# 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_email dstephan@chem.utoronto.ca _publ_contact_author_name 'Douglas W. Stephan' loop_ _publ_author_name 'Chunfang Jiang' 'Douglas W. Stephan' data_cj025_0m _database_code_depnum_ccdc_archive 'CCDC 873942' #TrackingRef 'combined-CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H28 B F15 N P' _chemical_formula_weight 945.49 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1234(5) _cell_length_b 11.7781(6) _cell_length_c 17.6664(9) _cell_angle_alpha 82.839(2) _cell_angle_beta 83.646(2) _cell_angle_gamma 83.741(2) _cell_volume 2067.47(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9502 _exptl_absorpt_correction_T_max 0.9502 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32322 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7265 _reflns_number_gt 5733 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+1.2999P] 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 7265 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3933(2) 0.92331(18) 0.16162(12) 0.0277(5) Uani 1 1 d . . . C2 C 0.5129(2) 0.8986(2) 0.11677(13) 0.0374(5) Uani 1 1 d . . . H2A H 0.5930 0.9168 0.1310 0.045 Uiso 1 1 calc R . . C3 C 0.5111(3) 0.8469(2) 0.05123(15) 0.0479(7) Uani 1 1 d . . . H3 H 0.5905 0.8298 0.0212 0.057 Uiso 1 1 calc R . . C4 C 0.3925(3) 0.8203(3) 0.03008(15) 0.0532(7) Uani 1 1 d . . . H4 H 0.3921 0.7858 -0.0144 0.064 Uiso 1 1 calc R . . C5 C 0.2742(3) 0.8444(2) 0.07422(15) 0.0504(7) Uani 1 1 d . . . H5 H 0.1947 0.8253 0.0597 0.061 Uiso 1 1 calc R . . C6 C 0.2735(2) 0.8968(2) 0.13983(13) 0.0355(5) Uani 1 1 d . . . H6 H 0.1935 0.9143 0.1693 0.043 Uiso 1 1 calc R . . C7 C 0.5035(2) 0.91993(18) 0.30977(12) 0.0255(4) Uiso 1 1 d . . . C8 C 0.5252(2) 0.9726(2) 0.37339(13) 0.0341(5) Uani 1 1 d . . . H8 H 0.4876 1.0471 0.3790 0.041 Uiso 1 1 calc R . . C9 C 0.6024(2) 0.9142(2) 0.42759(13) 0.0376(6) Uani 1 1 d . . . H9 H 0.6182 0.9497 0.4694 0.045 Uiso 1 1 calc R . . C10 C 0.6567(2) 0.8027(2) 0.42032(13) 0.0357(5) Uani 1 1 d . . . H10 H 0.7077 0.7631 0.4576 0.043 Uiso 1 1 calc R . . C11 C 0.6352(2) 0.7502(2) 0.35775(14) 0.0353(5) Uani 1 1 d . . . H11 H 0.6717 0.6752 0.3530 0.042 Uiso 1 1 calc R . . C12 C 0.5595(2) 0.80874(18) 0.30201(13) 0.0295(5) Uani 1 1 d . . . H12 H 0.5462 0.7736 0.2595 0.035 Uiso 1 1 calc R . . C13 C 0.16969(19) 0.94184(18) 0.33509(12) 0.0257(5) Uani 1 1 d . . . C14 C 0.1962(2) 0.82462(19) 0.33156(13) 0.0299(5) Uani 1 1 d . . . H14 H 0.2659 0.7967 0.2979 0.036 Uiso 1 1 calc R . . C15 C 0.1186(2) 0.7492(2) 0.37829(13) 0.0342(5) Uani 1 1 d . . . H15 H 0.1368 0.6705 0.3761 0.041 Uiso 1 1 calc R . . C16 C 0.0147(2) 0.7895(2) 0.42800(13) 0.0370(6) Uani 1 1 d . . . H16 H -0.0373 0.7384 0.4591 0.044 Uiso 1 1 calc R . . C17 C -0.0117(2) 0.9061(2) 0.43133(13) 0.0388(6) Uani 1 1 d . . . H17 H -0.0821 0.9336 0.4647 0.047 Uiso 1 1 calc R . . C18 C 0.0657(2) 0.9830(2) 0.38538(13) 0.0322(5) Uani 1 1 d . . . H18 H 0.0479 1.0616 0.3883 0.039 Uiso 1 1 calc R . . C19 C 0.4476(2) 1.13664(18) 0.20946(12) 0.0258(5) Uani 1 1 d . . . C20 C 0.3647(2) 1.2099(2) 0.16307(13) 0.0343(5) Uani 1 1 d . . . H20 H 0.2853 1.1861 0.1517 0.041 Uiso 1 1 calc R . . C21 C 0.4002(2) 1.3176(2) 0.13397(13) 0.0374(5) Uani 1 1 d . . . H21 H 0.3441 1.3669 0.1036 0.045 Uiso 1 1 calc R . . C22 C 0.5190(2) 1.3522(2) 0.15001(14) 0.0368(5) Uani 1 1 d . . . H22 H 0.5426 1.4251 0.1305 0.044 Uiso 1 1 calc R . . C23 C 0.6028(2) 1.2795(2) 0.19470(15) 0.0410(6) Uani 1 1 d . . . H23 H 0.6834 1.3030 0.2046 0.049 Uiso 1 1 calc R . . C24 C 0.5676(2) 1.17125(19) 0.22500(13) 0.0328(5) Uani 1 1 d . . . H24 H 0.6238 1.1223 0.2555 0.039 Uiso 1 1 calc R . . N1 N 0.24507(18) 1.02246(17) 0.28676(11) 0.0286(4) Uani 1 1 d . . . P1 P 0.39581(5) 0.99761(5) 0.24369(3) 0.02434(14) Uani 1 1 d . . . H2 H 0.219(2) 1.086(2) 0.2873(13) 0.026(7) Uiso 1 1 d . . . C25 C 0.9033(2) 0.35288(18) 0.35322(12) 0.0275(5) Uani 1 1 d . . . C26 C 0.8168(2) 0.26874(18) 0.37662(13) 0.0290(5) Uani 1 1 d . . . C27 C 0.7235(2) 0.2699(2) 0.43965(14) 0.0345(5) Uani 1 1 d . . . C28 C 0.7093(2) 0.3611(2) 0.48215(13) 0.0369(6) Uani 1 1 d . . . C29 C 0.7917(2) 0.4472(2) 0.46176(13) 0.0362(5) Uani 1 1 d . . . C30 C 0.8857(2) 0.44094(19) 0.39943(13) 0.0324(5) Uani 1 1 d . . . C31 C 0.9422(2) 0.39837(18) 0.19895(12) 0.0282(5) Uani 1 1 d . . . C32 C 0.8461(2) 0.49119(19) 0.19369(13) 0.0334(5) Uani 1 1 d . . . C33 C 0.7832(2) 0.5311(2) 0.12895(16) 0.0429(6) Uani 1 1 d . . . C34 C 0.8171(3) 0.4782(3) 0.06425(15) 0.0494(7) Uani 1 1 d . . . C35 C 0.9127(3) 0.3872(2) 0.06467(14) 0.0456(6) Uani 1 1 d . . . C36 C 0.9728(2) 0.3500(2) 0.13111(13) 0.0348(5) Uani 1 1 d . . . C37 C 1.1493(2) 0.40148(18) 0.28681(12) 0.0272(5) Uani 1 1 d . . . C38 C 1.1952(2) 0.50081(19) 0.24734(13) 0.0310(5) Uani 1 1 d . . . C39 C 1.3175(2) 0.53797(19) 0.25531(14) 0.0351(5) Uani 1 1 d . . . C40 C 1.3996(2) 0.4762(2) 0.30510(14) 0.0379(6) Uani 1 1 d . . . C41 C 1.3585(2) 0.3775(2) 0.34670(13) 0.0369(6) Uani 1 1 d . . . C42 C 1.2363(2) 0.34375(19) 0.33657(12) 0.0315(5) Uani 1 1 d . . . B1 B 1.0113(2) 0.3449(2) 0.27735(14) 0.0280(5) Uani 1 1 d . . . F1 F 0.82049(13) 0.17774(11) 0.33598(8) 0.0410(3) Uani 1 1 d . . . F2 F 0.64697(14) 0.18236(12) 0.46022(9) 0.0517(4) Uani 1 1 d . . . F3 F 0.61799(14) 0.36604(14) 0.54317(8) 0.0547(4) Uani 1 1 d . . . F4 F 0.78108(15) 0.53723(13) 0.50326(8) 0.0525(4) Uani 1 1 d . . . F5 F 0.96173(14) 0.53041(11) 0.38312(8) 0.0455(4) Uani 1 1 d . . . F6 F 0.80881(14) 0.54974(12) 0.25477(8) 0.0478(4) Uani 1 1 d . . . F7 F 0.68783(16) 0.62029(13) 0.12922(11) 0.0656(5) Uani 1 1 d . . . F8 F 0.75612(19) 0.51488(18) 0.00011(10) 0.0814(6) Uani 1 1 d . . . F9 F 0.94746(19) 0.33411(18) 0.00097(9) 0.0730(5) Uani 1 1 d . . . F10 F 1.06697(14) 0.25946(13) 0.12619(8) 0.0500(4) Uani 1 1 d . . . F11 F 1.12097(14) 0.56733(12) 0.19668(9) 0.0488(4) Uani 1 1 d . . . F12 F 1.35822(14) 0.63329(12) 0.21295(9) 0.0530(4) Uani 1 1 d . . . F13 F 1.51998(13) 0.50949(14) 0.31226(10) 0.0574(4) Uani 1 1 d . . . F14 F 1.43778(14) 0.31438(15) 0.39561(9) 0.0602(4) Uani 1 1 d . . . F15 F 1.20325(14) 0.24458(12) 0.37941(8) 0.0453(4) Uani 1 1 d . . . H1 H 1.0538 0.2342 0.2700 0.060 Uiso 1 1 d . . . C43 C 0.8916(3) 0.9250(3) 0.23002(17) 0.0588(8) Uani 1 1 d . . . H43 H 0.8920 0.9227 0.2828 0.071 Uiso 1 1 calc R . . C44 C 0.8909(3) 1.0265(3) 0.18557(16) 0.0520(7) Uani 1 1 d . . . H44 H 0.8933 1.0937 0.2078 0.062 Uiso 1 1 calc R . . C45 C 0.8868(3) 1.0319(3) 0.10831(17) 0.0614(8) Uani 1 1 d . . . H45 H 0.8850 1.1026 0.0782 0.074 Uiso 1 1 calc R . . C46 C 0.8853(3) 0.9338(4) 0.07541(18) 0.0741(10) Uani 1 1 d . . . H46 H 0.8809 0.9371 0.0229 0.089 Uiso 1 1 calc R . . C47 C 0.8902(3) 0.8292(3) 0.1206(3) 0.0815(13) Uani 1 1 d . . . H47 H 0.8923 0.7612 0.0985 0.098 Uiso 1 1 calc R . . C48 C 0.8919(3) 0.8266(3) 0.1983(2) 0.0708(10) Uani 1 1 d . . . H48 H 0.8931 0.7567 0.2293 0.085 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 C1 0.0292(11) 0.0246(11) 0.0286(11) -0.0026(9) -0.0022(9) -0.0007(9) C2 0.0318(12) 0.0433(14) 0.0361(13) -0.0079(11) 0.0009(10) 0.0008(10) C3 0.0468(15) 0.0579(17) 0.0366(14) -0.0142(12) 0.0032(12) 0.0082(13) C4 0.0646(18) 0.0607(18) 0.0377(15) -0.0219(13) -0.0116(13) 0.0040(15) C5 0.0474(15) 0.0640(19) 0.0453(15) -0.0179(14) -0.0164(13) -0.0042(13) C6 0.0293(12) 0.0443(14) 0.0337(13) -0.0073(10) -0.0052(10) -0.0013(10) C8 0.0385(13) 0.0286(12) 0.0344(13) -0.0044(10) -0.0019(10) -0.0002(10) C9 0.0428(14) 0.0404(14) 0.0302(12) -0.0058(10) -0.0054(10) -0.0033(11) C10 0.0289(12) 0.0405(14) 0.0355(13) 0.0054(10) -0.0043(10) -0.0032(10) C11 0.0301(12) 0.0288(12) 0.0449(14) -0.0004(10) -0.0021(10) 0.0006(10) C12 0.0264(11) 0.0281(12) 0.0344(12) -0.0055(9) -0.0018(9) -0.0028(9) C13 0.0217(10) 0.0291(12) 0.0270(11) -0.0033(9) -0.0029(9) -0.0047(9) C14 0.0252(11) 0.0307(12) 0.0337(12) -0.0052(10) -0.0002(9) -0.0039(9) C15 0.0336(12) 0.0312(13) 0.0390(13) -0.0017(10) -0.0070(10) -0.0077(10) C16 0.0327(12) 0.0427(15) 0.0352(13) 0.0037(11) -0.0007(10) -0.0138(11) C17 0.0312(12) 0.0500(16) 0.0340(13) -0.0085(11) 0.0081(10) -0.0061(11) C18 0.0291(11) 0.0327(13) 0.0350(13) -0.0082(10) 0.0003(10) -0.0024(10) C19 0.0253(11) 0.0241(11) 0.0266(11) -0.0041(9) 0.0025(9) -0.0003(9) C20 0.0292(12) 0.0345(13) 0.0386(13) 0.0002(10) -0.0062(10) -0.0018(10) C21 0.0387(13) 0.0322(13) 0.0366(13) 0.0039(10) -0.0019(11) 0.0063(10) C22 0.0399(13) 0.0245(12) 0.0423(14) 0.0014(10) 0.0073(11) -0.0031(10) C23 0.0327(13) 0.0364(14) 0.0537(16) 0.0006(12) -0.0030(11) -0.0107(11) C24 0.0263(11) 0.0303(12) 0.0405(13) 0.0030(10) -0.0045(10) -0.0037(9) N1 0.0260(10) 0.0201(10) 0.0374(11) -0.0034(8) 0.0046(8) 0.0004(8) P1 0.0210(3) 0.0236(3) 0.0280(3) -0.0035(2) 0.0004(2) -0.0021(2) C25 0.0264(11) 0.0274(12) 0.0295(11) -0.0026(9) -0.0058(9) -0.0038(9) C26 0.0277(11) 0.0230(11) 0.0379(13) -0.0041(9) -0.0108(10) -0.0010(9) C27 0.0250(11) 0.0322(13) 0.0442(14) 0.0121(10) -0.0073(10) -0.0084(10) C28 0.0281(12) 0.0490(15) 0.0295(12) 0.0033(11) 0.0034(10) -0.0006(11) C29 0.0396(13) 0.0363(13) 0.0331(13) -0.0110(10) -0.0014(11) 0.0002(11) C30 0.0343(12) 0.0283(12) 0.0353(13) -0.0021(10) -0.0008(10) -0.0104(10) C31 0.0227(10) 0.0294(12) 0.0332(12) -0.0023(9) -0.0020(9) -0.0076(9) C32 0.0321(12) 0.0275(12) 0.0405(13) -0.0011(10) -0.0015(10) -0.0073(10) C33 0.0338(13) 0.0313(14) 0.0615(18) 0.0103(12) -0.0117(12) -0.0042(11) C34 0.0457(15) 0.0582(18) 0.0436(16) 0.0167(13) -0.0192(13) -0.0134(14) C35 0.0465(15) 0.0629(18) 0.0299(13) -0.0070(12) -0.0035(11) -0.0141(14) C36 0.0244(11) 0.0398(14) 0.0399(13) -0.0035(11) -0.0032(10) -0.0027(10) C37 0.0251(11) 0.0275(12) 0.0293(11) -0.0087(9) 0.0015(9) -0.0011(9) C38 0.0282(11) 0.0275(12) 0.0375(13) -0.0071(10) -0.0042(10) 0.0018(9) C39 0.0341(12) 0.0262(12) 0.0457(14) -0.0117(10) 0.0052(11) -0.0068(10) C40 0.0228(11) 0.0473(15) 0.0475(14) -0.0205(12) -0.0004(10) -0.0074(10) C41 0.0279(12) 0.0484(15) 0.0351(13) -0.0098(11) -0.0075(10) 0.0036(11) C42 0.0333(12) 0.0312(12) 0.0304(12) -0.0051(10) -0.0016(10) -0.0038(10) B1 0.0291(13) 0.0231(13) 0.0323(13) -0.0049(10) -0.0039(10) -0.0026(10) F1 0.0390(7) 0.0297(7) 0.0577(9) -0.0097(6) -0.0087(6) -0.0096(6) F2 0.0381(8) 0.0444(9) 0.0702(10) 0.0119(7) -0.0004(7) -0.0191(7) F3 0.0424(8) 0.0724(11) 0.0428(9) 0.0020(8) 0.0144(7) -0.0054(8) F4 0.0602(9) 0.0527(9) 0.0456(9) -0.0217(7) 0.0093(7) -0.0053(7) F5 0.0499(8) 0.0356(8) 0.0538(9) -0.0182(7) 0.0127(7) -0.0200(6) F6 0.0536(9) 0.0322(8) 0.0553(9) -0.0091(7) -0.0019(7) 0.0078(6) F7 0.0546(10) 0.0420(9) 0.0956(13) 0.0139(9) -0.0251(9) 0.0084(8) F8 0.0870(13) 0.0984(15) 0.0585(11) 0.0223(10) -0.0412(10) -0.0093(11) F9 0.0815(12) 0.1049(15) 0.0360(9) -0.0213(9) -0.0088(8) -0.0062(11) F10 0.0394(8) 0.0631(10) 0.0483(9) -0.0228(7) -0.0042(7) 0.0102(7) F11 0.0414(8) 0.0356(8) 0.0674(10) 0.0136(7) -0.0150(7) -0.0075(6) F12 0.0468(8) 0.0366(8) 0.0755(11) -0.0024(7) 0.0034(8) -0.0181(7) F13 0.0294(7) 0.0735(11) 0.0761(11) -0.0218(9) -0.0069(7) -0.0176(7) F14 0.0404(8) 0.0816(12) 0.0588(10) 0.0047(9) -0.0236(8) -0.0016(8) F15 0.0442(8) 0.0450(9) 0.0454(8) 0.0096(7) -0.0121(7) -0.0076(7) C43 0.0420(16) 0.085(2) 0.0485(17) 0.0087(16) -0.0066(13) -0.0196(15) C44 0.0478(16) 0.0549(18) 0.0541(18) -0.0176(14) 0.0029(13) -0.0030(13) C45 0.075(2) 0.0518(18) 0.0541(19) 0.0065(14) -0.0087(16) -0.0042(15) C46 0.071(2) 0.114(3) 0.0435(17) -0.0255(19) 0.0170(15) -0.044(2) C47 0.0554(19) 0.067(2) 0.126(3) -0.056(2) 0.047(2) -0.0314(17) C48 0.0472(18) 0.051(2) 0.104(3) 0.017(2) 0.0078(18) -0.0035(15) _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 C6 1.390(3) . ? C1 C2 1.395(3) . ? C1 P1 1.788(2) . ? C2 C3 1.376(3) . ? C3 C4 1.375(4) . ? C4 C5 1.377(4) . ? C5 C6 1.378(3) . ? C7 C12 1.386(3) . ? C7 C8 1.398(3) . ? C7 P1 1.785(2) . ? C8 C9 1.373(3) . ? C9 C10 1.383(3) . ? C10 C11 1.380(3) . ? C11 C12 1.384(3) . ? C13 C14 1.385(3) . ? C13 C18 1.386(3) . ? C13 N1 1.423(3) . ? C14 C15 1.383(3) . ? C15 C16 1.376(3) . ? C16 C17 1.378(3) . ? C17 C18 1.386(3) . ? C19 C24 1.387(3) . ? C19 C20 1.393(3) . ? C19 P1 1.787(2) . ? C20 C21 1.378(3) . ? C21 C22 1.380(3) . ? C22 C23 1.378(3) . ? C23 C24 1.387(3) . ? N1 P1 1.6414(18) . ? C25 C30 1.383(3) . ? C25 C26 1.388(3) . ? C25 B1 1.639(3) . ? C26 F1 1.358(2) . ? C26 C27 1.379(3) . ? C27 F2 1.346(2) . ? C27 C28 1.372(3) . ? C28 F3 1.343(3) . ? C28 C29 1.371(3) . ? C29 F4 1.351(3) . ? C29 C30 1.377(3) . ? C30 F5 1.356(2) . ? C31 C36 1.381(3) . ? C31 C32 1.383(3) . ? C31 B1 1.645(3) . ? C32 F6 1.349(3) . ? C32 C33 1.377(3) . ? C33 F7 1.347(3) . ? C33 C34 1.363(4) . ? C34 F8 1.352(3) . ? C34 C35 1.363(4) . ? C35 F9 1.350(3) . ? C35 C36 1.382(3) . ? C36 F10 1.355(3) . ? C37 C42 1.379(3) . ? C37 C38 1.383(3) . ? C37 B1 1.645(3) . ? C38 F11 1.351(3) . ? C38 C39 1.385(3) . ? C39 F12 1.347(3) . ? C39 C40 1.365(3) . ? C40 F13 1.344(3) . ? C40 C41 1.374(3) . ? C41 F14 1.344(3) . ? C41 C42 1.376(3) . ? C42 F15 1.363(3) . ? C43 C44 1.346(4) . ? C43 C48 1.349(5) . ? C44 C45 1.364(4) . ? C45 C46 1.359(5) . ? C46 C47 1.381(5) . ? C47 C48 1.372(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 120.2(2) . . ? C6 C1 P1 120.79(17) . . ? C2 C1 P1 118.89(16) . . ? C3 C2 C1 119.4(2) . . ? C4 C3 C2 120.2(2) . . ? C3 C4 C5 120.6(2) . . ? C4 C5 C6 120.2(2) . . ? C5 C6 C1 119.4(2) . . ? C12 C7 C8 119.77(19) . . ? C12 C7 P1 122.40(16) . . ? C8 C7 P1 117.75(16) . . ? C9 C8 C7 119.8(2) . . ? C8 C9 C10 120.3(2) . . ? C11 C10 C9 120.0(2) . . ? C10 C11 C12 120.3(2) . . ? C11 C12 C7 119.7(2) . . ? C14 C13 C18 119.9(2) . . ? C14 C13 N1 121.55(19) . . ? C18 C13 N1 118.53(19) . . ? C15 C14 C13 119.8(2) . . ? C16 C15 C14 120.6(2) . . ? C15 C16 C17 119.6(2) . . ? C16 C17 C18 120.6(2) . . ? C13 C18 C17 119.5(2) . . ? C24 C19 C20 119.9(2) . . ? C24 C19 P1 122.68(17) . . ? C20 C19 P1 117.40(16) . . ? C21 C20 C19 120.2(2) . . ? C20 C21 C22 119.9(2) . . ? C23 C22 C21 120.4(2) . . ? C22 C23 C24 120.3(2) . . ? C23 C24 C19 119.4(2) . . ? C13 N1 P1 126.90(16) . . ? N1 P1 C7 110.07(10) . . ? N1 P1 C19 104.97(10) . . ? C7 P1 C19 111.87(10) . . ? N1 P1 C1 111.36(10) . . ? C7 P1 C1 111.33(10) . . ? C19 P1 C1 107.04(10) . . ? C30 C25 C26 112.99(19) . . ? C30 C25 B1 125.54(19) . . ? C26 C25 B1 121.46(19) . . ? F1 C26 C27 115.59(19) . . ? F1 C26 C25 119.79(19) . . ? C27 C26 C25 124.6(2) . . ? F2 C27 C28 119.7(2) . . ? F2 C27 C26 120.9(2) . . ? C28 C27 C26 119.4(2) . . ? F3 C28 C29 120.3(2) . . ? F3 C28 C27 121.1(2) . . ? C29 C28 C27 118.7(2) . . ? F4 C29 C28 119.9(2) . . ? F4 C29 C30 120.3(2) . . ? C28 C29 C30 119.8(2) . . ? F5 C30 C29 115.69(19) . . ? F5 C30 C25 119.85(19) . . ? C29 C30 C25 124.4(2) . . ? C36 C31 C32 113.0(2) . . ? C36 C31 B1 121.87(19) . . ? C32 C31 B1 125.1(2) . . ? F6 C32 C33 115.5(2) . . ? F6 C32 C31 119.9(2) . . ? C33 C32 C31 124.6(2) . . ? F7 C33 C34 119.9(2) . . ? F7 C33 C32 120.9(2) . . ? C34 C33 C32 119.2(2) . . ? F8 C34 C33 120.4(3) . . ? F8 C34 C35 120.0(3) . . ? C33 C34 C35 119.6(2) . . ? F9 C35 C34 120.2(2) . . ? F9 C35 C36 120.6(2) . . ? C34 C35 C36 119.2(2) . . ? F10 C36 C31 120.4(2) . . ? F10 C36 C35 115.1(2) . . ? C31 C36 C35 124.4(2) . . ? C42 C37 C38 113.36(19) . . ? C42 C37 B1 118.88(19) . . ? C38 C37 B1 127.68(19) . . ? F11 C38 C37 120.51(19) . . ? F11 C38 C39 115.8(2) . . ? C37 C38 C39 123.7(2) . . ? F12 C39 C40 119.4(2) . . ? F12 C39 C38 120.6(2) . . ? C40 C39 C38 120.0(2) . . ? F13 C40 C39 120.8(2) . . ? F13 C40 C41 120.3(2) . . ? C39 C40 C41 118.9(2) . . ? F14 C41 C40 120.2(2) . . ? F14 C41 C42 120.8(2) . . ? C40 C41 C42 119.0(2) . . ? F15 C42 C41 115.5(2) . . ? F15 C42 C37 119.52(19) . . ? C41 C42 C37 125.0(2) . . ? C25 B1 C37 111.93(17) . . ? C25 B1 C31 110.89(17) . . ? C37 B1 C31 113.37(18) . . ? C44 C43 C48 120.2(3) . . ? C43 C44 C45 120.7(3) . . ? C46 C45 C44 119.9(3) . . ? C45 C46 C47 119.5(3) . . ? C48 C47 C46 119.3(3) . . ? C43 C48 C47 120.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.226 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.044 #===end data_cj015_0m _database_code_depnum_ccdc_archive 'CCDC 873943' #TrackingRef 'combined-CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H17 B F20 N P' _chemical_formula_weight 957.35 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7826(7) _cell_length_b 16.5070(10) _cell_length_c 19.9076(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.530(2) _cell_angle_gamma 90.00 _cell_volume 3859.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8220 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.72 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9491 _exptl_absorpt_correction_T_max 0.9567 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34172 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.57 _reflns_number_total 8872 _reflns_number_gt 5638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0476P)^2^+2.7606P] 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 8872 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 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 C1 C 0.73604(19) 0.48005(14) -0.33731(12) 0.0398(5) Uani 1 1 d . . . C2 C 0.6450(2) 0.43257(16) -0.32359(13) 0.0500(6) Uani 1 1 d . . . C3 C 0.6197(3) 0.35875(17) -0.35410(15) 0.0599(8) Uani 1 1 d . . . C4 C 0.6869(3) 0.32948(16) -0.40073(17) 0.0645(9) Uani 1 1 d . . . C5 C 0.7763(3) 0.3748(2) -0.41799(19) 0.0750(10) Uani 1 1 d . . . C6 C 0.7983(2) 0.44805(17) -0.38690(16) 0.0584(7) Uani 1 1 d . . . C7 C 0.72272(19) 0.64589(14) -0.34439(12) 0.0387(5) Uani 1 1 d . . . C8 C 0.6486(2) 0.64700(15) -0.40171(12) 0.0451(6) Uani 1 1 d . . . C9 C 0.6141(2) 0.71698(19) -0.43565(13) 0.0568(7) Uani 1 1 d . . . C10 C 0.6521(3) 0.79027(17) -0.41150(15) 0.0589(8) Uani 1 1 d . . . C11 C 0.7235(2) 0.79349(15) -0.35441(15) 0.0527(7) Uani 1 1 d . . . C12 C 0.7575(2) 0.72260(15) -0.32318(13) 0.0441(6) Uani 1 1 d . . . C13 C 0.7390(2) 0.57403(13) -0.22408(12) 0.0389(5) Uani 1 1 d . . . C14 C 0.8144(2) 0.55082(15) -0.17112(13) 0.0482(6) Uani 1 1 d . . . C15 C 0.7958(3) 0.56277(17) -0.10396(14) 0.0615(8) Uani 1 1 d . . . C16 C 0.6970(3) 0.59772(19) -0.08808(14) 0.0651(8) Uani 1 1 d . . . C17 C 0.6185(3) 0.62024(18) -0.13758(15) 0.0612(8) Uani 1 1 d . . . C18 C 0.6407(2) 0.60762(16) -0.20362(13) 0.0497(6) Uani 1 1 d . . . C19 C 0.52288(19) 0.76039(14) 0.12732(12) 0.0400(5) Uani 1 1 d . . . C20 C 0.4679(2) 0.77529(15) 0.06476(13) 0.0438(6) Uani 1 1 d . . . C21 C 0.4268(2) 0.71318(18) 0.02383(13) 0.0526(7) Uani 1 1 d . . . C22 C 0.4418(2) 0.63454(17) 0.04477(15) 0.0559(7) Uani 1 1 d . . . C23 C 0.4963(2) 0.61854(16) 0.10661(15) 0.0515(7) Uani 1 1 d . . . C24 C 0.5354(2) 0.68076(16) 0.14741(13) 0.0450(6) Uani 1 1 d . . . C25 C 0.7830(2) 0.77570(15) 0.18242(14) 0.0453(6) Uani 1 1 d . . . C26 C 0.7962(2) 0.74720(17) 0.11738(15) 0.0553(7) Uani 1 1 d . . . H26 H 0.7572 0.7717 0.0803 0.066 Uiso 1 1 calc R . . C27 C 0.8671(3) 0.68265(19) 0.1086(2) 0.0709(9) Uani 1 1 d . . . H27 H 0.8759 0.6630 0.0656 0.085 Uiso 1 1 calc R . . C28 C 0.9247(3) 0.6474(2) 0.1632(2) 0.0807(11) Uani 1 1 d . . . H28 H 0.9718 0.6033 0.1569 0.097 Uiso 1 1 calc R . . C29 C 0.9145(3) 0.6759(2) 0.2270(2) 0.0801(10) Uani 1 1 d . . . H29 H 0.9560 0.6521 0.2635 0.096 Uiso 1 1 calc R . . C30 C 0.8422(2) 0.74031(18) 0.23742(17) 0.0610(8) Uani 1 1 d . . . H30 H 0.8337 0.7593 0.2807 0.073 Uiso 1 1 calc R . . C31 C 0.6829(2) 0.88590(14) 0.27909(12) 0.0398(5) Uani 1 1 d . . . C32 C 0.6168(3) 0.84129(16) 0.32039(13) 0.0564(7) Uani 1 1 d . . . H32 H 0.5764 0.7964 0.3033 0.068 Uiso 1 1 calc R . . C33 C 0.6113(3) 0.86353(19) 0.38651(14) 0.0634(8) Uani 1 1 d . . . H33 H 0.5672 0.8337 0.4143 0.076 Uiso 1 1 calc R . . C34 C 0.6704(3) 0.92932(19) 0.41155(14) 0.0606(7) Uani 1 1 d . . . H34 H 0.6659 0.9445 0.4563 0.073 Uiso 1 1 calc R . . C35 C 0.7362(3) 0.97297(19) 0.37129(14) 0.0622(8) Uani 1 1 d . . . H35 H 0.7765 1.0175 0.3890 0.075 Uiso 1 1 calc R . . C36 C 0.7437(2) 0.95209(16) 0.30489(13) 0.0510(6) Uani 1 1 d . . . H36 H 0.7890 0.9820 0.2778 0.061 Uiso 1 1 calc R . . C37 C 0.7246(2) 0.94140(15) 0.14555(12) 0.0428(6) Uani 1 1 d . . . C38 C 0.8320(2) 0.95198(18) 0.12406(16) 0.0631(8) Uani 1 1 d . . . H38 H 0.8875 0.9124 0.1326 0.076 Uiso 1 1 calc R . . C39 C 0.8568(3) 1.0218(2) 0.08981(19) 0.0819(11) Uani 1 1 d . . . H39 H 0.9292 1.0294 0.0752 0.098 Uiso 1 1 calc R . . C40 C 0.7756(3) 1.0795(2) 0.07745(18) 0.0857(11) Uani 1 1 d . . . H40 H 0.7928 1.1263 0.0543 0.103 Uiso 1 1 calc R . . C41 C 0.6694(3) 1.0699(2) 0.0984(2) 0.0919(12) Uani 1 1 d . . . H41 H 0.6147 1.1099 0.0897 0.110 Uiso 1 1 calc R . . C42 C 0.6430(3) 1.0007(2) 0.13268(17) 0.0724(9) Uani 1 1 d . . . H42 H 0.5704 0.9940 0.1471 0.087 Uiso 1 1 calc R . . N1 N 0.55690(19) 0.82438(14) 0.17172(12) 0.0474(5) Uani 1 1 d . . . B1 B 0.7715(2) 0.56684(16) -0.30211(13) 0.0376(6) Uani 1 1 d . . . F1 F 0.57401(16) 0.45767(13) -0.27878(10) 0.0900(7) Uani 1 1 d . . . F2 F 0.52792(19) 0.31674(13) -0.33866(10) 0.0986(7) Uani 1 1 d . . . F3 F 0.66339(18) 0.25750(10) -0.43045(12) 0.0987(7) Uani 1 1 d . . . F4 F 0.84187(19) 0.34826(16) -0.46680(15) 0.1309(11) Uani 1 1 d . . . F5 F 0.88566(16) 0.49121(13) -0.40916(11) 0.0965(7) Uani 1 1 d . . . F6 F 0.60466(13) 0.57748(10) -0.42795(8) 0.0613(4) Uani 1 1 d . . . F7 F 0.54238(17) 0.71239(13) -0.49151(9) 0.0850(6) Uani 1 1 d . . . F8 F 0.61769(18) 0.85863(11) -0.44395(10) 0.0875(6) Uani 1 1 d . . . F9 F 0.75996(16) 0.86569(9) -0.32994(10) 0.0759(5) Uani 1 1 d . . . F10 F 0.83014(13) 0.73005(9) -0.26750(8) 0.0584(4) Uani 1 1 d . . . F11 F 0.91380(14) 0.51546(10) -0.18407(9) 0.0692(5) Uani 1 1 d . . . F12 F 0.87597(19) 0.54066(13) -0.05513(9) 0.0965(7) Uani 1 1 d . . . F13 F 0.6789(2) 0.60950(14) -0.02259(9) 0.1007(7) Uani 1 1 d . . . F14 F 0.52048(19) 0.65414(14) -0.12191(11) 0.0988(7) Uani 1 1 d . . . F15 F 0.55691(13) 0.63115(12) -0.25031(9) 0.0716(5) Uani 1 1 d . . . F16 F 0.45147(14) 0.85129(9) 0.04425(8) 0.0626(4) Uani 1 1 d . . . F17 F 0.37063(16) 0.72979(12) -0.03557(9) 0.0794(5) Uani 1 1 d . . . F18 F 0.40239(16) 0.57367(11) 0.00559(10) 0.0859(6) Uani 1 1 d . . . F19 F 0.50810(16) 0.54180(10) 0.12760(10) 0.0785(5) Uani 1 1 d . . . F20 F 0.58548(14) 0.66295(10) 0.20827(8) 0.0645(4) Uani 1 1 d . . . P1 P 0.68681(5) 0.85638(4) 0.19367(3) 0.03777(15) Uani 1 1 d . . . H1 H 0.507(3) 0.8525(18) 0.1797(15) 0.060(9) Uiso 1 1 d . . . H2 H 0.8807(14) 0.5713(10) -0.3002(8) 0.006(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0376(13) 0.0364(12) 0.0449(13) 0.0010(10) 0.0008(10) -0.0013(10) C2 0.0564(16) 0.0502(15) 0.0437(14) 0.0006(12) 0.0064(12) -0.0121(13) C3 0.0683(19) 0.0484(16) 0.0604(18) 0.0136(14) -0.0111(15) -0.0265(15) C4 0.071(2) 0.0342(14) 0.084(2) -0.0122(14) -0.0198(18) 0.0032(14) C5 0.0528(18) 0.071(2) 0.101(3) -0.0418(19) 0.0057(17) 0.0066(16) C6 0.0433(15) 0.0561(17) 0.077(2) -0.0183(15) 0.0104(13) -0.0071(13) C7 0.0370(12) 0.0396(12) 0.0408(13) 0.0015(10) 0.0120(10) -0.0013(10) C8 0.0465(14) 0.0479(14) 0.0420(13) 0.0003(11) 0.0093(11) 0.0000(12) C9 0.0573(17) 0.072(2) 0.0425(15) 0.0160(14) 0.0104(13) 0.0161(15) C10 0.0688(19) 0.0474(16) 0.0648(19) 0.0231(14) 0.0327(16) 0.0182(14) C11 0.0571(16) 0.0371(14) 0.0679(18) 0.0054(13) 0.0306(14) 0.0027(12) C12 0.0433(14) 0.0415(14) 0.0492(15) -0.0003(11) 0.0140(11) -0.0005(11) C13 0.0432(13) 0.0298(11) 0.0434(13) 0.0006(10) 0.0011(10) -0.0038(10) C14 0.0528(15) 0.0364(13) 0.0540(16) 0.0052(11) -0.0041(12) -0.0050(12) C15 0.090(2) 0.0479(16) 0.0438(16) 0.0120(13) -0.0151(15) -0.0226(16) C16 0.098(3) 0.0568(18) 0.0420(16) -0.0053(13) 0.0180(16) -0.0243(18) C17 0.075(2) 0.0567(17) 0.0557(18) -0.0015(14) 0.0275(16) -0.0039(15) C18 0.0519(16) 0.0501(15) 0.0479(15) 0.0055(12) 0.0084(12) 0.0012(12) C19 0.0324(12) 0.0424(13) 0.0464(14) -0.0066(11) 0.0094(10) -0.0032(10) C20 0.0403(13) 0.0445(14) 0.0476(14) -0.0024(11) 0.0105(11) 0.0036(11) C21 0.0448(14) 0.0682(19) 0.0446(15) -0.0138(13) 0.0016(11) 0.0057(13) C22 0.0459(15) 0.0548(17) 0.0677(19) -0.0278(14) 0.0079(13) -0.0061(13) C23 0.0449(15) 0.0397(14) 0.0713(19) -0.0040(13) 0.0139(13) -0.0041(11) C24 0.0398(13) 0.0510(15) 0.0451(14) 0.0027(12) 0.0087(11) -0.0058(11) C25 0.0365(13) 0.0391(13) 0.0612(16) 0.0019(12) 0.0095(11) -0.0020(10) C26 0.0465(15) 0.0524(16) 0.0687(19) -0.0048(13) 0.0148(13) -0.0012(12) C27 0.0600(19) 0.0557(18) 0.101(3) -0.0121(18) 0.0292(18) 0.0018(15) C28 0.062(2) 0.0497(18) 0.135(3) 0.005(2) 0.033(2) 0.0101(16) C29 0.063(2) 0.068(2) 0.110(3) 0.030(2) 0.0079(19) 0.0152(17) C30 0.0521(17) 0.0570(17) 0.074(2) 0.0115(15) 0.0056(14) 0.0039(14) C31 0.0445(13) 0.0354(12) 0.0393(13) 0.0029(10) 0.0019(10) -0.0013(10) C32 0.0748(19) 0.0482(16) 0.0476(16) -0.0017(12) 0.0137(14) -0.0193(14) C33 0.081(2) 0.0663(19) 0.0448(16) 0.0073(14) 0.0150(14) -0.0121(16) C34 0.0727(19) 0.0705(19) 0.0382(14) -0.0017(13) 0.0018(13) 0.0013(16) C35 0.071(2) 0.0612(18) 0.0522(17) -0.0109(14) -0.0070(14) -0.0143(15) C36 0.0544(16) 0.0495(15) 0.0489(15) 0.0022(12) 0.0025(12) -0.0133(12) C37 0.0412(13) 0.0493(14) 0.0384(13) 0.0072(11) 0.0052(10) -0.0015(11) C38 0.0473(16) 0.0606(18) 0.083(2) 0.0211(16) 0.0156(15) 0.0015(13) C39 0.063(2) 0.082(2) 0.105(3) 0.034(2) 0.0288(19) -0.0058(18) C40 0.089(3) 0.082(2) 0.089(3) 0.050(2) 0.025(2) 0.005(2) C41 0.082(2) 0.092(3) 0.104(3) 0.059(2) 0.024(2) 0.026(2) C42 0.0539(17) 0.080(2) 0.086(2) 0.0399(18) 0.0193(16) 0.0154(16) N1 0.0341(11) 0.0487(13) 0.0602(14) -0.0173(11) 0.0084(10) 0.0000(10) B1 0.0359(14) 0.0348(13) 0.0420(15) -0.0013(11) 0.0024(11) -0.0030(11) F1 0.0798(13) 0.1138(16) 0.0821(13) -0.0353(11) 0.0423(10) -0.0528(12) F2 0.1195(17) 0.0860(14) 0.0901(14) 0.0040(11) 0.0070(12) -0.0677(13) F3 0.1019(15) 0.0439(10) 0.1420(19) -0.0318(11) -0.0427(13) 0.0058(10) F4 0.0859(15) 0.140(2) 0.171(2) -0.1062(19) 0.0342(15) -0.0055(14) F5 0.0726(12) 0.1128(16) 0.1106(16) -0.0533(13) 0.0484(11) -0.0383(12) F6 0.0663(10) 0.0609(10) 0.0542(9) -0.0038(8) -0.0119(8) -0.0030(8) F7 0.0928(14) 0.1033(15) 0.0565(11) 0.0197(10) -0.0099(10) 0.0250(11) F8 0.1117(15) 0.0683(12) 0.0872(13) 0.0419(10) 0.0370(11) 0.0327(11) F9 0.0872(13) 0.0346(8) 0.1103(15) 0.0002(9) 0.0355(11) -0.0024(8) F10 0.0604(9) 0.0446(8) 0.0695(10) -0.0099(7) 0.0004(8) -0.0089(7) F11 0.0616(10) 0.0629(10) 0.0798(12) 0.0111(9) -0.0145(9) 0.0148(8) F12 0.1180(16) 0.1070(16) 0.0584(11) 0.0266(11) -0.0322(11) -0.0253(13) F13 0.155(2) 0.1061(16) 0.0438(10) -0.0106(10) 0.0279(11) -0.0416(14) F14 0.1044(16) 0.1115(17) 0.0880(14) -0.0060(12) 0.0561(12) 0.0169(13) F15 0.0498(9) 0.1017(14) 0.0651(10) 0.0192(9) 0.0159(8) 0.0245(9) F16 0.0687(10) 0.0524(9) 0.0663(10) 0.0058(8) 0.0029(8) 0.0118(8) F17 0.0786(12) 0.1020(14) 0.0545(10) -0.0187(10) -0.0145(9) 0.0146(10) F18 0.0809(13) 0.0751(12) 0.1000(14) -0.0465(11) -0.0029(11) -0.0100(10) F19 0.0787(12) 0.0426(9) 0.1151(15) 0.0030(9) 0.0126(11) -0.0073(8) F20 0.0670(10) 0.0678(11) 0.0580(10) 0.0151(8) 0.0008(8) -0.0102(8) P1 0.0355(3) 0.0378(3) 0.0404(3) 0.0003(3) 0.0052(2) -0.0023(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 1.373(3) . ? C1 C6 1.381(4) . ? C1 B1 1.634(3) . ? C2 F1 1.336(3) . ? C2 C3 1.384(4) . ? C3 F2 1.340(3) . ? C3 C4 1.356(5) . ? C4 F3 1.346(3) . ? C4 C5 1.359(5) . ? C5 F4 1.360(4) . ? C5 C6 1.374(4) . ? C6 F5 1.355(3) . ? C7 C8 1.381(3) . ? C7 C12 1.386(3) . ? C7 B1 1.632(3) . ? C8 F6 1.347(3) . ? C8 C9 1.383(4) . ? C9 F7 1.345(3) . ? C9 C10 1.364(4) . ? C10 F8 1.347(3) . ? C10 C11 1.360(4) . ? C11 F9 1.345(3) . ? C11 C12 1.370(4) . ? C12 F10 1.351(3) . ? C13 C18 1.375(3) . ? C13 C14 1.378(3) . ? C13 B1 1.633(4) . ? C14 F11 1.351(3) . ? C14 C15 1.386(4) . ? C15 F12 1.351(3) . ? C15 C16 1.358(5) . ? C16 C17 1.350(4) . ? C16 F13 1.352(3) . ? C17 F14 1.342(4) . ? C17 C18 1.376(4) . ? C18 F15 1.358(3) . ? C19 C20 1.380(3) . ? C19 C24 1.378(3) . ? C19 N1 1.415(3) . ? C20 F16 1.329(3) . ? C20 C21 1.374(4) . ? C21 F17 1.337(3) . ? C21 C22 1.370(4) . ? C22 F18 1.333(3) . ? C22 C23 1.369(4) . ? C23 F19 1.338(3) . ? C23 C24 1.367(4) . ? C24 F20 1.338(3) . ? C25 C30 1.380(4) . ? C25 C26 1.398(4) . ? C25 P1 1.774(3) . ? C26 C27 1.374(4) . ? C27 C28 1.365(5) . ? C28 C29 1.369(5) . ? C29 C30 1.389(4) . ? C31 C36 1.383(3) . ? C31 C32 1.387(3) . ? C31 P1 1.773(2) . ? C32 C33 1.373(4) . ? C33 C34 1.363(4) . ? C34 C35 1.364(4) . ? C35 C36 1.376(4) . ? C37 C38 1.379(4) . ? C37 C42 1.382(4) . ? C37 P1 1.776(2) . ? C38 C39 1.383(4) . ? C39 C40 1.359(5) . ? C40 C41 1.359(5) . ? C41 C42 1.378(4) . ? N1 P1 1.645(2) . ? 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 C2 C1 C6 113.0(2) . . ? C2 C1 B1 126.3(2) . . ? C6 C1 B1 120.6(2) . . ? F1 C2 C1 119.7(2) . . ? F1 C2 C3 116.2(2) . . ? C1 C2 C3 124.1(3) . . ? F2 C3 C4 119.8(3) . . ? F2 C3 C2 120.3(3) . . ? C4 C3 C2 119.8(3) . . ? F3 C4 C5 120.7(3) . . ? F3 C4 C3 120.3(3) . . ? C5 C4 C3 118.9(3) . . ? C4 C5 F4 119.9(3) . . ? C4 C5 C6 119.5(3) . . ? F4 C5 C6 120.5(3) . . ? F5 C6 C5 115.9(3) . . ? F5 C6 C1 119.5(2) . . ? C5 C6 C1 124.6(3) . . ? C8 C7 C12 113.1(2) . . ? C8 C7 B1 127.6(2) . . ? C12 C7 B1 119.3(2) . . ? F6 C8 C9 115.7(2) . . ? F6 C8 C7 120.5(2) . . ? C9 C8 C7 123.8(2) . . ? F7 C9 C10 120.6(3) . . ? F7 C9 C8 119.9(3) . . ? C10 C9 C8 119.5(3) . . ? F8 C10 C11 120.7(3) . . ? F8 C10 C9 119.7(3) . . ? C11 C10 C9 119.5(2) . . ? F9 C11 C10 119.7(2) . . ? F9 C11 C12 121.2(3) . . ? C10 C11 C12 119.0(3) . . ? F10 C12 C11 116.0(2) . . ? F10 C12 C7 119.1(2) . . ? C11 C12 C7 124.9(3) . . ? C18 C13 C14 113.1(2) . . ? C18 C13 B1 125.3(2) . . ? C14 C13 B1 121.5(2) . . ? F11 C14 C13 119.4(2) . . ? F11 C14 C15 116.8(2) . . ? C13 C14 C15 123.8(3) . . ? F12 C15 C16 120.7(3) . . ? F12 C15 C14 120.0(3) . . ? C16 C15 C14 119.3(3) . . ? C17 C16 F13 120.9(3) . . ? C17 C16 C15 119.8(3) . . ? F13 C16 C15 119.3(3) . . ? F14 C17 C16 119.9(3) . . ? F14 C17 C18 121.1(3) . . ? C16 C17 C18 119.0(3) . . ? F15 C18 C13 119.8(2) . . ? F15 C18 C17 115.3(2) . . ? C13 C18 C17 124.9(3) . . ? C20 C19 C24 117.6(2) . . ? C20 C19 N1 121.4(2) . . ? C24 C19 N1 120.8(2) . . ? F16 C20 C21 119.1(2) . . ? F16 C20 C19 119.5(2) . . ? C21 C20 C19 121.4(2) . . ? F17 C21 C22 120.4(2) . . ? F17 C21 C20 119.9(3) . . ? C22 C21 C20 119.7(3) . . ? F18 C22 C21 120.4(3) . . ? F18 C22 C23 119.9(3) . . ? C21 C22 C23 119.8(2) . . ? F19 C23 C24 120.3(3) . . ? F19 C23 C22 119.6(2) . . ? C24 C23 C22 120.1(2) . . ? F20 C24 C23 118.5(2) . . ? F20 C24 C19 120.1(2) . . ? C23 C24 C19 121.4(2) . . ? C30 C25 C26 120.4(3) . . ? C30 C25 P1 120.3(2) . . ? C26 C25 P1 119.2(2) . . ? C27 C26 C25 119.5(3) . . ? C28 C27 C26 119.9(3) . . ? C27 C28 C29 121.2(3) . . ? C28 C29 C30 120.1(3) . . ? C25 C30 C29 118.9(3) . . ? C36 C31 C32 119.9(2) . . ? C36 C31 P1 121.40(19) . . ? C32 C31 P1 118.75(19) . . ? C33 C32 C31 119.8(3) . . ? C34 C33 C32 120.1(3) . . ? C33 C34 C35 120.2(3) . . ? C34 C35 C36 121.0(3) . . ? C35 C36 C31 118.9(3) . . ? C38 C37 C42 119.7(2) . . ? C38 C37 P1 122.9(2) . . ? C42 C37 P1 117.4(2) . . ? C37 C38 C39 119.6(3) . . ? C40 C39 C38 120.0(3) . . ? C39 C40 C41 121.0(3) . . ? C40 C41 C42 119.9(3) . . ? C41 C42 C37 119.8(3) . . ? C19 N1 P1 128.12(18) . . ? C7 B1 C1 114.33(19) . . ? C7 B1 C13 109.46(19) . . ? C1 B1 C13 113.60(19) . . ? N1 P1 C31 104.39(11) . . ? N1 P1 C37 112.21(12) . . ? C31 P1 C37 109.08(11) . . ? N1 P1 C25 108.40(12) . . ? C31 P1 C25 113.13(12) . . ? C37 P1 C25 109.60(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.538 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.050 #===end data_cj019_0m _database_code_depnum_ccdc_archive 'CCDC 873944' #TrackingRef 'combined-CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H26 B F15 N O2 P' _chemical_formula_weight 987.49 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1433(8) _cell_length_b 17.7446(16) _cell_length_c 26.879(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.266(3) _cell_angle_gamma 90.00 _cell_volume 4357.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8231 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 26.01 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9635 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37373 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9946 _reflns_number_gt 7243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0631P)^2^+5.7785P] 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 9946 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.003 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 0.22364(8) 0.70240(4) 0.16218(2) 0.02238(15) Uani 1 1 d . . . C1 C 0.1141(3) 0.78600(15) 0.15882(10) 0.0277(6) Uani 1 1 d . . . C2 C 0.1739(4) 0.85400(17) 0.17550(12) 0.0372(7) Uani 1 1 d . . . H2 H 0.2702 0.8560 0.1879 0.045 Uiso 1 1 calc R . . C3 C 0.0891(4) 0.91871(18) 0.17354(14) 0.0463(8) Uani 1 1 d . . . H3 H 0.1294 0.9643 0.1842 0.056 Uiso 1 1 calc R . . C4 C -0.0544(4) 0.91618(19) 0.15598(14) 0.0502(9) Uani 1 1 d . . . H4 H -0.1101 0.9600 0.1544 0.060 Uiso 1 1 calc R . . C5 C -0.1155(4) 0.8484(2) 0.14071(15) 0.0529(9) Uani 1 1 d . . . H5 H -0.2130 0.8465 0.1296 0.063 Uiso 1 1 calc R . . C6 C -0.0323(4) 0.78339(18) 0.14186(12) 0.0405(7) Uani 1 1 d . . . H6 H -0.0737 0.7379 0.1314 0.049 Uiso 1 1 calc R . . C7 C 0.1168(3) 0.62244(15) 0.14212(10) 0.0244(5) Uani 1 1 d . . . C8 C 0.0826(4) 0.61676(19) 0.09134(11) 0.0409(8) Uani 1 1 d . . . H8 H 0.1161 0.6529 0.0695 0.049 Uiso 1 1 calc R . . C9 C -0.0018(4) 0.5569(2) 0.07362(12) 0.0447(8) Uani 1 1 d . . . H9 H -0.0273 0.5537 0.0399 0.054 Uiso 1 1 calc R . . C10 C -0.0477(4) 0.50236(19) 0.10546(12) 0.0401(7) Uani 1 1 d . . . H10 H -0.1026 0.4618 0.0932 0.048 Uiso 1 1 calc R . . C11 C -0.0127(3) 0.50754(17) 0.15576(12) 0.0378(7) Uani 1 1 d . . . H11 H -0.0434 0.4702 0.1772 0.045 Uiso 1 1 calc R . . C12 C 0.0679(3) 0.56798(16) 0.17448(11) 0.0303(6) Uani 1 1 d . . . H12 H 0.0891 0.5720 0.2085 0.036 Uiso 1 1 calc R . . C13 C 0.3731(3) 0.70777(15) 0.12116(9) 0.0262(6) Uani 1 1 d . . . C14 C 0.4624(3) 0.64455(17) 0.11714(10) 0.0335(7) Uani 1 1 d . . . H14 H 0.4431 0.6012 0.1352 0.040 Uiso 1 1 calc R . . C15 C 0.5802(4) 0.6463(2) 0.08615(12) 0.0420(8) Uani 1 1 d . . . H15 H 0.6417 0.6048 0.0841 0.050 Uiso 1 1 calc R . . C16 C 0.6056(4) 0.7103(2) 0.05839(12) 0.0465(9) Uani 1 1 d . . . H16 H 0.6845 0.7117 0.0376 0.056 Uiso 1 1 calc R . . C17 C 0.5147(4) 0.77229(19) 0.06138(11) 0.0440(8) Uani 1 1 d . . . H17 H 0.5312 0.8146 0.0419 0.053 Uiso 1 1 calc R . . C18 C 0.3995(4) 0.77176(17) 0.09307(10) 0.0336(7) Uani 1 1 d . . . H18 H 0.3400 0.8140 0.0956 0.040 Uiso 1 1 calc R . . C19 C 0.4563(3) 0.68163(19) 0.23039(10) 0.0328(7) Uani 1 1 d . . . C20 C 0.5533(4) 0.7399(3) 0.22877(13) 0.0563(11) Uani 1 1 d . . . H20 H 0.5222 0.7881 0.2198 0.068 Uiso 1 1 calc R . . C21 C 0.7056(4) 0.7248(3) 0.24140(15) 0.0673(13) Uani 1 1 d . . . H21 H 0.7748 0.7632 0.2407 0.081 Uiso 1 1 calc R . . C22 C 0.7459(5) 0.6532(3) 0.25431(16) 0.0698(13) Uani 1 1 d . . . H22 H 0.8442 0.6433 0.2618 0.084 Uiso 1 1 calc R . . C23 C 0.6494(4) 0.5964(3) 0.25663(15) 0.0651(12) Uani 1 1 d . . . H23 H 0.6800 0.5486 0.2666 0.078 Uiso 1 1 calc R . . C24 C 0.5032(4) 0.6103(2) 0.24398(12) 0.0428(8) Uani 1 1 d . . . H24 H 0.4360 0.5710 0.2447 0.051 Uiso 1 1 calc R . . C25 C 0.3508(3) 0.70999(15) 0.38888(9) 0.0219(5) Uani 1 1 d . . . C26 C 0.4585(3) 0.65515(15) 0.38641(9) 0.0248(5) Uani 1 1 d . . . C27 C 0.5907(3) 0.65687(17) 0.41284(11) 0.0316(6) Uani 1 1 d . . . C28 C 0.6200(3) 0.7161(2) 0.44439(11) 0.0388(7) Uani 1 1 d . . . C29 C 0.5175(4) 0.77131(19) 0.44920(11) 0.0374(7) Uani 1 1 d . . . C30 C 0.3849(3) 0.76734(16) 0.42226(10) 0.0291(6) Uani 1 1 d . . . C31 C 0.1008(3) 0.77704(15) 0.34783(9) 0.0232(5) Uani 1 1 d . . . C32 C -0.0487(3) 0.78165(15) 0.35430(10) 0.0250(5) Uani 1 1 d . . . C33 C -0.1286(3) 0.84738(17) 0.34889(12) 0.0333(6) Uani 1 1 d . . . C34 C -0.0614(4) 0.91238(17) 0.33591(15) 0.0445(8) Uani 1 1 d . . . C35 C 0.0865(4) 0.91086(17) 0.32744(15) 0.0452(8) Uani 1 1 d . . . C36 C 0.1626(3) 0.84471(16) 0.33346(12) 0.0325(6) Uani 1 1 d . . . C37 C 0.1161(3) 0.62601(15) 0.36982(9) 0.0218(5) Uani 1 1 d . . . C38 C 0.0873(3) 0.56107(15) 0.34318(10) 0.0251(5) Uani 1 1 d . . . C39 C 0.0089(3) 0.50079(15) 0.36117(10) 0.0273(6) Uani 1 1 d . . . C40 C -0.0428(3) 0.50355(15) 0.40831(11) 0.0278(6) Uani 1 1 d . . . C41 C -0.0138(3) 0.56618(15) 0.43723(10) 0.0250(5) Uani 1 1 d . . . C42 C 0.0639(3) 0.62471(15) 0.41774(9) 0.0228(5) Uani 1 1 d . . . C43 C 0.2025(3) 0.69611(14) 0.25939(9) 0.0220(5) Uani 1 1 d . . . N1 N 0.2999(2) 0.69321(12) 0.21939(8) 0.0226(5) Uani 1 1 d . . . O1 O 0.27220(19) 0.69040(10) 0.30182(6) 0.0231(4) Uani 1 1 d . . . O2 O 0.0724(2) 0.70306(11) 0.24974(7) 0.0290(4) Uani 1 1 d . . . B1 B 0.2034(3) 0.70164(17) 0.35210(10) 0.0206(6) Uani 1 1 d . . . F1 F 0.43521(17) 0.59398(9) 0.35735(6) 0.0314(4) Uani 1 1 d . . . F2 F 0.68743(19) 0.60086(11) 0.40845(7) 0.0465(5) Uani 1 1 d . . . F3 F 0.7484(2) 0.71955(14) 0.47085(8) 0.0596(6) Uani 1 1 d . . . F4 F 0.5454(2) 0.83025(13) 0.47985(8) 0.0574(6) Uani 1 1 d . . . F5 F 0.2891(2) 0.82354(10) 0.43042(7) 0.0428(5) Uani 1 1 d . . . F6 F 0.30674(19) 0.84742(10) 0.32418(8) 0.0456(5) Uani 1 1 d . . . F7 F 0.1544(2) 0.97442(11) 0.31420(12) 0.0787(9) Uani 1 1 d . . . F8 F -0.1366(2) 0.97683(11) 0.33130(11) 0.0741(8) Uani 1 1 d . . . F9 F -0.27364(19) 0.84745(11) 0.35668(9) 0.0519(5) Uani 1 1 d . . . F10 F -0.12670(17) 0.72041(9) 0.36664(7) 0.0348(4) Uani 1 1 d . . . F11 F 0.1354(2) 0.55232(9) 0.29638(6) 0.0346(4) Uani 1 1 d . . . F12 F -0.0176(2) 0.43932(9) 0.33267(7) 0.0416(4) Uani 1 1 d . . . F13 F -0.1228(2) 0.44632(9) 0.42547(7) 0.0396(4) Uani 1 1 d . . . F14 F -0.06488(18) 0.57030(9) 0.48324(6) 0.0340(4) Uani 1 1 d . . . F15 F 0.08582(18) 0.68571(9) 0.44728(5) 0.0291(4) Uani 1 1 d . . . C47 C 0.1241(5) -0.0042(4) 0.0295(2) 0.0867(18) Uani 1 1 d . . . H47 H 0.2083 -0.0068 0.0500 0.104 Uiso 1 1 calc R . . C48 C 0.0286(6) -0.0637(3) 0.02752(18) 0.0821(15) Uani 1 1 d . . . H48 H 0.0493 -0.1070 0.0460 0.098 Uiso 1 1 calc R . . C49 C 0.0966(6) 0.0595(4) 0.0014(2) 0.0832(17) Uani 1 1 d . . . H49 H 0.1630 0.0992 0.0022 0.100 Uiso 1 1 calc R . . C44 C 0.4915(5) 0.4380(2) 0.03004(15) 0.0626(11) Uani 1 1 d . . . H44 H 0.4868 0.3955 0.0502 0.075 Uiso 1 1 calc R . . C45 C 0.3749(5) 0.4834(3) 0.02400(15) 0.0613(11) Uani 1 1 d . . . H45 H 0.2898 0.4725 0.0404 0.074 Uiso 1 1 calc R . . C46 C 0.6202(5) 0.4547(3) 0.00590(17) 0.0648(12) Uani 1 1 d . . . H46 H 0.7019 0.4238 0.0102 0.078 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 0.0264(3) 0.0223(3) 0.0185(3) -0.0003(3) 0.0010(2) -0.0044(3) C1 0.0338(15) 0.0240(14) 0.0253(13) 0.0026(11) 0.0017(11) 0.0018(11) C2 0.0427(18) 0.0296(15) 0.0395(17) -0.0026(13) 0.0052(13) -0.0027(13) C3 0.059(2) 0.0259(16) 0.054(2) -0.0048(14) 0.0076(17) -0.0015(15) C4 0.062(2) 0.0306(17) 0.058(2) 0.0047(16) 0.0015(18) 0.0123(16) C5 0.048(2) 0.042(2) 0.067(2) 0.0076(18) -0.0146(18) 0.0097(17) C6 0.0462(19) 0.0287(16) 0.0456(18) 0.0045(14) -0.0121(14) -0.0013(14) C7 0.0251(13) 0.0226(13) 0.0254(13) -0.0014(10) 0.0004(10) -0.0025(11) C8 0.056(2) 0.0414(18) 0.0247(14) 0.0004(13) -0.0009(13) -0.0207(16) C9 0.056(2) 0.049(2) 0.0281(15) -0.0066(14) -0.0043(14) -0.0207(17) C10 0.0401(18) 0.0372(17) 0.0427(18) -0.0085(14) -0.0019(13) -0.0147(14) C11 0.0411(18) 0.0307(16) 0.0415(17) 0.0041(13) 0.0012(13) -0.0138(14) C12 0.0341(16) 0.0300(15) 0.0266(14) 0.0025(11) -0.0010(11) -0.0064(12) C13 0.0323(15) 0.0284(14) 0.0179(12) -0.0031(10) 0.0020(10) -0.0094(12) C14 0.0430(18) 0.0313(15) 0.0269(14) 0.0005(12) 0.0093(12) -0.0050(13) C15 0.0455(19) 0.0441(18) 0.0375(17) -0.0065(14) 0.0141(14) -0.0037(15) C16 0.050(2) 0.057(2) 0.0342(17) -0.0079(15) 0.0197(14) -0.0184(17) C17 0.065(2) 0.0403(18) 0.0278(15) -0.0004(13) 0.0163(15) -0.0189(17) C18 0.0465(18) 0.0300(15) 0.0246(14) 0.0010(12) 0.0058(12) -0.0045(13) C19 0.0198(13) 0.060(2) 0.0190(13) -0.0073(13) 0.0039(10) -0.0126(13) C20 0.050(2) 0.083(3) 0.0348(18) 0.0013(18) -0.0010(15) -0.034(2) C21 0.042(2) 0.112(4) 0.049(2) -0.002(2) 0.0103(17) -0.036(2) C22 0.040(2) 0.119(4) 0.051(2) 0.005(3) 0.0112(17) -0.004(3) C23 0.040(2) 0.103(4) 0.052(2) 0.002(2) 0.0063(17) 0.022(2) C24 0.0301(16) 0.062(2) 0.0369(17) -0.0091(16) 0.0005(13) 0.0119(15) C25 0.0205(12) 0.0265(13) 0.0188(11) 0.0013(10) 0.0024(9) 0.0014(10) C26 0.0254(14) 0.0269(14) 0.0222(13) 0.0018(10) 0.0018(10) 0.0007(11) C27 0.0217(14) 0.0404(17) 0.0328(15) 0.0042(13) 0.0008(11) 0.0043(12) C28 0.0257(15) 0.056(2) 0.0345(16) 0.0019(14) -0.0062(12) -0.0052(14) C29 0.0386(17) 0.0460(18) 0.0270(15) -0.0104(13) -0.0043(12) -0.0073(14) C30 0.0300(15) 0.0330(15) 0.0246(13) -0.0040(11) 0.0035(11) 0.0023(12) C31 0.0231(13) 0.0250(13) 0.0215(12) 0.0013(10) 0.0011(10) 0.0015(10) C32 0.0231(13) 0.0253(13) 0.0269(13) -0.0002(11) 0.0037(10) 0.0014(11) C33 0.0242(14) 0.0320(15) 0.0440(17) -0.0007(13) 0.0051(12) 0.0064(12) C34 0.0327(17) 0.0241(15) 0.077(2) 0.0045(15) 0.0036(16) 0.0089(13) C35 0.0338(18) 0.0238(15) 0.078(3) 0.0111(16) 0.0064(16) -0.0020(13) C36 0.0207(14) 0.0301(15) 0.0469(17) 0.0050(13) 0.0040(12) 0.0012(11) C37 0.0194(12) 0.0242(13) 0.0216(12) 0.0003(10) -0.0010(9) 0.0041(10) C38 0.0263(14) 0.0264(13) 0.0226(13) -0.0003(10) 0.0014(10) 0.0050(11) C39 0.0269(14) 0.0220(13) 0.0326(14) -0.0032(11) -0.0043(11) 0.0014(11) C40 0.0222(13) 0.0232(13) 0.0380(15) 0.0080(12) -0.0008(11) 0.0006(11) C41 0.0209(13) 0.0290(14) 0.0254(13) 0.0054(11) 0.0034(10) 0.0052(11) C42 0.0219(13) 0.0243(13) 0.0222(12) -0.0005(10) -0.0008(10) 0.0033(10) C43 0.0221(13) 0.0216(12) 0.0226(12) -0.0014(10) 0.0041(9) -0.0017(10) N1 0.0207(11) 0.0281(12) 0.0192(10) -0.0006(9) 0.0026(8) -0.0022(9) O1 0.0207(9) 0.0304(10) 0.0183(8) -0.0009(7) 0.0034(7) 0.0025(7) O2 0.0210(10) 0.0394(11) 0.0264(9) 0.0012(8) 0.0010(7) 0.0023(8) B1 0.0210(14) 0.0239(14) 0.0168(13) -0.0008(11) 0.0016(10) 0.0018(11) F1 0.0296(9) 0.0276(8) 0.0368(9) -0.0057(7) -0.0016(7) 0.0074(7) F2 0.0265(9) 0.0533(12) 0.0592(12) 0.0035(10) -0.0053(8) 0.0151(8) F3 0.0347(11) 0.0861(17) 0.0561(12) -0.0060(12) -0.0224(9) -0.0013(11) F4 0.0587(13) 0.0634(14) 0.0487(12) -0.0281(10) -0.0150(10) -0.0052(11) F5 0.0442(11) 0.0421(10) 0.0419(10) -0.0193(8) -0.0028(8) 0.0107(8) F6 0.0238(9) 0.0351(10) 0.0786(14) 0.0139(9) 0.0111(9) -0.0005(7) F7 0.0409(12) 0.0288(11) 0.167(3) 0.0293(14) 0.0111(14) -0.0006(9) F8 0.0416(12) 0.0274(10) 0.154(3) 0.0158(13) 0.0144(14) 0.0154(9) F9 0.0237(9) 0.0401(11) 0.0928(16) 0.0062(10) 0.0144(9) 0.0117(8) F10 0.0232(8) 0.0315(9) 0.0503(10) 0.0089(8) 0.0068(7) 0.0004(7) F11 0.0492(11) 0.0317(9) 0.0234(8) -0.0076(7) 0.0070(7) -0.0001(8) F12 0.0536(12) 0.0270(9) 0.0442(10) -0.0096(8) 0.0008(8) -0.0079(8) F13 0.0401(10) 0.0315(9) 0.0473(10) 0.0086(8) 0.0039(8) -0.0104(8) F14 0.0373(10) 0.0374(9) 0.0281(8) 0.0074(7) 0.0097(7) 0.0004(8) F15 0.0357(9) 0.0301(8) 0.0218(8) -0.0044(6) 0.0058(6) -0.0018(7) C47 0.050(3) 0.136(5) 0.075(3) -0.050(4) 0.006(2) -0.006(3) C48 0.075(3) 0.117(4) 0.056(3) -0.033(3) 0.017(2) -0.007(3) C49 0.061(3) 0.113(5) 0.078(3) -0.046(3) 0.028(3) -0.029(3) C44 0.087(3) 0.056(2) 0.044(2) 0.0046(18) -0.007(2) -0.010(2) C45 0.057(2) 0.074(3) 0.053(2) -0.010(2) 0.0090(19) -0.015(2) C46 0.059(3) 0.067(3) 0.067(3) -0.017(2) -0.019(2) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N1 1.671(2) . ? P1 C1 1.790(3) . ? P1 C13 1.792(3) . ? P1 C7 1.793(3) . ? C1 C2 1.392(4) . ? C1 C6 1.398(4) . ? C2 C3 1.385(5) . ? C3 C4 1.377(5) . ? C4 C5 1.382(5) . ? C5 C6 1.381(5) . ? C7 C12 1.386(4) . ? C7 C8 1.392(4) . ? C8 C9 1.387(4) . ? C9 C10 1.368(5) . ? C10 C11 1.380(4) . ? C11 C12 1.384(4) . ? C13 C18 1.390(4) . ? C13 C14 1.394(4) . ? C14 C15 1.388(4) . ? C15 C16 1.383(5) . ? C16 C17 1.383(5) . ? C17 C18 1.380(4) . ? C19 C20 1.364(5) . ? C19 C24 1.381(5) . ? C19 N1 1.463(3) . ? C20 C21 1.445(6) . ? C21 C22 1.364(7) . ? C22 C23 1.342(7) . ? C23 C24 1.387(5) . ? C25 C30 1.384(4) . ? C25 C26 1.388(4) . ? C25 B1 1.646(4) . ? C26 F1 1.349(3) . ? C26 C27 1.378(4) . ? C27 F2 1.339(3) . ? C27 C28 1.370(4) . ? C28 F3 1.350(3) . ? C28 C29 1.365(5) . ? C29 F4 1.350(3) . ? C29 C30 1.389(4) . ? C30 F5 1.351(3) . ? C31 C36 1.389(4) . ? C31 C32 1.387(4) . ? C31 B1 1.636(4) . ? C32 F10 1.348(3) . ? C32 C33 1.381(4) . ? C33 F9 1.350(3) . ? C33 C34 1.359(4) . ? C34 F8 1.338(3) . ? C34 C35 1.381(5) . ? C35 F7 1.342(4) . ? C35 C36 1.371(4) . ? C36 F6 1.352(3) . ? C37 C38 1.377(4) . ? C37 C42 1.392(3) . ? C37 B1 1.642(4) . ? C38 F11 1.358(3) . ? C38 C39 1.385(4) . ? C39 F12 1.349(3) . ? C39 C40 1.371(4) . ? C40 F13 1.344(3) . ? C40 C41 1.376(4) . ? C41 F14 1.341(3) . ? C41 C42 1.374(4) . ? C42 F15 1.353(3) . ? C43 O2 1.214(3) . ? C43 O1 1.288(3) . ? C43 N1 1.424(3) . ? O1 B1 1.526(3) . ? C47 C49 1.376(8) . ? C47 C48 1.370(7) . ? C48 C49 1.361(7) 3 ? C49 C48 1.361(7) 3 ? C44 C45 1.341(6) . ? C44 C46 1.398(6) . ? C45 C46 1.364(6) 3_665 ? C46 C45 1.364(6) 3_665 ? 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 N1 P1 C1 109.85(12) . . ? N1 P1 C13 105.71(12) . . ? C1 P1 C13 111.33(13) . . ? N1 P1 C7 113.70(12) . . ? C1 P1 C7 110.09(13) . . ? C13 P1 C7 106.05(12) . . ? C2 C1 C6 119.5(3) . . ? C2 C1 P1 119.4(2) . . ? C6 C1 P1 121.0(2) . . ? C3 C2 C1 119.6(3) . . ? C4 C3 C2 120.7(3) . . ? C3 C4 C5 119.9(3) . . ? C6 C5 C4 120.3(3) . . ? C5 C6 C1 120.0(3) . . ? C12 C7 C8 119.9(3) . . ? C12 C7 P1 123.2(2) . . ? C8 C7 P1 116.8(2) . . ? C9 C8 C7 119.5(3) . . ? C10 C9 C8 120.5(3) . . ? C9 C10 C11 120.0(3) . . ? C10 C11 C12 120.5(3) . . ? C7 C12 C11 119.5(3) . . ? C18 C13 C14 120.0(3) . . ? C18 C13 P1 122.0(2) . . ? C14 C13 P1 117.9(2) . . ? C15 C14 C13 119.9(3) . . ? C16 C15 C14 119.6(3) . . ? C15 C16 C17 120.5(3) . . ? C18 C17 C16 120.4(3) . . ? C17 C18 C13 119.6(3) . . ? C20 C19 C24 120.5(3) . . ? C20 C19 N1 121.2(3) . . ? C24 C19 N1 118.2(3) . . ? C19 C20 C21 118.3(4) . . ? C22 C21 C20 118.7(4) . . ? C23 C22 C21 122.7(4) . . ? C22 C23 C24 118.9(5) . . ? C19 C24 C23 120.9(4) . . ? C30 C25 C26 113.9(2) . . ? C30 C25 B1 127.8(2) . . ? C26 C25 B1 118.3(2) . . ? F1 C26 C27 115.5(2) . . ? F1 C26 C25 119.7(2) . . ? C27 C26 C25 124.7(3) . . ? F2 C27 C28 120.7(3) . . ? F2 C27 C26 120.5(3) . . ? C28 C27 C26 118.8(3) . . ? F3 C28 C29 120.2(3) . . ? F3 C28 C27 120.4(3) . . ? C29 C28 C27 119.4(3) . . ? F4 C29 C28 120.0(3) . . ? F4 C29 C30 119.8(3) . . ? C28 C29 C30 120.2(3) . . ? F5 C30 C25 121.2(2) . . ? F5 C30 C29 115.9(3) . . ? C25 C30 C29 123.0(3) . . ? C36 C31 C32 113.5(2) . . ? C36 C31 B1 119.2(2) . . ? C32 C31 B1 127.2(2) . . ? F10 C32 C33 115.1(2) . . ? F10 C32 C31 121.1(2) . . ? C33 C32 C31 123.8(3) . . ? F9 C33 C34 119.7(3) . . ? F9 C33 C32 120.2(3) . . ? C34 C33 C32 120.1(3) . . ? F8 C34 C33 120.9(3) . . ? F8 C34 C35 120.3(3) . . ? C33 C34 C35 118.8(3) . . ? F7 C35 C36 120.9(3) . . ? F7 C35 C34 119.6(3) . . ? C36 C35 C34 119.5(3) . . ? F6 C36 C35 116.2(3) . . ? F6 C36 C31 119.5(2) . . ? C35 C36 C31 124.3(3) . . ? C38 C37 C42 113.7(2) . . ? C38 C37 B1 128.2(2) . . ? C42 C37 B1 118.1(2) . . ? F11 C38 C37 121.0(2) . . ? F11 C38 C39 115.2(2) . . ? C37 C38 C39 123.8(2) . . ? F12 C39 C40 119.5(2) . . ? F12 C39 C38 120.7(2) . . ? C40 C39 C38 119.8(2) . . ? F13 C40 C39 120.2(3) . . ? F13 C40 C41 120.8(2) . . ? C39 C40 C41 119.0(2) . . ? F14 C41 C42 121.0(2) . . ? F14 C41 C40 119.9(2) . . ? C42 C41 C40 119.1(2) . . ? F15 C42 C41 116.6(2) . . ? F15 C42 C37 118.8(2) . . ? C41 C42 C37 124.5(2) . . ? O2 C43 O1 130.1(2) . . ? O2 C43 N1 118.6(2) . . ? O1 C43 N1 111.3(2) . . ? C43 N1 C19 119.2(2) . . ? C43 N1 P1 116.14(17) . . ? C19 N1 P1 124.64(17) . . ? C43 O1 B1 124.5(2) . . ? O1 B1 C31 107.5(2) . . ? O1 B1 C37 111.9(2) . . ? C31 B1 C37 113.9(2) . . ? O1 B1 C25 100.80(19) . . ? C31 B1 C25 115.0(2) . . ? C37 B1 C25 107.2(2) . . ? C49 C47 C48 120.7(5) . . ? C49 C48 C47 120.0(6) 3 . ? C48 C49 C47 119.3(5) 3 . ? C45 C44 C46 119.7(4) . . ? C44 C45 C46 120.8(4) . 3_665 ? C45 C46 C44 119.5(4) 3_665 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.719 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.062 #===end data_cj027_0m _database_code_depnum_ccdc_archive 'CCDC 873945' #TrackingRef 'combined-CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H26 B F15 N P' _chemical_formula_weight 967.50 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7176(5) _cell_length_b 24.4998(11) _cell_length_c 15.8572(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.100(2) _cell_angle_gamma 90.00 _cell_volume 4131.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9947 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 25.38 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68246 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9497 _reflns_number_gt 6714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0600P)^2^+3.2847P] 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 9497 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.873 _refine_ls_shift/su_max 0.002 _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 C1 C 0.25658(17) 1.17772(8) 0.47252(12) 0.0195(4) Uani 1 1 d . . . C2 C 0.29281(18) 1.16172(8) 0.55614(12) 0.0239(4) Uani 1 1 d . . . H22 H 0.2565 1.1786 0.6013 0.029 Uiso 1 1 calc R . . C3 C 0.38243(19) 1.12096(9) 0.57313(13) 0.0263(4) Uani 1 1 d . . . H21 H 0.4067 1.1095 0.6300 0.032 Uiso 1 1 calc R . . C4 C 0.43643(19) 1.09698(9) 0.50763(13) 0.0274(4) Uani 1 1 d . . . H1 H 0.4977 1.0691 0.5196 0.033 Uiso 1 1 calc R . . C5 C 0.4016(2) 1.11345(10) 0.42464(13) 0.0326(5) Uani 1 1 d . . . H2 H 0.4393 1.0970 0.3798 0.039 Uiso 1 1 calc R . . C6 C 0.31215(19) 1.15371(9) 0.40695(12) 0.0268(4) Uani 1 1 d . . . H3 H 0.2885 1.1650 0.3499 0.032 Uiso 1 1 calc R . . C7 C 0.07828(18) 1.22822(8) 0.34012(12) 0.0211(4) Uani 1 1 d . . . C8 C 0.03113(19) 1.17840(8) 0.30666(13) 0.0268(4) Uani 1 1 d . . . H16 H 0.0291 1.1475 0.3426 0.032 Uiso 1 1 calc R . . C9 C -0.0124(2) 1.17439(9) 0.22130(14) 0.0328(5) Uani 1 1 d . . . H17 H -0.0439 1.1406 0.1983 0.039 Uiso 1 1 calc R . . C10 C -0.0105(2) 1.21931(10) 0.16937(14) 0.0381(6) Uani 1 1 d . . . H18 H -0.0401 1.2163 0.1106 0.046 Uiso 1 1 calc R . . C11 C 0.0343(2) 1.26876(10) 0.20212(14) 0.0405(6) Uani 1 1 d . . . H19 H 0.0346 1.2996 0.1658 0.049 Uiso 1 1 calc R . . C12 C 0.0785(2) 1.27366(9) 0.28742(13) 0.0307(5) Uani 1 1 d . . . H20 H 0.1088 1.3078 0.3099 0.037 Uiso 1 1 calc R . . C13 C 0.21440(18) 1.29502(7) 0.47369(12) 0.0196(4) Uani 1 1 d . . . C14 C 0.31137(19) 1.31115(8) 0.42765(12) 0.0239(4) Uani 1 1 d . . . H14 H 0.3345 1.2887 0.3833 0.029 Uiso 1 1 calc R . . C15 C 0.37324(19) 1.35973(8) 0.44691(13) 0.0269(4) Uani 1 1 d . . . H13 H 0.4388 1.3709 0.4155 0.032 Uiso 1 1 calc R . . C16 C 0.3398(2) 1.39249(8) 0.51220(13) 0.0289(5) Uani 1 1 d . . . H12 H 0.3828 1.4259 0.5254 0.035 Uiso 1 1 calc R . . C17 C 0.2443(2) 1.37649(8) 0.55783(13) 0.0273(5) Uani 1 1 d . . . H11 H 0.2217 1.3991 0.6022 0.033 Uiso 1 1 calc R . . C18 C 0.18105(19) 1.32765(8) 0.53926(12) 0.0235(4) Uani 1 1 d . . . H10 H 0.1157 1.3166 0.5709 0.028 Uiso 1 1 calc R . . C19 C -0.09832(18) 1.23318(8) 0.49416(12) 0.0217(4) Uani 1 1 d . . . C20 C -0.1321(2) 1.28439(8) 0.46173(13) 0.0269(4) Uani 1 1 d . . . H23 H -0.0694 1.3093 0.4486 0.032 Uiso 1 1 calc R . . C21 C -0.2580(2) 1.29881(9) 0.44869(14) 0.0316(5) Uani 1 1 d . . . H24 H -0.2816 1.3339 0.4266 0.038 Uiso 1 1 calc R . . C22 C -0.3488(2) 1.26287(10) 0.46750(15) 0.0368(5) Uani 1 1 d . . . H8 H -0.4350 1.2730 0.4583 0.044 Uiso 1 1 calc R . . C23 C -0.3146(2) 1.21202(10) 0.49977(17) 0.0406(6) Uani 1 1 d . . . H7 H -0.3775 1.1872 0.5129 0.049 Uiso 1 1 calc R . . C24 C -0.1896(2) 1.19688(9) 0.51319(15) 0.0324(5) Uani 1 1 d . . . H1A H -0.1665 1.1618 0.5353 0.039 Uiso 1 1 calc R . . C25 C 0.4238(2) 0.74676(8) 0.76671(12) 0.0231(4) Uani 1 1 d . . . C26 C 0.3234(2) 0.78146(8) 0.73941(13) 0.0294(5) Uani 1 1 d . . . H40 H 0.2432 0.7666 0.7198 0.035 Uiso 1 1 calc R . . C27 C 0.3407(3) 0.83764(9) 0.74093(14) 0.0361(5) Uani 1 1 d . . . H41 H 0.2726 0.8611 0.7214 0.043 Uiso 1 1 calc R . . C28 C 0.4557(3) 0.85955(9) 0.77053(14) 0.0396(6) Uani 1 1 d . . . H35 H 0.4663 0.8980 0.7724 0.048 Uiso 1 1 calc R . . C29 C 0.5561(3) 0.82585(9) 0.79757(14) 0.0387(6) Uani 1 1 d . . . H34 H 0.6356 0.8412 0.8178 0.046 Uiso 1 1 calc R . . C30 C 0.5410(2) 0.76932(9) 0.79528(13) 0.0295(5) Uani 1 1 d . . . H33 H 0.6104 0.7462 0.8131 0.035 Uiso 1 1 calc R . . C31 C 0.40842(18) 0.68817(8) 0.76496(12) 0.0222(4) Uani 1 1 d . . . C32 C 0.40743(17) 0.63917(8) 0.76371(12) 0.0196(4) Uani 1 1 d . . . C33 C 0.55576(17) 0.55263(7) 0.74932(11) 0.0167(4) Uani 1 1 d . . . C34 C 0.66513(18) 0.58347(7) 0.75984(11) 0.0193(4) Uani 1 1 d . . . C35 C 0.78453(18) 0.56205(8) 0.76179(12) 0.0224(4) Uani 1 1 d . . . C36 C 0.80069(18) 0.50694(9) 0.75271(12) 0.0243(4) Uani 1 1 d . . . C37 C 0.6964(2) 0.47402(8) 0.74229(12) 0.0236(4) Uani 1 1 d . . . C38 C 0.57860(18) 0.49703(8) 0.74091(12) 0.0201(4) Uani 1 1 d . . . C39 C 0.41033(17) 0.55974(7) 0.91765(12) 0.0183(4) Uani 1 1 d . . . C40 C 0.37677(19) 0.53765(8) 0.99146(11) 0.0214(4) Uani 1 1 d . . . C41 C 0.29173(19) 0.49554(8) 0.98618(12) 0.0228(4) Uani 1 1 d . . . C42 C 0.24372(18) 0.47651(8) 0.90727(12) 0.0227(4) Uani 1 1 d . . . C43 C 0.27939(17) 0.50048(8) 0.83500(11) 0.0189(4) Uani 1 1 d . . . C44 C 0.36279(17) 0.54382(7) 0.83614(11) 0.0165(4) Uani 1 1 d . . . C45 C 0.31314(17) 0.56304(7) 0.66477(11) 0.0177(4) Uani 1 1 d . . . C46 C 0.18671(19) 0.57643(8) 0.66286(12) 0.0223(4) Uani 1 1 d . . . C47 C 0.09744(19) 0.57165(9) 0.59298(13) 0.0271(4) Uani 1 1 d . . . C48 C 0.1332(2) 0.55306(9) 0.51764(12) 0.0278(5) Uani 1 1 d . . . C49 C 0.2567(2) 0.53969(8) 0.51469(12) 0.0242(4) Uani 1 1 d . . . C50 C 0.34301(18) 0.54452(7) 0.58712(12) 0.0192(4) Uani 1 1 d . . . N1 N 0.03086(15) 1.21683(7) 0.50976(10) 0.0230(4) Uani 1 1 d . . . H5 H 0.0533 1.1977 0.5561 0.028 Uiso 1 1 calc R . . B1 B 0.41056(19) 0.57461(8) 0.75237(13) 0.0168(4) Uani 1 1 d . . . F1 F 0.66258(11) 0.63829(4) 0.77018(8) 0.0294(3) Uani 1 1 d . . . F2 F 0.88581(11) 0.59502(5) 0.77397(8) 0.0354(3) Uani 1 1 d . . . F3 F 0.91676(11) 0.48575(6) 0.75512(9) 0.0397(3) Uani 1 1 d . . . F4 F 0.70956(12) 0.41976(5) 0.73263(9) 0.0366(3) Uani 1 1 d . . . F5 F 0.47966(11) 0.46222(4) 0.72935(8) 0.0279(3) Uani 1 1 d . . . F6 F 0.49758(10) 0.60027(4) 0.92845(7) 0.0251(3) Uani 1 1 d . . . F7 F 0.42579(12) 0.55713(5) 1.06804(7) 0.0305(3) Uani 1 1 d . . . F8 F 0.25559(13) 0.47299(5) 1.05651(7) 0.0363(3) Uani 1 1 d . . . F9 F 0.16184(12) 0.43475(5) 0.90145(8) 0.0365(3) Uani 1 1 d . . . F10 F 0.22660(11) 0.47828(5) 0.76090(7) 0.0265(3) Uani 1 1 d . . . F11 F 0.14459(11) 0.59592(6) 0.73388(7) 0.0324(3) Uani 1 1 d . . . F12 F -0.02332(11) 0.58521(6) 0.59719(8) 0.0415(3) Uani 1 1 d . . . F13 F 0.04856(13) 0.54841(6) 0.44811(8) 0.0417(3) Uani 1 1 d . . . F14 F 0.29404(13) 0.52188(6) 0.44168(7) 0.0381(3) Uani 1 1 d . . . F15 F 0.46244(10) 0.53025(5) 0.57728(7) 0.0255(3) Uani 1 1 d . . . P1 P 0.14062(5) 1.23033(2) 0.44975(3) 0.01883(11) 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 0.0143(9) 0.0198(9) 0.0240(9) 0.0000(8) 0.0008(7) -0.0005(7) C2 0.0203(10) 0.0298(11) 0.0219(9) -0.0002(8) 0.0047(8) 0.0005(8) C3 0.0207(10) 0.0331(11) 0.0244(10) 0.0105(9) 0.0001(8) -0.0016(8) C4 0.0197(10) 0.0265(10) 0.0358(11) 0.0040(9) 0.0031(9) 0.0045(8) C5 0.0274(12) 0.0430(13) 0.0277(11) -0.0040(10) 0.0047(9) 0.0120(10) C6 0.0254(11) 0.0352(12) 0.0198(9) 0.0015(8) 0.0035(8) 0.0058(9) C7 0.0191(9) 0.0206(9) 0.0226(9) 0.0011(8) -0.0015(8) 0.0012(8) C8 0.0269(11) 0.0204(10) 0.0315(11) 0.0028(8) -0.0033(9) 0.0019(8) C9 0.0350(12) 0.0261(11) 0.0338(11) -0.0068(9) -0.0095(10) 0.0010(9) C10 0.0447(14) 0.0414(14) 0.0245(11) 0.0018(10) -0.0102(10) -0.0017(11) C11 0.0534(16) 0.0335(12) 0.0306(12) 0.0097(10) -0.0101(11) -0.0074(11) C12 0.0374(12) 0.0231(10) 0.0287(11) 0.0044(9) -0.0070(9) -0.0049(9) C13 0.0201(10) 0.0169(9) 0.0208(9) 0.0029(7) -0.0020(7) -0.0018(7) C14 0.0248(11) 0.0234(10) 0.0234(10) 0.0017(8) 0.0029(8) 0.0006(8) C15 0.0231(10) 0.0267(11) 0.0303(10) 0.0072(9) 0.0014(9) -0.0040(8) C16 0.0295(11) 0.0213(10) 0.0341(11) 0.0036(9) -0.0033(9) -0.0027(8) C17 0.0328(12) 0.0217(10) 0.0263(10) -0.0003(8) -0.0007(9) 0.0021(9) C18 0.0238(10) 0.0238(10) 0.0229(9) 0.0009(8) 0.0031(8) -0.0001(8) C19 0.0178(9) 0.0244(10) 0.0226(9) -0.0015(8) 0.0018(7) 0.0040(8) C20 0.0240(11) 0.0252(10) 0.0316(11) 0.0031(9) 0.0039(9) 0.0009(8) C21 0.0281(12) 0.0306(12) 0.0357(12) 0.0068(9) 0.0021(9) 0.0111(9) C22 0.0208(11) 0.0450(14) 0.0446(13) 0.0049(11) 0.0042(10) 0.0104(10) C23 0.0234(12) 0.0417(13) 0.0575(16) 0.0125(12) 0.0090(11) -0.0008(10) C24 0.0243(11) 0.0260(11) 0.0475(13) 0.0102(10) 0.0064(10) 0.0031(9) C25 0.0343(12) 0.0171(9) 0.0191(9) 0.0008(7) 0.0076(8) 0.0012(8) C26 0.0397(13) 0.0213(10) 0.0275(11) 0.0007(8) 0.0059(9) 0.0035(9) C27 0.0598(16) 0.0195(10) 0.0305(11) 0.0035(9) 0.0111(11) 0.0068(10) C28 0.0743(19) 0.0144(10) 0.0341(12) 0.0005(9) 0.0224(12) -0.0039(11) C29 0.0528(16) 0.0324(12) 0.0340(12) -0.0047(10) 0.0172(11) -0.0200(11) C30 0.0359(12) 0.0258(11) 0.0277(11) 0.0012(9) 0.0070(9) -0.0047(9) C31 0.0224(10) 0.0215(10) 0.0230(9) 0.0014(8) 0.0045(8) 0.0019(8) C32 0.0179(9) 0.0206(10) 0.0208(9) 0.0005(7) 0.0044(7) 0.0014(7) C33 0.0171(9) 0.0194(9) 0.0141(8) 0.0013(7) 0.0032(7) 0.0006(7) C34 0.0222(10) 0.0186(9) 0.0175(9) -0.0001(7) 0.0037(7) 0.0013(7) C35 0.0163(10) 0.0296(11) 0.0211(9) 0.0000(8) 0.0026(8) -0.0022(8) C36 0.0182(10) 0.0326(11) 0.0228(10) 0.0035(8) 0.0055(8) 0.0086(8) C37 0.0293(11) 0.0181(9) 0.0243(10) 0.0020(8) 0.0061(8) 0.0069(8) C38 0.0205(10) 0.0193(9) 0.0208(9) 0.0020(7) 0.0040(7) -0.0013(8) C39 0.0166(9) 0.0145(9) 0.0232(9) -0.0025(7) 0.0002(7) 0.0020(7) C40 0.0247(10) 0.0227(10) 0.0160(9) -0.0024(7) -0.0007(8) 0.0056(8) C41 0.0254(10) 0.0260(10) 0.0180(9) 0.0056(8) 0.0071(8) 0.0025(8) C42 0.0209(10) 0.0209(10) 0.0270(10) 0.0005(8) 0.0065(8) -0.0066(8) C43 0.0194(9) 0.0199(9) 0.0170(9) -0.0033(7) 0.0003(7) -0.0011(7) C44 0.0154(9) 0.0154(9) 0.0190(9) -0.0006(7) 0.0032(7) 0.0033(7) C45 0.0198(10) 0.0148(8) 0.0190(9) 0.0030(7) 0.0038(7) -0.0014(7) C46 0.0229(10) 0.0264(10) 0.0185(9) 0.0022(8) 0.0061(8) 0.0033(8) C47 0.0179(10) 0.0346(11) 0.0283(10) 0.0057(9) 0.0007(8) 0.0030(8) C48 0.0286(11) 0.0322(11) 0.0201(10) 0.0021(8) -0.0065(8) -0.0021(9) C49 0.0336(12) 0.0241(10) 0.0155(9) -0.0008(8) 0.0049(8) 0.0014(9) C50 0.0191(10) 0.0165(9) 0.0225(9) 0.0009(7) 0.0044(7) 0.0008(7) N1 0.0191(8) 0.0238(8) 0.0259(8) 0.0077(7) 0.0024(7) 0.0021(7) B1 0.0155(10) 0.0153(10) 0.0198(10) 0.0001(8) 0.0037(8) -0.0001(8) F1 0.0234(6) 0.0181(6) 0.0471(7) -0.0045(5) 0.0054(5) -0.0039(5) F2 0.0169(6) 0.0399(7) 0.0493(8) -0.0035(6) 0.0031(5) -0.0060(5) F3 0.0223(7) 0.0432(8) 0.0545(8) 0.0036(6) 0.0079(6) 0.0145(6) F4 0.0389(8) 0.0195(6) 0.0527(8) 0.0009(6) 0.0113(6) 0.0111(5) F5 0.0261(6) 0.0154(5) 0.0429(7) -0.0027(5) 0.0073(5) -0.0033(5) F6 0.0268(6) 0.0199(6) 0.0272(6) -0.0049(5) -0.0023(5) -0.0071(5) F7 0.0398(7) 0.0334(7) 0.0167(5) -0.0061(5) -0.0032(5) 0.0021(5) F8 0.0472(8) 0.0429(8) 0.0207(6) 0.0082(5) 0.0117(5) -0.0053(6) F9 0.0392(8) 0.0380(7) 0.0333(7) 0.0020(6) 0.0091(6) -0.0222(6) F10 0.0316(7) 0.0277(6) 0.0193(5) -0.0040(5) -0.0002(5) -0.0137(5) F11 0.0224(6) 0.0540(8) 0.0215(6) -0.0038(5) 0.0059(5) 0.0119(6) F12 0.0196(6) 0.0698(10) 0.0337(7) 0.0024(7) -0.0026(5) 0.0107(6) F13 0.0376(8) 0.0585(9) 0.0249(6) -0.0014(6) -0.0122(6) 0.0025(7) F14 0.0469(8) 0.0496(8) 0.0178(6) -0.0079(6) 0.0037(5) 0.0088(6) F15 0.0231(6) 0.0310(6) 0.0237(6) -0.0030(5) 0.0079(5) 0.0049(5) P1 0.0179(2) 0.0181(2) 0.0200(2) 0.00177(19) 0.00077(18) -0.00045(19) _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 1.391(3) . ? C1 C6 1.391(3) . ? C1 P1 1.7960(19) . ? C2 C3 1.389(3) . ? C2 H22 0.9500 . ? C3 C4 1.381(3) . ? C3 H21 0.9500 . ? C4 C5 1.383(3) . ? C4 H1 0.9500 . ? C5 C6 1.380(3) . ? C5 H2 0.9500 . ? C6 H3 0.9500 . ? C7 C12 1.392(3) . ? C7 C8 1.400(3) . ? C7 P1 1.7843(19) . ? C8 C9 1.380(3) . ? C8 H16 0.9500 . ? C9 C10 1.376(3) . ? C9 H17 0.9500 . ? C10 C11 1.380(3) . ? C10 H18 0.9500 . ? C11 C12 1.382(3) . ? C11 H19 0.9500 . ? C12 H20 0.9500 . ? C13 C14 1.399(3) . ? C13 C18 1.393(3) . ? C13 P1 1.7908(19) . ? C14 C15 1.378(3) . ? C14 H14 0.9500 . ? C15 C16 1.391(3) . ? C15 H13 0.9500 . ? C16 C17 1.381(3) . ? C16 H12 0.9500 . ? C17 C18 1.389(3) . ? C17 H11 0.9500 . ? C18 H10 0.9500 . ? C19 C24 1.383(3) . ? C19 C20 1.387(3) . ? C19 N1 1.433(2) . ? C20 C21 1.386(3) . ? C20 H23 0.9500 . ? C21 C22 1.372(3) . ? C21 H24 0.9500 . ? C22 C23 1.379(3) . ? C22 H8 0.9500 . ? C23 C24 1.381(3) . ? C23 H7 0.9500 . ? C24 H1A 0.9500 . ? C25 C30 1.395(3) . ? C25 C26 1.398(3) . ? C25 C31 1.445(3) . ? C26 C27 1.389(3) . ? C26 H40 0.9500 . ? C27 C28 1.373(4) . ? C27 H41 0.9500 . ? C28 C29 1.382(4) . ? C28 H35 0.9500 . ? C29 C30 1.394(3) . ? C29 H34 0.9500 . ? C30 H33 0.9500 . ? C31 C32 1.201(3) . ? C32 B1 1.593(3) . ? C33 C34 1.387(3) . ? C33 C38 1.393(3) . ? C33 B1 1.653(3) . ? C34 F1 1.354(2) . ? C34 C35 1.380(3) . ? C35 F2 1.348(2) . ? C35 C36 1.371(3) . ? C36 F3 1.344(2) . ? C36 C37 1.371(3) . ? C37 F4 1.348(2) . ? C37 C38 1.381(3) . ? C38 F5 1.356(2) . ? C39 F6 1.360(2) . ? C39 C40 1.377(3) . ? C39 C44 1.385(2) . ? C40 F7 1.349(2) . ? C40 C41 1.372(3) . ? C41 F8 1.344(2) . ? C41 C42 1.374(3) . ? C42 F9 1.344(2) . ? C42 C43 1.383(3) . ? C43 F10 1.354(2) . ? C43 C44 1.387(3) . ? C44 B1 1.662(3) . ? C45 C50 1.386(3) . ? C45 C46 1.391(3) . ? C45 B1 1.656(3) . ? C46 F11 1.351(2) . ? C46 C47 1.377(3) . ? C47 F12 1.346(2) . ? C47 C48 1.377(3) . ? C48 F13 1.343(2) . ? C48 C49 1.370(3) . ? C49 F14 1.344(2) . ? C49 C50 1.388(3) . ? C50 F15 1.354(2) . ? N1 P1 1.6358(17) . ? N1 H5 0.8800 . ? 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 C2 C1 C6 119.90(18) . . ? C2 C1 P1 119.90(15) . . ? C6 C1 P1 120.18(15) . . ? C3 C2 C1 119.50(18) . . ? C3 C2 H22 120.3 . . ? C1 C2 H22 120.3 . . ? C4 C3 C2 120.27(18) . . ? C4 C3 H21 119.9 . . ? C2 C3 H21 119.9 . . ? C3 C4 C5 120.17(19) . . ? C3 C4 H1 119.9 . . ? C5 C4 H1 119.9 . . ? C6 C5 C4 120.07(19) . . ? C6 C5 H2 120.0 . . ? C4 C5 H2 120.0 . . ? C5 C6 C1 120.07(18) . . ? C5 C6 H3 120.0 . . ? C1 C6 H3 120.0 . . ? C12 C7 C8 119.80(18) . . ? C12 C7 P1 122.23(15) . . ? C8 C7 P1 117.94(15) . . ? C9 C8 C7 119.76(19) . . ? C9 C8 H16 120.1 . . ? C7 C8 H16 120.1 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H17 119.9 . . ? C8 C9 H17 119.9 . . ? C9 C10 C11 120.5(2) . . ? C9 C10 H18 119.8 . . ? C11 C10 H18 119.8 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H19 119.8 . . ? C10 C11 H19 119.8 . . ? C11 C12 C7 119.5(2) . . ? C11 C12 H20 120.3 . . ? C7 C12 H20 120.3 . . ? C14 C13 C18 120.22(18) . . ? C14 C13 P1 118.45(15) . . ? C18 C13 P1 121.26(15) . . ? C15 C14 C13 119.76(19) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.14(19) . . ? C14 C15 H13 119.9 . . ? C16 C15 H13 119.9 . . ? C17 C16 C15 120.10(19) . . ? C17 C16 H12 119.9 . . ? C15 C16 H12 119.9 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H11 119.8 . . ? C18 C17 H11 119.8 . . ? C17 C18 C13 119.29(19) . . ? C17 C18 H10 120.4 . . ? C13 C18 H10 120.4 . . ? C24 C19 C20 120.23(18) . . ? C24 C19 N1 118.50(17) . . ? C20 C19 N1 121.26(18) . . ? C21 C20 C19 119.4(2) . . ? C21 C20 H23 120.3 . . ? C19 C20 H23 120.3 . . ? C22 C21 C20 120.5(2) . . ? C22 C21 H24 119.7 . . ? C20 C21 H24 119.7 . . ? C21 C22 C23 119.8(2) . . ? C21 C22 H8 120.1 . . ? C23 C22 H8 120.1 . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H7 119.7 . . ? C22 C23 H7 119.7 . . ? C23 C24 C19 119.5(2) . . ? C23 C24 H1A 120.2 . . ? C19 C24 H1A 120.2 . . ? C30 C25 C26 119.17(19) . . ? C30 C25 C31 119.71(19) . . ? C26 C25 C31 121.11(19) . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H40 120.0 . . ? C25 C26 H40 120.0 . . ? C28 C27 C26 120.4(2) . . ? C28 C27 H41 119.8 . . ? C26 C27 H41 119.8 . . ? C27 C28 C29 120.3(2) . . ? C27 C28 H35 119.9 . . ? C29 C28 H35 119.9 . . ? C28 C29 C30 120.1(2) . . ? C28 C29 H34 119.9 . . ? C30 C29 H34 119.9 . . ? C29 C30 C25 119.9(2) . . ? C29 C30 H33 120.0 . . ? C25 C30 H33 120.0 . . ? C32 C31 C25 174.0(2) . . ? C31 C32 B1 174.0(2) . . ? C34 C33 C38 112.85(17) . . ? C34 C33 B1 127.12(16) . . ? C38 C33 B1 119.90(16) . . ? F1 C34 C35 114.03(17) . . ? F1 C34 C33 121.71(17) . . ? C35 C34 C33 124.25(18) . . ? F2 C35 C36 119.69(17) . . ? F2 C35 C34 120.23(18) . . ? C36 C35 C34 120.07(18) . . ? F3 C36 C37 120.93(19) . . ? F3 C36 C35 120.38(19) . . ? C37 C36 C35 118.68(18) . . ? F4 C37 C36 119.91(18) . . ? F4 C37 C38 120.61(18) . . ? C36 C37 C38 119.47(18) . . ? F5 C38 C37 116.36(17) . . ? F5 C38 C33 118.97(16) . . ? C37 C38 C33 124.67(18) . . ? F6 C39 C40 115.31(16) . . ? F6 C39 C44 119.39(16) . . ? C40 C39 C44 125.29(17) . . ? F7 C40 C41 120.17(17) . . ? F7 C40 C39 120.82(17) . . ? C41 C40 C39 119.01(17) . . ? F8 C41 C40 121.05(17) . . ? F8 C41 C42 120.15(18) . . ? C40 C41 C42 118.79(17) . . ? F9 C42 C41 119.26(17) . . ? F9 C42 C43 120.76(17) . . ? C41 C42 C43 119.98(17) . . ? F10 C43 C42 114.84(16) . . ? F10 C43 C44 121.24(16) . . ? C42 C43 C44 123.92(17) . . ? C39 C44 C43 112.94(16) . . ? C39 C44 B1 120.25(16) . . ? C43 C44 B1 126.77(16) . . ? C50 C45 C46 112.90(16) . . ? C50 C45 B1 127.61(16) . . ? C46 C45 B1 119.31(16) . . ? F11 C46 C47 115.49(17) . . ? F11 C46 C45 119.35(16) . . ? C47 C46 C45 125.16(18) . . ? F12 C47 C46 121.07(18) . . ? F12 C47 C48 119.83(18) . . ? C46 C47 C48 119.10(19) . . ? F13 C48 C49 120.61(19) . . ? F13 C48 C47 120.53(19) . . ? C49 C48 C47 118.85(18) . . ? F14 C49 C48 119.93(18) . . ? F14 C49 C50 120.11(18) . . ? C48 C49 C50 119.96(18) . . ? F15 C50 C45 120.80(16) . . ? F15 C50 C49 115.17(16) . . ? C45 C50 C49 124.02(18) . . ? C19 N1 P1 126.29(13) . . ? C19 N1 H5 116.9 . . ? P1 N1 H5 116.9 . . ? C32 B1 C33 111.09(15) . . ? C32 B1 C45 104.17(15) . . ? C33 B1 C45 114.71(15) . . ? C32 B1 C44 110.33(15) . . ? C33 B1 C44 105.04(14) . . ? C45 B1 C44 111.60(15) . . ? N1 P1 C7 110.57(9) . . ? N1 P1 C13 112.71(9) . . ? C7 P1 C13 109.55(9) . . ? N1 P1 C1 105.51(9) . . ? C7 P1 C1 109.97(9) . . ? C13 P1 C1 108.43(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.418 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.052 data_cj026_0m _database_code_depnum_ccdc_archive 'CCDC 873946' #TrackingRef 'cj026_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.25 H27 B F20 N P' _chemical_formula_weight 1126.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.6597(5) _cell_length_b 19.1776(4) _cell_length_c 24.7362(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.8180(10) _cell_angle_gamma 90.00 _cell_volume 9926.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4524 _exptl_absorpt_coefficient_mu 0.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9586 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83412 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 22636 _reflns_number_gt 13976 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+2.6114P] 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 22636 _refine_ls_number_parameters 1402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 P1 P 0.21363(4) 0.31021(4) 0.51568(3) 0.01949(17) Uani 1 1 d . . . P2 P 0.26042(4) 0.66490(4) 0.11802(3) 0.02119(17) Uani 1 1 d . . . N1 N 0.18735(12) 0.37807(12) 0.46818(11) 0.0199(5) Uani 1 1 d . . . N2 N 0.28151(12) 0.70749(12) 0.07136(11) 0.0216(5) Uani 1 1 d . . . B1 B 0.31172(17) 0.38545(17) 0.39974(15) 0.0219(7) Uani 1 1 d . . . B2 B 0.14391(17) 0.65299(17) -0.09623(15) 0.0221(7) Uani 1 1 d . . . F1 F 0.33796(9) 0.49603(9) 0.49939(8) 0.0336(4) Uani 1 1 d . . . F2 F 0.42049(10) 0.59937(10) 0.52848(9) 0.0433(5) Uani 1 1 d . . . F3 F 0.49190(10) 0.61708(11) 0.47016(12) 0.0536(6) Uani 1 1 d . . . F4 F 0.48286(11) 0.52361(11) 0.38367(11) 0.0521(6) Uani 1 1 d . . . F5 F 0.39637(11) 0.42099(10) 0.34939(10) 0.0437(5) Uani 1 1 d . . . F6 F 0.39940(8) 0.33214(10) 0.52138(8) 0.0309(4) Uani 1 1 d . . . F7 F 0.47754(10) 0.22505(12) 0.55090(10) 0.0495(6) Uani 1 1 d . . . F8 F 0.48404(11) 0.14516(12) 0.46221(12) 0.0604(7) Uani 1 1 d . . . F9 F 0.41123(11) 0.17997(11) 0.34282(10) 0.0523(6) Uani 1 1 d . . . F10 F 0.33463(10) 0.28865(10) 0.31130(9) 0.0396(5) Uani 1 1 d . . . F11 F 0.27427(10) 0.50837(10) 0.30839(9) 0.0408(5) Uani 1 1 d . . . F12 F 0.17592(13) 0.50867(12) 0.19807(10) 0.0579(7) Uani 1 1 d . . . F13 F 0.10304(12) 0.39260(14) 0.15137(9) 0.0630(7) Uani 1 1 d . . . F14 F 0.13017(11) 0.27505(11) 0.22121(9) 0.0489(6) Uani 1 1 d . . . F15 F 0.22797(9) 0.27382(9) 0.33362(8) 0.0331(4) Uani 1 1 d . . . F16 F 0.22033(9) 0.50430(9) 0.53099(9) 0.0359(5) Uani 1 1 d . . . F17 F 0.13180(11) 0.59466(10) 0.52954(10) 0.0478(6) Uani 1 1 d . . . F18 F 0.00627(11) 0.56284(11) 0.46623(11) 0.0539(6) Uani 1 1 d . . . F19 F -0.03108(10) 0.43845(13) 0.40665(11) 0.0541(6) Uani 1 1 d . . . F20 F 0.05680(9) 0.34822(10) 0.40839(9) 0.0361(5) Uani 1 1 d . . . F21 F 0.23229(9) 0.53682(9) -0.05693(9) 0.0336(4) Uani 1 1 d . . . F22 F 0.32275(10) 0.50759(11) -0.08918(11) 0.0506(6) Uani 1 1 d . . . F23 F 0.33513(11) 0.58723(13) -0.17433(12) 0.0583(7) Uani 1 1 d . . . F24 F 0.25403(11) 0.69642(13) -0.22657(10) 0.0536(6) Uani 1 1 d . . . F25 F 0.16579(10) 0.72774(10) -0.19472(8) 0.0379(5) Uani 1 1 d . . . F26 F 0.11889(9) 0.50558(9) -0.15863(8) 0.0325(4) Uani 1 1 d . . . F27 F 0.04268(10) 0.40895(9) -0.15215(9) 0.0381(5) Uani 1 1 d . . . F28 F -0.02791(10) 0.43319(10) -0.09357(9) 0.0401(5) Uani 1 1 d . . . F29 F -0.01754(9) 0.55942(9) -0.03757(8) 0.0308(4) Uani 1 1 d . . . F30 F 0.05991(8) 0.65647(9) -0.04057(8) 0.0272(4) Uani 1 1 d . . . F31 F 0.05350(10) 0.64147(9) -0.22473(8) 0.0368(5) Uani 1 1 d . . . F32 F -0.03657(11) 0.73266(11) -0.29469(8) 0.0466(6) Uani 1 1 d . . . F33 F -0.05202(10) 0.85430(10) -0.24613(9) 0.0420(5) Uani 1 1 d . . . F34 F 0.02773(10) 0.88479(10) -0.12752(9) 0.0387(5) Uani 1 1 d . . . F35 F 0.11813(9) 0.79740(9) -0.05736(8) 0.0331(4) Uani 1 1 d . . . F36 F 0.41209(9) 0.67517(10) 0.12605(9) 0.0391(5) Uani 1 1 d . . . F37 F 0.50342(10) 0.77372(14) 0.17302(11) 0.0601(7) Uani 1 1 d . . . F38 F 0.46978(12) 0.91091(13) 0.16612(12) 0.0691(8) Uani 1 1 d . . . F39 F 0.34570(13) 0.94773(11) 0.11504(12) 0.0627(7) Uani 1 1 d . . . F40 F 0.25390(10) 0.84892(10) 0.06804(10) 0.0415(5) Uani 1 1 d . . . C1 C 0.36173(15) 0.45259(15) 0.42158(14) 0.0258(7) Uani 1 1 d . . . C2 C 0.37121(15) 0.49996(16) 0.46721(14) 0.0266(7) Uani 1 1 d . . . C3 C 0.41411(16) 0.55521(16) 0.48392(15) 0.0314(7) Uani 1 1 d . . . C4 C 0.45058(16) 0.56420(17) 0.45483(17) 0.0346(8) Uani 1 1 d . . . C5 C 0.44493(16) 0.51731(18) 0.41054(17) 0.0356(8) Uani 1 1 d . . . C6 C 0.40147(16) 0.46383(17) 0.39511(16) 0.0307(7) Uani 1 1 d . . . C7 C 0.35916(15) 0.31608(15) 0.41419(14) 0.0252(7) Uani 1 1 d . . . C8 C 0.39895(15) 0.29569(16) 0.47424(14) 0.0249(7) Uani 1 1 d . . . C9 C 0.44022(16) 0.24004(18) 0.49101(15) 0.0339(8) Uani 1 1 d . . . C10 C 0.44442(17) 0.20008(18) 0.44686(18) 0.0396(9) Uani 1 1 d . . . C11 C 0.40749(17) 0.21789(18) 0.38678(17) 0.0366(8) Uani 1 1 d . . . C12 C 0.36711(16) 0.27474(17) 0.37182(15) 0.0306(7) Uani 1 1 d . . . C13 C 0.25816(15) 0.38992(16) 0.32729(14) 0.0251(7) Uani 1 1 d . . . C14 C 0.24175(17) 0.44799(17) 0.28940(14) 0.0310(7) Uani 1 1 d . . . C15 C 0.1905(2) 0.44952(19) 0.23120(16) 0.0402(9) Uani 1 1 d . . . C16 C 0.15337(19) 0.3913(2) 0.20766(15) 0.0409(9) Uani 1 1 d . . . C17 C 0.16761(17) 0.33196(19) 0.24305(15) 0.0359(8) Uani 1 1 d . . . C18 C 0.21810(16) 0.33331(16) 0.30084(14) 0.0282(7) Uani 1 1 d . . . C19 C 0.21579(14) 0.39962(14) 0.42844(13) 0.0198(6) Uani 1 1 d . . . C20 C 0.27305(15) 0.37713(15) 0.43927(13) 0.0205(6) Uani 1 1 d . . . H1 H 0.2954(13) 0.3488(14) 0.4763(13) 0.011(7) Uiso 1 1 d . . . C21 C 0.17232(14) 0.44760(15) 0.37866(13) 0.0218(6) Uani 1 1 d . . . C22 C 0.18927(16) 0.51730(15) 0.37985(14) 0.0270(7) Uani 1 1 d . . . H22 H 0.2274 0.5335 0.4115 0.032 Uiso 1 1 calc R . . C23 C 0.14967(16) 0.56294(17) 0.33419(15) 0.0321(7) Uani 1 1 d . . . H23 H 0.1613 0.6095 0.3354 0.038 Uiso 1 1 calc R . . C24 C 0.09325(17) 0.53926(18) 0.28720(15) 0.0353(8) Uani 1 1 d . . . H24 H 0.0668 0.5697 0.2565 0.042 Uiso 1 1 calc R . . C25 C 0.07598(17) 0.47041(18) 0.28575(15) 0.0341(8) Uani 1 1 d . . . H25 H 0.0377 0.4545 0.2541 0.041 Uiso 1 1 calc R . . C26 C 0.11533(15) 0.42450(17) 0.33126(14) 0.0280(7) Uani 1 1 d . . . H26 H 0.1033 0.3781 0.3298 0.034 Uiso 1 1 calc R . . C27 C 0.14087(14) 0.42393(15) 0.47055(13) 0.0207(6) Uani 1 1 d . . . C28 C 0.15840(15) 0.48688(16) 0.50089(14) 0.0258(7) Uani 1 1 d . . . C29 C 0.11366(18) 0.53358(16) 0.49968(16) 0.0330(8) Uani 1 1 d . . . C30 C 0.05036(18) 0.51747(18) 0.46760(17) 0.0360(8) Uani 1 1 d . . . C31 C 0.03126(16) 0.45483(19) 0.43749(16) 0.0353(8) Uani 1 1 d . . . C32 C 0.07659(15) 0.40866(17) 0.43923(14) 0.0274(7) Uani 1 1 d . . . C33 C 0.28540(15) 0.32542(16) 0.58557(13) 0.0239(6) Uani 1 1 d . . . C34 C 0.30174(17) 0.27744(18) 0.63311(14) 0.0333(8) Uani 1 1 d . . . H34 H 0.2754 0.2393 0.6280 0.040 Uiso 1 1 calc R . . C35 C 0.35695(18) 0.2864(2) 0.68782(16) 0.0420(9) Uani 1 1 d . . . H35 H 0.3673 0.2547 0.7195 0.050 Uiso 1 1 calc R . . C36 C 0.39661(17) 0.3425(2) 0.69528(16) 0.0403(9) Uani 1 1 d . . . H36 H 0.4341 0.3479 0.7318 0.048 Uiso 1 1 calc R . . C37 C 0.38089(16) 0.39040(18) 0.64890(15) 0.0346(8) Uani 1 1 d . . . H37 H 0.4077 0.4282 0.6544 0.042 Uiso 1 1 calc R . . C38 C 0.32515(15) 0.38262(16) 0.59395(14) 0.0268(7) Uani 1 1 d . . . H38 H 0.3144 0.4154 0.5630 0.032 Uiso 1 1 calc R . . C39 C 0.22496(14) 0.23893(14) 0.47520(13) 0.0209(6) Uani 1 1 d . . . C40 C 0.17414(15) 0.21909(15) 0.41919(14) 0.0256(7) Uani 1 1 d . . . H40 H 0.1356 0.2433 0.4033 0.031 Uiso 1 1 calc R . . C41 C 0.18139(17) 0.16343(16) 0.38758(15) 0.0309(7) Uani 1 1 d . . . H41 H 0.1473 0.1492 0.3510 0.037 Uiso 1 1 calc R . . C42 C 0.23897(18) 0.12900(17) 0.41006(16) 0.0348(8) Uani 1 1 d . . . H42 H 0.2436 0.0917 0.3884 0.042 Uiso 1 1 calc R . . C43 C 0.28995(18) 0.14938(16) 0.46457(16) 0.0337(8) Uani 1 1 d . . . H43 H 0.3289 0.1262 0.4790 0.040 Uiso 1 1 calc R . . C44 C 0.28345(16) 0.20416(15) 0.49782(15) 0.0267(7) Uani 1 1 d . . . H44 H 0.3176 0.2176 0.5347 0.032 Uiso 1 1 calc R . . C45 C 0.15370(14) 0.29059(15) 0.53848(13) 0.0225(6) Uani 1 1 d . . . C46 C 0.15019(16) 0.33290(17) 0.58296(14) 0.0281(7) Uani 1 1 d . . . H46 H 0.1791 0.3692 0.6006 0.034 Uiso 1 1 calc R . . C47 C 0.10324(17) 0.32050(18) 0.60067(16) 0.0351(8) Uani 1 1 d . . . H47 H 0.1009 0.3484 0.6303 0.042 Uiso 1 1 calc R . . C48 C 0.05995(17) 0.2665(2) 0.57399(17) 0.0391(9) Uani 1 1 d . . . H48 H 0.0281 0.2588 0.5853 0.047 Uiso 1 1 calc R . . C49 C 0.06391(17) 0.22397(18) 0.53045(17) 0.0364(8) Uani 1 1 d . . . H49 H 0.0351 0.1875 0.5132 0.044 Uiso 1 1 calc R . . C50 C 0.11074(16) 0.23573(17) 0.51254(15) 0.0302(7) Uani 1 1 d . . . H50 H 0.1134 0.2072 0.4834 0.036 Uiso 1 1 calc R . . C51 C 0.19186(15) 0.63257(16) -0.12524(13) 0.0240(6) Uani 1 1 d . . . C52 C 0.23452(15) 0.57727(16) -0.10102(14) 0.0269(7) Uani 1 1 d . . . C53 C 0.28173(16) 0.56097(17) -0.11639(17) 0.0342(8) Uani 1 1 d . . . C54 C 0.28822(18) 0.60096(19) -0.15963(17) 0.0378(9) Uani 1 1 d . . . C55 C 0.24799(18) 0.65540(19) -0.18502(16) 0.0369(8) Uani 1 1 d . . . C56 C 0.20152(16) 0.67026(17) -0.16795(14) 0.0292(7) Uani 1 1 d . . . C57 C 0.09755(14) 0.58640(15) -0.09660(13) 0.0227(6) Uani 1 1 d . . . C58 C 0.08858(15) 0.52155(16) -0.12550(13) 0.0255(7) Uani 1 1 d . . . C59 C 0.04834(16) 0.47051(16) -0.12367(14) 0.0283(7) Uani 1 1 d . . . C60 C 0.01240(15) 0.48206(16) -0.09405(14) 0.0277(7) Uani 1 1 d . . . C61 C 0.01840(15) 0.54522(16) -0.06557(13) 0.0243(6) Uani 1 1 d . . . C62 C 0.05957(15) 0.59474(15) -0.06775(13) 0.0230(6) Uani 1 1 d . . . C63 C 0.09136(14) 0.71342(15) -0.13685(13) 0.0221(6) Uani 1 1 d . . . C64 C 0.04858(16) 0.70146(16) -0.19835(14) 0.0268(7) Uani 1 1 d . . . C65 C 0.00188(16) 0.74720(17) -0.23524(14) 0.0317(8) Uani 1 1 d . . . C66 C -0.00591(16) 0.80934(17) -0.21144(14) 0.0292(7) Uani 1 1 d . . . C67 C 0.03457(16) 0.82404(16) -0.15158(14) 0.0266(7) Uani 1 1 d . . . C68 C 0.08136(15) 0.77694(16) -0.11585(13) 0.0238(6) Uani 1 1 d . . . C69 C 0.18818(14) 0.67416(15) -0.02449(13) 0.0209(6) Uani 1 1 d . . . H2 H 0.1701(16) 0.6636(16) 0.0025(15) 0.029(9) Uiso 1 1 d . . . C70 C 0.24618(14) 0.70169(15) 0.00365(12) 0.0202(6) Uani 1 1 d . . . C71 C 0.28366(14) 0.73046(16) -0.02577(13) 0.0237(6) Uani 1 1 d . . . C72 C 0.33885(15) 0.69748(17) -0.01993(14) 0.0289(7) Uani 1 1 d . . . H72 H 0.3536 0.6574 0.0037 0.035 Uiso 1 1 calc R . . C73 C 0.37181(16) 0.72427(19) -0.04930(16) 0.0356(8) Uani 1 1 d . . . H73 H 0.4082 0.7018 -0.0457 0.043 Uiso 1 1 calc R . . C74 C 0.35061(18) 0.78429(19) -0.08390(16) 0.0382(9) Uani 1 1 d . . . H74 H 0.3729 0.8021 -0.1033 0.046 Uiso 1 1 calc R . . C75 C 0.29659(18) 0.81785(18) -0.08976(16) 0.0366(8) Uani 1 1 d . . . H75 H 0.2823 0.8581 -0.1132 0.044 Uiso 1 1 calc R . . C76 C 0.26345(16) 0.79108(16) -0.06025(14) 0.0282(7) Uani 1 1 d . . . H76 H 0.2273 0.8142 -0.0637 0.034 Uiso 1 1 calc R . . C77 C 0.33020(15) 0.75981(15) 0.09659(13) 0.0237(6) Uani 1 1 d . . . C78 C 0.39462(16) 0.74231(17) 0.12300(14) 0.0297(7) Uani 1 1 d . . . C79 C 0.44164(17) 0.7923(2) 0.14720(16) 0.0391(9) Uani 1 1 d . . . C80 C 0.42459(19) 0.8614(2) 0.14444(17) 0.0436(9) Uani 1 1 d . . . C81 C 0.3618(2) 0.87987(18) 0.11782(17) 0.0400(9) Uani 1 1 d . . . C82 C 0.31510(16) 0.82940(16) 0.09394(14) 0.0287(7) Uani 1 1 d . . . C83 C 0.32715(16) 0.67254(18) 0.19332(14) 0.0293(7) Uani 1 1 d . . . C84 C 0.37066(19) 0.6182(2) 0.21941(16) 0.0462(10) Uani 1 1 d . . . H84 H 0.3640 0.5753 0.1998 0.055 Uiso 1 1 calc R . . C85 C 0.4244(2) 0.6295(3) 0.2754(2) 0.0686(14) Uani 1 1 d . . . H85 H 0.4546 0.5943 0.2924 0.082 Uiso 1 1 calc R . . C86 C 0.4336(2) 0.6919(3) 0.30610(18) 0.0689(15) Uani 1 1 d . . . H86 H 0.4695 0.6984 0.3437 0.083 Uiso 1 1 calc R . . C87 C 0.3897(2) 0.7440(3) 0.28095(17) 0.0552(12) Uani 1 1 d . . . H87 H 0.3957 0.7860 0.3019 0.066 Uiso 1 1 calc R . . C88 C 0.33579(17) 0.7354(2) 0.22425(15) 0.0371(8) Uani 1 1 d . . . H88 H 0.3061 0.7712 0.2074 0.045 Uiso 1 1 calc R . . C89 C 0.19285(15) 0.70023(15) 0.12336(13) 0.0227(6) Uani 1 1 d . . . C90 C 0.15213(15) 0.74921(16) 0.08252(14) 0.0264(7) Uani 1 1 d . . . H90 H 0.1597 0.7664 0.0514 0.032 Uiso 1 1 calc R . . C91 C 0.09977(17) 0.77230(18) 0.08874(17) 0.0351(8) Uani 1 1 d . . . H91 H 0.0722 0.8052 0.0616 0.042 Uiso 1 1 calc R . . C92 C 0.08836(18) 0.74677(18) 0.13487(17) 0.0388(9) Uani 1 1 d . . . H92 H 0.0530 0.7623 0.1384 0.047 Uiso 1 1 calc R . . C93 C 0.12918(18) 0.69834(18) 0.17582(16) 0.0360(8) Uani 1 1 d . . . H93 H 0.1213 0.6815 0.2069 0.043 Uiso 1 1 calc R . . C94 C 0.18183(16) 0.67483(17) 0.17066(15) 0.0290(7) Uani 1 1 d . . . H94 H 0.2096 0.6425 0.1984 0.035 Uiso 1 1 calc R . . C95 C 0.24526(15) 0.57599(15) 0.09364(13) 0.0247(7) Uani 1 1 d . . . C96 C 0.18892(17) 0.54298(17) 0.08420(15) 0.0305(7) Uani 1 1 d . . . H96 H 0.1581 0.5674 0.0899 0.037 Uiso 1 1 calc R . . C97 C 0.17893(19) 0.47348(18) 0.06622(17) 0.0400(9) Uani 1 1 d . . . H97 H 0.1414 0.4511 0.0598 0.048 Uiso 1 1 calc R . . C98 C 0.2247(2) 0.43806(18) 0.05799(18) 0.0449(10) Uani 1 1 d . . . H98 H 0.2179 0.3915 0.0461 0.054 Uiso 1 1 calc R . . C99 C 0.2809(2) 0.47039(18) 0.06707(18) 0.0428(9) Uani 1 1 d . . . H99 H 0.3116 0.4456 0.0615 0.051 Uiso 1 1 calc R . . C100 C 0.29107(18) 0.53960(17) 0.08440(16) 0.0337(8) Uani 1 1 d . . . H100 H 0.3283 0.5619 0.0899 0.040 Uiso 1 1 calc R . . C101 C 0.2530(3) 0.4678(4) 0.7031(2) 0.0773(16) Uani 1 1 d . . . H101 H 0.2879 0.4502 0.6999 0.093 Uiso 1 1 calc R . . C102 C 0.2289(3) 0.5314(4) 0.6777(3) 0.0952(19) Uani 1 1 d . . . H102 H 0.2468 0.5561 0.6571 0.114 Uiso 1 1 calc R . . C103 C 0.1769(4) 0.5588(3) 0.6830(3) 0.096(2) Uani 1 1 d . . . H103 H 0.1588 0.6015 0.6658 0.115 Uiso 1 1 calc R . . C104 C 0.1549(3) 0.5208(3) 0.7139(2) 0.092(2) Uani 1 1 d . . . H104 H 0.1217 0.5404 0.7190 0.111 Uiso 1 1 calc R . . C105 C 0.1745(2) 0.4584(3) 0.7383(2) 0.0640(13) Uani 1 1 d . . . H105 H 0.1547 0.4347 0.7578 0.077 Uiso 1 1 calc R . . C106 C 0.2273(3) 0.4290(3) 0.7333(2) 0.0716(15) Uani 1 1 d . . . C107 C 0.2524(4) 0.3642(4) 0.7580(3) 0.107(2) Uani 1 1 d . . . H10A H 0.2287 0.3449 0.7770 0.161 Uiso 1 1 calc R . . H10B H 0.2964 0.3695 0.7880 0.161 Uiso 1 1 calc R . . H10C H 0.2496 0.3336 0.7262 0.161 Uiso 1 1 calc R . . C201 C 0.5155(4) 0.9727(4) 0.3559(4) 0.154(7) Uiso 0.50 1 d PG . . C202 C 0.5308(4) 0.9981(3) 0.3118(4) 0.077(3) Uiso 0.50 1 d PG . . H20A H 0.5219 1.0443 0.2990 0.092 Uiso 0.50 1 calc PR . . C203 C 0.5595(4) 0.9546(4) 0.2867(3) 0.091(4) Uiso 0.50 1 d PG . . H20B H 0.5698 0.9716 0.2572 0.109 Uiso 0.50 1 calc PR . . C204 C 0.5728(4) 0.8856(4) 0.3058(3) 0.081(3) Uiso 0.50 1 d PG . . H20C H 0.5919 0.8565 0.2891 0.097 Uiso 0.50 1 calc PR . . C205 C 0.5574(4) 0.8602(3) 0.3499(4) 0.089(3) Uiso 0.50 1 d PG . . H20D H 0.5663 0.8141 0.3627 0.106 Uiso 0.50 1 calc PR . . C206 C 0.5287(4) 0.9037(4) 0.3750(3) 0.088(3) Uiso 0.50 1 d PG . . H20E H 0.5184 0.8867 0.4045 0.106 Uiso 0.50 1 calc PR . . C207 C 0.4943(10) 1.0036(10) 0.3851(9) 0.172(8) Uiso 0.50 1 d P . . H20F H 0.4856 1.0511 0.3714 0.258 Uiso 0.50 1 calc PR . . H20G H 0.5250 1.0027 0.4277 0.258 Uiso 0.50 1 calc PR . . H20H H 0.4555 0.9816 0.3795 0.258 Uiso 0.50 1 calc PR . . 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 0.0199(4) 0.0191(4) 0.0200(4) 0.0025(3) 0.0097(3) -0.0008(3) P2 0.0242(4) 0.0214(4) 0.0185(4) 0.0008(3) 0.0105(3) 0.0011(3) N1 0.0209(13) 0.0193(12) 0.0222(12) 0.0029(10) 0.0122(11) 0.0012(10) N2 0.0227(14) 0.0220(12) 0.0189(12) -0.0002(10) 0.0088(11) -0.0013(10) B1 0.0267(19) 0.0188(16) 0.0235(17) 0.0017(13) 0.0145(15) -0.0010(14) B2 0.0225(18) 0.0236(17) 0.0211(16) -0.0014(13) 0.0110(15) -0.0004(14) F1 0.0378(11) 0.0346(10) 0.0358(10) -0.0070(8) 0.0232(9) -0.0100(9) F2 0.0430(13) 0.0335(11) 0.0451(12) -0.0106(9) 0.0135(10) -0.0120(9) F3 0.0331(12) 0.0380(12) 0.0853(17) 0.0038(11) 0.0240(12) -0.0155(10) F4 0.0464(14) 0.0475(13) 0.0844(17) 0.0185(12) 0.0491(13) 0.0026(11) F5 0.0599(15) 0.0377(11) 0.0561(13) -0.0015(10) 0.0460(12) -0.0047(10) F6 0.0240(10) 0.0410(11) 0.0277(9) -0.0027(8) 0.0121(8) -0.0015(8) F7 0.0379(13) 0.0552(13) 0.0407(12) 0.0070(10) 0.0060(10) 0.0156(11) F8 0.0507(15) 0.0442(13) 0.0691(16) -0.0041(12) 0.0135(13) 0.0213(11) F9 0.0557(15) 0.0481(13) 0.0556(14) -0.0158(11) 0.0279(12) 0.0121(11) F10 0.0504(13) 0.0431(11) 0.0310(10) -0.0010(9) 0.0237(10) 0.0097(10) F11 0.0530(14) 0.0287(10) 0.0439(12) 0.0089(9) 0.0254(11) -0.0015(9) F12 0.0817(18) 0.0512(14) 0.0378(12) 0.0245(11) 0.0254(12) 0.0191(13) F13 0.0615(16) 0.0786(17) 0.0236(11) 0.0006(11) -0.0014(11) 0.0134(13) F14 0.0459(14) 0.0512(13) 0.0363(11) -0.0139(10) 0.0082(10) -0.0077(11) F15 0.0390(12) 0.0276(9) 0.0306(10) 0.0025(8) 0.0144(9) -0.0054(8) F16 0.0336(11) 0.0282(10) 0.0426(11) -0.0081(8) 0.0152(9) -0.0067(8) F17 0.0751(17) 0.0248(10) 0.0613(14) -0.0019(10) 0.0468(13) 0.0063(10) F18 0.0615(15) 0.0516(13) 0.0760(16) 0.0309(12) 0.0550(14) 0.0331(12) F19 0.0231(11) 0.0765(16) 0.0610(14) 0.0189(13) 0.0182(11) 0.0072(11) F20 0.0274(11) 0.0389(11) 0.0358(11) -0.0016(9) 0.0096(9) -0.0098(9) F21 0.0350(11) 0.0297(10) 0.0393(11) 0.0060(8) 0.0200(9) 0.0049(8) F22 0.0394(13) 0.0374(12) 0.0835(17) -0.0034(11) 0.0358(13) 0.0064(10) F23 0.0519(15) 0.0670(15) 0.0836(18) -0.0155(13) 0.0546(14) -0.0057(12) F24 0.0608(15) 0.0712(15) 0.0492(13) 0.0058(12) 0.0428(12) -0.0087(12) F25 0.0395(12) 0.0461(12) 0.0335(10) 0.0127(9) 0.0216(10) 0.0015(9) F26 0.0363(11) 0.0333(10) 0.0357(10) -0.0112(8) 0.0234(9) -0.0048(8) F27 0.0437(12) 0.0272(10) 0.0452(12) -0.0125(9) 0.0221(10) -0.0082(9) F28 0.0424(12) 0.0351(11) 0.0477(12) -0.0034(9) 0.0250(10) -0.0150(9) F29 0.0324(11) 0.0353(10) 0.0327(10) 0.0024(8) 0.0220(9) -0.0008(8) F30 0.0275(10) 0.0255(9) 0.0330(10) -0.0047(8) 0.0178(8) -0.0015(8) F31 0.0454(12) 0.0301(10) 0.0246(9) -0.0072(8) 0.0077(9) -0.0030(9) F32 0.0501(14) 0.0413(12) 0.0222(10) -0.0016(9) -0.0052(9) -0.0030(10) F33 0.0378(12) 0.0397(11) 0.0341(11) 0.0110(9) 0.0047(9) 0.0101(9) F34 0.0485(13) 0.0333(10) 0.0324(10) -0.0001(8) 0.0173(10) 0.0128(9) F35 0.0383(11) 0.0339(10) 0.0199(9) -0.0039(8) 0.0075(8) 0.0084(9) F36 0.0285(11) 0.0424(12) 0.0399(11) -0.0010(9) 0.0106(9) 0.0084(9) F37 0.0230(12) 0.0875(18) 0.0599(15) -0.0063(13) 0.0111(11) -0.0081(12) F38 0.0572(16) 0.0698(17) 0.0647(16) -0.0109(13) 0.0153(13) -0.0427(14) F39 0.0743(18) 0.0264(11) 0.0723(16) -0.0046(11) 0.0215(14) -0.0130(11) F40 0.0357(12) 0.0265(10) 0.0544(13) 0.0002(9) 0.0146(10) 0.0055(9) C1 0.0257(17) 0.0226(15) 0.0303(16) 0.0072(13) 0.0140(14) 0.0018(13) C2 0.0254(17) 0.0252(16) 0.0311(17) 0.0026(13) 0.0147(14) -0.0009(13) C3 0.0264(18) 0.0232(16) 0.0365(18) 0.0007(14) 0.0078(15) 0.0006(14) C4 0.0228(18) 0.0254(17) 0.053(2) 0.0106(16) 0.0154(17) -0.0015(14) C5 0.0277(19) 0.0329(18) 0.055(2) 0.0179(17) 0.0266(17) 0.0046(15) C6 0.0336(19) 0.0275(16) 0.0391(19) 0.0055(14) 0.0239(16) 0.0028(14) C7 0.0256(17) 0.0232(15) 0.0323(17) 0.0029(13) 0.0181(14) -0.0019(13) C8 0.0244(17) 0.0247(15) 0.0288(16) -0.0003(13) 0.0152(14) -0.0038(13) C9 0.0233(18) 0.0379(19) 0.0332(18) 0.0049(15) 0.0070(15) 0.0005(15) C10 0.031(2) 0.0283(18) 0.054(2) -0.0014(17) 0.0152(18) 0.0072(15) C11 0.035(2) 0.0330(18) 0.043(2) -0.0105(16) 0.0190(17) 0.0019(15) C12 0.0330(19) 0.0300(17) 0.0289(17) 0.0011(14) 0.0146(15) -0.0008(14) C13 0.0300(18) 0.0272(16) 0.0238(15) 0.0019(13) 0.0175(14) 0.0023(13) C14 0.040(2) 0.0325(18) 0.0274(17) 0.0027(14) 0.0212(16) 0.0027(15) C15 0.058(3) 0.040(2) 0.0275(18) 0.0126(16) 0.0237(18) 0.0149(18) C16 0.042(2) 0.055(2) 0.0198(16) 0.0020(16) 0.0099(16) 0.0124(19) C17 0.037(2) 0.0405(19) 0.0273(17) -0.0085(15) 0.0125(16) -0.0021(16) C18 0.0355(19) 0.0277(16) 0.0248(16) 0.0044(13) 0.0168(15) 0.0036(14) C19 0.0251(17) 0.0155(13) 0.0200(14) 0.0008(11) 0.0116(13) -0.0034(12) C20 0.0240(17) 0.0170(14) 0.0199(14) -0.0008(12) 0.0098(13) -0.0032(12) C21 0.0237(16) 0.0251(15) 0.0209(14) 0.0015(12) 0.0139(13) 0.0012(12) C22 0.0300(18) 0.0231(15) 0.0260(16) 0.0008(13) 0.0115(14) -0.0002(13) C23 0.036(2) 0.0251(16) 0.0332(18) 0.0051(14) 0.0150(16) 0.0032(14) C24 0.038(2) 0.0337(18) 0.0290(17) 0.0105(15) 0.0116(16) 0.0125(16) C25 0.0273(19) 0.041(2) 0.0266(17) 0.0034(15) 0.0066(15) 0.0012(15) C26 0.0274(18) 0.0287(16) 0.0253(16) -0.0003(13) 0.0099(14) -0.0030(14) C27 0.0203(16) 0.0222(15) 0.0213(14) 0.0068(12) 0.0111(13) 0.0037(12) C28 0.0289(18) 0.0235(15) 0.0278(16) 0.0049(13) 0.0155(14) 0.0007(13) C29 0.051(2) 0.0212(16) 0.0396(19) 0.0063(14) 0.0321(18) 0.0071(15) C30 0.043(2) 0.0355(19) 0.047(2) 0.0186(16) 0.0352(19) 0.0200(17) C31 0.0218(18) 0.048(2) 0.0393(19) 0.0172(17) 0.0170(16) 0.0068(16) C32 0.0266(18) 0.0297(17) 0.0256(16) 0.0063(13) 0.0119(14) -0.0004(14) C33 0.0229(16) 0.0263(16) 0.0212(15) 0.0020(12) 0.0093(13) 0.0011(13) C34 0.033(2) 0.0379(19) 0.0257(16) 0.0075(14) 0.0106(15) -0.0027(15) C35 0.041(2) 0.049(2) 0.0296(18) 0.0131(16) 0.0117(17) 0.0049(18) C36 0.029(2) 0.056(2) 0.0247(17) -0.0005(16) 0.0025(15) 0.0017(17) C37 0.0276(19) 0.0380(19) 0.0318(18) -0.0017(15) 0.0084(16) -0.0037(15) C38 0.0258(18) 0.0272(16) 0.0275(16) 0.0022(13) 0.0125(14) 0.0014(13) C39 0.0241(16) 0.0171(14) 0.0241(15) 0.0048(12) 0.0133(13) -0.0007(12) C40 0.0250(17) 0.0238(15) 0.0268(16) 0.0034(13) 0.0110(14) 0.0005(13) C41 0.039(2) 0.0263(16) 0.0271(16) -0.0040(13) 0.0150(15) -0.0086(15) C42 0.053(2) 0.0206(16) 0.0385(19) 0.0015(14) 0.0280(19) 0.0003(16) C43 0.040(2) 0.0221(16) 0.046(2) 0.0079(15) 0.0254(18) 0.0078(14) C44 0.0294(18) 0.0232(15) 0.0303(16) 0.0057(13) 0.0163(14) -0.0003(13) C45 0.0210(16) 0.0232(15) 0.0235(15) 0.0071(12) 0.0106(13) 0.0010(12) C46 0.0283(18) 0.0296(16) 0.0271(16) 0.0023(13) 0.0135(14) -0.0008(14) C47 0.040(2) 0.041(2) 0.0337(18) 0.0032(15) 0.0251(17) 0.0035(16) C48 0.031(2) 0.050(2) 0.046(2) 0.0108(18) 0.0260(18) 0.0018(17) C49 0.0302(19) 0.0364(19) 0.044(2) 0.0032(16) 0.0185(17) -0.0085(15) C50 0.0305(19) 0.0298(17) 0.0349(18) 0.0018(14) 0.0190(16) -0.0029(14) C51 0.0229(16) 0.0282(16) 0.0208(15) -0.0064(12) 0.0101(13) -0.0063(13) C52 0.0278(18) 0.0264(16) 0.0285(16) -0.0058(13) 0.0149(14) -0.0057(13) C53 0.0280(19) 0.0308(18) 0.045(2) -0.0107(16) 0.0185(17) -0.0016(15) C54 0.035(2) 0.044(2) 0.046(2) -0.0169(17) 0.0293(18) -0.0104(17) C55 0.041(2) 0.047(2) 0.0322(18) -0.0082(16) 0.0246(17) -0.0131(18) C56 0.0308(18) 0.0321(17) 0.0257(16) -0.0016(14) 0.0139(15) -0.0027(14) C57 0.0207(16) 0.0236(15) 0.0199(14) 0.0014(12) 0.0063(13) 0.0010(12) C58 0.0258(17) 0.0273(16) 0.0225(15) -0.0027(13) 0.0105(14) 0.0019(13) C59 0.0318(19) 0.0222(15) 0.0267(16) -0.0041(13) 0.0101(14) -0.0033(14) C60 0.0266(18) 0.0271(16) 0.0270(16) 0.0031(13) 0.0105(14) -0.0059(14) C61 0.0228(16) 0.0274(16) 0.0219(15) 0.0038(12) 0.0098(13) 0.0024(13) C62 0.0245(17) 0.0218(15) 0.0208(14) 0.0004(12) 0.0089(13) 0.0014(13) C63 0.0219(16) 0.0246(15) 0.0212(15) 0.0003(12) 0.0113(13) -0.0033(12) C64 0.0301(18) 0.0252(16) 0.0242(15) -0.0026(13) 0.0118(14) -0.0048(14) C65 0.0307(19) 0.0348(18) 0.0194(15) -0.0002(14) 0.0032(14) -0.0068(15) C66 0.0261(18) 0.0310(17) 0.0252(16) 0.0077(14) 0.0075(14) 0.0008(14) C67 0.0314(18) 0.0247(16) 0.0296(17) 0.0013(13) 0.0192(15) 0.0016(13) C68 0.0235(16) 0.0310(16) 0.0175(14) -0.0001(12) 0.0101(13) -0.0019(13) C69 0.0249(17) 0.0187(14) 0.0227(15) 0.0012(12) 0.0142(13) 0.0024(12) C70 0.0238(16) 0.0212(14) 0.0175(14) 0.0016(11) 0.0112(13) 0.0040(12) C71 0.0215(16) 0.0282(16) 0.0196(14) -0.0055(12) 0.0082(13) -0.0067(13) C72 0.0267(18) 0.0334(17) 0.0264(16) -0.0040(14) 0.0123(14) -0.0012(14) C73 0.0236(18) 0.051(2) 0.0370(19) -0.0122(17) 0.0181(16) -0.0084(16) C74 0.045(2) 0.043(2) 0.040(2) -0.0110(17) 0.0308(18) -0.0191(17) C75 0.049(2) 0.0313(18) 0.0371(19) -0.0014(15) 0.0264(18) -0.0112(16) C76 0.0319(19) 0.0274(16) 0.0278(16) -0.0004(13) 0.0160(15) -0.0031(14) C77 0.0248(17) 0.0273(16) 0.0180(14) -0.0017(12) 0.0092(13) -0.0046(13) C78 0.0295(19) 0.0364(18) 0.0236(16) -0.0003(14) 0.0126(14) -0.0012(15) C79 0.0228(19) 0.059(2) 0.0309(18) -0.0023(17) 0.0087(15) -0.0080(17) C80 0.042(2) 0.046(2) 0.037(2) -0.0028(17) 0.0130(18) -0.0229(19) C81 0.053(3) 0.0271(18) 0.0365(19) -0.0016(15) 0.0175(19) -0.0110(17) C82 0.0316(19) 0.0270(16) 0.0269(16) -0.0023(13) 0.0133(15) -0.0034(14) C83 0.0263(17) 0.0422(19) 0.0179(15) 0.0016(14) 0.0091(13) -0.0017(15) C84 0.049(2) 0.053(2) 0.0284(19) 0.0101(17) 0.0116(18) 0.0153(19) C85 0.048(3) 0.107(4) 0.036(2) 0.016(3) 0.007(2) 0.025(3) C86 0.036(2) 0.136(5) 0.0231(19) -0.009(3) 0.0043(18) 0.005(3) C87 0.043(3) 0.095(3) 0.029(2) -0.022(2) 0.0181(19) -0.020(2) C88 0.035(2) 0.052(2) 0.0262(17) -0.0086(16) 0.0165(16) -0.0080(17) C89 0.0246(17) 0.0223(15) 0.0238(15) -0.0044(12) 0.0136(13) -0.0014(13) C90 0.0283(18) 0.0250(16) 0.0267(16) -0.0014(13) 0.0135(14) -0.0004(13) C91 0.031(2) 0.0319(18) 0.043(2) -0.0007(15) 0.0178(17) 0.0061(15) C92 0.038(2) 0.039(2) 0.049(2) -0.0085(17) 0.0293(19) 0.0000(17) C93 0.047(2) 0.0374(19) 0.0358(19) -0.0063(16) 0.0293(18) -0.0080(17) C94 0.0337(19) 0.0307(17) 0.0265(16) -0.0019(13) 0.0172(15) -0.0032(14) C95 0.0325(18) 0.0213(15) 0.0221(15) 0.0029(12) 0.0141(14) 0.0028(13) C96 0.037(2) 0.0284(17) 0.0323(17) 0.0015(14) 0.0213(16) -0.0010(15) C97 0.049(2) 0.0277(18) 0.049(2) -0.0064(16) 0.0280(19) -0.0107(16) C98 0.064(3) 0.0224(17) 0.056(2) -0.0050(16) 0.034(2) -0.0012(18) C99 0.051(2) 0.0290(18) 0.058(2) -0.0029(17) 0.034(2) 0.0079(17) C100 0.039(2) 0.0288(17) 0.0400(19) 0.0005(15) 0.0237(17) 0.0042(15) C101 0.067(3) 0.114(5) 0.068(3) -0.015(3) 0.046(3) -0.031(3) C102 0.090(5) 0.104(5) 0.078(4) -0.017(4) 0.028(4) -0.004(4) C103 0.114(6) 0.075(4) 0.055(3) 0.004(3) 0.004(4) -0.005(4) C104 0.100(5) 0.094(5) 0.041(3) 0.003(3) -0.002(3) 0.002(4) C105 0.064(3) 0.090(4) 0.047(3) -0.013(3) 0.034(2) -0.012(3) C106 0.090(4) 0.067(3) 0.044(3) -0.008(2) 0.019(3) 0.001(3) C107 0.128(6) 0.102(5) 0.080(4) -0.006(4) 0.040(4) -0.006(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 N1 1.667(2) . ? P1 C39 1.787(3) . ? P1 C45 1.793(3) . ? P1 C33 1.794(3) . ? P2 N2 1.669(2) . ? P2 C95 1.788(3) . ? P2 C89 1.797(3) . ? P2 C83 1.800(3) . ? N1 C27 1.431(4) . ? N1 C19 1.486(3) . ? N2 C77 1.433(4) . ? N2 C70 1.486(4) . ? B1 C20 1.629(4) . ? B1 C13 1.645(5) . ? B1 C1 1.659(5) . ? B1 C7 1.668(5) . ? B2 C69 1.636(4) . ? B2 C51 1.648(4) . ? B2 C63 1.653(5) . ? B2 C57 1.681(4) . ? F1 C2 1.358(3) . ? F2 C3 1.342(4) . ? F3 C4 1.335(4) . ? F4 C5 1.349(4) . ? F5 C6 1.357(4) . ? F6 C8 1.355(3) . ? F7 C9 1.355(4) . ? F8 C10 1.342(4) . ? F9 C11 1.345(4) . ? F10 C12 1.352(4) . ? F11 C14 1.348(4) . ? F12 C15 1.347(4) . ? F13 C16 1.345(4) . ? F14 C17 1.349(4) . ? F15 C18 1.355(3) . ? F16 C28 1.340(4) . ? F17 C29 1.344(4) . ? F18 C30 1.347(4) . ? F19 C31 1.344(4) . ? F20 C32 1.346(4) . ? F21 C52 1.359(4) . ? F22 C53 1.354(4) . ? F23 C54 1.345(4) . ? F24 C55 1.354(4) . ? F25 C56 1.359(4) . ? F26 C58 1.352(3) . ? F27 C59 1.349(3) . ? F28 C60 1.341(3) . ? F29 C61 1.351(3) . ? F30 C62 1.360(3) . ? F31 C64 1.354(3) . ? F32 C65 1.349(4) . ? F33 C66 1.340(4) . ? F34 C67 1.352(3) . ? F35 C68 1.352(3) . ? F36 C78 1.344(4) . ? F37 C79 1.342(4) . ? F38 C80 1.340(4) . ? F39 C81 1.349(4) . ? F40 C82 1.335(4) . ? C1 C2 1.383(4) . ? C1 C6 1.391(4) . ? C2 C3 1.390(4) . ? C3 C4 1.368(5) . ? C4 C5 1.375(5) . ? C5 C6 1.374(5) . ? C7 C8 1.393(4) . ? C7 C12 1.395(4) . ? C8 C9 1.373(5) . ? C9 C10 1.375(5) . ? C10 C11 1.370(5) . ? C11 C12 1.381(5) . ? C13 C18 1.388(4) . ? C13 C14 1.389(4) . ? C14 C15 1.383(5) . ? C15 C16 1.371(5) . ? C16 C17 1.379(5) . ? C17 C18 1.370(5) . ? C19 C20 1.325(4) . ? C19 C21 1.496(4) . ? C21 C26 1.383(4) . ? C21 C22 1.392(4) . ? C22 C23 1.390(4) . ? C23 C24 1.375(5) . ? C24 C25 1.378(5) . ? C25 C26 1.389(4) . ? C27 C32 1.378(4) . ? C27 C28 1.379(4) . ? C28 C29 1.376(4) . ? C29 C30 1.364(5) . ? C30 C31 1.374(5) . ? C31 C32 1.376(5) . ? C33 C38 1.396(4) . ? C33 C34 1.398(4) . ? C34 C35 1.385(5) . ? C35 C36 1.382(5) . ? C36 C37 1.379(5) . ? C37 C38 1.391(5) . ? C39 C44 1.397(4) . ? C39 C40 1.398(4) . ? C40 C41 1.380(4) . ? C41 C42 1.376(5) . ? C42 C43 1.381(5) . ? C43 C44 1.386(4) . ? C45 C50 1.394(4) . ? C45 C46 1.401(4) . ? C46 C47 1.391(4) . ? C47 C48 1.388(5) . ? C48 C49 1.389(5) . ? C49 C50 1.390(5) . ? C51 C56 1.384(4) . ? C51 C52 1.392(4) . ? C52 C53 1.373(5) . ? C53 C54 1.382(5) . ? C54 C55 1.354(5) . ? C55 C56 1.379(5) . ? C57 C62 1.393(4) . ? C57 C58 1.400(4) . ? C58 C59 1.381(4) . ? C59 C60 1.375(5) . ? C60 C61 1.375(4) . ? C61 C62 1.379(4) . ? C63 C68 1.387(4) . ? C63 C64 1.398(4) . ? C64 C65 1.372(5) . ? C65 C66 1.379(5) . ? C66 C67 1.366(4) . ? C67 C68 1.382(4) . ? C69 C70 1.325(4) . ? C70 C71 1.491(4) . ? C71 C76 1.388(4) . ? C71 C72 1.396(4) . ? C72 C73 1.389(5) . ? C73 C74 1.381(5) . ? C74 C75 1.377(5) . ? C75 C76 1.395(4) . ? C77 C82 1.375(4) . ? C77 C78 1.390(4) . ? C78 C79 1.376(5) . ? C79 C80 1.377(5) . ? C80 C81 1.361(6) . ? C81 C82 1.378(5) . ? C83 C88 1.390(5) . ? C83 C84 1.394(5) . ? C84 C85 1.392(6) . ? C85 C86 1.378(7) . ? C86 C87 1.365(7) . ? C87 C88 1.397(5) . ? C89 C90 1.386(4) . ? C89 C94 1.400(4) . ? C90 C91 1.390(5) . ? C91 C92 1.379(5) . ? C92 C93 1.381(5) . ? C93 C94 1.385(5) . ? C95 C96 1.393(5) . ? C95 C100 1.395(4) . ? C96 C97 1.390(5) . ? C97 C98 1.371(5) . ? C98 C99 1.388(5) . ? C99 C100 1.381(5) . ? C101 C102 1.368(8) . ? C101 C106 1.380(7) . ? C102 C103 1.399(9) . ? C103 C104 1.327(9) . ? C104 C105 1.324(7) . ? C105 C106 1.429(7) . ? C106 C107 1.390(8) . ? C201 C207 1.21(2) . ? C201 C202 1.3900 . ? C201 C206 1.3900 . ? C202 C203 1.3900 . ? C203 C204 1.3900 . ? C204 C205 1.3900 . ? C205 C206 1.3900 . ? 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 N1 P1 C39 107.84(13) . . ? N1 P1 C45 107.21(13) . . ? C39 P1 C45 111.28(14) . . ? N1 P1 C33 115.24(13) . . ? C39 P1 C33 110.03(14) . . ? C45 P1 C33 105.24(14) . . ? N2 P2 C95 108.12(13) . . ? N2 P2 C89 115.44(13) . . ? C95 P2 C89 109.82(14) . . ? N2 P2 C83 105.95(14) . . ? C95 P2 C83 111.58(15) . . ? C89 P2 C83 105.91(14) . . ? C27 N1 C19 116.8(2) . . ? C27 N1 P1 119.48(18) . . ? C19 N1 P1 123.26(19) . . ? C77 N2 C70 117.3(2) . . ? C77 N2 P2 118.71(19) . . ? C70 N2 P2 123.38(19) . . ? C20 B1 C13 107.2(3) . . ? C20 B1 C1 113.3(2) . . ? C13 B1 C1 112.6(2) . . ? C20 B1 C7 107.7(2) . . ? C13 B1 C7 112.0(2) . . ? C1 B1 C7 104.0(2) . . ? C69 B2 C51 108.0(2) . . ? C69 B2 C63 113.9(2) . . ? C51 B2 C63 112.2(2) . . ? C69 B2 C57 106.3(2) . . ? C51 B2 C57 113.4(2) . . ? C63 B2 C57 103.0(2) . . ? C2 C1 C6 113.2(3) . . ? C2 C1 B1 126.5(3) . . ? C6 C1 B1 120.2(3) . . ? F1 C2 C1 121.6(3) . . ? F1 C2 C3 114.2(3) . . ? C1 C2 C3 124.1(3) . . ? F2 C3 C4 119.7(3) . . ? F2 C3 C2 120.8(3) . . ? C4 C3 C2 119.5(3) . . ? F3 C4 C3 120.3(3) . . ? F3 C4 C5 120.6(3) . . ? C3 C4 C5 119.1(3) . . ? F4 C5 C6 120.9(3) . . ? F4 C5 C4 119.6(3) . . ? C6 C5 C4 119.4(3) . . ? F5 C6 C5 116.6(3) . . ? F5 C6 C1 118.8(3) . . ? C5 C6 C1 124.6(3) . . ? C8 C7 C12 112.4(3) . . ? C8 C7 B1 120.3(3) . . ? C12 C7 B1 127.3(3) . . ? F6 C8 C9 115.0(3) . . ? F6 C8 C7 120.2(3) . . ? C9 C8 C7 124.9(3) . . ? F7 C9 C8 120.3(3) . . ? F7 C9 C10 119.9(3) . . ? C8 C9 C10 119.9(3) . . ? F8 C10 C11 120.7(3) . . ? F8 C10 C9 120.8(3) . . ? C11 C10 C9 118.5(3) . . ? F9 C11 C10 119.5(3) . . ? F9 C11 C12 120.5(3) . . ? C10 C11 C12 119.9(3) . . ? F10 C12 C11 114.7(3) . . ? F10 C12 C7 120.9(3) . . ? C11 C12 C7 124.5(3) . . ? C18 C13 C14 113.2(3) . . ? C18 C13 B1 118.8(3) . . ? C14 C13 B1 127.4(3) . . ? F11 C14 C15 115.1(3) . . ? F11 C14 C13 121.3(3) . . ? C15 C14 C13 123.5(3) . . ? F12 C15 C16 119.7(3) . . ? F12 C15 C14 120.2(3) . . ? C16 C15 C14 120.1(3) . . ? F13 C16 C15 120.5(3) . . ? F13 C16 C17 120.6(4) . . ? C15 C16 C17 119.0(3) . . ? F14 C17 C18 121.5(3) . . ? F14 C17 C16 119.6(3) . . ? C18 C17 C16 118.9(3) . . ? F15 C18 C17 115.5(3) . . ? F15 C18 C13 119.2(3) . . ? C17 C18 C13 125.3(3) . . ? C20 C19 N1 120.8(3) . . ? C20 C19 C21 127.7(3) . . ? N1 C19 C21 111.5(2) . . ? C19 C20 B1 130.9(3) . . ? C26 C21 C22 118.9(3) . . ? C26 C21 C19 121.6(3) . . ? C22 C21 C19 119.5(3) . . ? C23 C22 C21 120.6(3) . . ? C24 C23 C22 119.9(3) . . ? C23 C24 C25 119.8(3) . . ? C24 C25 C26 120.5(3) . . ? C21 C26 C25 120.2(3) . . ? C32 C27 C28 117.7(3) . . ? C32 C27 N1 120.9(3) . . ? C28 C27 N1 121.3(3) . . ? F16 C28 C29 118.7(3) . . ? F16 C28 C27 119.6(3) . . ? C29 C28 C27 121.7(3) . . ? F17 C29 C30 120.0(3) . . ? F17 C29 C28 120.7(3) . . ? C30 C29 C28 119.3(3) . . ? F18 C30 C29 119.7(3) . . ? F18 C30 C31 119.8(3) . . ? C29 C30 C31 120.5(3) . . ? F19 C31 C30 120.5(3) . . ? F19 C31 C32 120.0(3) . . ? C30 C31 C32 119.4(3) . . ? F20 C32 C31 118.5(3) . . ? F20 C32 C27 120.2(3) . . ? C31 C32 C27 121.4(3) . . ? C38 C33 C34 119.3(3) . . ? C38 C33 P1 122.7(2) . . ? C34 C33 P1 118.0(2) . . ? C35 C34 C33 120.3(3) . . ? C36 C35 C34 119.9(3) . . ? C37 C36 C35 120.3(3) . . ? C36 C37 C38 120.4(3) . . ? C37 C38 C33 119.7(3) . . ? C44 C39 C40 120.0(3) . . ? C44 C39 P1 121.4(2) . . ? C40 C39 P1 118.6(2) . . ? C41 C40 C39 119.7(3) . . ? C42 C41 C40 120.2(3) . . ? C41 C42 C43 120.5(3) . . ? C42 C43 C44 120.4(3) . . ? C43 C44 C39 119.2(3) . . ? C50 C45 C46 120.1(3) . . ? C50 C45 P1 121.8(2) . . ? C46 C45 P1 118.1(2) . . ? C47 C46 C45 119.8(3) . . ? C48 C47 C46 119.9(3) . . ? C47 C48 C49 120.3(3) . . ? C48 C49 C50 120.3(3) . . ? C49 C50 C45 119.6(3) . . ? C56 C51 C52 112.4(3) . . ? C56 C51 B2 126.9(3) . . ? C52 C51 B2 120.1(3) . . ? F21 C52 C53 115.7(3) . . ? F21 C52 C51 119.2(3) . . ? C53 C52 C51 125.1(3) . . ? F22 C53 C52 121.4(3) . . ? F22 C53 C54 119.5(3) . . ? C52 C53 C54 119.1(3) . . ? F23 C54 C55 121.0(3) . . ? F23 C54 C53 120.3(3) . . ? C55 C54 C53 118.6(3) . . ? C54 C55 F24 120.0(3) . . ? C54 C55 C56 120.4(3) . . ? F24 C55 C56 119.6(3) . . ? F25 C56 C55 115.0(3) . . ? F25 C56 C51 120.6(3) . . ? C55 C56 C51 124.4(3) . . ? C62 C57 C58 112.5(3) . . ? C62 C57 B2 119.0(3) . . ? C58 C57 B2 128.4(3) . . ? F26 C58 C59 115.3(3) . . ? F26 C58 C57 120.9(3) . . ? C59 C58 C57 123.7(3) . . ? F27 C59 C60 118.9(3) . . ? F27 C59 C58 120.3(3) . . ? C60 C59 C58 120.7(3) . . ? F28 C60 C61 121.0(3) . . ? F28 C60 C59 120.8(3) . . ? C61 C60 C59 118.3(3) . . ? F29 C61 C60 120.1(3) . . ? F29 C61 C62 120.4(3) . . ? C60 C61 C62 119.5(3) . . ? F30 C62 C61 114.9(3) . . ? F30 C62 C57 119.8(3) . . ? C61 C62 C57 125.2(3) . . ? C68 C63 C64 112.8(3) . . ? C68 C63 B2 126.8(3) . . ? C64 C63 B2 120.2(3) . . ? F31 C64 C65 116.5(3) . . ? F31 C64 C63 118.8(3) . . ? C65 C64 C63 124.6(3) . . ? F32 C65 C64 121.1(3) . . ? F32 C65 C66 119.2(3) . . ? C64 C65 C66 119.7(3) . . ? F33 C66 C67 120.7(3) . . ? F33 C66 C65 120.9(3) . . ? C67 C66 C65 118.4(3) . . ? F34 C67 C66 119.2(3) . . ? F34 C67 C68 120.4(3) . . ? C66 C67 C68 120.4(3) . . ? F35 C68 C67 114.7(3) . . ? F35 C68 C63 121.2(3) . . ? C67 C68 C63 124.1(3) . . ? C70 C69 B2 130.6(3) . . ? C69 C70 N2 121.4(3) . . ? C69 C70 C71 126.7(3) . . ? N2 C70 C71 111.9(2) . . ? C76 C71 C72 118.7(3) . . ? C76 C71 C70 119.8(3) . . ? C72 C71 C70 121.5(3) . . ? C73 C72 C71 120.3(3) . . ? C74 C73 C72 120.1(3) . . ? C75 C74 C73 120.4(3) . . ? C74 C75 C76 119.6(3) . . ? C71 C76 C75 120.9(3) . . ? C82 C77 C78 117.4(3) . . ? C82 C77 N2 121.4(3) . . ? C78 C77 N2 121.2(3) . . ? F36 C78 C79 118.6(3) . . ? F36 C78 C77 119.9(3) . . ? C79 C78 C77 121.5(3) . . ? F37 C79 C78 120.1(3) . . ? F37 C79 C80 120.5(3) . . ? C78 C79 C80 119.4(3) . . ? F38 C80 C81 119.7(4) . . ? F38 C80 C79 120.1(4) . . ? C81 C80 C79 120.2(3) . . ? F39 C81 C80 119.6(3) . . ? F39 C81 C82 120.3(4) . . ? C80 C81 C82 120.0(3) . . ? F40 C82 C77 119.6(3) . . ? F40 C82 C81 118.8(3) . . ? C77 C82 C81 121.5(3) . . ? C88 C83 C84 120.4(3) . . ? C88 C83 P2 118.2(3) . . ? C84 C83 P2 121.3(3) . . ? C85 C84 C83 118.5(4) . . ? C86 C85 C84 121.4(4) . . ? C87 C86 C85 119.6(4) . . ? C86 C87 C88 120.9(4) . . ? C83 C88 C87 119.1(4) . . ? C90 C89 C94 120.5(3) . . ? C90 C89 P2 122.8(2) . . ? C94 C89 P2 116.7(2) . . ? C89 C90 C91 119.2(3) . . ? C92 C91 C90 120.5(3) . . ? C91 C92 C93 120.4(3) . . ? C92 C93 C94 120.1(3) . . ? C93 C94 C89 119.3(3) . . ? C96 C95 C100 120.1(3) . . ? C96 C95 P2 121.0(2) . . ? C100 C95 P2 118.9(2) . . ? C97 C96 C95 119.7(3) . . ? C98 C97 C96 119.6(3) . . ? C97 C98 C99 121.2(3) . . ? C100 C99 C98 119.6(3) . . ? C99 C100 C95 119.7(3) . . ? C102 C101 C106 122.4(6) . . ? C101 C102 C103 119.2(7) . . ? C104 C103 C102 116.6(7) . . ? C105 C104 C103 127.6(7) . . ? C104 C105 C106 116.9(5) . . ? C101 C106 C107 121.0(6) . . ? C101 C106 C105 117.3(5) . . ? C107 C106 C105 121.7(6) . . ? C207 C201 C202 129.1(12) . . ? C207 C201 C206 110.8(12) . . ? C202 C201 C206 120.0 . . ? C203 C202 C201 120.0 . . ? C202 C203 C204 120.0 . . ? C203 C204 C205 120.0 . . ? C206 C205 C204 120.0 . . ? C205 C206 C201 120.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.237 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.100 #===end data_cj020_0ma _database_code_depnum_ccdc_archive 'CCDC 873947' #TrackingRef 'combined-CIFs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H30 B F15 N P' _chemical_formula_weight 947.51 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1999(8) _cell_length_b 17.1867(13) _cell_length_c 24.1364(19) _cell_angle_alpha 89.968(4) _cell_angle_beta 80.171(4) _cell_angle_gamma 83.358(4) _cell_volume 4140.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9363 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9681 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69928 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.86 _diffrn_reflns_theta_max 27.53 _reflns_number_total 18865 _reflns_number_gt 13852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0517P)^2^+0.8290P] 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 18865 _refine_ls_number_parameters 1197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group H1A H -0.934(2) 0.1588(11) 0.3452(8) 0.032(6) Uiso 1 1 d . . . H2A H 0.444(2) 0.7035(11) 0.2630(9) 0.032(6) Uiso 1 1 d . . . C1 C -1.16438(17) 0.30680(10) 0.31562(7) 0.0233(4) Uani 1 1 d . . . C2 C -1.1962(2) 0.37054(11) 0.28233(8) 0.0335(4) Uani 1 1 d . . . H2 H -1.1503 0.3734 0.2458 0.040 Uiso 1 1 calc R . . C3 C -1.2957(2) 0.42906(13) 0.30387(10) 0.0440(5) Uani 1 1 d . . . H3 H -1.3168 0.4714 0.2817 0.053 Uiso 1 1 calc R . . C4 C -1.3643(2) 0.42542(13) 0.35799(10) 0.0444(6) Uani 1 1 d . . . H4 H -1.4309 0.4654 0.3723 0.053 Uiso 1 1 calc R . . C5 C -1.3342(2) 0.36270(13) 0.39092(10) 0.0430(5) Uani 1 1 d . . . H5 H -1.3816 0.3600 0.4272 0.052 Uiso 1 1 calc R . . C6 C -1.23382(19) 0.30360(12) 0.37032(8) 0.0330(4) Uani 1 1 d . . . H6 H -1.2128 0.2618 0.3930 0.040 Uiso 1 1 calc R . . C7 C -0.88273(16) 0.29701(9) 0.30559(7) 0.0214(4) Uani 1 1 d . . . C8 C -0.85955(18) 0.30490(10) 0.36051(8) 0.0280(4) Uani 1 1 d . . . H8 H -0.9041 0.2768 0.3893 0.034 Uiso 1 1 calc R . . C9 C -0.7698(2) 0.35479(11) 0.37177(9) 0.0357(5) Uani 1 1 d . . . H9 H -0.7532 0.3599 0.4082 0.043 Uiso 1 1 calc R . . C10 C -0.7047(2) 0.39697(11) 0.32916(9) 0.0376(5) Uani 1 1 d . . . H10 H -0.6448 0.4306 0.3371 0.045 Uiso 1 1 calc R . . C11 C -0.7276(2) 0.38974(11) 0.27490(9) 0.0381(5) Uani 1 1 d . . . H11 H -0.6825 0.4179 0.2463 0.046 Uiso 1 1 calc R . . C12 C -0.81788(19) 0.34043(10) 0.26293(8) 0.0302(4) Uani 1 1 d . . . H12 H -0.8350 0.3364 0.2265 0.036 Uiso 1 1 calc R . . C13 C -1.00012(17) 0.21885(10) 0.21992(7) 0.0225(4) Uani 1 1 d . . . C14 C -1.11431(19) 0.21792(11) 0.19543(8) 0.0288(4) Uani 1 1 d . . . H14 H -1.1985 0.2334 0.2164 0.035 Uiso 1 1 calc R . . C15 C -1.1023(2) 0.19387(12) 0.13979(8) 0.0356(5) Uani 1 1 d . . . H15 H -1.1786 0.1928 0.1236 0.043 Uiso 1 1 calc R . . C16 C -0.9772(2) 0.17151(11) 0.10840(8) 0.0334(4) Uani 1 1 d . . . H16 H -0.9694 0.1561 0.0709 0.040 Uiso 1 1 calc R . . C17 C -0.86311(19) 0.17193(10) 0.13237(8) 0.0293(4) Uani 1 1 d . . . H17 H -0.7791 0.1568 0.1110 0.035 Uiso 1 1 calc R . . C18 C -0.87427(18) 0.19493(10) 0.18800(8) 0.0250(4) Uani 1 1 d . . . H18 H -0.7978 0.1945 0.2042 0.030 Uiso 1 1 calc R . . C19 C -1.07275(18) 0.09153(10) 0.33191(8) 0.0264(4) Uani 1 1 d . . . C20 C -0.9972(2) 0.03595(12) 0.28530(10) 0.0431(5) Uani 1 1 d . . . H20A H -1.0001 0.0600 0.2495 0.065 Uiso 1 1 calc R . . H20B H -1.0380 -0.0118 0.2865 0.065 Uiso 1 1 calc R . . H20C H -0.9056 0.0246 0.2903 0.065 Uiso 1 1 calc R . . C21 C -1.2177(2) 0.11177(12) 0.32447(10) 0.0420(5) Uani 1 1 d . . . H21A H -1.2638 0.1469 0.3543 0.063 Uiso 1 1 calc R . . H21B H -1.2604 0.0647 0.3255 0.063 Uiso 1 1 calc R . . H21C H -1.2204 0.1365 0.2889 0.063 Uiso 1 1 calc R . . C22 C -1.0693(2) 0.05490(11) 0.38917(9) 0.0391(5) Uani 1 1 d . . . H22A H -1.1174 0.0907 0.4181 0.059 Uiso 1 1 calc R . . H22B H -0.9781 0.0436 0.3946 0.059 Uiso 1 1 calc R . . H22C H -1.1104 0.0072 0.3909 0.059 Uiso 1 1 calc R . . C23 C -0.35533(17) 0.18664(9) 0.04152(7) 0.0204(4) Uani 1 1 d . . . C24 C -0.22533(17) 0.18709(10) 0.01270(7) 0.0231(4) Uani 1 1 d . . . C25 C -0.14512(18) 0.12172(11) -0.01175(7) 0.0268(4) Uani 1 1 d . . . C26 C -0.19285(19) 0.05012(10) -0.00843(8) 0.0280(4) Uani 1 1 d . . . C27 C -0.32164(19) 0.04570(10) 0.01876(8) 0.0278(4) Uani 1 1 d . . . C28 C -0.39826(17) 0.11244(10) 0.04218(7) 0.0246(4) Uani 1 1 d . . . C29 C -0.69393(18) 0.33483(10) 0.09055(7) 0.0242(4) Uani 1 1 d . . . C30 C -0.59734(17) 0.28257(9) 0.05778(7) 0.0212(4) Uani 1 1 d . . . C31 C -0.63685(18) 0.25775(10) 0.00922(8) 0.0251(4) Uani 1 1 d . . . C32 C -0.76117(19) 0.28088(11) -0.00522(8) 0.0303(4) Uani 1 1 d . . . C33 C -0.85277(18) 0.33117(11) 0.02945(9) 0.0305(4) Uani 1 1 d . . . C34 C -0.81927(18) 0.35821(10) 0.07814(8) 0.0293(4) Uani 1 1 d . . . C35 C -0.37768(16) 0.33988(9) 0.07590(7) 0.0197(3) Uani 1 1 d . . . C36 C -0.35960(18) 0.38147(10) 0.02652(7) 0.0268(4) Uani 1 1 d . . . C37 C -0.2944(2) 0.44774(10) 0.01878(8) 0.0305(4) Uani 1 1 d . . . C38 C -0.23985(18) 0.47488(10) 0.06252(8) 0.0271(4) Uani 1 1 d . . . C39 C -0.25451(17) 0.43624(9) 0.11240(8) 0.0232(4) Uani 1 1 d . . . C40 C -0.32482(16) 0.37170(9) 0.11867(7) 0.0198(3) Uani 1 1 d . . . C41 C -0.48336(17) 0.22662(9) 0.14115(7) 0.0213(4) Uani 1 1 d . . . C42 C -0.50918(17) 0.19808(10) 0.18686(7) 0.0232(4) Uani 1 1 d . . . C43 C -0.54115(17) 0.16565(10) 0.24198(7) 0.0246(4) Uani 1 1 d . . . C44 C -0.5919(2) 0.09309(12) 0.24818(9) 0.0386(5) Uani 1 1 d . . . H44 H -0.6057 0.0661 0.2167 0.046 Uiso 1 1 calc R . . C45 C -0.6216(2) 0.06155(15) 0.30104(12) 0.0566(7) Uani 1 1 d . . . H45 H -0.6548 0.0133 0.3048 0.068 Uiso 1 1 calc R . . C46 C -0.6022(3) 0.10097(19) 0.34782(11) 0.0669(9) Uani 1 1 d . . . H46 H -0.6213 0.0792 0.3832 0.080 Uiso 1 1 calc R . . C47 C -0.5544(2) 0.17268(18) 0.34242(10) 0.0589(8) Uani 1 1 d . . . H47 H -0.5426 0.1996 0.3743 0.071 Uiso 1 1 calc R . . C48 C -0.52356(19) 0.20524(13) 0.28987(8) 0.0366(5) Uani 1 1 d . . . H48 H -0.4910 0.2537 0.2867 0.044 Uiso 1 1 calc R . . C49 C 0.17070(16) 0.69027(9) 0.19846(7) 0.0204(3) Uani 1 1 d . . . C50 C 0.14476(18) 0.70213(10) 0.14410(7) 0.0254(4) Uani 1 1 d . . . H50 H 0.1780 0.7432 0.1232 0.030 Uiso 1 1 calc R . . C51 C 0.06926(19) 0.65260(11) 0.12113(8) 0.0314(4) Uani 1 1 d . . . H51 H 0.0519 0.6603 0.0848 0.038 Uiso 1 1 calc R . . C52 C 0.01989(19) 0.59160(11) 0.15245(9) 0.0335(5) Uani 1 1 d . . . H52 H -0.0300 0.5582 0.1368 0.040 Uiso 1 1 calc R . . C53 C 0.04382(19) 0.57980(11) 0.20657(9) 0.0323(4) Uani 1 1 d . . . H53 H 0.0091 0.5390 0.2273 0.039 Uiso 1 1 calc R . . C54 C 0.11966(17) 0.62873(10) 0.23004(8) 0.0251(4) Uani 1 1 d . . . H54 H 0.1364 0.6207 0.2664 0.030 Uiso 1 1 calc R . . C55 C 0.30022(17) 0.83284(9) 0.18495(7) 0.0203(4) Uani 1 1 d . . . C56 C 0.18519(18) 0.88180(10) 0.17884(8) 0.0261(4) Uani 1 1 d . . . H56 H 0.1013 0.8684 0.1947 0.031 Uiso 1 1 calc R . . C57 C 0.1955(2) 0.95023(10) 0.14924(8) 0.0309(4) Uani 1 1 d . . . H57 H 0.1188 0.9831 0.1452 0.037 Uiso 1 1 calc R . . C58 C 0.3211(2) 0.96951(11) 0.12560(8) 0.0356(5) Uani 1 1 d . . . H58 H 0.3282 1.0150 0.1049 0.043 Uiso 1 1 calc R . . C59 C 0.4352(2) 0.92209(11) 0.13241(8) 0.0362(5) Uani 1 1 d . . . H59 H 0.5189 0.9360 0.1168 0.043 Uiso 1 1 calc R . . C60 C 0.42589(18) 0.85357(11) 0.16250(8) 0.0284(4) Uani 1 1 d . . . H60 H 0.5030 0.8218 0.1676 0.034 Uiso 1 1 calc R . . C61 C 0.20564(16) 0.78661(9) 0.29546(7) 0.0191(3) Uani 1 1 d . . . C62 C 0.06945(17) 0.78571(10) 0.31612(7) 0.0230(4) Uani 1 1 d . . . H62 H 0.0168 0.7600 0.2959 0.028 Uiso 1 1 calc R . . C63 C 0.01314(18) 0.82321(10) 0.36679(8) 0.0269(4) Uani 1 1 d . . . H63 H -0.0775 0.8224 0.3807 0.032 Uiso 1 1 calc R . . C64 C 0.09102(18) 0.86187(10) 0.39682(8) 0.0272(4) Uani 1 1 d . . . H64 H 0.0525 0.8867 0.4309 0.033 Uiso 1 1 calc R . . C65 C 0.22597(18) 0.86379(10) 0.37638(7) 0.0245(4) Uani 1 1 d . . . H65 H 0.2776 0.8901 0.3967 0.029 Uiso 1 1 calc R . . C66 C 0.28395(17) 0.82672(9) 0.32586(7) 0.0223(4) Uani 1 1 d . . . H66 H 0.3744 0.8283 0.3120 0.027 Uiso 1 1 calc R . . C67 C 0.50662(17) 0.63406(10) 0.19526(7) 0.0233(4) Uani 1 1 d . . . C68 C 0.46560(19) 0.55438(10) 0.21491(9) 0.0332(4) Uani 1 1 d . . . H68A H 0.3748 0.5512 0.2101 0.050 Uiso 1 1 calc R . . H68B H 0.4724 0.5484 0.2539 0.050 Uiso 1 1 calc R . . H68C H 0.5238 0.5135 0.1930 0.050 Uiso 1 1 calc R . . C69 C 0.4913(2) 0.64509(13) 0.13415(8) 0.0424(5) Uani 1 1 d . . . H69A H 0.4004 0.6404 0.1302 0.064 Uiso 1 1 calc R . . H69B H 0.5504 0.6057 0.1111 0.064 Uiso 1 1 calc R . . H69C H 0.5134 0.6961 0.1225 0.064 Uiso 1 1 calc R . . C70 C 0.65018(18) 0.64117(12) 0.20196(9) 0.0363(5) Uani 1 1 d . . . H70A H 0.6591 0.6340 0.2406 0.054 Uiso 1 1 calc R . . H70B H 0.6727 0.6921 0.1904 0.054 Uiso 1 1 calc R . . H70C H 0.7095 0.6018 0.1790 0.054 Uiso 1 1 calc R . . N1 N -1.00535(15) 0.16511(8) 0.33282(6) 0.0242(3) Uani 1 1 d . . . N2 N 0.42089(14) 0.69686(8) 0.23292(7) 0.0217(3) Uani 1 1 d . . . B1 B -0.45203(19) 0.25898(11) 0.07878(8) 0.0204(4) Uani 1 1 d . . . F1 F -0.16556(10) 0.25383(6) 0.00735(5) 0.0335(3) Uani 1 1 d . . . F2 F -0.01963(11) 0.12757(7) -0.03857(5) 0.0393(3) Uani 1 1 d . . . F3 F -0.11647(12) -0.01405(6) -0.03218(5) 0.0398(3) Uani 1 1 d . . . F4 F -0.37096(12) -0.02409(6) 0.02151(5) 0.0415(3) Uani 1 1 d . . . F5 F -0.52444(10) 0.10371(6) 0.06750(5) 0.0345(3) Uani 1 1 d . . . F6 F -0.55231(11) 0.20911(6) -0.02830(4) 0.0354(3) Uani 1 1 d . . . F7 F -0.79174(12) 0.25487(7) -0.05363(5) 0.0476(3) Uani 1 1 d . . . F8 F -0.97389(11) 0.35431(7) 0.01614(6) 0.0455(3) Uani 1 1 d . . . F9 F -0.90858(11) 0.40762(7) 0.11286(5) 0.0451(3) Uani 1 1 d . . . F10 F -0.66618(11) 0.36620(6) 0.13802(4) 0.0325(2) Uani 1 1 d . . . F11 F -0.40250(12) 0.35460(7) -0.01931(4) 0.0412(3) Uani 1 1 d . . . F12 F -0.27928(14) 0.48413(7) -0.03067(5) 0.0506(3) Uani 1 1 d . . . F13 F -0.17260(12) 0.53836(6) 0.05632(5) 0.0427(3) Uani 1 1 d . . . F14 F -0.20176(11) 0.46180(6) 0.15584(4) 0.0324(3) Uani 1 1 d . . . F15 F -0.33702(10) 0.34013(6) 0.17029(4) 0.0287(2) Uani 1 1 d . . . P2 P 0.27999(4) 0.74779(2) 0.226981(18) 0.01763(9) Uani 1 1 d . . . P1 P -1.01445(4) 0.24211(2) 0.293123(19) 0.02006(10) Uani 1 1 d . . . C71 C 0.72144(16) 0.64545(10) 0.41978(7) 0.0208(4) Uani 1 1 d . . . C72 C 0.69098(17) 0.60467(10) 0.46896(7) 0.0252(4) Uani 1 1 d . . . C73 C 0.7559(2) 0.53361(11) 0.48062(8) 0.0320(4) Uani 1 1 d . . . C74 C 0.8588(2) 0.49818(11) 0.44100(9) 0.0356(5) Uani 1 1 d . . . C75 C 0.89355(19) 0.53507(11) 0.39128(8) 0.0323(4) Uani 1 1 d . . . C76 C 0.82480(18) 0.60694(10) 0.38185(8) 0.0264(4) Uani 1 1 d . . . C77 C 0.66578(16) 0.80238(10) 0.45019(7) 0.0206(4) Uani 1 1 d . . . C78 C 0.61268(17) 0.87908(10) 0.44170(7) 0.0238(4) Uani 1 1 d . . . C79 C 0.65061(18) 0.94487(10) 0.46435(8) 0.0269(4) Uani 1 1 d . . . C80 C 0.74347(19) 0.93635(10) 0.49982(8) 0.0285(4) Uani 1 1 d . . . C81 C 0.79526(17) 0.86255(11) 0.51169(7) 0.0259(4) Uani 1 1 d . . . C82 C 0.75749(17) 0.79771(10) 0.48682(7) 0.0228(4) Uani 1 1 d . . . C83 C 0.47423(16) 0.71351(9) 0.42236(7) 0.0206(4) Uani 1 1 d . . . C84 C 0.43193(17) 0.66195(10) 0.38658(7) 0.0222(4) Uani 1 1 d . . . C85 C 0.30241(18) 0.64300(10) 0.39124(8) 0.0256(4) Uani 1 1 d . . . C86 C 0.20656(17) 0.67572(11) 0.43407(8) 0.0276(4) Uani 1 1 d . . . C87 C 0.24221(17) 0.72663(11) 0.47130(8) 0.0266(4) Uani 1 1 d . . . C88 C 0.37334(17) 0.74369(10) 0.46492(7) 0.0231(4) Uani 1 1 d . . . C89 C 0.66908(17) 0.76236(10) 0.34842(7) 0.0224(4) Uani 1 1 d . . . C90 C 0.69605(17) 0.79756(10) 0.30564(7) 0.0231(4) Uani 1 1 d . . . C91 C 0.73114(17) 0.84231(10) 0.25590(7) 0.0222(4) Uani 1 1 d . . . C92 C 0.81891(17) 0.80953(11) 0.20879(7) 0.0251(4) Uani 1 1 d . . . H92 H 0.8566 0.7577 0.2094 0.030 Uiso 1 1 calc R . . C93 C 0.85060(19) 0.85320(12) 0.16123(8) 0.0329(4) Uani 1 1 d . . . H93 H 0.9074 0.8301 0.1298 0.040 Uiso 1 1 calc R . . C94 C 0.7986(2) 0.93074(12) 0.16006(9) 0.0383(5) Uani 1 1 d . . . H94 H 0.8206 0.9600 0.1281 0.046 Uiso 1 1 calc R . . C95 C 0.7133(2) 0.96476(12) 0.20674(9) 0.0398(5) Uani 1 1 d . . . H95 H 0.6789 1.0172 0.2063 0.048 Uiso 1 1 calc R . . C96 C 0.67901(19) 0.92083(11) 0.25410(8) 0.0318(4) Uani 1 1 d . . . H96 H 0.6206 0.9440 0.2850 0.038 Uiso 1 1 calc R . . B2 B 0.63390(19) 0.73000(11) 0.41056(8) 0.0200(4) Uani 1 1 d . . . F16 F 0.59418(11) 0.63760(6) 0.51085(4) 0.0354(3) Uani 1 1 d . . . F17 F 0.72051(14) 0.49884(7) 0.53017(5) 0.0522(3) Uani 1 1 d . . . F18 F 0.92355(14) 0.42861(7) 0.45139(6) 0.0561(4) Uani 1 1 d . . . F19 F 0.99245(13) 0.50136(7) 0.35176(6) 0.0541(4) Uani 1 1 d . . . F20 F 0.86771(12) 0.63789(7) 0.33124(5) 0.0420(3) Uani 1 1 d . . . F21 F 0.51756(10) 0.89253(6) 0.40915(4) 0.0310(2) Uani 1 1 d . . . F22 F 0.59744(11) 1.01710(6) 0.45244(5) 0.0374(3) Uani 1 1 d . . . F23 F 0.78076(12) 0.99967(6) 0.52329(5) 0.0416(3) Uani 1 1 d . . . F24 F 0.88483(11) 0.85306(7) 0.54690(5) 0.0377(3) Uani 1 1 d . . . F25 F 0.81864(10) 0.72838(6) 0.50043(4) 0.0303(2) Uani 1 1 d . . . F26 F 0.52179(10) 0.62646(6) 0.34314(4) 0.0300(2) Uani 1 1 d . . . F27 F 0.27061(11) 0.59267(6) 0.35413(5) 0.0380(3) Uani 1 1 d . . . F28 F 0.07962(10) 0.65892(7) 0.43917(5) 0.0407(3) Uani 1 1 d . . . F29 F 0.14797(11) 0.76099(7) 0.51273(5) 0.0398(3) Uani 1 1 d . . . F30 F 0.39816(10) 0.79391(6) 0.50454(4) 0.0329(3) 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 0.0195(9) 0.0292(9) 0.0213(9) -0.0007(7) -0.0048(7) -0.0015(7) C2 0.0346(11) 0.0376(11) 0.0266(11) 0.0029(8) -0.0073(9) 0.0056(9) C3 0.0432(13) 0.0414(12) 0.0457(14) -0.0020(10) -0.0159(11) 0.0147(10) C4 0.0262(11) 0.0458(13) 0.0578(16) -0.0186(11) -0.0082(11) 0.0113(9) C5 0.0339(12) 0.0498(13) 0.0394(13) -0.0097(10) 0.0091(10) -0.0027(10) C6 0.0307(11) 0.0367(11) 0.0290(11) 0.0015(8) 0.0014(9) -0.0032(9) C7 0.0188(9) 0.0217(8) 0.0235(10) 0.0007(7) -0.0039(7) -0.0008(7) C8 0.0295(10) 0.0285(9) 0.0265(10) 0.0022(8) -0.0076(8) -0.0020(8) C9 0.0383(12) 0.0357(11) 0.0363(12) -0.0042(9) -0.0167(10) -0.0032(9) C10 0.0309(11) 0.0320(10) 0.0516(14) -0.0074(9) -0.0095(10) -0.0071(9) C11 0.0381(12) 0.0342(10) 0.0420(13) 0.0020(9) 0.0010(10) -0.0153(9) C12 0.0342(11) 0.0302(10) 0.0265(10) 0.0025(8) -0.0031(8) -0.0082(8) C13 0.0243(9) 0.0228(8) 0.0194(9) 0.0021(7) -0.0025(7) -0.0002(7) C14 0.0253(10) 0.0350(10) 0.0250(10) -0.0012(8) -0.0058(8) 0.0036(8) C15 0.0373(12) 0.0437(11) 0.0266(11) -0.0050(9) -0.0132(9) 0.0040(9) C16 0.0492(13) 0.0296(10) 0.0203(10) -0.0036(8) -0.0057(9) 0.0002(9) C17 0.0311(10) 0.0221(9) 0.0296(11) -0.0006(8) 0.0056(8) 0.0017(8) C18 0.0232(9) 0.0247(9) 0.0264(10) 0.0027(7) -0.0023(8) -0.0023(7) C19 0.0271(10) 0.0228(9) 0.0304(11) 0.0032(7) -0.0059(8) -0.0066(7) C20 0.0482(13) 0.0339(11) 0.0454(14) -0.0070(10) -0.0001(11) -0.0096(10) C21 0.0329(11) 0.0352(11) 0.0629(15) 0.0070(10) -0.0170(11) -0.0120(9) C22 0.0524(13) 0.0312(10) 0.0378(12) 0.0124(9) -0.0118(10) -0.0158(10) C23 0.0245(9) 0.0231(8) 0.0146(9) 0.0011(7) -0.0030(7) -0.0065(7) C24 0.0264(9) 0.0254(9) 0.0187(9) 0.0031(7) -0.0035(7) -0.0084(7) C25 0.0228(9) 0.0383(10) 0.0168(9) 0.0021(8) 0.0019(7) -0.0016(8) C26 0.0369(11) 0.0264(9) 0.0184(9) -0.0031(7) -0.0046(8) 0.0056(8) C27 0.0387(11) 0.0209(8) 0.0252(10) 0.0005(7) -0.0072(8) -0.0065(8) C28 0.0240(9) 0.0276(9) 0.0217(9) 0.0020(7) -0.0002(7) -0.0073(7) C29 0.0281(10) 0.0244(9) 0.0200(9) 0.0024(7) -0.0021(8) -0.0063(7) C30 0.0246(9) 0.0206(8) 0.0189(9) 0.0038(7) -0.0013(7) -0.0077(7) C31 0.0273(10) 0.0259(9) 0.0221(10) -0.0003(7) -0.0028(8) -0.0053(7) C32 0.0328(11) 0.0351(10) 0.0274(11) 0.0046(8) -0.0118(9) -0.0126(9) C33 0.0227(10) 0.0309(10) 0.0405(12) 0.0119(9) -0.0100(9) -0.0078(8) C34 0.0257(10) 0.0242(9) 0.0349(11) 0.0053(8) 0.0031(8) -0.0020(8) C35 0.0204(9) 0.0205(8) 0.0173(9) -0.0004(7) -0.0003(7) -0.0034(7) C36 0.0333(10) 0.0304(9) 0.0193(9) 0.0009(7) -0.0071(8) -0.0107(8) C37 0.0403(11) 0.0276(9) 0.0246(10) 0.0092(8) -0.0035(9) -0.0109(8) C38 0.0293(10) 0.0192(8) 0.0332(11) 0.0010(7) -0.0028(8) -0.0095(7) C39 0.0226(9) 0.0211(8) 0.0264(10) -0.0065(7) -0.0067(7) -0.0011(7) C40 0.0218(9) 0.0188(8) 0.0181(9) 0.0013(6) -0.0028(7) -0.0002(7) C41 0.0204(9) 0.0210(8) 0.0226(10) -0.0004(7) -0.0037(7) -0.0028(7) C42 0.0217(9) 0.0249(9) 0.0225(10) 0.0016(7) -0.0025(7) -0.0022(7) C43 0.0185(9) 0.0326(9) 0.0201(9) 0.0071(7) -0.0002(7) 0.0039(7) C44 0.0339(11) 0.0380(11) 0.0427(13) 0.0156(9) -0.0036(10) -0.0042(9) C45 0.0392(13) 0.0579(15) 0.0653(19) 0.0409(14) 0.0065(12) 0.0015(11) C46 0.0452(15) 0.101(2) 0.0381(16) 0.0421(16) 0.0151(12) 0.0284(15) C47 0.0469(15) 0.097(2) 0.0210(12) -0.0003(13) -0.0018(10) 0.0338(14) C48 0.0288(11) 0.0498(12) 0.0271(11) -0.0011(9) -0.0037(9) 0.0110(9) C49 0.0176(8) 0.0212(8) 0.0220(9) -0.0020(7) -0.0026(7) -0.0021(7) C50 0.0269(10) 0.0277(9) 0.0221(10) -0.0008(7) -0.0045(8) -0.0052(7) C51 0.0287(10) 0.0385(11) 0.0279(11) -0.0104(8) -0.0077(8) -0.0036(8) C52 0.0261(10) 0.0328(10) 0.0424(13) -0.0136(9) -0.0055(9) -0.0079(8) C53 0.0289(10) 0.0264(9) 0.0409(12) -0.0019(8) 0.0000(9) -0.0096(8) C54 0.0249(9) 0.0244(9) 0.0259(10) 0.0006(7) -0.0021(8) -0.0050(7) C55 0.0244(9) 0.0209(8) 0.0160(9) 0.0000(7) -0.0024(7) -0.0062(7) C56 0.0282(10) 0.0259(9) 0.0243(10) 0.0042(7) -0.0034(8) -0.0051(7) C57 0.0395(11) 0.0242(9) 0.0295(11) 0.0046(8) -0.0087(9) -0.0019(8) C58 0.0536(13) 0.0270(9) 0.0306(11) 0.0095(8) -0.0118(10) -0.0162(9) C59 0.0376(12) 0.0403(11) 0.0338(12) 0.0088(9) -0.0035(9) -0.0218(9) C60 0.0255(10) 0.0312(9) 0.0293(11) 0.0028(8) -0.0040(8) -0.0084(8) C61 0.0212(9) 0.0176(8) 0.0178(9) 0.0024(6) -0.0028(7) -0.0002(6) C62 0.0210(9) 0.0263(9) 0.0213(9) 0.0010(7) -0.0025(7) -0.0035(7) C63 0.0198(9) 0.0337(10) 0.0247(10) 0.0033(8) 0.0017(8) -0.0004(7) C64 0.0331(10) 0.0275(9) 0.0177(9) -0.0009(7) -0.0001(8) 0.0032(8) C65 0.0285(10) 0.0230(8) 0.0224(10) -0.0021(7) -0.0071(8) -0.0013(7) C66 0.0198(9) 0.0211(8) 0.0256(10) 0.0000(7) -0.0035(7) -0.0017(7) C67 0.0218(9) 0.0245(9) 0.0215(9) -0.0050(7) -0.0003(7) 0.0012(7) C68 0.0286(10) 0.0250(9) 0.0440(13) -0.0054(8) -0.0019(9) -0.0013(8) C69 0.0501(14) 0.0483(13) 0.0226(11) -0.0063(9) -0.0015(10) 0.0134(10) C70 0.0228(10) 0.0370(11) 0.0468(13) -0.0139(9) -0.0002(9) -0.0019(8) N1 0.0228(8) 0.0259(8) 0.0262(9) 0.0064(6) -0.0093(7) -0.0055(6) N2 0.0227(8) 0.0243(7) 0.0173(8) -0.0037(6) -0.0042(6) 0.0020(6) B1 0.0234(10) 0.0207(9) 0.0176(10) 0.0011(7) -0.0023(8) -0.0068(8) F1 0.0303(6) 0.0320(6) 0.0364(7) 0.0004(5) 0.0069(5) -0.0142(5) F2 0.0282(6) 0.0507(7) 0.0326(7) 0.0022(5) 0.0100(5) -0.0008(5) F3 0.0469(7) 0.0333(6) 0.0341(7) -0.0059(5) -0.0041(6) 0.0126(5) F4 0.0534(8) 0.0214(5) 0.0486(8) -0.0027(5) -0.0022(6) -0.0093(5) F5 0.0297(6) 0.0297(6) 0.0426(7) -0.0037(5) 0.0057(5) -0.0146(5) F6 0.0387(6) 0.0427(6) 0.0245(6) -0.0111(5) -0.0075(5) -0.0003(5) F7 0.0486(7) 0.0622(8) 0.0401(7) -0.0030(6) -0.0267(6) -0.0123(6) F8 0.0263(6) 0.0500(7) 0.0639(9) 0.0147(6) -0.0170(6) -0.0063(5) F9 0.0315(7) 0.0411(7) 0.0563(8) -0.0045(6) 0.0028(6) 0.0079(5) F10 0.0373(6) 0.0339(6) 0.0243(6) -0.0082(5) -0.0025(5) -0.0007(5) F11 0.0653(8) 0.0475(7) 0.0194(6) 0.0088(5) -0.0146(6) -0.0318(6) F12 0.0818(10) 0.0457(7) 0.0322(7) 0.0195(6) -0.0140(7) -0.0349(7) F13 0.0557(8) 0.0313(6) 0.0466(7) 0.0064(5) -0.0102(6) -0.0263(6) F14 0.0374(6) 0.0301(5) 0.0337(6) -0.0058(5) -0.0131(5) -0.0105(5) F15 0.0403(6) 0.0292(5) 0.0202(5) 0.0034(4) -0.0117(5) -0.0094(5) P2 0.0185(2) 0.0181(2) 0.0164(2) 0.00104(16) -0.00228(17) -0.00372(16) P1 0.0188(2) 0.0235(2) 0.0180(2) 0.00288(17) -0.00388(18) -0.00204(17) C71 0.0169(8) 0.0245(8) 0.0211(9) -0.0007(7) -0.0027(7) -0.0037(7) C72 0.0224(9) 0.0301(9) 0.0208(10) -0.0003(7) 0.0002(7) 0.0004(7) C73 0.0388(11) 0.0304(10) 0.0263(11) 0.0082(8) -0.0045(9) -0.0042(9) C74 0.0420(12) 0.0239(9) 0.0402(13) 0.0012(9) -0.0120(10) 0.0061(9) C75 0.0296(10) 0.0308(10) 0.0326(11) -0.0068(8) -0.0004(9) 0.0055(8) C76 0.0262(10) 0.0295(9) 0.0226(10) 0.0014(8) -0.0007(8) -0.0040(8) C77 0.0175(8) 0.0261(9) 0.0165(9) 0.0012(7) 0.0021(7) -0.0029(7) C78 0.0188(9) 0.0316(9) 0.0200(9) 0.0018(7) -0.0009(7) -0.0026(7) C79 0.0259(10) 0.0238(9) 0.0269(10) 0.0001(7) 0.0049(8) 0.0008(7) C80 0.0322(10) 0.0302(9) 0.0220(10) -0.0069(8) 0.0034(8) -0.0111(8) C81 0.0225(9) 0.0369(10) 0.0180(9) -0.0032(8) -0.0015(7) -0.0053(8) C82 0.0198(9) 0.0277(9) 0.0189(9) 0.0017(7) 0.0009(7) -0.0010(7) C83 0.0198(9) 0.0234(8) 0.0188(9) 0.0052(7) -0.0040(7) -0.0021(7) C84 0.0240(9) 0.0240(8) 0.0177(9) 0.0027(7) -0.0024(7) -0.0005(7) C85 0.0283(10) 0.0255(9) 0.0261(10) 0.0051(7) -0.0104(8) -0.0075(7) C86 0.0188(9) 0.0336(10) 0.0328(11) 0.0134(8) -0.0082(8) -0.0075(8) C87 0.0197(9) 0.0338(10) 0.0232(10) 0.0067(8) 0.0022(8) 0.0020(7) C88 0.0236(9) 0.0263(9) 0.0199(9) 0.0019(7) -0.0045(7) -0.0033(7) C89 0.0213(9) 0.0251(8) 0.0206(9) -0.0017(7) -0.0027(7) -0.0029(7) C90 0.0200(9) 0.0277(9) 0.0216(10) -0.0005(7) -0.0030(7) -0.0032(7) C91 0.0211(9) 0.0272(9) 0.0202(9) 0.0035(7) -0.0060(7) -0.0071(7) C92 0.0219(9) 0.0309(9) 0.0233(10) 0.0017(7) -0.0044(8) -0.0051(7) C93 0.0275(10) 0.0484(12) 0.0225(10) 0.0045(9) -0.0001(8) -0.0090(9) C94 0.0354(11) 0.0498(12) 0.0317(12) 0.0212(10) -0.0066(9) -0.0124(10) C95 0.0416(12) 0.0316(10) 0.0464(14) 0.0142(9) -0.0084(11) -0.0034(9) C96 0.0329(11) 0.0318(10) 0.0288(11) 0.0015(8) 0.0001(9) -0.0035(8) B2 0.0185(9) 0.0250(9) 0.0160(10) 0.0011(8) -0.0015(8) -0.0030(8) F16 0.0331(6) 0.0447(6) 0.0217(6) 0.0080(5) 0.0063(5) 0.0067(5) F17 0.0694(9) 0.0414(7) 0.0403(8) 0.0217(6) -0.0006(7) 0.0033(6) F18 0.0717(9) 0.0317(6) 0.0581(9) 0.0072(6) -0.0093(7) 0.0194(6) F19 0.0525(8) 0.0487(8) 0.0476(8) -0.0047(6) 0.0101(7) 0.0228(6) F20 0.0407(7) 0.0456(7) 0.0289(7) 0.0084(5) 0.0152(5) 0.0087(5) F21 0.0270(6) 0.0319(6) 0.0348(6) 0.0035(5) -0.0108(5) 0.0014(4) F22 0.0417(7) 0.0243(5) 0.0429(7) 0.0021(5) -0.0013(5) 0.0010(5) F23 0.0528(8) 0.0345(6) 0.0391(7) -0.0122(5) -0.0065(6) -0.0144(5) F24 0.0364(6) 0.0483(7) 0.0326(7) -0.0065(5) -0.0168(5) -0.0056(5) F25 0.0327(6) 0.0297(5) 0.0300(6) 0.0003(4) -0.0139(5) 0.0027(5) F26 0.0306(6) 0.0342(6) 0.0248(6) -0.0056(5) -0.0035(5) -0.0038(5) F27 0.0406(7) 0.0384(6) 0.0406(7) -0.0019(5) -0.0161(6) -0.0147(5) F28 0.0234(6) 0.0524(7) 0.0495(8) 0.0121(6) -0.0086(5) -0.0145(5) F29 0.0226(6) 0.0574(7) 0.0345(7) -0.0014(6) 0.0061(5) -0.0009(5) F30 0.0271(6) 0.0439(6) 0.0258(6) -0.0098(5) 0.0028(5) -0.0069(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 C1 C6 1.392(3) . ? C1 C2 1.399(2) . ? C1 P1 1.7870(18) . ? C2 C3 1.377(3) . ? C3 C4 1.377(3) . ? C4 C5 1.376(3) . ? C5 C6 1.383(3) . ? C7 C12 1.391(2) . ? C7 C8 1.395(2) . ? C7 P1 1.7938(16) . ? C8 C9 1.384(2) . ? C9 C10 1.379(3) . ? C10 C11 1.377(3) . ? C11 C12 1.386(2) . ? C13 C14 1.395(2) . ? C13 C18 1.397(2) . ? C13 P1 1.7895(18) . ? C14 C15 1.386(3) . ? C15 C16 1.381(3) . ? C16 C17 1.386(3) . ? C17 C18 1.382(3) . ? C19 N1 1.509(2) . ? C19 C20 1.519(3) . ? C19 C21 1.520(3) . ? C19 C22 1.522(3) . ? C23 C24 1.389(2) . ? C23 C28 1.394(2) . ? C23 B1 1.656(3) . ? C24 F1 1.3560(18) . ? C24 C25 1.379(3) . ? C25 F2 1.347(2) . ? C25 C26 1.372(2) . ? C26 F3 1.342(2) . ? C26 C27 1.375(3) . ? C27 F4 1.3506(19) . ? C27 C28 1.374(3) . ? C28 F5 1.3522(19) . ? C29 F10 1.3529(19) . ? C29 C34 1.377(3) . ? C29 C30 1.390(2) . ? C30 C31 1.386(2) . ? C30 B1 1.654(3) . ? C31 F6 1.353(2) . ? C31 C32 1.386(3) . ? C32 F7 1.349(2) . ? C32 C33 1.366(3) . ? C33 F8 1.345(2) . ? C33 C34 1.374(3) . ? C34 F9 1.347(2) . ? C35 C40 1.384(2) . ? C35 C36 1.386(2) . ? C35 B1 1.655(2) . ? C36 F11 1.3568(19) . ? C36 C37 1.381(2) . ? C37 F12 1.341(2) . ? C37 C38 1.379(3) . ? C38 F13 1.3496(18) . ? C38 C39 1.369(2) . ? C39 F14 1.3526(18) . ? C39 C40 1.384(2) . ? C40 F15 1.3506(18) . ? C41 C42 1.207(2) . ? C41 B1 1.598(2) . ? C42 C43 1.442(2) . ? C43 C48 1.390(3) . ? C43 C44 1.403(3) . ? C44 C45 1.385(3) . ? C45 C46 1.372(4) . ? C46 C47 1.375(4) . ? C47 C48 1.387(3) . ? C49 C50 1.392(2) . ? C49 C54 1.401(2) . ? C49 P2 1.7921(16) . ? C50 C51 1.387(2) . ? C51 C52 1.384(3) . ? C52 C53 1.380(3) . ? C53 C54 1.388(2) . ? C55 C60 1.390(2) . ? C55 C56 1.392(2) . ? C55 P2 1.7902(16) . ? C56 C57 1.381(2) . ? C57 C58 1.388(3) . ? C58 C59 1.375(3) . ? C59 C60 1.387(2) . ? C61 C62 1.395(2) . ? C61 C66 1.407(2) . ? C61 P2 1.7911(18) . ? C62 C63 1.384(3) . ? C63 C64 1.385(2) . ? C64 C65 1.385(3) . ? C65 C66 1.382(2) . ? C67 N2 1.506(2) . ? C67 C70 1.519(2) . ? C67 C69 1.519(3) . ? C67 C68 1.530(2) . ? N1 P1 1.6366(15) . ? N2 P2 1.6221(15) . ? C71 C76 1.377(3) . ? C71 C72 1.386(2) . ? C71 B2 1.651(3) . ? C72 F16 1.359(2) . ? C72 C73 1.373(3) . ? C73 F17 1.349(2) . ? C73 C74 1.378(3) . ? C74 F18 1.342(2) . ? C74 C75 1.369(3) . ? C75 F19 1.342(2) . ? C75 C76 1.387(3) . ? C76 F20 1.355(2) . ? C77 C82 1.389(2) . ? C77 C78 1.395(2) . ? C77 B2 1.664(2) . ? C78 F21 1.3493(19) . ? C78 C79 1.379(2) . ? C79 F22 1.347(2) . ? C79 C80 1.377(3) . ? C80 F23 1.3489(19) . ? C80 C81 1.366(3) . ? C81 F24 1.3468(19) . ? C81 C82 1.389(2) . ? C82 F25 1.3469(19) . ? C83 C88 1.378(2) . ? C83 C84 1.391(2) . ? C83 B2 1.662(2) . ? C84 F26 1.362(2) . ? C84 C85 1.383(2) . ? C85 F27 1.3493(19) . ? C85 C86 1.367(3) . ? C86 F28 1.3443(19) . ? C86 C87 1.375(3) . ? C87 F29 1.347(2) . ? C87 C88 1.385(2) . ? C88 F30 1.3628(19) . ? C89 C90 1.204(2) . ? C89 B2 1.597(3) . ? C90 C91 1.441(2) . ? C91 C92 1.396(3) . ? C91 C96 1.396(3) . ? C92 C93 1.383(2) . ? C93 C94 1.379(3) . ? C94 C95 1.384(3) . ? C95 C96 1.387(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 C6 C1 C2 119.35(18) . . ? C6 C1 P1 120.12(14) . . ? C2 C1 P1 119.26(14) . . ? C3 C2 C1 119.8(2) . . ? C2 C3 C4 120.6(2) . . ? C5 C4 C3 120.0(2) . . ? C4 C5 C6 120.4(2) . . ? C5 C6 C1 119.88(19) . . ? C12 C7 C8 119.92(15) . . ? C12 C7 P1 120.55(13) . . ? C8 C7 P1 118.87(13) . . ? C9 C8 C7 119.47(17) . . ? C10 C9 C8 120.29(18) . . ? C11 C10 C9 120.54(17) . . ? C10 C11 C12 119.95(18) . . ? C11 C12 C7 119.81(18) . . ? C14 C13 C18 119.40(16) . . ? C14 C13 P1 120.61(14) . . ? C18 C13 P1 119.77(13) . . ? C15 C14 C13 120.06(18) . . ? C16 C15 C14 120.02(18) . . ? C15 C16 C17 120.41(18) . . ? C18 C17 C16 119.94(18) . . ? C17 C18 C13 120.17(16) . . ? N1 C19 C20 110.31(15) . . ? N1 C19 C21 110.29(14) . . ? C20 C19 C21 110.68(17) . . ? N1 C19 C22 105.75(14) . . ? C20 C19 C22 110.55(16) . . ? C21 C19 C22 109.15(17) . . ? C24 C23 C28 112.51(16) . . ? C24 C23 B1 127.92(14) . . ? C28 C23 B1 119.22(15) . . ? F1 C24 C25 114.11(15) . . ? F1 C24 C23 121.40(15) . . ? C25 C24 C23 124.47(15) . . ? F2 C25 C26 119.66(17) . . ? F2 C25 C24 120.41(16) . . ? C26 C25 C24 119.93(16) . . ? F3 C26 C25 120.76(17) . . ? F3 C26 C27 120.61(16) . . ? C25 C26 C27 118.62(17) . . ? F4 C27 C28 121.19(17) . . ? F4 C27 C26 119.35(16) . . ? C28 C27 C26 119.45(16) . . ? F5 C28 C27 116.06(15) . . ? F5 C28 C23 118.94(16) . . ? C27 C28 C23 124.99(16) . . ? F10 C29 C34 116.09(16) . . ? F10 C29 C30 119.48(15) . . ? C34 C29 C30 124.43(16) . . ? C31 C30 C29 113.38(16) . . ? C31 C30 B1 127.78(16) . . ? C29 C30 B1 118.83(14) . . ? F6 C31 C30 120.72(15) . . ? F6 C31 C32 115.37(16) . . ? C30 C31 C32 123.90(18) . . ? F7 C32 C33 119.75(16) . . ? F7 C32 C31 120.44(18) . . ? C33 C32 C31 119.81(17) . . ? F8 C33 C32 120.66(17) . . ? F8 C33 C34 120.28(18) . . ? C32 C33 C34 119.05(17) . . ? F9 C34 C33 119.79(17) . . ? F9 C34 C29 120.82(17) . . ? C33 C34 C29 119.39(18) . . ? C40 C35 C36 113.39(14) . . ? C40 C35 B1 126.44(14) . . ? C36 C35 B1 120.14(14) . . ? F11 C36 C37 115.82(15) . . ? F11 C36 C35 119.14(14) . . ? C37 C36 C35 124.97(16) . . ? F12 C37 C38 119.82(15) . . ? F12 C37 C36 121.40(16) . . ? C38 C37 C36 118.74(16) . . ? F13 C38 C39 120.34(16) . . ? F13 C38 C37 120.68(16) . . ? C39 C38 C37 118.98(15) . . ? F14 C39 C38 119.98(14) . . ? F14 C39 C40 119.97(15) . . ? C38 C39 C40 120.05(15) . . ? F15 C40 C35 121.40(14) . . ? F15 C40 C39 114.81(14) . . ? C35 C40 C39 123.79(15) . . ? C42 C41 B1 175.98(17) . . ? C41 C42 C43 178.76(19) . . ? C48 C43 C44 118.60(18) . . ? C48 C43 C42 121.23(17) . . ? C44 C43 C42 120.16(17) . . ? C45 C44 C43 120.2(2) . . ? C46 C45 C44 120.4(2) . . ? C45 C46 C47 119.9(2) . . ? C46 C47 C48 120.6(2) . . ? C47 C48 C43 120.2(2) . . ? C50 C49 C54 120.00(15) . . ? C50 C49 P2 120.91(12) . . ? C54 C49 P2 118.90(13) . . ? C51 C50 C49 119.93(16) . . ? C52 C51 C50 119.75(18) . . ? C53 C52 C51 120.80(16) . . ? C52 C53 C54 120.09(17) . . ? C53 C54 C49 119.42(17) . . ? C60 C55 C56 120.15(15) . . ? C60 C55 P2 122.00(13) . . ? C56 C55 P2 117.66(12) . . ? C57 C56 C55 120.06(17) . . ? C56 C57 C58 119.49(18) . . ? C59 C58 C57 120.70(17) . . ? C58 C59 C60 120.19(17) . . ? C59 C60 C55 119.36(18) . . ? C62 C61 C66 119.68(16) . . ? C62 C61 P2 121.48(12) . . ? C66 C61 P2 118.43(13) . . ? C63 C62 C61 119.68(15) . . ? C62 C63 C64 120.37(17) . . ? C63 C64 C65 120.39(17) . . ? C66 C65 C64 120.07(16) . . ? C65 C66 C61 119.80(16) . . ? N2 C67 C70 105.94(14) . . ? N2 C67 C69 111.62(15) . . ? C70 C67 C69 109.95(16) . . ? N2 C67 C68 108.51(14) . . ? C70 C67 C68 111.04(15) . . ? C69 C67 C68 109.73(16) . . ? C19 N1 P1 129.37(12) . . ? C67 N2 P2 131.00(12) . . ? C41 B1 C30 107.33(14) . . ? C41 B1 C35 112.70(13) . . ? C30 B1 C35 106.47(13) . . ? C41 B1 C23 105.19(13) . . ? C30 B1 C23 113.87(13) . . ? C35 B1 C23 111.35(14) . . ? N2 P2 C55 113.32(8) . . ? N2 P2 C61 107.29(8) . . ? C55 P2 C61 104.07(8) . . ? N2 P2 C49 111.86(8) . . ? C55 P2 C49 108.53(8) . . ? C61 P2 C49 111.53(8) . . ? N1 P1 C1 111.85(8) . . ? N1 P1 C13 113.76(8) . . ? C1 P1 C13 109.44(8) . . ? N1 P1 C7 105.94(8) . . ? C1 P1 C7 104.26(8) . . ? C13 P1 C7 111.14(8) . . ? C76 C71 C72 113.14(15) . . ? C76 C71 B2 126.57(15) . . ? C72 C71 B2 120.26(15) . . ? F16 C72 C73 115.77(16) . . ? F16 C72 C71 119.11(15) . . ? C73 C72 C71 125.04(17) . . ? F17 C73 C72 120.83(18) . . ? F17 C73 C74 120.13(17) . . ? C72 C73 C74 119.03(17) . . ? F18 C74 C75 120.96(19) . . ? F18 C74 C73 120.10(18) . . ? C75 C74 C73 118.94(17) . . ? F19 C75 C74 120.08(17) . . ? F19 C75 C76 120.36(17) . . ? C74 C75 C76 119.56(18) . . ? F20 C76 C71 121.34(15) . . ? F20 C76 C75 114.38(16) . . ? C71 C76 C75 124.28(17) . . ? C82 C77 C78 113.10(15) . . ? C82 C77 B2 126.79(15) . . ? C78 C77 B2 119.42(14) . . ? F21 C78 C79 115.56(15) . . ? F21 C78 C77 119.79(15) . . ? C79 C78 C77 124.65(16) . . ? F22 C79 C80 119.79(16) . . ? F22 C79 C78 120.83(16) . . ? C80 C79 C78 119.38(16) . . ? F23 C80 C81 120.56(16) . . ? F23 C80 C79 120.62(17) . . ? C81 C80 C79 118.80(16) . . ? F24 C81 C80 119.63(15) . . ? F24 C81 C82 120.18(16) . . ? C80 C81 C82 120.17(16) . . ? F25 C82 C77 121.63(15) . . ? F25 C82 C81 114.56(14) . . ? C77 C82 C81 123.80(16) . . ? C88 C83 C84 112.97(15) . . ? C88 C83 B2 128.37(15) . . ? C84 C83 B2 118.65(15) . . ? F26 C84 C85 115.72(15) . . ? F26 C84 C83 119.40(14) . . ? C85 C84 C83 124.87(17) . . ? F27 C85 C86 120.17(15) . . ? F27 C85 C84 120.59(17) . . ? C86 C85 C84 119.24(16) . . ? F28 C86 C85 120.39(16) . . ? F28 C86 C87 120.82(18) . . ? C85 C86 C87 118.78(16) . . ? F29 C87 C86 119.38(16) . . ? F29 C87 C88 120.75(16) . . ? C86 C87 C88 119.84(17) . . ? F30 C88 C83 120.70(14) . . ? F30 C88 C87 115.02(16) . . ? C83 C88 C87 124.28(16) . . ? C90 C89 B2 169.94(17) . . ? C89 C90 C91 177.27(18) . . ? C92 C91 C96 118.07(16) . . ? C92 C91 C90 121.66(16) . . ? C96 C91 C90 120.26(17) . . ? C93 C92 C91 120.86(17) . . ? C94 C93 C92 120.44(19) . . ? C93 C94 C95 119.59(18) . . ? C94 C95 C96 120.22(19) . . ? C95 C96 C91 120.80(19) . . ? C89 B2 C71 113.19(15) . . ? C89 B2 C83 108.70(13) . . ? C71 B2 C83 105.94(13) . . ? C89 B2 C77 102.59(13) . . ? C71 B2 C77 112.99(13) . . ? C83 B2 C77 113.54(14) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.408 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.052 #===end