# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email jan.paradies@kit.edu _publ_contact_author_phone ? _publ_contact_author_name 'Jan Paradies' loop_ _publ_author_name L.Greb P.Ona-Burgos A.Kubas F.Falk F.Breher K.Fink J.Paradies data_gemphoshbf4_1 _database_code_depnum_ccdc_archive 'CCDC 867393' #TrackingRef '- 2aHBF4-CCDC867393.txt' _audit_creation_date 2012-03-20 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common Gemphos _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H35 P2, B F4' _chemical_formula_sum 'C40 H35 B F4 P2' _chemical_formula_weight 664.43 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0035 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 0.0014 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0179 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1043 0.0967 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' _cell_length_a 9.6069(19) _cell_length_b 17.796(4) _cell_length_c 10.210(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.14(3) _cell_angle_gamma 90.00 _cell_volume 1668.0(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 12279 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 29.49 _cell_measurement_theta_min 2.07 _exptl_absorpt_coefficient_mu 0.19 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 692 _exptl_crystal_size_max 0.616 _exptl_crystal_size_mid 0.256 _exptl_crystal_size_min 0.143 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0440 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 15812 _diffrn_reflns_theta_full 29.15 _diffrn_reflns_theta_max 29.15 _diffrn_reflns_theta_min 2.09 _diffrn_ambient_temperature 200.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7301 _reflns_number_total 8685 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.421 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.043 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(6) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 428 _refine_ls_number_reflns 8685 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0411 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.0990 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 H1 H 0.396(3) 0.7547(14) 0.412(2) 0.043(6) Uiso 1 1 d . . . C1 C 0.3991(2) 0.55589(14) 0.3557(2) 0.0465(5) Uani 1 1 d . . . H1A H 0.4388 0.5888 0.2972 0.056 Uiso 1 1 calc R . . H1B H 0.4614 0.5106 0.3776 0.056 Uiso 1 1 calc R . . C2 C 0.4081(2) 0.59883(14) 0.4936(3) 0.0504(5) Uani 1 1 d . . . H2A H 0.4568 0.5662 0.5723 0.061 Uiso 1 1 calc R . . H2B H 0.4681 0.6446 0.4994 0.061 Uiso 1 1 calc R . . C3 C 0.2591(2) 0.62092(11) 0.5035(2) 0.0391(4) Uani 1 1 d . . . C4 C 0.1814(2) 0.68558(10) 0.44285(19) 0.0331(4) Uani 1 1 d . . . C5 C 0.0288(2) 0.68548(10) 0.3992(2) 0.0342(4) Uani 1 1 d . . . H5 H -0.0225 0.7286 0.3554 0.041 Uiso 1 1 calc R . . C6 C -0.0484(2) 0.62209(11) 0.4200(2) 0.0381(4) Uani 1 1 d . . . C7 C 0.0292(3) 0.56870(12) 0.5114(2) 0.0447(5) Uani 1 1 d . . . H7 H -0.0218 0.5326 0.5482 0.054 Uiso 1 1 calc R . . C8 C 0.1791(3) 0.56714(12) 0.5497(2) 0.0473(5) Uani 1 1 d . . . H8 H 0.2293 0.5284 0.6090 0.057 Uiso 1 1 calc R . . C9 C -0.2010(2) 0.60496(13) 0.3306(3) 0.0486(5) Uani 1 1 d . . . H9A H -0.2381 0.6480 0.2688 0.058 Uiso 1 1 calc R . . H9B H -0.2659 0.5980 0.3890 0.058 Uiso 1 1 calc R . . C10 C -0.2038(2) 0.53170(12) 0.2423(2) 0.0434(5) Uani 1 1 d . . . H10A H -0.2299 0.4880 0.2902 0.052 Uiso 1 1 calc R . . H10B H -0.2794 0.5371 0.1528 0.052 Uiso 1 1 calc R . . C11 C 0.0014(2) 0.57296(11) 0.15355(19) 0.0349(4) Uani 1 1 d . . . H11 H -0.0620 0.6060 0.0902 0.042 Uiso 1 1 calc R . . C12 C 0.1519(2) 0.58078(10) 0.17958(18) 0.0323(4) Uani 1 1 d . . . C13 C 0.2459(2) 0.53227(11) 0.2753(2) 0.0366(4) Uani 1 1 d . . . C14 C 0.1846(3) 0.46748(12) 0.3120(2) 0.0443(5) Uani 1 1 d . . . H14 H 0.2462 0.4276 0.3567 0.053 Uiso 1 1 calc R . . C15 C 0.0342(3) 0.46044(11) 0.2840(2) 0.0425(5) Uani 1 1 d . . . H15 H -0.0055 0.4160 0.3101 0.051 Uiso 1 1 calc R . . C16 C -0.0581(2) 0.51767(11) 0.2185(2) 0.0369(4) Uani 1 1 d . . . C17 C 0.3326(2) 0.80718(10) 0.61159(19) 0.0331(4) Uani 1 1 d . . . C18 C 0.4597(2) 0.84977(12) 0.6580(2) 0.0417(4) Uani 1 1 d . . . H18 H 0.5184 0.8592 0.5994 0.050 Uiso 1 1 calc R . . C19 C 0.4995(3) 0.87806(13) 0.7896(2) 0.0474(5) Uani 1 1 d . . . H19 H 0.5857 0.9072 0.8216 0.057 Uiso 1 1 calc R . . C20 C 0.4147(3) 0.86424(12) 0.8747(2) 0.0462(5) Uani 1 1 d . . . H20 H 0.4442 0.8828 0.9660 0.055 Uiso 1 1 calc R . . C21 C 0.2868(3) 0.82356(13) 0.8281(2) 0.0476(5) Uani 1 1 d . . . H21 H 0.2268 0.8157 0.8860 0.057 Uiso 1 1 calc R . . C22 C 0.2468(2) 0.79428(12) 0.6964(2) 0.0421(4) Uani 1 1 d . . . H22 H 0.1602 0.7653 0.6646 0.051 Uiso 1 1 calc R . . C23 C 0.1915(2) 0.84140(10) 0.32100(19) 0.0335(4) Uani 1 1 d . . . C24 C 0.2533(2) 0.86524(12) 0.2204(2) 0.0404(4) Uani 1 1 d . . . H24 H 0.3422 0.8440 0.2150 0.048 Uiso 1 1 calc R . . C25 C 0.1832(3) 0.92030(13) 0.1285(2) 0.0484(5) Uani 1 1 d . . . H25 H 0.2245 0.9374 0.0600 0.058 Uiso 1 1 calc R . . C26 C 0.0535(3) 0.95031(13) 0.1363(2) 0.0527(6) Uani 1 1 d . . . H26 H 0.0055 0.9876 0.0722 0.063 Uiso 1 1 calc R . . C27 C -0.0074(3) 0.92700(13) 0.2358(2) 0.0474(5) Uani 1 1 d . . . H27 H -0.0975 0.9477 0.2391 0.057 Uiso 1 1 calc R . . C28 C 0.0627(2) 0.87316(11) 0.3314(2) 0.0384(4) Uani 1 1 d . . . H28 H 0.0234 0.8584 0.4026 0.046 Uiso 1 1 calc R . . C29 C 0.0708(2) 0.69566(11) -0.0226(2) 0.0359(4) Uani 1 1 d . . . C30 C -0.0171(3) 0.75146(12) 0.0086(2) 0.0458(5) Uani 1 1 d . . . H30 H 0.0061 0.7709 0.0992 0.055 Uiso 1 1 calc R . . C31 C -0.1378(3) 0.77870(15) -0.0916(3) 0.0547(6) Uani 1 1 d . . . H31 H -0.1977 0.8159 -0.0688 0.066 Uiso 1 1 calc R . . C32 C -0.1711(3) 0.75201(15) -0.2234(3) 0.0555(6) Uani 1 1 d . . . H32 H -0.2521 0.7718 -0.2923 0.067 Uiso 1 1 calc R . . C33 C -0.0867(3) 0.69660(17) -0.2553(2) 0.0550(6) Uani 1 1 d . . . H33 H -0.1109 0.6775 -0.3462 0.066 Uiso 1 1 calc R . . C34 C 0.0342(2) 0.66822(14) -0.1552(2) 0.0442(4) Uani 1 1 d . . . H34 H 0.0917 0.6299 -0.1782 0.053 Uiso 1 1 calc R . . C35 C 0.3497(2) 0.62499(12) 0.0284(2) 0.0390(4) Uani 1 1 d . . . C36 C 0.4628(2) 0.67074(17) 0.0171(3) 0.0543(6) Uani 1 1 d . . . H36 H 0.4772 0.7184 0.0610 0.065 Uiso 1 1 calc R . . C37 C 0.5548(3) 0.6480(2) -0.0569(3) 0.0711(9) Uani 1 1 d . . . H37 H 0.6299 0.6806 -0.0655 0.085 Uiso 1 1 calc R . . C38 C 0.5382(3) 0.5784(2) -0.1183(3) 0.0748(10) Uani 1 1 d . . . H38 H 0.6014 0.5633 -0.1696 0.090 Uiso 1 1 calc R . . C39 C 0.4295(3) 0.53028(18) -0.1055(2) 0.0612(7) Uani 1 1 d . . . H39 H 0.4190 0.4819 -0.1467 0.073 Uiso 1 1 calc R . . C40 C 0.3353(3) 0.55325(14) -0.0316(2) 0.0470(5) Uani 1 1 d . . . H40 H 0.2612 0.5202 -0.0220 0.056 Uiso 1 1 calc R . . P1 P 0.28237(5) 0.77009(3) 0.43955(5) 0.03182(10) Uani 1 1 d . . . P2 P 0.22714(5) 0.66409(3) 0.11874(5) 0.03447(11) Uani 1 1 d . . . B1 B 0.6765(4) 0.8241(2) 0.3607(4) 0.0645(8) Uani 1 1 d . . . F1 F 0.8115(2) 0.83086(16) 0.4533(2) 0.0981(7) Uani 1 1 d . . . F2 F 0.5907(2) 0.88367(14) 0.3836(3) 0.1059(7) Uani 1 1 d . . . F3 F 0.6139(2) 0.75907(13) 0.3860(3) 0.1190(9) Uani 1 1 d . . . F4 F 0.6888(4) 0.8219(2) 0.2337(3) 0.1692(16) 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 C1 0.0350(10) 0.0559(13) 0.0475(11) 0.0074(10) 0.0106(9) 0.0085(10) C2 0.0372(11) 0.0436(11) 0.0589(13) -0.0014(10) -0.0037(9) 0.0053(9) C3 0.0416(11) 0.0355(9) 0.0341(9) -0.0023(7) 0.0017(8) 0.0011(8) C4 0.0370(9) 0.0308(9) 0.0317(8) -0.0042(6) 0.0107(7) -0.0009(7) C5 0.0354(9) 0.0301(9) 0.0392(9) -0.0036(7) 0.0141(7) -0.0006(7) C6 0.0413(11) 0.0363(9) 0.0431(10) -0.0069(8) 0.0221(8) -0.0047(8) C7 0.0594(14) 0.0403(10) 0.0374(10) -0.0006(8) 0.0191(9) -0.0117(10) C8 0.0626(14) 0.0368(10) 0.0358(10) 0.0034(8) 0.0041(9) -0.0021(10) C9 0.0374(11) 0.0441(12) 0.0676(14) -0.0058(10) 0.0204(10) -0.0061(9) C10 0.0413(11) 0.0398(10) 0.0482(11) -0.0018(8) 0.0116(9) -0.0121(9) C11 0.0387(10) 0.0319(9) 0.0321(9) -0.0038(7) 0.0073(7) -0.0015(8) C12 0.0389(9) 0.0289(8) 0.0305(8) -0.0047(6) 0.0122(7) -0.0009(7) C13 0.0383(10) 0.0361(9) 0.0368(9) -0.0019(7) 0.0129(8) 0.0059(8) C14 0.0509(12) 0.0349(10) 0.0483(11) 0.0039(8) 0.0167(9) 0.0094(9) C15 0.0539(12) 0.0287(9) 0.0463(11) -0.0003(8) 0.0169(9) -0.0041(9) C16 0.0407(10) 0.0314(9) 0.0367(9) -0.0069(7) 0.0086(8) -0.0070(8) C17 0.0333(9) 0.0293(9) 0.0344(9) -0.0006(7) 0.0068(7) -0.0003(7) C18 0.0332(10) 0.0419(10) 0.0496(11) -0.0030(8) 0.0114(8) -0.0067(8) C19 0.0406(11) 0.0426(11) 0.0509(11) -0.0029(9) 0.0008(9) -0.0059(9) C20 0.0585(13) 0.0369(10) 0.0363(10) -0.0035(8) 0.0033(9) 0.0017(9) C21 0.0624(14) 0.0427(11) 0.0417(11) -0.0007(9) 0.0214(10) -0.0095(10) C22 0.0471(11) 0.0389(9) 0.0413(10) -0.0055(8) 0.0147(9) -0.0122(9) C23 0.0363(9) 0.0304(8) 0.0332(9) -0.0007(7) 0.0096(7) -0.0020(7) C24 0.0399(11) 0.0401(10) 0.0443(10) 0.0015(8) 0.0173(8) -0.0035(9) C25 0.0588(14) 0.0452(11) 0.0467(11) 0.0094(9) 0.0241(10) -0.0040(11) C26 0.0673(16) 0.0433(12) 0.0488(12) 0.0136(10) 0.0191(11) 0.0128(11) C27 0.0521(13) 0.0429(11) 0.0503(12) 0.0025(9) 0.0196(10) 0.0136(10) C28 0.0449(11) 0.0356(9) 0.0381(9) -0.0002(8) 0.0176(8) 0.0016(8) C29 0.0359(9) 0.0335(9) 0.0385(9) 0.0043(7) 0.0114(8) -0.0015(8) C30 0.0434(11) 0.0427(11) 0.0489(11) -0.0042(9) 0.0100(9) 0.0028(9) C31 0.0469(12) 0.0488(13) 0.0660(14) -0.0003(11) 0.0128(10) 0.0120(11) C32 0.0473(12) 0.0663(16) 0.0502(12) 0.0124(11) 0.0104(10) 0.0107(11) C33 0.0538(13) 0.0753(16) 0.0346(11) -0.0001(10) 0.0111(10) 0.0083(12) C34 0.0453(11) 0.0498(11) 0.0395(10) 0.0000(9) 0.0155(8) 0.0062(11) C35 0.0321(9) 0.0472(11) 0.0380(9) 0.0061(8) 0.0108(7) 0.0070(8) C36 0.0420(11) 0.0633(14) 0.0596(13) 0.0192(12) 0.0181(10) 0.0043(12) C37 0.0525(15) 0.096(2) 0.0750(18) 0.0371(17) 0.0340(13) 0.0172(15) C38 0.0561(15) 0.125(3) 0.0510(14) 0.0267(17) 0.0271(12) 0.0401(18) C39 0.0631(16) 0.0791(18) 0.0379(11) 0.0021(11) 0.0094(11) 0.0341(15) C40 0.0441(11) 0.0539(13) 0.0405(10) -0.0029(9) 0.0085(9) 0.0102(10) P1 0.0297(2) 0.0317(2) 0.0349(2) -0.00087(19) 0.01088(17) -0.0005(2) P2 0.0349(2) 0.0316(2) 0.0366(2) -0.00131(19) 0.00993(18) -0.0010(2) B1 0.0473(16) 0.075(2) 0.074(2) -0.0107(16) 0.0234(14) -0.0147(15) F1 0.0513(10) 0.1398(19) 0.1067(16) -0.0295(14) 0.0285(10) -0.0063(11) F2 0.0754(13) 0.0872(14) 0.141(2) -0.0129(14) 0.0096(13) 0.0111(12) F3 0.0871(14) 0.0785(13) 0.226(3) -0.0062(17) 0.0989(18) -0.0132(12) F4 0.215(3) 0.229(4) 0.0756(15) -0.0460(19) 0.0630(19) -0.110(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.582(3) . ? C1 C13 1.518(3) . ? C2 C3 1.516(3) . ? C3 C4 1.411(3) . ? C3 C8 1.394(3) . ? C4 C5 1.401(3) . ? C4 P1 1.7951(19) . ? C5 C6 1.400(3) . ? C6 C7 1.385(3) . ? C6 C9 1.512(3) . ? C7 C8 1.377(4) . ? C9 C10 1.581(3) . ? C10 C16 1.510(3) . ? C11 C12 1.397(3) . ? C11 C16 1.400(3) . ? C12 C13 1.413(3) . ? C12 P2 1.836(2) . ? C13 C14 1.395(3) . ? C14 C15 1.393(3) . ? C15 C16 1.386(3) . ? C17 C18 1.396(3) . ? C17 C22 1.380(3) . ? C17 P1 1.8039(19) . ? C18 C19 1.379(3) . ? C19 C20 1.377(4) . ? C20 C21 1.384(3) . ? C21 C22 1.387(3) . ? C23 C24 1.396(3) . ? C23 C28 1.392(3) . ? C23 P1 1.793(2) . ? C24 C25 1.386(3) . ? C25 C26 1.380(4) . ? C26 C27 1.377(3) . ? C27 C28 1.392(3) . ? C29 C30 1.400(3) . ? C29 C34 1.383(3) . ? C29 P2 1.838(2) . ? C30 C31 1.388(3) . ? C31 C32 1.373(4) . ? C32 C33 1.375(4) . ? C33 C34 1.396(3) . ? C35 C36 1.390(3) . ? C35 C40 1.405(3) . ? C35 P2 1.833(2) . ? C36 C37 1.382(4) . ? C37 C38 1.376(5) . ? C38 C39 1.386(5) . ? C39 C40 1.399(3) . ? B1 F1 1.367(4) . ? B1 F2 1.403(4) . ? B1 F3 1.364(4) . ? B1 F4 1.337(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 C1 C2 113.89(18) . . ? C3 C2 C1 112.31(17) . . ? C4 C3 C2 124.7(2) . . ? C8 C3 C2 118.0(2) . . ? C8 C3 C4 115.8(2) . . ? C3 C4 P1 118.22(15) . . ? C5 C4 C3 120.44(18) . . ? C5 C4 P1 121.03(14) . . ? C6 C5 C4 120.29(18) . . ? C5 C6 C9 122.23(19) . . ? C7 C6 C5 116.79(19) . . ? C7 C6 C9 120.13(19) . . ? C8 C7 C6 121.0(2) . . ? C7 C8 C3 121.7(2) . . ? C6 C9 C10 111.20(18) . . ? C16 C10 C9 111.53(16) . . ? C12 C11 C16 121.61(18) . . ? C11 C12 C13 119.05(18) . . ? C11 C12 P2 120.29(14) . . ? C13 C12 P2 119.48(15) . . ? C12 C13 C1 121.69(19) . . ? C14 C13 C1 120.15(19) . . ? C14 C13 C12 117.14(19) . . ? C15 C14 C13 120.90(19) . . ? C16 C15 C14 120.67(19) . . ? C11 C16 C10 119.18(18) . . ? C15 C16 C10 122.37(19) . . ? C15 C16 C11 116.9(2) . . ? C18 C17 P1 119.04(16) . . ? C22 C17 C18 120.14(18) . . ? C22 C17 P1 120.82(14) . . ? C19 C18 C17 119.5(2) . . ? C20 C19 C18 120.3(2) . . ? C19 C20 C21 120.4(2) . . ? C20 C21 C22 119.6(2) . . ? C17 C22 C21 120.0(2) . . ? C24 C23 P1 118.93(16) . . ? C28 C23 C24 120.88(18) . . ? C28 C23 P1 120.18(15) . . ? C25 C24 C23 119.1(2) . . ? C26 C25 C24 120.1(2) . . ? C27 C26 C25 120.9(2) . . ? C26 C27 C28 120.1(2) . . ? C23 C28 C27 118.89(19) . . ? C30 C29 P2 116.50(16) . . ? C34 C29 C30 118.49(19) . . ? C34 C29 P2 125.02(16) . . ? C31 C30 C29 120.6(2) . . ? C32 C31 C30 120.3(2) . . ? C31 C32 C33 119.8(2) . . ? C32 C33 C34 120.5(2) . . ? C29 C34 C33 120.3(2) . . ? C36 C35 C40 118.4(2) . . ? C36 C35 P2 116.95(19) . . ? C40 C35 P2 124.66(17) . . ? C37 C36 C35 121.0(3) . . ? C38 C37 C36 120.4(3) . . ? C37 C38 C39 120.2(3) . . ? C38 C39 C40 119.7(3) . . ? C39 C40 C35 120.3(3) . . ? C4 P1 C17 106.22(9) . . ? C23 P1 C4 116.57(9) . . ? C23 P1 C17 109.62(9) . . ? C12 P2 C29 101.57(9) . . ? C35 P2 C12 103.83(9) . . ? C35 P2 C29 102.60(9) . . ? F1 B1 F2 107.6(3) . . ? F3 B1 F1 108.9(3) . . ? F3 B1 F2 107.2(3) . . ? F4 B1 F1 109.7(3) . . ? F4 B1 F2 114.1(4) . . ? F4 B1 F3 109.2(3) . . ? # Attachment '- 2bHBF4-CCDC867456.txt' data_lg2m _database_code_depnum_ccdc_archive 'CCDC 867456' #TrackingRef '- 2bHBF4-CCDC867456.txt' _audit_creation_date 2012-03-20 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H47 P2, B F4' _chemical_formula_sum 'C40 H47 B F4 P2' _chemical_formula_weight 676.53 _chemical_absolute_configuration ad _chemical_melting_point ? 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' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' _cell_length_a 9.4616(19) _cell_length_b 18.149(4) _cell_length_c 10.749(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.34(3) _cell_angle_gamma 90.00 _cell_volume 1741.7(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7917 _cell_measurement_temperature 200 _cell_measurement_theta_max 23.57 _cell_measurement_theta_min 2.01 _exptl_absorpt_coefficient_mu 0.18 _exptl_absorpt_correction_T_max 0.9162 _exptl_absorpt_correction_T_min 0.6391 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 716 _exptl_crystal_size_max 0.376 _exptl_crystal_size_mid 0.297 _exptl_crystal_size_min 0.203 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1477 _diffrn_reflns_av_unetI/netI 0.1538 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 14298 _diffrn_reflns_theta_full 26.75 _diffrn_reflns_theta_max 26.75 _diffrn_reflns_theta_min 2.01 _diffrn_ambient_temperature 200.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4018 _reflns_number_total 7282 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.696 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.075 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(17) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 416 _refine_ls_number_reflns 7282 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1290 _refine_ls_R_factor_gt 0.0836 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2051 _refine_ls_wR_factor_ref 0.2270 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.28822(19) 0.39637(9) 0.12233(14) 0.0512(4) Uani 1 1 d . . . P2 P 0.31728(17) 0.27800(8) 0.44784(13) 0.0454(4) Uani 1 1 d . . . H2 H 0.407(5) 0.280(3) 0.387(5) 0.034(12) Uiso 1 1 d . . . F1 F -0.3127(7) 0.2889(4) 0.4358(6) 0.1203(19) Uiso 1 1 d . A . F2 F -0.1454(7) 0.2014(4) 0.4277(6) 0.1167(18) Uiso 1 1 d . A . F3A F -0.2589(17) 0.2799(10) 0.2727(15) 0.134(4) Uiso 0.50 1 d P A 1 F3B F -0.3164(14) 0.2365(8) 0.2370(13) 0.112(4) Uiso 0.50 1 d P A 2 F4A F -0.3870(13) 0.1793(6) 0.3951(12) 0.100(3) Uiso 0.50 1 d P A 2 F4B F -0.3929(18) 0.1869(8) 0.3002(17) 0.139(5) Uiso 0.50 1 d P A 1 C1 C 0.4512(7) 0.5060(3) 0.3541(6) 0.0563(16) Uani 1 1 d . . . H1A H 0.4969 0.5522 0.3981 0.068 Uiso 1 1 calc R . . H1B H 0.5008 0.4927 0.2893 0.068 Uiso 1 1 calc R . . C2 C 0.4792(7) 0.4411(4) 0.4629(6) 0.0571(16) Uani 1 1 d . . . H2A H 0.5023 0.3948 0.4251 0.069 Uiso 1 1 calc R . . H2B H 0.5671 0.4540 0.5403 0.069 Uiso 1 1 calc R . . C3 C 0.3461(7) 0.4288(3) 0.5075(5) 0.0462(13) Uani 1 1 d . . . C4 C 0.2487(7) 0.3669(3) 0.4723(5) 0.0473(14) Uani 1 1 d . . . C5 C 0.0996(7) 0.3721(3) 0.4702(5) 0.0477(14) Uani 1 1 d . . . H5 H 0.0361 0.3301 0.4494 0.057 Uiso 1 1 calc R . . C6 C 0.0445(7) 0.4402(3) 0.4991(6) 0.0503(14) Uani 1 1 d . . . C7 C 0.1519(8) 0.4914(4) 0.5654(5) 0.0572(16) Uani 1 1 d . . . H7 H 0.1240 0.5308 0.6107 0.069 Uiso 1 1 calc R . . C8 C 0.2986(8) 0.4866(4) 0.5673(5) 0.0557(16) Uani 1 1 d . . . H8 H 0.3681 0.5238 0.6106 0.067 Uiso 1 1 calc R . . C9 C -0.1167(7) 0.4607(4) 0.4379(6) 0.0603(17) Uani 1 1 d . . . H9A H -0.1395 0.5030 0.4864 0.072 Uiso 1 1 calc R . . H9B H -0.1802 0.4188 0.4457 0.072 Uiso 1 1 calc R . . C10 C -0.1557(8) 0.4818(5) 0.2892(7) 0.0665(18) Uani 1 1 d . . . H10A H -0.2019 0.4387 0.2344 0.080 Uiso 1 1 calc R . . H10B H -0.2308 0.5220 0.2681 0.080 Uiso 1 1 calc R . . C11 C -0.0199(7) 0.5068(4) 0.2522(6) 0.0560(16) Uani 1 1 d . . . C12 C 0.0440(7) 0.4598(3) 0.1861(5) 0.0493(14) Uani 1 1 d . . . H12 H -0.0157 0.4220 0.1330 0.059 Uiso 1 1 calc R . . C13 C 0.1957(7) 0.4657(3) 0.1945(5) 0.0495(14) Uani 1 1 d . . . C14 C 0.2852(7) 0.5186(3) 0.2821(5) 0.0470(14) Uani 1 1 d . . . C15 C 0.2098(9) 0.5751(3) 0.3209(6) 0.0579(17) Uani 1 1 d . . . H15 H 0.2631 0.6186 0.3575 0.069 Uiso 1 1 calc R . . C16 C 0.0577(8) 0.5700(4) 0.3081(6) 0.0591(17) Uani 1 1 d . . . H16 H 0.0090 0.6089 0.3370 0.071 Uiso 1 1 calc R . . C17 C 0.1715(7) 0.2140(3) 0.3538(5) 0.0494(14) Uani 1 1 d . . . H17 H 0.1004 0.2045 0.4032 0.059 Uiso 1 1 calc R . . C18 C 0.0847(8) 0.2480(4) 0.2171(6) 0.0560(16) Uani 1 1 d . . . H18A H 0.0261 0.2909 0.2293 0.067 Uiso 1 1 calc R . . H18B H 0.1571 0.2656 0.1751 0.067 Uiso 1 1 calc R . . C19 C -0.0211(8) 0.1921(4) 0.1264(6) 0.0642(18) Uani 1 1 d . . . H19A H -0.1011 0.1790 0.1629 0.077 Uiso 1 1 calc R . . H19B H -0.0690 0.2146 0.0385 0.077 Uiso 1 1 calc R . . C20 C 0.0610(9) 0.1233(4) 0.1117(6) 0.0646(18) Uani 1 1 d . . . H20A H 0.1366 0.1356 0.0696 0.077 Uiso 1 1 calc R . . H20B H -0.0106 0.0877 0.0541 0.077 Uiso 1 1 calc R . . C21 C 0.1387(8) 0.0881(4) 0.2466(7) 0.0599(16) Uani 1 1 d . . . H21A H 0.0622 0.0735 0.2863 0.072 Uiso 1 1 calc R . . H21B H 0.1922 0.0431 0.2352 0.072 Uiso 1 1 calc R . . C22 C 0.2490(8) 0.1407(3) 0.3389(7) 0.0568(16) Uani 1 1 d . . . H22A H 0.3315 0.1512 0.3040 0.068 Uiso 1 1 calc R . . H22B H 0.2928 0.1173 0.4264 0.068 Uiso 1 1 calc R . . C23 C 0.4255(7) 0.2365(3) 0.6075(5) 0.0487(14) Uani 1 1 d . . . H23 H 0.4801 0.1926 0.5899 0.058 Uiso 1 1 calc R . . C24 C 0.5398(7) 0.2897(4) 0.6924(6) 0.0595(17) Uani 1 1 d . . . H24A H 0.4883 0.3346 0.7074 0.071 Uiso 1 1 calc R . . H24B H 0.6101 0.3043 0.6460 0.071 Uiso 1 1 calc R . . C25 C 0.6278(9) 0.2546(4) 0.8256(6) 0.071(2) Uani 1 1 d . . . H25A H 0.6856 0.2120 0.8110 0.085 Uiso 1 1 calc R . . H25B H 0.6995 0.2910 0.8807 0.085 Uiso 1 1 calc R . . C26 C 0.5228(9) 0.2294(4) 0.8968(6) 0.070(2) Uani 1 1 d . . . H26A H 0.4698 0.2725 0.9168 0.084 Uiso 1 1 calc R . . H26B H 0.5809 0.2058 0.9812 0.084 Uiso 1 1 calc R . . C27 C 0.4093(9) 0.1750(4) 0.8116(6) 0.0648(18) Uani 1 1 d . . . H27A H 0.3407 0.1591 0.8588 0.078 Uiso 1 1 calc R . . H27B H 0.4623 0.1308 0.7956 0.078 Uiso 1 1 calc R . . C28 C 0.3182(8) 0.2098(4) 0.6793(6) 0.0579(16) Uani 1 1 d . . . H28A H 0.2594 0.2519 0.6944 0.069 Uiso 1 1 calc R . . H28B H 0.2474 0.1731 0.6241 0.069 Uiso 1 1 calc R . . C29 C 0.1411(8) 0.3637(3) -0.0274(6) 0.0519(15) Uani 1 1 d . . . C30 C 0.0281(8) 0.4065(4) -0.1113(6) 0.0670(19) Uani 1 1 d . . . H30 H 0.0175 0.4564 -0.0890 0.080 Uiso 1 1 calc R . . C31 C -0.0693(9) 0.3777(5) -0.2268(7) 0.072(2) Uani 1 1 d . . . H31 H -0.1455 0.4082 -0.2829 0.086 Uiso 1 1 calc R . . C32 C -0.0583(9) 0.3070(4) -0.2617(6) 0.070(2) Uani 1 1 d . . . H32 H -0.1265 0.2880 -0.3413 0.085 Uiso 1 1 calc R . . C33 C 0.0519(9) 0.2628(4) -0.1813(7) 0.071(2) Uani 1 1 d . . . H33 H 0.0600 0.2128 -0.2042 0.085 Uiso 1 1 calc R . . C34 C 0.1525(8) 0.2922(4) -0.0652(6) 0.0595(17) Uani 1 1 d . . . H34 H 0.2307 0.2619 -0.0112 0.071 Uiso 1 1 calc R . . C35 C 0.3921(7) 0.4530(4) 0.0398(6) 0.0545(16) Uani 1 1 d . . . C36 C 0.3435(9) 0.5198(4) -0.0194(6) 0.0643(18) Uani 1 1 d . . . H36 H 0.2559 0.5418 -0.0113 0.077 Uiso 1 1 calc R . . C37 C 0.4214(11) 0.5551(5) -0.0910(7) 0.077(2) Uani 1 1 d . . . H37 H 0.3863 0.6012 -0.1316 0.092 Uiso 1 1 calc R . . C38 C 0.5457(11) 0.5253(6) -0.1036(8) 0.084(3) Uani 1 1 d . . . H38 H 0.5973 0.5502 -0.1535 0.101 Uiso 1 1 calc R . . C39 C 0.5984(9) 0.4597(6) -0.0458(8) 0.083(3) Uani 1 1 d . . . H39 H 0.6867 0.4393 -0.0552 0.099 Uiso 1 1 calc R . . C40 C 0.5232(8) 0.4217(5) 0.0280(7) 0.074(2) Uani 1 1 d . . . H40 H 0.5602 0.3759 0.0689 0.089 Uiso 1 1 calc R . . B2 B -0.2892(9) 0.2297(5) 0.3680(7) 0.0604(19) 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 0.0594(10) 0.0512(8) 0.0368(7) -0.0016(7) 0.0077(7) -0.0012(8) P2 0.0466(8) 0.0523(8) 0.0351(7) 0.0035(6) 0.0106(6) 0.0013(7) C1 0.055(4) 0.057(4) 0.050(3) -0.003(3) 0.009(3) -0.010(3) C2 0.063(4) 0.052(4) 0.050(3) -0.005(3) 0.009(3) -0.005(3) C3 0.048(3) 0.054(3) 0.029(2) 0.006(2) 0.004(2) 0.002(3) C4 0.058(4) 0.053(3) 0.029(2) 0.004(2) 0.011(2) 0.003(3) C5 0.055(4) 0.052(3) 0.034(3) 0.008(2) 0.011(2) 0.004(3) C6 0.056(4) 0.056(4) 0.038(3) 0.005(3) 0.015(3) 0.008(3) C7 0.077(5) 0.059(4) 0.034(3) -0.008(3) 0.017(3) -0.001(3) C8 0.067(4) 0.061(4) 0.031(3) 0.001(3) 0.006(3) -0.004(3) C9 0.059(4) 0.071(4) 0.052(4) -0.008(3) 0.019(3) 0.007(3) C10 0.052(4) 0.085(5) 0.056(4) 0.009(3) 0.009(3) 0.020(4) C11 0.058(4) 0.067(4) 0.040(3) 0.018(3) 0.012(3) 0.015(3) C12 0.054(4) 0.055(3) 0.032(2) 0.006(2) 0.004(2) 0.004(3) C13 0.064(4) 0.046(3) 0.034(3) 0.004(2) 0.011(3) -0.004(3) C14 0.057(4) 0.049(3) 0.032(2) 0.000(2) 0.011(2) -0.007(3) C15 0.084(5) 0.049(4) 0.046(3) 0.004(3) 0.028(3) 0.000(3) C16 0.078(5) 0.048(4) 0.052(3) 0.010(3) 0.022(3) 0.024(3) C17 0.057(4) 0.053(3) 0.035(3) 0.002(2) 0.010(2) -0.003(3) C18 0.060(4) 0.057(4) 0.041(3) 0.003(3) 0.004(3) -0.003(3) C19 0.067(4) 0.066(4) 0.046(3) -0.001(3) 0.000(3) -0.017(3) C20 0.076(5) 0.072(4) 0.045(3) 0.000(3) 0.019(3) -0.010(4) C21 0.066(4) 0.054(4) 0.061(4) -0.004(3) 0.024(3) 0.002(3) C22 0.060(4) 0.049(3) 0.056(3) 0.000(3) 0.012(3) 0.004(3) C23 0.052(3) 0.054(3) 0.037(3) 0.003(2) 0.010(2) 0.000(3) C24 0.052(4) 0.081(5) 0.041(3) 0.006(3) 0.008(3) -0.004(3) C25 0.074(5) 0.073(5) 0.043(3) 0.010(3) -0.011(3) 0.008(4) C26 0.088(5) 0.079(5) 0.031(3) 0.009(3) 0.004(3) 0.010(4) C27 0.086(5) 0.064(4) 0.040(3) 0.009(3) 0.014(3) 0.003(4) C28 0.072(4) 0.056(4) 0.041(3) 0.006(3) 0.012(3) 0.000(3) C29 0.068(4) 0.053(3) 0.038(3) -0.007(2) 0.022(3) -0.006(3) C30 0.076(5) 0.063(4) 0.047(3) -0.003(3) 0.001(3) -0.006(4) C31 0.068(4) 0.095(6) 0.045(3) -0.002(4) 0.008(3) -0.007(4) C32 0.080(5) 0.086(5) 0.040(3) -0.025(3) 0.013(3) -0.017(4) C33 0.078(5) 0.072(5) 0.068(4) -0.026(4) 0.031(4) -0.019(4) C34 0.067(4) 0.067(4) 0.047(3) -0.012(3) 0.022(3) -0.014(3) C35 0.057(4) 0.065(4) 0.040(3) -0.012(3) 0.013(3) -0.014(3) C36 0.087(5) 0.059(4) 0.044(3) -0.009(3) 0.017(3) -0.014(4) C37 0.095(6) 0.089(5) 0.049(4) -0.012(4) 0.027(4) -0.033(5) C38 0.084(6) 0.118(7) 0.053(4) -0.007(5) 0.026(4) -0.041(6) C39 0.054(4) 0.130(8) 0.062(5) -0.030(5) 0.018(4) -0.020(5) C40 0.053(4) 0.107(6) 0.054(4) -0.029(4) 0.008(3) -0.012(4) B2 0.054(4) 0.072(5) 0.048(4) -0.008(4) 0.007(3) 0.005(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 C13 1.845(7) . ? P1 C29 1.843(6) . ? P1 C35 1.840(7) . ? P2 C4 1.790(6) . ? P2 C17 1.831(6) . ? P2 C23 1.844(6) . ? F1 B2 1.356(10) . ? F2 B2 1.396(10) . ? F3A B2 1.467(17) . ? F3B B2 1.350(14) . ? F4A B2 1.399(14) . ? F4B B2 1.274(17) . ? C1 C2 1.618(9) . ? C1 C14 1.521(9) . ? C2 C3 1.505(9) . ? C3 C4 1.423(8) . ? C3 C8 1.380(9) . ? C4 C5 1.407(9) . ? C5 C6 1.415(9) . ? C6 C7 1.387(9) . ? C6 C9 1.495(9) . ? C7 C8 1.385(10) . ? C9 C10 1.565(9) . ? C10 C11 1.534(10) . ? C11 C12 1.373(9) . ? C11 C16 1.387(10) . ? C12 C13 1.412(9) . ? C13 C14 1.413(8) . ? C14 C15 1.389(9) . ? C15 C16 1.403(10) . ? C17 C18 1.555(8) . ? C17 C22 1.553(9) . ? C18 C19 1.527(9) . ? C19 C20 1.507(11) . ? C20 C21 1.531(9) . ? C21 C22 1.516(9) . ? C23 C24 1.511(9) . ? C23 C28 1.542(9) . ? C24 C25 1.536(8) . ? C25 C26 1.512(11) . ? C26 C27 1.522(10) . ? C27 C28 1.534(8) . ? C29 C30 1.386(10) . ? C29 C34 1.376(9) . ? C30 C31 1.381(9) . ? C31 C32 1.350(10) . ? C32 C33 1.372(11) . ? C33 C34 1.399(9) . ? C35 C36 1.375(10) . ? C35 C40 1.408(10) . ? C36 C37 1.387(11) . ? C37 C38 1.343(13) . ? C38 C39 1.357(13) . ? C39 C40 1.410(12) . ? 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 C29 P1 C13 105.1(3) . . ? C35 P1 C13 103.0(3) . . ? C35 P1 C29 97.4(3) . . ? C4 P2 C17 114.2(3) . . ? C4 P2 C23 110.4(3) . . ? C17 P2 C23 109.8(3) . . ? C14 C1 C2 111.8(5) . . ? C3 C2 C1 112.6(5) . . ? C4 C3 C2 124.7(5) . . ? C8 C3 C2 118.1(6) . . ? C8 C3 C4 116.2(6) . . ? C3 C4 P2 121.1(5) . . ? C5 C4 P2 118.0(5) . . ? C5 C4 C3 120.5(5) . . ? C4 C5 C6 119.7(6) . . ? C5 C6 C9 121.2(6) . . ? C7 C6 C5 116.0(6) . . ? C7 C6 C9 121.7(6) . . ? C8 C7 C6 121.7(6) . . ? C3 C8 C7 121.4(6) . . ? C6 C9 C10 111.8(5) . . ? C11 C10 C9 113.8(5) . . ? C12 C11 C10 120.1(6) . . ? C12 C11 C16 118.6(6) . . ? C16 C11 C10 120.0(6) . . ? C11 C12 C13 122.1(6) . . ? C12 C13 P1 122.3(4) . . ? C12 C13 C14 117.8(6) . . ? C14 C13 P1 118.8(5) . . ? C13 C14 C1 121.7(5) . . ? C15 C14 C1 120.4(5) . . ? C15 C14 C13 116.6(6) . . ? C14 C15 C16 122.3(6) . . ? C11 C16 C15 118.4(6) . . ? C18 C17 P2 109.6(4) . . ? C22 C17 P2 107.8(4) . . ? C22 C17 C18 111.2(5) . . ? C19 C18 C17 111.7(5) . . ? C20 C19 C18 111.5(6) . . ? C19 C20 C21 110.4(6) . . ? C22 C21 C20 111.6(6) . . ? C21 C22 C17 111.1(5) . . ? C24 C23 P2 111.5(4) . . ? C24 C23 C28 110.9(5) . . ? C28 C23 P2 109.8(4) . . ? C23 C24 C25 110.9(6) . . ? C26 C25 C24 110.7(6) . . ? C25 C26 C27 110.1(6) . . ? C26 C27 C28 111.0(6) . . ? C27 C28 C23 109.4(6) . . ? C30 C29 P1 125.8(5) . . ? C34 C29 P1 116.8(5) . . ? C34 C29 C30 117.1(6) . . ? C31 C30 C29 120.9(7) . . ? C32 C31 C30 121.4(7) . . ? C31 C32 C33 119.6(6) . . ? C32 C33 C34 119.3(7) . . ? C29 C34 C33 121.7(7) . . ? C36 C35 P1 124.4(6) . . ? C36 C35 C40 118.9(7) . . ? C40 C35 P1 116.4(6) . . ? C35 C36 C37 120.5(8) . . ? C38 C37 C36 120.9(9) . . ? C37 C38 C39 120.5(8) . . ? C38 C39 C40 120.7(8) . . ? C35 C40 C39 118.4(8) . . ? F1 B2 F2 110.6(6) . . ? F1 B2 F3A 89.4(8) . . ? F1 B2 F4A 99.7(8) . . ? F2 B2 F3A 99.4(9) . . ? F2 B2 F4A 105.9(8) . . ? F3B B2 F1 118.6(9) . . ? F3B B2 F2 109.5(8) . . ? F3B B2 F3A 39.6(7) . . ? F3B B2 F4A 111.5(9) . . ? F4A B2 F3A 147.9(10) . . ? F4B B2 F1 123.9(10) . . ? F4B B2 F2 119.1(9) . . ? F4B B2 F3A 105.8(11) . . ? F4B B2 F3B 67.4(10) . . ? F4B B2 F4A 44.2(8) . . ?