7 C6 H12 109.3 . . ? C5 C6 H12 109.3 . . ? C7 C6 H13 109.3 . . ? C5 C6 H13 109.3 . . ? H12 C6 H13 107.9 . . ? C6 C7 H14 109.5 . . ? C6 C7 H15 109.5 . . ? H14 C7 H15 109.5 . . ? C6 C7 H16 109.5 . . ? H14 C7 H16 109.5 . . ? H15 C7 H16 109.5 . . ? Si1 C8 H17 109.5 . . ? Si1 C8 H18 109.5 . . ? H17 C8 H18 109.5 . . ? Si1 C8 H19 109.5 . . ? H17 C8 H19 109.5 . . ? H18 C8 H19 109.5 . . ? Si1 C9 H20 109.5 . . ? Si1 C9 H21 109.5 . . ? H20 C9 H21 109.5 . . ? Si1 C9 H22 109.5 . . ? H20 C9 H22 109.5 . . ? H21 C9 H22 109.5 . . ? Si1 C10 H23 109.5 . . ? Si1 C10 H24 109.5 . . ? H23 C10 H24 109.5 . . ? Si1 C10 H25 109.5 . . ? H23 C10 H25 109.5 . . ? H24 C10 H25 109.5 . . ? C12 C11 C16 113.36(14) . . ? C12 C11 B1 127.95(13) . . ? C16 C11 B1 118.53(13) . . ? F1 C12 C13 116.56(13) . . ? F1 C12 C11 120.34(14) . . ? C13 C12 C11 123.10(14) . . ? F2 C13 C14 120.13(15) . . ? F2 C13 C12 117.92(15) . . ? C14 C13 C12 121.94(15) . . ? C13 C14 C15 116.47(15) . . ? C13 C14 H26 121.8 . . ? C15 C14 H26 121.8 . . ? F3 C15 C16 119.09(14) . . ? F3 C15 C14 120.14(14) . . ? C16 C15 C14 120.77(15) . . ? F4 C16 C15 116.95(13) . . ? F4 C16 C11 118.76(13) . . ? C15 C16 C11 124.27(14) . . ? C18 C17 C22 113.29(13) . . ? C18 C17 B1 121.78(13) . . ? C22 C17 B1 124.66(13) . . ? F5 C18 C19 116.89(13) . . ? F5 C18 C17 119.05(13) . . ? C19 C18 C17 124.06(14) . . ? F6 C19 C20 119.83(14) . . ? F6 C19 C18 119.26(14) . . ? C20 C19 C18 120.90(14) . . ? C21 C20 C19 116.95(14) . . ? C21 C20 H27 121.5 . . ? C19 C20 H27 121.5 . . ? F7 C21 C20 119.56(14) . . ? F7 C21 C22 118.91(14) . . ? C20 C21 C22 121.52(14) . . ? F8 C22 C21 115.99(13) . . ? F8 C22 C17 120.78(13) . . ? C21 C22 C17 123.22(14) . . ? C28 C23 C24 113.35(13) . . ? C28 C23 B1 126.25(13) . . ? C24 C23 B1 120.38(13) . . ? F9 C24 C25 116.72(13) . . ? F9 C24 C23 119.27(13) . . ? C25 C24 C23 124.01(14) . . ? F10 C25 C26 119.80(14) . . ? F10 C25 C24 119.19(14) . . ? C26 C25 C24 121.00(15) . . ? C27 C26 C25 116.63(14) . . ? C27 C26 H28 121.7 . . ? C25 C26 H28 121.7 . . ? F11 C27 C26 120.05(14) . . ? F11 C27 C28 118.08(14) . . ? C26 C27 C28 121.86(14) . . ? F12 C28 C27 115.61(13) . . ? F12 C28 C23 121.26(13) . . ? C27 C28 C23 123.13(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 P1 B1 C11 -78.00(13) . . . . ? C1 P1 B1 C17 165.52(9) . . . . ? C1 P1 B1 C23 46.54(13) . . . . ? C1 O1 Si1 C8 -170.60(14) . . . . ? C1 O1 Si1 C10 72.24(15) . . . . ? C1 O1 Si1 C9 -51.00(16) . . . . ? Si1 O1 C1 C5 -35.67(19) . . . . ? Si1 O1 C1 C2 89.09(16) . . . . ? Si1 O1 C1 P1 -151.92(10) . . . . ? B1 P1 C1 O1 -175.88(8) . . . . ? B1 P1 C1 C5 67.23(13) . . . . ? B1 P1 C1 C2 -59.12(14) . . . . ? O1 C1 C2 C3 43.72(18) . . . . ? C5 C1 C2 C3 168.31(13) . . . . ? P1 C1 C2 C3 -65.95(16) . . . . ? C1 C2 C3 C4 -176.77(14) . . . . ? O1 C1 C5 C6 177.66(13) . . . . ? C2 C1 C5 C6 53.64(18) . . . . ? P1 C1 C5 C6 -73.60(16) . . . . ? C1 C5 C6 C7 171.92(15) . . . . ? C17 B1 C11 C12 104.16(16) . . . . ? C23 B1 C11 C12 -129.35(15) . . . . ? P1 B1 C11 C12 -13.3(2) . . . . ? C17 B1 C11 C16 -70.82(16) . . . . ? C23 B1 C11 C16 55.68(18) . . . . ? P1 B1 C11 C16 171.68(11) . . . . ? C16 C11 C12 F1 178.78(13) . . . . ? B1 C11 C12 F1 3.6(2) . . . . ? C16 C11 C12 C13 -1.8(2) . . . . ? B1 C11 C12 C13 -177.00(14) . . . . ? F1 C12 C13 F2 -2.4(2) . . . . ? C11 C12 C13 F2 178.12(13) . . . . ? F1 C12 C13 C14 178.62(14) . . . . ? C11 C12 C13 C14 -0.8(2) . . . . ? F2 C13 C14 C15 -176.85(14) . . . . ? C12 C13 C14 C15 2.1(2) . . . . ? C13 C14 C15 F3 179.01(14) . . . . ? C13 C14 C15 C16 -0.6(2) . . . . ? F3 C15 C16 F4 -0.5(2) . . . . ? C14 C15 C16 F4 179.12(14) . . . . ? F3 C15 C16 C11 178.14(14) . . . . ? C14 C15 C16 C11 -2.2(2) . . . . ? C12 C11 C16 F4 -178.05(12) . . . . ? B1 C11 C16 F4 -2.4(2) . . . . ? C12 C11 C16 C15 3.3(2) . . . . ? B1 C11 C16 C15 179.01(14) . . . . ? C11 B1 C17 C18 -71.18(17) . . . . ? C23 B1 C17 C18 160.94(13) . . . . ? P1 B1 C17 C18 50.49(17) . . . . ? C11 B1 C17 C22 102.31(16) . . . . ? C23 B1 C17 C22 -25.6(2) . . . . ? P1 B1 C17 C22 -136.02(13) . . . . ? C22 C17 C18 F5 -177.34(13) . . . . ? B1 C17 C18 F5 -3.2(2) . . . . ? C22 C17 C18 C19 2.3(2) . . . . ? B1 C17 C18 C19 176.47(14) . . . . ? F5 C18 C19 F6 -2.0(2) . . . . ? C17 C18 C19 F6 178.37(14) . . . . ? F5 C18 C19 C20 178.98(15) . . . . ? C17 C18 C19 C20 -0.7(3) . . . . ? F6 C19 C20 C21 -179.96(14) . . . . ? C18 C19 C20 C21 -0.9(2) . . . . ? C19 C20 C21 F7 -178.87(15) . . . . ? C19 C20 C21 C22 0.7(2) . . . . ? F7 C21 C22 F8 1.5(2) . . . . ? C20 C21 C22 F8 -178.10(14) . . . . ? F7 C21 C22 C17 -179.30(14) . . . . ? C20 C21 C22 C17 1.1(3) . . . . ? C18 C17 C22 F8 176.67(13) . . . . ? B1 C17 C22 F8 2.7(2) . . . . ? C18 C17 C22 C21 -2.5(2) . . . . ? B1 C17 C22 C21 -176.48(14) . . . . ? C11 B1 C23 C28 11.6(2) . . . . ? C17 B1 C23 C28 134.04(14) . . . . ? P1 B1 C23 C28 -111.49(14) . . . . ? C11 B1 C23 C24 -170.32(12) . . . . ? C17 B1 C23 C24 -47.89(18) . . . . ? P1 B1 C23 C24 66.58(15) . . . . ? C28 C23 C24 F9 179.20(12) . . . . ? B1 C23 C24 F9 0.9(2) . . . . ? C28 C23 C24 C25 -0.7(2) . . . . ? B1 C23 C24 C25 -179.00(14) . . . . ? F9 C24 C25 F10 -1.1(2) . . . . ? C23 C24 C25 F10 178.76(13) . . . . ? F9 C24 C25 C26 179.59(13) . . . . ? C23 C24 C25 C26 -0.5(2) . . . . ? F10 C25 C26 C27 -178.19(14) . . . . ? C24 C25 C26 C27 1.1(2) . . . . ? C25 C26 C27 F11 179.58(14) . . . . ? C25 C26 C27 C28 -0.4(2) . . . . ? F11 C27 C28 F12 -0.7(2) . . . . ? C26 C27 C28 F12 179.29(13) . . . . ? F11 C27 C28 C23 179.14(13) . . . . ? C26 C27 C28 C23 -0.8(2) . . . . ? C24 C23 C28 F12 -178.79(13) . . . . ? B1 C23 C28 F12 -0.6(2) . . . . ? C24 C23 C28 C27 1.4(2) . . . . ? B1 C23 C28 C27 179.54(14) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.375 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.051 #===end data_kt012_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H6 B F12 P' _chemical_formula_weight 492.01 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 'orthorhombic' _symmetry_space_group_name_H-M 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 10.1556(3) _cell_length_b 17.4865(5) _cell_length_c 20.2840(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3602.15(17) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Block' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9468 _exptl_absorpt_correction_T_max 0.9468 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16575 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4140 _reflns_number_gt 3216 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0344P)^2^+1.7753P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4140 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.20804(5) 0.09437(3) 1.00006(2) 0.02406(11) Uani 1 1 d . . . H1 H 0.2983(18) 0.0625(10) 1.0355(9) 0.028(5) Uiso 1 1 d . . . H2 H 0.214(2) 0.1663(12) 1.0158(10) 0.036(5) Uiso 1 1 d . . . H3 H 0.102(2) 0.0676(11) 1.0300(10) 0.037(6) Uiso 1 1 d . . . B1 B 0.22180(18) 0.06785(10) 0.90228(8) 0.0184(3) Uani 1 1 d . . . C1 C 0.07040(15) 0.05414(9) 0.87803(8) 0.0190(3) Uani 1 1 d . . . C2 C -0.03082(16) 0.10318(9) 0.89512(8) 0.0227(3) Uani 1 1 d . . . C3 C -0.15921(17) 0.09477(10) 0.87441(9) 0.0275(4) Uani 1 1 d . . . C4 C -0.19380(18) 0.03517(11) 0.83348(9) 0.0285(4) Uani 1 1 d . . . C5 C -0.09591(17) -0.01421(10) 0.81481(8) 0.0246(4) Uani 1 1 d . . . C6 C 0.03237(16) -0.00451(9) 0.83578(8) 0.0216(3) Uani 1 1 d . . . C7 C 0.30881(15) -0.01072(9) 0.90264(7) 0.0182(3) Uani 1 1 d . . . C8 C 0.26542(16) -0.07424(9) 0.93753(8) 0.0225(3) Uani 1 1 d . . . C9 C 0.32678(18) -0.14452(9) 0.93705(8) 0.0257(4) Uani 1 1 d . . . C10 C 0.44031(19) -0.15526(10) 0.90126(9) 0.0279(4) Uani 1 1 d . . . C11 C 0.48750(17) -0.09362(10) 0.86696(9) 0.0249(4) Uani 1 1 d . . . C12 C 0.42385(16) -0.02363(9) 0.86756(8) 0.0202(3) Uani 1 1 d . . . C13 C 0.29126(15) 0.14098(9) 0.86659(8) 0.0185(3) Uani 1 1 d . . . C14 C 0.39852(17) 0.17869(10) 0.89396(8) 0.0230(3) Uani 1 1 d . . . C15 C 0.46038(17) 0.24001(10) 0.86535(9) 0.0275(4) Uani 1 1 d . . . C16 C 0.42040(19) 0.26706(10) 0.80492(10) 0.0307(4) Uani 1 1 d . . . C17 C 0.3159(2) 0.23086(10) 0.77576(9) 0.0317(4) Uani 1 1 d . . . C18 C 0.25300(17) 0.16983(9) 0.80565(8) 0.0234(3) Uani 1 1 d . . . F1 F -0.00301(10) 0.16383(5) 0.93509(5) 0.0294(2) Uani 1 1 d . . . F2 F -0.25137(11) 0.14456(7) 0.89497(6) 0.0433(3) Uani 1 1 d . . . F3 F -0.12392(10) -0.07338(6) 0.77445(5) 0.0339(3) Uani 1 1 d . . . F4 F 0.12260(9) -0.05368(6) 0.81150(5) 0.0317(2) Uani 1 1 d . . . F5 F 0.15272(10) -0.06753(6) 0.97350(5) 0.0326(3) Uani 1 1 d . . . F6 F 0.27447(12) -0.20265(6) 0.97162(5) 0.0377(3) Uani 1 1 d . . . F7 F 0.59866(11) -0.10095(6) 0.83097(6) 0.0384(3) Uani 1 1 d . . . F8 F 0.47735(9) 0.03222(5) 0.82984(5) 0.0278(2) Uani 1 1 d . . . F9 F 0.44529(10) 0.15350(6) 0.95303(5) 0.0346(3) Uani 1 1 d . . . F10 F 0.56111(11) 0.27432(7) 0.89721(6) 0.0421(3) Uani 1 1 d . . . F11 F 0.27252(14) 0.25427(8) 0.71620(6) 0.0553(4) Uani 1 1 d . . . F12 F 0.15183(11) 0.13819(6) 0.77204(5) 0.0359(3) Uani 1 1 d . . . H4 H -0.280(2) 0.0291(12) 0.8182(10) 0.040(6) Uiso 1 1 d . . . H5 H 0.463(2) 0.3060(13) 0.7840(10) 0.042(6) Uiso 1 1 d . . . H6 H 0.483(2) -0.2012(13) 0.9004(10) 0.040(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0276(2) 0.0252(2) 0.0194(2) -0.00032(18) 0.00322(18) 0.00005(18) B1 0.0196(9) 0.0180(8) 0.0177(8) 0.0003(7) 0.0017(7) 0.0001(7) C1 0.0190(8) 0.0188(8) 0.0193(7) 0.0052(6) 0.0022(6) -0.0009(6) C2 0.0246(8) 0.0192(8) 0.0243(8) 0.0029(7) 0.0029(7) 0.0007(6) C3 0.0218(8) 0.0305(9) 0.0301(9) 0.0048(8) 0.0033(7) 0.0083(7) C4 0.0182(8) 0.0385(10) 0.0287(9) 0.0077(8) -0.0011(7) -0.0010(7) C5 0.0252(9) 0.0252(8) 0.0233(8) 0.0025(7) -0.0018(7) -0.0050(7) C6 0.0203(8) 0.0214(8) 0.0230(8) 0.0018(7) 0.0014(6) 0.0013(6) C7 0.0191(8) 0.0175(7) 0.0181(7) -0.0006(6) -0.0032(6) -0.0013(6) C8 0.0216(8) 0.0231(8) 0.0226(8) 0.0018(7) 0.0009(7) -0.0018(6) C9 0.0343(10) 0.0175(8) 0.0252(8) 0.0058(7) -0.0064(7) -0.0042(7) C10 0.0352(10) 0.0179(8) 0.0308(9) -0.0017(7) -0.0089(8) 0.0059(7) C11 0.0216(8) 0.0248(8) 0.0283(9) -0.0054(7) -0.0011(7) 0.0046(7) C12 0.0199(8) 0.0187(7) 0.0220(8) 0.0009(7) -0.0017(6) -0.0015(6) C13 0.0189(7) 0.0160(7) 0.0204(7) -0.0016(6) 0.0038(6) 0.0009(6) C14 0.0255(8) 0.0225(8) 0.0211(8) -0.0012(7) 0.0006(7) -0.0004(7) C15 0.0271(9) 0.0234(8) 0.0321(9) -0.0080(8) 0.0040(8) -0.0085(7) C16 0.0374(10) 0.0198(8) 0.0350(10) 0.0025(8) 0.0078(8) -0.0083(7) C17 0.0423(11) 0.0276(9) 0.0252(9) 0.0087(8) -0.0015(8) -0.0045(8) C18 0.0245(8) 0.0211(8) 0.0245(8) -0.0005(7) -0.0015(7) -0.0037(7) F1 0.0308(5) 0.0203(5) 0.0371(6) -0.0040(4) 0.0028(5) 0.0038(4) F2 0.0258(6) 0.0508(7) 0.0532(7) -0.0055(6) 0.0015(5) 0.0196(5) F3 0.0288(6) 0.0381(6) 0.0348(6) -0.0067(5) -0.0074(5) -0.0063(4) F4 0.0237(5) 0.0338(6) 0.0377(6) -0.0153(5) -0.0048(5) 0.0067(4) F5 0.0304(6) 0.0297(5) 0.0378(6) 0.0110(5) 0.0126(5) -0.0006(4) F6 0.0538(7) 0.0194(5) 0.0400(6) 0.0099(5) 0.0004(5) -0.0059(5) F7 0.0311(6) 0.0319(6) 0.0521(7) -0.0031(5) 0.0129(5) 0.0106(5) F8 0.0248(5) 0.0221(5) 0.0365(6) 0.0038(4) 0.0108(4) 0.0009(4) F9 0.0311(6) 0.0459(6) 0.0268(5) 0.0062(5) -0.0087(4) -0.0117(5) F10 0.0403(6) 0.0408(6) 0.0452(7) -0.0075(6) -0.0029(5) -0.0230(5) F11 0.0705(9) 0.0554(8) 0.0399(7) 0.0290(6) -0.0163(6) -0.0247(7) F12 0.0370(6) 0.0427(6) 0.0280(5) 0.0104(5) -0.0104(5) -0.0159(5) _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 B1 2.0416(18) . ? P1 H1 1.292(18) . ? P1 H2 1.30(2) . ? P1 H3 1.33(2) . ? B1 C13 1.630(2) . ? B1 C1 1.632(2) . ? B1 C7 1.634(2) . ? C1 C2 1.383(2) . ? C1 C6 1.391(2) . ? C2 F1 1.3646(19) . ? C2 C3 1.378(2) . ? C3 F2 1.345(2) . ? C3 C4 1.378(3) . ? C4 C5 1.370(3) . ? C4 H4 0.94(2) . ? C5 F3 1.350(2) . ? C5 C6 1.381(2) . ? C6 F4 1.3496(18) . ? C7 C12 1.387(2) . ? C7 C8 1.389(2) . ? C8 F5 1.3624(19) . ? C8 C9 1.378(2) . ? C9 F6 1.3443(19) . ? C9 C10 1.375(3) . ? C10 C11 1.370(3) . ? C10 H6 0.91(2) . ? C11 F7 1.350(2) . ? C11 C12 1.384(2) . ? C12 F8 1.3544(18) . ? C13 C14 1.389(2) . ? C13 C18 1.391(2) . ? C14 F9 1.3622(19) . ? C14 C15 1.372(2) . ? C15 F10 1.351(2) . ? C15 C16 1.375(3) . ? C16 C17 1.370(3) . ? C16 H5 0.91(2) . ? C17 F11 1.349(2) . ? C17 C18 1.384(2) . ? C18 F12 1.3514(19) . ? 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 B1 P1 H1 113.2(8) . . ? B1 P1 H2 117.1(9) . . ? H1 P1 H2 104.4(12) . . ? B1 P1 H3 114.9(9) . . ? H1 P1 H3 99.9(12) . . ? H2 P1 H3 105.4(12) . . ? C13 B1 C1 112.90(13) . . ? C13 B1 C7 115.32(13) . . ? C1 B1 C7 112.80(13) . . ? C13 B1 P1 106.43(11) . . ? C1 B1 P1 105.17(11) . . ? C7 B1 P1 102.93(10) . . ? C2 C1 C6 113.90(15) . . ? C2 C1 B1 122.26(14) . . ? C6 C1 B1 123.75(14) . . ? F1 C2 C3 117.38(15) . . ? F1 C2 C1 118.50(15) . . ? C3 C2 C1 124.12(16) . . ? F2 C3 C2 119.68(16) . . ? F2 C3 C4 119.94(16) . . ? C2 C3 C4 120.38(16) . . ? C5 C4 C3 117.27(16) . . ? C5 C4 H4 121.1(13) . . ? C3 C4 H4 121.6(13) . . ? F3 C5 C4 119.85(15) . . ? F3 C5 C6 118.67(15) . . ? C4 C5 C6 121.47(16) . . ? F4 C6 C5 116.75(14) . . ? F4 C6 C1 120.39(14) . . ? C5 C6 C1 122.83(15) . . ? C12 C7 C8 113.50(14) . . ? C12 C7 B1 126.19(14) . . ? C8 C7 B1 120.22(14) . . ? F5 C8 C9 117.42(14) . . ? F5 C8 C7 118.07(14) . . ? C9 C8 C7 124.49(16) . . ? F6 C9 C10 120.22(15) . . ? F6 C9 C8 119.48(16) . . ? C10 C9 C8 120.31(15) . . ? C11 C10 C9 117.00(16) . . ? C11 C10 H6 120.9(14) . . ? C9 C10 H6 122.1(13) . . ? F7 C11 C10 119.50(15) . . ? F7 C11 C12 118.62(15) . . ? C10 C11 C12 121.87(16) . . ? F8 C12 C11 116.44(14) . . ? F8 C12 C7 120.70(14) . . ? C11 C12 C7 122.82(15) . . ? C14 C13 C18 113.71(14) . . ? C14 C13 B1 122.30(14) . . ? C18 C13 B1 123.95(14) . . ? F9 C14 C15 117.72(15) . . ? F9 C14 C13 118.13(14) . . ? C15 C14 C13 124.15(16) . . ? F10 C15 C14 119.46(16) . . ? F10 C15 C16 119.83(16) . . ? C14 C15 C16 120.71(16) . . ? C17 C16 C15 117.05(16) . . ? C17 C16 H5 120.6(14) . . ? C15 C16 H5 122.3(14) . . ? F11 C17 C16 119.95(16) . . ? F11 C17 C18 118.39(16) . . ? C16 C17 C18 121.66(17) . . ? F12 C18 C17 116.47(15) . . ? F12 C18 C13 120.82(14) . . ? C17 C18 C13 122.70(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 B1 C1 C2 -70.42(19) . . . . ? C7 B1 C1 C2 156.65(15) . . . . ? P1 B1 C1 C2 45.22(18) . . . . ? C13 B1 C1 C6 105.81(17) . . . . ? C7 B1 C1 C6 -27.1(2) . . . . ? P1 B1 C1 C6 -138.55(14) . . . . ? C6 C1 C2 F1 -178.36(13) . . . . ? B1 C1 C2 F1 -1.8(2) . . . . ? C6 C1 C2 C3 1.8(2) . . . . ? B1 C1 C2 C3 178.34(16) . . . . ? F1 C2 C3 F2 -1.4(2) . . . . ? C1 C2 C3 F2 178.47(16) . . . . ? F1 C2 C3 C4 179.39(15) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? F2 C3 C4 C5 -179.24(16) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C3 C4 C5 F3 -179.62(15) . . . . ? C3 C4 C5 C6 -0.4(3) . . . . ? F3 C5 C6 F4 3.0(2) . . . . ? C4 C5 C6 F4 -176.25(15) . . . . ? F3 C5 C6 C1 -179.16(14) . . . . ? C4 C5 C6 C1 1.6(3) . . . . ? C2 C1 C6 F4 175.59(14) . . . . ? B1 C1 C6 F4 -0.9(2) . . . . ? C2 C1 C6 C5 -2.2(2) . . . . ? B1 C1 C6 C5 -178.68(15) . . . . ? C13 B1 C7 C12 -10.4(2) . . . . ? C1 B1 C7 C12 121.29(16) . . . . ? P1 B1 C7 C12 -125.89(15) . . . . ? C13 B1 C7 C8 173.33(14) . . . . ? C1 B1 C7 C8 -54.92(19) . . . . ? P1 B1 C7 C8 57.89(16) . . . . ? C12 C7 C8 F5 -179.78(14) . . . . ? B1 C7 C8 F5 -3.1(2) . . . . ? C12 C7 C8 C9 -1.5(2) . . . . ? B1 C7 C8 C9 175.18(15) . . . . ? F5 C8 C9 F6 -0.2(2) . . . . ? C7 C8 C9 F6 -178.55(15) . . . . ? F5 C8 C9 C10 179.45(15) . . . . ? C7 C8 C9 C10 1.2(3) . . . . ? F6 C9 C10 C11 179.63(16) . . . . ? C8 C9 C10 C11 -0.1(3) . . . . ? C9 C10 C11 F7 -179.99(15) . . . . ? C9 C10 C11 C12 -0.5(3) . . . . ? F7 C11 C12 F8 1.8(2) . . . . ? C10 C11 C12 F8 -177.70(15) . . . . ? F7 C11 C12 C7 179.57(15) . . . . ? C10 C11 C12 C7 0.1(3) . . . . ? C8 C7 C12 F8 178.57(14) . . . . ? B1 C7 C12 F8 2.1(2) . . . . ? C8 C7 C12 C11 0.9(2) . . . . ? B1 C7 C12 C11 -175.57(15) . . . . ? C1 B1 C13 C14 157.82(14) . . . . ? C7 B1 C13 C14 -70.48(19) . . . . ? P1 B1 C13 C14 42.94(18) . . . . ? C1 B1 C13 C18 -24.5(2) . . . . ? C7 B1 C13 C18 107.17(18) . . . . ? P1 B1 C13 C18 -139.40(14) . . . . ? C18 C13 C14 F9 -178.57(14) . . . . ? B1 C13 C14 F9 -0.7(2) . . . . ? C18 C13 C14 C15 1.6(2) . . . . ? B1 C13 C14 C15 179.51(16) . . . . ? F9 C14 C15 F10 -2.1(2) . . . . ? C13 C14 C15 F10 177.67(15) . . . . ? F9 C14 C15 C16 178.26(16) . . . . ? C13 C14 C15 C16 -1.9(3) . . . . ? F10 C15 C16 C17 -178.64(17) . . . . ? C14 C15 C16 C17 1.0(3) . . . . ? C15 C16 C17 F11 -179.50(17) . . . . ? C15 C16 C17 C18 0.1(3) . . . . ? F11 C17 C18 F12 0.1(3) . . . . ? C16 C17 C18 F12 -179.46(17) . . . . ? F11 C17 C18 C13 179.29(16) . . . . ? C16 C17 C18 C13 -0.3(3) . . . . ? C14 C13 C18 F12 178.61(15) . . . . ? B1 C13 C18 F12 0.8(2) . . . . ? C14 C13 C18 C17 -0.5(2) . . . . ? B1 C13 C18 C17 -178.35(16) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.345 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.049 #===end