data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Simon John Lancaster' 'David L. Hughes' 'Andrew J. Mountford' _publ_contact_author_name 'Dr Simon John Lancaster' _publ_contact_author_address ; Dr Simon John Lancaster School of Chemical Sciences and Pharmacy University of East Anglia Earlham Road Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email ' S.LANCASTER@UEA.AC.UK' _publ_section_title ; Intra- and inter-molecular C-H---F-C and N-H---F-C hydrogen bonding in secondary amine adducts of B(C6F5)3: relevance to key interactions in alkene polymerisation catalysis ; data_andym5 _database_code_CSD 211286 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 1' _chemical_melting_point ? _chemical_formula_moiety 'C22 H9 B F15 N' _chemical_formula_structural (C6F5)3B-cyclo-NHC4H8 _chemical_formula_sum 'C22 H9 B F15 N' _chemical_formula_weight 583.11 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' #(equiv. to no. 14) 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 14.232(1) _cell_length_b 11.510(1) _cell_length_c 14.543(1) _cell_angle_alpha 90.00 _cell_angle_beta 117.22(1) _cell_angle_gamma 90.00 _cell_volume 2118.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square prisms' _exptl_crystal_colour 'clear, colourless,' _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12139 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.33 _reflns_number_total 3616 _reflns_number_gt 3125 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (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^)+(0.0468P)^2^+0.365P] 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 3616 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 B B 0.48088(13) 0.75710(14) 0.21110(12) 0.0211(3) Uani 1 1 d . . . C11 C 0.59764(12) 0.76273(13) 0.21265(11) 0.0216(3) Uani 1 1 d . . . C12 C 0.62797(12) 0.82526(13) 0.14887(12) 0.0237(3) Uani 1 1 d . . . F12 F 0.55721(7) 0.89404(8) 0.07208(7) 0.0300(2) Uani 1 1 d . . . C13 C 0.72923(13) 0.82328(14) 0.15673(13) 0.0291(4) Uani 1 1 d . . . F13 F 0.75192(8) 0.88810(9) 0.09221(8) 0.0397(3) Uani 1 1 d . . . C14 C 0.80539(12) 0.75350(15) 0.22931(14) 0.0324(4) Uani 1 1 d . . . F14 F 0.90329(8) 0.74909(10) 0.23709(9) 0.0477(3) Uani 1 1 d . . . C15 C 0.77940(13) 0.68687(14) 0.29356(13) 0.0297(4) Uani 1 1 d . . . F15 F 0.85299(8) 0.61778(9) 0.36544(8) 0.0415(3) Uani 1 1 d . . . C16 C 0.67859(12) 0.69215(13) 0.28332(12) 0.0247(3) Uani 1 1 d . . . F16 F 0.65820(7) 0.62493(8) 0.34898(7) 0.0315(2) Uani 1 1 d . . . C21 C 0.43886(12) 0.62367(13) 0.17087(12) 0.0226(3) Uani 1 1 d . . . C22 C 0.41155(12) 0.59284(13) 0.06883(12) 0.0244(3) Uani 1 1 d . . . F22 F 0.41292(8) 0.67525(8) 0.00206(7) 0.0304(2) Uani 1 1 d . . . C23 C 0.38576(12) 0.48193(14) 0.02867(12) 0.0280(4) Uani 1 1 d . . . F23 F 0.36199(8) 0.46041(9) -0.07079(7) 0.0385(3) Uani 1 1 d . . . C24 C 0.38616(13) 0.39260(13) 0.09234(14) 0.0299(4) Uani 1 1 d . . . F24 F 0.36438(8) 0.28336(8) 0.05657(9) 0.0408(3) Uani 1 1 d . . . C25 C 0.41119(13) 0.41730(13) 0.19370(13) 0.0281(4) Uani 1 1 d . . . F25 F 0.40984(8) 0.33176(8) 0.25621(8) 0.0376(3) Uani 1 1 d . . . C26 C 0.43886(12) 0.52926(13) 0.23115(12) 0.0251(3) Uani 1 1 d . . . F26 F 0.46959(8) 0.54112(8) 0.33374(7) 0.0321(2) Uani 1 1 d . . . C31 C 0.48824(12) 0.79168(13) 0.32508(11) 0.0215(3) Uani 1 1 d . . . C32 C 0.41292(12) 0.75957(13) 0.35689(12) 0.0244(3) Uani 1 1 d . . . F32 F 0.32526(7) 0.69909(8) 0.29241(7) 0.0316(2) Uani 1 1 d . . . C33 C 0.41908(13) 0.78416(14) 0.45291(13) 0.0278(4) Uani 1 1 d . . . F33 F 0.34271(8) 0.74899(9) 0.47663(8) 0.0407(3) Uani 1 1 d . . . C34 C 0.50408(14) 0.84600(14) 0.52396(12) 0.0271(3) Uani 1 1 d . . . F34 F 0.51056(9) 0.87325(9) 0.61666(7) 0.0364(3) Uani 1 1 d . . . C35 C 0.58041(12) 0.88267(13) 0.49722(12) 0.0246(3) Uani 1 1 d . . . F35 F 0.66346(7) 0.94585(8) 0.56460(7) 0.0328(2) Uani 1 1 d . . . C36 C 0.57098(12) 0.85661(13) 0.39996(12) 0.0228(3) Uani 1 1 d . . . F36 F 0.64919(7) 0.90023(8) 0.38117(7) 0.0295(2) Uani 1 1 d . . . N4 N 0.40086(10) 0.84965(11) 0.12714(10) 0.0226(3) Uani 1 1 d . . . H4 H 0.4111 0.8431 0.0700 0.027 Uiso 1 1 calc R . . C41 C 0.28273(12) 0.82780(14) 0.09103(13) 0.0278(4) Uani 1 1 d . . . H41A H 0.2502 0.7941 0.0223 0.033 Uiso 1 1 calc R . . H41B H 0.2729 0.7751 0.1380 0.033 Uiso 1 1 calc R . . C42 C 0.23408(13) 0.94602(15) 0.09045(13) 0.0319(4) Uani 1 1 d . . . H42A H 0.1751 0.9386 0.1062 0.038 Uiso 1 1 calc R . . H42B H 0.2101 0.9841 0.0240 0.038 Uiso 1 1 calc R . . C43 C 0.32565(13) 1.01284(15) 0.17573(13) 0.0324(4) Uani 1 1 d . . . H43A H 0.3139 1.0960 0.1676 0.039 Uiso 1 1 calc R . . H43B H 0.3353 0.9901 0.2437 0.039 Uiso 1 1 calc R . . C44 C 0.41982(13) 0.97737(13) 0.15961(13) 0.0273(3) Uani 1 1 d . . . H44A H 0.4851 0.9864 0.2230 0.033 Uiso 1 1 calc R . . H44B H 0.4237 1.0243 0.1060 0.033 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 B 0.0227(8) 0.0200(8) 0.0214(9) 0.0005(6) 0.0107(7) -0.0007(6) C11 0.0238(8) 0.0203(7) 0.0223(8) -0.0047(6) 0.0119(7) -0.0025(6) C12 0.0257(8) 0.0216(8) 0.0238(8) -0.0030(6) 0.0114(7) -0.0021(6) F12 0.0337(5) 0.0291(5) 0.0303(5) 0.0071(4) 0.0173(4) 0.0008(4) C13 0.0339(9) 0.0263(8) 0.0360(9) -0.0065(7) 0.0236(8) -0.0080(6) F13 0.0469(6) 0.0368(6) 0.0523(6) -0.0027(4) 0.0374(6) -0.0110(4) C14 0.0222(8) 0.0346(9) 0.0452(10) -0.0126(7) 0.0196(8) -0.0056(7) F14 0.0266(5) 0.0525(7) 0.0716(8) -0.0098(6) 0.0290(6) -0.0037(5) C15 0.0245(8) 0.0284(9) 0.0317(9) -0.0051(7) 0.0090(8) 0.0031(6) F15 0.0271(5) 0.0404(6) 0.0480(6) 0.0025(5) 0.0095(5) 0.0098(4) C16 0.0275(8) 0.0239(8) 0.0234(8) -0.0016(6) 0.0123(7) -0.0014(6) F16 0.0333(5) 0.0331(5) 0.0285(5) 0.0082(4) 0.0143(4) 0.0050(4) C21 0.0207(7) 0.0214(8) 0.0271(8) -0.0006(6) 0.0122(7) 0.0001(5) C22 0.0245(8) 0.0238(8) 0.0266(8) 0.0001(6) 0.0131(7) -0.0008(6) F22 0.0418(6) 0.0264(5) 0.0253(5) -0.0005(4) 0.0174(5) -0.0014(4) C23 0.0256(8) 0.0301(9) 0.0289(9) -0.0082(6) 0.0129(7) -0.0011(6) F23 0.0455(6) 0.0381(6) 0.0336(5) -0.0155(4) 0.0197(5) -0.0062(4) C24 0.0278(8) 0.0205(8) 0.0451(10) -0.0100(7) 0.0198(8) -0.0044(6) F24 0.0469(6) 0.0227(5) 0.0580(7) -0.0145(4) 0.0284(5) -0.0089(4) C25 0.0278(8) 0.0207(8) 0.0411(9) 0.0033(7) 0.0203(8) 0.0001(6) F25 0.0470(6) 0.0222(5) 0.0520(6) 0.0058(4) 0.0299(5) -0.0015(4) C26 0.0257(8) 0.0256(8) 0.0267(8) -0.0007(6) 0.0142(7) -0.0001(6) F26 0.0440(6) 0.0278(5) 0.0276(5) 0.0024(4) 0.0189(5) -0.0025(4) C31 0.0226(7) 0.0194(7) 0.0236(8) 0.0013(6) 0.0114(7) 0.0022(6) C32 0.0224(7) 0.0235(8) 0.0271(8) -0.0013(6) 0.0113(7) -0.0020(6) F32 0.0266(5) 0.0385(6) 0.0321(5) -0.0059(4) 0.0156(4) -0.0104(4) C33 0.0301(8) 0.0300(9) 0.0310(9) 0.0010(6) 0.0206(8) 0.0003(7) F33 0.0437(6) 0.0510(7) 0.0426(6) -0.0055(5) 0.0328(5) -0.0112(5) C34 0.0369(9) 0.0254(8) 0.0228(8) 0.0000(6) 0.0169(8) 0.0048(7) F34 0.0523(6) 0.0372(6) 0.0266(5) -0.0039(4) 0.0239(5) -0.0002(4) C35 0.0252(8) 0.0215(8) 0.0228(8) -0.0031(6) 0.0074(7) 0.0014(6) F35 0.0303(5) 0.0354(5) 0.0280(5) -0.0105(4) 0.0092(4) -0.0042(4) C36 0.0216(7) 0.0218(8) 0.0274(8) 0.0006(6) 0.0132(7) 0.0015(6) F36 0.0262(5) 0.0336(5) 0.0327(5) -0.0088(4) 0.0169(4) -0.0093(4) N4 0.0227(7) 0.0217(7) 0.0243(7) -0.0008(5) 0.0115(6) -0.0014(5) C41 0.0204(8) 0.0308(9) 0.0279(8) 0.0024(6) 0.0072(7) -0.0007(6) C42 0.0267(8) 0.0378(10) 0.0327(9) 0.0032(7) 0.0149(8) 0.0072(7) C43 0.0382(10) 0.0290(9) 0.0321(9) -0.0017(7) 0.0179(8) 0.0056(7) C44 0.0315(8) 0.0189(8) 0.0307(8) 0.0002(6) 0.0135(7) 0.0004(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 B N4 1.628(2) . ? B C11 1.653(2) . ? B C21 1.655(2) . ? B C31 1.661(2) . ? C11 C12 1.390(2) . ? C11 C16 1.400(2) . ? C12 F12 1.3636(18) . ? C12 C13 1.393(2) . ? C13 F13 1.3486(18) . ? C13 C14 1.374(2) . ? C14 F14 1.3463(19) . ? C14 C15 1.384(2) . ? C15 F15 1.3491(19) . ? C15 C16 1.374(2) . ? C16 F16 1.3595(18) . ? C21 C26 1.396(2) . ? C21 C22 1.397(2) . ? C22 F22 1.3640(18) . ? C22 C23 1.382(2) . ? C23 F23 1.3491(18) . ? C23 C24 1.382(2) . ? C24 F24 1.3418(18) . ? C24 C25 1.378(2) . ? C25 F25 1.3461(18) . ? C25 C26 1.384(2) . ? C26 F26 1.3560(18) . ? C31 C32 1.398(2) . ? C31 C36 1.399(2) . ? C32 F32 1.3602(17) . ? C32 C33 1.388(2) . ? C33 F33 1.3444(19) . ? C33 C34 1.376(2) . ? C34 F34 1.3457(17) . ? C34 C35 1.377(2) . ? C35 F35 1.3515(17) . ? C35 C36 1.391(2) . ? C36 F36 1.3580(17) . ? N4 C44 1.5298(19) . ? N4 C41 1.5356(19) . ? N4 H4 0.9100 . ? C41 C42 1.525(2) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.533(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.518(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 B C11 109.80(12) . . ? N4 B C21 109.05(12) . . ? C11 B C21 103.87(12) . . ? N4 B C31 107.15(11) . . ? C11 B C31 111.90(12) . . ? C21 B C31 115.01(12) . . ? C12 C11 C16 112.83(14) . . ? C12 C11 B 128.94(13) . . ? C16 C11 B 118.15(13) . . ? F12 C12 C11 120.59(14) . . ? F12 C12 C13 115.19(14) . . ? C11 C12 C13 124.22(15) . . ? F13 C13 C14 120.14(15) . . ? F13 C13 C12 120.13(15) . . ? C14 C13 C12 119.72(15) . . ? F14 C14 C13 120.61(16) . . ? F14 C14 C15 120.55(16) . . ? C13 C14 C15 118.83(15) . . ? F15 C15 C16 120.79(15) . . ? F15 C15 C14 119.83(15) . . ? C16 C15 C14 119.37(15) . . ? F16 C16 C15 116.51(14) . . ? F16 C16 C11 118.52(13) . . ? C15 C16 C11 124.95(14) . . ? C26 C21 C22 112.91(14) . . ? C26 C21 B 127.17(14) . . ? C22 C21 B 119.42(13) . . ? F22 C22 C23 115.41(14) . . ? F22 C22 C21 119.47(13) . . ? C23 C22 C21 125.08(15) . . ? F23 C23 C22 120.70(15) . . ? F23 C23 C24 120.26(14) . . ? C22 C23 C24 119.03(15) . . ? F24 C24 C25 120.58(15) . . ? F24 C24 C23 120.53(15) . . ? C25 C24 C23 118.88(14) . . ? F25 C25 C24 119.66(14) . . ? F25 C25 C26 120.30(15) . . ? C24 C25 C26 120.04(15) . . ? F26 C26 C25 114.66(14) . . ? F26 C26 C21 121.32(13) . . ? C25 C26 C21 124.00(15) . . ? C32 C31 C36 112.55(13) . . ? C32 C31 B 124.00(13) . . ? C36 C31 B 123.45(13) . . ? F32 C32 C33 114.46(13) . . ? F32 C32 C31 120.50(13) . . ? C33 C32 C31 125.04(14) . . ? F33 C33 C34 119.96(14) . . ? F33 C33 C32 120.69(14) . . ? C34 C33 C32 119.35(14) . . ? F34 C34 C33 120.44(14) . . ? F34 C34 C35 120.67(14) . . ? C33 C34 C35 118.86(14) . . ? F35 C35 C34 120.10(13) . . ? F35 C35 C36 119.93(14) . . ? C34 C35 C36 119.96(14) . . ? F36 C36 C35 114.71(13) . . ? F36 C36 C31 121.09(13) . . ? C35 C36 C31 124.19(14) . . ? C44 N4 C41 105.90(11) . . ? C44 N4 B 115.66(11) . . ? C41 N4 B 115.48(11) . . ? C44 N4 H4 106.4 . . ? C41 N4 H4 106.4 . . ? B N4 H4 106.4 . . ? C42 C41 N4 106.21(12) . . ? C42 C41 H41A 110.5 . . ? N4 C41 H41A 110.5 . . ? C42 C41 H41B 110.5 . . ? N4 C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? C41 C42 C43 103.14(13) . . ? C41 C42 H42A 111.1 . . ? C43 C42 H42A 111.1 . . ? C41 C42 H42B 111.1 . . ? C43 C42 H42B 111.1 . . ? H42A C42 H42B 109.1 . . ? C44 C43 C42 102.95(13) . . ? C44 C43 H43A 111.2 . . ? C42 C43 H43A 111.2 . . ? C44 C43 H43B 111.2 . . ? C42 C43 H43B 111.2 . . ? H43A C43 H43B 109.1 . . ? C43 C44 N4 105.22(12) . . ? C43 C44 H44A 110.7 . . ? N4 C44 H44A 110.7 . . ? C43 C44 H44B 110.7 . . ? N4 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 B C11 C12 -5.8(2) . . . . ? C21 B C11 C12 110.66(16) . . . . ? C31 B C11 C12 -124.69(16) . . . . ? N4 B C11 C16 177.58(12) . . . . ? C21 B C11 C16 -65.92(16) . . . . ? C31 B C11 C16 58.73(17) . . . . ? C16 C11 C12 F12 176.74(12) . . . . ? B C11 C12 F12 0.0(2) . . . . ? C16 C11 C12 C13 -3.0(2) . . . . ? B C11 C12 C13 -179.70(14) . . . . ? F12 C12 C13 F13 1.1(2) . . . . ? C11 C12 C13 F13 -179.13(13) . . . . ? F12 C12 C13 C14 -177.74(13) . . . . ? C11 C12 C13 C14 2.0(2) . . . . ? F13 C13 C14 F14 0.1(2) . . . . ? C12 C13 C14 F14 179.02(14) . . . . ? F13 C13 C14 C15 -179.19(14) . . . . ? C12 C13 C14 C15 -0.3(2) . . . . ? F14 C14 C15 F15 0.7(2) . . . . ? C13 C14 C15 F15 -179.95(14) . . . . ? F14 C14 C15 C16 -179.37(14) . . . . ? C13 C14 C15 C16 0.0(2) . . . . ? F15 C15 C16 F16 0.1(2) . . . . ? C14 C15 C16 F16 -179.77(13) . . . . ? F15 C15 C16 C11 178.66(13) . . . . ? C14 C15 C16 C11 -1.2(2) . . . . ? C12 C11 C16 F16 -178.87(13) . . . . ? B C11 C16 F16 -1.76(19) . . . . ? C12 C11 C16 C15 2.6(2) . . . . ? B C11 C16 C15 179.74(14) . . . . ? N4 B C21 C26 -140.60(15) . . . . ? C11 B C21 C26 102.38(17) . . . . ? C31 B C21 C26 -20.2(2) . . . . ? N4 B C21 C22 48.07(18) . . . . ? C11 B C21 C22 -68.95(16) . . . . ? C31 B C21 C22 168.43(13) . . . . ? C26 C21 C22 F22 -177.03(14) . . . . ? B C21 C22 F22 -4.5(2) . . . . ? C26 C21 C22 C23 0.6(2) . . . . ? B C21 C22 C23 173.11(15) . . . . ? F22 C22 C23 F23 -1.2(2) . . . . ? C21 C22 C23 F23 -178.97(14) . . . . ? F22 C22 C23 C24 177.79(14) . . . . ? C21 C22 C23 C24 0.1(3) . . . . ? F23 C23 C24 F24 0.9(2) . . . . ? C22 C23 C24 F24 -178.13(14) . . . . ? F23 C23 C24 C25 179.75(14) . . . . ? C22 C23 C24 C25 0.7(2) . . . . ? F24 C24 C25 F25 -2.5(2) . . . . ? C23 C24 C25 F25 178.64(15) . . . . ? F24 C24 C25 C26 176.64(15) . . . . ? C23 C24 C25 C26 -2.2(2) . . . . ? F25 C25 C26 F26 4.0(2) . . . . ? C24 C25 C26 F26 -175.18(13) . . . . ? F25 C25 C26 C21 -177.76(14) . . . . ? C24 C25 C26 C21 3.1(3) . . . . ? C22 C21 C26 F26 175.97(13) . . . . ? B C21 C26 F26 4.2(2) . . . . ? C22 C21 C26 C25 -2.2(2) . . . . ? B C21 C26 C25 -173.98(15) . . . . ? N4 B C31 C32 81.07(17) . . . . ? C11 B C31 C32 -158.53(14) . . . . ? C21 B C31 C32 -40.3(2) . . . . ? N4 B C31 C36 -98.85(15) . . . . ? C11 B C31 C36 21.55(19) . . . . ? C21 B C31 C36 139.75(14) . . . . ? C36 C31 C32 F32 177.96(13) . . . . ? B C31 C32 F32 -2.0(2) . . . . ? C36 C31 C32 C33 -2.3(2) . . . . ? B C31 C32 C33 177.79(14) . . . . ? F32 C32 C33 F33 0.1(2) . . . . ? C31 C32 C33 F33 -179.65(14) . . . . ? F32 C32 C33 C34 -179.39(13) . . . . ? C31 C32 C33 C34 0.8(2) . . . . ? F33 C33 C34 F34 -1.1(2) . . . . ? C32 C33 C34 F34 178.43(14) . . . . ? F33 C33 C34 C35 -178.96(14) . . . . ? C32 C33 C34 C35 0.6(2) . . . . ? F34 C34 C35 F35 0.6(2) . . . . ? C33 C34 C35 F35 178.47(13) . . . . ? F34 C34 C35 C36 -178.15(14) . . . . ? C33 C34 C35 C36 -0.3(2) . . . . ? F35 C35 C36 F36 -0.7(2) . . . . ? C34 C35 C36 F36 178.09(13) . . . . ? F35 C35 C36 C31 179.83(13) . . . . ? C34 C35 C36 C31 -1.4(2) . . . . ? C32 C31 C36 F36 -176.92(13) . . . . ? B C31 C36 F36 3.0(2) . . . . ? C32 C31 C36 C35 2.6(2) . . . . ? B C31 C36 C35 -177.51(14) . . . . ? C11 B N4 C44 -74.76(15) . . . . ? C21 B N4 C44 172.04(12) . . . . ? C31 B N4 C44 46.97(16) . . . . ? C11 B N4 C41 160.79(12) . . . . ? C21 B N4 C41 47.60(16) . . . . ? C31 B N4 C41 -77.48(15) . . . . ? C44 N4 C41 C42 7.03(16) . . . . ? B N4 C41 C42 136.42(13) . . . . ? N4 C41 C42 C43 -29.35(16) . . . . ? C41 C42 C43 C44 40.60(16) . . . . ? C42 C43 C44 N4 -36.56(16) . . . . ? C41 N4 C44 C43 18.37(16) . . . . ? B N4 C44 C43 -110.92(14) . . . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.203 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.046 #======END data_andym9 _database_code_CSD 211287 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'complex 2' _chemical_melting_point ? _chemical_formula_moiety 'C23 H11 B F15 N' _chemical_formula_structural (C6F5)3B-NHC5H10 _chemical_formula_sum 'C23 H11 B F15 N' _chemical_formula_weight 597.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn #(equiv. to no. 7) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 10.186(2) _cell_length_b 13.026(3) _cell_length_c 17.501(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.63(3) _cell_angle_gamma 90.00 _cell_volume 2306.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'clear, colourless' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12844 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.38 _reflns_number_total 7190 _reflns_number_gt 6488 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (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^)+(0.0319P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(3) _refine_ls_number_reflns 7190 _refine_ls_number_parameters 721 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.2149(3) 0.4358(2) 0.17913(15) 0.0341(5) Uani 1 1 d . . . C11 C 0.2920(2) 0.54875(17) 0.18867(13) 0.0358(5) Uani 1 1 d . . . C12 C 0.3958(2) 0.57522(18) 0.14637(13) 0.0390(5) Uani 1 1 d . . . F12 F 0.42892(14) 0.51099(11) 0.09017(8) 0.0470(3) Uani 1 1 d . . . C13 C 0.4724(2) 0.66344(19) 0.15778(14) 0.0401(5) Uani 1 1 d . . . F13 F 0.56937(14) 0.68298(11) 0.11373(8) 0.0494(4) Uani 1 1 d . . . C14 C 0.4480(3) 0.73094(19) 0.21476(16) 0.0461(6) Uani 1 1 d . . . F14 F 0.52204(17) 0.81697(12) 0.22769(10) 0.0617(4) Uani 1 1 d . . . C15 C 0.3481(3) 0.70901(19) 0.25955(15) 0.0457(6) Uani 1 1 d . . . F15 F 0.32351(17) 0.77454(12) 0.31632(10) 0.0614(4) Uani 1 1 d . . . C16 C 0.2743(2) 0.62071(18) 0.24618(14) 0.0399(5) Uani 1 1 d . . . F16 F 0.18064(15) 0.60610(11) 0.29423(8) 0.0505(4) Uani 1 1 d . . . C21 C 0.3216(2) 0.35810(17) 0.22936(13) 0.0330(5) Uani 1 1 d . . . C22 C 0.3305(2) 0.35579(18) 0.30914(14) 0.0381(5) Uani 1 1 d . . . F22 F 0.24407(14) 0.41125(12) 0.34591(8) 0.0484(3) Uani 1 1 d . . . C23 C 0.4249(2) 0.30126(18) 0.35619(14) 0.0399(5) Uani 1 1 d . . . F23 F 0.42595(15) 0.30333(12) 0.43323(8) 0.0530(4) Uani 1 1 d . . . C24 C 0.5195(2) 0.24469(18) 0.32366(15) 0.0402(5) Uani 1 1 d . . . F24 F 0.61159(15) 0.19152(12) 0.36810(9) 0.0539(4) Uani 1 1 d . . . C25 C 0.5177(2) 0.24561(18) 0.24504(15) 0.0407(5) Uani 1 1 d . . . F25 F 0.61171(14) 0.19437(12) 0.21205(9) 0.0545(4) Uani 1 1 d . . . C26 C 0.4208(2) 0.30048(17) 0.20016(13) 0.0365(5) Uani 1 1 d . . . F26 F 0.42963(14) 0.29626(11) 0.12308(8) 0.0456(3) Uani 1 1 d . . . C31 C 0.0659(2) 0.43550(18) 0.20586(13) 0.0356(5) Uani 1 1 d . . . C32 C -0.0208(2) 0.51944(18) 0.19595(15) 0.0397(5) Uani 1 1 d . . . F32 F 0.01683(14) 0.60584(11) 0.15998(9) 0.0520(4) Uani 1 1 d . . . C33 C -0.1436(2) 0.5222(2) 0.22139(16) 0.0458(6) Uani 1 1 d . . . F33 F -0.21995(15) 0.60716(13) 0.21163(11) 0.0633(4) Uani 1 1 d . . . C34 C -0.1891(2) 0.4367(2) 0.25697(15) 0.0474(6) Uani 1 1 d . . . F34 F -0.31045(15) 0.43886(14) 0.28172(10) 0.0627(4) Uani 1 1 d . . . C35 C -0.1109(2) 0.3503(2) 0.26636(13) 0.0404(5) Uani 1 1 d . . . F35 F -0.15544(15) 0.26533(13) 0.29953(9) 0.0537(4) Uani 1 1 d . . . C36 C 0.0117(2) 0.35171(18) 0.24060(13) 0.0359(5) Uani 1 1 d . . . F36 F 0.08227(13) 0.26239(10) 0.25153(8) 0.0459(3) Uani 1 1 d . . . N4 N 0.19819(19) 0.40148(15) 0.08905(11) 0.0374(4) Uani 1 1 d . . . H4 H 0.2815 0.3973 0.0753 0.045 Uiso 1 1 calc R . . C41 C 0.1372(3) 0.29555(19) 0.07436(14) 0.0428(6) Uani 1 1 d . . . H41A H 0.0446 0.2976 0.0822 0.051 Uiso 1 1 calc R . . H41B H 0.1814 0.2466 0.1104 0.051 Uiso 1 1 calc R . . C42 C 0.1506(3) 0.2614(2) -0.00782(15) 0.0529(7) Uani 1 1 d . . . H42A H 0.2435 0.2554 -0.0145 0.064 Uiso 1 1 calc R . . H42B H 0.1102 0.1944 -0.0168 0.064 Uiso 1 1 calc R . . C43 C 0.0848(3) 0.3376(3) -0.06603(16) 0.0616(8) Uani 1 1 d . . . H43A H -0.0101 0.3364 -0.0644 0.074 Uiso 1 1 calc R . . H43B H 0.1020 0.3178 -0.1174 0.074 Uiso 1 1 calc R . . C44 C 0.1373(3) 0.4474(2) -0.04870(16) 0.0563(7) Uani 1 1 d . . . H44A H 0.2292 0.4511 -0.0580 0.068 Uiso 1 1 calc R . . H44B H 0.0876 0.4956 -0.0830 0.068 Uiso 1 1 calc R . . C45 C 0.1254(3) 0.4772(2) 0.03412(15) 0.0463(6) Uani 1 1 d . . . H45A H 0.1617 0.5453 0.0441 0.056 Uiso 1 1 calc R . . H45B H 0.0328 0.4788 0.0424 0.056 Uiso 1 1 calc R . . B5 B 0.1555(2) 0.99205(19) 0.48160(13) 0.0297(5) Uani 1 1 d . . . C51 C 0.1335(2) 0.86491(17) 0.48164(12) 0.0336(5) Uani 1 1 d . . . C52 C 0.2148(2) 0.79133(18) 0.52140(14) 0.0391(5) Uani 1 1 d . . . F52 F 0.32007(13) 0.82048(10) 0.57309(9) 0.0474(3) Uani 1 1 d . . . C53 C 0.1981(3) 0.68572(18) 0.51365(15) 0.0438(6) Uani 1 1 d . . . F53 F 0.28227(16) 0.62056(11) 0.55582(10) 0.0606(4) Uani 1 1 d . . . C54 C 0.0974(3) 0.64730(19) 0.46262(16) 0.0458(6) Uani 1 1 d . . . F54 F 0.07965(19) 0.54481(12) 0.45371(11) 0.0642(5) Uani 1 1 d . . . C55 C 0.0135(3) 0.7157(2) 0.42098(14) 0.0437(6) Uani 1 1 d . . . F55 F -0.08613(16) 0.68005(12) 0.37077(9) 0.0574(4) Uani 1 1 d . . . C56 C 0.0335(2) 0.82091(17) 0.43113(13) 0.0360(5) Uani 1 1 d . . . F56 F -0.05357(14) 0.88297(11) 0.38865(8) 0.0450(3) Uani 1 1 d . . . C61 C 0.2298(2) 1.01222(16) 0.40359(12) 0.0306(4) Uani 1 1 d . . . C62 C 0.1631(2) 1.03920(16) 0.33208(12) 0.0325(5) Uani 1 1 d . . . F62 F 0.03264(13) 1.06110(10) 0.32437(7) 0.0390(3) Uani 1 1 d . . . C63 C 0.2237(2) 1.04433(18) 0.26482(13) 0.0377(5) Uani 1 1 d . . . F63 F 0.15277(15) 1.06971(11) 0.19760(7) 0.0481(3) Uani 1 1 d . . . C64 C 0.3573(3) 1.02202(18) 0.26719(13) 0.0402(5) Uani 1 1 d . . . F64 F 0.41632(16) 1.02696(12) 0.20221(8) 0.0528(4) Uani 1 1 d . . . C65 C 0.4279(2) 0.99528(18) 0.33609(14) 0.0384(5) Uani 1 1 d . . . F65 F 0.55766(14) 0.97256(12) 0.33960(8) 0.0509(4) Uani 1 1 d . . . C66 C 0.3629(2) 0.98976(17) 0.40098(12) 0.0325(5) Uani 1 1 d . . . F66 F 0.43876(12) 0.95799(11) 0.46628(7) 0.0415(3) Uani 1 1 d . . . C71 C 0.0200(2) 1.06095(17) 0.48653(12) 0.0316(4) Uani 1 1 d . . . C72 C -0.0890(2) 1.02385(18) 0.51955(12) 0.0359(5) Uani 1 1 d . . . F72 F -0.09352(13) 0.92501(11) 0.54411(7) 0.0412(3) Uani 1 1 d . . . C73 C -0.1984(2) 1.0832(2) 0.53126(14) 0.0447(6) Uani 1 1 d . . . F73 F -0.30048(15) 1.04157(15) 0.56321(9) 0.0625(4) Uani 1 1 d . . . C74 C -0.2013(2) 1.1856(2) 0.51088(15) 0.0486(7) Uani 1 1 d . . . F74 F -0.30434(16) 1.24593(14) 0.52457(10) 0.0677(5) Uani 1 1 d . . . C75 C -0.0976(3) 1.2268(2) 0.47698(14) 0.0452(6) Uani 1 1 d . . . F75 F -0.09849(17) 1.32711(12) 0.45739(9) 0.0591(4) Uani 1 1 d . . . C76 C 0.0091(2) 1.16384(18) 0.46569(13) 0.0367(5) Uani 1 1 d . . . F76 F 0.10874(13) 1.21071(10) 0.43295(8) 0.0428(3) Uani 1 1 d . . . N8 N 0.25451(17) 1.02543(13) 0.55748(10) 0.0284(4) Uani 1 1 d . . . H8 H 0.3240 0.9812 0.5597 0.034 Uiso 1 1 calc R . . C81 C 0.3138(2) 1.13186(17) 0.55716(12) 0.0347(5) Uani 1 1 d . . . H81A H 0.2456 1.1827 0.5619 0.042 Uiso 1 1 calc R . . H81B H 0.3495 1.1434 0.5088 0.042 Uiso 1 1 calc R . . C82 C 0.4235(2) 1.14337(19) 0.62383(13) 0.0383(5) Uani 1 1 d . . . H82A H 0.4597 1.2122 0.6236 0.046 Uiso 1 1 calc R . . H82B H 0.4940 1.0953 0.6172 0.046 Uiso 1 1 calc R . . C83 C 0.3713(2) 1.1233(2) 0.70098(14) 0.0431(6) Uani 1 1 d . . . H83A H 0.4443 1.1243 0.7418 0.052 Uiso 1 1 calc R . . H83B H 0.3102 1.1774 0.7111 0.052 Uiso 1 1 calc R . . C84 C 0.3012(2) 1.0198(2) 0.70072(14) 0.0429(6) Uani 1 1 d . . . H84A H 0.2610 1.0121 0.7480 0.051 Uiso 1 1 calc R . . H84B H 0.3653 0.9651 0.6986 0.051 Uiso 1 1 calc R . . C85 C 0.1944(2) 1.0106(2) 0.63191(12) 0.0357(5) Uani 1 1 d . . . H85A H 0.1533 0.9435 0.6321 0.043 Uiso 1 1 calc R . . H85B H 0.1267 1.0620 0.6359 0.043 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 B1 0.0375(13) 0.0297(14) 0.0356(13) 0.0004(10) 0.0061(10) -0.0029(10) C11 0.0390(12) 0.0332(12) 0.0347(12) 0.0064(9) 0.0022(9) -0.0028(9) C12 0.0438(13) 0.0355(13) 0.0372(13) 0.0037(10) 0.0019(10) -0.0034(9) F12 0.0491(8) 0.0469(8) 0.0474(8) -0.0037(6) 0.0158(6) -0.0106(6) C13 0.0367(12) 0.0416(14) 0.0409(13) 0.0116(10) 0.0004(10) -0.0065(10) F13 0.0440(8) 0.0550(9) 0.0488(8) 0.0136(7) 0.0040(6) -0.0139(6) C14 0.0512(14) 0.0334(13) 0.0516(15) 0.0054(11) -0.0036(11) -0.0115(11) F14 0.0688(10) 0.0447(9) 0.0704(11) -0.0011(8) 0.0024(8) -0.0265(8) C15 0.0565(15) 0.0342(13) 0.0451(14) -0.0003(11) 0.0009(11) -0.0040(11) F15 0.0809(11) 0.0404(9) 0.0642(10) -0.0151(7) 0.0139(8) -0.0126(7) C16 0.0479(14) 0.0330(13) 0.0394(13) 0.0030(10) 0.0071(10) -0.0021(10) F16 0.0611(9) 0.0411(8) 0.0527(9) -0.0073(6) 0.0217(7) -0.0092(6) C21 0.0371(12) 0.0267(11) 0.0363(12) 0.0007(9) 0.0090(9) -0.0019(8) C22 0.0404(12) 0.0326(12) 0.0421(13) -0.0009(10) 0.0076(10) 0.0019(9) F22 0.0526(9) 0.0542(9) 0.0393(8) -0.0003(6) 0.0091(6) 0.0128(7) C23 0.0430(13) 0.0375(13) 0.0382(13) 0.0034(10) 0.0002(10) -0.0061(9) F23 0.0576(9) 0.0631(10) 0.0374(8) 0.0087(7) 0.0014(6) 0.0013(7) C24 0.0369(12) 0.0324(13) 0.0492(15) 0.0055(10) -0.0037(10) -0.0021(9) F24 0.0486(8) 0.0508(9) 0.0584(9) 0.0064(7) -0.0098(7) 0.0080(6) C25 0.0359(12) 0.0340(13) 0.0511(15) -0.0079(10) 0.0004(10) 0.0000(9) F25 0.0439(8) 0.0545(9) 0.0639(10) -0.0181(7) 0.0014(7) 0.0119(6) C26 0.0416(12) 0.0296(12) 0.0384(13) -0.0053(9) 0.0044(10) -0.0051(9) F26 0.0478(8) 0.0532(9) 0.0367(7) -0.0072(6) 0.0087(6) 0.0038(6) C31 0.0371(12) 0.0345(13) 0.0356(13) 0.0022(9) 0.0061(9) -0.0016(9) C32 0.0393(13) 0.0319(13) 0.0475(14) 0.0046(10) 0.0028(10) -0.0004(9) F32 0.0541(9) 0.0360(8) 0.0652(10) 0.0143(7) 0.0043(7) 0.0050(6) C33 0.0369(13) 0.0444(15) 0.0547(16) -0.0073(12) -0.0007(11) 0.0040(10) F33 0.0463(9) 0.0566(10) 0.0850(12) -0.0057(8) -0.0009(8) 0.0159(7) C34 0.0329(13) 0.0647(18) 0.0447(14) -0.0113(12) 0.0054(10) -0.0076(11) F34 0.0375(8) 0.0815(12) 0.0716(11) -0.0160(9) 0.0173(7) -0.0066(7) C35 0.0421(13) 0.0448(14) 0.0353(13) -0.0004(10) 0.0083(10) -0.0091(10) F35 0.0510(9) 0.0615(10) 0.0500(9) 0.0070(7) 0.0117(7) -0.0198(7) C36 0.0367(12) 0.0325(12) 0.0385(12) 0.0025(9) 0.0036(9) -0.0001(9) F36 0.0486(8) 0.0335(7) 0.0571(9) 0.0098(6) 0.0124(6) -0.0019(6) N4 0.0387(11) 0.0382(11) 0.0349(10) 0.0025(8) 0.0031(8) -0.0054(8) C41 0.0476(14) 0.0380(13) 0.0427(14) -0.0047(10) 0.0054(10) -0.0122(10) C42 0.0595(16) 0.0543(17) 0.0450(15) -0.0102(12) 0.0066(12) -0.0122(13) C43 0.0616(18) 0.085(2) 0.0363(15) -0.0102(14) -0.0011(12) -0.0088(15) C44 0.0630(18) 0.0671(19) 0.0376(14) 0.0099(13) 0.0004(12) 0.0013(14) C45 0.0492(14) 0.0478(15) 0.0406(14) 0.0073(11) -0.0004(11) -0.0010(11) B5 0.0316(12) 0.0338(13) 0.0236(12) 0.0020(9) 0.0027(9) -0.0004(10) C51 0.0395(12) 0.0335(12) 0.0293(11) 0.0004(9) 0.0102(8) -0.0017(9) C52 0.0375(13) 0.0360(14) 0.0450(14) 0.0031(10) 0.0104(10) 0.0003(9) F52 0.0385(7) 0.0374(8) 0.0641(10) 0.0057(6) -0.0034(6) 0.0042(5) C53 0.0478(14) 0.0327(14) 0.0527(15) 0.0069(11) 0.0138(11) 0.0053(10) F53 0.0619(10) 0.0354(8) 0.0843(12) 0.0125(8) 0.0079(8) 0.0099(7) C54 0.0612(16) 0.0277(13) 0.0524(15) -0.0056(11) 0.0231(12) -0.0073(11) F54 0.0873(12) 0.0309(8) 0.0782(11) -0.0084(7) 0.0263(9) -0.0095(7) C55 0.0528(15) 0.0438(15) 0.0359(13) -0.0086(10) 0.0111(11) -0.0126(11) F55 0.0725(11) 0.0498(10) 0.0493(9) -0.0130(7) 0.0041(8) -0.0204(8) C56 0.0427(12) 0.0361(13) 0.0307(12) -0.0009(9) 0.0102(9) -0.0028(9) F56 0.0539(8) 0.0457(8) 0.0331(7) -0.0003(6) -0.0044(6) -0.0060(6) C61 0.0355(11) 0.0276(11) 0.0292(11) -0.0008(8) 0.0059(8) -0.0021(8) C62 0.0392(12) 0.0293(12) 0.0294(12) 0.0000(9) 0.0061(9) -0.0021(8) F62 0.0414(7) 0.0444(8) 0.0301(7) 0.0032(5) -0.0002(5) 0.0034(6) C63 0.0541(14) 0.0335(13) 0.0260(11) 0.0006(9) 0.0069(9) -0.0029(10) F63 0.0713(10) 0.0476(9) 0.0256(7) 0.0039(6) 0.0060(6) 0.0029(7) C64 0.0582(16) 0.0339(13) 0.0320(13) -0.0048(9) 0.0203(11) -0.0088(10) F64 0.0692(10) 0.0565(9) 0.0378(8) -0.0035(7) 0.0278(7) -0.0079(7) C65 0.0399(13) 0.0350(13) 0.0428(14) -0.0096(10) 0.0155(10) -0.0053(9) F65 0.0431(8) 0.0610(10) 0.0519(9) -0.0106(7) 0.0190(6) -0.0022(6) C66 0.0357(12) 0.0314(12) 0.0307(12) -0.0022(9) 0.0049(9) -0.0012(8) F66 0.0353(7) 0.0525(9) 0.0370(7) -0.0026(6) 0.0050(5) 0.0082(6) C71 0.0318(11) 0.0385(12) 0.0240(10) -0.0012(9) 0.0011(8) 0.0021(9) C72 0.0362(12) 0.0446(14) 0.0266(11) -0.0034(9) 0.0026(9) 0.0050(9) F72 0.0393(7) 0.0500(9) 0.0359(7) 0.0036(6) 0.0109(5) -0.0027(6) C73 0.0338(12) 0.0655(19) 0.0344(13) -0.0038(11) 0.0028(9) 0.0086(10) F73 0.0372(9) 0.0962(13) 0.0572(10) 0.0006(8) 0.0183(7) 0.0108(8) C74 0.0400(14) 0.0656(19) 0.0386(13) -0.0132(12) -0.0021(10) 0.0225(11) F74 0.0552(10) 0.0836(13) 0.0628(10) -0.0148(9) 0.0005(8) 0.0399(9) C75 0.0558(15) 0.0420(15) 0.0348(13) -0.0071(10) -0.0077(11) 0.0174(11) F75 0.0744(11) 0.0423(9) 0.0564(9) -0.0057(7) -0.0107(8) 0.0226(7) C76 0.0420(12) 0.0367(13) 0.0299(11) -0.0026(9) -0.0019(9) 0.0045(9) F76 0.0515(8) 0.0337(7) 0.0425(8) 0.0029(6) 0.0025(6) 0.0001(6) N8 0.0288(9) 0.0313(10) 0.0259(9) 0.0014(7) 0.0060(7) 0.0022(7) C81 0.0443(12) 0.0295(12) 0.0304(11) -0.0015(9) 0.0048(9) -0.0026(9) C82 0.0404(13) 0.0373(13) 0.0365(12) -0.0043(10) 0.0022(9) -0.0038(9) C83 0.0414(13) 0.0562(16) 0.0303(11) -0.0063(11) -0.0019(9) 0.0033(10) C84 0.0401(13) 0.0598(17) 0.0282(11) 0.0038(10) 0.0014(9) 0.0000(11) C85 0.0345(12) 0.0496(15) 0.0231(11) 0.0011(9) 0.0046(8) 0.0022(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N4 1.629(3) . ? B1 C31 1.639(3) . ? B1 C21 1.660(3) . ? B1 C11 1.667(3) . ? C11 C12 1.402(3) . ? C11 C16 1.402(3) . ? C12 F12 1.363(3) . ? C12 C13 1.390(3) . ? C13 F13 1.346(3) . ? C13 C14 1.374(4) . ? C14 F14 1.355(3) . ? C14 C15 1.384(4) . ? C15 F15 1.355(3) . ? C15 C16 1.379(3) . ? C16 F16 1.356(3) . ? C21 C22 1.389(3) . ? C21 C26 1.402(3) . ? C22 F22 1.357(3) . ? C22 C23 1.387(3) . ? C23 F23 1.347(3) . ? C23 C24 1.386(4) . ? C24 F24 1.340(3) . ? C24 C25 1.374(4) . ? C25 F25 1.350(3) . ? C25 C26 1.387(3) . ? C26 F26 1.363(3) . ? C31 C36 1.394(3) . ? C31 C32 1.403(3) . ? C32 F32 1.366(3) . ? C32 C33 1.376(4) . ? C33 F33 1.353(3) . ? C33 C34 1.382(4) . ? C34 F34 1.356(3) . ? C34 C35 1.378(4) . ? C35 F35 1.352(3) . ? C35 C36 1.376(3) . ? C36 F36 1.369(3) . ? N4 C45 1.511(3) . ? N4 C41 1.523(3) . ? C41 C42 1.526(4) . ? C42 C43 1.521(4) . ? C43 C44 1.545(5) . ? C44 C45 1.519(4) . ? B5 N8 1.631(3) . ? B5 C71 1.656(3) . ? B5 C61 1.657(3) . ? B5 C51 1.671(3) . ? C51 C56 1.393(3) . ? C51 C52 1.398(3) . ? C52 F52 1.374(3) . ? C52 C53 1.391(3) . ? C53 F53 1.362(3) . ? C53 C54 1.374(4) . ? C54 F54 1.354(3) . ? C54 C55 1.383(4) . ? C55 F55 1.346(3) . ? C55 C56 1.394(3) . ? C56 F56 1.356(3) . ? C61 C66 1.393(3) . ? C61 C62 1.398(3) . ? C62 F62 1.351(3) . ? C62 C63 1.393(3) . ? C63 F63 1.349(3) . ? C63 C64 1.387(4) . ? C64 F64 1.348(3) . ? C64 C65 1.375(4) . ? C65 F65 1.349(3) . ? C65 C66 1.381(3) . ? C66 F66 1.367(3) . ? C71 C76 1.390(3) . ? C71 C72 1.396(3) . ? C72 F72 1.360(3) . ? C72 C73 1.391(3) . ? C73 F73 1.350(3) . ? C73 C74 1.380(4) . ? C74 F74 1.355(3) . ? C74 C75 1.378(4) . ? C75 F75 1.351(3) . ? C75 C76 1.394(3) . ? C76 F76 1.366(3) . ? N8 C81 1.512(3) . ? N8 C85 1.514(3) . ? C81 C82 1.527(3) . ? C82 C83 1.530(3) . ? C83 C84 1.526(4) . ? C84 C85 1.531(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 N4 B1 C31 106.18(18) . . ? N4 B1 C21 109.51(18) . . ? C31 B1 C21 114.71(19) . . ? N4 B1 C11 109.57(18) . . ? C31 B1 C11 114.50(19) . . ? C21 B1 C11 102.32(18) . . ? C12 C11 C16 112.5(2) . . ? C12 C11 B1 122.6(2) . . ? C16 C11 B1 124.3(2) . . ? F12 C12 C13 115.4(2) . . ? F12 C12 C11 119.6(2) . . ? C13 C12 C11 124.9(2) . . ? F13 C13 C14 120.1(2) . . ? F13 C13 C12 120.7(2) . . ? C14 C13 C12 119.2(2) . . ? F14 C14 C13 120.4(2) . . ? F14 C14 C15 120.5(2) . . ? C13 C14 C15 119.1(2) . . ? F15 C15 C16 120.4(2) . . ? F15 C15 C14 119.7(2) . . ? C16 C15 C14 119.9(2) . . ? F16 C16 C15 114.9(2) . . ? F16 C16 C11 120.6(2) . . ? C15 C16 C11 124.5(2) . . ? C22 C21 C26 112.9(2) . . ? C22 C21 B1 120.6(2) . . ? C26 C21 B1 126.0(2) . . ? F22 C22 C23 115.7(2) . . ? F22 C22 C21 119.6(2) . . ? C23 C22 C21 124.6(2) . . ? F23 C23 C24 119.8(2) . . ? F23 C23 C22 120.6(2) . . ? C24 C23 C22 119.7(2) . . ? F24 C24 C25 120.8(2) . . ? F24 C24 C23 120.6(2) . . ? C25 C24 C23 118.5(2) . . ? F25 C25 C24 119.7(2) . . ? F25 C25 C26 120.4(2) . . ? C24 C25 C26 119.8(2) . . ? F26 C26 C25 114.6(2) . . ? F26 C26 C21 121.0(2) . . ? C25 C26 C21 124.4(2) . . ? C36 C31 C32 112.9(2) . . ? C36 C31 B1 123.6(2) . . ? C32 C31 B1 123.6(2) . . ? F32 C32 C33 116.2(2) . . ? F32 C32 C31 119.5(2) . . ? C33 C32 C31 124.2(2) . . ? F33 C33 C32 120.8(2) . . ? F33 C33 C34 119.9(2) . . ? C32 C33 C34 119.4(2) . . ? F34 C34 C35 121.0(2) . . ? F34 C34 C33 119.6(2) . . ? C35 C34 C33 119.5(2) . . ? F35 C35 C36 120.9(2) . . ? F35 C35 C34 120.1(2) . . ? C36 C35 C34 119.0(2) . . ? F36 C36 C35 115.1(2) . . ? F36 C36 C31 119.9(2) . . ? C35 C36 C31 125.0(2) . . ? C45 N4 C41 108.87(18) . . ? C45 N4 B1 115.18(19) . . ? C41 N4 B1 114.04(17) . . ? N4 C41 C42 110.1(2) . . ? C43 C42 C41 111.1(2) . . ? C42 C43 C44 110.9(2) . . ? C45 C44 C43 111.1(2) . . ? N4 C45 C44 110.7(2) . . ? N8 B5 C71 104.69(16) . . ? N8 B5 C61 109.28(17) . . ? C71 B5 C61 114.81(18) . . ? N8 B5 C51 109.51(17) . . ? C71 B5 C51 115.13(18) . . ? C61 B5 C51 103.38(17) . . ? C56 C51 C52 112.4(2) . . ? C56 C51 B5 119.71(19) . . ? C52 C51 B5 127.5(2) . . ? F52 C52 C53 114.5(2) . . ? F52 C52 C51 120.7(2) . . ? C53 C52 C51 124.8(2) . . ? F53 C53 C54 120.1(2) . . ? F53 C53 C52 120.1(2) . . ? C54 C53 C52 119.8(2) . . ? F54 C54 C53 120.9(2) . . ? F54 C54 C55 120.6(2) . . ? C53 C54 C55 118.5(2) . . ? F55 C55 C54 119.7(2) . . ? F55 C55 C56 120.7(2) . . ? C54 C55 C56 119.6(2) . . ? F56 C56 C51 119.11(19) . . ? F56 C56 C55 116.1(2) . . ? C51 C56 C55 124.8(2) . . ? C66 C61 C62 113.41(19) . . ? C66 C61 B5 122.20(19) . . ? C62 C61 B5 123.83(19) . . ? F62 C62 C63 115.63(19) . . ? F62 C62 C61 120.87(19) . . ? C63 C62 C61 123.5(2) . . ? F63 C63 C64 120.2(2) . . ? F63 C63 C62 120.3(2) . . ? C64 C63 C62 119.6(2) . . ? F64 C64 C65 120.9(2) . . ? F64 C64 C63 119.7(2) . . ? C65 C64 C63 119.4(2) . . ? F65 C65 C64 120.4(2) . . ? F65 C65 C66 120.7(2) . . ? C64 C65 C66 118.9(2) . . ? F66 C66 C65 115.15(19) . . ? F66 C66 C61 119.62(18) . . ? C65 C66 C61 125.2(2) . . ? C76 C71 C72 113.5(2) . . ? C76 C71 B5 123.42(19) . . ? C72 C71 B5 122.8(2) . . ? F72 C72 C73 115.0(2) . . ? F72 C72 C71 121.08(19) . . ? C73 C72 C71 123.9(2) . . ? F73 C73 C74 120.1(2) . . ? F73 C73 C72 120.4(2) . . ? C74 C73 C72 119.5(2) . . ? F74 C74 C75 119.9(3) . . ? F74 C74 C73 120.6(2) . . ? C75 C74 C73 119.5(2) . . ? F75 C75 C74 120.2(2) . . ? F75 C75 C76 121.1(2) . . ? C74 C75 C76 118.7(2) . . ? F76 C76 C71 120.00(19) . . ? F76 C76 C75 115.2(2) . . ? C71 C76 C75 124.8(2) . . ? C81 N8 C85 108.75(16) . . ? C81 N8 B5 116.80(16) . . ? C85 N8 B5 113.14(16) . . ? N8 C81 C82 110.15(18) . . ? C81 C82 C83 111.1(2) . . ? C84 C83 C82 111.0(2) . . ? C83 C84 C85 111.2(2) . . ? N8 C85 C84 110.23(18) . . ? 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 N4 B1 C11 C12 -38.2(3) . . . . ? C31 B1 C11 C12 -157.4(2) . . . . ? C21 B1 C11 C12 77.9(2) . . . . ? N4 B1 C11 C16 151.2(2) . . . . ? C31 B1 C11 C16 32.0(3) . . . . ? C21 B1 C11 C16 -92.7(3) . . . . ? C16 C11 C12 F12 177.5(2) . . . . ? B1 C11 C12 F12 5.9(3) . . . . ? C16 C11 C12 C13 -1.3(3) . . . . ? B1 C11 C12 C13 -172.9(2) . . . . ? F12 C12 C13 F13 1.8(3) . . . . ? C11 C12 C13 F13 -179.3(2) . . . . ? F12 C12 C13 C14 -178.2(2) . . . . ? C11 C12 C13 C14 0.6(4) . . . . ? F13 C13 C14 F14 -0.8(4) . . . . ? C12 C13 C14 F14 179.3(2) . . . . ? F13 C13 C14 C15 -179.7(2) . . . . ? C12 C13 C14 C15 0.3(4) . . . . ? F14 C14 C15 F15 0.6(4) . . . . ? C13 C14 C15 F15 179.5(2) . . . . ? F14 C14 C15 C16 -179.4(2) . . . . ? C13 C14 C15 C16 -0.4(4) . . . . ? F15 C15 C16 F16 -1.0(4) . . . . ? C14 C15 C16 F16 179.0(2) . . . . ? F15 C15 C16 C11 179.7(2) . . . . ? C14 C15 C16 C11 -0.3(4) . . . . ? C12 C11 C16 F16 -178.1(2) . . . . ? B1 C11 C16 F16 -6.7(3) . . . . ? C12 C11 C16 C15 1.1(3) . . . . ? B1 C11 C16 C15 172.6(2) . . . . ? N4 B1 C21 C22 -165.18(19) . . . . ? C31 B1 C21 C22 -45.9(3) . . . . ? C11 B1 C21 C22 78.6(2) . . . . ? N4 B1 C21 C26 23.8(3) . . . . ? C31 B1 C21 C26 143.1(2) . . . . ? C11 B1 C21 C26 -92.4(2) . . . . ? C26 C21 C22 F22 177.52(19) . . . . ? B1 C21 C22 F22 5.4(3) . . . . ? C26 C21 C22 C23 -1.2(3) . . . . ? B1 C21 C22 C23 -173.3(2) . . . . ? F22 C22 C23 F23 1.3(3) . . . . ? C21 C22 C23 F23 -179.9(2) . . . . ? F22 C22 C23 C24 -178.3(2) . . . . ? C21 C22 C23 C24 0.5(4) . . . . ? F23 C23 C24 F24 0.4(3) . . . . ? C22 C23 C24 F24 180.0(2) . . . . ? F23 C23 C24 C25 -178.7(2) . . . . ? C22 C23 C24 C25 0.9(3) . . . . ? F24 C24 C25 F25 -1.6(3) . . . . ? C23 C24 C25 F25 177.5(2) . . . . ? F24 C24 C25 C26 179.5(2) . . . . ? C23 C24 C25 C26 -1.5(3) . . . . ? F25 C25 C26 F26 0.6(3) . . . . ? C24 C25 C26 F26 179.6(2) . . . . ? F25 C25 C26 C21 -178.2(2) . . . . ? C24 C25 C26 C21 0.7(3) . . . . ? C22 C21 C26 F26 -178.19(19) . . . . ? B1 C21 C26 F26 -6.6(3) . . . . ? C22 C21 C26 C25 0.6(3) . . . . ? B1 C21 C26 C25 172.2(2) . . . . ? N4 B1 C31 C36 93.6(3) . . . . ? C21 B1 C31 C36 -27.5(3) . . . . ? C11 B1 C31 C36 -145.3(2) . . . . ? N4 B1 C31 C32 -86.2(3) . . . . ? C21 B1 C31 C32 152.8(2) . . . . ? C11 B1 C31 C32 34.9(3) . . . . ? C36 C31 C32 F32 -177.5(2) . . . . ? B1 C31 C32 F32 2.3(3) . . . . ? C36 C31 C32 C33 3.5(3) . . . . ? B1 C31 C32 C33 -176.7(2) . . . . ? F32 C32 C33 F33 -1.0(3) . . . . ? C31 C32 C33 F33 178.1(2) . . . . ? F32 C32 C33 C34 178.7(2) . . . . ? C31 C32 C33 C34 -2.3(4) . . . . ? F33 C33 C34 F34 0.1(4) . . . . ? C32 C33 C34 F34 -179.6(2) . . . . ? F33 C33 C34 C35 179.7(2) . . . . ? C32 C33 C34 C35 0.0(4) . . . . ? F34 C34 C35 F35 1.1(3) . . . . ? C33 C34 C35 F35 -178.5(2) . . . . ? F34 C34 C35 C36 -179.8(2) . . . . ? C33 C34 C35 C36 0.6(4) . . . . ? F35 C35 C36 F36 -0.2(3) . . . . ? C34 C35 C36 F36 -179.4(2) . . . . ? F35 C35 C36 C31 -179.9(2) . . . . ? C34 C35 C36 C31 0.9(4) . . . . ? C32 C31 C36 F36 177.5(2) . . . . ? B1 C31 C36 F36 -2.3(3) . . . . ? C32 C31 C36 C35 -2.8(3) . . . . ? B1 C31 C36 C35 177.4(2) . . . . ? C31 B1 N4 C45 67.1(2) . . . . ? C21 B1 N4 C45 -168.53(19) . . . . ? C11 B1 N4 C45 -57.1(2) . . . . ? C31 B1 N4 C41 -59.8(2) . . . . ? C21 B1 N4 C41 64.5(2) . . . . ? C11 B1 N4 C41 176.00(19) . . . . ? C45 N4 C41 C42 61.1(3) . . . . ? B1 N4 C41 C42 -168.8(2) . . . . ? N4 C41 C42 C43 -58.1(3) . . . . ? C41 C42 C43 C44 53.7(3) . . . . ? C42 C43 C44 C45 -53.2(3) . . . . ? C41 N4 C45 C44 -60.9(3) . . . . ? B1 N4 C45 C44 169.6(2) . . . . ? C43 C44 C45 N4 57.2(3) . . . . ? N8 B5 C51 C56 167.45(18) . . . . ? C71 B5 C51 C56 49.8(3) . . . . ? C61 B5 C51 C56 -76.2(2) . . . . ? N8 B5 C51 C52 -20.6(3) . . . . ? C71 B5 C51 C52 -138.2(2) . . . . ? C61 B5 C51 C52 95.8(2) . . . . ? C56 C51 C52 F52 179.14(19) . . . . ? B5 C51 C52 F52 6.7(4) . . . . ? C56 C51 C52 C53 -1.3(3) . . . . ? B5 C51 C52 C53 -173.7(2) . . . . ? F52 C52 C53 F53 0.3(3) . . . . ? C51 C52 C53 F53 -179.3(2) . . . . ? F52 C52 C53 C54 -178.9(2) . . . . ? C51 C52 C53 C54 1.5(4) . . . . ? F53 C53 C54 F54 0.4(4) . . . . ? C52 C53 C54 F54 179.6(2) . . . . ? F53 C53 C54 C55 179.7(2) . . . . ? C52 C53 C54 C55 -1.0(4) . . . . ? F54 C54 C55 F55 -0.5(4) . . . . ? C53 C54 C55 F55 -179.8(2) . . . . ? F54 C54 C55 C56 179.9(2) . . . . ? C53 C54 C55 C56 0.5(4) . . . . ? C52 C51 C56 F56 179.80(19) . . . . ? B5 C51 C56 F56 -7.1(3) . . . . ? C52 C51 C56 C55 0.7(3) . . . . ? B5 C51 C56 C55 173.8(2) . . . . ? F55 C55 C56 F56 0.9(3) . . . . ? C54 C55 C56 F56 -179.5(2) . . . . ? F55 C55 C56 C51 179.9(2) . . . . ? C54 C55 C56 C51 -0.4(4) . . . . ? N8 B5 C61 C66 40.6(3) . . . . ? C71 B5 C61 C66 157.89(19) . . . . ? C51 B5 C61 C66 -75.9(2) . . . . ? N8 B5 C61 C62 -148.53(19) . . . . ? C71 B5 C61 C62 -31.3(3) . . . . ? C51 B5 C61 C62 94.9(2) . . . . ? C66 C61 C62 F62 178.56(18) . . . . ? B5 C61 C62 F62 7.0(3) . . . . ? C66 C61 C62 C63 -0.7(3) . . . . ? B5 C61 C62 C63 -172.2(2) . . . . ? F62 C62 C63 F63 -0.1(3) . . . . ? C61 C62 C63 F63 179.2(2) . . . . ? F62 C62 C63 C64 -179.4(2) . . . . ? C61 C62 C63 C64 -0.1(3) . . . . ? F63 C63 C64 F64 0.8(3) . . . . ? C62 C63 C64 F64 -179.96(19) . . . . ? F63 C63 C64 C65 -179.3(2) . . . . ? C62 C63 C64 C65 -0.1(3) . . . . ? F64 C64 C65 F65 -0.6(3) . . . . ? C63 C64 C65 F65 179.5(2) . . . . ? F64 C64 C65 C66 -179.1(2) . . . . ? C63 C64 C65 C66 1.0(3) . . . . ? F65 C65 C66 F66 -1.4(3) . . . . ? C64 C65 C66 F66 177.0(2) . . . . ? F65 C65 C66 C61 179.5(2) . . . . ? C64 C65 C66 C61 -2.0(3) . . . . ? C62 C61 C66 F66 -177.25(19) . . . . ? B5 C61 C66 F66 -5.6(3) . . . . ? C62 C61 C66 C65 1.7(3) . . . . ? B5 C61 C66 C65 173.4(2) . . . . ? N8 B5 C71 C76 78.6(2) . . . . ? C61 B5 C71 C76 -41.2(3) . . . . ? C51 B5 C71 C76 -161.13(19) . . . . ? N8 B5 C71 C72 -94.6(2) . . . . ? C61 B5 C71 C72 145.6(2) . . . . ? C51 B5 C71 C72 25.7(3) . . . . ? C76 C71 C72 F72 -179.15(18) . . . . ? B5 C71 C72 F72 -5.4(3) . . . . ? C76 C71 C72 C73 -0.3(3) . . . . ? B5 C71 C72 C73 173.4(2) . . . . ? F72 C72 C73 F73 -1.5(3) . . . . ? C71 C72 C73 F73 179.6(2) . . . . ? F72 C72 C73 C74 177.7(2) . . . . ? C71 C72 C73 C74 -1.2(3) . . . . ? F73 C73 C74 F74 1.8(3) . . . . ? C72 C73 C74 F74 -177.3(2) . . . . ? F73 C73 C74 C75 -178.8(2) . . . . ? C72 C73 C74 C75 2.1(4) . . . . ? F74 C74 C75 F75 0.0(3) . . . . ? C73 C74 C75 F75 -179.4(2) . . . . ? F74 C74 C75 C76 178.1(2) . . . . ? C73 C74 C75 C76 -1.3(4) . . . . ? C72 C71 C76 F76 179.72(18) . . . . ? B5 C71 C76 F76 6.0(3) . . . . ? C72 C71 C76 C75 1.1(3) . . . . ? B5 C71 C76 C75 -172.6(2) . . . . ? F75 C75 C76 F76 -0.9(3) . . . . ? C74 C75 C76 F76 -179.0(2) . . . . ? F75 C75 C76 C71 177.7(2) . . . . ? C74 C75 C76 C71 -0.3(4) . . . . ? C71 B5 N8 C81 -71.4(2) . . . . ? C61 B5 N8 C81 52.1(2) . . . . ? C51 B5 N8 C81 164.64(17) . . . . ? C71 B5 N8 C85 56.0(2) . . . . ? C61 B5 N8 C85 179.47(17) . . . . ? C51 B5 N8 C85 -67.9(2) . . . . ? C85 N8 C81 C82 61.6(2) . . . . ? B5 N8 C81 C82 -168.87(18) . . . . ? N8 C81 C82 C83 -58.1(2) . . . . ? C81 C82 C83 C84 53.4(3) . . . . ? C82 C83 C84 C85 -53.1(3) . . . . ? C81 N8 C85 C84 -61.2(2) . . . . ? B5 N8 C85 C84 167.23(18) . . . . ? C83 C84 C85 N8 57.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.147 _refine_diff_density_min -0.149 _refine_diff_density_rms 0.035