# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 ata_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Warren Piers' _publ_contact_author_email WPIERS@UCALGARY.CA _publ_section_title ; Borenium Cations Derived from BODIPY Dyes ; loop_ _publ_author_name 'Warren Piers' 'Catherine Bonnier' 'Masood Parvez' 'Ted S Sorensen' # Attachment '2-F.cif' data_Compound_II _database_code_depnum_ccdc_archive 'CCDC 687820' #----------------------------------------------------------------------------- _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SAPI91 (Fan, 1991)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #----------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H23 B2 F21 N2' _chemical_formula_weight 964.24 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' 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' B B 0.0013 0.0007 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.156(2) _cell_length_b 14.767(2) _cell_length_c 24.693(4) _cell_angle_alpha 92.013(7) _cell_angle_beta 94.606(10) _cell_angle_gamma 101.549(11) _cell_volume 3967.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32528 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9650 _exptl_absorpt_correction_T_max 0.9743 _exptl_absorpt_process_details 'SORTAV: (Blessing, 1997)' _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32528 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17599 _reflns_number_gt 10383 _reflns_threshold_expression >2sigma(I) _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^)+(0.068P)^2^+2.85P] 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 17599 _refine_ls_number_parameters 1214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1712 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.007 _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 N1 N -0.0899(2) 0.05747(17) 0.30171(12) 0.0543(7) Uani 0.768(3) 1 d P A 1 N2 N 0.0623(2) 0.04436(18) 0.23800(12) 0.0561(7) Uani 0.768(3) 1 d P A 1 B1 B 0.0130(4) 0.1015(3) 0.27461(17) 0.0631(10) Uani 0.768(3) 1 d P A 1 C4 C -0.1353(3) -0.03929(19) 0.29507(13) 0.0543(7) Uani 0.768(3) 1 d P A 1 C5 C -0.0839(3) -0.0909(2) 0.25959(14) 0.0551(8) Uani 0.768(3) 1 d P A 1 H5 H -0.1148 -0.1558 0.2555 0.066 Uiso 0.768(3) 1 calc PR A 1 C6 C 0.0111(3) -0.0522(2) 0.22952(13) 0.0556(7) Uani 0.768(3) 1 d P A 1 F1 F 0.0663(3) 0.19560(18) 0.28806(12) 0.0858(9) Uani 0.768(3) 1 d P A 1 C6' C -0.0899(2) 0.05747(17) 0.30171(12) 0.0543(7) Uani 0.232(3) 1 d P A 2 C4' C 0.0623(2) 0.04436(18) 0.23800(12) 0.0561(7) Uani 0.232(3) 1 d P A 2 C5' C 0.0130(4) 0.1015(3) 0.27461(17) 0.0631(10) Uani 0.232(3) 1 d P A 2 H5' H 0.0470 0.1657 0.2806 0.076 Uiso 0.232(3) 1 calc PR A 2 N2' N -0.1353(3) -0.03929(19) 0.29507(13) 0.0543(7) Uani 0.232(3) 1 d P A 2 B1' B -0.0839(3) -0.0909(2) 0.25959(14) 0.0551(8) Uani 0.232(3) 1 d P A 2 N1' N 0.0111(3) -0.0522(2) 0.22952(13) 0.0556(7) Uani 0.232(3) 1 d P A 2 F1' F -0.1592(9) -0.1998(6) 0.2480(4) 0.0858(9) Uani 0.232(3) 1 d P A 2 C1 C -0.1616(3) 0.0920(2) 0.33774(14) 0.0581(8) Uani 1 1 d . . . C2 C -0.2471(3) 0.0186(2) 0.35505(14) 0.0589(8) Uani 1 1 d . A . C3 C -0.2304(3) -0.0625(2) 0.32884(14) 0.0547(8) Uani 1 1 d . . . C7 C 0.0740(3) -0.0893(2) 0.19051(14) 0.0570(8) Uani 1 1 d . . . C8 C 0.1647(3) -0.0175(3) 0.17444(15) 0.0638(9) Uani 1 1 d . A . C9 C 0.1571(3) 0.0636(3) 0.20338(15) 0.0651(9) Uani 1 1 d . . . C10 C -0.1503(3) 0.1915(2) 0.35101(17) 0.0711(10) Uani 1 1 d . A . H10A H -0.2290 0.2029 0.3617 0.107 Uiso 1 1 calc R . . H10B H -0.1277 0.2265 0.3191 0.107 Uiso 1 1 calc R . . H10C H -0.0866 0.2115 0.3811 0.107 Uiso 1 1 calc R . . C11 C -0.3367(3) 0.0273(2) 0.39618(17) 0.0716(10) Uani 1 1 d . . . H11A H -0.4058 -0.0268 0.3911 0.086 Uiso 1 1 calc R A . H11B H -0.3705 0.0834 0.3896 0.086 Uiso 1 1 calc R . . C12 C -0.2801(5) 0.0333(3) 0.45447(19) 0.0976(14) Uani 1 1 d . A . H12A H -0.2480 -0.0227 0.4616 0.146 Uiso 1 1 calc R . . H12B H -0.3428 0.0386 0.4794 0.146 Uiso 1 1 calc R . . H12C H -0.2130 0.0877 0.4601 0.146 Uiso 1 1 calc R . . C13 C -0.2996(3) -0.1591(2) 0.33335(17) 0.0719(10) Uani 1 1 d . A . H13A H -0.2942 -0.1753 0.3715 0.108 Uiso 1 1 calc R . . H13B H -0.2641 -0.2018 0.3114 0.108 Uiso 1 1 calc R . . H13C H -0.3859 -0.1635 0.3202 0.108 Uiso 1 1 calc R . . C15 C 0.0450(3) -0.1868(2) 0.16906(14) 0.0633(9) Uani 1 1 d . A . H15A H 0.0089 -0.2267 0.1970 0.095 Uiso 1 1 calc R . . H15B H 0.1204 -0.2052 0.1593 0.095 Uiso 1 1 calc R . . H15C H -0.0137 -0.1931 0.1367 0.095 Uiso 1 1 calc R . . C16 C 0.2504(3) -0.0272(3) 0.13169(17) 0.0813(11) Uani 1 1 d . . . H16A H 0.2762 -0.0873 0.1347 0.098 Uiso 1 1 calc R A . H16B H 0.3249 0.0225 0.1383 0.098 Uiso 1 1 calc R . . C17 C 0.1917(4) -0.0218(4) 0.07444(18) 0.0999(14) Uani 1 1 d . A . H17A H 0.1212 -0.0734 0.0668 0.150 Uiso 1 1 calc R . . H17B H 0.2520 -0.0256 0.0481 0.150 Uiso 1 1 calc R . . H17C H 0.1642 0.0369 0.0715 0.150 Uiso 1 1 calc R . . C18 C 0.2300(4) 0.1575(3) 0.1999(2) 0.0939(14) Uani 1 1 d . A . H18A H 0.2911 0.1564 0.1736 0.141 Uiso 1 1 calc R . . H18B H 0.2719 0.1798 0.2357 0.141 Uiso 1 1 calc R . . H18C H 0.1756 0.1990 0.1880 0.141 Uiso 1 1 calc R . . N3 N 0.3781(3) 0.4829(2) 0.01436(11) 0.0519(7) Uani 0.50 1 d P . 1 B2 B 0.4657(3) 0.5558(2) 0.04298(13) 0.0521(8) Uani 0.50 1 d P B 1 N4' N 0.5885(3) 0.5719(2) 0.02645(11) 0.0549(7) Uani 0.50 1 d P . 1 F2 F 0.4380(5) 0.6087(6) 0.0743(4) 0.199(5) Uani 0.25 1 d P B 1 C24' C 0.6219(3) 0.5171(2) -0.01436(11) 0.0519(7) Uani 0.50 1 d P . 2 C23' C 0.5343(3) 0.4442(2) -0.04298(13) 0.0521(8) Uani 0.50 1 d P . 2 H23' H 0.5560 0.4078 -0.0717 0.063 Uiso 0.50 1 calc PR . 2 C22 C 0.4115(3) 0.4281(2) -0.02645(11) 0.0549(7) Uani 0.50 1 d P . 2 F2' F 0.5620(5) 0.3913(6) -0.0743(4) 0.199(5) Uani 0.25 1 d P C 2 C19 C 0.2553(3) 0.4506(2) 0.02155(13) 0.0596(8) Uani 1 1 d . . . C20 C 0.2125(3) 0.3737(3) -0.01463(15) 0.0695(10) Uani 1 1 d . . . C21 C 0.3099(3) 0.3611(2) -0.04488(14) 0.0629(9) Uani 1 1 d . . . C28 C 0.1828(3) 0.4941(3) 0.05941(16) 0.0755(10) Uani 1 1 d . . . H28A H 0.2383 0.5288 0.0892 0.113 Uiso 1 1 calc R . . H28B H 0.1227 0.4458 0.0743 0.113 Uiso 1 1 calc R . . H28C H 0.1398 0.5363 0.0396 0.113 Uiso 1 1 calc R . . C29 C 0.0926(4) 0.3105(3) -0.0166(2) 0.0970(14) Uani 1 1 d . . . H29A H 0.0309 0.3457 -0.0057 0.116 Uiso 1 1 calc R . . H29B H 0.0680 0.2860 -0.0546 0.116 Uiso 1 1 calc R . . C30 C 0.0918(5) 0.2331(4) 0.0185(3) 0.133(2) Uani 1 1 d . . . H30A H 0.1259 0.1852 0.0002 0.199 Uiso 1 1 calc R . . H30B H 0.0073 0.2073 0.0261 0.199 Uiso 1 1 calc R . . H30C H 0.1418 0.2547 0.0527 0.199 Uiso 1 1 calc R . . C31 C 0.3055(4) 0.2916(3) -0.09051(17) 0.0808(11) Uani 1 1 d . . . H31A H 0.2608 0.3095 -0.1229 0.121 Uiso 1 1 calc R . . H31B H 0.2634 0.2307 -0.0802 0.121 Uiso 1 1 calc R . . H31C H 0.3893 0.2888 -0.0985 0.121 Uiso 1 1 calc R . . N4 N 0.4164(2) 0.43476(16) 0.46668(10) 0.0421(6) Uani 0.50 1 d P D 1 B2' B 0.5301(3) 0.47341(19) 0.44740(12) 0.0402(6) Uani 0.50 1 d P . 1 C24 C 0.3865(2) 0.45857(17) 0.51779(10) 0.0431(6) Uani 0.50 1 d P . 1 F2A' F 0.5730(4) 0.4509(3) 0.40281(16) 0.0685(10) Uani 0.25 1 d P E 1 C22' C 0.5836(2) 0.56524(16) 0.53332(10) 0.0421(6) Uani 0.50 1 d P . 2 C23 C 0.4699(3) 0.52659(19) 0.55260(12) 0.0402(6) Uani 0.50 1 d P . 2 H23 H 0.4493 0.5450 0.5873 0.048 Uiso 0.50 1 calc PR . 2 N3' N 0.6135(2) 0.54143(17) 0.48221(10) 0.0431(6) Uani 0.50 1 d P . 2 F2A F 0.4270(4) 0.5491(3) 0.59719(16) 0.0685(10) Uani 0.25 1 d P F 2 C25 C 0.2711(3) 0.4072(2) 0.52603(13) 0.0510(7) Uani 1 1 d . . . C26 C 0.2286(3) 0.3502(2) 0.47898(13) 0.0515(7) Uani 1 1 d . D . C27 C 0.3175(3) 0.36744(19) 0.44214(13) 0.0479(7) Uani 1 1 d . . . C33 C 0.2072(3) 0.4131(3) 0.57617(14) 0.0636(9) Uani 1 1 d . . . H33A H 0.2453 0.3817 0.6051 0.095 Uiso 1 1 calc R . . H33B H 0.1204 0.3833 0.5688 0.095 Uiso 1 1 calc R . . H33C H 0.2138 0.4782 0.5877 0.095 Uiso 1 1 calc R . . C34 C 0.1109(3) 0.2791(2) 0.47108(15) 0.0672(9) Uani 1 1 d . . . H34A H 0.0836 0.2700 0.4318 0.081 Uiso 1 1 calc R D . H34B H 0.0467 0.3023 0.4896 0.081 Uiso 1 1 calc R . . C35 C 0.1249(3) 0.1870(2) 0.49328(18) 0.0772(11) Uani 1 1 d . D . H35A H 0.1875 0.1632 0.4746 0.116 Uiso 1 1 calc R . . H35B H 0.0463 0.1428 0.4872 0.116 Uiso 1 1 calc R . . H35C H 0.1501 0.1954 0.5324 0.116 Uiso 1 1 calc R . . C36 C 0.3119(3) 0.3257(2) 0.38643(14) 0.0607(8) Uani 1 1 d . D . H36A H 0.3612 0.2777 0.3866 0.091 Uiso 1 1 calc R . . H36B H 0.3444 0.3737 0.3620 0.091 Uiso 1 1 calc R . . H36C H 0.2264 0.2981 0.3738 0.091 Uiso 1 1 calc R . . B3 B 0.6836(3) 0.2488(2) 0.13023(13) 0.0448(7) Uani 1 1 d . . . B4 B 0.2525(3) 0.7206(2) 0.36513(13) 0.0413(7) Uani 1 1 d . . . F3 F 0.52057(15) 0.11498(12) 0.20122(7) 0.0569(4) Uani 1 1 d . . . F4 F 0.5389(2) -0.05697(13) 0.21809(9) 0.0764(6) Uani 1 1 d . . . F5 F 0.7100(2) -0.13396(13) 0.17224(10) 0.0847(7) Uani 1 1 d . . . F6 F 0.86737(19) -0.03097(15) 0.10801(9) 0.0825(6) Uani 1 1 d . . . F7 F 0.85614(16) 0.14501(14) 0.09256(8) 0.0662(5) Uani 1 1 d . . . F8 F 0.45194(15) 0.14343(14) 0.08267(7) 0.0662(5) Uani 1 1 d . . . F9 F 0.38467(18) 0.09213(16) -0.02191(8) 0.0814(6) Uani 1 1 d . . . F10 F 0.53807(18) 0.15051(16) -0.09958(7) 0.0761(6) Uani 1 1 d . . . F11 F 0.76089(17) 0.26264(15) -0.06983(7) 0.0710(5) Uani 1 1 d . . . F12 F 0.82898(15) 0.31563(13) 0.03295(7) 0.0594(5) Uani 1 1 d . . . F13 F 0.92211(15) 0.22930(13) 0.19710(8) 0.0646(5) Uani 1 1 d . . . F14 F 1.11097(16) 0.36474(14) 0.22640(8) 0.0717(5) Uani 1 1 d . . . F15 F 1.11411(17) 0.54013(14) 0.19492(8) 0.0757(6) Uani 1 1 d . . . F16 F 0.9182(2) 0.57480(14) 0.13169(9) 0.0801(6) Uani 1 1 d . . . F17 F 0.72718(16) 0.43895(12) 0.09993(7) 0.0618(5) Uani 1 1 d . . . F18 F 0.69338(14) 0.26345(11) 0.24616(6) 0.0490(4) Uani 1 1 d . . . F19 F 0.55675(17) 0.34389(14) 0.30848(7) 0.0657(5) Uani 1 1 d . . . F20 F 0.37199(17) 0.42083(14) 0.26278(8) 0.0662(5) Uani 1 1 d . . . F21 F 0.33107(18) 0.41578(16) 0.15277(8) 0.0795(6) Uani 1 1 d . . . F22 F 0.46679(17) 0.33801(15) 0.08925(7) 0.0679(5) Uani 1 1 d . . . F23 F 0.01587(16) 0.74777(13) 0.30125(8) 0.0632(5) Uani 1 1 d . . . F24 F -0.16801(18) 0.61526(18) 0.26297(9) 0.0929(7) Uani 1 1 d . . . F25 F -0.1705(2) 0.43476(18) 0.28539(11) 0.1119(10) Uani 1 1 d . . . F26 F 0.0270(2) 0.39235(13) 0.34421(11) 0.1015(8) Uani 1 1 d . . . F27 F 0.21818(18) 0.52472(11) 0.37969(8) 0.0655(5) Uani 1 1 d . . . F28 F 0.23824(16) 0.74916(13) 0.25071(7) 0.0619(5) Uani 1 1 d . . . F29 F 0.3720(2) 0.69502(17) 0.17589(8) 0.0832(6) Uani 1 1 d . . . F30 F 0.5569(2) 0.60616(16) 0.20524(8) 0.0836(6) Uani 1 1 d . . . F31 F 0.60278(17) 0.57255(14) 0.31133(8) 0.0719(5) Uani 1 1 d . . . F32 F 0.47536(16) 0.62806(12) 0.38696(7) 0.0578(4) Uani 1 1 d . . . F33 F 0.48394(15) 0.81692(12) 0.41840(7) 0.0571(4) Uani 1 1 d . . . F34 F 0.55872(17) 0.83307(14) 0.52412(8) 0.0711(5) Uani 1 1 d . . . F35 F 0.41254(19) 0.74451(15) 0.59695(7) 0.0711(5) Uani 1 1 d . . . F36 F 0.18975(18) 0.63776(13) 0.56115(7) 0.0677(5) Uani 1 1 d . . . F37 F 0.11348(15) 0.61989(11) 0.45688(7) 0.0553(4) Uani 1 1 d . . . F38 F 0.06407(15) 0.79289(11) 0.41452(7) 0.0551(4) Uani 1 1 d . . . F39 F 0.02996(19) 0.96659(13) 0.41911(9) 0.0751(6) Uani 1 1 d . . . F40 F 0.1831(2) 1.10170(12) 0.37139(10) 0.0873(7) Uani 1 1 d . . . F41 F 0.3707(2) 1.05847(13) 0.31887(10) 0.0850(7) Uani 1 1 d . . . F42 F 0.40780(16) 0.88711(12) 0.31388(8) 0.0627(5) Uani 1 1 d . . . C37 C 0.6908(2) 0.1423(2) 0.14716(11) 0.0455(7) Uani 1 1 d . . . C38 C 0.6121(3) 0.0850(2) 0.17807(12) 0.0487(7) Uani 1 1 d . . . C39 C 0.6185(3) -0.0060(2) 0.18752(13) 0.0570(8) Uani 1 1 d . . . C40 C 0.7038(3) -0.0448(2) 0.16433(15) 0.0624(9) Uani 1 1 d . . . C41 C 0.7832(3) 0.0068(2) 0.13202(14) 0.0609(9) Uani 1 1 d . . . C42 C 0.7753(3) 0.0975(2) 0.12472(12) 0.0531(7) Uani 1 1 d . . . C43 C 0.6431(2) 0.2327(2) 0.06419(11) 0.0463(7) Uani 1 1 d . . . C44 C 0.5317(3) 0.1756(2) 0.04599(12) 0.0544(8) Uani 1 1 d . . . C45 C 0.4950(3) 0.1475(2) -0.00736(13) 0.0599(8) Uani 1 1 d . . . C46 C 0.5724(3) 0.1768(2) -0.04676(12) 0.0596(8) Uani 1 1 d . . . C47 C 0.6837(3) 0.2334(2) -0.03161(12) 0.0560(8) Uani 1 1 d . . . C48 C 0.7164(3) 0.2602(2) 0.02233(12) 0.0499(7) Uani 1 1 d . . . C49 C 0.8134(2) 0.3256(2) 0.14569(11) 0.0444(6) Uani 1 1 d . . . C50 C 0.9158(3) 0.3131(2) 0.17820(12) 0.0489(7) Uani 1 1 d . . . C51 C 1.0157(3) 0.3833(2) 0.19433(12) 0.0540(8) Uani 1 1 d . . . C52 C 1.0179(3) 0.4713(2) 0.17904(13) 0.0563(8) Uani 1 1 d . . . C53 C 0.9186(3) 0.4882(2) 0.14711(13) 0.0565(8) Uani 1 1 d . . . C54 C 0.8211(3) 0.4167(2) 0.13144(12) 0.0506(7) Uani 1 1 d . . . C55 C 0.5866(2) 0.29408(19) 0.16447(11) 0.0427(6) Uani 1 1 d . . . C56 C 0.6032(2) 0.30051(19) 0.22074(11) 0.0419(6) Uani 1 1 d . . . C57 C 0.5343(3) 0.3420(2) 0.25395(11) 0.0475(7) Uani 1 1 d . . . C58 C 0.4418(3) 0.3804(2) 0.23104(13) 0.0511(7) Uani 1 1 d . . . C59 C 0.4210(3) 0.3775(2) 0.17568(13) 0.0536(8) Uani 1 1 d . . . C60 C 0.4931(3) 0.3355(2) 0.14388(12) 0.0502(7) Uani 1 1 d . . . C61 C 0.1267(3) 0.64424(18) 0.34449(12) 0.0450(7) Uani 1 1 d . . . C62 C 0.0245(3) 0.6604(2) 0.31380(13) 0.0516(7) Uani 1 1 d . . . C63 C -0.0739(3) 0.5923(3) 0.29333(14) 0.0659(9) Uani 1 1 d . . . C64 C -0.0744(4) 0.5021(3) 0.30429(16) 0.0752(12) Uani 1 1 d . . . C65 C 0.0246(4) 0.4813(2) 0.33358(16) 0.0696(10) Uani 1 1 d . . . C66 C 0.1215(3) 0.5508(2) 0.35207(14) 0.0559(8) Uani 1 1 d . . . C67 C 0.3499(2) 0.69378(18) 0.32321(11) 0.0427(6) Uani 1 1 d . . . C68 C 0.3301(3) 0.7067(2) 0.26806(12) 0.0488(7) Uani 1 1 d . . . C69 C 0.3979(3) 0.6795(2) 0.22877(12) 0.0581(8) Uani 1 1 d . . . C70 C 0.4906(3) 0.6346(2) 0.24308(13) 0.0575(8) Uani 1 1 d . . . C71 C 0.5141(3) 0.6188(2) 0.29648(13) 0.0510(7) Uani 1 1 d . . . C72 C 0.4452(3) 0.64807(19) 0.33519(12) 0.0452(7) Uani 1 1 d . . . C73 C 0.2962(2) 0.71577(18) 0.43076(11) 0.0415(6) Uani 1 1 d . . . C74 C 0.4083(3) 0.76883(19) 0.45234(12) 0.0452(7) Uani 1 1 d . . . C75 C 0.4487(3) 0.7793(2) 0.50668(13) 0.0516(7) Uani 1 1 d . . . C76 C 0.3748(3) 0.7340(2) 0.54350(12) 0.0537(8) Uani 1 1 d . . . C77 C 0.2637(3) 0.6811(2) 0.52506(13) 0.0511(7) Uani 1 1 d . . . C78 C 0.2265(3) 0.67281(18) 0.47014(12) 0.0440(6) Uani 1 1 d . . . C79 C 0.2352(2) 0.82881(18) 0.36278(11) 0.0420(6) Uani 1 1 d . . . C80 C 0.1427(3) 0.85680(19) 0.38948(12) 0.0466(7) Uani 1 1 d . . . C81 C 0.1231(3) 0.9457(2) 0.39285(13) 0.0554(8) Uani 1 1 d . . . C82 C 0.2000(3) 1.0138(2) 0.36883(15) 0.0620(9) Uani 1 1 d . . . C83 C 0.2944(3) 0.9917(2) 0.34238(14) 0.0599(8) Uani 1 1 d . . . C84 C 0.3107(3) 0.9017(2) 0.34007(13) 0.0503(7) 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 N1 0.0551(16) 0.0382(13) 0.0667(18) 0.0093(12) 0.0030(13) 0.0025(11) N2 0.0510(15) 0.0538(16) 0.0629(18) 0.0194(13) 0.0063(13) 0.0058(12) B1 0.062(2) 0.059(2) 0.071(3) 0.0240(19) 0.0057(19) 0.0145(18) C4 0.0570(17) 0.0440(15) 0.062(2) 0.0100(14) 0.0043(15) 0.0106(13) C5 0.0546(18) 0.0538(18) 0.059(2) 0.0136(16) -0.0007(16) 0.0161(15) C6 0.0487(16) 0.0629(19) 0.0557(19) 0.0146(15) -0.0007(14) 0.0124(14) F1 0.097(2) 0.0568(15) 0.091(2) 0.0109(13) -0.0112(16) -0.0072(13) C6' 0.0551(16) 0.0382(13) 0.0667(18) 0.0093(12) 0.0030(13) 0.0025(11) C4' 0.0510(15) 0.0538(16) 0.0629(18) 0.0194(13) 0.0063(13) 0.0058(12) C5' 0.062(2) 0.059(2) 0.071(3) 0.0240(19) 0.0057(19) 0.0145(18) N2' 0.0570(17) 0.0440(15) 0.062(2) 0.0100(14) 0.0043(15) 0.0106(13) B1' 0.0546(18) 0.0538(18) 0.059(2) 0.0136(16) -0.0007(16) 0.0161(15) N1' 0.0487(16) 0.0629(19) 0.0557(19) 0.0146(15) -0.0007(14) 0.0124(14) F1' 0.097(2) 0.0568(15) 0.091(2) 0.0109(13) -0.0112(16) -0.0072(13) C1 0.0566(19) 0.0437(16) 0.072(2) 0.0035(15) 0.0057(16) 0.0052(14) C2 0.0566(19) 0.0456(17) 0.072(2) 0.0025(15) 0.0074(16) 0.0033(14) C3 0.0496(17) 0.0423(16) 0.070(2) 0.0068(15) 0.0078(15) 0.0035(13) C7 0.0478(17) 0.064(2) 0.058(2) 0.0093(16) -0.0049(15) 0.0115(15) C8 0.0482(18) 0.079(2) 0.065(2) 0.0142(18) 0.0033(16) 0.0119(17) C9 0.0560(19) 0.067(2) 0.073(2) 0.0195(18) 0.0041(17) 0.0105(16) C10 0.072(2) 0.0475(18) 0.091(3) 0.0049(18) 0.003(2) 0.0054(16) C11 0.063(2) 0.0517(19) 0.098(3) -0.0001(19) 0.028(2) 0.0010(16) C12 0.124(4) 0.095(3) 0.088(3) 0.020(3) 0.038(3) 0.042(3) C13 0.070(2) 0.0460(18) 0.097(3) 0.0037(18) 0.026(2) -0.0021(16) C15 0.0577(19) 0.071(2) 0.059(2) 0.0015(17) 0.0011(16) 0.0119(16) C16 0.060(2) 0.098(3) 0.086(3) 0.012(2) 0.019(2) 0.011(2) C17 0.093(3) 0.126(4) 0.078(3) 0.017(3) 0.027(2) 0.006(3) C18 0.071(3) 0.077(3) 0.135(4) 0.028(3) 0.039(3) 0.004(2) N3 0.0536(16) 0.0654(17) 0.0392(15) 0.0071(13) 0.0059(12) 0.0165(14) B2 0.057(2) 0.061(2) 0.0438(18) -0.0011(15) 0.0174(15) 0.0207(16) N4' 0.0608(18) 0.0621(17) 0.0419(16) 0.0056(13) 0.0064(13) 0.0115(14) F2 0.086(4) 0.220(8) 0.268(10) -0.176(8) 0.024(5) 0.004(4) C24' 0.0536(16) 0.0654(17) 0.0392(15) 0.0071(13) 0.0059(12) 0.0165(14) C23' 0.057(2) 0.061(2) 0.0438(18) -0.0011(15) 0.0174(15) 0.0207(16) C22 0.0608(18) 0.0621(17) 0.0419(16) 0.0056(13) 0.0064(13) 0.0115(14) F2' 0.086(4) 0.220(8) 0.268(10) -0.176(8) 0.024(5) 0.004(4) C19 0.0572(19) 0.074(2) 0.0491(19) 0.0191(17) 0.0045(15) 0.0146(16) C20 0.065(2) 0.077(2) 0.064(2) 0.0154(19) 0.0051(18) 0.0058(18) C21 0.057(2) 0.069(2) 0.060(2) 0.0089(17) 0.0027(16) 0.0072(16) C28 0.063(2) 0.091(3) 0.077(3) 0.015(2) 0.0103(19) 0.023(2) C29 0.060(2) 0.110(4) 0.112(4) -0.007(3) 0.022(2) -0.008(2) C30 0.118(4) 0.114(4) 0.169(6) 0.039(4) 0.060(4) 0.007(3) C31 0.068(2) 0.088(3) 0.079(3) -0.012(2) 0.000(2) 0.006(2) N4 0.0404(13) 0.0402(13) 0.0461(15) 0.0106(11) 0.0052(11) 0.0072(10) B2' 0.0444(16) 0.0406(15) 0.0391(16) 0.0053(12) 0.0126(13) 0.0126(12) C24 0.0404(13) 0.0449(14) 0.0456(15) 0.0101(11) 0.0091(11) 0.0092(11) F2A' 0.080(3) 0.062(2) 0.064(2) -0.0036(18) 0.018(2) 0.0124(19) C22' 0.0404(13) 0.0402(13) 0.0461(15) 0.0106(11) 0.0052(11) 0.0072(10) C23 0.0444(16) 0.0406(15) 0.0391(16) 0.0053(12) 0.0126(13) 0.0126(12) N3' 0.0404(13) 0.0449(14) 0.0456(15) 0.0101(11) 0.0091(11) 0.0092(11) F2A 0.080(3) 0.062(2) 0.064(2) -0.0036(18) 0.018(2) 0.0124(19) C25 0.0383(15) 0.0563(18) 0.061(2) 0.0192(15) 0.0106(14) 0.0094(13) C26 0.0385(15) 0.0578(18) 0.0568(19) 0.0151(15) 0.0042(14) 0.0043(13) C27 0.0410(15) 0.0456(16) 0.0570(19) 0.0123(14) 0.0033(13) 0.0073(12) C33 0.0480(18) 0.075(2) 0.066(2) 0.0119(17) 0.0163(16) 0.0014(16) C34 0.0439(17) 0.080(2) 0.071(2) 0.0066(19) 0.0077(16) -0.0053(16) C35 0.068(2) 0.061(2) 0.098(3) -0.003(2) 0.031(2) -0.0077(17) C36 0.0517(18) 0.063(2) 0.064(2) 0.0042(16) 0.0057(15) 0.0031(15) B3 0.0406(17) 0.059(2) 0.0332(17) 0.0033(14) 0.0027(13) 0.0069(14) B4 0.0426(16) 0.0371(16) 0.0451(18) 0.0096(13) 0.0092(14) 0.0064(13) F3 0.0536(10) 0.0593(10) 0.0556(11) 0.0047(8) 0.0126(8) 0.0032(8) F4 0.0904(14) 0.0577(11) 0.0733(14) 0.0124(10) 0.0067(11) -0.0051(10) F5 0.0965(16) 0.0555(12) 0.0975(17) -0.0069(11) -0.0247(13) 0.0191(11) F6 0.0736(13) 0.0895(15) 0.0909(16) -0.0161(12) -0.0049(11) 0.0400(12) F7 0.0524(10) 0.0878(13) 0.0624(12) 0.0022(10) 0.0126(9) 0.0211(9) F8 0.0478(10) 0.0984(14) 0.0421(10) 0.0047(9) 0.0027(8) -0.0096(9) F9 0.0592(12) 0.1170(17) 0.0509(12) -0.0066(11) -0.0081(9) -0.0157(11) F10 0.0724(12) 0.1129(16) 0.0352(10) -0.0126(10) -0.0021(9) 0.0057(11) F11 0.0666(12) 0.1035(15) 0.0384(10) -0.0003(10) 0.0145(9) 0.0035(10) F12 0.0472(10) 0.0822(12) 0.0429(10) 0.0000(9) 0.0071(7) -0.0017(9) F13 0.0500(10) 0.0653(11) 0.0729(13) 0.0125(9) -0.0177(9) 0.0060(8) F14 0.0411(10) 0.0882(14) 0.0774(14) 0.0015(11) -0.0118(9) 0.0007(9) F15 0.0598(11) 0.0779(13) 0.0750(14) -0.0094(10) 0.0071(10) -0.0184(10) F16 0.0932(15) 0.0585(12) 0.0816(15) 0.0136(10) 0.0022(12) -0.0006(10) F17 0.0618(11) 0.0667(11) 0.0561(11) 0.0146(9) -0.0034(9) 0.0130(9) F18 0.0499(9) 0.0594(10) 0.0370(9) 0.0042(7) -0.0063(7) 0.0137(7) F19 0.0768(12) 0.0904(14) 0.0337(10) -0.0012(9) 0.0047(8) 0.0271(10) F20 0.0609(11) 0.0792(13) 0.0642(12) -0.0017(10) 0.0166(9) 0.0247(10) F21 0.0656(12) 0.1193(17) 0.0674(13) 0.0183(12) 0.0043(10) 0.0499(12) F22 0.0643(11) 0.1107(15) 0.0362(10) 0.0143(9) -0.0019(8) 0.0367(11) F23 0.0518(10) 0.0673(12) 0.0688(12) 0.0047(9) -0.0070(9) 0.0129(8) F24 0.0452(11) 0.140(2) 0.0805(15) -0.0238(14) -0.0027(10) -0.0025(12) F25 0.0863(16) 0.1034(17) 0.118(2) -0.0520(15) 0.0366(14) -0.0495(14) F26 0.130(2) 0.0403(11) 0.126(2) -0.0097(11) 0.0537(16) -0.0153(11) F27 0.0812(13) 0.0391(9) 0.0810(13) 0.0124(9) 0.0239(11) 0.0161(9) F28 0.0609(11) 0.0786(12) 0.0504(11) 0.0144(9) 0.0013(8) 0.0240(9) F29 0.0975(16) 0.1165(18) 0.0418(11) 0.0135(11) 0.0136(10) 0.0320(13) F30 0.0875(15) 0.1104(17) 0.0630(13) 0.0022(12) 0.0334(11) 0.0343(13) F31 0.0638(12) 0.0904(14) 0.0732(13) 0.0088(11) 0.0193(10) 0.0379(11) F32 0.0639(11) 0.0710(11) 0.0477(10) 0.0150(8) 0.0109(8) 0.0314(9) F33 0.0477(9) 0.0655(11) 0.0531(10) 0.0124(8) 0.0086(8) -0.0036(8) F34 0.0573(11) 0.0905(14) 0.0600(12) 0.0025(10) -0.0072(9) 0.0070(10) F35 0.0840(13) 0.0927(14) 0.0427(11) 0.0096(9) 0.0032(9) 0.0324(11) F36 0.0845(13) 0.0710(12) 0.0542(11) 0.0211(9) 0.0313(10) 0.0189(10) F37 0.0524(10) 0.0536(10) 0.0593(11) 0.0114(8) 0.0193(8) 0.0017(8) F38 0.0542(10) 0.0498(9) 0.0649(11) 0.0075(8) 0.0188(8) 0.0129(8) F39 0.0875(14) 0.0623(12) 0.0849(15) -0.0029(10) 0.0131(11) 0.0366(11) F40 0.1236(18) 0.0383(10) 0.1021(17) 0.0059(10) -0.0063(14) 0.0277(11) F41 0.0997(16) 0.0473(11) 0.1008(17) 0.0314(11) 0.0095(13) -0.0069(10) F42 0.0582(11) 0.0551(10) 0.0743(13) 0.0224(9) 0.0201(9) 0.0012(8) C37 0.0417(15) 0.0572(17) 0.0348(15) -0.0029(13) -0.0059(12) 0.0080(13) C38 0.0484(16) 0.0527(17) 0.0412(16) -0.0026(13) -0.0034(13) 0.0051(13) C39 0.0594(19) 0.0572(19) 0.0476(18) -0.0020(15) -0.0083(15) 0.0015(15) C40 0.069(2) 0.0497(19) 0.064(2) -0.0042(16) -0.0168(18) 0.0114(16) C41 0.0556(19) 0.070(2) 0.058(2) -0.0159(17) -0.0114(16) 0.0252(17) C42 0.0461(17) 0.067(2) 0.0444(17) -0.0003(15) -0.0027(14) 0.0112(15) C43 0.0390(15) 0.0634(18) 0.0352(15) 0.0035(13) -0.0001(12) 0.0088(13) C44 0.0450(16) 0.076(2) 0.0382(17) 0.0030(15) 0.0033(13) 0.0024(15) C45 0.0468(17) 0.079(2) 0.0454(19) -0.0020(16) -0.0043(14) -0.0018(16) C46 0.061(2) 0.081(2) 0.0336(17) -0.0048(15) -0.0015(14) 0.0117(17) C47 0.0492(17) 0.081(2) 0.0374(17) 0.0026(15) 0.0111(14) 0.0086(16) C48 0.0420(16) 0.0677(19) 0.0377(16) 0.0001(14) 0.0027(12) 0.0065(14) C49 0.0396(14) 0.0580(17) 0.0353(15) 0.0051(13) 0.0033(12) 0.0084(12) C50 0.0411(15) 0.0577(18) 0.0455(17) 0.0043(14) 0.0002(13) 0.0056(13) C51 0.0368(15) 0.077(2) 0.0452(18) 0.0010(15) -0.0012(13) 0.0058(14) C52 0.0470(17) 0.066(2) 0.0480(18) -0.0041(15) 0.0100(14) -0.0083(15) C53 0.061(2) 0.0559(19) 0.0489(18) 0.0082(15) 0.0104(15) 0.0014(15) C54 0.0460(16) 0.0639(19) 0.0405(17) 0.0049(14) 0.0012(13) 0.0087(14) C55 0.0385(14) 0.0526(16) 0.0348(15) 0.0064(12) -0.0003(11) 0.0049(12) C56 0.0381(14) 0.0486(15) 0.0371(15) 0.0059(12) -0.0019(12) 0.0055(12) C57 0.0505(16) 0.0582(18) 0.0308(15) 0.0024(13) 0.0018(12) 0.0049(14) C58 0.0457(16) 0.0562(18) 0.0522(19) 0.0031(14) 0.0102(14) 0.0097(13) C59 0.0426(16) 0.071(2) 0.0513(19) 0.0132(15) 0.0017(14) 0.0198(14) C60 0.0462(16) 0.0696(19) 0.0353(16) 0.0097(14) -0.0005(13) 0.0132(14) C61 0.0448(15) 0.0396(15) 0.0504(17) 0.0022(12) 0.0159(13) 0.0037(12) C62 0.0453(16) 0.0540(18) 0.0531(19) -0.0031(14) 0.0112(14) 0.0029(13) C63 0.0441(18) 0.087(3) 0.059(2) -0.0173(18) 0.0120(16) -0.0041(17) C64 0.065(2) 0.070(2) 0.075(3) -0.033(2) 0.031(2) -0.0264(19) C65 0.084(3) 0.0393(17) 0.080(3) -0.0116(16) 0.039(2) -0.0116(17) C66 0.0609(19) 0.0444(17) 0.063(2) 0.0000(14) 0.0250(16) 0.0044(15) C67 0.0419(15) 0.0403(14) 0.0453(16) 0.0088(12) 0.0085(12) 0.0037(11) C68 0.0463(16) 0.0551(17) 0.0455(17) 0.0105(14) 0.0053(13) 0.0093(13) C69 0.064(2) 0.071(2) 0.0380(17) 0.0087(15) 0.0089(15) 0.0093(16) C70 0.0563(19) 0.067(2) 0.052(2) 0.0019(16) 0.0216(15) 0.0131(16) C71 0.0447(16) 0.0557(17) 0.055(2) 0.0056(14) 0.0117(14) 0.0136(13) C72 0.0473(16) 0.0474(16) 0.0421(16) 0.0098(13) 0.0076(13) 0.0098(13) C73 0.0434(15) 0.0388(14) 0.0452(16) 0.0089(12) 0.0109(12) 0.0115(12) C74 0.0433(15) 0.0493(16) 0.0452(17) 0.0127(13) 0.0088(13) 0.0109(12) C75 0.0469(17) 0.0577(18) 0.0517(19) 0.0056(14) 0.0013(14) 0.0148(14) C76 0.067(2) 0.0626(19) 0.0391(17) 0.0096(14) 0.0065(15) 0.0297(16) C77 0.0627(19) 0.0486(16) 0.0496(18) 0.0160(14) 0.0211(15) 0.0208(15) C78 0.0457(16) 0.0413(15) 0.0487(17) 0.0097(12) 0.0137(13) 0.0128(12) C79 0.0427(15) 0.0386(14) 0.0435(16) 0.0084(12) 0.0009(12) 0.0053(11) C80 0.0494(16) 0.0403(15) 0.0495(17) 0.0058(13) 0.0021(13) 0.0080(12) C81 0.064(2) 0.0464(17) 0.058(2) -0.0008(14) 0.0012(16) 0.0184(15) C82 0.081(2) 0.0351(16) 0.068(2) 0.0058(15) -0.0099(18) 0.0148(15) C83 0.069(2) 0.0394(16) 0.066(2) 0.0177(15) -0.0003(17) -0.0015(15) C84 0.0485(17) 0.0465(16) 0.0543(18) 0.0135(14) 0.0042(14) 0.0044(13) _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 N1 C1 1.392(4) . ? N1 C4 1.416(4) . ? N1 B1 1.429(5) . ? N2 C9 1.404(4) . ? N2 C6 1.427(4) . ? N2 B1 1.430(5) . ? B1 F1 1.414(5) . ? C4 C5 1.373(4) . ? C4 C3 1.399(4) . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 C7 1.395(5) . ? C1 C2 1.396(4) . ? C1 C10 1.473(4) . ? C2 C3 1.394(4) . ? C2 C11 1.501(5) . ? C3 C13 1.492(4) . ? C7 C8 1.404(5) . ? C7 C15 1.480(5) . ? C8 C9 1.394(5) . ? C8 C16 1.502(5) . ? C9 C18 1.469(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.517(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.521(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N3 C19 1.386(4) . ? N3 N4' 1.390(4) 2_665 ? N3 B2 1.424(4) . ? B2 F2 1.182(6) . ? B2 N4' 1.437(4) . ? N4' C21 1.381(4) 2_665 ? N4' N3 1.390(4) 2_665 ? C24' C19 1.386(4) 2_665 ? C24' C22 1.390(4) 2_665 ? C24' C23' 1.424(4) . ? C23' C22 1.437(4) . ? C23' H23' 0.9500 . ? C22 C21 1.381(4) . ? C22 C24' 1.390(4) 2_665 ? C19 C24' 1.386(4) 2_665 ? C19 C20 1.400(5) . ? C19 C28 1.493(5) . ? C20 C21 1.405(5) . ? C20 C29 1.466(5) . ? C21 N4' 1.381(4) 2_665 ? C21 C31 1.489(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.458(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N4 C24 1.382(4) . ? N4 C27 1.408(4) . ? N4 B2' 1.411(4) . ? B2' F2A' 1.294(5) . ? B2' C24 1.432(4) 2_666 ? C24 C25 1.392(4) . ? C24 B2' 1.432(4) 2_666 ? C22' N3' 1.382(4) . ? C22' C27 1.408(4) 2_666 ? C22' C23 1.411(4) . ? C23 N3' 1.432(4) 2_666 ? C23 H23 0.9500 . ? N3' C25 1.392(4) 2_666 ? N3' C23 1.432(4) 2_666 ? C25 N3' 1.392(4) 2_666 ? C25 C26 1.402(5) . ? C25 C33 1.486(4) . ? C26 C27 1.391(4) . ? C26 C34 1.502(4) . ? C27 C22' 1.408(4) 2_666 ? C27 C36 1.479(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.517(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? B3 C55 1.652(4) . ? B3 C43 1.652(4) . ? B3 C37 1.657(5) . ? B3 C49 1.658(4) . ? B4 C61 1.647(4) . ? B4 C79 1.650(4) . ? B4 C67 1.653(4) . ? B4 C73 1.663(4) . ? F3 C38 1.350(3) . ? F4 C39 1.343(4) . ? F5 C40 1.352(4) . ? F6 C41 1.349(4) . ? F7 C42 1.356(4) . ? F8 C44 1.352(3) . ? F9 C45 1.348(3) . ? F10 C46 1.350(3) . ? F11 C47 1.352(3) . ? F12 C48 1.355(3) . ? F13 C50 1.350(3) . ? F14 C51 1.352(3) . ? F15 C52 1.344(3) . ? F16 C53 1.348(4) . ? F17 C54 1.355(3) . ? F18 C56 1.360(3) . ? F19 C57 1.348(3) . ? F20 C58 1.352(3) . ? F21 C59 1.344(3) . ? F22 C60 1.361(3) . ? F23 C62 1.358(4) . ? F24 C63 1.346(4) . ? F25 C64 1.348(4) . ? F26 C65 1.354(4) . ? F27 C66 1.357(4) . ? F28 C68 1.354(3) . ? F29 C69 1.352(4) . ? F30 C70 1.343(4) . ? F31 C71 1.345(3) . ? F32 C72 1.354(3) . ? F33 C74 1.354(3) . ? F34 C75 1.350(4) . ? F35 C76 1.347(4) . ? F36 C77 1.353(3) . ? F37 C78 1.353(3) . ? F38 C80 1.356(3) . ? F39 C81 1.349(4) . ? F40 C82 1.349(3) . ? F41 C83 1.348(4) . ? F42 C84 1.354(4) . ? C37 C38 1.387(4) . ? C37 C42 1.394(4) . ? C38 C39 1.387(4) . ? C39 C40 1.358(5) . ? C40 C41 1.374(5) . ? C41 C42 1.377(5) . ? C43 C44 1.387(4) . ? C43 C48 1.390(4) . ? C44 C45 1.372(4) . ? C45 C46 1.377(4) . ? C46 C47 1.367(4) . ? C47 C48 1.375(4) . ? C49 C50 1.389(4) . ? C49 C54 1.390(4) . ? C50 C51 1.384(4) . ? C51 C52 1.363(5) . ? C52 C53 1.377(5) . ? C53 C54 1.375(4) . ? C55 C60 1.383(4) . ? C55 C56 1.384(4) . ? C56 C57 1.376(4) . ? C57 C58 1.367(4) . ? C58 C59 1.366(4) . ? C59 C60 1.383(4) . ? C61 C62 1.383(4) . ? C61 C66 1.390(4) . ? C62 C63 1.380(4) . ? C63 C64 1.368(6) . ? C64 C65 1.364(6) . ? C65 C66 1.369(5) . ? C67 C72 1.387(4) . ? C67 C68 1.388(4) . ? C68 C69 1.374(4) . ? C69 C70 1.366(5) . ? C70 C71 1.361(4) . ? C71 C72 1.383(4) . ? C73 C78 1.386(4) . ? C73 C74 1.390(4) . ? C74 C75 1.374(4) . ? C75 C76 1.377(4) . ? C76 C77 1.361(5) . ? C77 C78 1.380(4) . ? C79 C80 1.389(4) . ? C79 C84 1.392(4) . ? C80 C81 1.374(4) . ? C81 C82 1.370(5) . ? C82 C83 1.369(5) . ? C83 C84 1.378(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 106.9(2) . . ? C1 N1 B1 131.9(3) . . ? C4 N1 B1 121.2(3) . . ? C9 N2 C6 106.2(3) . . ? C9 N2 B1 132.6(3) . . ? C6 N2 B1 121.1(3) . . ? F1 B1 N1 119.4(4) . . ? F1 B1 N2 123.5(3) . . ? N1 B1 N2 116.9(3) . . ? C5 C4 C3 132.7(3) . . ? C5 C4 N1 119.3(3) . . ? C3 C4 N1 108.0(3) . . ? C4 C5 C6 122.6(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C7 132.8(3) . . ? C5 C6 N2 118.6(3) . . ? C7 C6 N2 108.6(3) . . ? N1 C1 C2 109.1(3) . . ? N1 C1 C10 123.2(3) . . ? C2 C1 C10 127.6(3) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 C11 127.1(3) . . ? C1 C2 C11 125.1(3) . . ? C2 C3 C4 108.2(3) . . ? C2 C3 C13 128.4(3) . . ? C4 C3 C13 123.4(3) . . ? C6 C7 C8 107.9(3) . . ? C6 C7 C15 125.0(3) . . ? C8 C7 C15 127.1(3) . . ? C9 C8 C7 108.1(3) . . ? C9 C8 C16 126.7(3) . . ? C7 C8 C16 125.1(4) . . ? C8 C9 N2 109.3(3) . . ? C8 C9 C18 128.7(4) . . ? N2 C9 C18 122.0(4) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 C12 113.2(3) . . ? C2 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C2 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 C17 112.4(3) . . ? C8 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? C8 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C9 C18 H18A 109.5 . . ? C9 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C9 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 N3 N4' 108.7(3) . 2_665 ? C19 N3 B2 130.1(3) . . ? N4' N3 B2 121.2(3) 2_665 . ? F2 B2 N3 122.6(4) . . ? F2 B2 N4' 119.8(4) . . ? N3 B2 N4' 117.0(3) . . ? C21 N4' N3 108.3(3) 2_665 2_665 ? C21 N4' B2 129.9(3) 2_665 . ? N3 N4' B2 121.8(3) 2_665 . ? C19 C24' C22 108.7(3) 2_665 2_665 ? C19 C24' C23' 130.1(3) 2_665 . ? C22 C24' C23' 121.2(3) 2_665 . ? C24' C23' C22 117.0(3) . . ? C24' C23' H23' 121.5 . . ? C22 C23' H23' 121.5 . . ? C21 C22 C24' 108.3(3) . 2_665 ? C21 C22 C23' 129.9(3) . . ? C24' C22 C23' 121.8(3) 2_665 . ? C24' C19 C20 107.4(3) 2_665 . ? N3 C19 C20 107.4(3) . . ? C24' C19 C28 125.2(3) 2_665 . ? N3 C19 C28 125.2(3) . . ? C20 C19 C28 127.3(3) . . ? C19 C20 C21 107.9(3) . . ? C19 C20 C29 126.5(4) . . ? C21 C20 C29 125.3(4) . . ? N4' C21 C20 107.8(3) 2_665 . ? C22 C21 C20 107.8(3) . . ? N4' C21 C31 125.1(3) 2_665 . ? C22 C21 C31 125.1(3) . . ? C20 C21 C31 127.1(3) . . ? C19 C28 H28A 109.5 . . ? C19 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C19 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C20 113.3(4) . . ? C30 C29 H29A 108.9 . . ? C20 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? C20 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C21 C31 H31A 109.5 . . ? C21 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C21 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C24 N4 C27 107.6(2) . . ? C24 N4 B2' 122.1(2) . . ? C27 N4 B2' 130.3(3) . . ? F2A' B2' N4 127.8(3) . . ? F2A' B2' C24 114.6(3) . 2_666 ? N4 B2' C24 117.4(2) . 2_666 ? N4 C24 C25 109.0(2) . . ? N4 C24 B2' 120.5(2) . 2_666 ? C25 C24 B2' 130.6(3) . 2_666 ? N3' C22' C27 107.6(2) . 2_666 ? N3' C22' C23 122.1(2) . . ? C27 C22' C23 130.3(3) 2_666 . ? C22' C23 N3' 117.4(2) . 2_666 ? C22' C23 H23 121.3 . . ? N3' C23 H23 121.3 2_666 . ? C22' N3' C25 109.0(2) . 2_666 ? C22' N3' C23 120.5(2) . 2_666 ? C25 N3' C23 130.6(3) 2_666 2_666 ? N3' C25 C26 107.5(3) 2_666 . ? C24 C25 C26 107.5(3) . . ? N3' C25 C33 125.1(3) 2_666 . ? C24 C25 C33 125.1(3) . . ? C26 C25 C33 127.4(3) . . ? C27 C26 C25 108.1(3) . . ? C27 C26 C34 126.0(3) . . ? C25 C26 C34 125.8(3) . . ? C26 C27 C22' 107.9(3) . 2_666 ? C26 C27 N4 107.9(3) . . ? C26 C27 C36 127.6(3) . . ? C22' C27 C36 124.5(3) 2_666 . ? N4 C27 C36 124.5(3) . . ? C25 C33 H33A 109.5 . . ? C25 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C25 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 C35 112.2(3) . . ? C26 C34 H34A 109.2 . . ? C35 C34 H34A 109.2 . . ? C26 C34 H34B 109.2 . . ? C35 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C27 C36 H36A 109.5 . . ? C27 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C27 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C55 B3 C43 113.9(2) . . ? C55 B3 C37 113.0(2) . . ? C43 B3 C37 101.4(2) . . ? C55 B3 C49 101.4(2) . . ? C43 B3 C49 113.7(2) . . ? C37 B3 C49 114.0(2) . . ? C61 B4 C79 113.5(2) . . ? C61 B4 C67 101.4(2) . . ? C79 B4 C67 113.8(2) . . ? C61 B4 C73 113.1(2) . . ? C79 B4 C73 101.0(2) . . ? C67 B4 C73 114.7(2) . . ? C38 C37 C42 112.6(3) . . ? C38 C37 B3 127.4(3) . . ? C42 C37 B3 119.7(3) . . ? F3 C38 C39 114.5(3) . . ? F3 C38 C37 121.2(3) . . ? C39 C38 C37 124.3(3) . . ? F4 C39 C40 119.7(3) . . ? F4 C39 C38 120.7(3) . . ? C40 C39 C38 119.7(3) . . ? F5 C40 C39 120.5(3) . . ? F5 C40 C41 119.9(3) . . ? C39 C40 C41 119.5(3) . . ? F6 C41 C40 120.4(3) . . ? F6 C41 C42 120.8(3) . . ? C40 C41 C42 118.8(3) . . ? F7 C42 C41 116.2(3) . . ? F7 C42 C37 118.7(3) . . ? C41 C42 C37 125.1(3) . . ? C44 C43 C48 113.0(3) . . ? C44 C43 B3 119.5(2) . . ? C48 C43 B3 126.9(2) . . ? F8 C44 C45 116.2(3) . . ? F8 C44 C43 119.0(3) . . ? C45 C44 C43 124.8(3) . . ? F9 C45 C44 121.3(3) . . ? F9 C45 C46 119.5(3) . . ? C44 C45 C46 119.2(3) . . ? F10 C46 C47 120.7(3) . . ? F10 C46 C45 120.3(3) . . ? C47 C46 C45 119.0(3) . . ? F11 C47 C46 119.7(3) . . ? F11 C47 C48 120.5(3) . . ? C46 C47 C48 119.8(3) . . ? F12 C48 C47 115.0(3) . . ? F12 C48 C43 120.8(2) . . ? C47 C48 C43 124.2(3) . . ? C50 C49 C54 112.9(3) . . ? C50 C49 B3 127.0(3) . . ? C54 C49 B3 119.6(2) . . ? F13 C50 C51 115.3(3) . . ? F13 C50 C49 120.8(3) . . ? C51 C50 C49 123.9(3) . . ? F14 C51 C52 119.7(3) . . ? F14 C51 C50 119.7(3) . . ? C52 C51 C50 120.5(3) . . ? F15 C52 C51 121.0(3) . . ? F15 C52 C53 120.8(3) . . ? C51 C52 C53 118.3(3) . . ? F16 C53 C54 120.9(3) . . ? F16 C53 C52 119.4(3) . . ? C54 C53 C52 119.7(3) . . ? F17 C54 C53 116.0(3) . . ? F17 C54 C49 119.2(3) . . ? C53 C54 C49 124.8(3) . . ? C60 C55 C56 113.0(3) . . ? C60 C55 B3 127.8(2) . . ? C56 C55 B3 119.0(2) . . ? F18 C56 C57 116.2(2) . . ? F18 C56 C55 118.9(2) . . ? C57 C56 C55 124.8(3) . . ? F19 C57 C58 120.3(3) . . ? F19 C57 C56 120.4(3) . . ? C58 C57 C56 119.3(3) . . ? F20 C58 C59 120.5(3) . . ? F20 C58 C57 120.4(3) . . ? C59 C58 C57 119.1(3) . . ? F21 C59 C58 119.5(3) . . ? F21 C59 C60 120.8(3) . . ? C58 C59 C60 119.7(3) . . ? F22 C60 C59 115.1(2) . . ? F22 C60 C55 120.8(3) . . ? C59 C60 C55 124.1(3) . . ? C62 C61 C66 112.7(3) . . ? C62 C61 B4 126.9(2) . . ? C66 C61 B4 120.0(3) . . ? F23 C62 C63 114.9(3) . . ? F23 C62 C61 120.6(3) . . ? C63 C62 C61 124.6(3) . . ? F24 C63 C64 120.8(3) . . ? F24 C63 C62 119.9(4) . . ? C64 C63 C62 119.3(4) . . ? F25 C64 C65 120.7(4) . . ? F25 C64 C63 120.2(4) . . ? C65 C64 C63 119.1(3) . . ? F26 C65 C64 120.1(3) . . ? F26 C65 C66 120.2(4) . . ? C64 C65 C66 119.7(3) . . ? F27 C66 C65 116.5(3) . . ? F27 C66 C61 118.9(3) . . ? C65 C66 C61 124.6(3) . . ? C72 C67 C68 112.9(3) . . ? C72 C67 B4 127.3(2) . . ? C68 C67 B4 119.3(2) . . ? F28 C68 C69 116.4(3) . . ? F28 C68 C67 119.0(3) . . ? C69 C68 C67 124.6(3) . . ? F29 C69 C70 119.7(3) . . ? F29 C69 C68 120.5(3) . . ? C70 C69 C68 119.7(3) . . ? F30 C70 C71 120.6(3) . . ? F30 C70 C69 120.7(3) . . ? C71 C70 C69 118.6(3) . . ? F31 C71 C70 119.7(3) . . ? F31 C71 C72 120.0(3) . . ? C70 C71 C72 120.3(3) . . ? F32 C72 C71 115.5(2) . . ? F32 C72 C67 120.7(2) . . ? C71 C72 C67 123.8(3) . . ? C78 C73 C74 112.9(3) . . ? C78 C73 B4 127.2(2) . . ? C74 C73 B4 119.3(2) . . ? F33 C74 C75 115.9(3) . . ? F33 C74 C73 119.0(2) . . ? C75 C74 C73 125.0(3) . . ? F34 C75 C74 121.0(3) . . ? F34 C75 C76 120.1(3) . . ? C74 C75 C76 118.9(3) . . ? F35 C76 C77 121.4(3) . . ? F35 C76 C75 119.5(3) . . ? C77 C76 C75 119.1(3) . . ? F36 C77 C76 119.3(3) . . ? F36 C77 C78 120.5(3) . . ? C76 C77 C78 120.1(3) . . ? F37 C78 C77 114.7(2) . . ? F37 C78 C73 121.3(3) . . ? C77 C78 C73 124.0(3) . . ? C80 C79 C84 112.8(3) . . ? C80 C79 B4 119.7(2) . . ? C84 C79 B4 127.2(3) . . ? F38 C80 C81 115.9(3) . . ? F38 C80 C79 118.9(2) . . ? C81 C80 C79 125.1(3) . . ? F39 C81 C82 119.9(3) . . ? F39 C81 C80 121.2(3) . . ? C82 C81 C80 118.9(3) . . ? F40 C82 C83 120.3(3) . . ? F40 C82 C81 120.3(3) . . ? C83 C82 C81 119.4(3) . . ? F41 C83 C82 119.7(3) . . ? F41 C83 C84 120.5(3) . . ? C82 C83 C84 119.8(3) . . ? F42 C84 C83 115.4(3) . . ? F42 C84 C79 120.6(3) . . ? C83 C84 C79 124.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 B1 F1 7.4(6) . . . . ? C4 N1 B1 F1 -171.2(3) . . . . ? C1 N1 B1 N2 -177.5(3) . . . . ? C4 N1 B1 N2 3.9(5) . . . . ? C9 N2 B1 F1 -8.2(6) . . . . ? C6 N2 B1 F1 174.4(3) . . . . ? C9 N2 B1 N1 176.9(3) . . . . ? C6 N2 B1 N1 -0.5(5) . . . . ? C1 N1 C4 C5 177.4(3) . . . . ? B1 N1 C4 C5 -3.7(4) . . . . ? C1 N1 C4 C3 -2.4(3) . . . . ? B1 N1 C4 C3 176.5(3) . . . . ? C3 C4 C5 C6 179.5(3) . . . . ? N1 C4 C5 C6 -0.2(5) . . . . ? C4 C5 C6 C7 -177.7(3) . . . . ? C4 C5 C6 N2 3.6(5) . . . . ? C9 N2 C6 C5 178.8(3) . . . . ? B1 N2 C6 C5 -3.2(4) . . . . ? C9 N2 C6 C7 -0.2(3) . . . . ? B1 N2 C6 C7 177.8(3) . . . . ? C4 N1 C1 C2 2.2(4) . . . . ? B1 N1 C1 C2 -176.5(3) . . . . ? C4 N1 C1 C10 -174.1(3) . . . . ? B1 N1 C1 C10 7.2(6) . . . . ? N1 C1 C2 C3 -1.2(4) . . . . ? C10 C1 C2 C3 174.9(3) . . . . ? N1 C1 C2 C11 176.8(3) . . . . ? C10 C1 C2 C11 -7.1(6) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C11 C2 C3 C4 -178.3(3) . . . . ? C1 C2 C3 C13 -179.5(4) . . . . ? C11 C2 C3 C13 2.6(6) . . . . ? C5 C4 C3 C2 -178.1(3) . . . . ? N1 C4 C3 C2 1.7(4) . . . . ? C5 C4 C3 C13 1.1(6) . . . . ? N1 C4 C3 C13 -179.1(3) . . . . ? C5 C6 C7 C8 -178.6(3) . . . . ? N2 C6 C7 C8 0.3(3) . . . . ? C5 C6 C7 C15 3.7(5) . . . . ? N2 C6 C7 C15 -177.5(3) . . . . ? C6 C7 C8 C9 -0.2(4) . . . . ? C15 C7 C8 C9 177.5(3) . . . . ? C6 C7 C8 C16 -177.9(3) . . . . ? C15 C7 C8 C16 -0.2(5) . . . . ? C7 C8 C9 N2 0.1(4) . . . . ? C16 C8 C9 N2 177.7(3) . . . . ? C7 C8 C9 C18 -178.3(4) . . . . ? C16 C8 C9 C18 -0.7(6) . . . . ? C6 N2 C9 C8 0.1(4) . . . . ? B1 N2 C9 C8 -177.6(3) . . . . ? C6 N2 C9 C18 178.6(3) . . . . ? B1 N2 C9 C18 1.0(6) . . . . ? C3 C2 C11 C12 97.2(4) . . . . ? C1 C2 C11 C12 -80.4(5) . . . . ? C9 C8 C16 C17 -94.9(5) . . . . ? C7 C8 C16 C17 82.4(5) . . . . ? C19 N3 B2 F2 -10.2(9) . . . . ? N4' N3 B2 F2 173.1(8) 2_665 . . . ? C19 N3 B2 N4' 178.8(3) . . . . ? N4' N3 B2 N4' 2.1(5) 2_665 . . . ? F2 B2 N4' C21 5.9(9) . . . 2_665 ? N3 B2 N4' C21 177.2(3) . . . 2_665 ? F2 B2 N4' N3 -173.4(7) . . . 2_665 ? N3 B2 N4' N3 -2.1(5) . . . 2_665 ? C19 C24' C23' C22 -178.8(3) 2_665 . . . ? C22 C24' C23' C22 -2.1(5) 2_665 . . . ? C24' C23' C22 C21 -177.2(3) . . . . ? C24' C23' C22 C24' 2.1(5) . . . 2_665 ? N4' N3 C19 C24' -20(100) 2_665 . . 2_665 ? B2 N3 C19 C24' 163(100) . . . 2_665 ? N4' N3 C19 C20 1.0(4) 2_665 . . . ? B2 N3 C19 C20 -176.0(3) . . . . ? N4' N3 C19 C28 -176.3(3) 2_665 . . . ? B2 N3 C19 C28 6.6(5) . . . . ? C24' C19 C20 C21 -1.5(4) 2_665 . . . ? N3 C19 C20 C21 -1.5(4) . . . . ? C28 C19 C20 C21 175.8(3) . . . . ? C24' C19 C20 C29 171.9(4) 2_665 . . . ? N3 C19 C20 C29 171.9(4) . . . . ? C28 C19 C20 C29 -10.8(6) . . . . ? C24' C22 C21 N4' 0(100) 2_665 . . 2_665 ? C23' C22 C21 N4' 0(34) . . . 2_665 ? C24' C22 C21 C20 -0.8(4) 2_665 . . . ? C23' C22 C21 C20 178.5(3) . . . . ? C24' C22 C21 C31 176.6(3) 2_665 . . . ? C23' C22 C21 C31 -4.0(6) . . . . ? C19 C20 C21 N4' 1.5(4) . . . 2_665 ? C29 C20 C21 N4' -172.1(4) . . . 2_665 ? C19 C20 C21 C22 1.5(4) . . . . ? C29 C20 C21 C22 -172.1(4) . . . . ? C19 C20 C21 C31 -175.9(4) . . . . ? C29 C20 C21 C31 10.5(6) . . . . ? C19 C20 C29 C30 -88.8(6) . . . . ? C21 C20 C29 C30 83.6(6) . . . . ? C24 N4 B2' F2A' 173.2(3) . . . . ? C27 N4 B2' F2A' -4.5(5) . . . . ? C24 N4 B2' C24 -2.1(4) . . . 2_666 ? C27 N4 B2' C24 -179.8(3) . . . 2_666 ? C27 N4 C24 C25 0.3(3) . . . . ? B2' N4 C24 C25 -177.9(2) . . . . ? C27 N4 C24 B2' -179.7(2) . . . 2_666 ? B2' N4 C24 B2' 2.1(4) . . . 2_666 ? N3' C22' C23 N3' 2.1(4) . . . 2_666 ? C27 C22' C23 N3' 179.8(3) 2_666 . . 2_666 ? C27 C22' N3' C25 -0.3(3) 2_666 . . 2_666 ? C23 C22' N3' C25 177.9(2) . . . 2_666 ? C27 C22' N3' C23 179.7(2) 2_666 . . 2_666 ? C23 C22' N3' C23 -2.1(4) . . . 2_666 ? N4 C24 C25 N3' -111(85) . . . 2_666 ? B2' C24 C25 N3' 69(85) 2_666 . . 2_666 ? N4 C24 C25 C26 0.1(3) . . . . ? B2' C24 C25 C26 -179.9(3) 2_666 . . . ? N4 C24 C25 C33 179.9(3) . . . . ? B2' C24 C25 C33 -0.1(5) 2_666 . . . ? N3' C25 C26 C27 -0.4(3) 2_666 . . . ? C24 C25 C26 C27 -0.4(3) . . . . ? C33 C25 C26 C27 179.7(3) . . . . ? N3' C25 C26 C34 176.4(3) 2_666 . . . ? C24 C25 C26 C34 176.4(3) . . . . ? C33 C25 C26 C34 -3.5(5) . . . . ? C25 C26 C27 C22' 0.7(3) . . . 2_666 ? C34 C26 C27 C22' -176.2(3) . . . 2_666 ? C25 C26 C27 N4 0.7(3) . . . . ? C34 C26 C27 N4 -176.2(3) . . . . ? C25 C26 C27 C36 -178.1(3) . . . . ? C34 C26 C27 C36 5.1(5) . . . . ? C24 N4 C27 C26 -0.6(3) . . . . ? B2' N4 C27 C26 177.4(3) . . . . ? C24 N4 C27 C22' -114(100) . . . 2_666 ? B2' N4 C27 C22' 64(100) . . . 2_666 ? C24 N4 C27 C36 178.2(3) . . . . ? B2' N4 C27 C36 -3.7(5) . . . . ? C27 C26 C34 C35 91.4(4) . . . . ? C25 C26 C34 C35 -84.8(4) . . . . ? C55 B3 C37 C38 12.0(4) . . . . ? C43 B3 C37 C38 -110.3(3) . . . . ? C49 B3 C37 C38 127.1(3) . . . . ? C55 B3 C37 C42 -175.2(2) . . . . ? C43 B3 C37 C42 62.4(3) . . . . ? C49 B3 C37 C42 -60.2(3) . . . . ? C42 C37 C38 F3 -177.2(2) . . . . ? B3 C37 C38 F3 -4.0(4) . . . . ? C42 C37 C38 C39 2.1(4) . . . . ? B3 C37 C38 C39 175.3(3) . . . . ? F3 C38 C39 F4 -0.8(4) . . . . ? C37 C38 C39 F4 179.8(3) . . . . ? F3 C38 C39 C40 177.3(3) . . . . ? C37 C38 C39 C40 -2.1(5) . . . . ? F4 C39 C40 F5 -0.7(5) . . . . ? C38 C39 C40 F5 -178.7(3) . . . . ? F4 C39 C40 C41 178.4(3) . . . . ? C38 C39 C40 C41 0.4(5) . . . . ? F5 C40 C41 F6 0.1(5) . . . . ? C39 C40 C41 F6 -179.0(3) . . . . ? F5 C40 C41 C42 -179.8(3) . . . . ? C39 C40 C41 C42 1.1(5) . . . . ? F6 C41 C42 F7 -0.1(4) . . . . ? C40 C41 C42 F7 179.8(3) . . . . ? F6 C41 C42 C37 179.2(3) . . . . ? C40 C41 C42 C37 -1.0(5) . . . . ? C38 C37 C42 F7 178.6(2) . . . . ? B3 C37 C42 F7 4.9(4) . . . . ? C38 C37 C42 C41 -0.6(4) . . . . ? B3 C37 C42 C41 -174.3(3) . . . . ? C55 B3 C43 C44 -59.6(4) . . . . ? C37 B3 C43 C44 62.1(3) . . . . ? C49 B3 C43 C44 -175.1(3) . . . . ? C55 B3 C43 C48 130.1(3) . . . . ? C37 B3 C43 C48 -108.2(3) . . . . ? C49 B3 C43 C48 14.6(4) . . . . ? C48 C43 C44 F8 179.6(3) . . . . ? B3 C43 C44 F8 8.0(4) . . . . ? C48 C43 C44 C45 0.3(5) . . . . ? B3 C43 C44 C45 -171.3(3) . . . . ? F8 C44 C45 F9 1.0(5) . . . . ? C43 C44 C45 F9 -179.7(3) . . . . ? F8 C44 C45 C46 -179.1(3) . . . . ? C43 C44 C45 C46 0.2(6) . . . . ? F9 C45 C46 F10 0.3(5) . . . . ? C44 C45 C46 F10 -179.6(3) . . . . ? F9 C45 C46 C47 179.6(3) . . . . ? C44 C45 C46 C47 -0.3(5) . . . . ? F10 C46 C47 F11 -0.8(5) . . . . ? C45 C46 C47 F11 179.9(3) . . . . ? F10 C46 C47 C48 179.3(3) . . . . ? C45 C46 C47 C48 0.0(5) . . . . ? F11 C47 C48 F12 -0.5(5) . . . . ? C46 C47 C48 F12 179.4(3) . . . . ? F11 C47 C48 C43 -179.4(3) . . . . ? C46 C47 C48 C43 0.6(5) . . . . ? C44 C43 C48 F12 -179.5(3) . . . . ? B3 C43 C48 F12 -8.6(5) . . . . ? C44 C43 C48 C47 -0.7(5) . . . . ? B3 C43 C48 C47 170.2(3) . . . . ? C55 B3 C49 C50 110.2(3) . . . . ? C43 B3 C49 C50 -127.1(3) . . . . ? C37 B3 C49 C50 -11.5(4) . . . . ? C55 B3 C49 C54 -61.1(3) . . . . ? C43 B3 C49 C54 61.6(4) . . . . ? C37 B3 C49 C54 177.2(3) . . . . ? C54 C49 C50 F13 178.1(3) . . . . ? B3 C49 C50 F13 6.3(5) . . . . ? C54 C49 C50 C51 -0.7(4) . . . . ? B3 C49 C50 C51 -172.5(3) . . . . ? F13 C50 C51 F14 0.6(4) . . . . ? C49 C50 C51 F14 179.5(3) . . . . ? F13 C50 C51 C52 -178.1(3) . . . . ? C49 C50 C51 C52 0.8(5) . . . . ? F14 C51 C52 F15 0.7(5) . . . . ? C50 C51 C52 F15 179.4(3) . . . . ? F14 C51 C52 C53 -178.9(3) . . . . ? C50 C51 C52 C53 -0.2(5) . . . . ? F15 C52 C53 F16 0.0(5) . . . . ? C51 C52 C53 F16 179.6(3) . . . . ? F15 C52 C53 C54 -179.9(3) . . . . ? C51 C52 C53 C54 -0.3(5) . . . . ? F16 C53 C54 F17 0.3(4) . . . . ? C52 C53 C54 F17 -179.8(3) . . . . ? F16 C53 C54 C49 -179.6(3) . . . . ? C52 C53 C54 C49 0.3(5) . . . . ? C50 C49 C54 F17 -179.7(3) . . . . ? B3 C49 C54 F17 -7.2(4) . . . . ? C50 C49 C54 C53 0.2(4) . . . . ? B3 C49 C54 C53 172.7(3) . . . . ? C43 B3 C55 C60 -13.8(4) . . . . ? C37 B3 C55 C60 -128.9(3) . . . . ? C49 B3 C55 C60 108.7(3) . . . . ? C43 B3 C55 C56 172.4(2) . . . . ? C37 B3 C55 C56 57.4(3) . . . . ? C49 B3 C55 C56 -65.0(3) . . . . ? C60 C55 C56 F18 -179.2(2) . . . . ? B3 C55 C56 F18 -4.6(4) . . . . ? C60 C55 C56 C57 0.9(4) . . . . ? B3 C55 C56 C57 175.5(3) . . . . ? F18 C56 C57 F19 -0.6(4) . . . . ? C55 C56 C57 F19 179.3(3) . . . . ? F18 C56 C57 C58 -179.8(2) . . . . ? C55 C56 C57 C58 0.1(4) . . . . ? F19 C57 C58 F20 0.1(4) . . . . ? C56 C57 C58 F20 179.3(3) . . . . ? F19 C57 C58 C59 -179.9(3) . . . . ? C56 C57 C58 C59 -0.7(4) . . . . ? F20 C58 C59 F21 0.5(5) . . . . ? C57 C58 C59 F21 -179.4(3) . . . . ? F20 C58 C59 C60 -179.7(3) . . . . ? C57 C58 C59 C60 0.3(5) . . . . ? F21 C59 C60 F22 1.1(4) . . . . ? C58 C59 C60 F22 -178.6(3) . . . . ? F21 C59 C60 C55 -179.5(3) . . . . ? C58 C59 C60 C55 0.8(5) . . . . ? C56 C55 C60 F22 178.0(3) . . . . ? B3 C55 C60 F22 4.0(5) . . . . ? C56 C55 C60 C59 -1.3(4) . . . . ? B3 C55 C60 C59 -175.4(3) . . . . ? C79 B4 C61 C62 17.8(4) . . . . ? C67 B4 C61 C62 -104.5(3) . . . . ? C73 B4 C61 C62 132.2(3) . . . . ? C79 B4 C61 C66 -170.0(3) . . . . ? C67 B4 C61 C66 67.6(3) . . . . ? C73 B4 C61 C66 -55.6(3) . . . . ? C66 C61 C62 F23 -178.3(3) . . . . ? B4 C61 C62 F23 -5.6(4) . . . . ? C66 C61 C62 C63 1.1(4) . . . . ? B4 C61 C62 C63 173.7(3) . . . . ? F23 C62 C63 F24 0.7(4) . . . . ? C61 C62 C63 F24 -178.7(3) . . . . ? F23 C62 C63 C64 -179.3(3) . . . . ? C61 C62 C63 C64 1.3(5) . . . . ? F24 C63 C64 F25 -1.0(5) . . . . ? C62 C63 C64 F25 179.0(3) . . . . ? F24 C63 C64 C65 177.7(3) . . . . ? C62 C63 C64 C65 -2.3(5) . . . . ? F25 C64 C65 F26 -0.3(5) . . . . ? C63 C64 C65 F26 -179.0(3) . . . . ? F25 C64 C65 C66 179.6(3) . . . . ? C63 C64 C65 C66 0.9(5) . . . . ? F26 C65 C66 F27 1.5(5) . . . . ? C64 C65 C66 F27 -178.3(3) . . . . ? F26 C65 C66 C61 -178.4(3) . . . . ? C64 C65 C66 C61 1.8(5) . . . . ? C62 C61 C66 F27 177.5(3) . . . . ? B4 C61 C66 F27 4.2(4) . . . . ? C62 C61 C66 C65 -2.6(4) . . . . ? B4 C61 C66 C65 -175.9(3) . . . . ? C61 B4 C67 C72 -105.7(3) . . . . ? C79 B4 C67 C72 132.1(3) . . . . ? C73 B4 C67 C72 16.5(4) . . . . ? C61 B4 C67 C68 65.8(3) . . . . ? C79 B4 C67 C68 -56.4(3) . . . . ? C73 B4 C67 C68 -172.0(2) . . . . ? C72 C67 C68 F28 178.9(2) . . . . ? B4 C67 C68 F28 6.2(4) . . . . ? C72 C67 C68 C69 -1.2(4) . . . . ? B4 C67 C68 C69 -173.9(3) . . . . ? F28 C68 C69 F29 -0.1(4) . . . . ? C67 C68 C69 F29 -180.0(3) . . . . ? F28 C68 C69 C70 -178.7(3) . . . . ? C67 C68 C69 C70 1.4(5) . . . . ? F29 C69 C70 F30 0.4(5) . . . . ? C68 C69 C70 F30 179.0(3) . . . . ? F29 C69 C70 C71 -179.2(3) . . . . ? C68 C69 C70 C71 -0.6(5) . . . . ? F30 C70 C71 F31 -1.4(5) . . . . ? C69 C70 C71 F31 178.2(3) . . . . ? F30 C70 C71 C72 -179.8(3) . . . . ? C69 C70 C71 C72 -0.2(5) . . . . ? F31 C71 C72 F32 1.0(4) . . . . ? C70 C71 C72 F32 179.4(3) . . . . ? F31 C71 C72 C67 -178.1(3) . . . . ? C70 C71 C72 C67 0.3(5) . . . . ? C68 C67 C72 F32 -178.7(2) . . . . ? B4 C67 C72 F32 -6.7(4) . . . . ? C68 C67 C72 C71 0.4(4) . . . . ? B4 C67 C72 C71 172.3(3) . . . . ? C61 B4 C73 C78 -16.2(4) . . . . ? C79 B4 C73 C78 105.4(3) . . . . ? C67 B4 C73 C78 -131.8(3) . . . . ? C61 B4 C73 C74 172.7(2) . . . . ? C79 B4 C73 C74 -65.6(3) . . . . ? C67 B4 C73 C74 57.1(3) . . . . ? C78 C73 C74 F33 -178.0(2) . . . . ? B4 C73 C74 F33 -5.7(4) . . . . ? C78 C73 C74 C75 -0.1(4) . . . . ? B4 C73 C74 C75 172.2(3) . . . . ? F33 C74 C75 F34 -1.4(4) . . . . ? C73 C74 C75 F34 -179.4(3) . . . . ? F33 C74 C75 C76 178.5(3) . . . . ? C73 C74 C75 C76 0.5(5) . . . . ? F34 C75 C76 F35 0.6(4) . . . . ? C74 C75 C76 F35 -179.2(3) . . . . ? F34 C75 C76 C77 179.3(3) . . . . ? C74 C75 C76 C77 -0.6(4) . . . . ? F35 C76 C77 F36 -0.2(4) . . . . ? C75 C76 C77 F36 -178.8(3) . . . . ? F35 C76 C77 C78 178.9(3) . . . . ? C75 C76 C77 C78 0.3(4) . . . . ? F36 C77 C78 F37 0.4(4) . . . . ? C76 C77 C78 F37 -178.7(2) . . . . ? F36 C77 C78 C73 179.2(2) . . . . ? C76 C77 C78 C73 0.1(4) . . . . ? C74 C73 C78 F37 178.6(2) . . . . ? B4 C73 C78 F37 7.0(4) . . . . ? C74 C73 C78 C77 -0.2(4) . . . . ? B4 C73 C78 C77 -171.8(3) . . . . ? C61 B4 C79 C80 54.9(3) . . . . ? C67 B4 C79 C80 170.2(3) . . . . ? C73 B4 C79 C80 -66.4(3) . . . . ? C61 B4 C79 C84 -130.9(3) . . . . ? C67 B4 C79 C84 -15.7(4) . . . . ? C73 B4 C79 C84 107.7(3) . . . . ? C84 C79 C80 F38 -178.6(2) . . . . ? B4 C79 C80 F38 -3.6(4) . . . . ? C84 C79 C80 C81 1.5(4) . . . . ? B4 C79 C80 C81 176.5(3) . . . . ? F38 C80 C81 F39 -0.7(4) . . . . ? C79 C80 C81 F39 179.2(3) . . . . ? F38 C80 C81 C82 179.4(3) . . . . ? C79 C80 C81 C82 -0.7(5) . . . . ? F39 C81 C82 F40 0.1(5) . . . . ? C80 C81 C82 F40 179.9(3) . . . . ? F39 C81 C82 C83 179.9(3) . . . . ? C80 C81 C82 C83 -0.3(5) . . . . ? F40 C82 C83 F41 0.1(5) . . . . ? C81 C82 C83 F41 -179.7(3) . . . . ? F40 C82 C83 C84 180.0(3) . . . . ? C81 C82 C83 C84 0.2(5) . . . . ? F41 C83 C84 F42 1.0(4) . . . . ? C82 C83 C84 F42 -178.9(3) . . . . ? F41 C83 C84 C79 -179.3(3) . . . . ? C82 C83 C84 C79 0.9(5) . . . . ? C80 C79 C84 F42 178.1(3) . . . . ? B4 C79 C84 F42 3.6(5) . . . . ? C80 C79 C84 C83 -1.6(4) . . . . ? B4 C79 C84 C83 -176.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.287 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.048 # start Validation Reply Form _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; _vrf_PLAT245_Compound_I ; PROBLEM: U(iso) H23' Smaller than U(eq) F2' by ... 0.14 AngSq RESPONSE: Due to disorder. The anions lie about inversion centers. However, the model was refined with appropriate constrains. ; # end Validation Reply Form data_Compound_III _database_code_depnum_ccdc_archive 'CCDC 687821' #----------------------------------------------------------------------------- _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1991)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #----------------------------------------------------------------------------- _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H24 B2 F20 N2' _chemical_formula_weight 946.24 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' 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' B B 0.0013 0.0007 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.085(2) _cell_length_b 14.768(3) _cell_length_c 24.420(6) _cell_angle_alpha 92.761(10) _cell_angle_beta 95.149(14) _cell_angle_gamma 100.781(12) _cell_volume 3902.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 26433 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 25.4 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_type 'Multi-scan method' _exptl_absorpt_correction_T_min 0.9732 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details 'SORTAV: (Blessing, 1997)' _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26433 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.38 _reflns_number_total 14169 _reflns_number_gt 9780 _reflns_threshold_expression >2sigma(I) _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^)+(0.0512P)^2^+2.2502P] 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 14169 _refine_ls_number_parameters 1190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.009 _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 N1 N -0.0854(2) 0.05657(16) 0.30093(10) 0.0479(7) Uani 0.702(16) 1 d P A 1 N2 N 0.0648(2) 0.04374(17) 0.23687(10) 0.0470(7) Uani 0.702(16) 1 d P A 1 B1 B 0.0127(3) 0.0991(2) 0.27272(14) 0.0516(9) Uani 0.702(16) 1 d P A 1 H1 H 0.0430 0.1638 0.2778 0.062 Uiso 0.702(16) 1 calc PR A 1 C4 C -0.1309(2) -0.03946(16) 0.29308(11) 0.0413(7) Uani 0.702(16) 1 d P A 1 C5 C -0.0802(3) -0.0927(2) 0.25654(12) 0.0446(7) Uani 0.702(16) 1 d P A 1 H5 H -0.1110 -0.1573 0.2513 0.054 Uiso 0.702(16) 1 calc PR A 1 C6 C 0.0153(2) -0.05190(17) 0.22767(11) 0.0416(7) Uani 0.702(16) 1 d P A 1 C6' C -0.0854(2) 0.05657(16) 0.30093(10) 0.0479(7) Uani 0.298(16) 1 d P A 2 C4' C 0.0648(2) 0.04374(17) 0.23687(10) 0.0470(7) Uani 0.298(16) 1 d P A 2 C5' C 0.0127(3) 0.0991(2) 0.27272(14) 0.0516(9) Uani 0.298(16) 1 d P A 2 H5' H 0.0430 0.1638 0.2778 0.062 Uiso 0.298(16) 1 calc PR A 2 N2' N -0.1309(2) -0.03946(16) 0.29308(11) 0.0413(7) Uani 0.298(16) 1 d P A 2 B1' B -0.0802(3) -0.0927(2) 0.25654(12) 0.0446(7) Uani 0.298(16) 1 d P A 2 H1' H -0.1110 -0.1573 0.2513 0.054 Uiso 0.298(16) 1 calc PR A 2 N1' N 0.0153(2) -0.05190(17) 0.22767(11) 0.0416(7) Uani 0.298(16) 1 d P A 2 C1 C -0.1577(3) 0.09262(19) 0.33813(13) 0.0522(7) Uani 1 1 d . . . C2 C -0.2431(3) 0.01833(19) 0.35487(13) 0.0498(7) Uani 1 1 d . A . C3 C -0.2260(2) -0.06214(18) 0.32744(12) 0.0442(7) Uani 1 1 d . . . C7 C 0.0803(2) -0.0884(2) 0.18788(12) 0.0461(7) Uani 1 1 d . . . C8 C 0.1694(3) -0.0173(2) 0.17245(12) 0.0500(7) Uani 1 1 d . A . C9 C 0.1600(3) 0.0648(2) 0.20226(13) 0.0535(8) Uani 1 1 d . . . C10 C -0.1500(3) 0.1898(2) 0.34999(15) 0.0618(9) Uani 1 1 d . A . H10A H -0.2317 0.2053 0.3419 0.093 Uiso 1 1 calc R . . H10B H -0.0918 0.2246 0.3271 0.093 Uiso 1 1 calc R . . H10C H -0.1213 0.2058 0.3890 0.093 Uiso 1 1 calc R . . C11 C -0.3319(3) 0.0276(2) 0.39661(14) 0.0598(9) Uani 1 1 d . . . H11A H -0.4007 -0.0265 0.3913 0.072 Uiso 1 1 calc R A . H11B H -0.3670 0.0835 0.3902 0.072 Uiso 1 1 calc R . . C12 C -0.2731(4) 0.0342(3) 0.45568(15) 0.0775(11) Uani 1 1 d . A . H12A H -0.2352 -0.0198 0.4619 0.116 Uiso 1 1 calc R . . H12B H -0.3365 0.0360 0.4810 0.116 Uiso 1 1 calc R . . H12C H -0.2098 0.0906 0.4622 0.116 Uiso 1 1 calc R . . C13 C -0.2945(3) -0.15809(19) 0.33021(14) 0.0553(8) Uani 1 1 d . A . H13A H -0.3299 -0.1641 0.3655 0.083 Uiso 1 1 calc R . . H13B H -0.2378 -0.2012 0.3270 0.083 Uiso 1 1 calc R . . H13C H -0.3608 -0.1723 0.3000 0.083 Uiso 1 1 calc R . . C15 C 0.0495(3) -0.1860(2) 0.16565(12) 0.0509(7) Uani 1 1 d . A . H15A H 0.0260 -0.2261 0.1953 0.076 Uiso 1 1 calc R . . H15B H 0.1216 -0.2028 0.1503 0.076 Uiso 1 1 calc R . . H15C H -0.0194 -0.1937 0.1367 0.076 Uiso 1 1 calc R . . C16 C 0.2557(3) -0.0269(2) 0.12947(14) 0.0639(9) Uani 1 1 d . . . H16A H 0.2840 -0.0863 0.1327 0.077 Uiso 1 1 calc R A . H16B H 0.3290 0.0235 0.1363 0.077 Uiso 1 1 calc R . . C17 C 0.1950(4) -0.0235(3) 0.07129(15) 0.0790(11) Uani 1 1 d . A . H17A H 0.1250 -0.0753 0.0636 0.118 Uiso 1 1 calc R . . H17B H 0.2553 -0.0278 0.0447 0.118 Uiso 1 1 calc R . . H17C H 0.1657 0.0348 0.0681 0.118 Uiso 1 1 calc R . . C18 C 0.2247(4) 0.1581(2) 0.1978(2) 0.0929(14) Uani 1 1 d . A . H18A H 0.2903 0.1575 0.1735 0.139 Uiso 1 1 calc R . . H18B H 0.2610 0.1851 0.2344 0.139 Uiso 1 1 calc R . . H18C H 0.1668 0.1952 0.1824 0.139 Uiso 1 1 calc R . . N3 N 0.3797(2) 0.48437(17) 0.01439(9) 0.0386(5) Uani 0.50 1 d P . 1 B2 B 0.4662(3) 0.5583(2) 0.04176(12) 0.0411(7) Uani 0.50 1 d P B 1 H2 H 0.4442 0.5969 0.0699 0.049 Uiso 0.50 1 calc PR B 1 N4' N 0.5864(2) 0.57242(16) 0.02576(10) 0.0414(6) Uani 0.50 1 d P . 1 C24' C 0.6203(2) 0.51563(17) -0.01439(9) 0.0386(5) Uani 0.50 1 d P . 2 C23' C 0.5338(3) 0.4417(2) -0.04176(12) 0.0411(7) Uani 0.50 1 d P . 2 H23' H 0.5558 0.4031 -0.0699 0.049 Uiso 0.50 1 calc PR . 2 C22 C 0.4136(2) 0.42758(16) -0.02576(10) 0.0414(6) Uani 0.50 1 d P . 2 C19 C 0.2549(2) 0.4518(2) 0.02232(11) 0.0447(7) Uani 1 1 d . . . C20 C 0.2130(3) 0.3735(2) -0.01318(12) 0.0523(8) Uani 1 1 d . . . C21 C 0.3090(3) 0.3581(2) -0.04449(12) 0.0524(8) Uani 1 1 d . . . C28 C 0.1837(3) 0.5003(2) 0.05796(15) 0.0637(9) Uani 1 1 d . . . H28A H 0.2401 0.5386 0.0869 0.096 Uiso 1 1 calc R . . H28B H 0.1244 0.4549 0.0748 0.096 Uiso 1 1 calc R . . H28C H 0.1393 0.5396 0.0359 0.096 Uiso 1 1 calc R . . C29 C 0.0874(3) 0.3132(2) -0.01689(15) 0.0667(10) Uani 1 1 d . . . H29A H 0.0617 0.2895 -0.0556 0.080 Uiso 1 1 calc R . . H29B H 0.0272 0.3503 -0.0053 0.080 Uiso 1 1 calc R . . C30 C 0.0867(4) 0.2331(3) 0.0191(2) 0.0966(14) Uani 1 1 d . . . H30A H 0.1439 0.1950 0.0068 0.145 Uiso 1 1 calc R . . H30B H 0.0032 0.1957 0.0166 0.145 Uiso 1 1 calc R . . H30C H 0.1125 0.2565 0.0574 0.145 Uiso 1 1 calc R . . C31 C 0.3027(3) 0.2933(3) -0.09208(14) 0.0698(10) Uani 1 1 d . . . H31A H 0.2593 0.3152 -0.1240 0.105 Uiso 1 1 calc R . . H31B H 0.2583 0.2324 -0.0841 0.105 Uiso 1 1 calc R . . H31C H 0.3865 0.2889 -0.1001 0.105 Uiso 1 1 calc R . . N4 N 0.41413(19) 0.43546(15) 0.46653(9) 0.0335(5) Uani 0.50 1 d P C 1 B2' B 0.5275(2) 0.47177(18) 0.44655(11) 0.0346(6) Uani 0.50 1 d P . 1 H2' H 0.5457 0.4526 0.4110 0.042 Uiso 0.50 1 calc PR . 1 C24 C 0.38716(19) 0.46250(15) 0.51879(9) 0.0342(5) Uani 0.50 1 d P . 1 C22' C 0.58587(19) 0.56454(15) 0.53347(9) 0.0335(5) Uani 0.50 1 d P . 2 C23 C 0.4725(2) 0.52823(18) 0.55345(11) 0.0346(6) Uani 0.50 1 d P . 2 H23 H 0.4543 0.5474 0.5890 0.042 Uiso 0.50 1 calc PR . 2 N3' N 0.61284(19) 0.53750(15) 0.48121(9) 0.0342(5) Uani 0.50 1 d P . 2 C25 C 0.2706(2) 0.41272(18) 0.52728(11) 0.0381(6) Uani 1 1 d . . . C26 C 0.2259(2) 0.35447(18) 0.48035(11) 0.0391(6) Uani 1 1 d . C . C27 C 0.3136(2) 0.36884(17) 0.44237(11) 0.0374(6) Uani 1 1 d . . . C33 C 0.2091(3) 0.4221(2) 0.57837(12) 0.0524(7) Uani 1 1 d . . . H33A H 0.2084 0.3665 0.5988 0.079 Uiso 1 1 calc R . . H33B H 0.1241 0.4299 0.5686 0.079 Uiso 1 1 calc R . . H33C H 0.2543 0.4762 0.6014 0.079 Uiso 1 1 calc R . . C34 C 0.1076(2) 0.2850(2) 0.47309(12) 0.0501(7) Uani 1 1 d . . . H34A H 0.0775 0.2754 0.4334 0.060 Uiso 1 1 calc R C . H34B H 0.0446 0.3095 0.4925 0.060 Uiso 1 1 calc R . . C35 C 0.1225(3) 0.1926(2) 0.49514(14) 0.0602(9) Uani 1 1 d . C . H35A H 0.1863 0.1688 0.4767 0.090 Uiso 1 1 calc R . . H35B H 0.0440 0.1485 0.4880 0.090 Uiso 1 1 calc R . . H35C H 0.1468 0.2009 0.5349 0.090 Uiso 1 1 calc R . . C36 C 0.3057(3) 0.32570(19) 0.38582(11) 0.0453(7) Uani 1 1 d . C . H36A H 0.3469 0.2725 0.3865 0.068 Uiso 1 1 calc R . . H36B H 0.3461 0.3709 0.3619 0.068 Uiso 1 1 calc R . . H36C H 0.2188 0.3051 0.3716 0.068 Uiso 1 1 calc R . . B3 B 0.6808(3) 0.2523(2) 0.13289(12) 0.0362(7) Uani 1 1 d . . . B4 B 0.2598(3) 0.7235(2) 0.36464(12) 0.0358(7) Uani 1 1 d . . . F3 F 0.51803(13) 0.12075(10) 0.20390(6) 0.0453(4) Uani 1 1 d . . . F4 F 0.53537(16) -0.05199(11) 0.21932(7) 0.0582(4) Uani 1 1 d . . . F5 F 0.70690(16) -0.13077(11) 0.17274(8) 0.0634(5) Uani 1 1 d . . . F6 F 0.86593(15) -0.02919(12) 0.10935(8) 0.0623(5) Uani 1 1 d . . . F7 F 0.85505(14) 0.14745(11) 0.09499(6) 0.0509(4) Uani 1 1 d . . . F8 F 0.44657(13) 0.14960(12) 0.08381(6) 0.0520(4) Uani 1 1 d . . . F9 F 0.37728(14) 0.09840(13) -0.02256(7) 0.0619(5) Uani 1 1 d . . . F10 F 0.53164(15) 0.15294(12) -0.10044(6) 0.0576(4) Uani 1 1 d . . . F11 F 0.75752(14) 0.26127(11) -0.06918(6) 0.0511(4) Uani 1 1 d . . . F12 F 0.82779(13) 0.31449(11) 0.03517(6) 0.0463(4) Uani 1 1 d . . . F13 F 0.91993(13) 0.23173(11) 0.20255(6) 0.0481(4) Uani 1 1 d . . . F14 F 1.11292(13) 0.36403(12) 0.23071(7) 0.0549(4) Uani 1 1 d . . . F15 F 1.11948(14) 0.53852(12) 0.19616(7) 0.0592(5) Uani 1 1 d . . . F16 F 0.92293(16) 0.57413(11) 0.13167(7) 0.0605(5) Uani 1 1 d . . . F17 F 0.72624(14) 0.44079(11) 0.10142(6) 0.0484(4) Uani 1 1 d . . . F18 F 0.69330(12) 0.26955(10) 0.25020(6) 0.0389(3) Uani 1 1 d . . . F19 F 0.55868(14) 0.35470(11) 0.31328(6) 0.0486(4) Uani 1 1 d . . . F20 F 0.37034(14) 0.42973(11) 0.26674(6) 0.0513(4) Uani 1 1 d . . . F21 F 0.32666(15) 0.42284(13) 0.15497(7) 0.0596(5) Uani 1 1 d . . . F22 F 0.46225(14) 0.34281(12) 0.09106(6) 0.0522(4) Uani 1 1 d . . . F23 F 0.02201(13) 0.75266(11) 0.29932(7) 0.0498(4) Uani 1 1 d . . . F24 F -0.16615(14) 0.62272(14) 0.26107(7) 0.0671(5) Uani 1 1 d . . . F25 F -0.17246(16) 0.44288(13) 0.28496(8) 0.0764(6) Uani 1 1 d . . . F26 F 0.02645(18) 0.39770(11) 0.34427(8) 0.0712(6) Uani 1 1 d . . . F27 F 0.22351(15) 0.52734(10) 0.37888(7) 0.0504(4) Uani 1 1 d . . . F28 F 0.24328(14) 0.75097(12) 0.24859(6) 0.0529(4) Uani 1 1 d . . . F29 F 0.37555(17) 0.69389(14) 0.17262(7) 0.0665(5) Uani 1 1 d . . . F30 F 0.56120(16) 0.60278(13) 0.20199(7) 0.0647(5) Uani 1 1 d . . . F31 F 0.60913(15) 0.57005(12) 0.30980(7) 0.0575(4) Uani 1 1 d . . . F32 F 0.48340(14) 0.62892(11) 0.38636(6) 0.0459(4) Uani 1 1 d . . . F33 F 0.49312(13) 0.81882(11) 0.41862(6) 0.0471(4) Uani 1 1 d . . . F34 F 0.56944(15) 0.83763(13) 0.52588(7) 0.0594(5) Uani 1 1 d . . . F35 F 0.42521(16) 0.75041(13) 0.59952(7) 0.0612(5) Uani 1 1 d . . . F36 F 0.20238(16) 0.64267(11) 0.56252(7) 0.0570(4) Uani 1 1 d . . . F37 F 0.12263(13) 0.62420(10) 0.45699(6) 0.0464(4) Uani 1 1 d . . . F38 F 0.07064(13) 0.79716(10) 0.41474(6) 0.0462(4) Uani 1 1 d . . . F39 F 0.03537(16) 0.97096(11) 0.42028(8) 0.0622(5) Uani 1 1 d . . . F40 F 0.18715(19) 1.10490(11) 0.37256(8) 0.0736(5) Uani 1 1 d . . . F41 F 0.37591(18) 1.06038(12) 0.31954(8) 0.0737(6) Uani 1 1 d . . . F42 F 0.41344(14) 0.88846(11) 0.31345(7) 0.0538(4) Uani 1 1 d . . . C37 C 0.6884(2) 0.14620(18) 0.14974(10) 0.0376(6) Uani 1 1 d . . . C38 C 0.6102(2) 0.08955(18) 0.18044(11) 0.0393(6) Uani 1 1 d . . . C39 C 0.6156(3) -0.00170(19) 0.18895(11) 0.0447(7) Uani 1 1 d . . . C40 C 0.7017(3) -0.04128(19) 0.16541(12) 0.0478(7) Uani 1 1 d . . . C41 C 0.7816(3) 0.0101(2) 0.13368(12) 0.0488(7) Uani 1 1 d . . . C42 C 0.7735(2) 0.10036(19) 0.12682(11) 0.0418(6) Uani 1 1 d . . . C43 C 0.6401(2) 0.23617(18) 0.06582(10) 0.0374(6) Uani 1 1 d . . . C44 C 0.5271(2) 0.1805(2) 0.04688(11) 0.0428(7) Uani 1 1 d . . . C45 C 0.4888(2) 0.1526(2) -0.00744(11) 0.0462(7) Uani 1 1 d . . . C46 C 0.5667(3) 0.1797(2) -0.04699(11) 0.0460(7) Uani 1 1 d . . . C47 C 0.6792(2) 0.23462(19) -0.03102(10) 0.0419(6) Uani 1 1 d . . . C48 C 0.7132(2) 0.26148(18) 0.02404(10) 0.0386(6) Uani 1 1 d . . . C49 C 0.8120(2) 0.32781(18) 0.14895(10) 0.0368(6) Uani 1 1 d . . . C50 C 0.9150(2) 0.31520(18) 0.18212(10) 0.0383(6) Uani 1 1 d . . . C51 C 1.0174(2) 0.3834(2) 0.19761(11) 0.0423(7) Uani 1 1 d . . . C52 C 1.0210(2) 0.4705(2) 0.18088(11) 0.0448(7) Uani 1 1 d . . . C53 C 0.9215(3) 0.48831(19) 0.14834(11) 0.0444(7) Uani 1 1 d . . . C54 C 0.8215(2) 0.41824(19) 0.13368(10) 0.0403(6) Uani 1 1 d . . . C55 C 0.5842(2) 0.29916(17) 0.16731(10) 0.0354(6) Uani 1 1 d . . . C56 C 0.6023(2) 0.30708(17) 0.22444(10) 0.0352(6) Uani 1 1 d . . . C57 C 0.5341(2) 0.34985(18) 0.25805(10) 0.0378(6) Uani 1 1 d . . . C58 C 0.4395(2) 0.38824(18) 0.23474(11) 0.0401(6) Uani 1 1 d . . . C59 C 0.4172(2) 0.3839(2) 0.17834(11) 0.0434(7) Uani 1 1 d . . . C60 C 0.4896(2) 0.34110(19) 0.14629(10) 0.0411(6) Uani 1 1 d . . . C61 C 0.1325(2) 0.64776(17) 0.34313(10) 0.0367(6) Uani 1 1 d . . . C62 C 0.0295(2) 0.66538(18) 0.31224(11) 0.0408(6) Uani 1 1 d . . . C63 C -0.0712(2) 0.5990(2) 0.29195(12) 0.0489(7) Uani 1 1 d . . . C64 C -0.0738(3) 0.5088(2) 0.30320(13) 0.0531(8) Uani 1 1 d . . . C65 C 0.0264(3) 0.48629(19) 0.33291(13) 0.0527(8) Uani 1 1 d . . . C66 C 0.1265(2) 0.55454(18) 0.35098(12) 0.0436(7) Uani 1 1 d . . . C67 C 0.3568(2) 0.69522(17) 0.32197(10) 0.0372(6) Uani 1 1 d . . . C68 C 0.3360(2) 0.70825(19) 0.26606(11) 0.0430(6) Uani 1 1 d . . . C69 C 0.4027(3) 0.6793(2) 0.22610(11) 0.0489(7) Uani 1 1 d . . . C70 C 0.4959(3) 0.6338(2) 0.24040(12) 0.0481(7) Uani 1 1 d . . . C71 C 0.5205(2) 0.61808(19) 0.29484(12) 0.0442(7) Uani 1 1 d . . . C72 C 0.4519(2) 0.64870(18) 0.33384(10) 0.0382(6) Uani 1 1 d . . . C73 C 0.3056(2) 0.71896(17) 0.43070(11) 0.0365(6) Uani 1 1 d . . . C74 C 0.4178(2) 0.77219(18) 0.45277(11) 0.0388(6) Uani 1 1 d . . . C75 C 0.4594(2) 0.78315(19) 0.50787(12) 0.0439(7) Uani 1 1 d . . . C76 C 0.3869(3) 0.7397(2) 0.54520(11) 0.0467(7) Uani 1 1 d . . . C77 C 0.2751(3) 0.68603(18) 0.52630(11) 0.0431(7) Uani 1 1 d . . . C78 C 0.2365(2) 0.67677(17) 0.47055(11) 0.0382(6) Uani 1 1 d . . . C79 C 0.2415(2) 0.83190(17) 0.36249(11) 0.0378(6) Uani 1 1 d . . . C80 C 0.1490(2) 0.86052(17) 0.39000(11) 0.0404(6) Uani 1 1 d . . . C81 C 0.1286(3) 0.94937(19) 0.39383(12) 0.0475(7) Uani 1 1 d . . . C82 C 0.2049(3) 1.01695(19) 0.36977(13) 0.0533(8) Uani 1 1 d . . . C83 C 0.2998(3) 0.99417(19) 0.34303(13) 0.0534(8) Uani 1 1 d . . . C84 C 0.3164(2) 0.90409(18) 0.34031(12) 0.0442(7) 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 N1 0.0573(16) 0.0377(14) 0.0498(15) 0.0075(11) 0.0137(12) 0.0069(11) N2 0.0498(15) 0.0447(15) 0.0465(15) 0.0119(12) 0.0076(12) 0.0053(11) B1 0.060(2) 0.0459(18) 0.052(2) 0.0168(16) 0.0106(16) 0.0119(16) C4 0.0455(15) 0.0350(14) 0.0444(15) 0.0089(11) 0.0060(12) 0.0078(11) C5 0.0448(17) 0.0458(17) 0.0450(17) 0.0099(14) 0.0016(14) 0.0127(13) C6 0.0397(14) 0.0436(15) 0.0418(15) 0.0078(12) 0.0020(12) 0.0086(11) C6' 0.0573(16) 0.0377(14) 0.0498(15) 0.0075(11) 0.0137(12) 0.0069(11) C4' 0.0498(15) 0.0447(15) 0.0465(15) 0.0119(12) 0.0076(12) 0.0053(11) C5' 0.060(2) 0.0459(18) 0.052(2) 0.0168(16) 0.0106(16) 0.0119(16) N2' 0.0455(15) 0.0350(14) 0.0444(15) 0.0089(11) 0.0060(12) 0.0078(11) B1' 0.0448(17) 0.0458(17) 0.0450(17) 0.0099(14) 0.0016(14) 0.0127(13) N1' 0.0397(14) 0.0436(15) 0.0418(15) 0.0078(12) 0.0020(12) 0.0086(11) C1 0.0590(18) 0.0386(16) 0.061(2) 0.0068(14) 0.0174(15) 0.0077(14) C2 0.0512(17) 0.0404(16) 0.0572(19) 0.0030(14) 0.0138(14) 0.0031(13) C3 0.0442(15) 0.0382(15) 0.0508(17) 0.0074(13) 0.0088(13) 0.0061(12) C7 0.0389(15) 0.0570(18) 0.0420(16) 0.0047(14) -0.0001(13) 0.0100(13) C8 0.0431(16) 0.0583(19) 0.0468(17) 0.0068(14) 0.0038(13) 0.0042(14) C9 0.0486(17) 0.0554(18) 0.0557(19) 0.0105(15) 0.0112(15) 0.0036(14) C10 0.067(2) 0.0467(18) 0.074(2) 0.0102(16) 0.0143(17) 0.0106(15) C11 0.063(2) 0.0449(17) 0.071(2) -0.0012(15) 0.0282(17) 0.0010(15) C12 0.096(3) 0.086(3) 0.065(2) 0.022(2) 0.032(2) 0.037(2) C13 0.0529(18) 0.0428(16) 0.068(2) 0.0044(15) 0.0152(16) -0.0017(13) C15 0.0507(17) 0.0590(19) 0.0421(17) -0.0017(14) 0.0023(13) 0.0105(14) C16 0.0524(19) 0.073(2) 0.066(2) 0.0077(17) 0.0188(17) 0.0027(16) C17 0.077(2) 0.098(3) 0.059(2) 0.009(2) 0.0200(19) 0.002(2) C18 0.083(3) 0.058(2) 0.148(4) 0.027(2) 0.067(3) 0.0092(19) N3 0.0377(13) 0.0485(14) 0.0323(13) 0.0072(11) 0.0094(10) 0.0116(11) B2 0.0439(16) 0.0447(16) 0.0373(16) 0.0023(13) 0.0117(13) 0.0117(13) N4' 0.0409(14) 0.0447(14) 0.0385(14) 0.0019(11) 0.0099(11) 0.0057(11) C24' 0.0377(13) 0.0485(14) 0.0323(13) 0.0072(11) 0.0094(10) 0.0116(11) C23' 0.0439(16) 0.0447(16) 0.0373(16) 0.0023(13) 0.0117(13) 0.0117(13) C22 0.0409(14) 0.0447(14) 0.0385(14) 0.0019(11) 0.0099(11) 0.0057(11) C19 0.0384(15) 0.0578(18) 0.0393(16) 0.0049(14) 0.0073(12) 0.0111(13) C20 0.0377(15) 0.070(2) 0.0480(18) 0.0074(15) 0.0107(13) 0.0045(14) C21 0.0457(17) 0.0585(18) 0.0496(18) -0.0041(15) 0.0112(14) 0.0004(14) C28 0.0493(18) 0.067(2) 0.080(2) 0.0063(18) 0.0175(17) 0.0170(16) C29 0.0452(18) 0.081(2) 0.066(2) -0.0075(18) 0.0183(16) -0.0106(16) C30 0.071(3) 0.075(3) 0.138(4) 0.016(3) 0.032(3) -0.013(2) C31 0.0483(18) 0.093(3) 0.064(2) -0.0131(19) 0.0096(16) 0.0056(17) N4 0.0332(12) 0.0316(12) 0.0361(13) 0.0063(10) 0.0069(10) 0.0050(10) B2' 0.0381(15) 0.0324(14) 0.0357(15) 0.0052(12) 0.0106(12) 0.0086(12) C24 0.0331(12) 0.0341(12) 0.0369(13) 0.0062(10) 0.0093(10) 0.0065(10) C22' 0.0332(12) 0.0316(12) 0.0361(13) 0.0063(10) 0.0069(10) 0.0050(10) C23 0.0381(15) 0.0324(14) 0.0357(15) 0.0052(12) 0.0106(12) 0.0086(12) N3' 0.0331(12) 0.0341(12) 0.0369(13) 0.0062(10) 0.0093(10) 0.0065(10) C25 0.0319(13) 0.0404(14) 0.0429(16) 0.0086(12) 0.0101(12) 0.0050(11) C26 0.0324(13) 0.0401(14) 0.0443(16) 0.0072(12) 0.0056(12) 0.0037(11) C27 0.0363(14) 0.0353(14) 0.0408(15) 0.0067(11) 0.0038(12) 0.0061(11) C33 0.0432(16) 0.0580(18) 0.0531(18) 0.0004(14) 0.0142(14) -0.0011(14) C34 0.0379(15) 0.0571(18) 0.0495(18) -0.0012(14) 0.0054(13) -0.0052(13) C35 0.0548(18) 0.0480(18) 0.074(2) -0.0023(16) 0.0258(17) -0.0071(14) C36 0.0427(15) 0.0452(16) 0.0470(17) 0.0015(13) 0.0078(13) 0.0046(12) B3 0.0348(15) 0.0477(17) 0.0260(15) 0.0051(13) 0.0044(12) 0.0066(13) B4 0.0341(15) 0.0362(16) 0.0374(17) 0.0091(13) 0.0071(13) 0.0038(12) F3 0.0432(9) 0.0478(9) 0.0442(9) 0.0049(7) 0.0130(7) 0.0027(7) F4 0.0654(11) 0.0494(10) 0.0554(11) 0.0122(8) 0.0052(9) -0.0023(8) F5 0.0682(11) 0.0458(10) 0.0723(12) -0.0025(9) -0.0177(9) 0.0139(8) F6 0.0533(10) 0.0686(11) 0.0676(12) -0.0121(9) -0.0014(9) 0.0264(9) F7 0.0425(9) 0.0666(10) 0.0454(9) 0.0021(8) 0.0103(7) 0.0129(8) F8 0.0372(8) 0.0767(11) 0.0353(9) 0.0060(8) 0.0055(7) -0.0077(8) F9 0.0433(9) 0.0885(13) 0.0412(9) -0.0051(9) -0.0028(7) -0.0141(9) F10 0.0540(10) 0.0822(12) 0.0299(9) -0.0076(8) -0.0006(7) 0.0015(9) F11 0.0482(9) 0.0717(11) 0.0310(8) 0.0012(7) 0.0113(7) 0.0023(8) F12 0.0355(8) 0.0657(10) 0.0326(8) 0.0013(7) 0.0059(6) -0.0040(7) F13 0.0398(8) 0.0560(10) 0.0471(9) 0.0074(8) -0.0062(7) 0.0097(7) F14 0.0343(8) 0.0740(11) 0.0523(10) -0.0025(8) -0.0066(7) 0.0069(8) F15 0.0436(9) 0.0671(11) 0.0571(11) -0.0079(9) 0.0054(8) -0.0114(8) F16 0.0650(11) 0.0487(10) 0.0625(11) 0.0115(8) 0.0036(9) -0.0034(8) F17 0.0465(9) 0.0540(9) 0.0430(9) 0.0116(7) -0.0025(7) 0.0065(7) F18 0.0378(8) 0.0480(8) 0.0307(8) 0.0053(6) -0.0010(6) 0.0091(6) F19 0.0542(9) 0.0644(10) 0.0293(8) 0.0034(7) 0.0081(7) 0.0146(8) F20 0.0483(9) 0.0607(10) 0.0494(10) 0.0023(8) 0.0144(8) 0.0179(8) F21 0.0499(10) 0.0855(12) 0.0525(10) 0.0157(9) 0.0042(8) 0.0338(9) F22 0.0493(9) 0.0803(12) 0.0314(9) 0.0125(8) 0.0006(7) 0.0229(8) F23 0.0421(9) 0.0521(10) 0.0551(10) 0.0062(8) -0.0021(7) 0.0113(7) F24 0.0354(9) 0.0980(14) 0.0619(12) -0.0148(10) -0.0002(8) 0.0046(9) F25 0.0564(11) 0.0734(12) 0.0838(14) -0.0321(10) 0.0239(10) -0.0259(9) F26 0.0887(13) 0.0361(9) 0.0853(14) -0.0041(9) 0.0354(11) -0.0078(9) F27 0.0585(10) 0.0365(8) 0.0600(10) 0.0117(7) 0.0161(8) 0.0120(7) F28 0.0482(9) 0.0716(11) 0.0416(9) 0.0165(8) 0.0017(7) 0.0165(8) F29 0.0702(12) 0.0952(14) 0.0348(10) 0.0138(9) 0.0096(8) 0.0133(10) F30 0.0643(11) 0.0856(13) 0.0478(10) -0.0008(9) 0.0237(9) 0.0162(10) F31 0.0502(10) 0.0704(11) 0.0588(11) 0.0064(9) 0.0147(8) 0.0244(9) F32 0.0478(9) 0.0551(9) 0.0399(9) 0.0125(7) 0.0083(7) 0.0187(7) F33 0.0394(8) 0.0562(9) 0.0423(9) 0.0112(7) 0.0073(7) -0.0030(7) F34 0.0472(9) 0.0805(12) 0.0462(10) 0.0045(9) -0.0042(8) 0.0051(9) F35 0.0715(11) 0.0826(12) 0.0360(9) 0.0126(8) 0.0067(8) 0.0285(10) F36 0.0693(11) 0.0621(10) 0.0473(10) 0.0199(8) 0.0283(8) 0.0177(9) F37 0.0439(9) 0.0457(9) 0.0497(9) 0.0087(7) 0.0180(7) 0.0012(7) F38 0.0451(9) 0.0408(8) 0.0551(10) 0.0065(7) 0.0158(7) 0.0085(7) F39 0.0700(11) 0.0512(10) 0.0699(12) -0.0050(9) 0.0088(9) 0.0246(9) F40 0.0975(14) 0.0332(9) 0.0875(14) 0.0034(9) -0.0068(11) 0.0137(9) F41 0.0854(13) 0.0435(10) 0.0864(14) 0.0256(9) 0.0092(11) -0.0083(9) F42 0.0488(9) 0.0507(9) 0.0615(11) 0.0204(8) 0.0161(8) -0.0007(7) C37 0.0332(13) 0.0476(15) 0.0299(14) -0.0020(11) 0.0001(11) 0.0047(12) C38 0.0368(14) 0.0461(16) 0.0334(14) -0.0017(12) -0.0003(12) 0.0064(12) C39 0.0438(16) 0.0454(16) 0.0389(16) 0.0012(13) -0.0052(13) -0.0017(13) C40 0.0514(17) 0.0397(16) 0.0480(17) -0.0026(13) -0.0145(14) 0.0081(13) C41 0.0427(16) 0.0576(19) 0.0450(17) -0.0114(14) -0.0049(13) 0.0148(14) C42 0.0363(14) 0.0519(17) 0.0347(15) 0.0001(12) -0.0007(12) 0.0049(12) C43 0.0312(13) 0.0492(15) 0.0305(14) 0.0043(12) 0.0018(11) 0.0047(11) C44 0.0375(15) 0.0592(17) 0.0300(15) 0.0063(13) 0.0060(12) 0.0027(13) C45 0.0353(15) 0.0603(18) 0.0369(16) -0.0003(13) -0.0004(12) -0.0041(13) C46 0.0471(16) 0.0606(18) 0.0275(15) -0.0040(13) 0.0002(12) 0.0066(14) C47 0.0404(15) 0.0559(17) 0.0295(14) 0.0044(12) 0.0100(12) 0.0064(13) C48 0.0313(13) 0.0502(16) 0.0316(14) 0.0016(12) 0.0014(11) 0.0017(12) C49 0.0334(13) 0.0494(16) 0.0272(13) 0.0026(11) 0.0053(11) 0.0059(11) C50 0.0344(14) 0.0469(16) 0.0340(14) 0.0026(12) 0.0053(11) 0.0079(12) C51 0.0290(14) 0.0649(19) 0.0319(14) -0.0028(13) 0.0002(11) 0.0087(13) C52 0.0359(15) 0.0544(18) 0.0388(16) -0.0055(13) 0.0078(12) -0.0046(13) C53 0.0462(16) 0.0463(16) 0.0390(16) 0.0045(13) 0.0077(13) 0.0024(13) C54 0.0363(14) 0.0548(17) 0.0293(14) 0.0039(12) 0.0040(11) 0.0069(12) C55 0.0315(13) 0.0427(14) 0.0301(14) 0.0062(11) 0.0024(11) 0.0017(11) C56 0.0310(13) 0.0420(14) 0.0322(14) 0.0082(11) 0.0019(11) 0.0048(11) C57 0.0397(14) 0.0446(15) 0.0283(14) 0.0063(11) 0.0055(11) 0.0037(12) C58 0.0357(14) 0.0465(15) 0.0391(16) 0.0017(12) 0.0107(12) 0.0075(12) C59 0.0345(14) 0.0555(17) 0.0428(17) 0.0117(13) 0.0044(12) 0.0128(13) C60 0.0366(14) 0.0564(17) 0.0300(14) 0.0101(12) 0.0023(11) 0.0067(12) C61 0.0359(14) 0.0384(14) 0.0364(15) 0.0025(11) 0.0115(12) 0.0048(11) C62 0.0370(14) 0.0433(16) 0.0422(16) -0.0003(12) 0.0121(12) 0.0049(12) C63 0.0341(15) 0.065(2) 0.0450(17) -0.0099(14) 0.0111(13) 0.0030(14) C64 0.0418(17) 0.0562(19) 0.0532(19) -0.0191(15) 0.0202(15) -0.0131(14) C65 0.064(2) 0.0338(16) 0.0583(19) -0.0055(13) 0.0292(17) -0.0046(14) C66 0.0438(16) 0.0403(16) 0.0477(17) 0.0024(13) 0.0153(13) 0.0057(13) C67 0.0343(14) 0.0390(14) 0.0365(15) 0.0081(11) 0.0064(11) -0.0004(11) C68 0.0370(15) 0.0513(16) 0.0409(16) 0.0115(13) 0.0050(12) 0.0061(12) C69 0.0484(17) 0.0627(19) 0.0337(16) 0.0107(14) 0.0073(13) 0.0022(14) C70 0.0469(17) 0.0562(18) 0.0415(17) 0.0021(14) 0.0185(14) 0.0043(14) C71 0.0365(15) 0.0474(16) 0.0497(18) 0.0051(13) 0.0099(13) 0.0072(12) C72 0.0391(14) 0.0418(15) 0.0332(15) 0.0080(12) 0.0061(12) 0.0039(12) C73 0.0359(14) 0.0357(14) 0.0404(15) 0.0086(11) 0.0101(12) 0.0091(11) C74 0.0381(14) 0.0434(15) 0.0381(16) 0.0121(12) 0.0103(12) 0.0105(12) C75 0.0378(15) 0.0493(16) 0.0449(17) 0.0056(13) 0.0029(13) 0.0092(12) C76 0.0577(18) 0.0570(18) 0.0325(16) 0.0097(13) 0.0071(13) 0.0261(15) C77 0.0508(17) 0.0435(15) 0.0429(17) 0.0171(13) 0.0203(14) 0.0187(13) C78 0.0410(15) 0.0355(14) 0.0412(16) 0.0090(12) 0.0119(12) 0.0101(12) C79 0.0377(14) 0.0378(14) 0.0364(15) 0.0089(11) -0.0019(11) 0.0044(11) C80 0.0411(15) 0.0346(14) 0.0441(16) 0.0063(12) 0.0014(12) 0.0038(12) C81 0.0523(17) 0.0406(16) 0.0486(17) -0.0006(13) -0.0028(14) 0.0111(13) C82 0.069(2) 0.0305(15) 0.0574(19) 0.0039(13) -0.0084(16) 0.0094(14) C83 0.0604(19) 0.0352(16) 0.0576(19) 0.0159(14) -0.0037(16) -0.0076(14) C84 0.0417(15) 0.0415(16) 0.0472(17) 0.0111(13) 0.0033(13) 0.0004(12) _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 N1 B1 1.404(4) . ? N1 C4 1.411(3) . ? N1 C1 1.412(4) . ? N2 B1 1.402(4) . ? N2 C9 1.410(4) . ? N2 C6 1.416(3) . ? B1 H1 0.9500 . ? C4 C5 1.385(4) . ? C4 C3 1.408(4) . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 C7 1.405(4) . ? C1 C2 1.411(4) . ? C1 C10 1.435(4) . ? C2 C3 1.388(4) . ? C2 C11 1.499(4) . ? C3 C13 1.485(4) . ? C7 C8 1.392(4) . ? C7 C15 1.482(4) . ? C8 C9 1.411(4) . ? C8 C16 1.501(4) . ? C9 C18 1.443(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.520(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.524(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N3 N4' 1.383(3) 2_665 ? N3 B2 1.407(4) . ? N3 C19 1.411(3) . ? B2 N4' 1.403(4) . ? B2 H2 0.9500 . ? N4' N3 1.383(3) 2_665 ? N4' C21 1.422(4) 2_665 ? C24' C22 1.383(3) 2_665 ? C24' C23' 1.407(4) . ? C24' C19 1.410(3) 2_665 ? C23' C22 1.403(4) . ? C23' H23' 0.9500 . ? C22 C24' 1.383(3) 2_665 ? C22 C21 1.422(4) . ? C19 C20 1.391(4) . ? C19 C24' 1.410(3) 2_665 ? C19 C28 1.472(4) . ? C20 C21 1.410(4) . ? C20 C29 1.499(4) . ? C21 N4' 1.422(4) 2_665 ? C21 C31 1.457(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.507(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N4 C24 1.393(3) . ? N4 C27 1.405(3) . ? N4 B2' 1.410(3) . ? B2' C24 1.410(4) 2_666 ? B2' H2' 0.9500 . ? C24 C25 1.400(3) . ? C24 B2' 1.410(4) 2_666 ? C22' N3' 1.393(3) . ? C22' C27 1.405(3) 2_666 ? C22' C23 1.410(3) . ? C23 N3' 1.410(3) 2_666 ? C23 H23 0.9500 . ? N3' C25 1.400(3) 2_666 ? N3' C23 1.410(3) 2_666 ? C25 C26 1.394(4) . ? C25 N3' 1.400(3) 2_666 ? C25 C33 1.487(4) . ? C26 C27 1.398(4) . ? C26 C34 1.498(4) . ? C27 C22' 1.405(3) 2_666 ? C27 C36 1.481(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.523(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? B3 C55 1.648(4) . ? B3 C43 1.653(4) . ? B3 C37 1.654(4) . ? B3 C49 1.662(4) . ? B4 C79 1.654(4) . ? B4 C61 1.654(4) . ? B4 C73 1.656(4) . ? B4 C67 1.656(4) . ? F3 C38 1.356(3) . ? F4 C39 1.348(3) . ? F5 C40 1.353(3) . ? F6 C41 1.354(3) . ? F7 C42 1.359(3) . ? F8 C44 1.360(3) . ? F9 C45 1.351(3) . ? F10 C46 1.346(3) . ? F11 C47 1.353(3) . ? F12 C48 1.359(3) . ? F13 C50 1.360(3) . ? F14 C51 1.356(3) . ? F15 C52 1.349(3) . ? F16 C53 1.347(3) . ? F17 C54 1.361(3) . ? F18 C56 1.360(3) . ? F19 C57 1.348(3) . ? F20 C58 1.346(3) . ? F21 C59 1.345(3) . ? F22 C60 1.358(3) . ? F23 C62 1.357(3) . ? F24 C63 1.349(3) . ? F25 C64 1.347(3) . ? F26 C65 1.351(3) . ? F27 C66 1.356(3) . ? F28 C68 1.351(3) . ? F29 C69 1.350(3) . ? F30 C70 1.348(3) . ? F31 C71 1.350(3) . ? F32 C72 1.359(3) . ? F33 C74 1.354(3) . ? F34 C75 1.353(3) . ? F35 C76 1.348(3) . ? F36 C77 1.353(3) . ? F37 C78 1.356(3) . ? F38 C80 1.356(3) . ? F39 C81 1.345(3) . ? F40 C82 1.349(3) . ? F41 C83 1.352(3) . ? F42 C84 1.359(3) . ? C37 C38 1.385(4) . ? C37 C42 1.400(4) . ? C38 C39 1.385(4) . ? C39 C40 1.363(4) . ? C40 C41 1.375(4) . ? C41 C42 1.369(4) . ? C43 C48 1.382(3) . ? C43 C44 1.390(4) . ? C44 C45 1.375(4) . ? C45 C46 1.377(4) . ? C46 C47 1.368(4) . ? C47 C48 1.382(4) . ? C49 C50 1.386(4) . ? C49 C54 1.391(4) . ? C50 C51 1.380(4) . ? C51 C52 1.363(4) . ? C52 C53 1.375(4) . ? C53 C54 1.375(4) . ? C55 C60 1.387(4) . ? C55 C56 1.388(3) . ? C56 C57 1.372(4) . ? C57 C58 1.375(4) . ? C58 C59 1.374(4) . ? C59 C60 1.382(4) . ? C61 C62 1.384(4) . ? C61 C66 1.389(4) . ? C62 C63 1.377(4) . ? C63 C64 1.369(4) . ? C64 C65 1.374(5) . ? C65 C66 1.376(4) . ? C67 C72 1.379(4) . ? C67 C68 1.393(4) . ? C68 C69 1.375(4) . ? C69 C70 1.363(4) . ? C70 C71 1.372(4) . ? C71 C72 1.381(4) . ? C73 C74 1.388(4) . ? C73 C78 1.391(3) . ? C74 C75 1.374(4) . ? C75 C76 1.372(4) . ? C76 C77 1.368(4) . ? C77 C78 1.382(4) . ? C79 C84 1.387(4) . ? C79 C80 1.393(4) . ? C80 C81 1.373(4) . ? C81 C82 1.373(4) . ? C82 C83 1.372(4) . ? C83 C84 1.376(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 N1 C4 120.7(2) . . ? B1 N1 C1 131.9(3) . . ? C4 N1 C1 107.3(2) . . ? B1 N2 C9 132.3(3) . . ? B1 N2 C6 120.3(2) . . ? C9 N2 C6 107.3(2) . . ? N2 B1 N1 118.4(3) . . ? N2 B1 H1 120.8 . . ? N1 B1 H1 120.8 . . ? C5 C4 C3 132.1(2) . . ? C5 C4 N1 120.0(2) . . ? C3 C4 N1 107.8(2) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 131.8(3) . . ? C5 C6 N2 120.2(2) . . ? C7 C6 N2 108.0(2) . . ? C2 C1 N1 108.1(2) . . ? C2 C1 C10 128.4(3) . . ? N1 C1 C10 123.2(3) . . ? C3 C2 C1 108.0(2) . . ? C3 C2 C11 127.6(2) . . ? C1 C2 C11 124.4(3) . . ? C2 C3 C4 108.7(2) . . ? C2 C3 C13 128.7(3) . . ? C4 C3 C13 122.6(2) . . ? C8 C7 C6 108.5(3) . . ? C8 C7 C15 128.1(3) . . ? C6 C7 C15 123.3(2) . . ? C7 C8 C9 108.1(3) . . ? C7 C8 C16 125.3(3) . . ? C9 C8 C16 126.6(3) . . ? N2 C9 C8 108.1(2) . . ? N2 C9 C18 122.3(3) . . ? C8 C9 C18 129.4(3) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 C12 113.2(3) . . ? C2 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C2 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 C17 112.3(3) . . ? C8 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C8 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C9 C18 H18A 109.5 . . ? C9 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C9 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4' N3 B2 120.8(2) 2_665 . ? N4' N3 C19 109.0(2) 2_665 . ? B2 N3 C19 130.2(2) . . ? N4' B2 N3 117.2(2) . . ? N4' B2 H2 121.4 . . ? N3 B2 H2 121.4 . . ? N3 N4' B2 122.0(2) 2_665 . ? N3 N4' C21 108.0(2) 2_665 2_665 ? B2 N4' C21 129.9(2) . 2_665 ? C22 C24' C23' 120.8(2) 2_665 . ? C22 C24' C19 109.0(2) 2_665 2_665 ? C23' C24' C19 130.2(2) . 2_665 ? C22 C23' C24' 117.2(2) . . ? C22 C23' H23' 121.4 . . ? C24' C23' H23' 121.4 . . ? C24' C22 C23' 122.0(2) 2_665 . ? C24' C22 C21 108.0(2) 2_665 . ? C23' C22 C21 129.9(2) . . ? C20 C19 C24' 107.2(2) . 2_665 ? C20 C19 N3 107.2(2) . . ? C20 C19 C28 128.4(3) . . ? C24' C19 C28 124.1(3) 2_665 . ? N3 C19 C28 124.1(3) . . ? C19 C20 C21 109.1(2) . . ? C19 C20 C29 125.9(3) . . ? C21 C20 C29 125.0(3) . . ? C20 C21 N4' 106.7(2) . 2_665 ? C20 C21 C22 106.7(2) . . ? C20 C21 C31 128.5(3) . . ? N4' C21 C31 124.4(3) 2_665 . ? C22 C21 C31 124.4(3) . . ? C19 C28 H28A 109.5 . . ? C19 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C19 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C20 C29 C30 111.2(3) . . ? C20 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? C20 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C21 C31 H31A 109.5 . . ? C21 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C21 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C24 N4 C27 107.87(19) . . ? C24 N4 B2' 121.6(2) . . ? C27 N4 B2' 130.5(2) . . ? C24 B2' N4 117.6(2) 2_666 . ? C24 B2' H2' 121.2 2_666 . ? N4 B2' H2' 121.2 . . ? N4 C24 C25 108.1(2) . . ? N4 C24 B2' 120.8(2) . 2_666 ? C25 C24 B2' 131.0(2) . 2_666 ? N3' C22' C27 107.87(19) . 2_666 ? N3' C22' C23 121.6(2) . . ? C27 C22' C23 130.5(2) 2_666 . ? N3' C23 C22' 117.6(2) 2_666 . ? N3' C23 H23 121.2 2_666 . ? C22' C23 H23 121.2 . . ? C22' N3' C25 108.1(2) . 2_666 ? C22' N3' C23 120.8(2) . 2_666 ? C25 N3' C23 131.0(2) 2_666 2_666 ? C26 C25 N3' 108.0(2) . 2_666 ? C26 C25 C24 108.0(2) . . ? C26 C25 C33 127.5(2) . . ? N3' C25 C33 124.4(2) 2_666 . ? C24 C25 C33 124.4(2) . . ? C25 C26 C27 108.1(2) . . ? C25 C26 C34 125.9(2) . . ? C27 C26 C34 125.9(2) . . ? C26 C27 C22' 107.8(2) . 2_666 ? C26 C27 N4 107.8(2) . . ? C26 C27 C36 128.2(2) . . ? C22' C27 C36 124.0(2) 2_666 . ? N4 C27 C36 124.0(2) . . ? C25 C33 H33A 109.5 . . ? C25 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C25 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 C35 112.3(2) . . ? C26 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? C26 C34 H34B 109.1 . . ? C35 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C27 C36 H36A 109.5 . . ? C27 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C27 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C55 B3 C43 114.0(2) . . ? C55 B3 C37 113.1(2) . . ? C43 B3 C37 101.8(2) . . ? C55 B3 C49 101.6(2) . . ? C43 B3 C49 113.2(2) . . ? C37 B3 C49 113.7(2) . . ? C79 B4 C61 113.1(2) . . ? C79 B4 C73 101.4(2) . . ? C61 B4 C73 113.4(2) . . ? C79 B4 C67 113.8(2) . . ? C61 B4 C67 101.3(2) . . ? C73 B4 C67 114.4(2) . . ? C38 C37 C42 112.4(2) . . ? C38 C37 B3 127.8(2) . . ? C42 C37 B3 119.4(2) . . ? F3 C38 C39 114.5(2) . . ? F3 C38 C37 120.9(2) . . ? C39 C38 C37 124.6(2) . . ? F4 C39 C40 119.9(3) . . ? F4 C39 C38 120.7(3) . . ? C40 C39 C38 119.4(3) . . ? F5 C40 C39 120.0(3) . . ? F5 C40 C41 120.6(3) . . ? C39 C40 C41 119.4(3) . . ? F6 C41 C42 121.1(3) . . ? F6 C41 C40 119.7(3) . . ? C42 C41 C40 119.2(3) . . ? F7 C42 C41 116.3(2) . . ? F7 C42 C37 118.7(2) . . ? C41 C42 C37 125.0(3) . . ? C48 C43 C44 113.0(2) . . ? C48 C43 B3 127.1(2) . . ? C44 C43 B3 119.2(2) . . ? F8 C44 C45 116.0(2) . . ? F8 C44 C43 119.2(2) . . ? C45 C44 C43 124.9(2) . . ? F9 C45 C44 121.3(2) . . ? F9 C45 C46 119.6(2) . . ? C44 C45 C46 119.1(2) . . ? F10 C46 C47 120.9(2) . . ? F10 C46 C45 120.3(2) . . ? C47 C46 C45 118.8(2) . . ? F11 C47 C46 119.7(2) . . ? F11 C47 C48 120.3(2) . . ? C46 C47 C48 119.9(2) . . ? F12 C48 C47 114.8(2) . . ? F12 C48 C43 121.0(2) . . ? C47 C48 C43 124.2(2) . . ? C50 C49 C54 112.5(2) . . ? C50 C49 B3 127.3(2) . . ? C54 C49 B3 119.8(2) . . ? F13 C50 C51 115.0(2) . . ? F13 C50 C49 120.6(2) . . ? C51 C50 C49 124.4(3) . . ? F14 C51 C52 120.2(2) . . ? F14 C51 C50 119.7(3) . . ? C52 C51 C50 120.1(2) . . ? F15 C52 C51 121.1(3) . . ? F15 C52 C53 120.3(3) . . ? C51 C52 C53 118.6(2) . . ? F16 C53 C52 119.5(2) . . ? F16 C53 C54 121.1(3) . . ? C52 C53 C54 119.4(3) . . ? F17 C54 C53 116.2(2) . . ? F17 C54 C49 118.9(2) . . ? C53 C54 C49 124.9(3) . . ? C60 C55 C56 113.0(2) . . ? C60 C55 B3 127.8(2) . . ? C56 C55 B3 118.9(2) . . ? F18 C56 C57 116.1(2) . . ? F18 C56 C55 118.8(2) . . ? C57 C56 C55 125.0(2) . . ? F19 C57 C56 121.0(2) . . ? F19 C57 C58 119.8(2) . . ? C56 C57 C58 119.2(2) . . ? F20 C58 C59 120.6(2) . . ? F20 C58 C57 120.5(2) . . ? C59 C58 C57 119.0(2) . . ? F21 C59 C58 119.6(2) . . ? F21 C59 C60 120.8(2) . . ? C58 C59 C60 119.6(2) . . ? F22 C60 C59 115.0(2) . . ? F22 C60 C55 120.8(2) . . ? C59 C60 C55 124.2(2) . . ? C62 C61 C66 113.1(2) . . ? C62 C61 B4 126.5(2) . . ? C66 C61 B4 120.1(2) . . ? F23 C62 C63 114.7(3) . . ? F23 C62 C61 120.7(2) . . ? C63 C62 C61 124.6(3) . . ? F24 C63 C64 120.4(3) . . ? F24 C63 C62 120.2(3) . . ? C64 C63 C62 119.4(3) . . ? F25 C64 C63 120.6(3) . . ? F25 C64 C65 120.5(3) . . ? C63 C64 C65 119.0(3) . . ? F26 C65 C64 120.1(3) . . ? F26 C65 C66 120.3(3) . . ? C64 C65 C66 119.6(3) . . ? F27 C66 C65 116.6(3) . . ? F27 C66 C61 119.2(2) . . ? C65 C66 C61 124.2(3) . . ? C72 C67 C68 113.0(2) . . ? C72 C67 B4 127.2(2) . . ? C68 C67 B4 119.3(2) . . ? F28 C68 C69 116.3(2) . . ? F28 C68 C67 119.1(2) . . ? C69 C68 C67 124.6(3) . . ? F29 C69 C70 119.5(3) . . ? F29 C69 C68 120.8(3) . . ? C70 C69 C68 119.7(3) . . ? F30 C70 C69 121.1(3) . . ? F30 C70 C71 120.3(3) . . ? C69 C70 C71 118.6(3) . . ? F31 C71 C70 119.8(2) . . ? F31 C71 C72 120.2(2) . . ? C70 C71 C72 119.9(3) . . ? F32 C72 C67 120.8(2) . . ? F32 C72 C71 115.1(2) . . ? C67 C72 C71 124.1(2) . . ? C74 C73 C78 112.9(2) . . ? C74 C73 B4 119.3(2) . . ? C78 C73 B4 127.1(2) . . ? F33 C74 C75 116.0(2) . . ? F33 C74 C73 119.1(2) . . ? C75 C74 C73 124.9(2) . . ? F34 C75 C76 119.6(3) . . ? F34 C75 C74 121.0(2) . . ? C76 C75 C74 119.4(3) . . ? F35 C76 C77 120.8(2) . . ? F35 C76 C75 120.4(3) . . ? C77 C76 C75 118.8(3) . . ? F36 C77 C76 119.6(3) . . ? F36 C77 C78 120.3(3) . . ? C76 C77 C78 120.1(2) . . ? F37 C78 C77 114.7(2) . . ? F37 C78 C73 121.4(2) . . ? C77 C78 C73 123.9(2) . . ? C84 C79 C80 112.8(2) . . ? C84 C79 B4 127.5(2) . . ? C80 C79 B4 119.4(2) . . ? F38 C80 C81 116.0(2) . . ? F38 C80 C79 119.0(2) . . ? C81 C80 C79 125.0(2) . . ? F39 C81 C80 121.3(2) . . ? F39 C81 C82 119.8(3) . . ? C80 C81 C82 118.9(3) . . ? F40 C82 C83 120.2(3) . . ? F40 C82 C81 120.5(3) . . ? C83 C82 C81 119.3(3) . . ? F41 C83 C82 119.7(3) . . ? F41 C83 C84 120.7(3) . . ? C82 C83 C84 119.6(3) . . ? F42 C84 C83 115.3(2) . . ? F42 C84 C79 120.4(2) . . ? C83 C84 C79 124.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N2 B1 N1 178.3(3) . . . . ? C6 N2 B1 N1 2.9(4) . . . . ? C4 N1 B1 N2 -0.4(4) . . . . ? C1 N1 B1 N2 -178.5(3) . . . . ? B1 N1 C4 C5 -1.1(4) . . . . ? C1 N1 C4 C5 177.4(3) . . . . ? B1 N1 C4 C3 178.6(3) . . . . ? C1 N1 C4 C3 -2.9(3) . . . . ? C3 C4 C5 C6 -179.5(3) . . . . ? N1 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 C7 -178.2(3) . . . . ? C4 C5 C6 N2 2.4(4) . . . . ? B1 N2 C6 C5 -3.9(4) . . . . ? C9 N2 C6 C5 179.7(3) . . . . ? B1 N2 C6 C7 176.5(3) . . . . ? C9 N2 C6 C7 0.1(3) . . . . ? B1 N1 C1 C2 -179.1(3) . . . . ? C4 N1 C1 C2 2.7(3) . . . . ? B1 N1 C1 C10 7.3(5) . . . . ? C4 N1 C1 C10 -170.9(3) . . . . ? N1 C1 C2 C3 -1.5(4) . . . . ? C10 C1 C2 C3 171.7(3) . . . . ? N1 C1 C2 C11 176.6(3) . . . . ? C10 C1 C2 C11 -10.2(6) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C11 C2 C3 C4 -178.4(3) . . . . ? C1 C2 C3 C13 -178.8(3) . . . . ? C11 C2 C3 C13 3.2(5) . . . . ? C5 C4 C3 C2 -178.3(3) . . . . ? N1 C4 C3 C2 2.1(3) . . . . ? C5 C4 C3 C13 0.2(5) . . . . ? N1 C4 C3 C13 -179.4(3) . . . . ? C5 C6 C7 C8 -179.2(3) . . . . ? N2 C6 C7 C8 0.3(3) . . . . ? C5 C6 C7 C15 3.8(5) . . . . ? N2 C6 C7 C15 -176.7(3) . . . . ? C6 C7 C8 C9 -0.6(3) . . . . ? C15 C7 C8 C9 176.2(3) . . . . ? C6 C7 C8 C16 -177.9(3) . . . . ? C15 C7 C8 C16 -1.1(5) . . . . ? B1 N2 C9 C8 -176.3(3) . . . . ? C6 N2 C9 C8 -0.5(3) . . . . ? B1 N2 C9 C18 -0.7(5) . . . . ? C6 N2 C9 C18 175.1(3) . . . . ? C7 C8 C9 N2 0.7(3) . . . . ? C16 C8 C9 N2 177.9(3) . . . . ? C7 C8 C9 C18 -174.6(4) . . . . ? C16 C8 C9 C18 2.7(6) . . . . ? C3 C2 C11 C12 97.9(4) . . . . ? C1 C2 C11 C12 -79.8(4) . . . . ? C7 C8 C16 C17 81.4(4) . . . . ? C9 C8 C16 C17 -95.5(4) . . . . ? N4' N3 B2 N4' 1.2(4) 2_665 . . . ? C19 N3 B2 N4' 178.0(3) . . . . ? N3 B2 N4' N3 -1.3(4) . . . 2_665 ? N3 B2 N4' C21 178.0(3) . . . 2_665 ? C22 C24' C23' C22 -1.2(4) 2_665 . . . ? C19 C24' C23' C22 -178.0(3) 2_665 . . . ? C24' C23' C22 C24' 1.3(4) . . . 2_665 ? C24' C23' C22 C21 -178.0(3) . . . . ? N4' N3 C19 C20 0.6(3) 2_665 . . . ? B2 N3 C19 C20 -176.4(3) . . . . ? N4' N3 C19 C24' -92(100) 2_665 . . 2_665 ? B2 N3 C19 C24' 91(100) . . . 2_665 ? N4' N3 C19 C28 -173.7(3) 2_665 . . . ? B2 N3 C19 C28 9.3(5) . . . . ? C24' C19 C20 C21 -1.7(3) 2_665 . . . ? N3 C19 C20 C21 -1.7(3) . . . . ? C28 C19 C20 C21 172.3(3) . . . . ? C24' C19 C20 C29 176.8(3) 2_665 . . . ? N3 C19 C20 C29 176.8(3) . . . . ? C28 C19 C20 C29 -9.2(5) . . . . ? C19 C20 C21 N4' 2.2(4) . . . 2_665 ? C29 C20 C21 N4' -176.4(3) . . . 2_665 ? C19 C20 C21 C22 2.2(4) . . . . ? C29 C20 C21 C22 -176.4(3) . . . . ? C19 C20 C21 C31 -169.9(3) . . . . ? C29 C20 C21 C31 11.5(6) . . . . ? C24' C22 C21 C20 -1.8(3) 2_665 . . . ? C23' C22 C21 C20 177.6(3) . . . . ? C24' C22 C21 N4' -72(100) 2_665 . . 2_665 ? C23' C22 C21 N4' 107(100) . . . 2_665 ? C24' C22 C21 C31 170.8(3) 2_665 . . . ? C23' C22 C21 C31 -9.9(5) . . . . ? C19 C20 C29 C30 -93.5(4) . . . . ? C21 C20 C29 C30 84.9(4) . . . . ? C24 N4 B2' C24 -0.6(4) . . . 2_666 ? C27 N4 B2' C24 -178.6(2) . . . 2_666 ? C27 N4 C24 C25 0.2(3) . . . . ? B2' N4 C24 C25 -178.2(2) . . . . ? C27 N4 C24 B2' 179.0(2) . . . 2_666 ? B2' N4 C24 B2' 0.6(4) . . . 2_666 ? N3' C22' C23 N3' 0.6(4) . . . 2_666 ? C27 C22' C23 N3' 178.6(2) 2_666 . . 2_666 ? C27 C22' N3' C25 -0.2(3) 2_666 . . 2_666 ? C23 C22' N3' C25 178.2(2) . . . 2_666 ? C27 C22' N3' C23 -179.0(2) 2_666 . . 2_666 ? C23 C22' N3' C23 -0.6(4) . . . 2_666 ? N4 C24 C25 C26 0.4(3) . . . . ? B2' C24 C25 C26 -178.3(3) 2_666 . . . ? N4 C24 C25 N3' 43(100) . . . 2_666 ? B2' C24 C25 N3' -135(100) 2_666 . . 2_666 ? N4 C24 C25 C33 180.0(2) . . . . ? B2' C24 C25 C33 1.3(4) 2_666 . . . ? N3' C25 C26 C27 -0.8(3) 2_666 . . . ? C24 C25 C26 C27 -0.8(3) . . . . ? C33 C25 C26 C27 179.6(3) . . . . ? N3' C25 C26 C34 176.2(3) 2_666 . . . ? C24 C25 C26 C34 176.2(3) . . . . ? C33 C25 C26 C34 -3.4(5) . . . . ? C25 C26 C27 C22' 1.0(3) . . . 2_666 ? C34 C26 C27 C22' -176.1(3) . . . 2_666 ? C25 C26 C27 N4 1.0(3) . . . . ? C34 C26 C27 N4 -176.1(3) . . . . ? C25 C26 C27 C36 -177.5(3) . . . . ? C34 C26 C27 C36 5.5(5) . . . . ? C24 N4 C27 C26 -0.8(3) . . . . ? B2' N4 C27 C26 177.5(2) . . . . ? C24 N4 C27 C22' 13(100) . . . 2_666 ? B2' N4 C27 C22' -169(100) . . . 2_666 ? C24 N4 C27 C36 177.8(2) . . . . ? B2' N4 C27 C36 -4.0(4) . . . . ? C25 C26 C34 C35 -86.1(3) . . . . ? C27 C26 C34 C35 90.5(3) . . . . ? C55 B3 C37 C38 12.4(4) . . . . ? C43 B3 C37 C38 -110.3(3) . . . . ? C49 B3 C37 C38 127.6(3) . . . . ? C55 B3 C37 C42 -175.3(2) . . . . ? C43 B3 C37 C42 62.1(3) . . . . ? C49 B3 C37 C42 -60.0(3) . . . . ? C42 C37 C38 F3 -177.2(2) . . . . ? B3 C37 C38 F3 -4.4(4) . . . . ? C42 C37 C38 C39 1.2(4) . . . . ? B3 C37 C38 C39 174.1(2) . . . . ? F3 C38 C39 F4 -1.3(4) . . . . ? C37 C38 C39 F4 -179.8(2) . . . . ? F3 C38 C39 C40 177.5(2) . . . . ? C37 C38 C39 C40 -1.0(4) . . . . ? F4 C39 C40 F5 -0.3(4) . . . . ? C38 C39 C40 F5 -179.0(2) . . . . ? F4 C39 C40 C41 178.8(2) . . . . ? C38 C39 C40 C41 0.0(4) . . . . ? F5 C40 C41 F6 0.3(4) . . . . ? C39 C40 C41 F6 -178.8(2) . . . . ? F5 C40 C41 C42 179.6(2) . . . . ? C39 C40 C41 C42 0.6(4) . . . . ? F6 C41 C42 F7 -0.6(4) . . . . ? C40 C41 C42 F7 -180.0(2) . . . . ? F6 C41 C42 C37 179.1(2) . . . . ? C40 C41 C42 C37 -0.3(4) . . . . ? C38 C37 C42 F7 179.1(2) . . . . ? B3 C37 C42 F7 5.6(3) . . . . ? C38 C37 C42 C41 -0.6(4) . . . . ? B3 C37 C42 C41 -174.1(3) . . . . ? C55 B3 C43 C48 130.6(3) . . . . ? C37 B3 C43 C48 -107.3(3) . . . . ? C49 B3 C43 C48 15.1(4) . . . . ? C55 B3 C43 C44 -59.3(3) . . . . ? C37 B3 C43 C44 62.8(3) . . . . ? C49 B3 C43 C44 -174.8(2) . . . . ? C48 C43 C44 F8 179.2(2) . . . . ? B3 C43 C44 F8 7.8(4) . . . . ? C48 C43 C44 C45 -0.4(4) . . . . ? B3 C43 C44 C45 -171.8(3) . . . . ? F8 C44 C45 F9 0.5(4) . . . . ? C43 C44 C45 F9 -179.9(3) . . . . ? F8 C44 C45 C46 -178.7(3) . . . . ? C43 C44 C45 C46 0.9(5) . . . . ? F9 C45 C46 F10 0.4(4) . . . . ? C44 C45 C46 F10 179.7(3) . . . . ? F9 C45 C46 C47 179.9(3) . . . . ? C44 C45 C46 C47 -0.8(5) . . . . ? F10 C46 C47 F11 -1.1(4) . . . . ? C45 C46 C47 F11 179.4(3) . . . . ? F10 C46 C47 C48 179.8(3) . . . . ? C45 C46 C47 C48 0.3(4) . . . . ? F11 C47 C48 F12 -0.2(4) . . . . ? C46 C47 C48 F12 178.8(2) . . . . ? F11 C47 C48 C43 -178.8(3) . . . . ? C46 C47 C48 C43 0.2(5) . . . . ? C44 C43 C48 F12 -178.7(2) . . . . ? B3 C43 C48 F12 -8.1(4) . . . . ? C44 C43 C48 C47 -0.2(4) . . . . ? B3 C43 C48 C47 170.4(3) . . . . ? C55 B3 C49 C50 109.8(3) . . . . ? C43 B3 C49 C50 -127.5(3) . . . . ? C37 B3 C49 C50 -12.0(4) . . . . ? C55 B3 C49 C54 -62.6(3) . . . . ? C43 B3 C49 C54 60.1(3) . . . . ? C37 B3 C49 C54 175.6(2) . . . . ? C54 C49 C50 F13 177.7(2) . . . . ? B3 C49 C50 F13 4.8(4) . . . . ? C54 C49 C50 C51 -1.4(4) . . . . ? B3 C49 C50 C51 -174.3(2) . . . . ? F13 C50 C51 F14 0.2(3) . . . . ? C49 C50 C51 F14 179.3(2) . . . . ? F13 C50 C51 C52 -178.1(2) . . . . ? C49 C50 C51 C52 1.1(4) . . . . ? F14 C51 C52 F15 0.9(4) . . . . ? C50 C51 C52 F15 179.1(2) . . . . ? F14 C51 C52 C53 -178.6(2) . . . . ? C50 C51 C52 C53 -0.3(4) . . . . ? F15 C52 C53 F16 0.2(4) . . . . ? C51 C52 C53 F16 179.6(2) . . . . ? F15 C52 C53 C54 -179.3(2) . . . . ? C51 C52 C53 C54 0.1(4) . . . . ? F16 C53 C54 F17 0.5(4) . . . . ? C52 C53 C54 F17 180.0(2) . . . . ? F16 C53 C54 C49 179.9(2) . . . . ? C52 C53 C54 C49 -0.6(4) . . . . ? C50 C49 C54 F17 -179.4(2) . . . . ? B3 C49 C54 F17 -5.9(3) . . . . ? C50 C49 C54 C53 1.2(4) . . . . ? B3 C49 C54 C53 174.7(2) . . . . ? C43 B3 C55 C60 -13.1(4) . . . . ? C37 B3 C55 C60 -128.7(3) . . . . ? C49 B3 C55 C60 109.0(3) . . . . ? C43 B3 C55 C56 173.4(2) . . . . ? C37 B3 C55 C56 57.8(3) . . . . ? C49 B3 C55 C56 -64.5(3) . . . . ? C60 C55 C56 F18 -179.4(2) . . . . ? B3 C55 C56 F18 -5.0(3) . . . . ? C60 C55 C56 C57 1.2(4) . . . . ? B3 C55 C56 C57 175.6(2) . . . . ? F18 C56 C57 F19 0.9(3) . . . . ? C55 C56 C57 F19 -179.6(2) . . . . ? F18 C56 C57 C58 -179.2(2) . . . . ? C55 C56 C57 C58 0.3(4) . . . . ? F19 C57 C58 F20 -0.8(4) . . . . ? C56 C57 C58 F20 179.3(2) . . . . ? F19 C57 C58 C59 178.9(2) . . . . ? C56 C57 C58 C59 -1.0(4) . . . . ? F20 C58 C59 F21 1.1(4) . . . . ? C57 C58 C59 F21 -178.7(2) . . . . ? F20 C58 C59 C60 179.9(2) . . . . ? C57 C58 C59 C60 0.2(4) . . . . ? F21 C59 C60 F22 0.6(4) . . . . ? C58 C59 C60 F22 -178.2(2) . . . . ? F21 C59 C60 C55 -179.7(2) . . . . ? C58 C59 C60 C55 1.5(4) . . . . ? C56 C55 C60 F22 177.6(2) . . . . ? B3 C55 C60 F22 3.8(4) . . . . ? C56 C55 C60 C59 -2.0(4) . . . . ? B3 C55 C60 C59 -175.8(2) . . . . ? C79 B4 C61 C62 17.4(4) . . . . ? C73 B4 C61 C62 132.2(3) . . . . ? C67 B4 C61 C62 -104.8(3) . . . . ? C79 B4 C61 C66 -169.2(2) . . . . ? C73 B4 C61 C66 -54.4(3) . . . . ? C67 B4 C61 C66 68.7(3) . . . . ? C66 C61 C62 F23 -178.0(2) . . . . ? B4 C61 C62 F23 -4.2(4) . . . . ? C66 C61 C62 C63 1.5(4) . . . . ? B4 C61 C62 C63 175.3(2) . . . . ? F23 C62 C63 F24 1.1(4) . . . . ? C61 C62 C63 F24 -178.4(2) . . . . ? F23 C62 C63 C64 -179.2(2) . . . . ? C61 C62 C63 C64 1.3(4) . . . . ? F24 C63 C64 F25 -1.9(4) . . . . ? C62 C63 C64 F25 178.4(2) . . . . ? F24 C63 C64 C65 177.4(2) . . . . ? C62 C63 C64 C65 -2.3(4) . . . . ? F25 C64 C65 F26 -0.3(4) . . . . ? C63 C64 C65 F26 -179.6(2) . . . . ? F25 C64 C65 C66 179.7(2) . . . . ? C63 C64 C65 C66 0.4(4) . . . . ? F26 C65 C66 F27 1.6(4) . . . . ? C64 C65 C66 F27 -178.4(2) . . . . ? F26 C65 C66 C61 -177.3(2) . . . . ? C64 C65 C66 C61 2.7(4) . . . . ? C62 C61 C66 F27 177.6(2) . . . . ? B4 C61 C66 F27 3.4(4) . . . . ? C62 C61 C66 C65 -3.5(4) . . . . ? B4 C61 C66 C65 -177.7(2) . . . . ? C79 B4 C67 C72 132.7(3) . . . . ? C61 B4 C67 C72 -105.5(3) . . . . ? C73 B4 C67 C72 16.8(4) . . . . ? C79 B4 C67 C68 -55.6(3) . . . . ? C61 B4 C67 C68 66.1(3) . . . . ? C73 B4 C67 C68 -171.5(2) . . . . ? C72 C67 C68 F28 178.4(2) . . . . ? B4 C67 C68 F28 5.7(4) . . . . ? C72 C67 C68 C69 -0.7(4) . . . . ? B4 C67 C68 C69 -173.4(2) . . . . ? F28 C68 C69 F29 0.2(4) . . . . ? C67 C68 C69 F29 179.3(2) . . . . ? F28 C68 C69 C70 -178.5(2) . . . . ? C67 C68 C69 C70 0.6(4) . . . . ? F29 C69 C70 F30 -0.2(4) . . . . ? C68 C69 C70 F30 178.5(2) . . . . ? F29 C69 C70 C71 -178.7(2) . . . . ? C68 C69 C70 C71 0.0(4) . . . . ? F30 C70 C71 F31 -1.1(4) . . . . ? C69 C70 C71 F31 177.5(2) . . . . ? F30 C70 C71 C72 -178.9(2) . . . . ? C69 C70 C71 C72 -0.4(4) . . . . ? C68 C67 C72 F32 -179.0(2) . . . . ? B4 C67 C72 F32 -7.0(4) . . . . ? C68 C67 C72 C71 0.2(4) . . . . ? B4 C67 C72 C71 172.3(2) . . . . ? F31 C71 C72 F32 1.7(4) . . . . ? C70 C71 C72 F32 179.6(2) . . . . ? F31 C71 C72 C67 -177.6(2) . . . . ? C70 C71 C72 C67 0.3(4) . . . . ? C79 B4 C73 C74 -64.8(3) . . . . ? C61 B4 C73 C74 173.6(2) . . . . ? C67 B4 C73 C74 58.0(3) . . . . ? C79 B4 C73 C78 105.4(3) . . . . ? C61 B4 C73 C78 -16.3(4) . . . . ? C67 B4 C73 C78 -131.8(3) . . . . ? C78 C73 C74 F33 -178.6(2) . . . . ? B4 C73 C74 F33 -7.1(3) . . . . ? C78 C73 C74 C75 0.4(4) . . . . ? B4 C73 C74 C75 171.9(3) . . . . ? F33 C74 C75 F34 0.0(4) . . . . ? C73 C74 C75 F34 -179.0(2) . . . . ? F33 C74 C75 C76 178.6(2) . . . . ? C73 C74 C75 C76 -0.4(4) . . . . ? F34 C75 C76 F35 -0.5(4) . . . . ? C74 C75 C76 F35 -179.2(2) . . . . ? F34 C75 C76 C77 179.0(2) . . . . ? C74 C75 C76 C77 0.4(4) . . . . ? F35 C76 C77 F36 -0.4(4) . . . . ? C75 C76 C77 F36 -180.0(2) . . . . ? F35 C76 C77 C78 179.1(2) . . . . ? C75 C76 C77 C78 -0.4(4) . . . . ? F36 C77 C78 F37 1.5(3) . . . . ? C76 C77 C78 F37 -178.1(2) . . . . ? F36 C77 C78 C73 180.0(2) . . . . ? C76 C77 C78 C73 0.4(4) . . . . ? C74 C73 C78 F37 178.0(2) . . . . ? B4 C73 C78 F37 7.3(4) . . . . ? C74 C73 C78 C77 -0.4(4) . . . . ? B4 C73 C78 C77 -171.1(2) . . . . ? C61 B4 C79 C84 -131.4(3) . . . . ? C73 B4 C79 C84 106.8(3) . . . . ? C67 B4 C79 C84 -16.5(4) . . . . ? C61 B4 C79 C80 55.5(3) . . . . ? C73 B4 C79 C80 -66.3(3) . . . . ? C67 B4 C79 C80 170.4(2) . . . . ? C84 C79 C80 F38 -178.6(2) . . . . ? B4 C79 C80 F38 -4.5(4) . . . . ? C84 C79 C80 C81 2.3(4) . . . . ? B4 C79 C80 C81 176.4(3) . . . . ? F38 C80 C81 F39 -0.6(4) . . . . ? C79 C80 C81 F39 178.6(2) . . . . ? F38 C80 C81 C82 179.8(2) . . . . ? C79 C80 C81 C82 -1.0(4) . . . . ? F39 C81 C82 F40 0.1(4) . . . . ? C80 C81 C82 F40 179.7(3) . . . . ? F39 C81 C82 C83 179.8(3) . . . . ? C80 C81 C82 C83 -0.5(4) . . . . ? F40 C82 C83 F41 0.2(4) . . . . ? C81 C82 C83 F41 -179.6(3) . . . . ? F40 C82 C83 C84 -179.7(3) . . . . ? C81 C82 C83 C84 0.6(5) . . . . ? F41 C83 C84 F42 0.7(4) . . . . ? C82 C83 C84 F42 -179.4(3) . . . . ? F41 C83 C84 C79 -178.9(3) . . . . ? C82 C83 C84 C79 0.9(5) . . . . ? C80 C79 C84 F42 178.1(2) . . . . ? B4 C79 C84 F42 4.6(4) . . . . ? C80 C79 C84 C83 -2.2(4) . . . . ? B4 C79 C84 C83 -175.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.363 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.046 # Attachment '1.cif' data_Compound_I _database_code_depnum_ccdc_archive 'CCDC 689180' #----------------------------------------------------------------------------- _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SAPI91 (Fan, 1991)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #----------------------------------------------------------------------------- _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H23 B F2 N2' _chemical_formula_weight 304.18 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.554(2) _cell_length_b 9.258(4) _cell_length_c 12.068(5) _cell_angle_alpha 100.439(18) _cell_angle_beta 103.76(2) _cell_angle_gamma 113.981(19) _cell_volume 805.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6894 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9824 _exptl_absorpt_correction_T_max 0.9929 _exptl_absorpt_process_details 'SORTAV: (Blessing, 1997)' _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6894 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3646 _reflns_number_gt 2753 _reflns_threshold_expression >2sigma(I) _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^)+(0.0570P)^2^+0.3200P] 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 3646 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F 1.15855(13) 0.64149(12) 0.19618(8) 0.0351(2) Uani 1 1 d . . . F2 F 1.30258(11) 0.92308(12) 0.25579(8) 0.0347(2) Uani 1 1 d . . . N1 N 1.10842(15) 0.78665(15) 0.36072(11) 0.0232(3) Uani 1 1 d . . . N2 N 0.97635(16) 0.77993(15) 0.15053(11) 0.0241(3) Uani 1 1 d . . . C1 C 1.21829(19) 0.79126(18) 0.46387(13) 0.0245(3) Uani 1 1 d . . . C2 C 1.14124(19) 0.79963(18) 0.55474(13) 0.0251(3) Uani 1 1 d . . . C3 C 0.97506(19) 0.79559(18) 0.50284(13) 0.0252(3) Uani 1 1 d . . . C4 C 0.95609(18) 0.78922(17) 0.38204(13) 0.0234(3) Uani 1 1 d . . . C5 C 0.81921(19) 0.78625(18) 0.29154(13) 0.0253(3) Uani 1 1 d . . . H5 H 0.7167 0.7878 0.3083 0.030 Uiso 1 1 calc R . . C6 C 0.82644(19) 0.78111(18) 0.17769(13) 0.0255(3) Uani 1 1 d . . . C7 C 0.7036(2) 0.77735(19) 0.07337(13) 0.0278(3) Uani 1 1 d . . . C8 C 0.7809(2) 0.77610(19) -0.01542(13) 0.0275(3) Uani 1 1 d . . . C9 C 0.9490(2) 0.77705(18) 0.03501(13) 0.0260(3) Uani 1 1 d . . . C10 C 1.3903(2) 0.7805(2) 0.47245(14) 0.0305(3) Uani 1 1 d . . . H10A H 1.4727 0.8301 0.5563 0.037 Uiso 1 1 calc R . . H10B H 1.4494 0.8408 0.4229 0.037 Uiso 1 1 calc R . . H10C H 1.3614 0.6635 0.4438 0.037 Uiso 1 1 calc R . . C11 C 1.2215(2) 0.80255(19) 0.68078(13) 0.0291(3) Uani 1 1 d . . . H11A H 1.1874 0.8679 0.7357 0.035 Uiso 1 1 calc R . . H11B H 1.3562 0.8592 0.7054 0.035 Uiso 1 1 calc R . . C12 C 1.1574(3) 0.6296(2) 0.69324(16) 0.0421(4) Uani 1 1 d . . . H12A H 1.2167 0.6380 0.7760 0.051 Uiso 1 1 calc R . . H12B H 1.1892 0.5638 0.6382 0.051 Uiso 1 1 calc R . . H12C H 1.0248 0.5753 0.6736 0.051 Uiso 1 1 calc R . . C13 C 0.8362(2) 0.7911(2) 0.55957(14) 0.0333(4) Uani 1 1 d . . . H13A H 0.7326 0.7886 0.5013 0.050 Uiso 0.50 1 calc PR . . H13B H 0.8912 0.8905 0.6297 0.050 Uiso 0.50 1 calc PR . . H13C H 0.7937 0.6914 0.5849 0.050 Uiso 0.50 1 calc PR . . H13D H 0.8791 0.7918 0.6426 0.050 Uiso 0.50 1 calc PR . . H13E H 0.7205 0.6898 0.5142 0.050 Uiso 0.50 1 calc PR . . H13F H 0.8180 0.8889 0.5590 0.050 Uiso 0.50 1 calc PR . . C15 C 0.5225(2) 0.7717(2) 0.06262(16) 0.0391(4) Uani 1 1 d . . . H15A H 0.5033 0.7741 0.1397 0.059 Uiso 0.50 1 calc PR . . H15B H 0.4251 0.6691 0.0004 0.059 Uiso 0.50 1 calc PR . . H15C H 0.5210 0.8681 0.0407 0.059 Uiso 0.50 1 calc PR . . H15D H 0.4630 0.7668 -0.0191 0.059 Uiso 0.50 1 calc PR . . H15E H 0.5412 0.8718 0.1201 0.059 Uiso 0.50 1 calc PR . . H15F H 0.4453 0.6728 0.0798 0.059 Uiso 0.50 1 calc PR . . C16 C 0.7036(2) 0.7710(2) -0.14220(14) 0.0323(4) Uani 1 1 d . . . H16A H 0.8045 0.8375 -0.1675 0.039 Uiso 1 1 calc R . . H16B H 0.6223 0.8227 -0.1454 0.039 Uiso 1 1 calc R . . C17 C 0.5969(3) 0.5950(2) -0.22960(16) 0.0428(4) Uani 1 1 d . . . H17A H 0.5466 0.5983 -0.3105 0.051 Uiso 1 1 calc R . . H17B H 0.4971 0.5283 -0.2048 0.051 Uiso 1 1 calc R . . H17C H 0.6782 0.5450 -0.2299 0.051 Uiso 1 1 calc R . . C18 C 1.0802(2) 0.7726(2) -0.02565(14) 0.0332(4) Uani 1 1 d . . . H18A H 1.1846 0.7745 0.0312 0.050 Uiso 0.50 1 calc PR . . H18B H 1.1227 0.8697 -0.0538 0.050 Uiso 0.50 1 calc PR . . H18C H 1.0197 0.6707 -0.0943 0.050 Uiso 0.50 1 calc PR . . H18D H 1.0334 0.7688 -0.1091 0.050 Uiso 0.50 1 calc PR . . H18E H 1.0954 0.6735 -0.0241 0.050 Uiso 0.50 1 calc PR . . H18F H 1.1983 0.8726 0.0163 0.050 Uiso 0.50 1 calc PR . . B1 B 1.1424(2) 0.7824(2) 0.23976(15) 0.0246(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 F1 0.0428(5) 0.0416(6) 0.0335(5) 0.0107(4) 0.0163(4) 0.0301(5) F2 0.0230(4) 0.0416(6) 0.0342(5) 0.0158(4) 0.0102(4) 0.0084(4) N1 0.0202(6) 0.0252(6) 0.0257(6) 0.0080(5) 0.0081(5) 0.0119(5) N2 0.0225(6) 0.0277(7) 0.0243(6) 0.0083(5) 0.0097(5) 0.0127(5) C1 0.0228(7) 0.0233(7) 0.0261(7) 0.0072(6) 0.0064(6) 0.0110(6) C2 0.0250(7) 0.0223(7) 0.0264(7) 0.0075(6) 0.0083(6) 0.0102(6) C3 0.0252(7) 0.0240(7) 0.0272(7) 0.0078(6) 0.0109(6) 0.0113(6) C4 0.0218(7) 0.0237(7) 0.0266(7) 0.0075(6) 0.0104(6) 0.0115(6) C5 0.0223(7) 0.0265(7) 0.0296(8) 0.0087(6) 0.0107(6) 0.0127(6) C6 0.0212(7) 0.0283(8) 0.0285(8) 0.0089(6) 0.0085(6) 0.0130(6) C7 0.0251(7) 0.0297(8) 0.0286(8) 0.0090(6) 0.0067(6) 0.0143(6) C8 0.0265(7) 0.0265(8) 0.0276(8) 0.0085(6) 0.0069(6) 0.0121(6) C9 0.0271(7) 0.0256(8) 0.0256(7) 0.0083(6) 0.0095(6) 0.0122(6) C10 0.0255(8) 0.0370(9) 0.0321(8) 0.0109(7) 0.0088(6) 0.0181(7) C11 0.0286(8) 0.0320(8) 0.0242(7) 0.0077(6) 0.0079(6) 0.0132(6) C12 0.0536(11) 0.0413(10) 0.0332(9) 0.0157(8) 0.0121(8) 0.0238(9) C13 0.0315(8) 0.0422(10) 0.0322(8) 0.0127(7) 0.0172(7) 0.0190(7) C15 0.0304(8) 0.0550(11) 0.0367(9) 0.0148(8) 0.0088(7) 0.0258(8) C16 0.0341(8) 0.0359(9) 0.0276(8) 0.0128(7) 0.0079(6) 0.0176(7) C17 0.0446(10) 0.0431(10) 0.0315(9) 0.0071(8) 0.0049(8) 0.0186(8) C18 0.0318(8) 0.0424(9) 0.0285(8) 0.0114(7) 0.0146(7) 0.0179(7) B1 0.0216(8) 0.0283(9) 0.0265(8) 0.0094(7) 0.0096(6) 0.0132(7) _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 F1 B1 1.3891(19) . ? F2 B1 1.3938(19) . ? N1 C1 1.3514(19) . ? N1 C4 1.3954(17) . ? N1 B1 1.552(2) . ? N2 C9 1.3511(19) . ? N2 C6 1.4007(18) . ? N2 B1 1.554(2) . ? C1 C2 1.413(2) . ? C1 C10 1.495(2) . ? C2 C3 1.393(2) . ? C2 C11 1.503(2) . ? C3 C4 1.415(2) . ? C3 C13 1.496(2) . ? C4 C5 1.385(2) . ? C5 C6 1.383(2) . ? C5 H5 0.9500 . ? C6 C7 1.420(2) . ? C7 C8 1.387(2) . ? C7 C15 1.501(2) . ? C8 C9 1.418(2) . ? C8 C16 1.499(2) . ? C9 C18 1.488(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.516(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15D 0.9800 . ? C15 H15E 0.9800 . ? C15 H15F 0.9800 . ? C16 C17 1.520(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18D 0.9800 . ? C18 H18E 0.9800 . ? C18 H18F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 107.56(12) . . ? C1 N1 B1 127.45(12) . . ? C4 N1 B1 124.99(12) . . ? C9 N2 C6 107.62(12) . . ? C9 N2 B1 127.37(12) . . ? C6 N2 B1 125.01(12) . . ? N1 C1 C2 110.05(12) . . ? N1 C1 C10 122.41(13) . . ? C2 C1 C10 127.48(13) . . ? C3 C2 C1 106.86(13) . . ? C3 C2 C11 127.48(13) . . ? C1 C2 C11 125.58(13) . . ? C2 C3 C4 106.98(13) . . ? C2 C3 C13 127.70(14) . . ? C4 C3 C13 125.27(13) . . ? C5 C4 N1 120.45(13) . . ? C5 C4 C3 131.02(13) . . ? N1 C4 C3 108.53(12) . . ? C6 C5 C4 122.33(13) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 N2 120.17(13) . . ? C5 C6 C7 131.55(13) . . ? N2 C6 C7 108.28(13) . . ? C8 C7 C6 107.12(13) . . ? C8 C7 C15 127.31(14) . . ? C6 C7 C15 125.56(14) . . ? C7 C8 C9 107.06(13) . . ? C7 C8 C16 127.72(14) . . ? C9 C8 C16 125.21(14) . . ? N2 C9 C8 109.92(13) . . ? N2 C9 C18 122.65(13) . . ? C8 C9 C18 127.42(14) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 C12 112.61(13) . . ? C2 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C2 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C13 H13D 109.5 . . ? H13A C13 H13D 141.1 . . ? H13B C13 H13D 56.3 . . ? H13C C13 H13D 56.3 . . ? C3 C13 H13E 109.5 . . ? H13A C13 H13E 56.3 . . ? H13B C13 H13E 141.1 . . ? H13C C13 H13E 56.3 . . ? H13D C13 H13E 109.5 . . ? C3 C13 H13F 109.5 . . ? H13A C13 H13F 56.3 . . ? H13B C13 H13F 56.3 . . ? H13C C13 H13F 141.1 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C15 H15D 109.5 . . ? H15A C15 H15D 141.1 . . ? H15B C15 H15D 56.3 . . ? H15C C15 H15D 56.3 . . ? C7 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.1 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C7 C15 H15F 109.5 . . ? H15A C15 H15F 56.3 . . ? H15B C15 H15F 56.3 . . ? H15C C15 H15F 141.1 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? C8 C16 C17 112.72(14) . . ? C8 C16 H16A 109.0 . . ? C17 C16 H16A 109.0 . . ? C8 C16 H16B 109.0 . . ? C17 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C9 C18 H18A 109.5 . . ? C9 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C9 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C9 C18 H18D 109.5 . . ? H18A C18 H18D 141.1 . . ? H18B C18 H18D 56.3 . . ? H18C C18 H18D 56.3 . . ? C9 C18 H18E 109.5 . . ? H18A C18 H18E 56.3 . . ? H18B C18 H18E 141.1 . . ? H18C C18 H18E 56.3 . . ? H18D C18 H18E 109.5 . . ? C9 C18 H18F 109.5 . . ? H18A C18 H18F 56.3 . . ? H18B C18 H18F 56.3 . . ? H18C C18 H18F 141.1 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? F1 B1 F2 108.79(12) . . ? F1 B1 N1 110.40(12) . . ? F2 B1 N1 110.04(12) . . ? F1 B1 N2 110.35(12) . . ? F2 B1 N2 110.22(12) . . ? N1 B1 N2 107.05(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C2 -0.94(16) . . . . ? B1 N1 C1 C2 178.05(13) . . . . ? C4 N1 C1 C10 176.45(13) . . . . ? B1 N1 C1 C10 -4.6(2) . . . . ? N1 C1 C2 C3 1.55(17) . . . . ? C10 C1 C2 C3 -175.68(14) . . . . ? N1 C1 C2 C11 178.47(13) . . . . ? C10 C1 C2 C11 1.2(2) . . . . ? C1 C2 C3 C4 -1.50(16) . . . . ? C11 C2 C3 C4 -178.35(14) . . . . ? C1 C2 C3 C13 176.05(15) . . . . ? C11 C2 C3 C13 -0.8(3) . . . . ? C1 N1 C4 C5 179.73(13) . . . . ? B1 N1 C4 C5 0.7(2) . . . . ? C1 N1 C4 C3 -0.02(16) . . . . ? B1 N1 C4 C3 -179.05(13) . . . . ? C2 C3 C4 C5 -178.74(15) . . . . ? C13 C3 C4 C5 3.6(3) . . . . ? C2 C3 C4 N1 0.97(16) . . . . ? C13 C3 C4 N1 -176.66(14) . . . . ? N1 C4 C5 C6 -0.2(2) . . . . ? C3 C4 C5 C6 179.52(15) . . . . ? C4 C5 C6 N2 -0.5(2) . . . . ? C4 C5 C6 C7 179.97(15) . . . . ? C9 N2 C6 C5 -179.15(14) . . . . ? B1 N2 C6 C5 0.6(2) . . . . ? C9 N2 C6 C7 0.51(16) . . . . ? B1 N2 C6 C7 -179.76(13) . . . . ? C5 C6 C7 C8 178.85(16) . . . . ? N2 C6 C7 C8 -0.75(17) . . . . ? C5 C6 C7 C15 -2.5(3) . . . . ? N2 C6 C7 C15 177.92(15) . . . . ? C6 C7 C8 C9 0.70(17) . . . . ? C15 C7 C8 C9 -177.95(15) . . . . ? C6 C7 C8 C16 179.48(15) . . . . ? C15 C7 C8 C16 0.8(3) . . . . ? C6 N2 C9 C8 -0.07(17) . . . . ? B1 N2 C9 C8 -179.80(13) . . . . ? C6 N2 C9 C18 -179.09(14) . . . . ? B1 N2 C9 C18 1.2(2) . . . . ? C7 C8 C9 N2 -0.40(17) . . . . ? C16 C8 C9 N2 -179.23(14) . . . . ? C7 C8 C9 C18 178.56(15) . . . . ? C16 C8 C9 C18 -0.3(3) . . . . ? C3 C2 C11 C12 86.50(19) . . . . ? C1 C2 C11 C12 -89.79(18) . . . . ? C7 C8 C16 C17 -93.6(2) . . . . ? C9 C8 C16 C17 85.0(2) . . . . ? C1 N1 B1 F1 60.50(19) . . . . ? C4 N1 B1 F1 -120.67(14) . . . . ? C1 N1 B1 F2 -59.59(19) . . . . ? C4 N1 B1 F2 119.24(14) . . . . ? C1 N1 B1 N2 -179.37(13) . . . . ? C4 N1 B1 N2 -0.54(19) . . . . ? C9 N2 B1 F1 -60.26(19) . . . . ? C6 N2 B1 F1 120.06(15) . . . . ? C9 N2 B1 F2 59.92(19) . . . . ? C6 N2 B1 F2 -119.76(15) . . . . ? C9 N2 B1 N1 179.58(13) . . . . ? C6 N2 B1 N1 -0.10(19) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.250 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.040