# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Warren Piers' _publ_contact_author_email WPIERS@UCALGARY.CA _publ_section_title ; Spirocyclic Boronium Ions: Precursors to Persistent Neutral Radicals. ; loop_ _publ_author_name 'Warren Piers' 'Brian Keay' 'Masood Parvez' 'Thomas K. Wood' # Attachment '1_Me.cif' data_Compound_I _database_code_depnum_ccdc_archive 'CCDC 736470' #----------------------------------------------------------------------------- _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)' #----------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50.50 H45 B4 Cl F8 N4' _chemical_formula_weight 938.59 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' Cl Cl 0.1484 0.1585 '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 10.8262(3) _cell_length_b 13.2946(2) _cell_length_c 17.0262(4) _cell_angle_alpha 81.4549(13) _cell_angle_beta 83.1495(10) _cell_angle_gamma 71.8584(11) _cell_volume 2295.95(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9744 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9544 _exptl_absorpt_correction_T_max 0.9693 _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 'Bruker APEX2 CCD' _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 19376 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.45 _reflns_number_total 10376 _reflns_number_gt 7774 _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^)+(0.0620P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10376 _refine_ls_number_parameters 636 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.1996 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _exptl_special_details ; The asymmetric unit contains a half molecule of dichloromethane with gross disorder, its H-atoms were ignored. ; 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 0.4416(2) 0.20771(17) 0.85271(13) 0.0280(5) Uani 1 1 d . . . N2 N 0.3207(2) 0.38458(17) 0.81222(13) 0.0271(5) Uani 1 1 d . . . B1 B 0.3034(3) 0.2688(2) 0.81687(18) 0.0276(6) Uani 1 1 d . . . N3 N 0.3896(2) 0.29843(17) 0.33447(13) 0.0278(5) Uani 1 1 d . . . N4 N 0.2788(2) 0.19521(17) 0.28809(14) 0.0301(5) Uani 1 1 d . . . B2 B 0.2581(3) 0.3188(2) 0.29125(19) 0.0286(6) Uani 1 1 d . . . C1 C 0.4882(3) 0.1020(2) 0.87338(16) 0.0313(6) Uani 1 1 d . . . H1 H 0.4410 0.0566 0.8631 0.038 Uiso 1 1 calc R . . C2 C 0.6044(3) 0.0585(2) 0.90952(16) 0.0344(6) Uani 1 1 d . . . C3 C 0.6712(3) 0.1278(2) 0.92290(18) 0.0380(6) Uani 1 1 d . . . H3 H 0.7503 0.1000 0.9484 0.046 Uiso 1 1 calc R . . C4 C 0.6250(3) 0.2361(2) 0.89980(17) 0.0341(6) Uani 1 1 d . . . H4 H 0.6718 0.2829 0.9079 0.041 Uiso 1 1 calc R . . C5 C 0.5084(3) 0.2738(2) 0.86450(15) 0.0291(5) Uani 1 1 d . . . C6 C 0.4345(2) 0.3836(2) 0.83792(15) 0.0275(5) Uani 1 1 d . . . C7 C 0.4643(3) 0.4778(2) 0.83771(17) 0.0330(6) Uani 1 1 d . . . H7 H 0.5450 0.4771 0.8547 0.040 Uiso 1 1 calc R . . C8 C 0.3742(3) 0.5721(2) 0.81227(17) 0.0348(6) Uani 1 1 d . . . H8 H 0.3930 0.6373 0.8121 0.042 Uiso 1 1 calc R . . C9 C 0.2557(3) 0.5739(2) 0.78676(17) 0.0322(6) Uani 1 1 d . . . C10 C 0.2333(3) 0.4768(2) 0.78692(16) 0.0309(6) Uani 1 1 d . . . H10 H 0.1543 0.4754 0.7687 0.037 Uiso 1 1 calc R . . C11 C 0.6547(3) -0.0593(2) 0.9348(2) 0.0452(8) Uani 1 1 d . . . H11A H 0.5856 -0.0920 0.9331 0.068 Uiso 1 1 calc R . . H11B H 0.6818 -0.0716 0.9891 0.068 Uiso 1 1 calc R . . H11C H 0.7294 -0.0912 0.8985 0.068 Uiso 1 1 calc R . . C12 C 0.1543(3) 0.6754(2) 0.7599(2) 0.0443(7) Uani 1 1 d . . . H12A H 0.0943 0.6597 0.7281 0.066 Uiso 1 1 calc R . . H12B H 0.1967 0.7245 0.7275 0.066 Uiso 1 1 calc R . . H12C H 0.1056 0.7083 0.8066 0.066 Uiso 1 1 calc R . . C13 C 0.1873(3) 0.2549(2) 0.88011(17) 0.0312(6) Uani 1 1 d . . . C14 C 0.1636(3) 0.2984(3) 0.95273(18) 0.0402(7) Uani 1 1 d . . . H14 H 0.2128 0.3428 0.9621 0.048 Uiso 1 1 calc R . . C15 C 0.0708(3) 0.2783(3) 1.0111(2) 0.0524(9) Uani 1 1 d . . . H15 H 0.0557 0.3097 1.0593 0.063 Uiso 1 1 calc R . . C16 C 0.0006(3) 0.2127(3) 0.9985(2) 0.0578(10) Uani 1 1 d . . . H16 H -0.0613 0.1965 1.0388 0.069 Uiso 1 1 calc R . . C17 C 0.0207(3) 0.1704(3) 0.9272(2) 0.0526(9) Uani 1 1 d . . . H17 H -0.0281 0.1251 0.9191 0.063 Uiso 1 1 calc R . . C18 C 0.1112(3) 0.1925(2) 0.86611(19) 0.0380(7) Uani 1 1 d . . . C19 C 0.1209(3) 0.1490(3) 0.7882(2) 0.0456(8) Uani 1 1 d . . . H19A H 0.0323 0.1710 0.7692 0.055 Uiso 1 1 calc R . . H19B H 0.1491 0.0702 0.7986 0.055 Uiso 1 1 calc R . . C20 C 0.2113(3) 0.1810(2) 0.72113(18) 0.0359(6) Uani 1 1 d . . . C21 C 0.2076(3) 0.1530(3) 0.6453(2) 0.0480(8) Uani 1 1 d . . . H21 H 0.1498 0.1148 0.6380 0.058 Uiso 1 1 calc R . . C22 C 0.2860(4) 0.1798(3) 0.5816(2) 0.0534(9) Uani 1 1 d . . . H22 H 0.2811 0.1608 0.5307 0.064 Uiso 1 1 calc R . . C23 C 0.3723(3) 0.2343(3) 0.59081(19) 0.0475(8) Uani 1 1 d . . . H23 H 0.4273 0.2523 0.5468 0.057 Uiso 1 1 calc R . . C24 C 0.3771(3) 0.2624(2) 0.66543(17) 0.0361(6) Uani 1 1 d . . . H24 H 0.4363 0.2998 0.6719 0.043 Uiso 1 1 calc R . . C25 C 0.2971(3) 0.2370(2) 0.73171(16) 0.0302(6) Uani 1 1 d . . . C26 C 0.4327(3) 0.3742(2) 0.35578(16) 0.0309(6) Uani 1 1 d . . . H26 H 0.3826 0.4470 0.3462 0.037 Uiso 1 1 calc R . . C27 C 0.5491(3) 0.3480(2) 0.39167(16) 0.0335(6) Uani 1 1 d . . . C28 C 0.6187(3) 0.2404(3) 0.40587(18) 0.0399(7) Uani 1 1 d . . . H28 H 0.6977 0.2202 0.4314 0.048 Uiso 1 1 calc R . . C29 C 0.5748(3) 0.1625(3) 0.38335(18) 0.0390(7) Uani 1 1 d . . . H29 H 0.6229 0.0892 0.3923 0.047 Uiso 1 1 calc R . . C30 C 0.4585(3) 0.1945(2) 0.34737(16) 0.0315(6) Uani 1 1 d . . . C31 C 0.3888(3) 0.1302(2) 0.31919(17) 0.0313(6) Uani 1 1 d . . . C32 C 0.4189(3) 0.0206(2) 0.32279(19) 0.0389(7) Uani 1 1 d . . . H32 H 0.4985 -0.0248 0.3425 0.047 Uiso 1 1 calc R . . C33 C 0.3313(3) -0.0216(2) 0.2972(2) 0.0404(7) Uani 1 1 d . . . H33 H 0.3498 -0.0967 0.3004 0.048 Uiso 1 1 calc R . . C34 C 0.2156(3) 0.0452(2) 0.26677(19) 0.0378(6) Uani 1 1 d . . . C35 C 0.1944(3) 0.1544(2) 0.26202(18) 0.0345(6) Uani 1 1 d . . . H35 H 0.1180 0.2016 0.2397 0.041 Uiso 1 1 calc R . . C36 C 0.5965(3) 0.4336(3) 0.41490(19) 0.0431(7) Uani 1 1 d . . . H36A H 0.5314 0.5031 0.4038 0.065 Uiso 1 1 calc R . . H36B H 0.6790 0.4337 0.3841 0.065 Uiso 1 1 calc R . . H36C H 0.6100 0.4197 0.4719 0.065 Uiso 1 1 calc R . . C37 C 0.1155(3) 0.0029(3) 0.2402(2) 0.0505(8) Uani 1 1 d . . . H37A H 0.1341 -0.0060 0.1835 0.076 Uiso 1 1 calc R . . H37B H 0.0285 0.0532 0.2489 0.076 Uiso 1 1 calc R . . H37C H 0.1188 -0.0661 0.2711 0.076 Uiso 1 1 calc R . . C38 C 0.1306(2) 0.3699(2) 0.34546(16) 0.0280(5) Uani 1 1 d . . . C39 C 0.0845(3) 0.3116(2) 0.41157(17) 0.0352(6) Uani 1 1 d . . . H39 H 0.1297 0.2381 0.4236 0.042 Uiso 1 1 calc R . . C40 C -0.0247(3) 0.3574(3) 0.45999(18) 0.0385(7) Uani 1 1 d . . . H40 H -0.0534 0.3160 0.5046 0.046 Uiso 1 1 calc R . . C41 C -0.0920(3) 0.4646(3) 0.44262(18) 0.0386(7) Uani 1 1 d . . . H41 H -0.1670 0.4971 0.4754 0.046 Uiso 1 1 calc R . . C42 C -0.0494(3) 0.5240(2) 0.37736(17) 0.0346(6) Uani 1 1 d . . . H42 H -0.0956 0.5974 0.3658 0.041 Uiso 1 1 calc R . . C43 C 0.0608(2) 0.4778(2) 0.32793(16) 0.0295(5) Uani 1 1 d . . . C44 C 0.1032(3) 0.5468(2) 0.25797(18) 0.0343(6) Uani 1 1 d . . . H44A H 0.1510 0.5891 0.2780 0.041 Uiso 1 1 calc R . . H44B H 0.0240 0.5978 0.2354 0.041 Uiso 1 1 calc R . . C45 C 0.1879(3) 0.4897(2) 0.19141(16) 0.0298(6) Uani 1 1 d . . . C46 C 0.1919(3) 0.5460(2) 0.11528(17) 0.0365(6) Uani 1 1 d . . . H46 H 0.1365 0.6171 0.1059 0.044 Uiso 1 1 calc R . . C47 C 0.2748(3) 0.5001(3) 0.05371(18) 0.0425(7) Uani 1 1 d . . . H47 H 0.2761 0.5394 0.0024 0.051 Uiso 1 1 calc R . . C48 C 0.3563(3) 0.3965(3) 0.06688(18) 0.0407(7) Uani 1 1 d . . . H48 H 0.4162 0.3655 0.0253 0.049 Uiso 1 1 calc R . . C49 C 0.3498(3) 0.3386(2) 0.14112(17) 0.0332(6) Uani 1 1 d . . . H49 H 0.4033 0.2667 0.1492 0.040 Uiso 1 1 calc R . . C50 C 0.2661(2) 0.3833(2) 0.20481(16) 0.0285(5) Uani 1 1 d . . . B3 B 0.2638(3) 0.7122(3) 0.3635(2) 0.0384(7) Uani 1 1 d . . . F1 F 0.1332(2) 0.76362(18) 0.35455(15) 0.0681(6) Uani 1 1 d . . . F2 F 0.3098(2) 0.76013(18) 0.41517(13) 0.0646(6) Uani 1 1 d . . . F3 F 0.3320(2) 0.7188(2) 0.28999(13) 0.0779(8) Uani 1 1 d . . . F4 F 0.2787(2) 0.60721(15) 0.39359(13) 0.0601(6) Uani 1 1 d . . . B4 B 0.7003(4) 0.1420(3) 0.1333(2) 0.0410(8) Uani 1 1 d . . . F5 F 0.6725(2) 0.23684(16) 0.08343(13) 0.0577(5) Uani 1 1 d . A . F6 F 0.6570(6) 0.0723(3) 0.1073(2) 0.125(2) Uani 0.763(3) 1 d P A 1 F7 F 0.8295(3) 0.1067(3) 0.1434(3) 0.1141(19) Uani 0.763(3) 1 d P A 1 F8 F 0.6438(5) 0.1667(3) 0.2069(2) 0.0989(14) Uani 0.763(3) 1 d P A 1 F6' F 0.792(2) 0.0657(10) 0.0903(8) 0.125(2) Uani 0.237(3) 1 d P A 2 F7' F 0.7633(12) 0.1291(10) 0.1984(12) 0.1141(19) Uani 0.237(3) 1 d P A 2 F8' F 0.5919(15) 0.1078(10) 0.1758(7) 0.0989(14) Uani 0.237(3) 1 d P A 2 Cl1 Cl 0.86435(17) -0.00330(13) 0.50588(11) 0.0777(6) Uani 0.712(4) 1 d P . . Cl2 Cl 0.9457(7) 0.0638(5) 0.4271(4) 0.131(3) Uani 0.288(4) 1 d P . . C51 C 1.0292(16) -0.0708(12) 0.4876(13) 0.082(5) Uani 0.3560(18) 1 d P . 1 C51' C 1.058(5) -0.037(4) 0.467(4) 0.082(5) Uani 0.1440(18) 1 d P . 2 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 0.0269(11) 0.0303(11) 0.0270(11) -0.0026(9) -0.0033(9) -0.0086(9) N2 0.0253(11) 0.0290(11) 0.0285(11) -0.0023(9) -0.0056(9) -0.0094(9) B1 0.0272(14) 0.0243(13) 0.0313(15) 0.0000(11) -0.0071(12) -0.0076(11) N3 0.0252(11) 0.0289(11) 0.0276(11) -0.0014(9) -0.0041(9) -0.0055(9) N4 0.0276(11) 0.0252(11) 0.0357(12) -0.0022(9) -0.0044(9) -0.0055(9) B2 0.0256(14) 0.0241(14) 0.0353(16) -0.0006(12) -0.0086(12) -0.0055(11) C1 0.0323(14) 0.0288(13) 0.0300(14) -0.0011(11) -0.0032(11) -0.0057(11) C2 0.0340(14) 0.0366(15) 0.0264(14) 0.0011(11) -0.0014(11) -0.0041(12) C3 0.0264(13) 0.0478(17) 0.0347(15) -0.0009(13) -0.0069(11) -0.0042(12) C4 0.0288(13) 0.0401(15) 0.0329(15) -0.0035(12) -0.0058(11) -0.0088(12) C5 0.0289(13) 0.0329(14) 0.0262(13) -0.0037(10) -0.0019(10) -0.0104(11) C6 0.0242(12) 0.0326(13) 0.0263(13) -0.0038(10) -0.0030(10) -0.0090(10) C7 0.0311(14) 0.0356(14) 0.0367(15) -0.0051(12) -0.0057(11) -0.0148(11) C8 0.0415(16) 0.0307(14) 0.0368(15) -0.0083(11) -0.0023(12) -0.0154(12) C9 0.0340(14) 0.0310(14) 0.0317(14) -0.0059(11) -0.0020(11) -0.0089(11) C10 0.0280(13) 0.0314(14) 0.0345(14) -0.0040(11) -0.0076(11) -0.0087(11) C11 0.0436(17) 0.0364(16) 0.0448(18) 0.0043(13) -0.0071(14) 0.0008(13) C12 0.0427(17) 0.0319(15) 0.057(2) -0.0058(14) -0.0081(15) -0.0069(13) C13 0.0258(13) 0.0318(14) 0.0344(14) 0.0030(11) -0.0061(11) -0.0081(11) C14 0.0321(15) 0.0471(17) 0.0376(16) -0.0022(13) -0.0029(12) -0.0075(13) C15 0.0414(18) 0.065(2) 0.0361(17) 0.0056(16) 0.0029(14) -0.0018(16) C16 0.0361(17) 0.064(2) 0.056(2) 0.0211(18) 0.0063(16) -0.0071(16) C17 0.0348(16) 0.0453(19) 0.073(3) 0.0195(17) -0.0052(16) -0.0167(14) C18 0.0303(14) 0.0309(14) 0.0498(18) 0.0103(12) -0.0093(13) -0.0096(11) C19 0.0472(18) 0.0354(16) 0.062(2) 0.0018(14) -0.0179(16) -0.0216(14) C20 0.0359(15) 0.0273(13) 0.0450(17) -0.0025(12) -0.0163(13) -0.0061(11) C21 0.0513(19) 0.0389(17) 0.057(2) -0.0113(15) -0.0285(17) -0.0072(14) C22 0.060(2) 0.056(2) 0.0398(18) -0.0137(16) -0.0229(17) -0.0008(17) C23 0.0518(19) 0.0486(19) 0.0333(16) -0.0043(14) -0.0082(14) -0.0009(15) C24 0.0372(15) 0.0325(14) 0.0355(15) -0.0025(12) -0.0060(12) -0.0054(12) C25 0.0297(13) 0.0251(12) 0.0343(14) -0.0002(10) -0.0107(11) -0.0044(10) C26 0.0290(13) 0.0337(14) 0.0295(14) -0.0042(11) -0.0021(11) -0.0087(11) C27 0.0290(13) 0.0473(17) 0.0260(13) -0.0046(12) -0.0017(11) -0.0139(12) C28 0.0291(14) 0.0547(19) 0.0346(16) -0.0046(13) -0.0088(12) -0.0087(13) C29 0.0308(14) 0.0417(16) 0.0379(16) -0.0006(13) -0.0087(12) -0.0010(12) C30 0.0280(13) 0.0305(13) 0.0310(14) 0.0003(11) -0.0021(11) -0.0032(11) C31 0.0295(13) 0.0271(13) 0.0334(14) 0.0002(11) -0.0032(11) -0.0042(11) C32 0.0375(15) 0.0294(14) 0.0433(17) 0.0008(12) -0.0047(13) -0.0024(12) C33 0.0424(16) 0.0242(13) 0.0515(19) -0.0037(12) 0.0035(14) -0.0086(12) C34 0.0369(15) 0.0318(14) 0.0454(17) -0.0075(12) 0.0035(13) -0.0124(12) C35 0.0304(14) 0.0304(14) 0.0434(16) -0.0045(12) -0.0058(12) -0.0090(11) C36 0.0371(16) 0.059(2) 0.0408(17) -0.0119(15) -0.0071(13) -0.0207(15) C37 0.0442(18) 0.0400(17) 0.074(2) -0.0150(16) -0.0010(17) -0.0200(15) C38 0.0256(12) 0.0284(13) 0.0305(13) -0.0030(10) -0.0077(10) -0.0071(10) C39 0.0343(14) 0.0338(14) 0.0359(15) 0.0003(12) -0.0067(12) -0.0086(12) C40 0.0351(15) 0.0468(17) 0.0343(15) -0.0029(13) -0.0007(12) -0.0149(13) C41 0.0282(14) 0.0505(18) 0.0378(16) -0.0131(13) -0.0029(12) -0.0092(13) C42 0.0289(14) 0.0356(15) 0.0385(15) -0.0089(12) -0.0091(11) -0.0044(11) C43 0.0254(12) 0.0307(13) 0.0338(14) -0.0071(11) -0.0082(10) -0.0066(10) C44 0.0337(14) 0.0244(13) 0.0429(16) -0.0016(11) -0.0084(12) -0.0050(11) C45 0.0284(13) 0.0292(13) 0.0345(14) -0.0010(11) -0.0094(11) -0.0114(11) C46 0.0381(15) 0.0360(15) 0.0367(15) 0.0042(12) -0.0138(12) -0.0127(12) C47 0.0500(18) 0.0530(19) 0.0287(15) 0.0021(13) -0.0114(13) -0.0215(15) C48 0.0430(17) 0.0515(18) 0.0320(15) -0.0109(13) -0.0024(13) -0.0181(14) C49 0.0315(14) 0.0336(14) 0.0354(15) -0.0062(11) -0.0052(11) -0.0093(11) C50 0.0262(12) 0.0284(13) 0.0333(14) -0.0036(11) -0.0073(10) -0.0098(10) B3 0.0390(18) 0.0409(18) 0.0376(18) -0.0015(14) -0.0033(14) -0.0164(15) F1 0.0529(13) 0.0646(14) 0.0767(16) 0.0041(12) -0.0167(11) -0.0046(11) F2 0.0909(17) 0.0696(14) 0.0513(12) -0.0108(10) -0.0121(11) -0.0455(13) F3 0.0790(16) 0.129(2) 0.0412(12) -0.0200(13) 0.0148(11) -0.0566(16) F4 0.0751(15) 0.0375(10) 0.0666(14) -0.0034(9) -0.0169(11) -0.0123(10) B4 0.0377(18) 0.0420(19) 0.044(2) -0.0079(16) -0.0015(15) -0.0128(15) F5 0.0682(14) 0.0429(11) 0.0573(13) -0.0044(9) -0.0051(10) -0.0105(10) F6 0.261(6) 0.088(2) 0.086(3) 0.037(2) -0.091(3) -0.129(3) F7 0.0401(19) 0.076(2) 0.204(5) 0.057(3) -0.011(2) -0.0195(18) F8 0.153(4) 0.082(3) 0.0479(19) -0.0035(16) 0.013(2) -0.024(2) F6' 0.261(6) 0.088(2) 0.086(3) 0.037(2) -0.091(3) -0.129(3) F7' 0.0401(19) 0.076(2) 0.204(5) 0.057(3) -0.011(2) -0.0195(18) F8' 0.153(4) 0.082(3) 0.0479(19) -0.0035(16) 0.013(2) -0.024(2) Cl1 0.0731(11) 0.0648(10) 0.0955(13) -0.0177(8) -0.0103(9) -0.0158(8) Cl2 0.139(6) 0.109(4) 0.113(5) -0.029(4) -0.015(4) 0.018(4) C51 0.062(9) 0.061(10) 0.138(15) -0.052(10) -0.006(8) -0.022(6) C51' 0.062(9) 0.061(10) 0.138(15) -0.052(10) -0.006(8) -0.022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.344(3) . ? N1 C5 1.348(3) . ? N1 B1 1.608(4) . ? N2 C10 1.342(3) . ? N2 C6 1.351(3) . ? N2 B1 1.598(3) . ? B1 C25 1.584(4) . ? B1 C13 1.592(4) . ? N3 C26 1.344(3) . ? N3 C30 1.349(3) . ? N3 B2 1.610(3) . ? N4 C35 1.342(3) . ? N4 C31 1.349(3) . ? N4 B2 1.596(4) . ? B2 C38 1.587(4) . ? B2 C50 1.597(4) . ? C1 C2 1.386(4) . ? C1 H1 0.9500 . ? C2 C3 1.393(4) . ? C2 C11 1.504(4) . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.461(4) . ? C6 C7 1.387(4) . ? C7 C8 1.375(4) . ? C7 H7 0.9500 . ? C8 C9 1.395(4) . ? C8 H8 0.9500 . ? C9 C10 1.385(4) . ? C9 C12 1.500(4) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.399(4) . ? C13 C14 1.404(4) . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.376(6) . ? C15 H15 0.9500 . ? C16 C17 1.379(6) . ? C16 H16 0.9500 . ? C17 C18 1.404(4) . ? C17 H17 0.9500 . ? C18 C19 1.504(5) . ? C19 C20 1.513(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.400(4) . ? C20 C21 1.404(4) . ? C21 C22 1.370(5) . ? C21 H21 0.9500 . ? C22 C23 1.383(5) . ? C22 H22 0.9500 . ? C23 C24 1.387(4) . ? C23 H23 0.9500 . ? C24 C25 1.405(4) . ? C24 H24 0.9500 . ? C26 C27 1.390(4) . ? C26 H26 0.9500 . ? C27 C28 1.394(4) . ? C27 C36 1.502(4) . ? C28 C29 1.384(4) . ? C28 H28 0.9500 . ? C29 C30 1.384(4) . ? C29 H29 0.9500 . ? C30 C31 1.463(4) . ? C31 C32 1.384(4) . ? C32 C33 1.381(4) . ? C32 H32 0.9500 . ? C33 C34 1.397(4) . ? C33 H33 0.9500 . ? C34 C35 1.389(4) . ? C34 C37 1.505(4) . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.402(4) . ? C38 C43 1.403(4) . ? C39 C40 1.385(4) . ? C39 H39 0.9500 . ? C40 C41 1.389(4) . ? C40 H40 0.9500 . ? C41 C42 1.384(4) . ? C41 H41 0.9500 . ? C42 C43 1.402(4) . ? C42 H42 0.9500 . ? C43 C44 1.509(4) . ? C44 C45 1.509(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.401(4) . ? C45 C50 1.404(4) . ? C46 C47 1.379(4) . ? C46 H46 0.9500 . ? C47 C48 1.388(5) . ? C47 H47 0.9500 . ? C48 C49 1.385(4) . ? C48 H48 0.9500 . ? C49 C50 1.404(4) . ? C49 H49 0.9500 . ? B3 F2 1.377(4) . ? B3 F4 1.380(4) . ? B3 F3 1.381(4) . ? B3 F1 1.382(4) . ? B4 F6 1.311(5) . ? B4 F7' 1.332(18) . ? B4 F7 1.353(5) . ? B4 F8 1.366(5) . ? B4 F5 1.381(4) . ? B4 F6' 1.403(19) . ? B4 F8' 1.462(15) . ? Cl1 C51 1.744(17) . ? Cl1 C51 1.755(13) 2_756 ? Cl2 C51' 1.63(6) . ? Cl2 C51' 1.78(6) 2_756 ? 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 C5 120.9(2) . . ? C1 N1 B1 125.6(2) . . ? C5 N1 B1 113.4(2) . . ? C10 N2 C6 120.8(2) . . ? C10 N2 B1 125.6(2) . . ? C6 N2 B1 113.6(2) . . ? C25 B1 C13 114.5(2) . . ? C25 B1 N2 112.4(2) . . ? C13 B1 N2 111.5(2) . . ? C25 B1 N1 111.9(2) . . ? C13 B1 N1 110.3(2) . . ? N2 B1 N1 94.44(18) . . ? C26 N3 C30 120.8(2) . . ? C26 N3 B2 125.7(2) . . ? C30 N3 B2 113.5(2) . . ? C35 N4 C31 120.4(2) . . ? C35 N4 B2 125.6(2) . . ? C31 N4 B2 113.9(2) . . ? C38 B2 N4 111.3(2) . . ? C38 B2 C50 113.8(2) . . ? N4 B2 C50 112.7(2) . . ? C38 B2 N3 112.5(2) . . ? N4 B2 N3 94.26(19) . . ? C50 B2 N3 110.7(2) . . ? N1 C1 C2 120.8(3) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C1 C2 C3 117.8(3) . . ? C1 C2 C11 120.8(3) . . ? C3 C2 C11 121.4(3) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 117.6(3) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 109.2(2) . . ? C4 C5 C6 129.3(2) . . ? N2 C6 C7 120.7(2) . . ? N2 C6 C5 109.3(2) . . ? C7 C6 C5 130.0(2) . . ? C8 C7 C6 118.3(2) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 121.3(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 117.4(3) . . ? C10 C9 C12 119.9(3) . . ? C8 C9 C12 122.7(3) . . ? N2 C10 C9 121.5(2) . . ? N2 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.3(3) . . ? C18 C13 B1 119.8(3) . . ? C14 C13 B1 121.8(2) . . ? C15 C14 C13 122.0(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C16 C15 C14 119.4(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 121.9(3) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C13 C18 C17 118.6(3) . . ? C13 C18 C19 122.9(3) . . ? C17 C18 C19 118.6(3) . . ? C18 C19 C20 117.6(2) . . ? C18 C19 H19A 107.9 . . ? C20 C19 H19A 107.9 . . ? C18 C19 H19B 107.9 . . ? C20 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? C25 C20 C21 119.2(3) . . ? C25 C20 C19 122.9(3) . . ? C21 C20 C19 117.9(3) . . ? C22 C21 C20 121.3(3) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 118.9(3) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C23 C24 C25 122.0(3) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C20 C25 C24 118.2(3) . . ? C20 C25 B1 120.1(3) . . ? C24 C25 B1 121.8(2) . . ? N3 C26 C27 121.1(3) . . ? N3 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 117.7(3) . . ? C26 C27 C36 120.6(3) . . ? C28 C27 C36 121.7(3) . . ? C29 C28 C27 121.1(3) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C30 C29 C28 118.0(3) . . ? C30 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? N3 C30 C29 121.3(3) . . ? N3 C30 C31 109.2(2) . . ? C29 C30 C31 129.5(3) . . ? N4 C31 C32 120.9(3) . . ? N4 C31 C30 109.2(2) . . ? C32 C31 C30 129.9(3) . . ? C33 C32 C31 118.7(3) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 120.6(3) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 117.4(3) . . ? C35 C34 C37 120.1(3) . . ? C33 C34 C37 122.5(3) . . ? N4 C35 C34 121.8(3) . . ? N4 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? 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 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C43 117.9(2) . . ? C39 C38 B2 122.5(2) . . ? C43 C38 B2 119.6(2) . . ? C40 C39 C38 122.2(3) . . ? C40 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? C39 C40 C41 119.3(3) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C42 C41 C40 119.8(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 121.2(3) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C42 C43 C38 119.6(3) . . ? C42 C43 C44 118.7(2) . . ? C38 C43 C44 121.6(2) . . ? C43 C44 C45 116.4(2) . . ? C43 C44 H44A 108.2 . . ? C45 C44 H44A 108.2 . . ? C43 C44 H44B 108.2 . . ? C45 C44 H44B 108.2 . . ? H44A C44 H44B 107.3 . . ? C46 C45 C50 119.6(3) . . ? C46 C45 C44 118.7(2) . . ? C50 C45 C44 121.6(2) . . ? C47 C46 C45 121.1(3) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C46 C47 C48 119.9(3) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C49 C48 C47 119.5(3) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 121.7(3) . . ? C48 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? C45 C50 C49 118.1(3) . . ? C45 C50 B2 119.3(2) . . ? C49 C50 B2 122.7(2) . . ? F2 B3 F4 109.3(3) . . ? F2 B3 F3 109.1(3) . . ? F4 B3 F3 110.7(3) . . ? F2 B3 F1 110.3(3) . . ? F4 B3 F1 108.9(3) . . ? F3 B3 F1 108.5(3) . . ? F6 B4 F7' 127.5(6) . . ? F6 B4 F7 113.5(4) . . ? F7' B4 F7 49.6(7) . . ? F6 B4 F8 112.2(4) . . ? F7' B4 F8 54.4(7) . . ? F7 B4 F8 103.9(4) . . ? F6 B4 F5 111.1(3) . . ? F7' B4 F5 121.4(6) . . ? F7 B4 F5 109.4(3) . . ? F8 B4 F5 106.2(3) . . ? F6 B4 F6' 63.6(6) . . ? F7' B4 F6' 99.4(9) . . ? F7 B4 F6' 55.5(6) . . ? F8 B4 F6' 145.8(6) . . ? F5 B4 F6' 106.6(5) . . ? F6 B4 F8' 58.3(6) . . ? F7' B4 F8' 94.2(8) . . ? F7 B4 F8' 130.9(6) . . ? F8 B4 F8' 54.3(5) . . ? F5 B4 F8' 118.6(6) . . ? F6' B4 F8' 115.2(8) . . ? Cl1 C51 Cl1 114.8(8) . 2_756 ? Cl2 C51' Cl2 119(3) . 2_756 ? 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 C10 N2 B1 C25 65.2(3) . . . . ? C6 N2 B1 C25 -115.8(2) . . . . ? C10 N2 B1 C13 -65.0(3) . . . . ? C6 N2 B1 C13 114.0(2) . . . . ? C10 N2 B1 N1 -178.9(2) . . . . ? C6 N2 B1 N1 0.1(3) . . . . ? C1 N1 B1 C25 -65.5(3) . . . . ? C5 N1 B1 C25 117.4(2) . . . . ? C1 N1 B1 C13 63.3(3) . . . . ? C5 N1 B1 C13 -113.8(2) . . . . ? C1 N1 B1 N2 178.2(2) . . . . ? C5 N1 B1 N2 1.1(3) . . . . ? C35 N4 B2 C38 59.3(3) . . . . ? C31 N4 B2 C38 -116.9(3) . . . . ? C35 N4 B2 C50 -70.0(3) . . . . ? C31 N4 B2 C50 113.8(3) . . . . ? C35 N4 B2 N3 175.4(3) . . . . ? C31 N4 B2 N3 -0.7(3) . . . . ? C26 N3 B2 C38 -64.6(3) . . . . ? C30 N3 B2 C38 116.5(2) . . . . ? C26 N3 B2 N4 -179.7(2) . . . . ? C30 N3 B2 N4 1.3(3) . . . . ? C26 N3 B2 C50 64.1(3) . . . . ? C30 N3 B2 C50 -114.9(2) . . . . ? C5 N1 C1 C2 1.9(4) . . . . ? B1 N1 C1 C2 -175.0(2) . . . . ? N1 C1 C2 C3 -0.6(4) . . . . ? N1 C1 C2 C11 178.3(3) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C11 C2 C3 C4 -179.9(3) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C1 N1 C5 C4 -1.6(4) . . . . ? B1 N1 C5 C4 175.6(2) . . . . ? C1 N1 C5 C6 -179.1(2) . . . . ? B1 N1 C5 C6 -1.9(3) . . . . ? C3 C4 C5 N1 -0.1(4) . . . . ? C3 C4 C5 C6 176.9(3) . . . . ? C10 N2 C6 C7 -0.9(4) . . . . ? B1 N2 C6 C7 -180.0(2) . . . . ? C10 N2 C6 C5 177.9(2) . . . . ? B1 N2 C6 C5 -1.2(3) . . . . ? N1 C5 C6 N2 1.9(3) . . . . ? C4 C5 C6 N2 -175.4(3) . . . . ? N1 C5 C6 C7 -179.4(3) . . . . ? C4 C5 C6 C7 3.3(5) . . . . ? N2 C6 C7 C8 1.3(4) . . . . ? C5 C6 C7 C8 -177.2(3) . . . . ? C6 C7 C8 C9 -0.3(4) . . . . ? C7 C8 C9 C10 -1.0(4) . . . . ? C7 C8 C9 C12 178.9(3) . . . . ? C6 N2 C10 C9 -0.5(4) . . . . ? B1 N2 C10 C9 178.5(3) . . . . ? C8 C9 C10 N2 1.4(4) . . . . ? C12 C9 C10 N2 -178.5(3) . . . . ? C25 B1 C13 C18 16.8(3) . . . . ? N2 B1 C13 C18 145.8(2) . . . . ? N1 B1 C13 C18 -110.6(3) . . . . ? C25 B1 C13 C14 -167.4(2) . . . . ? N2 B1 C13 C14 -38.3(3) . . . . ? N1 B1 C13 C14 65.3(3) . . . . ? C18 C13 C14 C15 2.0(4) . . . . ? B1 C13 C14 C15 -173.9(3) . . . . ? C13 C14 C15 C16 1.0(5) . . . . ? C14 C15 C16 C17 -2.0(5) . . . . ? C15 C16 C17 C18 -0.1(5) . . . . ? C14 C13 C18 C17 -4.1(4) . . . . ? B1 C13 C18 C17 171.9(3) . . . . ? C14 C13 C18 C19 175.2(3) . . . . ? B1 C13 C18 C19 -8.8(4) . . . . ? C16 C17 C18 C13 3.2(5) . . . . ? C16 C17 C18 C19 -176.1(3) . . . . ? C13 C18 C19 C20 -4.0(4) . . . . ? C17 C18 C19 C20 175.2(3) . . . . ? C18 C19 C20 C25 8.4(4) . . . . ? C18 C19 C20 C21 -171.4(3) . . . . ? C25 C20 C21 C22 -0.3(5) . . . . ? C19 C20 C21 C22 179.6(3) . . . . ? C20 C21 C22 C23 0.8(5) . . . . ? C21 C22 C23 C24 -0.7(5) . . . . ? C22 C23 C24 C25 0.0(5) . . . . ? C21 C20 C25 C24 -0.4(4) . . . . ? C19 C20 C25 C24 179.7(3) . . . . ? C21 C20 C25 B1 -179.6(3) . . . . ? C19 C20 C25 B1 0.5(4) . . . . ? C23 C24 C25 C20 0.5(4) . . . . ? C23 C24 C25 B1 179.7(3) . . . . ? C13 B1 C25 C20 -12.6(3) . . . . ? N2 B1 C25 C20 -141.2(2) . . . . ? N1 B1 C25 C20 113.9(3) . . . . ? C13 B1 C25 C24 168.2(2) . . . . ? N2 B1 C25 C24 39.5(3) . . . . ? N1 B1 C25 C24 -65.3(3) . . . . ? C30 N3 C26 C27 0.0(4) . . . . ? B2 N3 C26 C27 -178.8(2) . . . . ? N3 C26 C27 C28 -0.9(4) . . . . ? N3 C26 C27 C36 179.7(3) . . . . ? C26 C27 C28 C29 1.4(4) . . . . ? C36 C27 C28 C29 -179.3(3) . . . . ? C27 C28 C29 C30 -1.0(5) . . . . ? C26 N3 C30 C29 0.5(4) . . . . ? B2 N3 C30 C29 179.5(3) . . . . ? C26 N3 C30 C31 179.5(2) . . . . ? B2 N3 C30 C31 -1.5(3) . . . . ? C28 C29 C30 N3 0.0(4) . . . . ? C28 C29 C30 C31 -178.8(3) . . . . ? C35 N4 C31 C32 1.9(4) . . . . ? B2 N4 C31 C32 178.3(3) . . . . ? C35 N4 C31 C30 -176.4(2) . . . . ? B2 N4 C31 C30 0.0(3) . . . . ? N3 C30 C31 N4 0.9(3) . . . . ? C29 C30 C31 N4 179.9(3) . . . . ? N3 C30 C31 C32 -177.2(3) . . . . ? C29 C30 C31 C32 1.8(5) . . . . ? N4 C31 C32 C33 -2.9(4) . . . . ? C30 C31 C32 C33 175.0(3) . . . . ? C31 C32 C33 C34 1.3(5) . . . . ? C32 C33 C34 C35 1.2(5) . . . . ? C32 C33 C34 C37 -178.3(3) . . . . ? C31 N4 C35 C34 0.8(4) . . . . ? B2 N4 C35 C34 -175.2(3) . . . . ? C33 C34 C35 N4 -2.3(4) . . . . ? C37 C34 C35 N4 177.2(3) . . . . ? N4 B2 C38 C39 31.2(3) . . . . ? C50 B2 C38 C39 159.8(2) . . . . ? N3 B2 C38 C39 -73.2(3) . . . . ? N4 B2 C38 C43 -149.5(2) . . . . ? C50 B2 C38 C43 -20.9(3) . . . . ? N3 B2 C38 C43 106.2(3) . . . . ? C43 C38 C39 C40 -1.2(4) . . . . ? B2 C38 C39 C40 178.1(3) . . . . ? C38 C39 C40 C41 0.4(4) . . . . ? C39 C40 C41 C42 0.1(4) . . . . ? C40 C41 C42 C43 0.2(4) . . . . ? C41 C42 C43 C38 -1.0(4) . . . . ? C41 C42 C43 C44 -179.5(2) . . . . ? C39 C38 C43 C42 1.5(4) . . . . ? B2 C38 C43 C42 -177.9(2) . . . . ? C39 C38 C43 C44 180.0(2) . . . . ? B2 C38 C43 C44 0.6(4) . . . . ? C42 C43 C44 C45 -158.8(2) . . . . ? C38 C43 C44 C45 22.7(4) . . . . ? C43 C44 C45 C46 157.3(2) . . . . ? C43 C44 C45 C50 -25.1(4) . . . . ? C50 C45 C46 C47 -2.4(4) . . . . ? C44 C45 C46 C47 175.2(3) . . . . ? C45 C46 C47 C48 -0.1(4) . . . . ? C46 C47 C48 C49 2.6(4) . . . . ? C47 C48 C49 C50 -2.5(4) . . . . ? C46 C45 C50 C49 2.4(4) . . . . ? C44 C45 C50 C49 -175.1(2) . . . . ? C46 C45 C50 B2 -178.4(2) . . . . ? C44 C45 C50 B2 4.1(4) . . . . ? C48 C49 C50 C45 0.0(4) . . . . ? C48 C49 C50 B2 -179.1(2) . . . . ? C38 B2 C50 C45 18.5(3) . . . . ? N4 B2 C50 C45 146.4(2) . . . . ? N3 B2 C50 C45 -109.5(3) . . . . ? C38 B2 C50 C49 -162.4(2) . . . . ? N4 B2 C50 C49 -34.5(3) . . . . ? N3 B2 C50 C49 69.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.952 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.063 # start Validation Reply Form _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. 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