# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kehr, Gerald' 'Erker, G.' 'Frohlich, Roland' 'Momming, Cornelia' _publ_contact_author_name 'Kehr, Gerald' _publ_contact_author_email erker@uni-muenster.de _publ_section_title ; The Frustrated Lewis Pair Induced Formation of a Pentafulvene [6+4] Cycloaddition Product ; # Attachment '- 7.cif' data_erk5376 _database_code_depnum_ccdc_archive 'CCDC 798300' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H55 B F10 P' _chemical_formula_weight 971.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.3700(4) _cell_length_b 11.0380(3) _cell_length_c 36.1547(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.729(1) _cell_angle_gamma 90.00 _cell_volume 4936.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7177 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7262 _exptl_absorpt_correction_T_max 0.9245 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26710 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 67.45 _reflns_number_total 8274 _reflns_number_gt 5776 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _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^)+(0.0513P)^2^+2.5972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8274 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.34529(5) 0.88221(6) 0.178392(19) 0.03905(18) Uani 1 1 d . . . B1 B 0.1025(2) 0.7850(3) 0.14832(9) 0.0387(7) Uani 1 1 d . . . C01 C 0.3126(2) 0.7351(2) 0.15942(8) 0.0410(6) Uani 1 1 d . . . H01A H 0.3178 0.7363 0.1324 0.049 Uiso 1 1 calc R . . H01B H 0.3624 0.6736 0.1692 0.049 Uiso 1 1 calc R . . C02 C 0.1954(2) 0.7072(2) 0.17115(8) 0.0428(6) Uani 1 1 d . . . H02A H 0.1887 0.7244 0.1976 0.051 Uiso 1 1 calc R . . H02B H 0.1815 0.6206 0.1675 0.051 Uiso 1 1 calc R . . C21 C 0.4742(2) 0.9515(2) 0.16572(7) 0.0431(7) Uani 1 1 d . . . C22 C 0.5004(2) 1.0604(3) 0.18464(8) 0.0452(7) Uani 1 1 d . . . C23 C 0.5969(2) 1.1179(3) 0.17598(8) 0.0500(7) Uani 1 1 d . . . H23 H 0.6145 1.1905 0.1882 0.060 Uiso 1 1 calc R . . C24 C 0.6674(2) 1.0733(3) 0.15027(8) 0.0503(7) Uani 1 1 d . . . C25 C 0.6396(2) 0.9681(3) 0.13190(8) 0.0516(7) Uani 1 1 d . . . H25 H 0.6869 0.9371 0.1141 0.062 Uiso 1 1 calc R . . C26 C 0.5437(2) 0.9058(3) 0.13878(8) 0.0461(7) Uani 1 1 d . . . C27 C 0.4297(2) 1.1206(3) 0.21286(9) 0.0563(8) Uani 1 1 d . . . H27A H 0.4392 1.0805 0.2366 0.084 Uiso 1 1 calc R . . H27B H 0.3547 1.1148 0.2050 0.084 Uiso 1 1 calc R . . H27C H 0.4499 1.2052 0.2152 0.084 Uiso 1 1 calc R . . C28 C 0.7714(3) 1.1397(3) 0.14168(10) 0.0680(9) Uani 1 1 d . . . H28A H 0.7568 1.2029 0.1237 0.102 Uiso 1 1 calc R . . H28B H 0.8235 1.0831 0.1317 0.102 Uiso 1 1 calc R . . H28C H 0.8006 1.1756 0.1642 0.102 Uiso 1 1 calc R . . C29 C 0.5230(3) 0.7932(3) 0.11578(9) 0.0618(9) Uani 1 1 d . . . H29A H 0.5830 0.7806 0.0992 0.093 Uiso 1 1 calc R . . H29B H 0.4568 0.8034 0.1015 0.093 Uiso 1 1 calc R . . H29C H 0.5161 0.7237 0.1320 0.093 Uiso 1 1 calc R . . C31 C 0.3560(2) 0.8578(2) 0.22876(8) 0.0431(6) Uani 1 1 d . . . C32 C 0.4502(2) 0.7965(3) 0.24169(8) 0.0471(7) Uani 1 1 d . . . C33 C 0.4645(3) 0.7805(3) 0.27956(8) 0.0521(8) Uani 1 1 d . . . H33 H 0.5275 0.7410 0.2880 0.063 Uiso 1 1 calc R . . C34 C 0.3917(3) 0.8190(3) 0.30535(8) 0.0512(8) Uani 1 1 d . . . C35 C 0.2992(2) 0.8758(3) 0.29214(8) 0.0513(7) Uani 1 1 d . . . H35 H 0.2474 0.9015 0.3093 0.062 Uiso 1 1 calc R . . C36 C 0.2792(2) 0.8967(3) 0.25467(8) 0.0466(7) Uani 1 1 d . . . C37 C 0.5388(2) 0.7483(3) 0.21760(9) 0.0638(9) Uani 1 1 d . . . H37A H 0.5880 0.8135 0.2115 0.096 Uiso 1 1 calc R . . H37B H 0.5074 0.7151 0.1951 0.096 Uiso 1 1 calc R . . H37C H 0.5781 0.6853 0.2308 0.096 Uiso 1 1 calc R . . C38 C 0.4127(3) 0.8033(3) 0.34624(9) 0.0724(10) Uani 1 1 d . . . H38A H 0.4250 0.7183 0.3516 0.109 Uiso 1 1 calc R . . H38B H 0.3506 0.8317 0.3599 0.109 Uiso 1 1 calc R . . H38C H 0.4760 0.8498 0.3535 0.109 Uiso 1 1 calc R . . C39 C 0.1763(2) 0.9635(3) 0.24495(9) 0.0638(9) Uani 1 1 d . . . H39A H 0.1279 0.9613 0.2658 0.096 Uiso 1 1 calc R . . H39B H 0.1417 0.9252 0.2238 0.096 Uiso 1 1 calc R . . H39C H 0.1931 1.0471 0.2390 0.096 Uiso 1 1 calc R . . C41 C 0.0008(2) 0.7996(2) 0.17837(7) 0.0398(6) Uani 1 1 d . . . C42 C -0.0449(2) 0.9044(3) 0.19245(8) 0.0444(7) Uani 1 1 d . . . F42 F -0.01009(13) 1.01530(14) 0.18104(5) 0.0568(4) Uani 1 1 d . . . C43 C -0.1241(2) 0.9079(3) 0.21851(8) 0.0529(8) Uani 1 1 d . . . F43 F -0.16185(14) 1.01470(19) 0.23077(5) 0.0756(6) Uani 1 1 d . . . C44 C -0.1636(2) 0.8025(4) 0.23264(8) 0.0579(9) Uani 1 1 d . . . F44 F -0.23906(14) 0.8031(2) 0.25922(5) 0.0805(6) Uani 1 1 d . . . C45 C -0.1240(2) 0.6947(3) 0.21975(8) 0.0541(8) Uani 1 1 d . . . F45 F -0.15943(16) 0.5890(2) 0.23341(5) 0.0802(6) Uani 1 1 d . . . C46 C -0.0446(2) 0.6960(3) 0.19343(8) 0.0460(7) Uani 1 1 d . . . F46 F -0.01008(14) 0.58506(15) 0.18210(5) 0.0609(5) Uani 1 1 d . . . C51 C 0.0472(2) 0.7103(2) 0.11300(7) 0.0402(6) Uani 1 1 d . . . C52 C 0.0908(2) 0.6115(3) 0.09503(8) 0.0510(7) Uani 1 1 d . . . F52 F 0.19230(15) 0.57227(16) 0.10418(5) 0.0712(5) Uani 1 1 d . . . C53 C 0.0402(3) 0.5481(3) 0.06719(9) 0.0662(9) Uani 1 1 d . . . F53 F 0.0898(2) 0.45237(19) 0.05156(7) 0.1047(8) Uani 1 1 d . . . C54 C -0.0602(3) 0.5835(3) 0.05511(9) 0.0699(10) Uani 1 1 d . . . F54 F -0.1110(2) 0.5224(2) 0.02772(6) 0.1085(8) Uani 1 1 d . . . C55 C -0.1074(3) 0.6821(3) 0.07098(9) 0.0589(8) Uani 1 1 d . . . F55 F -0.20511(16) 0.7205(2) 0.05846(6) 0.0873(7) Uani 1 1 d . . . C56 C -0.0536(2) 0.7422(3) 0.09864(8) 0.0475(7) Uani 1 1 d . . . F56 F -0.10426(13) 0.84196(16) 0.11182(5) 0.0611(5) Uani 1 1 d . . . C1 C 0.1993(2) 0.9206(2) 0.09337(7) 0.0368(6) Uani 1 1 d . . . H1 H 0.2411 0.8459 0.0886 0.044 Uiso 1 1 calc R . . C2 C 0.1174(2) 0.9426(3) 0.06086(7) 0.0450(7) Uani 1 1 d . . . H2 H 0.0640 0.8764 0.0579 0.054 Uiso 1 1 calc R . . C3 C 0.0658(3) 1.0656(3) 0.06468(9) 0.0607(9) Uani 1 1 d . . . H3 H 0.0007 1.0809 0.0770 0.073 Uiso 1 1 calc R . . C4 C 0.1248(3) 1.1485(3) 0.04843(10) 0.0719(10) Uani 1 1 d . . . H4 H 0.1076 1.2314 0.0473 0.086 Uiso 1 1 calc R . . C5 C 0.2241(3) 1.0916(3) 0.03180(9) 0.0590(8) Uani 1 1 d . . . H5 H 0.2451 1.1305 0.0083 0.071 Uiso 1 1 calc R . . C6 C 0.3180(3) 1.0900(3) 0.06093(9) 0.0593(9) Uani 1 1 d . . . C7 C 0.2760(2) 1.0287(2) 0.09540(8) 0.0441(7) Uani 1 1 d . . . C8 C 0.2929(2) 1.0628(2) 0.12992(8) 0.0439(7) Uani 1 1 d . . . H8 H 0.3352 1.1303 0.1366 0.053 Uiso 1 1 calc R . . C9 C 0.2378(2) 0.9827(2) 0.15749(7) 0.0381(6) Uani 1 1 d . . . H9 H 0.2025 1.0317 0.1768 0.046 Uiso 1 1 calc R . . C10 C 0.1511(2) 0.9146(2) 0.13295(7) 0.0369(6) Uani 1 1 d . . . H10 H 0.0881 0.9698 0.1321 0.044 Uiso 1 1 calc R . . C11 C 0.1843(2) 0.9630(3) 0.02646(8) 0.0484(7) Uani 1 1 d . . . C12 C 0.1994(3) 0.8884(3) -0.00152(8) 0.0581(8) Uani 1 1 d . . . C13 C 0.3538(4) 1.2205(4) 0.06961(11) 0.0968(15) Uani 1 1 d . . . H13A H 0.2952 1.2636 0.0814 0.145 Uiso 1 1 calc R . . H13B H 0.3725 1.2614 0.0468 0.145 Uiso 1 1 calc R . . H13C H 0.4163 1.2189 0.0861 0.145 Uiso 1 1 calc R . . C14 C 0.4146(3) 1.0196(4) 0.04581(10) 0.0809(12) Uani 1 1 d . . . H14A H 0.4732 1.0208 0.0639 0.121 Uiso 1 1 calc R . . H14B H 0.4383 1.0570 0.0230 0.121 Uiso 1 1 calc R . . H14C H 0.3933 0.9365 0.0410 0.121 Uiso 1 1 calc R . . C15 C 0.2652(3) 0.9211(4) -0.03519(9) 0.0911(13) Uani 1 1 d . . . H15A H 0.2908 1.0038 -0.0329 0.137 Uiso 1 1 calc R . . H15B H 0.2204 0.9135 -0.0573 0.137 Uiso 1 1 calc R . . H15C H 0.3266 0.8667 -0.0369 0.137 Uiso 1 1 calc R . . C16 C 0.1523(3) 0.7625(3) -0.00310(10) 0.0743(10) Uani 1 1 d . . . H16A H 0.1133 0.7464 0.0195 0.111 Uiso 1 1 calc R . . H16B H 0.2101 0.7039 -0.0056 0.111 Uiso 1 1 calc R . . H16C H 0.1032 0.7563 -0.0241 0.111 Uiso 1 1 calc R . . C101 C 0.6717(5) 1.4669(5) 0.10225(14) 0.1150(17) Uani 1 1 d . . . H101 H 0.7092 1.4702 0.0798 0.138 Uiso 1 1 calc R . . C102 C 0.5658(5) 1.4398(4) 0.10256(14) 0.1134(19) Uani 1 1 d . . . H102 H 0.5290 1.4248 0.0801 0.136 Uiso 1 1 calc R . . C103 C 0.5111(4) 1.4339(4) 0.13493(18) 0.1105(16) Uani 1 1 d . . . H103 H 0.4371 1.4147 0.1349 0.133 Uiso 1 1 calc R . . C104 C 0.5648(6) 1.4563(4) 0.16727(15) 0.1089(17) Uani 1 1 d . . . H104 H 0.5277 1.4525 0.1898 0.131 Uiso 1 1 calc R . . C105 C 0.6706(5) 1.4837(4) 0.16720(14) 0.1093(17) Uani 1 1 d . . . H105 H 0.7073 1.4987 0.1897 0.131 Uiso 1 1 calc R . . C106 C 0.7243(4) 1.4897(4) 0.13506(16) 0.1109(16) Uani 1 1 d . . . H106 H 0.7981 1.5097 0.1352 0.133 Uiso 1 1 calc R . . C201 C -0.4433(8) 0.4119(8) -0.01706(17) 0.139(2) Uani 1 1 d . . . H201 H -0.4041 0.3505 -0.0289 0.167 Uiso 1 1 calc R . . C202 C -0.3909(6) 0.5104(11) -0.0031(2) 0.144(3) Uani 1 1 d . . . H202 H -0.3155 0.5173 -0.0053 0.173 Uiso 1 1 calc R . . C203 C -0.4477(8) 0.5981(8) 0.0138(2) 0.139(3) Uani 1 1 d . . . H203 H -0.4118 0.6665 0.0235 0.167 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0327(4) 0.0430(4) 0.0415(4) -0.0026(3) 0.0022(3) 0.0013(3) B1 0.0332(16) 0.0393(17) 0.0436(17) -0.0021(14) 0.0031(13) -0.0021(13) C01 0.0342(14) 0.0409(15) 0.0480(16) -0.0006(12) 0.0004(12) 0.0066(12) C02 0.0390(15) 0.0401(15) 0.0495(16) 0.0025(13) 0.0041(13) -0.0018(12) C21 0.0352(15) 0.0503(17) 0.0438(16) -0.0022(13) -0.0004(12) 0.0001(12) C22 0.0372(15) 0.0543(17) 0.0440(16) 0.0008(13) -0.0007(13) 0.0016(13) C23 0.0464(17) 0.0532(17) 0.0502(17) 0.0009(14) -0.0074(14) -0.0056(14) C24 0.0375(16) 0.0655(19) 0.0480(17) 0.0084(15) -0.0022(14) -0.0069(14) C25 0.0381(16) 0.068(2) 0.0485(17) 0.0040(15) 0.0060(13) 0.0015(14) C26 0.0365(15) 0.0550(17) 0.0469(17) 0.0000(14) 0.0061(13) 0.0021(13) C27 0.0521(18) 0.0536(18) 0.063(2) -0.0153(15) 0.0009(15) -0.0057(15) C28 0.0476(19) 0.087(2) 0.069(2) 0.0095(19) 0.0006(16) -0.0184(18) C29 0.0515(19) 0.067(2) 0.067(2) -0.0168(17) 0.0185(16) 0.0008(16) C31 0.0390(15) 0.0450(16) 0.0453(16) -0.0011(13) 0.0028(13) -0.0027(12) C32 0.0410(16) 0.0509(16) 0.0493(17) -0.0017(14) -0.0073(13) -0.0004(13) C33 0.0529(18) 0.0494(17) 0.0538(19) 0.0034(14) -0.0085(15) 0.0001(14) C34 0.063(2) 0.0432(16) 0.0475(17) 0.0028(14) -0.0067(15) -0.0085(14) C35 0.0576(19) 0.0529(17) 0.0436(17) -0.0046(14) 0.0091(14) -0.0096(15) C36 0.0416(16) 0.0528(17) 0.0455(17) -0.0032(14) 0.0039(13) -0.0056(13) C37 0.0479(19) 0.081(2) 0.062(2) -0.0026(18) -0.0083(16) 0.0221(17) C38 0.099(3) 0.069(2) 0.0492(19) 0.0061(17) -0.0082(19) -0.008(2) C39 0.0476(19) 0.094(3) 0.0502(19) -0.0020(18) 0.0099(15) 0.0130(17) C41 0.0333(14) 0.0489(16) 0.0373(15) -0.0008(12) 0.0018(12) -0.0035(12) C42 0.0337(14) 0.0522(17) 0.0473(17) -0.0040(14) 0.0037(13) -0.0021(13) F42 0.0504(10) 0.0486(10) 0.0717(11) -0.0078(8) 0.0145(9) 0.0070(8) C43 0.0338(15) 0.077(2) 0.0484(17) -0.0161(16) 0.0056(13) 0.0034(15) F43 0.0519(11) 0.0987(15) 0.0766(13) -0.0267(11) 0.0170(10) 0.0146(10) C44 0.0306(15) 0.104(3) 0.0394(17) -0.0083(18) 0.0063(13) -0.0083(17) F44 0.0441(10) 0.1438(19) 0.0542(11) -0.0098(12) 0.0183(9) -0.0165(11) C45 0.0433(17) 0.077(2) 0.0422(17) 0.0037(16) 0.0043(14) -0.0243(16) F45 0.0722(13) 0.1036(16) 0.0652(12) 0.0139(11) 0.0132(10) -0.0425(12) C46 0.0421(16) 0.0530(18) 0.0430(16) -0.0023(14) 0.0024(13) -0.0075(13) F46 0.0628(11) 0.0502(10) 0.0698(11) 0.0052(9) 0.0110(9) -0.0142(8) C51 0.0418(16) 0.0354(14) 0.0435(15) 0.0016(12) 0.0060(12) -0.0045(12) C52 0.0587(19) 0.0430(16) 0.0513(18) -0.0029(14) 0.0044(15) -0.0020(14) F52 0.0722(13) 0.0609(11) 0.0808(13) -0.0150(10) 0.0061(10) 0.0210(9) C53 0.093(3) 0.0438(18) 0.062(2) -0.0168(16) 0.011(2) -0.0087(18) F53 0.153(2) 0.0659(14) 0.0956(16) -0.0396(12) 0.0044(15) 0.0108(14) C54 0.084(3) 0.069(2) 0.057(2) -0.0135(18) -0.0048(19) -0.034(2) F54 0.132(2) 0.1086(18) 0.0845(15) -0.0380(14) -0.0198(14) -0.0439(16) C55 0.054(2) 0.067(2) 0.0556(19) 0.0009(17) -0.0095(16) -0.0159(16) F55 0.0606(12) 0.1229(18) 0.0777(13) -0.0007(12) -0.0225(11) -0.0207(12) C56 0.0438(16) 0.0504(17) 0.0485(17) -0.0023(14) 0.0064(14) -0.0076(14) F56 0.0466(10) 0.0712(12) 0.0652(11) -0.0091(9) -0.0072(8) 0.0105(8) C1 0.0337(14) 0.0354(14) 0.0413(15) 0.0009(11) 0.0047(12) 0.0000(11) C2 0.0413(16) 0.0480(16) 0.0456(16) 0.0059(13) 0.0002(13) -0.0035(13) C3 0.0533(19) 0.070(2) 0.059(2) 0.0088(17) -0.0037(16) 0.0152(17) C4 0.091(3) 0.052(2) 0.073(2) 0.0100(18) -0.014(2) 0.0095(19) C5 0.072(2) 0.0557(19) 0.0494(18) 0.0152(15) -0.0003(16) -0.0153(17) C6 0.060(2) 0.066(2) 0.0513(18) 0.0084(16) 0.0020(16) -0.0263(16) C7 0.0384(15) 0.0466(16) 0.0473(17) 0.0072(13) 0.0011(13) -0.0066(12) C8 0.0413(16) 0.0385(15) 0.0518(17) 0.0012(13) -0.0020(13) -0.0075(12) C9 0.0336(14) 0.0391(14) 0.0415(15) -0.0032(12) 0.0045(12) 0.0010(11) C10 0.0317(13) 0.0376(14) 0.0414(15) 0.0006(11) 0.0021(11) 0.0026(11) C11 0.0449(17) 0.0587(18) 0.0415(16) 0.0088(14) -0.0043(13) -0.0063(14) C12 0.0572(19) 0.074(2) 0.0433(17) 0.0009(16) -0.0020(15) -0.0087(17) C13 0.138(4) 0.084(3) 0.068(2) 0.020(2) -0.007(2) -0.064(3) C14 0.046(2) 0.140(4) 0.057(2) 0.013(2) 0.0104(17) -0.022(2) C15 0.094(3) 0.132(4) 0.047(2) -0.011(2) 0.012(2) -0.023(3) C16 0.083(3) 0.075(2) 0.065(2) -0.0155(19) -0.0044(19) -0.010(2) C101 0.145(5) 0.112(4) 0.088(3) 0.008(3) 0.005(3) -0.048(4) C102 0.173(6) 0.089(3) 0.077(3) 0.020(3) -0.036(4) -0.051(3) C103 0.113(4) 0.079(3) 0.139(5) 0.005(3) -0.009(4) -0.031(3) C104 0.166(6) 0.069(3) 0.093(4) -0.008(2) 0.026(4) -0.026(3) C105 0.162(5) 0.093(3) 0.071(3) 0.013(3) -0.031(3) -0.030(3) C106 0.115(4) 0.106(4) 0.112(4) 0.017(3) -0.024(3) -0.028(3) C201 0.141(7) 0.158(7) 0.118(5) 0.045(4) -0.022(4) -0.002(5) C202 0.098(5) 0.200(8) 0.134(6) 0.089(6) -0.025(5) -0.022(6) C203 0.142(7) 0.151(6) 0.124(5) 0.067(5) -0.053(5) -0.046(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 C01 1.806(3) . ? P1 C21 1.832(3) . ? P1 C31 1.844(3) . ? P1 C9 1.882(3) . ? B1 C02 1.648(4) . ? B1 C10 1.651(4) . ? B1 C51 1.660(4) . ? B1 C41 1.680(4) . ? C01 C02 1.546(4) . ? C01 H01A 0.9800 . ? C01 H01B 0.9800 . ? C02 H02A 0.9800 . ? C02 H02B 0.9800 . ? C21 C26 1.401(4) . ? C21 C22 1.419(4) . ? C22 C23 1.391(4) . ? C22 C27 1.506(4) . ? C23 C24 1.375(4) . ? C23 H23 0.9400 . ? C24 C25 1.379(4) . ? C24 C28 1.516(4) . ? C25 C26 1.396(4) . ? C25 H25 0.9400 . ? C26 C29 1.515(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C31 C36 1.410(4) . ? C31 C32 1.421(4) . ? C32 C33 1.390(4) . ? C32 C37 1.505(4) . ? C33 C34 1.372(4) . ? C33 H33 0.9400 . ? C34 C35 1.385(4) . ? C34 C38 1.508(4) . ? C35 C36 1.393(4) . ? C35 H35 0.9400 . ? C36 C39 1.509(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C41 C42 1.387(4) . ? C41 C46 1.388(4) . ? C42 F42 1.363(3) . ? C42 C43 1.368(4) . ? C43 F43 1.345(3) . ? C43 C44 1.363(5) . ? C44 F44 1.348(3) . ? C44 C45 1.371(5) . ? C45 F45 1.343(3) . ? C45 C46 1.377(4) . ? C46 F46 1.361(3) . ? C51 C52 1.382(4) . ? C51 C56 1.390(4) . ? C52 F52 1.365(3) . ? C52 C53 1.370(4) . ? C53 F53 1.349(4) . ? C53 C54 1.369(5) . ? C54 F54 1.347(3) . ? C54 C55 1.365(5) . ? C55 F55 1.353(4) . ? C55 C56 1.366(4) . ? C56 F56 1.356(3) . ? C1 C7 1.526(4) . ? C1 C10 1.558(4) . ? C1 C2 1.561(4) . ? C1 H1 0.9900 . ? C2 C3 1.507(4) . ? C2 C11 1.520(4) . ? C2 H2 0.9900 . ? C3 C4 1.313(5) . ? C3 H3 0.9400 . ? C4 C5 1.512(5) . ? C4 H4 0.9400 . ? C5 C11 1.514(4) . ? C5 C6 1.558(4) . ? C5 H5 0.9900 . ? C6 C7 1.516(4) . ? C6 C14 1.532(5) . ? C6 C13 1.538(5) . ? C7 C8 1.318(4) . ? C8 C9 1.502(4) . ? C8 H8 0.9400 . ? C9 C10 1.574(3) . ? C9 H9 0.9900 . ? C10 H10 0.9900 . ? C11 C12 1.319(4) . ? C12 C16 1.508(5) . ? C12 C15 1.516(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C101 C102 1.344(7) . ? C101 C106 1.369(6) . ? C101 H101 0.9400 . ? C102 C103 1.361(7) . ? C102 H102 0.9400 . ? C103 C104 1.360(7) . ? C103 H103 0.9400 . ? C104 C105 1.343(7) . ? C104 H104 0.9400 . ? C105 C106 1.348(7) . ? C105 H105 0.9400 . ? C106 H106 0.9400 . ? C201 C203 1.359(9) 3_465 ? C201 C202 1.359(9) . ? C201 H201 0.9400 . ? C202 C203 1.349(9) . ? C202 H202 0.9400 . ? C203 C201 1.359(9) 3_465 ? C203 H203 0.9400 . ? 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 C01 P1 C21 118.13(13) . . ? C01 P1 C31 104.85(13) . . ? C21 P1 C31 104.85(12) . . ? C01 P1 C9 102.93(12) . . ? C21 P1 C9 105.44(12) . . ? C31 P1 C9 121.61(12) . . ? C02 B1 C10 111.4(2) . . ? C02 B1 C51 113.9(2) . . ? C10 B1 C51 108.6(2) . . ? C02 B1 C41 104.4(2) . . ? C10 B1 C41 114.4(2) . . ? C51 B1 C41 103.9(2) . . ? C02 C01 P1 106.31(18) . . ? C02 C01 H01A 110.5 . . ? P1 C01 H01A 110.5 . . ? C02 C01 H01B 110.5 . . ? P1 C01 H01B 110.5 . . ? H01A C01 H01B 108.7 . . ? C01 C02 B1 114.2(2) . . ? C01 C02 H02A 108.7 . . ? B1 C02 H02A 108.7 . . ? C01 C02 H02B 108.7 . . ? B1 C02 H02B 108.7 . . ? H02A C02 H02B 107.6 . . ? C26 C21 C22 120.1(3) . . ? C26 C21 P1 124.6(2) . . ? C22 C21 P1 115.3(2) . . ? C23 C22 C21 118.0(3) . . ? C23 C22 C27 117.2(3) . . ? C21 C22 C27 124.7(3) . . ? C24 C23 C22 122.8(3) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C23 C24 C25 118.1(3) . . ? C23 C24 C28 120.8(3) . . ? C25 C24 C28 121.1(3) . . ? C24 C25 C26 122.4(3) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C25 C26 C21 118.5(3) . . ? C25 C26 C29 116.3(3) . . ? C21 C26 C29 125.2(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C36 C31 C32 118.9(2) . . ? C36 C31 P1 124.8(2) . . ? C32 C31 P1 116.3(2) . . ? C33 C32 C31 118.6(3) . . ? C33 C32 C37 116.2(3) . . ? C31 C32 C37 125.3(3) . . ? C34 C33 C32 123.6(3) . . ? C34 C33 H33 118.2 . . ? C32 C33 H33 118.2 . . ? C33 C34 C35 116.9(3) . . ? C33 C34 C38 121.6(3) . . ? C35 C34 C38 121.4(3) . . ? C34 C35 C36 123.1(3) . . ? C34 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C31 118.9(3) . . ? C35 C36 C39 116.5(3) . . ? C31 C36 C39 124.6(2) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C46 112.0(2) . . ? C42 C41 B1 129.0(2) . . ? C46 C41 B1 119.0(2) . . ? F42 C42 C43 114.5(3) . . ? F42 C42 C41 120.4(2) . . ? C43 C42 C41 125.1(3) . . ? F43 C43 C44 119.8(3) . . ? F43 C43 C42 120.4(3) . . ? C44 C43 C42 119.8(3) . . ? F44 C44 C43 121.2(3) . . ? F44 C44 C45 120.0(3) . . ? C43 C44 C45 118.8(3) . . ? F45 C45 C44 120.6(3) . . ? F45 C45 C46 120.1(3) . . ? C44 C45 C46 119.2(3) . . ? F46 C46 C45 115.4(3) . . ? F46 C46 C41 119.5(2) . . ? C45 C46 C41 125.1(3) . . ? C52 C51 C56 112.2(2) . . ? C52 C51 B1 126.5(2) . . ? C56 C51 B1 121.3(2) . . ? F52 C52 C53 115.2(3) . . ? F52 C52 C51 120.0(2) . . ? C53 C52 C51 124.8(3) . . ? F53 C53 C54 120.4(3) . . ? F53 C53 C52 120.1(3) . . ? C54 C53 C52 119.5(3) . . ? F54 C54 C55 120.7(4) . . ? F54 C54 C53 120.3(4) . . ? C55 C54 C53 119.0(3) . . ? F55 C55 C54 119.6(3) . . ? F55 C55 C56 121.2(3) . . ? C54 C55 C56 119.2(3) . . ? F56 C56 C55 115.4(3) . . ? F56 C56 C51 119.4(2) . . ? C55 C56 C51 125.2(3) . . ? C7 C1 C10 103.5(2) . . ? C7 C1 C2 108.2(2) . . ? C10 C1 C2 116.5(2) . . ? C7 C1 H1 109.4 . . ? C10 C1 H1 109.4 . . ? C2 C1 H1 109.4 . . ? C3 C2 C11 100.2(2) . . ? C3 C2 C1 110.0(2) . . ? C11 C2 C1 106.5(2) . . ? C3 C2 H2 113.1 . . ? C11 C2 H2 113.1 . . ? C1 C2 H2 113.1 . . ? C4 C3 C2 110.4(3) . . ? C4 C3 H3 124.8 . . ? C2 C3 H3 124.8 . . ? C3 C4 C5 110.4(3) . . ? C3 C4 H4 124.8 . . ? C5 C4 H4 124.8 . . ? C4 C5 C11 100.1(3) . . ? C4 C5 C6 109.8(3) . . ? C11 C5 C6 108.3(2) . . ? C4 C5 H5 112.6 . . ? C11 C5 H5 112.6 . . ? C6 C5 H5 112.6 . . ? C7 C6 C14 110.1(3) . . ? C7 C6 C13 110.6(3) . . ? C14 C6 C13 108.9(3) . . ? C7 C6 C5 107.5(2) . . ? C14 C6 C5 110.0(3) . . ? C13 C6 C5 109.7(3) . . ? C8 C7 C6 126.8(3) . . ? C8 C7 C1 111.1(2) . . ? C6 C7 C1 122.0(2) . . ? C7 C8 C9 113.1(2) . . ? C7 C8 H8 123.4 . . ? C9 C8 H8 123.4 . . ? C8 C9 C10 102.6(2) . . ? C8 C9 P1 106.79(17) . . ? C10 C9 P1 114.66(17) . . ? C8 C9 H9 110.8 . . ? C10 C9 H9 110.8 . . ? P1 C9 H9 110.8 . . ? C1 C10 C9 103.40(19) . . ? C1 C10 B1 119.4(2) . . ? C9 C10 B1 118.2(2) . . ? C1 C10 H10 104.7 . . ? C9 C10 H10 104.7 . . ? B1 C10 H10 104.7 . . ? C12 C11 C5 129.3(3) . . ? C12 C11 C2 128.3(3) . . ? C5 C11 C2 102.4(2) . . ? C11 C12 C16 123.1(3) . . ? C11 C12 C15 123.4(3) . . ? C16 C12 C15 113.6(3) . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 C14 H14A 109.5 . . ? C6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C102 C101 C106 119.1(5) . . ? C102 C101 H101 120.5 . . ? C106 C101 H101 120.5 . . ? C101 C102 C103 120.9(5) . . ? C101 C102 H102 119.6 . . ? C103 C102 H102 119.6 . . ? C104 C103 C102 119.2(5) . . ? C104 C103 H103 120.4 . . ? C102 C103 H103 120.4 . . ? C105 C104 C103 120.3(5) . . ? C105 C104 H104 119.9 . . ? C103 C104 H104 119.9 . . ? C104 C105 C106 120.3(5) . . ? C104 C105 H105 119.9 . . ? C106 C105 H105 119.9 . . ? C105 C106 C101 120.3(5) . . ? C105 C106 H106 119.9 . . ? C101 C106 H106 119.9 . . ? C203 C201 C202 120.2(7) 3_465 . ? C203 C201 H201 119.9 3_465 . ? C202 C201 H201 119.9 . . ? C203 C202 C201 119.6(7) . . ? C203 C202 H202 120.2 . . ? C201 C202 H202 120.2 . . ? C202 C203 C201 120.2(7) . 3_465 ? C202 C203 H203 119.9 . . ? C201 C203 H203 119.9 3_465 . ? 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 C21 P1 C01 C02 -173.67(17) . . . . ? C31 P1 C01 C02 70.07(19) . . . . ? C9 P1 C01 C02 -58.04(19) . . . . ? P1 C01 C02 B1 74.0(2) . . . . ? C10 B1 C02 C01 -26.4(3) . . . . ? C51 B1 C02 C01 96.9(3) . . . . ? C41 B1 C02 C01 -150.4(2) . . . . ? C01 P1 C21 C26 8.3(3) . . . . ? C31 P1 C21 C26 124.6(2) . . . . ? C9 P1 C21 C26 -106.0(2) . . . . ? C01 P1 C21 C22 -173.34(19) . . . . ? C31 P1 C21 C22 -57.1(2) . . . . ? C9 P1 C21 C22 72.4(2) . . . . ? C26 C21 C22 C23 -1.0(4) . . . . ? P1 C21 C22 C23 -179.4(2) . . . . ? C26 C21 C22 C27 177.3(3) . . . . ? P1 C21 C22 C27 -1.2(4) . . . . ? C21 C22 C23 C24 -0.5(4) . . . . ? C27 C22 C23 C24 -178.9(3) . . . . ? C22 C23 C24 C25 1.3(4) . . . . ? C22 C23 C24 C28 179.7(3) . . . . ? C23 C24 C25 C26 -0.6(4) . . . . ? C28 C24 C25 C26 -179.0(3) . . . . ? C24 C25 C26 C21 -0.8(4) . . . . ? C24 C25 C26 C29 178.6(3) . . . . ? C22 C21 C26 C25 1.6(4) . . . . ? P1 C21 C26 C25 179.9(2) . . . . ? C22 C21 C26 C29 -177.8(3) . . . . ? P1 C21 C26 C29 0.5(4) . . . . ? C01 P1 C31 C36 -106.9(2) . . . . ? C21 P1 C31 C36 128.0(2) . . . . ? C9 P1 C31 C36 8.9(3) . . . . ? C01 P1 C31 C32 74.1(2) . . . . ? C21 P1 C31 C32 -51.0(2) . . . . ? C9 P1 C31 C32 -170.12(19) . . . . ? C36 C31 C32 C33 -1.8(4) . . . . ? P1 C31 C32 C33 177.2(2) . . . . ? C36 C31 C32 C37 179.3(3) . . . . ? P1 C31 C32 C37 -1.6(4) . . . . ? C31 C32 C33 C34 1.0(4) . . . . ? C37 C32 C33 C34 179.9(3) . . . . ? C32 C33 C34 C35 0.6(4) . . . . ? C32 C33 C34 C38 -177.9(3) . . . . ? C33 C34 C35 C36 -1.3(4) . . . . ? C38 C34 C35 C36 177.1(3) . . . . ? C34 C35 C36 C31 0.5(4) . . . . ? C34 C35 C36 C39 -178.0(3) . . . . ? C32 C31 C36 C35 1.2(4) . . . . ? P1 C31 C36 C35 -177.8(2) . . . . ? C32 C31 C36 C39 179.4(3) . . . . ? P1 C31 C36 C39 0.4(4) . . . . ? C02 B1 C41 C42 120.2(3) . . . . ? C10 B1 C41 C42 -1.9(4) . . . . ? C51 B1 C41 C42 -120.2(3) . . . . ? C02 B1 C41 C46 -56.8(3) . . . . ? C10 B1 C41 C46 -178.9(2) . . . . ? C51 B1 C41 C46 62.8(3) . . . . ? C46 C41 C42 F42 179.6(2) . . . . ? B1 C41 C42 F42 2.4(4) . . . . ? C46 C41 C42 C43 1.0(4) . . . . ? B1 C41 C42 C43 -176.2(3) . . . . ? F42 C42 C43 F43 0.3(4) . . . . ? C41 C42 C43 F43 178.9(2) . . . . ? F42 C42 C43 C44 -178.5(2) . . . . ? C41 C42 C43 C44 0.2(4) . . . . ? F43 C43 C44 F44 -1.0(4) . . . . ? C42 C43 C44 F44 177.8(2) . . . . ? F43 C43 C44 C45 -180.0(3) . . . . ? C42 C43 C44 C45 -1.2(4) . . . . ? F44 C44 C45 F45 -0.2(4) . . . . ? C43 C44 C45 F45 178.8(3) . . . . ? F44 C44 C45 C46 -178.0(2) . . . . ? C43 C44 C45 C46 1.0(4) . . . . ? F45 C45 C46 F46 2.3(4) . . . . ? C44 C45 C46 F46 -179.8(2) . . . . ? F45 C45 C46 C41 -177.6(2) . . . . ? C44 C45 C46 C41 0.2(4) . . . . ? C42 C41 C46 F46 178.9(2) . . . . ? B1 C41 C46 F46 -3.6(4) . . . . ? C42 C41 C46 C45 -1.2(4) . . . . ? B1 C41 C46 C45 176.3(3) . . . . ? C02 B1 C51 C52 -20.4(4) . . . . ? C10 B1 C51 C52 104.4(3) . . . . ? C41 B1 C51 C52 -133.4(3) . . . . ? C02 B1 C51 C56 158.2(2) . . . . ? C10 B1 C51 C56 -77.0(3) . . . . ? C41 B1 C51 C56 45.3(3) . . . . ? C56 C51 C52 F52 176.2(2) . . . . ? B1 C51 C52 F52 -5.1(4) . . . . ? C56 C51 C52 C53 -2.3(4) . . . . ? B1 C51 C52 C53 176.4(3) . . . . ? F52 C52 C53 F53 1.7(5) . . . . ? C51 C52 C53 F53 -179.7(3) . . . . ? F52 C52 C53 C54 -177.6(3) . . . . ? C51 C52 C53 C54 1.0(5) . . . . ? F53 C53 C54 F54 0.6(5) . . . . ? C52 C53 C54 F54 179.9(3) . . . . ? F53 C53 C54 C55 -178.8(3) . . . . ? C52 C53 C54 C55 0.5(5) . . . . ? F54 C54 C55 F55 -1.6(5) . . . . ? C53 C54 C55 F55 177.8(3) . . . . ? F54 C54 C55 C56 -179.9(3) . . . . ? C53 C54 C55 C56 -0.5(5) . . . . ? F55 C55 C56 F56 -0.9(4) . . . . ? C54 C55 C56 F56 177.4(3) . . . . ? F55 C55 C56 C51 -179.3(3) . . . . ? C54 C55 C56 C51 -1.1(5) . . . . ? C52 C51 C56 F56 -176.1(2) . . . . ? B1 C51 C56 F56 5.1(4) . . . . ? C52 C51 C56 C55 2.4(4) . . . . ? B1 C51 C56 C55 -176.4(3) . . . . ? C7 C1 C2 C3 -51.8(3) . . . . ? C10 C1 C2 C3 64.2(3) . . . . ? C7 C1 C2 C11 55.9(3) . . . . ? C10 C1 C2 C11 172.0(2) . . . . ? C11 C2 C3 C4 -24.0(3) . . . . ? C1 C2 C3 C4 87.9(3) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 C11 24.7(3) . . . . ? C3 C4 C5 C6 -89.1(3) . . . . ? C4 C5 C6 C7 53.6(3) . . . . ? C11 C5 C6 C7 -54.7(3) . . . . ? C4 C5 C6 C14 173.5(3) . . . . ? C11 C5 C6 C14 65.1(3) . . . . ? C4 C5 C6 C13 -66.7(4) . . . . ? C11 C5 C6 C13 -175.1(3) . . . . ? C14 C6 C7 C8 102.4(4) . . . . ? C13 C6 C7 C8 -17.9(5) . . . . ? C5 C6 C7 C8 -137.7(3) . . . . ? C14 C6 C7 C1 -82.2(3) . . . . ? C13 C6 C7 C1 157.4(3) . . . . ? C5 C6 C7 C1 37.6(4) . . . . ? C10 C1 C7 C8 13.0(3) . . . . ? C2 C1 C7 C8 137.2(2) . . . . ? C10 C1 C7 C6 -163.0(3) . . . . ? C2 C1 C7 C6 -38.8(3) . . . . ? C6 C7 C8 C9 179.0(3) . . . . ? C1 C7 C8 C9 3.2(3) . . . . ? C7 C8 C9 C10 -17.7(3) . . . . ? C7 C8 C9 P1 103.2(2) . . . . ? C01 P1 C9 C8 -109.63(19) . . . . ? C21 P1 C9 C8 14.8(2) . . . . ? C31 P1 C9 C8 133.62(18) . . . . ? C01 P1 C9 C10 3.3(2) . . . . ? C21 P1 C9 C10 127.73(19) . . . . ? C31 P1 C9 C10 -113.4(2) . . . . ? C7 C1 C10 C9 -22.5(2) . . . . ? C2 C1 C10 C9 -141.1(2) . . . . ? C7 C1 C10 B1 -156.3(2) . . . . ? C2 C1 C10 B1 85.1(3) . . . . ? C8 C9 C10 C1 24.0(2) . . . . ? P1 C9 C10 C1 -91.4(2) . . . . ? C8 C9 C10 B1 158.5(2) . . . . ? P1 C9 C10 B1 43.1(3) . . . . ? C02 B1 C10 C1 92.2(3) . . . . ? C51 B1 C10 C1 -34.0(3) . . . . ? C41 B1 C10 C1 -149.6(2) . . . . ? C02 B1 C10 C9 -35.0(3) . . . . ? C51 B1 C10 C9 -161.2(2) . . . . ? C41 B1 C10 C9 83.2(3) . . . . ? C4 C5 C11 C12 139.2(3) . . . . ? C6 C5 C11 C12 -105.9(4) . . . . ? C4 C5 C11 C2 -38.2(3) . . . . ? C6 C5 C11 C2 76.7(3) . . . . ? C3 C2 C11 C12 -139.4(3) . . . . ? C1 C2 C11 C12 106.0(3) . . . . ? C3 C2 C11 C5 38.1(3) . . . . ? C1 C2 C11 C5 -76.6(3) . . . . ? C5 C11 C12 C16 -178.8(3) . . . . ? C2 C11 C12 C16 -2.0(5) . . . . ? C5 C11 C12 C15 0.9(5) . . . . ? C2 C11 C12 C15 177.7(3) . . . . ? C106 C101 C102 C103 -0.5(8) . . . . ? C101 C102 C103 C104 0.2(8) . . . . ? C102 C103 C104 C105 -0.1(8) . . . . ? C103 C104 C105 C106 0.3(8) . . . . ? C104 C105 C106 C101 -0.6(8) . . . . ? C102 C101 C106 C105 0.7(8) . . . . ? C203 C201 C202 C203 -0.1(11) 3_465 . . . ? C201 C202 C203 C201 0.1(11) . . . 3_465 ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 67.45 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.292 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.042