# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email SESSLER@MAIL.CM.UTEXAS.EDU _publ_contact_author_name 'Prof Jonathan L. Sessler' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Department of Chemistry and Biochemistry The University of Texas at Austin 1 University Station - A5300 Austin TX 78712-0165 UNITED STATES OF AMERICA ; _publ_section_title ; Octaethylporphyrin and expanded porphyrin complexes containing coordinated BF2 groups ; loop_ _publ_author_name J.L.Sessler P.D.W.Boyd P.J.Brothers M.C.Hodgson T.Kohler ; V.Lynch ; S.Meyer D.Seidel J.M.Veauthier data_bisbf2_a _database_code_depnum_ccdc_archive 'CCDC 228378' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H54 B2 Cl2 F4 N6' _chemical_formula_weight 835.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.4372(1) _cell_length_b 15.8642(1) _cell_length_c 20.6260(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4396.85(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10067 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10067 _reflns_number_gt 7949 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+0.7956P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(8) _refine_ls_number_reflns 10067 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1675 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.37855(14) 0.11266(13) 0.15503(10) 0.0246(4) Uani 1 1 d . . . N2 N 0.28991(15) 0.29475(14) 0.16127(9) 0.0250(4) Uani 1 1 d . . . N3 N 0.37020(15) 0.47650(13) 0.15061(11) 0.0289(5) Uani 1 1 d . . . N4 N 0.55704(15) 0.47937(13) 0.14499(11) 0.0284(5) Uani 1 1 d . . . N5 N 0.64576(14) 0.29946(14) 0.14858(10) 0.0245(4) Uani 1 1 d . . . N6 N 0.56649(14) 0.11576(13) 0.14843(11) 0.0260(5) Uani 1 1 d . . . C1 C 0.38510(19) 0.02807(16) 0.17112(13) 0.0280(5) Uani 1 1 d . . . C2 C 0.2872(2) -0.00297(17) 0.18133(14) 0.0323(6) Uani 1 1 d . . . C3 C 0.22199(19) 0.06433(17) 0.17110(13) 0.0302(6) Uani 1 1 d . . . C4 C 0.28088(19) 0.13598(16) 0.15519(12) 0.0256(5) Uani 1 1 d . . . C5 C 0.24614(17) 0.22099(16) 0.13900(12) 0.0257(5) Uani 1 1 d . . . C6 C 0.16875(18) 0.24399(17) 0.09734(13) 0.0278(5) Uani 1 1 d . . . C7 C 0.16737(17) 0.33333(17) 0.09415(13) 0.0294(6) Uani 1 1 d . . . C8 C 0.24368(17) 0.36380(16) 0.13483(12) 0.0263(5) Uani 1 1 d . . . C9 C 0.27348(18) 0.45133(16) 0.14759(12) 0.0271(5) Uani 1 1 d . . . C10 C 0.2113(2) 0.52148(17) 0.16080(13) 0.0326(6) Uani 1 1 d . . . C11 C 0.2728(2) 0.59005(16) 0.17248(13) 0.0311(6) Uani 1 1 d . . . C12 C 0.37270(19) 0.56167(17) 0.16618(14) 0.0313(6) Uani 1 1 d . . . C13 C 0.4628(2) 0.60381(16) 0.17018(13) 0.0315(6) Uani 1 1 d . . . H13 H 0.4629 0.6628 0.1805 0.038 Uiso 1 1 d R . . C14 C 0.55375(19) 0.56483(16) 0.15945(12) 0.0275(5) Uani 1 1 d . . . C15 C 0.6526(2) 0.59584(17) 0.15950(13) 0.0304(6) Uani 1 1 d . . . C16 C 0.71465(19) 0.52909(16) 0.14521(12) 0.0286(5) Uani 1 1 d . . . C17 C 0.65386(18) 0.45637(17) 0.13620(12) 0.0271(5) Uani 1 1 d . . . C18 C 0.68589(17) 0.36969(16) 0.12099(12) 0.0254(5) Uani 1 1 d . . . C19 C 0.75791(18) 0.34456(18) 0.07642(13) 0.0292(6) Uani 1 1 d . . . C20 C 0.76077(17) 0.25522(17) 0.07824(12) 0.0265(5) Uani 1 1 d . . . C21 C 0.68982(17) 0.22854(15) 0.12320(11) 0.0242(5) Uani 1 1 d . . . C22 C 0.66142(18) 0.14210(16) 0.14079(12) 0.0240(5) Uani 1 1 d . . . C23 C 0.72656(18) 0.07205(16) 0.15206(13) 0.0276(5) Uani 1 1 d . . . C24 C 0.6667(2) 0.00272(17) 0.16644(13) 0.0298(6) Uani 1 1 d . . . C25 C 0.56631(19) 0.03092(16) 0.16413(13) 0.0289(6) Uani 1 1 d . . . C26 C 0.4770(2) -0.01141(16) 0.17545(14) 0.0302(6) Uani 1 1 d . . . H26 H 0.4791 -0.0700 0.1869 0.036 Uiso 1 1 d R . . C27 C 0.2601(2) -0.09084(17) 0.20012(16) 0.0393(7) Uani 1 1 d . . . H27C H 0.2191 -0.0909 0.2383 0.059 Uiso 1 1 d R . . H27A H 0.3201 -0.1221 0.2075 0.059 Uiso 1 1 d R . . H27B H 0.2258 -0.1168 0.1645 0.059 Uiso 1 1 d R . . C28 C 0.1111(2) 0.0612(2) 0.18002(16) 0.0400(7) Uani 1 1 d . . . H28C H 0.0800 0.0431 0.1405 0.060 Uiso 1 1 d R . . H28A H 0.0866 0.1161 0.1913 0.060 Uiso 1 1 d R . . H28B H 0.0939 0.0226 0.2141 0.060 Uiso 1 1 d R . . C29 C 0.10389(19) 0.18743(19) 0.05783(13) 0.0353(6) Uani 1 1 d . . . H29C H 0.0955 0.2097 0.0149 0.053 Uiso 1 1 d R . . H29A H 0.0404 0.1807 0.0785 0.053 Uiso 1 1 d R . . H29B H 0.1352 0.1331 0.0561 0.053 Uiso 1 1 d R . . C30 C 0.1035(2) 0.3847(2) 0.04906(14) 0.0384(7) Uani 1 1 d . . . H30C H 0.0395 0.3936 0.0685 0.058 Uiso 1 1 d R . . H30A H 0.0952 0.3555 0.0086 0.058 Uiso 1 1 d R . . H30B H 0.1341 0.4382 0.0406 0.058 Uiso 1 1 d R . . C31 C 0.0991(2) 0.52162(19) 0.16487(16) 0.0389(7) Uani 1 1 d . . . H31C H 0.0734 0.4652 0.1641 0.058 Uiso 1 1 d R . . H31A H 0.0742 0.5537 0.1289 0.058 Uiso 1 1 d R . . H31B H 0.0795 0.5503 0.2038 0.058 Uiso 1 1 d R . . C32 C 0.2420(2) 0.67821(17) 0.18892(16) 0.0403(7) Uani 1 1 d . . . H32C H 0.2194 0.6818 0.2330 0.060 Uiso 1 1 d R . . H32A H 0.1904 0.6945 0.1592 0.060 Uiso 1 1 d R . . H32B H 0.2976 0.7149 0.1815 0.060 Uiso 1 1 d R . . C33 C 0.6832(2) 0.68557(16) 0.17347(15) 0.0376(6) Uani 1 1 d . . . H33C H 0.7238 0.7065 0.1387 0.056 Uiso 1 1 d R . . H33A H 0.7197 0.6881 0.2134 0.056 Uiso 1 1 d R . . H33B H 0.6249 0.7201 0.1778 0.056 Uiso 1 1 d R . . C34 C 0.82617(19) 0.53215(18) 0.14412(15) 0.0356(6) Uani 1 1 d . . . H34C H 0.8495 0.5696 0.1774 0.053 Uiso 1 1 d R . . H34A H 0.8478 0.5509 0.1022 0.053 Uiso 1 1 d R . . H34B H 0.8519 0.4763 0.1505 0.053 Uiso 1 1 d R . . C35 C 0.81174(19) 0.39867(19) 0.02831(14) 0.0360(6) Uani 1 1 d . . . H35C H 0.7741 0.4483 0.0180 0.054 Uiso 1 1 d R . . H35A H 0.8234 0.3658 -0.0100 0.054 Uiso 1 1 d R . . H35B H 0.8753 0.4138 0.0460 0.054 Uiso 1 1 d R . . C36 C 0.82257(19) 0.2014(2) 0.03379(13) 0.0364(6) Uani 1 1 d . . . H36C H 0.8177 0.2202 -0.0103 0.055 Uiso 1 1 d R . . H36A H 0.7994 0.1443 0.0378 0.055 Uiso 1 1 d R . . H36B H 0.8904 0.2027 0.0483 0.055 Uiso 1 1 d R . . C37 C 0.8383(2) 0.07387(19) 0.15507(15) 0.0383(7) Uani 1 1 d . . . H37C H 0.8617 0.0417 0.1914 0.057 Uiso 1 1 d R . . H37A H 0.8598 0.1314 0.1588 0.057 Uiso 1 1 d R . . H37B H 0.8649 0.0515 0.1155 0.057 Uiso 1 1 d R . . C38 C 0.7017(2) -0.08395(18) 0.18207(15) 0.0376(7) Uani 1 1 d . . . H38C H 0.6480 -0.1175 0.1987 0.056 Uiso 1 1 d R . . H38A H 0.7542 -0.0795 0.2134 0.056 Uiso 1 1 d R . . H38B H 0.7293 -0.1091 0.1438 0.056 Uiso 1 1 d R . . F1 F 0.46549(11) 0.21509(10) 0.09099(7) 0.0365(4) Uani 1 1 d . . . F2 F 0.47501(11) 0.22084(9) 0.20301(7) 0.0321(4) Uani 1 1 d . . . F3 F 0.46964(11) 0.37205(9) 0.20054(8) 0.0375(4) Uani 1 1 d . . . F4 F 0.46159(12) 0.37583(10) 0.08885(9) 0.0421(4) Uani 1 1 d . . . B1 B 0.4706(2) 0.16999(17) 0.14714(14) 0.0255(6) Uani 1 1 d . . . B2 B 0.4645(2) 0.42270(18) 0.14439(16) 0.0311(6) Uani 1 1 d . . . H5N H 0.598(2) 0.2971(18) 0.1756(14) 0.026(6) Uiso 1 1 d . . . H2N H 0.351(2) 0.2980(18) 0.1810(12) 0.023(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0174(9) 0.0244(11) 0.0319(11) -0.0001(9) 0.0017(8) -0.0008(8) N2 0.0208(9) 0.0251(10) 0.0290(9) -0.0014(9) -0.0002(8) -0.0001(9) N3 0.0256(11) 0.0256(11) 0.0354(12) 0.0019(10) -0.0018(9) 0.0013(9) N4 0.0251(11) 0.0285(12) 0.0315(11) -0.0044(9) -0.0031(9) 0.0013(9) N5 0.0171(9) 0.0250(10) 0.0315(10) -0.0011(10) 0.0024(8) 0.0021(9) N6 0.0172(9) 0.0263(11) 0.0346(11) -0.0008(9) 0.0000(8) 0.0036(8) C1 0.0278(12) 0.0229(13) 0.0334(13) 0.0004(10) -0.0010(11) -0.0040(10) C2 0.0313(14) 0.0299(14) 0.0358(14) -0.0044(11) 0.0017(11) -0.0068(11) C3 0.0261(12) 0.0333(15) 0.0313(13) -0.0017(11) 0.0010(11) -0.0042(11) C4 0.0218(11) 0.0282(13) 0.0266(12) -0.0036(10) -0.0014(10) -0.0057(10) C5 0.0189(11) 0.0308(14) 0.0274(11) -0.0024(10) 0.0023(9) -0.0047(10) C6 0.0170(11) 0.0342(14) 0.0323(13) 0.0000(11) 0.0026(10) 0.0001(10) C7 0.0143(11) 0.0383(14) 0.0357(13) 0.0044(11) -0.0033(10) 0.0040(10) C8 0.0182(11) 0.0304(13) 0.0304(13) -0.0027(10) 0.0021(10) 0.0036(10) C9 0.0198(11) 0.0314(13) 0.0301(12) 0.0001(11) 0.0003(10) 0.0050(10) C10 0.0276(13) 0.0327(14) 0.0374(15) 0.0017(11) 0.0034(11) 0.0055(11) C11 0.0344(13) 0.0275(14) 0.0312(13) 0.0009(10) 0.0029(11) 0.0038(11) C12 0.0306(13) 0.0275(14) 0.0357(14) 0.0004(11) 0.0015(11) 0.0037(11) C13 0.0373(13) 0.0236(12) 0.0335(13) -0.0017(10) 0.0005(12) -0.0025(12) C14 0.0305(13) 0.0218(12) 0.0302(13) -0.0021(10) -0.0024(10) -0.0038(10) C15 0.0302(13) 0.0301(14) 0.0309(13) 0.0028(11) -0.0013(11) -0.0054(11) C16 0.0282(12) 0.0294(14) 0.0281(12) 0.0013(11) 0.0000(11) -0.0061(11) C17 0.0212(11) 0.0349(14) 0.0253(12) 0.0009(11) 0.0006(10) -0.0007(10) C18 0.0177(11) 0.0312(14) 0.0274(12) 0.0031(10) -0.0034(9) -0.0021(10) C19 0.0178(12) 0.0380(15) 0.0319(13) 0.0040(11) -0.0024(10) -0.0015(10) C20 0.0157(11) 0.0355(14) 0.0283(12) -0.0016(10) -0.0049(10) 0.0012(10) C21 0.0161(11) 0.0289(13) 0.0276(12) -0.0039(10) -0.0021(9) 0.0021(9) C22 0.0208(11) 0.0261(13) 0.0250(11) -0.0019(10) -0.0021(10) 0.0013(10) C23 0.0245(12) 0.0241(12) 0.0341(13) -0.0047(10) -0.0015(11) 0.0072(10) C24 0.0283(13) 0.0299(14) 0.0312(13) -0.0023(10) -0.0018(11) 0.0051(11) C25 0.0271(12) 0.0243(13) 0.0353(14) -0.0040(11) -0.0031(11) 0.0024(10) C26 0.0315(14) 0.0223(12) 0.0368(14) 0.0009(10) -0.0036(12) 0.0006(11) C27 0.0374(15) 0.0290(15) 0.0515(17) 0.0000(12) 0.0034(13) -0.0095(12) C28 0.0271(13) 0.0403(17) 0.0527(17) 0.0035(13) 0.0064(13) -0.0079(12) C29 0.0207(11) 0.0477(18) 0.0375(14) -0.0018(12) -0.0030(11) -0.0027(12) C30 0.0247(13) 0.0494(18) 0.0410(15) 0.0030(13) -0.0079(11) 0.0113(13) C31 0.0276(13) 0.0399(16) 0.0492(17) 0.0018(13) 0.0052(13) 0.0114(12) C32 0.0407(16) 0.0296(15) 0.0505(17) -0.0022(12) 0.0080(13) 0.0083(12) C33 0.0406(15) 0.0289(15) 0.0434(15) 0.0010(11) -0.0019(13) -0.0095(12) C34 0.0250(13) 0.0372(15) 0.0447(15) 0.0045(13) -0.0046(12) -0.0117(11) C35 0.0197(12) 0.0506(18) 0.0376(14) 0.0065(13) 0.0033(11) -0.0028(12) C36 0.0251(12) 0.0479(16) 0.0361(13) -0.0027(13) 0.0016(10) 0.0036(13) C37 0.0239(12) 0.0431(17) 0.0480(17) -0.0010(13) -0.0064(12) 0.0094(12) C38 0.0340(15) 0.0352(16) 0.0437(16) 0.0015(12) -0.0009(12) 0.0108(12) F1 0.0226(7) 0.0408(9) 0.0462(9) 0.0137(7) -0.0017(6) 0.0014(7) F2 0.0236(7) 0.0263(8) 0.0465(8) -0.0057(6) 0.0006(6) -0.0026(6) F3 0.0225(7) 0.0289(8) 0.0609(10) 0.0070(7) 0.0039(7) -0.0006(7) F4 0.0223(7) 0.0422(9) 0.0619(11) -0.0224(8) 0.0006(7) -0.0017(7) B1 0.0170(12) 0.0221(13) 0.0374(15) 0.0002(11) -0.0045(12) -0.0012(11) B2 0.0229(13) 0.0248(14) 0.0455(17) -0.0059(13) 0.0044(14) 0.0002(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 C4 1.364(3) . ? N1 C1 1.385(3) . ? N1 B1 1.544(3) . ? N2 C8 1.372(3) . ? N2 C5 1.388(3) . ? N2 H2N 0.92(3) . ? N3 C9 1.361(3) . ? N3 C12 1.389(3) . ? N3 B2 1.533(4) . ? N4 C17 1.363(3) . ? N4 C14 1.389(3) . ? N4 B2 1.535(4) . ? N5 C18 1.362(3) . ? N5 C21 1.375(3) . ? N5 H5N 0.85(3) . ? N6 C22 1.351(3) . ? N6 C25 1.384(3) . ? N6 B1 1.549(3) . ? C1 C26 1.387(4) . ? C1 C2 1.420(4) . ? C2 C3 1.397(4) . ? C2 C27 1.492(4) . ? C3 C4 1.423(4) . ? C3 C28 1.503(4) . ? C4 C5 1.466(4) . ? C5 C6 1.398(4) . ? C6 C7 1.419(4) . ? C6 C29 1.493(4) . ? C7 C8 1.410(4) . ? C7 C30 1.505(4) . ? C8 C9 1.469(4) . ? C9 C10 1.418(4) . ? C10 C11 1.387(4) . ? C10 C31 1.509(4) . ? C11 C12 1.422(4) . ? C11 C32 1.497(4) . ? C12 C13 1.386(4) . ? C13 C14 1.387(4) . ? C13 H13 0.9600 . ? C14 C15 1.416(4) . ? C15 C16 1.380(4) . ? C15 C33 1.509(4) . ? C16 C17 1.426(4) . ? C16 C34 1.499(4) . ? C17 C18 1.475(4) . ? C18 C19 1.393(4) . ? C19 C20 1.418(4) . ? C19 C35 1.498(4) . ? C20 C21 1.396(3) . ? C20 C36 1.503(4) . ? C21 C22 1.469(4) . ? C22 C23 1.434(3) . ? C23 C24 1.395(4) . ? C23 C37 1.503(4) . ? C24 C25 1.421(4) . ? C24 C38 1.489(4) . ? C25 C26 1.395(4) . ? C26 H26 0.9601 . ? C27 H27C 0.9600 . ? C27 H27A 0.9599 . ? C27 H27B 0.9600 . ? C28 H28C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C29 H29C 0.9601 . ? C29 H29A 0.9600 . ? C29 H29B 0.9599 . ? C30 H30C 0.9600 . ? C30 H30A 0.9599 . ? C30 H30B 0.9600 . ? C31 H31C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C32 H32C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C33 H33C 0.9601 . ? C33 H33A 0.9601 . ? C33 H33B 0.9600 . ? C34 H34C 0.9598 . ? C34 H34A 0.9598 . ? C34 H34B 0.9599 . ? C35 H35C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9601 . ? C36 H36C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9601 . ? C37 H37C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9599 . ? C38 H38C 0.9599 . ? C38 H38A 0.9600 . ? C38 H38B 0.9599 . ? F1 B1 1.363(3) . ? F2 B1 1.408(3) . ? F3 B2 1.411(4) . ? F4 B2 1.366(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 N1 C1 108.9(2) . . ? C4 N1 B1 127.7(2) . . ? C1 N1 B1 123.0(2) . . ? C8 N2 C5 110.5(2) . . ? C8 N2 H2N 122.4(18) . . ? C5 N2 H2N 125.0(18) . . ? C9 N3 C12 108.6(2) . . ? C9 N3 B2 128.5(2) . . ? C12 N3 B2 122.7(2) . . ? C17 N4 C14 108.7(2) . . ? C17 N4 B2 128.0(2) . . ? C14 N4 B2 123.2(2) . . ? C18 N5 C21 109.86(19) . . ? C18 N5 H5N 127(2) . . ? C21 N5 H5N 123(2) . . ? C22 N6 C25 109.2(2) . . ? C22 N6 B1 127.7(2) . . ? C25 N6 B1 122.9(2) . . ? N1 C1 C26 120.6(2) . . ? N1 C1 C2 108.2(2) . . ? C26 C1 C2 131.2(2) . . ? C3 C2 C1 107.1(2) . . ? C3 C2 C27 126.9(2) . . ? C1 C2 C27 126.1(2) . . ? C2 C3 C4 107.2(2) . . ? C2 C3 C28 125.3(3) . . ? C4 C3 C28 127.3(3) . . ? N1 C4 C3 108.6(2) . . ? N1 C4 C5 123.8(2) . . ? C3 C4 C5 127.6(2) . . ? N2 C5 C6 107.4(2) . . ? N2 C5 C4 124.4(2) . . ? C6 C5 C4 128.1(2) . . ? C5 C6 C7 107.4(2) . . ? C5 C6 C29 127.8(2) . . ? C7 C6 C29 124.6(2) . . ? C8 C7 C6 107.8(2) . . ? C8 C7 C30 126.7(3) . . ? C6 C7 C30 125.2(2) . . ? N2 C8 C7 107.0(2) . . ? N2 C8 C9 124.1(2) . . ? C7 C8 C9 129.0(2) . . ? N3 C9 C10 108.9(2) . . ? N3 C9 C8 123.1(2) . . ? C10 C9 C8 128.0(2) . . ? C11 C10 C9 107.3(2) . . ? C11 C10 C31 125.7(3) . . ? C9 C10 C31 126.9(3) . . ? C10 C11 C12 107.4(2) . . ? C10 C11 C32 127.4(3) . . ? C12 C11 C32 125.3(3) . . ? C13 C12 N3 120.3(2) . . ? C13 C12 C11 131.8(3) . . ? N3 C12 C11 107.8(2) . . ? C12 C13 C14 123.0(2) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 117.9 . . ? C13 C14 N4 119.8(2) . . ? C13 C14 C15 132.1(2) . . ? N4 C14 C15 108.0(2) . . ? C16 C15 C14 107.5(2) . . ? C16 C15 C33 126.8(2) . . ? C14 C15 C33 125.7(2) . . ? C15 C16 C17 107.6(2) . . ? C15 C16 C34 125.6(2) . . ? C17 C16 C34 126.6(2) . . ? N4 C17 C16 108.2(2) . . ? N4 C17 C18 123.8(2) . . ? C16 C17 C18 128.0(2) . . ? N5 C18 C19 108.5(2) . . ? N5 C18 C17 123.9(2) . . ? C19 C18 C17 127.6(2) . . ? C18 C19 C20 106.7(2) . . ? C18 C19 C35 127.5(3) . . ? C20 C19 C35 125.2(3) . . ? C21 C20 C19 107.6(2) . . ? C21 C20 C36 127.6(2) . . ? C19 C20 C36 124.5(3) . . ? N5 C21 C20 107.4(2) . . ? N5 C21 C22 123.9(2) . . ? C20 C21 C22 128.7(2) . . ? N6 C22 C23 108.5(2) . . ? N6 C22 C21 124.2(2) . . ? C23 C22 C21 127.2(2) . . ? C24 C23 C22 107.1(2) . . ? C24 C23 C37 125.7(2) . . ? C22 C23 C37 127.0(2) . . ? C23 C24 C25 107.0(2) . . ? C23 C24 C38 126.3(2) . . ? C25 C24 C38 126.7(2) . . ? N6 C25 C26 120.6(2) . . ? N6 C25 C24 108.2(2) . . ? C26 C25 C24 131.2(2) . . ? C1 C26 C25 122.5(2) . . ? C1 C26 H26 118.7 . . ? C25 C26 H26 118.8 . . ? C2 C27 H27C 110.7 . . ? C2 C27 H27A 108.6 . . ? H27C C27 H27A 110.6 . . ? C2 C27 H27B 108.6 . . ? H27C C27 H27B 110.6 . . ? H27A C27 H27B 107.6 . . ? C3 C28 H28C 109.7 . . ? C3 C28 H28A 109.8 . . ? H28C C28 H28A 109.2 . . ? C3 C28 H28B 110.4 . . ? H28C C28 H28B 109.2 . . ? H28A C28 H28B 108.6 . . ? C6 C29 H29C 110.6 . . ? C6 C29 H29A 110.1 . . ? H29C C29 H29A 110.3 . . ? C6 C29 H29B 107.7 . . ? H29C C29 H29B 110.3 . . ? H29A C29 H29B 107.8 . . ? C7 C30 H30C 109.4 . . ? C7 C30 H30A 110.0 . . ? H30C C30 H30A 109.3 . . ? C7 C30 H30B 110.3 . . ? H30C C30 H30B 109.3 . . ? H30A C30 H30B 108.5 . . ? C10 C31 H31C 110.9 . . ? C10 C31 H31A 107.8 . . ? H31C C31 H31A 110.8 . . ? C10 C31 H31B 108.8 . . ? H31C C31 H31B 110.9 . . ? H31A C31 H31B 107.4 . . ? C11 C32 H32C 110.9 . . ? C11 C32 H32A 107.9 . . ? H32C C32 H32A 111.2 . . ? C11 C32 H32B 108.4 . . ? H32C C32 H32B 111.1 . . ? H32A C32 H32B 107.2 . . ? C15 C33 H33C 109.8 . . ? C15 C33 H33A 110.1 . . ? H33C C33 H33A 109.6 . . ? C15 C33 H33B 109.5 . . ? H33C C33 H33B 109.6 . . ? H33A C33 H33B 108.3 . . ? C16 C34 H34C 109.6 . . ? C16 C34 H34A 109.0 . . ? H34C C34 H34A 110.8 . . ? C16 C34 H34B 109.2 . . ? H34C C34 H34B 110.7 . . ? H34A C34 H34B 107.5 . . ? C19 C35 H35C 111.3 . . ? C19 C35 H35A 108.2 . . ? H35C C35 H35A 110.4 . . ? C19 C35 H35B 108.7 . . ? H35C C35 H35B 110.4 . . ? H35A C35 H35B 107.7 . . ? C20 C36 H36C 111.3 . . ? C20 C36 H36A 107.7 . . ? H36C C36 H36A 110.7 . . ? C20 C36 H36B 108.8 . . ? H36C C36 H36B 110.6 . . ? H36A C36 H36B 107.6 . . ? C23 C37 H37C 110.5 . . ? C23 C37 H37A 108.8 . . ? H37C C37 H37A 110.2 . . ? C23 C37 H37B 109.3 . . ? H37C C37 H37B 110.2 . . ? H37A C37 H37B 107.9 . . ? C24 C38 H38C 110.6 . . ? C24 C38 H38A 108.1 . . ? H38C C38 H38A 110.7 . . ? C24 C38 H38B 109.2 . . ? H38C C38 H38B 110.7 . . ? H38A C38 H38B 107.5 . . ? F1 B1 F2 113.4(2) . . ? F1 B1 N1 111.0(2) . . ? F2 B1 N1 106.5(2) . . ? F1 B1 N6 110.4(2) . . ? F2 B1 N6 105.6(2) . . ? N1 B1 N6 109.7(2) . . ? F4 B2 F3 112.3(2) . . ? F4 B2 N3 110.5(2) . . ? F3 B2 N3 106.8(2) . . ? F4 B2 N4 110.4(2) . . ? F3 B2 N4 106.7(2) . . ? N3 B2 N4 110.1(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.551 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.072 data_oepbf _database_code_depnum_ccdc_archive 'CCDC 228379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H60 B3 F6 N5 O' _chemical_formula_weight 797.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.2302(3) _cell_length_b 13.7883(5) _cell_length_c 15.1221(6) _cell_angle_alpha 88.661(2) _cell_angle_beta 84.853(2) _cell_angle_gamma 79.504(2) _cell_volume 2088.88(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour 'black or dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9847 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1582 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 22.43 _reflns_number_total 9847 _reflns_number_gt 5750 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.5(9) _refine_ls_number_reflns 9847 _refine_ls_number_parameters 1037 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.007 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 0.2816(6) 0.2654(5) 0.6006(3) 0.0304(15) Uani 1 1 d . . . N2 N 0.1752(5) 0.3518(4) 0.7346(3) 0.0281(15) Uani 1 1 d . . . N3 N 0.3966(6) 0.1929(4) 0.8667(3) 0.0255(14) Uani 1 1 d . . . N4 N 0.5051(6) 0.1045(4) 0.7335(3) 0.0321(16) Uani 1 1 d . . . C1 C 0.3780(8) 0.2054(5) 0.5483(4) 0.0291(19) Uani 1 1 d . . . C2 C 0.3757(8) 0.2426(6) 0.4575(4) 0.037(2) Uani 1 1 d . . . C3 C 0.2830(7) 0.3279(6) 0.4588(4) 0.031(2) Uani 1 1 d . . . C4 C 0.2262(7) 0.3436(6) 0.5499(4) 0.0300(19) Uani 1 1 d . . . C5 C 0.1422(7) 0.4237(5) 0.5911(4) 0.033(2) Uani 1 1 d . . . H5 H 0.0964 0.4748 0.5550 0.040 Uiso 1 1 d R . . C6 C 0.1228(7) 0.4309(6) 0.6841(5) 0.033(2) Uani 1 1 d . . . C7 C 0.0671(7) 0.5118(5) 0.7391(4) 0.0316(19) Uani 1 1 d . . . C8 C 0.0867(7) 0.4842(5) 0.8251(4) 0.0306(19) Uani 1 1 d . . . C9 C 0.1580(7) 0.3819(6) 0.8224(4) 0.0315(19) Uani 1 1 d . . . C10 C 0.2092(7) 0.3376(5) 0.8998(4) 0.0323(19) Uani 1 1 d . . . H10 H 0.1648 0.3707 0.9524 0.039 Uiso 1 1 d R . . C11 C 0.3091(7) 0.2564(6) 0.9215(4) 0.0314(19) Uani 1 1 d . . . C12 C 0.3436(7) 0.2324(6) 1.0127(4) 0.034(2) Uani 1 1 d . . . C13 C 0.4457(8) 0.1528(6) 1.0094(4) 0.036(2) Uani 1 1 d . . . C14 C 0.4772(7) 0.1276(5) 0.9175(4) 0.0304(19) Uani 1 1 d . . . C15 C 0.5697(7) 0.0507(5) 0.8764(4) 0.037(2) Uani 1 1 d . . . H15 H 0.6276 0.0066 0.9120 0.045 Uiso 1 1 d R . . C16 C 0.5832(8) 0.0380(6) 0.7842(5) 0.040(2) Uani 1 1 d . . . C17 C 0.6648(7) -0.0346(6) 0.7266(5) 0.041(2) Uani 1 1 d . . . C18 C 0.6342(8) -0.0112(6) 0.6422(5) 0.044(2) Uani 1 1 d . . . C19 C 0.5335(8) 0.0761(6) 0.6445(4) 0.038(2) Uani 1 1 d . . . C20 C 0.4754(8) 0.1244(6) 0.5707(4) 0.040(2) Uani 1 1 d . . . H20 H 0.5196 0.0929 0.5174 0.049 Uiso 1 1 d R . . C21 C 0.4617(8) 0.1979(5) 0.3787(4) 0.044(2) Uani 1 1 d . . . H21A H 0.5520 0.1788 0.3938 0.053 Uiso 1 1 d R . . H21B H 0.4602 0.2466 0.3322 0.053 Uiso 1 1 d R . . C22 C 0.4153(9) 0.1090(6) 0.3442(4) 0.064(3) Uani 1 1 d . . . H22A H 0.4713 0.0817 0.2931 0.096 Uiso 1 1 d R . . H22B H 0.4179 0.0603 0.3907 0.096 Uiso 1 1 d R . . H22C H 0.3253 0.1286 0.3287 0.096 Uiso 1 1 d R . . C23 C 0.2389(7) 0.3937(6) 0.3840(4) 0.040(2) Uani 1 1 d . . . H23A H 0.3136 0.3972 0.3415 0.048 Uiso 1 1 d R . . H23B H 0.2073 0.4581 0.4086 0.048 Uiso 1 1 d R . . C24 C 0.1257(7) 0.3603(6) 0.3400(4) 0.055(3) Uani 1 1 d . . . H24A H 0.0980 0.4060 0.2935 0.083 Uiso 1 1 d R . . H24B H 0.1581 0.2960 0.3152 0.083 Uiso 1 1 d R . . H24C H 0.0512 0.3574 0.3827 0.083 Uiso 1 1 d R . . C25 C 0.0057(7) 0.6129(5) 0.7059(5) 0.045(2) Uani 1 1 d . . . H25A H 0.0671 0.6334 0.6607 0.054 Uiso 1 1 d R . . H25B H -0.0062 0.6589 0.7539 0.054 Uiso 1 1 d R . . C26 C -0.1263(7) 0.6156(6) 0.6652(5) 0.054(2) Uani 1 1 d . . . H26A H -0.1603 0.6810 0.6447 0.082 Uiso 1 1 d R . . H26B H -0.1143 0.5705 0.6165 0.082 Uiso 1 1 d R . . H26C H -0.1883 0.5962 0.7106 0.082 Uiso 1 1 d R . . C27 C 0.0486(7) 0.5470(5) 0.9074(4) 0.042(2) Uani 1 1 d . . . H27A H 0.0263 0.5068 0.9572 0.050 Uiso 1 1 d R . . H27B H -0.0277 0.5971 0.8985 0.050 Uiso 1 1 d R . . C28 C 0.1632(7) 0.6003(5) 0.9245(4) 0.047(2) Uani 1 1 d . . . H28A H 0.1413 0.6405 0.9766 0.071 Uiso 1 1 d R . . H28B H 0.2388 0.5496 0.9335 0.071 Uiso 1 1 d R . . H28C H 0.1844 0.6404 0.8745 0.071 Uiso 1 1 d R . . C29 C 0.2772(7) 0.2900(5) 1.0943(4) 0.038(2) Uani 1 1 d . . . H29A H 0.2970 0.2500 1.1458 0.045 Uiso 1 1 d R . . H29B H 0.1822 0.3028 1.0918 0.045 Uiso 1 1 d R . . C30 C 0.3279(7) 0.3889(5) 1.1040(4) 0.042(2) Uani 1 1 d . . . H30A H 0.2846 0.4223 1.1567 0.062 Uiso 1 1 d R . . H30B H 0.4227 0.3761 1.1076 0.062 Uiso 1 1 d R . . H30C H 0.3068 0.4295 1.0530 0.062 Uiso 1 1 d R . . C31 C 0.5143(7) 0.1000(6) 1.0855(4) 0.039(2) Uani 1 1 d . . . H31A H 0.5390 0.0307 1.0734 0.047 Uiso 1 1 d R . . H31B H 0.4517 0.1081 1.1372 0.047 Uiso 1 1 d R . . C32 C 0.6358(7) 0.1397(6) 1.1067(4) 0.053(2) Uani 1 1 d . . . H32A H 0.6751 0.1054 1.1565 0.080 Uiso 1 1 d R . . H32B H 0.6991 0.1307 1.0554 0.080 Uiso 1 1 d R . . H32C H 0.6110 0.2088 1.1198 0.080 Uiso 1 1 d R . . C33 C 0.7546(9) -0.1205(6) 0.7629(5) 0.063(3) Uani 1 1 d . . . H33A H 0.8049 -0.0973 0.8060 0.075 Uiso 1 1 d R . . H33B H 0.8160 -0.1499 0.7150 0.075 Uiso 1 1 d R . . C34 C 0.6784(8) -0.2009(6) 0.8020(5) 0.067(3) Uani 1 1 d . . . H34A H 0.7396 -0.2553 0.8241 0.101 Uiso 1 1 d R . . H34B H 0.6178 -0.1712 0.8501 0.101 Uiso 1 1 d R . . H34C H 0.6290 -0.2242 0.7584 0.101 Uiso 1 1 d R . . C35 C 0.6894(9) -0.0694(7) 0.5605(5) 0.073(3) Uani 1 1 d . . . H35A H 0.7773 -0.1053 0.5682 0.088 Uiso 1 1 d R . . H35B H 0.6961 -0.0231 0.5127 0.088 Uiso 1 1 d R . . C36 C 0.6014(10) -0.1407(7) 0.5350(6) 0.099(4) Uani 1 1 d . . . H36A H 0.6382 -0.1751 0.4814 0.149 Uiso 1 1 d R . . H36B H 0.5957 -0.1874 0.5827 0.149 Uiso 1 1 d R . . H36C H 0.5138 -0.1045 0.5267 0.149 Uiso 1 1 d R . . F1 F 0.0823(4) 0.2230(3) 0.6729(2) 0.0360(10) Uani 1 1 d . . . F2 F 0.4394(4) 0.2794(3) 0.7340(2) 0.0314(10) Uani 1 1 d . . . O1 O 0.2747(4) 0.1765(3) 0.7425(3) 0.0265(12) Uani 1 1 d . . . B1 B 0.2056(9) 0.2483(7) 0.6920(5) 0.031(2) Uani 1 1 d . . . B2 B 0.4029(9) 0.1932(7) 0.7659(5) 0.035(2) Uani 1 1 d . . . N1A N 0.1880(7) -0.0037(5) 0.7408(4) 0.0550(19) Uani 1 1 d U . . H1A H 0.2151 0.0549 0.7365 0.066 Uiso 1 1 d R . . C1A C 0.0817(11) 0.0080(7) 0.8110(8) 0.120(4) Uani 1 1 d U . . H1AA H 0.0444 -0.0511 0.8169 0.144 Uiso 1 1 d R . . H1AB H 0.0118 0.0624 0.8002 0.144 Uiso 1 1 d R . . C2A C 0.1470(10) 0.0262(8) 0.9022(5) 0.096(4) Uani 1 1 d U . . H2AA H 0.0810 0.0328 0.9520 0.144 Uiso 1 1 d R . . H2AB H 0.2167 -0.0288 0.9120 0.144 Uiso 1 1 d R . . H2AC H 0.1839 0.0854 0.8953 0.144 Uiso 1 1 d R . . C3A C 0.3037(12) -0.0774(8) 0.7453(9) 0.140(5) Uani 1 1 d U . . H3AA H 0.3497 -0.0637 0.7948 0.168 Uiso 1 1 d R . . H3AB H 0.3619 -0.0745 0.6923 0.168 Uiso 1 1 d R . . C4A C 0.2722(11) -0.1835(8) 0.7566(9) 0.160(5) Uani 1 1 d U . . H4AA H 0.3530 -0.2309 0.7597 0.239 Uiso 1 1 d R . . H4AB H 0.2151 -0.1868 0.8101 0.239 Uiso 1 1 d R . . H4AC H 0.2274 -0.1977 0.7066 0.239 Uiso 1 1 d R . . C5A C 0.0919(14) -0.0064(9) 0.6585(7) 0.151(5) Uani 1 1 d U . . H5AA H 0.0318 0.0551 0.6525 0.182 Uiso 1 1 d R . . H5AB H 0.0436 -0.0601 0.6638 0.182 Uiso 1 1 d R . . C6A C 0.2040(16) -0.0175(11) 0.5785(10) 0.212(7) Uani 1 1 d U . . H6AA H 0.1698 -0.0208 0.5218 0.318 Uiso 1 1 d R . . H6AB H 0.2515 0.0365 0.5785 0.318 Uiso 1 1 d R . . H6AC H 0.2633 -0.0780 0.5897 0.318 Uiso 1 1 d R . . B1A B 0.0832(13) -0.2329(9) 0.4883(7) 0.062(3) Uani 1 1 d . . . F1A F 0.1001(5) -0.3344(4) 0.4800(3) 0.0878(17) Uani 1 1 d . . . F2A F 0.0209(5) -0.2042(3) 0.5709(3) 0.0743(15) Uani 1 1 d . . . F3A F 0.0208(6) -0.1862(4) 0.4230(3) 0.105(2) Uani 1 1 d . . . F4A F 0.2117(6) -0.2159(5) 0.4879(4) 0.130(3) Uani 1 1 d . . . N1' N 0.7897(6) 0.4023(4) 0.0763(3) 0.0314(15) Uani 1 1 d . . . N2' N 0.8572(5) 0.3007(4) 0.2038(3) 0.0309(15) Uani 1 1 d . . . N3' N 0.6048(6) 0.4512(4) 0.3472(3) 0.0291(15) Uani 1 1 d . . . N4' N 0.5362(5) 0.5550(4) 0.2178(4) 0.0310(15) Uani 1 1 d . . . C1' C 0.7087(7) 0.4715(6) 0.0272(4) 0.034(2) Uani 1 1 d . . . C2' C 0.7320(7) 0.4395(6) -0.0642(4) 0.0321(19) Uani 1 1 d . . . C3' C 0.8209(7) 0.3539(5) -0.0680(4) 0.033(2) Uani 1 1 d . . . C4' C 0.8532(7) 0.3277(6) 0.0196(4) 0.0297(18) Uani 1 1 d . . . C5' C 0.9244(7) 0.2449(6) 0.0562(4) 0.034(2) Uani 1 1 d . . . H5' H 0.9803 0.1982 0.0167 0.040 Uiso 1 1 d R . . C6' C 0.9210(8) 0.2257(6) 0.1481(5) 0.038(2) Uani 1 1 d . . . C7' C 0.9565(7) 0.1362(6) 0.1975(5) 0.041(2) Uani 1 1 d . . . C8' C 0.9134(8) 0.1588(7) 0.2855(5) 0.053(2) Uani 1 1 d . . . C9' C 0.8453(7) 0.2628(6) 0.2904(5) 0.036(2) Uani 1 1 d . . . C10' C 0.7716(7) 0.3008(6) 0.3695(4) 0.038(2) Uani 1 1 d . . . H10' H 0.7973 0.2581 0.4184 0.045 Uiso 1 1 d R . . C11' C 0.6748(7) 0.3792(6) 0.3952(4) 0.0318(19) Uani 1 1 d . . . C12' C 0.6178(7) 0.3948(6) 0.4884(4) 0.034(2) Uani 1 1 d . . . C13' C 0.5211(7) 0.4765(6) 0.4904(4) 0.0299(19) Uani 1 1 d . . . C14' C 0.5143(8) 0.5120(6) 0.4000(4) 0.034(2) Uani 1 1 d . . . C15' C 0.4322(7) 0.5937(6) 0.3632(5) 0.039(2) Uani 1 1 d . . . H15' H 0.3631 0.6341 0.4002 0.047 Uiso 1 1 d R . . C16' C 0.4458(7) 0.6163(5) 0.2740(4) 0.0291(18) Uani 1 1 d . . . C17' C 0.3826(7) 0.6978(6) 0.2224(5) 0.035(2) Uani 1 1 d . . . C18' C 0.4337(8) 0.6827(6) 0.1356(5) 0.037(2) Uani 1 1 d . . . C19' C 0.5344(8) 0.5933(6) 0.1331(5) 0.037(2) Uani 1 1 d . . . C20' C 0.6100(7) 0.5535(5) 0.0564(4) 0.035(2) Uani 1 1 d . . . H20' H 0.5874 0.5960 0.0068 0.042 Uiso 1 1 d R . . C21' C 0.6629(7) 0.4931(6) -0.1410(4) 0.043(2) Uani 1 1 d . . . H21C H 0.7148 0.4731 -0.1958 0.052 Uiso 1 1 d R . . H21D H 0.6589 0.5626 -0.1337 0.052 Uiso 1 1 d R . . C22' C 0.5238(8) 0.4729(7) -0.1471(5) 0.068(3) Uani 1 1 d . . . H22D H 0.4809 0.5077 -0.1955 0.102 Uiso 1 1 d R . . H22E H 0.5291 0.4032 -0.1545 0.102 Uiso 1 1 d R . . H22F H 0.4729 0.4932 -0.0921 0.102 Uiso 1 1 d R . . C23' C 0.8703(7) 0.2906(5) -0.1477(4) 0.040(2) Uani 1 1 d . . . H23C H 0.9572 0.2534 -0.1392 0.048 Uiso 1 1 d R . . H23D H 0.8784 0.3318 -0.1992 0.048 Uiso 1 1 d R . . C24' C 0.7766(8) 0.2196(6) -0.1655(4) 0.056(2) Uani 1 1 d . . . H24D H 0.8112 0.1802 -0.2167 0.084 Uiso 1 1 d R . . H24E H 0.7696 0.1775 -0.1145 0.084 Uiso 1 1 d R . . H24F H 0.6900 0.2566 -0.1751 0.084 Uiso 1 1 d R . . C25' C 1.0250(8) 0.0393(6) 0.1570(5) 0.049(2) Uani 1 1 d . . . H25C H 0.9856 0.0295 0.1034 0.059 Uiso 1 1 d R . . H25D H 1.0111 -0.0130 0.1978 0.059 Uiso 1 1 d R . . C26' C 1.1761(8) 0.0344(6) 0.1384(5) 0.065(3) Uani 1 1 d . . . H26D H 1.2176 -0.0279 0.1129 0.098 Uiso 1 1 d R . . H26E H 1.1894 0.0865 0.0972 0.098 Uiso 1 1 d R . . H26F H 1.2151 0.0436 0.1923 0.098 Uiso 1 1 d R . . C27' C 0.9294(13) 0.0881(7) 0.3630(6) 0.102(5) Uani 1 1 d D . . H27E H 1.0107 0.0414 0.3512 0.122 Uiso 0.42 1 d PR . . H27F H 0.9377 0.1238 0.4153 0.122 Uiso 0.42 1 d PR . . H27C H 0.9540 0.0235 0.3375 0.122 Uiso 0.58 1 d PR . . H27D H 0.8420 0.0913 0.3930 0.122 Uiso 0.58 1 d PR . . C28' C 1.0128(15) 0.0880(13) 0.4250(9) 0.086(6) Uani 0.58 1 d PD . . H28D H 1.0061 0.0354 0.4668 0.129 Uiso 0.58 1 d PR . . H28E H 1.1029 0.0810 0.3985 0.129 Uiso 0.58 1 d PR . . H28F H 0.9887 0.1501 0.4550 0.129 Uiso 0.58 1 d PR . . C28A C 0.842(2) 0.031(2) 0.3779(16) 0.115(12) Uani 0.42 1 d PD . . H28G H 0.8587 -0.0125 0.4274 0.172 Uiso 0.42 1 d PR . . H28H H 0.7606 0.0775 0.3913 0.172 Uiso 0.42 1 d PR . . H28I H 0.8344 -0.0059 0.3264 0.172 Uiso 0.42 1 d PR . . C29' C 0.6664(7) 0.3307(6) 0.5649(4) 0.044(2) Uani 1 1 d . . . H29C H 0.6787 0.2628 0.5478 0.052 Uiso 1 1 d R . . H29D H 0.5970 0.3416 0.6126 0.052 Uiso 1 1 d R . . C30' C 0.7958(8) 0.3527(6) 0.5975(5) 0.061(3) Uani 1 1 d . . . H30D H 0.8196 0.3102 0.6469 0.091 Uiso 1 1 d R . . H30E H 0.8658 0.3407 0.5502 0.091 Uiso 1 1 d R . . H30F H 0.7833 0.4202 0.6156 0.091 Uiso 1 1 d R . . C31' C 0.4356(8) 0.5258(6) 0.5697(4) 0.048(2) Uani 1 1 d . . . H31C H 0.4228 0.4765 0.6139 0.058 Uiso 1 1 d R . . H31D H 0.3498 0.5561 0.5520 0.058 Uiso 1 1 d R . . C32' C 0.5015(9) 0.6016(7) 0.6102(5) 0.078(3) Uani 1 1 d . . . H32D H 0.4468 0.6319 0.6606 0.117 Uiso 1 1 d R . . H32E H 0.5869 0.5708 0.6283 0.117 Uiso 1 1 d R . . H32F H 0.5133 0.6510 0.5659 0.117 Uiso 1 1 d R . . C33' C 0.2836(7) 0.7829(5) 0.2601(5) 0.045(2) Uani 1 1 d . . . H33C H 0.2230 0.7597 0.3042 0.054 Uiso 1 1 d R . . H33D H 0.2329 0.8146 0.2137 0.054 Uiso 1 1 d R . . C34' C 0.3526(8) 0.8591(6) 0.3014(5) 0.060(2) Uani 1 1 d . . . H34D H 0.2871 0.9134 0.3250 0.091 Uiso 1 1 d R . . H34E H 0.4022 0.8276 0.3484 0.091 Uiso 1 1 d R . . H34F H 0.4122 0.8831 0.2571 0.091 Uiso 1 1 d R . . C35' C 0.3956(8) 0.7451(6) 0.0568(5) 0.051(2) Uani 1 1 d . . . H35C H 0.3024 0.7735 0.0645 0.061 Uiso 1 1 d R . . H35D H 0.4099 0.7043 0.0050 0.061 Uiso 1 1 d R . . C36' C 0.4774(8) 0.8237(6) 0.0415(5) 0.065(3) Uani 1 1 d . . . H36D H 0.4506 0.8618 -0.0099 0.098 Uiso 1 1 d R . . H36E H 0.4619 0.8655 0.0926 0.098 Uiso 1 1 d R . . H36F H 0.5705 0.7956 0.0326 0.098 Uiso 1 1 d R . . F1' F 0.9723(4) 0.4299(3) 0.1531(2) 0.0353(10) Uani 1 1 d . . . F2' F 0.5957(4) 0.3797(3) 0.2083(2) 0.0351(10) Uani 1 1 d . . . O1' O 0.7630(4) 0.4763(3) 0.2260(2) 0.0272(12) Uani 1 1 d . . . B1' B 0.8424(9) 0.4072(7) 0.1697(5) 0.033(2) Uani 1 1 d . . . B2' B 0.6263(9) 0.4636(6) 0.2474(5) 0.032(2) Uani 1 1 d . . . N1B N 0.8477(6) 0.6507(5) 0.2671(3) 0.0411(17) Uani 1 1 d . . . H1B H 0.8357 0.5919 0.2482 0.049 Uiso 1 1 d R . . C1B C 0.9958(8) 0.6461(6) 0.2610(5) 0.056(2) Uani 1 1 d . . . H1BA H 1.0363 0.5901 0.2942 0.067 Uiso 1 1 d R . . H1BB H 1.0130 0.7046 0.2875 0.067 Uiso 1 1 d R . . C2B C 1.0603(9) 0.6399(6) 0.1670(4) 0.064(3) Uani 1 1 d . . . H2BA H 1.1548 0.6380 0.1656 0.096 Uiso 1 1 d R . . H2BB H 1.0440 0.5810 0.1408 0.096 Uiso 1 1 d R . . H2BC H 1.0206 0.6964 0.1341 0.096 Uiso 1 1 d R . . C3B C 0.7872(8) 0.6588(7) 0.3633(4) 0.060(3) Uani 1 1 d . . . H3BA H 0.6921 0.6637 0.3652 0.072 Uiso 1 1 d R . . H3BB H 0.8051 0.7180 0.3881 0.072 Uiso 1 1 d R . . C4B C 0.8427(8) 0.5735(6) 0.4191(5) 0.064(3) Uani 1 1 d . . . H4BA H 0.8037 0.5812 0.4793 0.096 Uiso 1 1 d R . . H4BB H 0.8236 0.5143 0.3950 0.096 Uiso 1 1 d R . . H4BC H 0.9376 0.5691 0.4180 0.096 Uiso 1 1 d R . . C5B C 0.7725(9) 0.7251(5) 0.2092(5) 0.061(3) Uani 1 1 d . . . H5BA H 0.6802 0.7189 0.2166 0.073 Uiso 1 1 d R . . H5BB H 0.8039 0.7120 0.1481 0.073 Uiso 1 1 d R . . C6B C 0.7803(8) 0.8290(6) 0.2298(6) 0.076(3) Uani 1 1 d . . . H6BA H 0.7290 0.8743 0.1914 0.114 Uiso 1 1 d R . . H6BB H 0.7474 0.8430 0.2905 0.114 Uiso 1 1 d R . . H6BC H 0.8723 0.8360 0.2213 0.114 Uiso 1 1 d R . . B1B B 0.9222(12) 0.8461(10) -0.0184(7) 0.063(3) Uani 1 1 d . . . F1B F 0.9840(5) 0.8177(4) -0.1007(3) 0.0806(16) Uani 1 1 d . . . F2B F 1.0141(5) 0.8474(3) 0.0403(3) 0.0786(16) Uani 1 1 d . . . F3B F 0.8508(6) 0.9410(4) -0.0274(3) 0.0997(19) Uani 1 1 d . . . F4B F 0.8381(6) 0.7831(5) 0.0071(3) 0.121(2) 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 0.033(4) 0.038(4) 0.021(3) -0.011(3) 0.001(3) -0.008(3) N2 0.030(4) 0.026(4) 0.028(4) -0.002(3) -0.002(3) -0.004(3) N3 0.030(4) 0.023(4) 0.023(4) -0.001(3) 0.002(3) -0.004(3) N4 0.047(4) 0.022(4) 0.026(4) -0.006(3) -0.005(3) -0.003(3) C1 0.044(6) 0.027(5) 0.020(4) 0.000(4) -0.008(4) -0.014(5) C2 0.045(6) 0.041(6) 0.028(5) 0.005(4) -0.010(4) -0.017(5) C3 0.045(5) 0.039(6) 0.010(4) -0.001(4) -0.004(4) -0.009(5) C4 0.033(5) 0.028(5) 0.032(5) 0.004(4) -0.014(4) -0.006(4) C5 0.034(5) 0.029(5) 0.039(5) -0.002(4) -0.014(4) -0.002(4) C6 0.039(5) 0.031(5) 0.031(5) -0.010(4) -0.008(4) -0.011(4) C7 0.038(5) 0.022(5) 0.035(5) -0.008(4) -0.003(4) -0.006(4) C8 0.035(5) 0.026(5) 0.028(5) -0.005(4) -0.001(4) 0.002(4) C9 0.035(5) 0.035(5) 0.024(5) -0.004(4) -0.004(4) -0.005(4) C10 0.024(5) 0.043(6) 0.030(5) -0.015(4) 0.004(4) -0.005(4) C11 0.035(5) 0.038(5) 0.020(4) -0.005(4) 0.003(4) -0.004(5) C12 0.036(5) 0.048(6) 0.018(4) 0.000(4) -0.004(4) -0.008(5) C13 0.044(6) 0.036(6) 0.030(5) -0.001(4) -0.008(4) -0.014(5) C14 0.032(5) 0.024(5) 0.034(5) -0.012(4) 0.007(4) -0.006(4) C15 0.058(6) 0.030(5) 0.028(5) -0.001(4) -0.004(4) -0.017(5) C16 0.042(5) 0.036(6) 0.042(5) 0.004(5) -0.001(4) -0.010(5) C17 0.039(5) 0.027(5) 0.049(6) -0.007(4) 0.001(4) 0.009(4) C18 0.066(6) 0.027(5) 0.034(5) 0.001(4) 0.005(4) -0.001(5) C19 0.048(6) 0.039(6) 0.029(5) 0.001(4) -0.007(4) -0.012(5) C20 0.056(6) 0.044(6) 0.022(4) -0.005(4) 0.005(4) -0.016(5) C21 0.061(6) 0.038(6) 0.031(5) 0.005(4) -0.001(4) -0.004(5) C22 0.107(8) 0.056(7) 0.034(5) -0.003(5) -0.003(5) -0.027(6) C23 0.040(5) 0.049(6) 0.030(4) -0.006(4) 0.002(4) -0.008(4) C24 0.064(6) 0.074(7) 0.037(5) 0.009(5) -0.012(4) -0.034(6) C25 0.047(6) 0.035(6) 0.050(5) -0.004(4) -0.013(4) 0.003(5) C26 0.057(6) 0.055(6) 0.046(5) -0.001(4) -0.014(4) 0.011(5) C27 0.051(6) 0.033(5) 0.036(5) -0.020(4) -0.006(4) 0.010(5) C28 0.060(6) 0.036(5) 0.044(5) -0.011(4) -0.007(4) -0.001(5) C29 0.051(5) 0.042(5) 0.020(4) -0.016(4) 0.001(4) -0.007(4) C30 0.048(5) 0.045(6) 0.035(4) -0.018(4) -0.006(4) -0.015(4) C31 0.034(5) 0.042(5) 0.040(5) -0.002(4) -0.001(4) -0.006(4) C32 0.057(6) 0.062(6) 0.044(5) 0.005(4) -0.019(4) -0.017(5) C33 0.080(7) 0.047(6) 0.050(5) -0.006(5) 0.002(5) 0.015(6) C34 0.068(7) 0.038(6) 0.081(6) 0.013(5) 0.024(5) 0.012(5) C35 0.074(7) 0.072(8) 0.049(6) 0.004(5) 0.015(5) 0.040(6) C36 0.139(11) 0.071(8) 0.076(7) -0.051(6) 0.007(7) 0.007(8) F1 0.042(3) 0.036(3) 0.030(2) -0.0073(19) -0.0041(18) -0.006(2) F2 0.035(3) 0.031(3) 0.028(2) -0.0042(19) 0.0006(17) -0.006(2) O1 0.034(3) 0.024(3) 0.021(2) 0.000(2) -0.003(2) -0.005(3) B1 0.030(6) 0.038(6) 0.025(5) -0.005(4) 0.006(4) -0.008(5) B2 0.040(7) 0.031(6) 0.031(5) 0.001(5) 0.010(4) -0.001(5) N1A 0.070(5) 0.046(5) 0.053(4) -0.010(4) 0.005(4) -0.026(4) C1A 0.123(10) 0.058(8) 0.170(10) 0.008(7) 0.066(9) -0.031(7) C2A 0.140(9) 0.104(8) 0.052(6) 0.021(6) -0.005(6) -0.050(7) C3A 0.104(10) 0.054(8) 0.252(13) -0.003(8) 0.059(9) -0.024(8) C4A 0.129(10) 0.045(7) 0.293(14) 0.023(8) 0.072(9) -0.030(7) C5A 0.270(14) 0.130(10) 0.083(8) -0.015(7) 0.012(9) -0.124(11) C6A 0.294(16) 0.188(14) 0.189(13) -0.054(11) 0.017(12) -0.146(13) B1A 0.087(10) 0.067(10) 0.044(7) -0.013(6) 0.003(7) -0.047(8) F1A 0.111(5) 0.071(4) 0.080(4) -0.033(3) -0.013(3) -0.006(4) F2A 0.104(4) 0.055(3) 0.056(3) -0.014(3) 0.025(3) -0.009(3) F3A 0.145(6) 0.090(5) 0.059(3) -0.004(3) -0.010(3) 0.031(4) F4A 0.113(6) 0.175(7) 0.115(5) -0.047(5) 0.028(4) -0.075(5) N1' 0.034(4) 0.032(4) 0.027(3) -0.003(3) -0.001(3) -0.003(3) N2' 0.039(4) 0.033(4) 0.022(4) -0.010(3) -0.007(3) -0.008(3) N3' 0.027(4) 0.033(4) 0.025(4) -0.008(3) 0.003(3) 0.001(3) N4' 0.027(4) 0.032(4) 0.031(4) -0.003(3) -0.003(3) 0.001(3) C1' 0.037(5) 0.043(6) 0.019(4) -0.005(4) -0.002(4) 0.000(5) C2' 0.039(5) 0.034(5) 0.024(4) -0.010(4) -0.001(4) -0.007(4) C3' 0.050(6) 0.028(5) 0.025(4) -0.011(4) -0.008(4) -0.010(5) C4' 0.028(5) 0.030(5) 0.032(5) 0.000(4) -0.006(4) -0.005(4) C5' 0.031(5) 0.042(6) 0.026(5) -0.016(4) 0.004(4) -0.004(4) C6' 0.046(6) 0.029(5) 0.040(5) -0.008(4) -0.006(4) -0.009(5) C7' 0.038(5) 0.027(5) 0.059(6) -0.005(5) -0.010(4) -0.004(4) C8' 0.057(6) 0.052(7) 0.048(6) -0.009(5) -0.005(5) -0.001(5) C9' 0.041(5) 0.024(5) 0.042(5) -0.005(4) -0.012(4) 0.001(4) C10' 0.046(6) 0.043(6) 0.028(5) 0.010(4) -0.010(4) -0.016(5) C11' 0.036(5) 0.026(5) 0.033(5) -0.015(4) -0.008(4) 0.000(4) C12' 0.035(5) 0.038(6) 0.032(5) 0.004(4) -0.001(4) -0.015(5) C13' 0.019(5) 0.049(6) 0.026(5) -0.006(4) 0.007(3) -0.021(4) C14' 0.035(5) 0.042(6) 0.028(5) -0.003(4) -0.001(4) -0.010(5) C15' 0.031(5) 0.048(6) 0.039(5) -0.019(4) 0.009(4) -0.009(5) C16' 0.027(5) 0.034(5) 0.025(5) -0.006(4) -0.004(4) 0.001(4) C17' 0.025(5) 0.039(6) 0.039(5) -0.007(4) -0.007(4) 0.004(4) C18' 0.042(5) 0.026(5) 0.042(5) 0.006(4) -0.013(4) 0.000(4) C19' 0.051(6) 0.034(5) 0.030(5) -0.006(4) -0.009(4) -0.010(5) C20' 0.045(6) 0.028(5) 0.035(5) 0.002(4) -0.011(4) -0.011(5) C21' 0.050(6) 0.042(6) 0.035(4) -0.006(4) -0.008(4) 0.001(5) C22' 0.051(7) 0.089(8) 0.063(6) -0.017(5) -0.024(5) 0.002(6) C23' 0.052(6) 0.037(5) 0.036(4) -0.007(4) -0.006(4) -0.016(5) C24' 0.056(6) 0.065(7) 0.047(5) -0.024(4) 0.014(4) -0.018(5) C25' 0.067(7) 0.033(6) 0.041(5) -0.004(4) -0.008(4) 0.008(5) C26' 0.055(7) 0.043(6) 0.095(7) -0.015(5) -0.006(5) -0.001(5) C27' 0.178(14) 0.047(8) 0.050(7) 0.004(6) 0.002(8) 0.052(8) C28' 0.072(13) 0.126(17) 0.054(11) 0.032(11) -0.032(9) 0.006(12) C28A 0.11(2) 0.16(3) 0.09(2) 0.09(2) -0.043(16) -0.06(2) C29' 0.043(6) 0.050(6) 0.037(5) 0.002(4) 0.000(4) -0.006(5) C30' 0.058(6) 0.082(7) 0.046(5) 0.007(5) -0.022(4) -0.013(5) C31' 0.050(6) 0.055(6) 0.036(5) 0.001(4) 0.008(4) -0.008(5) C32' 0.082(7) 0.084(8) 0.072(6) -0.050(6) 0.017(5) -0.029(6) C33' 0.047(6) 0.032(5) 0.052(5) -0.016(4) -0.009(4) 0.002(5) C34' 0.067(6) 0.045(6) 0.066(6) -0.021(5) 0.018(5) -0.008(5) C35' 0.049(6) 0.040(6) 0.061(6) -0.004(5) 0.006(4) -0.004(5) C36' 0.063(7) 0.068(7) 0.057(6) -0.008(5) 0.004(5) 0.005(6) F1' 0.032(3) 0.034(3) 0.038(2) -0.0068(19) -0.0008(18) -0.003(2) F2' 0.046(3) 0.028(3) 0.032(2) -0.006(2) -0.0079(19) -0.005(2) O1' 0.031(3) 0.028(3) 0.021(3) -0.009(2) -0.001(2) -0.001(3) B1' 0.026(6) 0.031(6) 0.042(6) -0.002(5) -0.015(4) 0.002(5) B2' 0.046(7) 0.025(6) 0.027(5) -0.004(4) -0.005(4) -0.005(5) N1B 0.039(5) 0.043(5) 0.040(4) -0.010(3) 0.000(3) -0.007(4) C1B 0.060(7) 0.059(7) 0.053(6) -0.010(5) -0.009(4) -0.017(5) C2B 0.090(7) 0.055(6) 0.044(5) -0.010(5) 0.025(5) -0.021(6) C3B 0.075(7) 0.077(7) 0.036(5) -0.031(5) 0.017(5) -0.044(6) C4B 0.088(7) 0.076(7) 0.037(5) 0.006(5) -0.016(5) -0.036(6) C5B 0.078(7) 0.023(5) 0.085(6) 0.014(5) -0.026(5) -0.008(5) C6B 0.065(7) 0.044(7) 0.113(8) -0.006(6) 0.008(5) -0.003(6) B1B 0.070(9) 0.081(10) 0.037(7) -0.002(6) -0.009(7) -0.011(8) F1B 0.084(4) 0.078(4) 0.068(4) 0.008(3) 0.004(3) 0.009(3) F2B 0.096(4) 0.054(4) 0.089(4) 0.000(3) -0.041(3) -0.005(3) F3B 0.093(4) 0.099(5) 0.084(4) -0.023(3) -0.021(3) 0.053(4) F4B 0.111(5) 0.185(7) 0.085(4) 0.035(4) -0.003(3) -0.085(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.370(8) . ? N1 C4 1.374(8) . ? N1 B1 1.559(9) . ? N2 C6 1.371(8) . ? N2 C9 1.386(7) . ? N2 B1 1.547(10) . ? N3 C11 1.367(8) . ? N3 C14 1.375(8) . ? N3 B2 1.521(9) . ? N4 C16 1.370(8) . ? N4 C19 1.400(8) . ? N4 B2 1.516(10) . ? C1 C20 1.411(10) . ? C1 C2 1.455(8) . ? C2 C3 1.369(9) . ? C2 C21 1.491(9) . ? C3 C4 1.453(9) . ? C3 C23 1.484(9) . ? C4 C5 1.392(9) . ? C5 C6 1.406(9) . ? C5 H5 0.9601 . ? C6 C7 1.410(9) . ? C7 C8 1.369(8) . ? C7 C25 1.514(9) . ? C8 C9 1.464(9) . ? C8 C27 1.514(8) . ? C9 C10 1.407(9) . ? C10 C11 1.425(9) . ? C10 H10 0.9601 . ? C11 C12 1.470(8) . ? C12 C13 1.369(9) . ? C12 C29 1.520(9) . ? C13 C14 1.434(9) . ? C13 C31 1.506(9) . ? C14 C15 1.402(9) . ? C15 C16 1.400(9) . ? C15 H15 0.9601 . ? C16 C17 1.437(10) . ? C17 C18 1.359(9) . ? C17 C33 1.487(10) . ? C18 C19 1.433(10) . ? C18 C35 1.499(10) . ? C19 C20 1.409(9) . ? C20 H20 0.9600 . ? C21 C22 1.511(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9601 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9599 . ? C23 C24 1.531(8) . ? C23 H23A 0.9601 . ? C23 H23B 0.9601 . ? C24 H24A 0.9601 . ? C24 H24B 0.9601 . ? C24 H24C 0.9599 . ? C25 C26 1.528(8) . ? C25 H25A 0.9601 . ? C25 H25B 0.9600 . ? C26 H26A 0.9601 . ? C26 H26B 0.9599 . ? C26 H26C 0.9600 . ? C27 C28 1.536(9) . ? C27 H27A 0.9600 . ? C27 H27B 0.9601 . ? C28 H28A 0.9600 . ? C28 H28B 0.9599 . ? C28 H28C 0.9601 . ? C29 C30 1.558(8) . ? C29 H29A 0.9599 . ? C29 H29B 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.508(8) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C32 H32A 0.9601 . ? C32 H32B 0.9600 . ? C32 H32C 0.9601 . ? C33 C34 1.546(10) . ? C33 H33A 0.9599 . ? C33 H33B 0.9601 . ? C34 H34A 0.9600 . ? C34 H34B 0.9601 . ? C34 H34C 0.9600 . ? C35 C36 1.526(11) . ? C35 H35A 0.9600 . ? C35 H35B 0.9601 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9602 . ? F1 B1 1.423(8) . ? F2 B2 1.373(9) . ? O1 B1 1.367(9) . ? O1 B2 1.447(9) . ? N1A C3A 1.419(12) . ? N1A C1A 1.440(10) . ? N1A C5A 1.658(12) . ? N1A H1A 0.9000 . ? C1A C2A 1.628(12) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9601 . ? C2A H2AA 0.9600 . ? C2A H2AB 0.9602 . ? C2A H2AC 0.9599 . ? C3A C4A 1.556(12) . ? C3A H3AA 0.9599 . ? C3A H3AB 0.9601 . ? C4A H4AA 0.9601 . ? C4A H4AB 0.9599 . ? C4A H4AC 0.9600 . ? C5A C6A 1.581(16) . ? C5A H5AA 0.9600 . ? C5A H5AB 0.9600 . ? C6A H6AA 0.9601 . ? C6A H6AB 0.9600 . ? C6A H6AC 0.9600 . ? B1A F3A 1.315(12) . ? B1A F4A 1.377(11) . ? B1A F2A 1.383(11) . ? B1A F1A 1.386(12) . ? N1' C4' 1.383(8) . ? N1' C1' 1.393(8) . ? N1' B1' 1.563(9) . ? N2' C6' 1.379(8) . ? N2' C9' 1.402(8) . ? N2' B1' 1.530(10) . ? N3' C14' 1.346(8) . ? N3' C11' 1.351(8) . ? N3' B2' 1.516(9) . ? N4' C19' 1.374(8) . ? N4' C16' 1.378(8) . ? N4' B2' 1.504(10) . ? C1' C20' 1.421(9) . ? C1' C2' 1.447(8) . ? C2' C3' 1.350(9) . ? C2' C21' 1.521(9) . ? C3' C4' 1.418(8) . ? C3' C23' 1.500(8) . ? C4' C5' 1.370(9) . ? C5' C6' 1.408(9) . ? C5' H5' 0.9601 . ? C6' C7' 1.434(9) . ? C7' C8' 1.388(10) . ? C7' C25' 1.508(10) . ? C8' C9' 1.476(10) . ? C8' C27' 1.507(11) . ? C9' C10' 1.412(10) . ? C10' C11' 1.364(9) . ? C10' H10' 0.9600 . ? C11' C12' 1.482(9) . ? C12' C13' 1.356(9) . ? C12' C29' 1.504(9) . ? C13' C14' 1.445(9) . ? C13' C31' 1.516(9) . ? C14' C15' 1.412(9) . ? C15' C16' 1.378(9) . ? C15' H15' 0.9601 . ? C16' C17' 1.440(9) . ? C17' C18' 1.375(9) . ? C17' C33' 1.490(9) . ? C18' C19' 1.455(10) . ? C18' C35' 1.491(9) . ? C19' C20' 1.399(10) . ? C20' H20' 0.9600 . ? C21' C22' 1.510(9) . ? C21' H21C 0.9600 . ? C21' H21D 0.9601 . ? C22' H22D 0.9600 . ? C22' H22E 0.9601 . ? C22' H22F 0.9601 . ? C23' C24' 1.532(8) . ? C23' H23C 0.9601 . ? C23' H23D 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25' C26' 1.535(9) . ? C25' H25C 0.9599 . ? C25' H25D 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9602 . ? C27' C28A 1.293(13) . ? C27' C28' 1.323(11) . ? C27' H27E 0.9601 . ? C27' H27F 0.9599 . ? C27' H27C 0.9601 . ? C27' H27D 0.9600 . ? C28' H27E 1.3049 . ? C28' H27F 0.8566 . ? C28' H28D 0.9600 . ? C28' H28E 0.9599 . ? C28' H28F 0.9601 . ? C28A H27C 1.2357 . ? C28A H27D 0.8627 . ? C28A H28G 0.9599 . ? C28A H28H 0.9601 . ? C28A H28I 0.9601 . ? C29' C30' 1.535(9) . ? C29' H29C 0.9599 . ? C29' H29D 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9601 . ? C30' H30F 0.9600 . ? C31' C32' 1.511(9) . ? C31' H31C 0.9601 . ? C31' H31D 0.9599 . ? C32' H32D 0.9601 . ? C32' H32E 0.9601 . ? C32' H32F 0.9600 . ? C33' C34' 1.540(9) . ? C33' H33C 0.9599 . ? C33' H33D 0.9600 . ? C34' H34D 0.9600 . ? C34' H34E 0.9601 . ? C34' H34F 0.9599 . ? C35' C36' 1.486(10) . ? C35' H35C 0.9600 . ? C35' H35D 0.9600 . ? C36' H36D 0.9601 . ? C36' H36E 0.9599 . ? C36' H36F 0.9601 . ? F1' B1' 1.419(9) . ? F2' B2' 1.408(8) . ? O1' B1' 1.387(9) . ? O1' B2' 1.447(9) . ? N1B C5B 1.484(8) . ? N1B C1B 1.499(8) . ? N1B C3B 1.526(8) . ? N1B H1B 0.8999 . ? C1B C2B 1.510(9) . ? C1B H1BA 0.9601 . ? C1B H1BB 0.9599 . ? C2B H2BA 0.9599 . ? C2B H2BB 0.9600 . ? C2B H2BC 0.9602 . ? C3B C4B 1.489(10) . ? C3B H3BA 0.9601 . ? C3B H3BB 0.9600 . ? C4B H4BA 0.9602 . ? C4B H4BB 0.9599 . ? C4B H4BC 0.9601 . ? C5B C6B 1.492(10) . ? C5B H5BA 0.9600 . ? C5B H5BB 0.9600 . ? C6B H6BA 0.9599 . ? C6B H6BB 0.9601 . ? C6B H6BC 0.9600 . ? B1B F2B 1.352(11) . ? B1B F4B 1.356(12) . ? B1B F1B 1.376(11) . ? B1B F3B 1.388(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 108.5(5) . . ? C1 N1 B1 132.2(6) . . ? C4 N1 B1 117.2(6) . . ? C6 N2 C9 107.3(6) . . ? C6 N2 B1 118.4(5) . . ? C9 N2 B1 132.1(6) . . ? C11 N3 C14 109.1(5) . . ? C11 N3 B2 125.6(6) . . ? C14 N3 B2 125.3(6) . . ? C16 N4 C19 108.3(6) . . ? C16 N4 B2 127.1(6) . . ? C19 N4 B2 124.6(6) . . ? N1 C1 C20 130.7(6) . . ? N1 C1 C2 108.5(6) . . ? C20 C1 C2 120.7(7) . . ? C3 C2 C1 107.1(6) . . ? C3 C2 C21 126.6(6) . . ? C1 C2 C21 126.3(7) . . ? C2 C3 C4 107.3(6) . . ? C2 C3 C23 129.2(6) . . ? C4 C3 C23 123.4(7) . . ? N1 C4 C5 119.5(6) . . ? N1 C4 C3 108.4(6) . . ? C5 C4 C3 131.8(7) . . ? C4 C5 C6 121.3(7) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.6 . . ? N2 C6 C5 118.8(7) . . ? N2 C6 C7 110.2(6) . . ? C5 C6 C7 130.7(7) . . ? C8 C7 C6 108.0(7) . . ? C8 C7 C25 127.1(6) . . ? C6 C7 C25 124.8(6) . . ? C7 C8 C9 106.5(6) . . ? C7 C8 C27 127.5(7) . . ? C9 C8 C27 126.0(6) . . ? N2 C9 C10 131.9(7) . . ? N2 C9 C8 108.0(6) . . ? C10 C9 C8 119.5(6) . . ? C9 C10 C11 137.1(6) . . ? C9 C10 H10 111.6 . . ? C11 C10 H10 111.2 . . ? N3 C11 C10 129.7(6) . . ? N3 C11 C12 106.9(6) . . ? C10 C11 C12 123.2(6) . . ? C13 C12 C11 108.0(6) . . ? C13 C12 C29 127.6(6) . . ? C11 C12 C29 124.4(7) . . ? C12 C13 C14 106.6(6) . . ? C12 C13 C31 128.1(7) . . ? C14 C13 C31 125.3(7) . . ? N3 C14 C15 119.7(6) . . ? N3 C14 C13 109.3(6) . . ? C15 C14 C13 131.0(7) . . ? C16 C15 C14 121.9(7) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 119.3 . . ? N4 C16 C15 118.4(7) . . ? N4 C16 C17 108.5(6) . . ? C15 C16 C17 133.1(8) . . ? C18 C17 C16 107.4(7) . . ? C18 C17 C33 131.2(7) . . ? C16 C17 C33 121.2(7) . . ? C17 C18 C19 108.5(7) . . ? C17 C18 C35 126.2(8) . . ? C19 C18 C35 125.1(7) . . ? N4 C19 C20 126.7(7) . . ? N4 C19 C18 107.2(6) . . ? C20 C19 C18 126.1(7) . . ? C19 C20 C1 141.5(7) . . ? C19 C20 H20 109.0 . . ? C1 C20 H20 109.5 . . ? C2 C21 C22 112.6(6) . . ? C2 C21 H21A 109.6 . . ? C22 C21 H21A 109.1 . . ? C2 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 108.3 . . ? C21 C22 H22A 111.4 . . ? C21 C22 H22B 108.2 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 108.7 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 111.9(6) . . ? C3 C23 H23A 109.7 . . ? C24 C23 H23A 111.1 . . ? C3 C23 H23B 106.6 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 108.3 . . ? C23 C24 H24A 109.2 . . ? C23 C24 H24B 108.6 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 110.6 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C25 C26 113.9(6) . . ? C7 C25 H25A 108.2 . . ? C26 C25 H25A 107.4 . . ? C7 C25 H25B 109.0 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 110.5 . . ? C25 C26 H26B 110.4 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 107.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 109.7(6) . . ? C8 C27 H27A 110.0 . . ? C28 C27 H27A 111.7 . . ? C8 C27 H27B 110.0 . . ? C28 C27 H27B 107.0 . . ? H27A C27 H27B 108.5 . . ? C27 C28 H28A 111.1 . . ? C27 C28 H28B 106.3 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 111.0 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C29 C30 112.6(5) . . ? C12 C29 H29A 108.3 . . ? C30 C29 H29A 108.4 . . ? C12 C29 H29B 109.6 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.0 . . ? C29 C30 H30A 109.9 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 108.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C13 C31 C32 113.5(6) . . ? C13 C31 H31A 110.2 . . ? C32 C31 H31A 109.4 . . ? C13 C31 H31B 107.7 . . ? C32 C31 H31B 107.9 . . ? H31A C31 H31B 108.0 . . ? C31 C32 H32A 110.9 . . ? C31 C32 H32B 108.0 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C17 C33 C34 112.6(7) . . ? C17 C33 H33A 108.8 . . ? C34 C33 H33A 111.7 . . ? C17 C33 H33B 108.1 . . ? C34 C33 H33B 107.2 . . ? H33A C33 H33B 108.3 . . ? C33 C34 H34A 110.2 . . ? C33 C34 H34B 106.8 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 111.4 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C35 C36 113.3(7) . . ? C18 C35 H35A 110.2 . . ? C36 C35 H35A 109.4 . . ? C18 C35 H35B 107.2 . . ? C36 C35 H35B 108.4 . . ? H35A C35 H35B 108.2 . . ? C35 C36 H36A 111.0 . . ? C35 C36 H36B 108.1 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.2 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? B1 O1 B2 116.2(6) . . ? O1 B1 F1 110.7(6) . . ? O1 B1 N2 114.3(6) . . ? F1 B1 N2 108.0(6) . . ? O1 B1 N1 113.4(6) . . ? F1 B1 N1 106.3(5) . . ? N2 B1 N1 103.6(6) . . ? F2 B2 O1 115.4(7) . . ? F2 B2 N4 111.0(6) . . ? O1 B2 N4 106.7(6) . . ? F2 B2 N3 109.1(6) . . ? O1 B2 N3 106.8(6) . . ? N4 B2 N3 107.5(6) . . ? C3A N1A C1A 121.2(8) . . ? C3A N1A C5A 119.1(8) . . ? C1A N1A C5A 96.2(8) . . ? C3A N1A H1A 107.2 . . ? C1A N1A H1A 105.2 . . ? C5A N1A H1A 106.3 . . ? N1A C1A C2A 107.1(8) . . ? N1A C1A H1AA 109.6 . . ? C2A C1A H1AA 109.5 . . ? N1A C1A H1AB 112.1 . . ? C2A C1A H1AB 109.9 . . ? H1AA C1A H1AB 108.7 . . ? C1A C2A H2AA 111.0 . . ? C1A C2A H2AB 108.9 . . ? H2AA C2A H2AB 109.5 . . ? C1A C2A H2AC 108.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? N1A C3A C4A 113.3(9) . . ? N1A C3A H3AA 108.6 . . ? C4A C3A H3AA 108.6 . . ? N1A C3A H3AB 109.1 . . ? C4A C3A H3AB 109.1 . . ? H3AA C3A H3AB 108.0 . . ? C3A C4A H4AA 110.5 . . ? C3A C4A H4AB 109.2 . . ? H4AA C4A H4AB 109.5 . . ? C3A C4A H4AC 108.7 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? C6A C5A N1A 98.5(10) . . ? C6A C5A H5AA 109.0 . . ? N1A C5A H5AA 111.7 . . ? C6A C5A H5AB 113.6 . . ? N1A C5A H5AB 112.9 . . ? H5AA C5A H5AB 110.5 . . ? C5A C6A H6AA 113.3 . . ? C5A C6A H6AB 109.8 . . ? H6AA C6A H6AB 109.5 . . ? C5A C6A H6AC 105.3 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? F3A B1A F4A 112.0(9) . . ? F3A B1A F2A 112.6(11) . . ? F4A B1A F2A 106.2(8) . . ? F3A B1A F1A 112.1(8) . . ? F4A B1A F1A 103.4(10) . . ? F2A B1A F1A 110.1(8) . . ? C4' N1' C1' 108.0(5) . . ? C4' N1' B1' 118.1(6) . . ? C1' N1' B1' 132.1(6) . . ? C6' N2' C9' 108.6(6) . . ? C6' N2' B1' 118.8(6) . . ? C9' N2' B1' 130.8(6) . . ? C14' N3' C11' 111.0(6) . . ? C14' N3' B2' 124.1(6) . . ? C11' N3' B2' 124.8(6) . . ? C19' N4' C16' 109.4(6) . . ? C19' N4' B2' 126.3(6) . . ? C16' N4' B2' 124.2(6) . . ? N1' C1' C20' 129.7(6) . . ? N1' C1' C2' 106.7(6) . . ? C20' C1' C2' 123.2(6) . . ? C3' C2' C1' 108.4(6) . . ? C3' C2' C21' 127.0(6) . . ? C1' C2' C21' 124.6(7) . . ? C2' C3' C4' 108.0(6) . . ? C2' C3' C23' 127.7(6) . . ? C4' C3' C23' 124.1(7) . . ? C5' C4' N1' 117.9(6) . . ? C5' C4' C3' 133.3(7) . . ? N1' C4' C3' 108.6(6) . . ? C4' C5' C6' 123.6(7) . . ? C4' C5' H5' 117.8 . . ? C6' C5' H5' 118.6 . . ? N2' C6' C5' 117.2(7) . . ? N2' C6' C7' 110.5(6) . . ? C5' C6' C7' 131.7(7) . . ? C8' C7' C6' 106.0(7) . . ? C8' C7' C25' 129.6(7) . . ? C6' C7' C25' 124.4(7) . . ? C7' C8' C9' 108.7(7) . . ? C7' C8' C27' 125.7(8) . . ? C9' C8' C27' 125.5(8) . . ? N2' C9' C10' 132.7(7) . . ? N2' C9' C8' 106.1(6) . . ? C10' C9' C8' 120.6(7) . . ? C11' C10' C9' 138.2(7) . . ? C11' C10' H10' 112.2 . . ? C9' C10' H10' 109.5 . . ? N3' C11' C10' 131.0(7) . . ? N3' C11' C12' 105.9(6) . . ? C10' C11' C12' 122.9(7) . . ? C13' C12' C11' 107.8(6) . . ? C13' C12' C29' 128.3(7) . . ? C11' C12' C29' 123.9(7) . . ? C12' C13' C14' 106.6(6) . . ? C12' C13' C31' 128.8(7) . . ? C14' C13' C31' 124.5(7) . . ? N3' C14' C15' 120.2(6) . . ? N3' C14' C13' 108.6(6) . . ? C15' C14' C13' 131.2(7) . . ? C16' C15' C14' 121.6(7) . . ? C16' C15' H15' 118.2 . . ? C14' C15' H15' 120.1 . . ? N4' C16' C15' 119.7(7) . . ? N4' C16' C17' 108.2(6) . . ? C15' C16' C17' 132.1(7) . . ? C18' C17' C16' 107.4(7) . . ? C18' C17' C33' 128.1(7) . . ? C16' C17' C33' 124.4(6) . . ? C17' C18' C19' 107.6(6) . . ? C17' C18' C35' 127.4(7) . . ? C19' C18' C35' 125.0(7) . . ? N4' C19' C20' 127.6(7) . . ? N4' C19' C18' 107.5(6) . . ? C20' C19' C18' 124.9(7) . . ? C19' C20' C1' 141.4(7) . . ? C19' C20' H20' 109.1 . . ? C1' C20' H20' 109.5 . . ? C22' C21' C2' 113.4(6) . . ? C22' C21' H21C 108.1 . . ? C2' C21' H21C 109.2 . . ? C22' C21' H21D 109.4 . . ? C2' C21' H21D 108.1 . . ? H21C C21' H21D 108.5 . . ? C21' C22' H22D 112.5 . . ? C21' C22' H22E 108.6 . . ? H22D C22' H22E 109.5 . . ? C21' C22' H22F 107.3 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C3' C23' C24' 112.6(6) . . ? C3' C23' H23C 109.2 . . ? C24' C23' H23C 109.3 . . ? C3' C23' H23D 109.4 . . ? C24' C23' H23D 108.3 . . ? H23C C23' H23D 107.9 . . ? C23' C24' H24D 110.3 . . ? C23' C24' H24E 108.5 . . ? H24D C24' H24E 109.5 . . ? C23' C24' H24F 109.6 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C7' C25' C26' 112.0(7) . . ? C7' C25' H25C 109.1 . . ? C26' C25' H25C 110.6 . . ? C7' C25' H25D 108.8 . . ? C26' C25' H25D 107.9 . . ? H25C C25' H25D 108.3 . . ? C25' C26' H26D 110.6 . . ? C25' C26' H26E 107.6 . . ? H26D C26' H26E 109.5 . . ? C25' C26' H26F 110.3 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C28A C27' C28' 115.9(15) . . ? C28A C27' C8' 117.5(14) . . ? C28' C27' C8' 125.9(13) . . ? C28A C27' H27E 102.1 . . ? C28' C27' H27E 67.6 . . ? C8' C27' H27E 108.6 . . ? C28A C27' H27F 111.2 . . ? C28' C27' H27F 40.3 . . ? C8' C27' H27F 109.3 . . ? H27E C27' H27F 107.7 . . ? C28A C27' H27C 64.6 . . ? C28' C27' H27C 104.2 . . ? C8' C27' H27C 105.8 . . ? H27E C27' H27C 43.9 . . ? H27F C27' H27C 141.2 . . ? C28A C27' H27D 41.8 . . ? C28' C27' H27D 106.9 . . ? C8' C27' H27D 106.3 . . ? H27E C27' H27D 139.4 . . ? H27F C27' H27D 79.2 . . ? H27C C27' H27D 106.4 . . ? C27' C28' H27E 42.8 . . ? C27' C28' H27F 46.4 . . ? H27E C28' H27F 89.1 . . ? C27' C28' H28D 110.7 . . ? H27E C28' H28D 99.7 . . ? H27F C28' H28D 114.0 . . ? C27' C28' H28E 110.3 . . ? H27E C28' H28E 76.2 . . ? H27F C28' H28E 135.8 . . ? H28D C28' H28E 109.5 . . ? C27' C28' H28F 107.4 . . ? H27E C28' H28F 145.5 . . ? H27F C28' H28F 62.6 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C27' C28A H27C 44.6 . . ? C27' C28A H27D 47.9 . . ? H27C C28A H27D 92.5 . . ? C27' C28A H28G 113.3 . . ? H27C C28A H28G 102.3 . . ? H27D C28A H28G 110.4 . . ? C27' C28A H28H 102.8 . . ? H27C C28A H28H 142.5 . . ? H27D C28A H28H 58.2 . . ? H28G C28A H28H 109.5 . . ? C27' C28A H28I 112.0 . . ? H27C C28A H28I 76.9 . . ? H27D C28A H28I 140.1 . . ? H28G C28A H28I 109.5 . . ? H28H C28A H28I 109.5 . . ? C12' C29' C30' 113.9(6) . . ? C12' C29' H29C 108.9 . . ? C30' C29' H29C 109.8 . . ? C12' C29' H29D 107.1 . . ? C30' C29' H29D 109.0 . . ? H29C C29' H29D 107.9 . . ? C29' C30' H30D 109.2 . . ? C29' C30' H30E 109.2 . . ? H30D C30' H30E 109.5 . . ? C29' C30' H30F 110.0 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? C32' C31' C13' 111.4(6) . . ? C32' C31' H31C 108.4 . . ? C13' C31' H31C 108.9 . . ? C32' C31' H31D 110.2 . . ? C13' C31' H31D 109.6 . . ? H31C C31' H31D 108.3 . . ? C31' C32' H32D 110.6 . . ? C31' C32' H32E 109.8 . . ? H32D C32' H32E 109.5 . . ? C31' C32' H32F 108.0 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C17' C33' C34' 111.6(6) . . ? C17' C33' H33C 109.7 . . ? C34' C33' H33C 109.7 . . ? C17' C33' H33D 109.2 . . ? C34' C33' H33D 108.6 . . ? H33C C33' H33D 108.1 . . ? C33' C34' H34D 110.1 . . ? C33' C34' H34E 108.6 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.7 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C36' C35' C18' 111.7(7) . . ? C36' C35' H35C 110.5 . . ? C18' C35' H35C 109.7 . . ? C36' C35' H35D 108.0 . . ? C18' C35' H35D 108.9 . . ? H35C C35' H35D 107.9 . . ? C35' C36' H36D 109.3 . . ? C35' C36' H36E 108.3 . . ? H36D C36' H36E 109.5 . . ? C35' C36' H36F 110.8 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? B1' O1' B2' 116.7(6) . . ? O1' B1' F1' 110.5(6) . . ? O1' B1' N2' 114.6(6) . . ? F1' B1' N2' 107.8(6) . . ? O1' B1' N1' 114.0(6) . . ? F1' B1' N1' 105.6(6) . . ? N2' B1' N1' 103.7(6) . . ? F2' B2' O1' 113.5(6) . . ? F2' B2' N4' 110.0(6) . . ? O1' B2' N4' 108.0(6) . . ? F2' B2' N3' 107.4(6) . . ? O1' B2' N3' 107.9(6) . . ? N4' B2' N3' 110.0(6) . . ? C5B N1B C1B 115.9(6) . . ? C5B N1B C3B 111.6(7) . . ? C1B N1B C3B 111.6(5) . . ? C5B N1B H1B 105.5 . . ? C1B N1B H1B 105.7 . . ? C3B N1B H1B 105.6 . . ? N1B C1B C2B 113.7(6) . . ? N1B C1B H1BA 109.4 . . ? C2B C1B H1BA 109.0 . . ? N1B C1B H1BB 108.2 . . ? C2B C1B H1BB 108.3 . . ? H1BA C1B H1BB 108.1 . . ? C1B C2B H2BA 111.3 . . ? C1B C2B H2BB 108.2 . . ? H2BA C2B H2BB 109.5 . . ? C1B C2B H2BC 108.9 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? C4B C3B N1B 112.8(7) . . ? C4B C3B H3BA 108.9 . . ? N1B C3B H3BA 109.9 . . ? C4B C3B H3BB 108.6 . . ? N1B C3B H3BB 108.5 . . ? H3BA C3B H3BB 108.0 . . ? C3B C4B H4BA 110.7 . . ? C3B C4B H4BB 108.7 . . ? H4BA C4B H4BB 109.5 . . ? C3B C4B H4BC 109.0 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? N1B C5B C6B 113.9(7) . . ? N1B C5B H5BA 108.3 . . ? C6B C5B H5BA 107.6 . . ? N1B C5B H5BB 109.9 . . ? C6B C5B H5BB 109.1 . . ? H5BA C5B H5BB 107.8 . . ? C5B C6B H6BA 110.9 . . ? C5B C6B H6BB 109.6 . . ? H6BA C6B H6BB 109.5 . . ? C5B C6B H6BC 108.0 . . ? H6BA C6B H6BC 109.5 . . ? H6BB C6B H6BC 109.5 . . ? F2B B1B F4B 112.0(9) . . ? F2B B1B F1B 110.3(9) . . ? F4B B1B F1B 108.2(9) . . ? F2B B1B F3B 108.8(9) . . ? F4B B1B F3B 110.2(10) . . ? F1B B1B F3B 107.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C20 170.0(7) . . . . ? B1 N1 C1 C20 -27.1(12) . . . . ? C4 N1 C1 C2 -5.3(7) . . . . ? B1 N1 C1 C2 157.6(6) . . . . ? N1 C1 C2 C3 3.7(7) . . . . ? C20 C1 C2 C3 -172.2(6) . . . . ? N1 C1 C2 C21 -178.3(6) . . . . ? C20 C1 C2 C21 5.8(10) . . . . ? C1 C2 C3 C4 -0.7(8) . . . . ? C21 C2 C3 C4 -178.7(6) . . . . ? C1 C2 C3 C23 -178.2(6) . . . . ? C21 C2 C3 C23 3.8(12) . . . . ? C1 N1 C4 C5 -168.9(6) . . . . ? B1 N1 C4 C5 25.2(9) . . . . ? C1 N1 C4 C3 4.9(7) . . . . ? B1 N1 C4 C3 -160.9(6) . . . . ? C2 C3 C4 N1 -2.6(8) . . . . ? C23 C3 C4 N1 175.1(6) . . . . ? C2 C3 C4 C5 170.2(7) . . . . ? C23 C3 C4 C5 -12.1(11) . . . . ? N1 C4 C5 C6 6.2(10) . . . . ? C3 C4 C5 C6 -166.0(7) . . . . ? C9 N2 C6 C5 172.2(5) . . . . ? B1 N2 C6 C5 -22.5(9) . . . . ? C9 N2 C6 C7 -2.1(8) . . . . ? B1 N2 C6 C7 163.3(6) . . . . ? C4 C5 C6 N2 -7.8(10) . . . . ? C4 C5 C6 C7 165.0(7) . . . . ? N2 C6 C7 C8 1.1(8) . . . . ? C5 C6 C7 C8 -172.2(7) . . . . ? N2 C6 C7 C25 177.3(6) . . . . ? C5 C6 C7 C25 3.9(12) . . . . ? C6 C7 C8 C9 0.2(8) . . . . ? C25 C7 C8 C9 -175.8(7) . . . . ? C6 C7 C8 C27 177.7(7) . . . . ? C25 C7 C8 C27 1.7(12) . . . . ? C6 N2 C9 C10 -168.9(7) . . . . ? B1 N2 C9 C10 28.5(12) . . . . ? C6 N2 C9 C8 2.2(7) . . . . ? B1 N2 C9 C8 -160.4(7) . . . . ? C7 C8 C9 N2 -1.5(8) . . . . ? C27 C8 C9 N2 -179.0(6) . . . . ? C7 C8 C9 C10 170.9(6) . . . . ? C27 C8 C9 C10 -6.7(11) . . . . ? N2 C9 C10 C11 11.2(14) . . . . ? C8 C9 C10 C11 -159.0(8) . . . . ? C14 N3 C11 C10 178.3(7) . . . . ? B2 N3 C11 C10 -2.5(11) . . . . ? C14 N3 C11 C12 3.7(7) . . . . ? B2 N3 C11 C12 -177.1(6) . . . . ? C9 C10 C11 N3 2.6(14) . . . . ? C9 C10 C11 C12 176.5(8) . . . . ? N3 C11 C12 C13 -2.9(8) . . . . ? C10 C11 C12 C13 -178.0(7) . . . . ? N3 C11 C12 C29 175.6(6) . . . . ? C10 C11 C12 C29 0.5(10) . . . . ? C11 C12 C13 C14 1.0(8) . . . . ? C29 C12 C13 C14 -177.4(6) . . . . ? C11 C12 C13 C31 -179.1(6) . . . . ? C29 C12 C13 C31 2.5(13) . . . . ? C11 N3 C14 C15 175.8(6) . . . . ? B2 N3 C14 C15 -3.5(10) . . . . ? C11 N3 C14 C13 -3.2(8) . . . . ? B2 N3 C14 C13 177.6(6) . . . . ? C12 C13 C14 N3 1.3(8) . . . . ? C31 C13 C14 N3 -178.6(6) . . . . ? C12 C13 C14 C15 -177.5(7) . . . . ? C31 C13 C14 C15 2.6(12) . . . . ? N3 C14 C15 C16 0.2(10) . . . . ? C13 C14 C15 C16 178.8(7) . . . . ? C19 N4 C16 C15 -178.8(6) . . . . ? B2 N4 C16 C15 0.4(11) . . . . ? C19 N4 C16 C17 0.4(8) . . . . ? B2 N4 C16 C17 179.6(7) . . . . ? C14 C15 C16 N4 1.4(10) . . . . ? C14 C15 C16 C17 -177.6(8) . . . . ? N4 C16 C17 C18 -0.3(9) . . . . ? C15 C16 C17 C18 178.7(8) . . . . ? N4 C16 C17 C33 -176.1(7) . . . . ? C15 C16 C17 C33 2.9(13) . . . . ? C16 C17 C18 C19 0.1(9) . . . . ? C33 C17 C18 C19 175.3(8) . . . . ? C16 C17 C18 C35 -176.5(8) . . . . ? C33 C17 C18 C35 -1.3(15) . . . . ? C16 N4 C19 C20 -179.9(7) . . . . ? B2 N4 C19 C20 1.0(11) . . . . ? C16 N4 C19 C18 -0.4(8) . . . . ? B2 N4 C19 C18 -179.5(7) . . . . ? C17 C18 C19 N4 0.2(8) . . . . ? C35 C18 C19 N4 176.8(7) . . . . ? C17 C18 C19 C20 179.7(7) . . . . ? C35 C18 C19 C20 -3.7(13) . . . . ? N4 C19 C20 C1 -2.4(15) . . . . ? C18 C19 C20 C1 178.2(9) . . . . ? N1 C1 C20 C19 -11.1(15) . . . . ? C2 C1 C20 C19 163.7(9) . . . . ? C3 C2 C21 C22 -104.7(8) . . . . ? C1 C2 C21 C22 77.7(9) . . . . ? C2 C3 C23 C24 86.8(9) . . . . ? C4 C3 C23 C24 -90.3(8) . . . . ? C8 C7 C25 C26 -114.9(8) . . . . ? C6 C7 C25 C26 69.7(9) . . . . ? C7 C8 C27 C28 -88.8(8) . . . . ? C9 C8 C27 C28 88.2(8) . . . . ? C13 C12 C29 C30 101.2(9) . . . . ? C11 C12 C29 C30 -77.0(8) . . . . ? C12 C13 C31 C32 -91.7(9) . . . . ? C14 C13 C31 C32 88.2(9) . . . . ? C18 C17 C33 C34 -98.2(10) . . . . ? C16 C17 C33 C34 76.5(9) . . . . ? C17 C18 C35 C36 94.3(10) . . . . ? C19 C18 C35 C36 -81.7(10) . . . . ? B2 O1 B1 F1 179.5(5) . . . . ? B2 O1 B1 N2 -58.3(8) . . . . ? B2 O1 B1 N1 60.1(8) . . . . ? C6 N2 B1 O1 171.1(6) . . . . ? C9 N2 B1 O1 -27.9(10) . . . . ? C6 N2 B1 F1 -65.2(7) . . . . ? C9 N2 B1 F1 95.8(8) . . . . ? C6 N2 B1 N1 47.2(8) . . . . ? C9 N2 B1 N1 -151.7(6) . . . . ? C1 N1 B1 O1 25.4(10) . . . . ? C4 N1 B1 O1 -172.8(6) . . . . ? C1 N1 B1 F1 -96.5(8) . . . . ? C4 N1 B1 F1 65.3(8) . . . . ? C1 N1 B1 N2 149.9(6) . . . . ? C4 N1 B1 N2 -48.4(7) . . . . ? B1 O1 B2 F2 -0.1(9) . . . . ? B1 O1 B2 N4 -124.0(6) . . . . ? B1 O1 B2 N3 121.3(6) . . . . ? C16 N4 B2 F2 116.2(7) . . . . ? C19 N4 B2 F2 -64.8(9) . . . . ? C16 N4 B2 O1 -117.2(7) . . . . ? C19 N4 B2 O1 61.8(8) . . . . ? C16 N4 B2 N3 -3.0(10) . . . . ? C19 N4 B2 N3 176.0(6) . . . . ? C11 N3 B2 F2 65.0(9) . . . . ? C14 N3 B2 F2 -115.9(7) . . . . ? C11 N3 B2 O1 -60.4(9) . . . . ? C14 N3 B2 O1 118.7(7) . . . . ? C11 N3 B2 N4 -174.6(6) . . . . ? C14 N3 B2 N4 4.5(10) . . . . ? C3A N1A C1A C2A 56.9(11) . . . . ? C5A N1A C1A C2A -173.4(7) . . . . ? C1A N1A C3A C4A 57.2(14) . . . . ? C5A N1A C3A C4A -61.6(13) . . . . ? C3A N1A C5A C6A -49.8(11) . . . . ? C1A N1A C5A C6A 179.1(9) . . . . ? C4' N1' C1' C20' 170.1(7) . . . . ? B1' N1' C1' C20' -26.2(12) . . . . ? C4' N1' C1' C2' -3.7(7) . . . . ? B1' N1' C1' C2' 160.0(7) . . . . ? N1' C1' C2' C3' 1.2(8) . . . . ? C20' C1' C2' C3' -173.1(7) . . . . ? N1' C1' C2' C21' 179.4(6) . . . . ? C20' C1' C2' C21' 5.0(11) . . . . ? C1' C2' C3' C4' 1.8(8) . . . . ? C21' C2' C3' C4' -176.3(6) . . . . ? C1' C2' C3' C23' 176.7(6) . . . . ? C21' C2' C3' C23' -1.4(13) . . . . ? C1' N1' C4' C5' -171.5(6) . . . . ? B1' N1' C4' C5' 22.2(9) . . . . ? C1' N1' C4' C3' 4.9(7) . . . . ? B1' N1' C4' C3' -161.4(6) . . . . ? C2' C3' C4' C5' 171.4(8) . . . . ? C23' C3' C4' C5' -3.7(12) . . . . ? C2' C3' C4' N1' -4.2(8) . . . . ? C23' C3' C4' N1' -179.3(6) . . . . ? N1' C4' C5' C6' 9.3(10) . . . . ? C3' C4' C5' C6' -166.0(7) . . . . ? C9' N2' C6' C5' 170.4(6) . . . . ? B1' N2' C6' C5' -23.1(9) . . . . ? C9' N2' C6' C7' -1.7(8) . . . . ? B1' N2' C6' C7' 164.7(6) . . . . ? C4' C5' C6' N2' -9.3(10) . . . . ? C4' C5' C6' C7' 160.9(8) . . . . ? N2' C6' C7' C8' -0.4(8) . . . . ? C5' C6' C7' C8' -171.1(7) . . . . ? N2' C6' C7' C25' 178.7(7) . . . . ? C5' C6' C7' C25' 8.0(13) . . . . ? C6' C7' C8' C9' 2.3(8) . . . . ? C25' C7' C8' C9' -176.8(7) . . . . ? C6' C7' C8' C27' -179.6(9) . . . . ? C25' C7' C8' C27' 1.4(14) . . . . ? C6' N2' C9' C10' -168.0(7) . . . . ? B1' N2' C9' C10' 27.7(12) . . . . ? C6' N2' C9' C8' 3.0(8) . . . . ? B1' N2' C9' C8' -161.2(7) . . . . ? C7' C8' C9' N2' -3.3(8) . . . . ? C27' C8' C9' N2' 178.5(8) . . . . ? C7' C8' C9' C10' 169.1(6) . . . . ? C27' C8' C9' C10' -9.1(13) . . . . ? N2' C9' C10' C11' 8.9(15) . . . . ? C8' C9' C10' C11' -161.1(8) . . . . ? C14' N3' C11' C10' 177.4(7) . . . . ? B2' N3' C11' C10' -3.7(12) . . . . ? C14' N3' C11' C12' 2.3(7) . . . . ? B2' N3' C11' C12' -178.7(6) . . . . ? C9' C10' C11' N3' 4.8(15) . . . . ? C9' C10' C11' C12' 179.1(7) . . . . ? N3' C11' C12' C13' -2.0(8) . . . . ? C10' C11' C12' C13' -177.5(7) . . . . ? N3' C11' C12' C29' 180.0(6) . . . . ? C10' C11' C12' C29' 4.4(11) . . . . ? C11' C12' C13' C14' 0.9(8) . . . . ? C29' C12' C13' C14' 178.8(6) . . . . ? C11' C12' C13' C31' -177.8(6) . . . . ? C29' C12' C13' C31' 0.1(12) . . . . ? C11' N3' C14' C15' 178.7(6) . . . . ? B2' N3' C14' C15' -0.2(10) . . . . ? C11' N3' C14' C13' -1.9(8) . . . . ? B2' N3' C14' C13' 179.2(6) . . . . ? C12' C13' C14' N3' 0.5(8) . . . . ? C31' C13' C14' N3' 179.3(6) . . . . ? C12' C13' C14' C15' 179.8(7) . . . . ? C31' C13' C14' C15' -1.4(12) . . . . ? N3' C14' C15' C16' -3.0(10) . . . . ? C13' C14' C15' C16' 177.8(7) . . . . ? C19' N4' C16' C15' -178.7(6) . . . . ? B2' N4' C16' C15' -1.4(10) . . . . ? C19' N4' C16' C17' 0.2(7) . . . . ? B2' N4' C16' C17' 177.4(6) . . . . ? C14' C15' C16' N4' 3.7(10) . . . . ? C14' C15' C16' C17' -174.8(7) . . . . ? N4' C16' C17' C18' 1.5(8) . . . . ? C15' C16' C17' C18' -179.8(7) . . . . ? N4' C16' C17' C33' -176.6(6) . . . . ? C15' C16' C17' C33' 2.0(12) . . . . ? C16' C17' C18' C19' -2.6(8) . . . . ? C33' C17' C18' C19' 175.5(7) . . . . ? C16' C17' C18' C35' 177.6(7) . . . . ? C33' C17' C18' C35' -4.3(12) . . . . ? C16' N4' C19' C20' -179.4(7) . . . . ? B2' N4' C19' C20' 3.5(11) . . . . ? C16' N4' C19' C18' -1.8(7) . . . . ? B2' N4' C19' C18' -178.9(6) . . . . ? C17' C18' C19' N4' 2.8(8) . . . . ? C35' C18' C19' N4' -177.4(6) . . . . ? C17' C18' C19' C20' -179.6(7) . . . . ? C35' C18' C19' C20' 0.2(12) . . . . ? N4' C19' C20' C1' -0.3(15) . . . . ? C18' C19' C20' C1' -177.5(8) . . . . ? N1' C1' C20' C19' -14.1(15) . . . . ? C2' C1' C20' C19' 158.8(8) . . . . ? C3' C2' C21' C22' 98.1(9) . . . . ? C1' C2' C21' C22' -79.8(9) . . . . ? C2' C3' C23' C24' -84.2(9) . . . . ? C4' C3' C23' C24' 89.9(8) . . . . ? C8' C7' C25' C26' -100.7(9) . . . . ? C6' C7' C25' C26' 80.4(9) . . . . ? C7' C8' C27' C28A -83(2) . . . . ? C9' C8' C27' C28A 94.9(19) . . . . ? C7' C8' C27' C28' 107.5(14) . . . . ? C9' C8' C27' C28' -74.7(17) . . . . ? C13' C12' C29' C30' -99.3(9) . . . . ? C11' C12' C29' C30' 78.3(9) . . . . ? C12' C13' C31' C32' 89.0(9) . . . . ? C14' C13' C31' C32' -89.5(8) . . . . ? C18' C17' C33' C34' -97.7(8) . . . . ? C16' C17' C33' C34' 80.1(8) . . . . ? C17' C18' C35' C36' 89.5(9) . . . . ? C19' C18' C35' C36' -90.3(9) . . . . ? B2' O1' B1' F1' 178.8(5) . . . . ? B2' O1' B1' N2' -59.2(8) . . . . ? B2' O1' B1' N1' 60.0(8) . . . . ? C6' N2' B1' O1' 172.4(6) . . . . ? C9' N2' B1' O1' -24.7(10) . . . . ? C6' N2' B1' F1' -64.1(7) . . . . ? C9' N2' B1' F1' 98.8(8) . . . . ? C6' N2' B1' N1' 47.5(8) . . . . ? C9' N2' B1' N1' -149.6(6) . . . . ? C4' N1' B1' O1' -172.3(6) . . . . ? C1' N1' B1' O1' 25.2(11) . . . . ? C4' N1' B1' F1' 66.1(8) . . . . ? C1' N1' B1' F1' -96.3(8) . . . . ? C4' N1' B1' N2' -47.1(8) . . . . ? C1' N1' B1' N2' 150.5(7) . . . . ? B1' O1' B2' F2' 1.4(8) . . . . ? B1' O1' B2' N4' -120.9(6) . . . . ? B1' O1' B2' N3' 120.2(6) . . . . ? C19' N4' B2' F2' -66.5(9) . . . . ? C16' N4' B2' F2' 116.7(7) . . . . ? C19' N4' B2' O1' 57.8(8) . . . . ? C16' N4' B2' O1' -118.9(7) . . . . ? C19' N4' B2' N3' 175.4(6) . . . . ? C16' N4' B2' N3' -1.3(10) . . . . ? C14' N3' B2' F2' -117.6(7) . . . . ? C11' N3' B2' F2' 63.7(9) . . . . ? C14' N3' B2' O1' 119.8(7) . . . . ? C11' N3' B2' O1' -59.0(9) . . . . ? C14' N3' B2' N4' 2.2(9) . . . . ? C11' N3' B2' N4' -176.6(6) . . . . ? C5B N1B C1B C2B -49.7(9) . . . . ? C3B N1B C1B C2B -179.0(7) . . . . ? C5B N1B C3B C4B 168.5(6) . . . . ? C1B N1B C3B C4B -60.1(8) . . . . ? C1B N1B C5B C6B -63.2(9) . . . . ? C3B N1B C5B C6B 66.0(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A O1 0.90 1.89 2.788(7) 173.1 . N1B H1B O1' 0.90 1.93 2.803(7) 164.1 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.43 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.367 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.058 data_bisbf2 _database_code_depnum_ccdc_archive 'CCDC 228380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H58 B2 Cl6 F4 N8' _chemical_formula_weight 1117.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1909(2) _cell_length_b 13.2259(2) _cell_length_c 19.4190(3) _cell_angle_alpha 93.425(1) _cell_angle_beta 103.208(1) _cell_angle_gamma 99.454(1) _cell_volume 2991.34(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour 'metallic blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Three molecules of methylene chloride solvate were found to be disordered. The molecules could not be satisfactorily modeled. The contributions by these solvate molecules to the scattering were removed by use of the utility, SQUEEZE (Sluis and Spek, 1990). ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25852 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13719 _reflns_number_gt 7534 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990) Acta Cryst. A46, 194-201. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0121(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13719 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 2.371 _refine_ls_restrained_S_all 2.371 _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 N1 N 0.39158(19) 0.17260(16) 0.45787(11) 0.0300(6) Uani 1 1 d . . . N2 N 0.3365(2) 0.33294(17) 0.35405(12) 0.0356(6) Uani 1 1 d . . . H2N H 0.4024 0.3608 0.3857 0.043 Uiso 1 1 d R . . N3 N 0.3894(2) 0.47337(17) 0.21177(12) 0.0357(6) Uani 1 1 d . . . H3N H 0.3783 0.4203 0.1782 0.043 Uiso 1 1 d R . . N4 N 0.5552(2) 0.55007(16) 0.11758(12) 0.0359(6) Uani 1 1 d . . . N5 N 0.6836(2) 0.42908(16) 0.09324(11) 0.0339(6) Uani 1 1 d . . . N6 N 0.76689(19) 0.30715(16) 0.21651(11) 0.0326(6) Uani 1 1 d . . . H6N H 0.7772 0.3734 0.2342 0.039 Uiso 1 1 d R . . N7 N 0.72954(19) 0.18603(16) 0.37211(11) 0.0306(6) Uani 1 1 d . . . H7N H 0.6719 0.1330 0.3532 0.037 Uiso 1 1 d R . . N8 N 0.59980(19) 0.15881(16) 0.49154(11) 0.0279(5) Uani 1 1 d . . . C1 C 0.3784(2) 0.12127(19) 0.51782(14) 0.0305(7) Uani 1 1 d . . . C2 C 0.2621(2) 0.1098(2) 0.52119(15) 0.0326(7) Uani 1 1 d . . . C3 C 0.2043(3) 0.1510(2) 0.46222(16) 0.0389(7) Uani 1 1 d . . . C4 C 0.2864(2) 0.1900(2) 0.42408(15) 0.0322(7) Uani 1 1 d . . . C5 C 0.2651(2) 0.2446(2) 0.36138(15) 0.0353(7) Uani 1 1 d . . . C6 C 0.1747(3) 0.2266(2) 0.30105(16) 0.0425(8) Uani 1 1 d . . . C7 C 0.1914(3) 0.3068(2) 0.25781(16) 0.0426(8) Uani 1 1 d . . . C8 C 0.2921(3) 0.3722(2) 0.29181(15) 0.0365(7) Uani 1 1 d . . . C9 C 0.3535(3) 0.4677(2) 0.27379(15) 0.0380(7) Uani 1 1 d . . . C10 C 0.3870(3) 0.5651(2) 0.31132(16) 0.0449(8) Uani 1 1 d . . . C11 C 0.4431(3) 0.6299(2) 0.27003(16) 0.0442(8) Uani 1 1 d . . . C12 C 0.4438(3) 0.5717(2) 0.20874(14) 0.0355(7) Uani 1 1 d . . . C13 C 0.4910(3) 0.6050(2) 0.14935(14) 0.0354(7) Uani 1 1 d . . . C14 C 0.4774(3) 0.6953(2) 0.11582(15) 0.0395(8) Uani 1 1 d . . . C15 C 0.5372(3) 0.6965(2) 0.06304(15) 0.0394(8) Uani 1 1 d . . . C16 C 0.5866(3) 0.6066(2) 0.06403(15) 0.0375(7) Uani 1 1 d . . . C17 C 0.6558(3) 0.5719(2) 0.02465(15) 0.0420(8) Uani 1 1 d . . . H17 H 0.6727 0.6107 -0.0131 0.050 Uiso 1 1 d R . . C18 C 0.7037(3) 0.4851(2) 0.03752(14) 0.0365(7) Uani 1 1 d . . . C19 C 0.7755(3) 0.4393(2) 0.00364(15) 0.0382(7) Uani 1 1 d . . . C22 C 0.7473(3) 0.2743(2) 0.14590(14) 0.0341(7) Uani 1 1 d . . . C20 C 0.7991(3) 0.3536(2) 0.03728(15) 0.0390(7) Uani 1 1 d . . . C21 C 0.7422(3) 0.3474(2) 0.09277(14) 0.0378(7) Uani 1 1 d . . . C23 C 0.7401(3) 0.1688(2) 0.14064(15) 0.0419(8) Uani 1 1 d . . . C24 C 0.7548(3) 0.1374(2) 0.21044(15) 0.0370(7) Uani 1 1 d . . . C25 C 0.7712(2) 0.2263(2) 0.25694(14) 0.0310(7) Uani 1 1 d . . . C26 C 0.7937(2) 0.2439(2) 0.33340(14) 0.0283(6) Uani 1 1 d . . . C27 C 0.8743(2) 0.3160(2) 0.38076(15) 0.0313(7) Uani 1 1 d . . . C28 C 0.8574(2) 0.3021(2) 0.45005(14) 0.0302(7) Uani 1 1 d . . . C29 C 0.7676(2) 0.2213(2) 0.44295(14) 0.0289(7) Uani 1 1 d . . . C30 C 0.7151(2) 0.17633(19) 0.49781(14) 0.0267(6) Uani 1 1 d . . . C31 C 0.7708(2) 0.1430(2) 0.56128(14) 0.0313(7) Uani 1 1 d . . . C32 C 0.6867(2) 0.10405(19) 0.59623(14) 0.0298(7) Uani 1 1 d . . . C33 C 0.5817(2) 0.11485(19) 0.55266(14) 0.0281(6) Uani 1 1 d . . . C34 C 0.4710(2) 0.09433(18) 0.56265(14) 0.0286(7) Uani 1 1 d . . . H34 H 0.4589 0.0608 0.6035 0.034 Uiso 1 1 d R . . C35 C 0.2132(3) 0.0660(2) 0.57875(16) 0.0443(8) Uani 1 1 d . . . H35C H 0.2741 0.0554 0.6172 0.066 Uiso 1 1 d R . . H35A H 0.1630 0.0016 0.5603 0.066 Uiso 1 1 d R . . H35B H 0.1692 0.1117 0.5955 0.066 Uiso 1 1 d R . . C36 C 0.0842(3) 0.1677(3) 0.44926(18) 0.0531(9) Uani 1 1 d . . . H36C H 0.0686 0.2110 0.4116 0.080 Uiso 1 1 d R . . H36A H 0.0725 0.1990 0.4923 0.080 Uiso 1 1 d R . . H36B H 0.0333 0.1023 0.4373 0.080 Uiso 1 1 d R . . C37 C 0.0769(3) 0.1351(3) 0.28056(19) 0.0593(10) Uani 1 1 d . . . H37A H 0.0810 0.0904 0.3179 0.089 Uiso 1 1 d R . . H37B H 0.0056 0.1597 0.2727 0.089 Uiso 1 1 d R . . H37C H 0.0815 0.0978 0.2377 0.089 Uiso 1 1 d R . . C38 C 0.1115(3) 0.3192(3) 0.18860(17) 0.0564(9) Uani 1 1 d . . . H38A H 0.1421 0.3791 0.1686 0.085 Uiso 1 1 d R . . H38B H 0.1014 0.2593 0.1558 0.085 Uiso 1 1 d R . . H38C H 0.0389 0.3269 0.1975 0.085 Uiso 1 1 d R . . C39 C 0.3629(4) 0.5966(3) 0.38140(17) 0.0665(11) Uani 1 1 d . . . H39A H 0.3216 0.5381 0.3975 0.100 Uiso 1 1 d R . . H39B H 0.4346 0.6209 0.4154 0.100 Uiso 1 1 d R . . H39C H 0.3184 0.6504 0.3764 0.100 Uiso 1 1 d R . . C40 C 0.5029(3) 0.7403(2) 0.29395(18) 0.0619(10) Uani 1 1 d . . . H40A H 0.5364 0.7684 0.2575 0.093 Uiso 1 1 d R . . H40B H 0.4479 0.7802 0.3033 0.093 Uiso 1 1 d R . . H40C H 0.5619 0.7423 0.3366 0.093 Uiso 1 1 d R . . C41 C 0.4047(3) 0.7702(2) 0.12973(17) 0.0510(9) Uani 1 1 d . . . H41C H 0.4528 0.8349 0.1501 0.077 Uiso 1 1 d R . . H41A H 0.3599 0.7452 0.1620 0.077 Uiso 1 1 d R . . H41B H 0.3534 0.7799 0.0862 0.077 Uiso 1 1 d R . . C42 C 0.5478(3) 0.7775(2) 0.01300(16) 0.0494(9) Uani 1 1 d . . . H42A H 0.5085 0.8312 0.0241 0.074 Uiso 1 1 d R . . H42B H 0.6272 0.8059 0.0178 0.074 Uiso 1 1 d R . . H42C H 0.5142 0.7474 -0.0350 0.074 Uiso 1 1 d R . . C43 C 0.8216(3) 0.4796(2) -0.05720(16) 0.0519(9) Uani 1 1 d . . . H43C H 0.9032 0.4833 -0.0459 0.078 Uiso 1 1 d R . . H43A H 0.8050 0.5470 -0.0652 0.078 Uiso 1 1 d R . . H43B H 0.7878 0.4343 -0.1000 0.078 Uiso 1 1 d R . . C44 C 0.8808(3) 0.2868(2) 0.02234(17) 0.0515(9) Uani 1 1 d . . . H44C H 0.9009 0.2467 0.0614 0.077 Uiso 1 1 d R . . H44A H 0.9486 0.3291 0.0155 0.077 Uiso 1 1 d R . . H44B H 0.8459 0.2417 -0.0204 0.077 Uiso 1 1 d R . . C45 C 0.7118(3) 0.0945(2) 0.07409(17) 0.0607(10) Uani 1 1 d . . . H45C H 0.6989 0.1314 0.0328 0.091 Uiso 1 1 d R . . H45A H 0.6446 0.0443 0.0728 0.091 Uiso 1 1 d R . . H45B H 0.7745 0.0589 0.0744 0.091 Uiso 1 1 d R . . C46 C 0.7587(3) 0.0303(2) 0.23008(17) 0.0561(10) Uani 1 1 d . . . H46C H 0.7876 0.0323 0.2806 0.084 Uiso 1 1 d R . . H46A H 0.8077 -0.0008 0.2064 0.084 Uiso 1 1 d R . . H46B H 0.6832 -0.0111 0.2166 0.084 Uiso 1 1 d R . . C47 C 0.9685(3) 0.3926(2) 0.36343(16) 0.0435(8) Uani 1 1 d . . . H47A H 0.9611 0.3865 0.3130 0.065 Uiso 1 1 d R . . H47B H 0.9617 0.4611 0.3790 0.065 Uiso 1 1 d R . . H47C H 1.0419 0.3791 0.3872 0.065 Uiso 1 1 d R . . C48 C 0.9189(3) 0.3690(2) 0.51664(15) 0.0422(8) Uani 1 1 d . . . H48A H 0.8919 0.3433 0.5562 0.063 Uiso 1 1 d R . . H48B H 0.9997 0.3697 0.5248 0.063 Uiso 1 1 d R . . H48C H 0.9046 0.4378 0.5117 0.063 Uiso 1 1 d R . . C49 C 0.8969(2) 0.1395(2) 0.58631(15) 0.0407(8) Uani 1 1 d . . . H49C H 0.9350 0.1575 0.5494 0.061 Uiso 1 1 d R . . H49A H 0.9065 0.0717 0.5985 0.061 Uiso 1 1 d R . . H49B H 0.9298 0.1871 0.6281 0.061 Uiso 1 1 d R . . C50 C 0.7062(3) 0.0592(2) 0.66540(14) 0.0378(7) Uani 1 1 d . . . H50C H 0.6343 0.0409 0.6780 0.057 Uiso 1 1 d R . . H50A H 0.7574 0.1083 0.7019 0.057 Uiso 1 1 d R . . H50B H 0.7397 -0.0011 0.6619 0.057 Uiso 1 1 d R . . B1 B 0.5079(3) 0.1983(2) 0.43610(17) 0.0308(8) Uani 1 1 d . . . F1 F 0.49417(13) 0.14730(12) 0.36845(8) 0.0421(4) Uani 1 1 d . . . F2 F 0.54107(13) 0.30292(11) 0.43453(9) 0.0434(4) Uani 1 1 d . . . B2 B 0.6050(3) 0.4549(3) 0.14132(18) 0.0394(9) Uani 1 1 d . . . F3 F 0.66587(17) 0.47707(13) 0.21288(8) 0.0548(5) Uani 1 1 d . . . F4 F 0.51632(16) 0.36919(12) 0.13614(9) 0.0504(5) 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 0.0286(14) 0.0330(13) 0.0320(14) 0.0087(10) 0.0124(12) 0.0067(11) N2 0.0318(14) 0.0441(15) 0.0346(15) 0.0119(11) 0.0125(12) 0.0085(12) N3 0.0485(16) 0.0315(14) 0.0297(14) 0.0031(10) 0.0129(12) 0.0095(12) N4 0.0535(17) 0.0307(13) 0.0276(13) 0.0073(10) 0.0141(13) 0.0115(12) N5 0.0455(16) 0.0347(14) 0.0250(13) 0.0080(10) 0.0133(12) 0.0081(12) N6 0.0437(16) 0.0283(13) 0.0264(14) 0.0047(10) 0.0092(12) 0.0067(11) N7 0.0312(14) 0.0335(13) 0.0286(14) 0.0075(10) 0.0112(11) 0.0027(11) N8 0.0268(14) 0.0341(13) 0.0251(13) 0.0085(10) 0.0105(11) 0.0043(10) C1 0.0340(18) 0.0303(16) 0.0304(16) 0.0090(12) 0.0126(14) 0.0063(13) C2 0.0344(18) 0.0310(16) 0.0388(18) 0.0084(13) 0.0182(15) 0.0091(13) C3 0.0357(19) 0.0392(17) 0.047(2) 0.0135(14) 0.0156(16) 0.0105(14) C4 0.0282(17) 0.0397(17) 0.0359(17) 0.0116(13) 0.0137(14) 0.0152(13) C5 0.0312(18) 0.0454(18) 0.0340(18) 0.0102(14) 0.0114(15) 0.0136(15) C6 0.0348(19) 0.053(2) 0.043(2) 0.0138(15) 0.0113(17) 0.0132(16) C7 0.039(2) 0.060(2) 0.0376(19) 0.0198(16) 0.0137(16) 0.0222(17) C8 0.0383(19) 0.0503(19) 0.0284(17) 0.0137(14) 0.0125(15) 0.0197(16) C9 0.048(2) 0.0432(18) 0.0323(17) 0.0134(14) 0.0174(16) 0.0195(15) C10 0.063(2) 0.049(2) 0.0314(18) 0.0090(15) 0.0178(17) 0.0227(17) C11 0.059(2) 0.0388(18) 0.0379(19) 0.0056(15) 0.0161(17) 0.0124(16) C12 0.051(2) 0.0317(17) 0.0256(16) 0.0050(12) 0.0089(15) 0.0108(14) C13 0.048(2) 0.0326(16) 0.0259(16) 0.0044(13) 0.0098(15) 0.0061(14) C14 0.060(2) 0.0247(16) 0.0328(18) 0.0021(13) 0.0102(16) 0.0081(15) C15 0.055(2) 0.0290(16) 0.0345(18) 0.0073(13) 0.0113(16) 0.0049(15) C16 0.052(2) 0.0301(17) 0.0311(17) 0.0083(13) 0.0119(16) 0.0055(15) C17 0.054(2) 0.0415(19) 0.0330(18) 0.0094(14) 0.0150(16) 0.0077(16) C18 0.048(2) 0.0362(17) 0.0248(16) 0.0050(13) 0.0100(15) 0.0023(15) C19 0.0426(19) 0.0457(18) 0.0276(16) 0.0082(14) 0.0117(15) 0.0061(15) C22 0.0423(19) 0.0387(18) 0.0246(17) 0.0071(13) 0.0112(14) 0.0107(14) C20 0.0434(19) 0.0486(19) 0.0278(17) 0.0046(14) 0.0111(15) 0.0124(15) C21 0.0421(19) 0.0437(18) 0.0268(17) 0.0044(13) 0.0085(15) 0.0049(15) C23 0.056(2) 0.0444(19) 0.0282(17) 0.0061(14) 0.0120(16) 0.0146(16) C24 0.0432(19) 0.0362(17) 0.0336(17) 0.0092(14) 0.0103(15) 0.0094(14) C25 0.0306(17) 0.0357(16) 0.0300(17) 0.0107(13) 0.0098(14) 0.0092(13) C26 0.0267(16) 0.0363(16) 0.0262(16) 0.0102(13) 0.0100(14) 0.0105(13) C27 0.0286(17) 0.0339(16) 0.0361(17) 0.0104(13) 0.0144(14) 0.0074(13) C28 0.0277(16) 0.0362(16) 0.0280(16) 0.0072(13) 0.0075(13) 0.0067(13) C29 0.0265(16) 0.0354(16) 0.0268(16) 0.0060(12) 0.0087(13) 0.0075(13) C30 0.0292(17) 0.0284(15) 0.0248(15) 0.0029(11) 0.0102(13) 0.0062(12) C31 0.0329(18) 0.0346(16) 0.0261(16) 0.0013(12) 0.0088(14) 0.0036(13) C32 0.0339(18) 0.0324(16) 0.0261(16) 0.0061(12) 0.0118(14) 0.0070(13) C33 0.0295(18) 0.0279(15) 0.0271(16) 0.0025(12) 0.0076(14) 0.0052(13) C34 0.0364(18) 0.0235(14) 0.0260(15) 0.0026(11) 0.0088(14) 0.0043(13) C35 0.044(2) 0.0466(19) 0.053(2) 0.0227(15) 0.0249(17) 0.0135(15) C36 0.039(2) 0.066(2) 0.067(2) 0.0230(18) 0.0261(18) 0.0201(17) C37 0.040(2) 0.070(2) 0.069(3) 0.0250(19) 0.0092(19) 0.0132(18) C38 0.048(2) 0.077(2) 0.045(2) 0.0201(17) 0.0043(18) 0.0166(19) C39 0.103(3) 0.069(2) 0.042(2) 0.0036(17) 0.037(2) 0.031(2) C40 0.099(3) 0.044(2) 0.044(2) -0.0006(16) 0.017(2) 0.020(2) C41 0.069(3) 0.0437(19) 0.049(2) 0.0133(15) 0.0184(19) 0.0260(17) C42 0.069(2) 0.0371(18) 0.049(2) 0.0140(15) 0.0233(19) 0.0123(16) C43 0.063(2) 0.061(2) 0.0383(19) 0.0134(15) 0.0223(18) 0.0139(18) C44 0.055(2) 0.068(2) 0.041(2) 0.0157(16) 0.0194(18) 0.0234(18) C45 0.094(3) 0.049(2) 0.043(2) 0.0029(16) 0.018(2) 0.022(2) C46 0.080(3) 0.045(2) 0.046(2) 0.0129(16) 0.015(2) 0.0173(18) C47 0.044(2) 0.0490(19) 0.0390(19) 0.0097(14) 0.0163(16) 0.0017(15) C48 0.043(2) 0.0461(18) 0.0330(18) 0.0025(14) 0.0081(15) -0.0020(15) C49 0.0358(19) 0.0536(19) 0.0353(18) 0.0141(14) 0.0100(15) 0.0095(15) C50 0.0388(19) 0.0440(18) 0.0319(17) 0.0102(13) 0.0094(15) 0.0079(14) B1 0.029(2) 0.038(2) 0.0268(19) 0.0064(15) 0.0102(16) 0.0038(15) F1 0.0293(10) 0.0694(12) 0.0279(9) 0.0046(8) 0.0096(8) 0.0061(8) F2 0.0376(10) 0.0382(10) 0.0537(11) 0.0211(8) 0.0077(9) 0.0039(8) B2 0.052(2) 0.037(2) 0.032(2) 0.0081(15) 0.0132(19) 0.0080(18) F3 0.0847(15) 0.0600(12) 0.0297(10) 0.0065(8) 0.0171(10) 0.0364(10) F4 0.0710(13) 0.0383(10) 0.0545(11) 0.0091(8) 0.0363(10) 0.0150(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C4 1.363(3) . ? N1 C1 1.409(3) . ? N1 B1 1.561(4) . ? N2 C5 1.373(3) . ? N2 C8 1.375(3) . ? N2 H2N 0.9000 . ? N3 C12 1.370(3) . ? N3 C9 1.375(3) . ? N3 H3N 0.9000 . ? N4 C13 1.369(3) . ? N4 C16 1.402(3) . ? N4 B2 1.536(4) . ? N5 C21 1.390(4) . ? N5 C18 1.392(3) . ? N5 B2 1.544(4) . ? N6 C25 1.365(3) . ? N6 C22 1.368(3) . ? N6 H6N 0.8998 . ? N7 C29 1.373(3) . ? N7 C26 1.380(3) . ? N7 H7N 0.9000 . ? N8 C30 1.362(3) . ? N8 C33 1.398(3) . ? N8 B1 1.548(4) . ? C1 C34 1.371(4) . ? C1 C2 1.418(4) . ? C2 C3 1.391(4) . ? C2 C35 1.486(4) . ? C3 C4 1.425(4) . ? C3 C36 1.484(4) . ? C4 C5 1.447(4) . ? C5 C6 1.391(4) . ? C6 C7 1.409(4) . ? C6 C37 1.515(4) . ? C7 C8 1.380(4) . ? C7 C38 1.505(4) . ? C8 C9 1.463(4) . ? C9 C10 1.391(4) . ? C10 C11 1.409(4) . ? C10 C39 1.505(4) . ? C11 C12 1.381(4) . ? C11 C40 1.515(4) . ? C12 C13 1.461(4) . ? C13 C14 1.410(4) . ? C14 C15 1.386(4) . ? C14 C41 1.485(4) . ? C15 C16 1.418(4) . ? C15 C42 1.498(4) . ? C16 C17 1.374(4) . ? C17 C18 1.381(4) . ? C17 H17 0.9599 . ? C18 C19 1.398(4) . ? C19 C20 1.380(4) . ? C19 C43 1.509(4) . ? C22 C23 1.380(4) . ? C22 C21 1.454(4) . ? C20 C21 1.408(4) . ? C20 C44 1.499(4) . ? C23 C24 1.422(4) . ? C23 C45 1.513(4) . ? C24 C25 1.397(4) . ? C24 C46 1.494(4) . ? C25 C26 1.444(4) . ? C26 C27 1.377(4) . ? C27 C28 1.425(3) . ? C27 C47 1.514(4) . ? C28 C29 1.374(4) . ? C28 C48 1.490(4) . ? C29 C30 1.470(3) . ? C30 C31 1.398(4) . ? C31 C32 1.402(4) . ? C31 C49 1.511(4) . ? C32 C33 1.398(4) . ? C32 C50 1.486(4) . ? C33 C34 1.392(4) . ? C34 H34 0.9600 . ? C35 H35C 0.9601 . ? C35 H35A 0.9600 . ? C35 H35B 0.9599 . ? C36 H36C 0.9599 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C37 H37A 0.9601 . ? C37 H37B 0.9600 . ? C37 H37C 0.9599 . ? C38 H38A 0.9599 . ? C38 H38B 0.9599 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9599 . ? C39 H39C 0.9601 . ? C40 H40A 0.9599 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41C 0.9600 . ? C41 H41A 0.9601 . ? C41 H41B 0.9600 . ? C42 H42A 0.9599 . ? C42 H42B 0.9601 . ? C42 H42C 0.9601 . ? C43 H43C 0.9600 . ? C43 H43A 0.9599 . ? C43 H43B 0.9600 . ? C44 H44C 0.9599 . ? C44 H44A 0.9599 . ? C44 H44B 0.9601 . ? C45 H45C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9601 . ? C46 H46C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9599 . ? C48 H48A 0.9602 . ? C48 H48B 0.9601 . ? C48 H48C 0.9600 . ? C49 H49C 0.9600 . ? C49 H49A 0.9601 . ? C49 H49B 0.9599 . ? C50 H50C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? B1 F2 1.380(3) . ? B1 F1 1.402(3) . ? B2 F3 1.406(4) . ? B2 F4 1.414(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 C4 N1 C1 107.5(2) . . ? C4 N1 B1 128.9(2) . . ? C1 N1 B1 123.6(2) . . ? C5 N2 C8 110.1(2) . . ? C5 N2 H2N 124.5 . . ? C8 N2 H2N 125.4 . . ? C12 N3 C9 109.9(2) . . ? C12 N3 H3N 125.4 . . ? C9 N3 H3N 124.7 . . ? C13 N4 C16 107.3(2) . . ? C13 N4 B2 128.8(2) . . ? C16 N4 B2 123.1(2) . . ? C21 N5 C18 106.6(2) . . ? C21 N5 B2 129.5(2) . . ? C18 N5 B2 123.8(2) . . ? C25 N6 C22 111.0(2) . . ? C25 N6 H6N 124.3 . . ? C22 N6 H6N 124.6 . . ? C29 N7 C26 109.8(2) . . ? C29 N7 H7N 125.8 . . ? C26 N7 H7N 124.4 . . ? C30 N8 C33 106.6(2) . . ? C30 N8 B1 127.2(2) . . ? C33 N8 B1 125.2(2) . . ? C34 C1 N1 120.6(2) . . ? C34 C1 C2 130.8(2) . . ? N1 C1 C2 108.6(2) . . ? C3 C2 C1 107.0(2) . . ? C3 C2 C35 126.9(3) . . ? C1 C2 C35 126.0(3) . . ? C2 C3 C4 107.5(3) . . ? C2 C3 C36 125.4(3) . . ? C4 C3 C36 126.3(3) . . ? N1 C4 C3 109.4(2) . . ? N1 C4 C5 124.3(2) . . ? C3 C4 C5 126.3(3) . . ? N2 C5 C6 106.7(2) . . ? N2 C5 C4 122.3(3) . . ? C6 C5 C4 130.9(3) . . ? C5 C6 C7 108.2(3) . . ? C5 C6 C37 127.8(3) . . ? C7 C6 C37 123.9(3) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 C38 127.0(3) . . ? C6 C7 C38 125.7(3) . . ? N2 C8 C7 107.7(2) . . ? N2 C8 C9 119.4(3) . . ? C7 C8 C9 132.8(3) . . ? N3 C9 C10 107.4(2) . . ? N3 C9 C8 122.4(3) . . ? C10 C9 C8 130.2(3) . . ? C9 C10 C11 107.3(2) . . ? C9 C10 C39 126.4(3) . . ? C11 C10 C39 126.3(3) . . ? C12 C11 C10 107.9(3) . . ? C12 C11 C40 127.0(3) . . ? C10 C11 C40 124.8(3) . . ? N3 C12 C11 107.6(2) . . ? N3 C12 C13 124.2(2) . . ? C11 C12 C13 128.2(3) . . ? N4 C13 C14 110.0(2) . . ? N4 C13 C12 123.6(2) . . ? C14 C13 C12 126.4(3) . . ? C15 C14 C13 106.9(3) . . ? C15 C14 C41 126.2(3) . . ? C13 C14 C41 126.7(3) . . ? C14 C15 C16 107.9(2) . . ? C14 C15 C42 126.6(3) . . ? C16 C15 C42 125.5(3) . . ? C17 C16 N4 120.4(3) . . ? C17 C16 C15 131.7(3) . . ? N4 C16 C15 107.9(2) . . ? C16 C17 C18 123.2(3) . . ? C16 C17 H17 118.2 . . ? C18 C17 H17 118.6 . . ? C17 C18 N5 119.9(3) . . ? C17 C18 C19 131.0(3) . . ? N5 C18 C19 109.1(2) . . ? C20 C19 C18 107.9(2) . . ? C20 C19 C43 126.6(3) . . ? C18 C19 C43 125.5(3) . . ? N6 C22 C23 107.1(2) . . ? N6 C22 C21 120.8(2) . . ? C23 C22 C21 132.0(2) . . ? C19 C20 C21 107.4(3) . . ? C19 C20 C44 125.9(3) . . ? C21 C20 C44 126.4(3) . . ? N5 C21 C20 109.0(2) . . ? N5 C21 C22 123.1(2) . . ? C20 C21 C22 127.8(3) . . ? C22 C23 C24 107.9(2) . . ? C22 C23 C45 128.3(3) . . ? C24 C23 C45 123.7(3) . . ? C25 C24 C23 106.9(2) . . ? C25 C24 C46 126.9(3) . . ? C23 C24 C46 126.1(3) . . ? N6 C25 C24 107.0(2) . . ? N6 C25 C26 120.3(2) . . ? C24 C25 C26 132.7(2) . . ? C27 C26 N7 107.4(2) . . ? C27 C26 C25 130.4(2) . . ? N7 C26 C25 122.2(2) . . ? C26 C27 C28 107.7(2) . . ? C26 C27 C47 126.5(2) . . ? C28 C27 C47 125.8(3) . . ? C29 C28 C27 107.3(2) . . ? C29 C28 C48 126.5(2) . . ? C27 C28 C48 126.0(2) . . ? N7 C29 C28 107.9(2) . . ? N7 C29 C30 122.8(2) . . ? C28 C29 C30 129.3(2) . . ? N8 C30 C31 110.0(2) . . ? N8 C30 C29 122.7(2) . . ? C31 C30 C29 127.4(2) . . ? C30 C31 C32 107.5(2) . . ? C30 C31 C49 127.5(2) . . ? C32 C31 C49 124.8(2) . . ? C33 C32 C31 106.3(2) . . ? C33 C32 C50 127.3(2) . . ? C31 C32 C50 126.4(3) . . ? C34 C33 C32 131.1(2) . . ? C34 C33 N8 119.2(2) . . ? C32 C33 N8 109.6(2) . . ? C1 C34 C33 123.4(2) . . ? C1 C34 H34 118.1 . . ? C33 C34 H34 118.5 . . ? C2 C35 H35C 109.6 . . ? C2 C35 H35A 109.1 . . ? H35C C35 H35A 109.9 . . ? C2 C35 H35B 110.3 . . ? H35C C35 H35B 109.9 . . ? H35A C35 H35B 108.1 . . ? C3 C36 H36C 110.4 . . ? C3 C36 H36A 108.9 . . ? H36C C36 H36A 110.3 . . ? C3 C36 H36B 109.2 . . ? H36C C36 H36B 110.3 . . ? H36A C36 H36B 107.8 . . ? C6 C37 H37A 110.1 . . ? C6 C37 H37B 108.9 . . ? H37A C37 H37B 109.5 . . ? C6 C37 H37C 109.4 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C7 C38 H38A 110.2 . . ? C7 C38 H38B 109.6 . . ? H38A C38 H38B 109.5 . . ? C7 C38 H38C 108.6 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C10 C39 H39A 109.4 . . ? C10 C39 H39B 108.6 . . ? H39A C39 H39B 109.5 . . ? C10 C39 H39C 110.4 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C11 C40 H40A 109.9 . . ? C11 C40 H40B 109.0 . . ? H40A C40 H40B 109.5 . . ? C11 C40 H40C 109.4 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C14 C41 H41C 109.2 . . ? C14 C41 H41A 110.3 . . ? H41C C41 H41A 109.4 . . ? C14 C41 H41B 110.1 . . ? H41C C41 H41B 109.4 . . ? H41A C41 H41B 108.5 . . ? C15 C42 H42A 109.2 . . ? C15 C42 H42B 109.7 . . ? H42A C42 H42B 109.5 . . ? C15 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C19 C43 H43C 109.0 . . ? C19 C43 H43A 110.8 . . ? H43C C43 H43A 109.1 . . ? C19 C43 H43B 110.3 . . ? H43C C43 H43B 109.1 . . ? H43A C43 H43B 108.7 . . ? C20 C44 H44C 109.9 . . ? C20 C44 H44A 109.7 . . ? H44C C44 H44A 109.7 . . ? C20 C44 H44B 109.8 . . ? H44C C44 H44B 109.6 . . ? H44A C44 H44B 108.3 . . ? C23 C45 H45C 109.9 . . ? C23 C45 H45A 110.2 . . ? H45C C45 H45A 109.6 . . ? C23 C45 H45B 109.2 . . ? H45C C45 H45B 109.6 . . ? H45A C45 H45B 108.3 . . ? C24 C46 H46C 109.4 . . ? C24 C46 H46A 110.5 . . ? H46C C46 H46A 109.1 . . ? C24 C46 H46B 110.2 . . ? H46C C46 H46B 109.1 . . ? H46A C46 H46B 108.7 . . ? C27 C47 H47A 109.4 . . ? C27 C47 H47B 109.3 . . ? H47A C47 H47B 109.5 . . ? C27 C47 H47C 109.8 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C28 C48 H48A 109.8 . . ? C28 C48 H48B 109.6 . . ? H48A C48 H48B 109.5 . . ? C28 C48 H48C 109.0 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C31 C49 H49C 109.7 . . ? C31 C49 H49A 110.0 . . ? H49C C49 H49A 109.9 . . ? C31 C49 H49B 109.3 . . ? H49C C49 H49B 109.9 . . ? H49A C49 H49B 108.1 . . ? C32 C50 H50C 109.3 . . ? C32 C50 H50A 110.3 . . ? H50C C50 H50A 109.3 . . ? C32 C50 H50B 110.1 . . ? H50C C50 H50B 109.3 . . ? H50A C50 H50B 108.5 . . ? F2 B1 F1 109.6(2) . . ? F2 B1 N8 109.2(2) . . ? F1 B1 N8 110.5(2) . . ? F2 B1 N1 111.7(2) . . ? F1 B1 N1 107.9(2) . . ? N8 B1 N1 107.8(2) . . ? F3 B2 F4 108.4(2) . . ? F3 B2 N4 108.1(2) . . ? F4 B2 N4 110.6(3) . . ? F3 B2 N5 111.4(3) . . ? F4 B2 N5 109.0(2) . . ? N4 B2 N5 109.3(2) . . ? 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 C34 -179.5(2) . . . . ? B1 N1 C1 C34 2.6(4) . . . . ? C4 N1 C1 C2 -1.6(3) . . . . ? B1 N1 C1 C2 -179.4(2) . . . . ? C34 C1 C2 C3 179.6(3) . . . . ? N1 C1 C2 C3 1.9(3) . . . . ? C34 C1 C2 C35 1.9(5) . . . . ? N1 C1 C2 C35 -175.8(3) . . . . ? C1 C2 C3 C4 -1.5(3) . . . . ? C35 C2 C3 C4 176.1(3) . . . . ? C1 C2 C3 C36 -171.6(3) . . . . ? C35 C2 C3 C36 6.1(5) . . . . ? C1 N1 C4 C3 0.6(3) . . . . ? B1 N1 C4 C3 178.3(3) . . . . ? C1 N1 C4 C5 177.6(3) . . . . ? B1 N1 C4 C5 -4.7(4) . . . . ? C2 C3 C4 N1 0.6(3) . . . . ? C36 C3 C4 N1 170.6(3) . . . . ? C2 C3 C4 C5 -176.3(3) . . . . ? C36 C3 C4 C5 -6.4(5) . . . . ? C8 N2 C5 C6 1.5(3) . . . . ? C8 N2 C5 C4 -176.1(2) . . . . ? N1 C4 C5 N2 -42.2(4) . . . . ? C3 C4 C5 N2 134.3(3) . . . . ? N1 C4 C5 C6 140.8(3) . . . . ? C3 C4 C5 C6 -42.7(5) . . . . ? N2 C5 C6 C7 -1.2(3) . . . . ? C4 C5 C6 C7 176.1(3) . . . . ? N2 C5 C6 C37 175.4(3) . . . . ? C4 C5 C6 C37 -7.3(5) . . . . ? C5 C6 C7 C8 0.5(3) . . . . ? C37 C6 C7 C8 -176.3(3) . . . . ? C5 C6 C7 C38 -177.8(3) . . . . ? C37 C6 C7 C38 5.4(5) . . . . ? C5 N2 C8 C7 -1.1(3) . . . . ? C5 N2 C8 C9 178.9(2) . . . . ? C6 C7 C8 N2 0.3(3) . . . . ? C38 C7 C8 N2 178.6(3) . . . . ? C6 C7 C8 C9 -179.7(3) . . . . ? C38 C7 C8 C9 -1.4(5) . . . . ? C12 N3 C9 C10 -0.5(3) . . . . ? C12 N3 C9 C8 179.8(3) . . . . ? N2 C8 C9 N3 122.4(3) . . . . ? C7 C8 C9 N3 -57.6(5) . . . . ? N2 C8 C9 C10 -57.3(4) . . . . ? C7 C8 C9 C10 122.7(4) . . . . ? N3 C9 C10 C11 0.5(3) . . . . ? C8 C9 C10 C11 -179.7(3) . . . . ? N3 C9 C10 C39 178.0(3) . . . . ? C8 C9 C10 C39 -2.3(5) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C39 C10 C11 C12 -177.8(3) . . . . ? C9 C10 C11 C40 -174.1(3) . . . . ? C39 C10 C11 C40 8.5(5) . . . . ? C9 N3 C12 C11 0.2(3) . . . . ? C9 N3 C12 C13 -178.9(3) . . . . ? C10 C11 C12 N3 0.1(4) . . . . ? C40 C11 C12 N3 173.7(3) . . . . ? C10 C11 C12 C13 179.2(3) . . . . ? C40 C11 C12 C13 -7.3(6) . . . . ? C16 N4 C13 C14 1.6(3) . . . . ? B2 N4 C13 C14 171.3(3) . . . . ? C16 N4 C13 C12 -179.0(3) . . . . ? B2 N4 C13 C12 -9.3(5) . . . . ? N3 C12 C13 N4 -45.2(4) . . . . ? C11 C12 C13 N4 135.8(3) . . . . ? N3 C12 C13 C14 134.1(3) . . . . ? C11 C12 C13 C14 -44.9(5) . . . . ? N4 C13 C14 C15 -1.3(3) . . . . ? C12 C13 C14 C15 179.3(3) . . . . ? N4 C13 C14 C41 173.7(3) . . . . ? C12 C13 C14 C41 -5.7(5) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C41 C14 C15 C16 -174.6(3) . . . . ? C13 C14 C15 C42 180.0(3) . . . . ? C41 C14 C15 C42 4.9(5) . . . . ? C13 N4 C16 C17 177.4(3) . . . . ? B2 N4 C16 C17 7.0(4) . . . . ? C13 N4 C16 C15 -1.3(3) . . . . ? B2 N4 C16 C15 -171.8(3) . . . . ? C14 C15 C16 C17 -178.0(3) . . . . ? C42 C15 C16 C17 2.4(5) . . . . ? C14 C15 C16 N4 0.6(3) . . . . ? C42 C15 C16 N4 -179.0(3) . . . . ? N4 C16 C17 C18 -4.1(5) . . . . ? C15 C16 C17 C18 174.4(3) . . . . ? C16 C17 C18 N5 -0.8(5) . . . . ? C16 C17 C18 C19 -179.7(3) . . . . ? C21 N5 C18 C17 180.0(3) . . . . ? B2 N5 C18 C17 2.8(4) . . . . ? C21 N5 C18 C19 -0.9(3) . . . . ? B2 N5 C18 C19 -178.1(3) . . . . ? C17 C18 C19 C20 179.9(3) . . . . ? N5 C18 C19 C20 0.9(3) . . . . ? C17 C18 C19 C43 1.9(5) . . . . ? N5 C18 C19 C43 -177.1(3) . . . . ? C25 N6 C22 C23 -0.7(3) . . . . ? C25 N6 C22 C21 -178.4(3) . . . . ? C18 C19 C20 C21 -0.6(3) . . . . ? C43 C19 C20 C21 177.4(3) . . . . ? C18 C19 C20 C44 -174.4(3) . . . . ? C43 C19 C20 C44 3.5(5) . . . . ? C18 N5 C21 C20 0.5(3) . . . . ? B2 N5 C21 C20 177.5(3) . . . . ? C18 N5 C21 C22 176.4(3) . . . . ? B2 N5 C21 C22 -6.6(5) . . . . ? C19 C20 C21 N5 0.0(3) . . . . ? C44 C20 C21 N5 173.8(3) . . . . ? C19 C20 C21 C22 -175.6(3) . . . . ? C44 C20 C21 C22 -1.8(5) . . . . ? N6 C22 C21 N5 -43.9(4) . . . . ? C23 C22 C21 N5 139.1(3) . . . . ? N6 C22 C21 C20 131.2(3) . . . . ? C23 C22 C21 C20 -45.8(5) . . . . ? N6 C22 C23 C24 0.6(3) . . . . ? C21 C22 C23 C24 177.9(3) . . . . ? N6 C22 C23 C45 175.6(3) . . . . ? C21 C22 C23 C45 -7.1(6) . . . . ? C22 C23 C24 C25 -0.3(3) . . . . ? C45 C23 C24 C25 -175.6(3) . . . . ? C22 C23 C24 C46 -176.9(3) . . . . ? C45 C23 C24 C46 7.7(5) . . . . ? C22 N6 C25 C24 0.6(3) . . . . ? C22 N6 C25 C26 178.6(2) . . . . ? C23 C24 C25 N6 -0.2(3) . . . . ? C46 C24 C25 N6 176.5(3) . . . . ? C23 C24 C25 C26 -177.8(3) . . . . ? C46 C24 C25 C26 -1.2(5) . . . . ? C29 N7 C26 C27 0.6(3) . . . . ? C29 N7 C26 C25 -178.3(2) . . . . ? N6 C25 C26 C27 -45.2(4) . . . . ? C24 C25 C26 C27 132.2(3) . . . . ? N6 C25 C26 N7 133.4(3) . . . . ? C24 C25 C26 N7 -49.2(4) . . . . ? N7 C26 C27 C28 -0.7(3) . . . . ? C25 C26 C27 C28 178.1(3) . . . . ? N7 C26 C27 C47 176.1(3) . . . . ? C25 C26 C27 C47 -5.1(5) . . . . ? C26 C27 C28 C29 0.5(3) . . . . ? C47 C27 C28 C29 -176.4(3) . . . . ? C26 C27 C28 C48 -174.5(3) . . . . ? C47 C27 C28 C48 8.7(5) . . . . ? C26 N7 C29 C28 -0.3(3) . . . . ? C26 N7 C29 C30 179.0(2) . . . . ? C27 C28 C29 N7 -0.1(3) . . . . ? C48 C28 C29 N7 174.8(3) . . . . ? C27 C28 C29 C30 -179.4(3) . . . . ? C48 C28 C29 C30 -4.5(5) . . . . ? C33 N8 C30 C31 0.9(3) . . . . ? B1 N8 C30 C31 169.9(2) . . . . ? C33 N8 C30 C29 179.3(2) . . . . ? B1 N8 C30 C29 -11.7(4) . . . . ? N7 C29 C30 N8 -48.8(4) . . . . ? C28 C29 C30 N8 130.4(3) . . . . ? N7 C29 C30 C31 129.3(3) . . . . ? C28 C29 C30 C31 -51.5(4) . . . . ? N8 C30 C31 C32 -0.6(3) . . . . ? C29 C30 C31 C32 -178.9(2) . . . . ? N8 C30 C31 C49 174.4(3) . . . . ? C29 C30 C31 C49 -3.9(5) . . . . ? C30 C31 C32 C33 0.1(3) . . . . ? C49 C31 C32 C33 -175.1(2) . . . . ? C30 C31 C32 C50 179.4(2) . . . . ? C49 C31 C32 C50 4.3(4) . . . . ? C31 C32 C33 C34 -176.0(3) . . . . ? C50 C32 C33 C34 4.6(5) . . . . ? C31 C32 C33 N8 0.5(3) . . . . ? C50 C32 C33 N8 -178.9(2) . . . . ? C30 N8 C33 C34 176.2(2) . . . . ? B1 N8 C33 C34 6.9(4) . . . . ? C30 N8 C33 C32 -0.8(3) . . . . ? B1 N8 C33 C32 -170.1(2) . . . . ? N1 C1 C34 C33 -0.1(4) . . . . ? C2 C1 C34 C33 -177.5(3) . . . . ? C32 C33 C34 C1 171.7(3) . . . . ? N8 C33 C34 C1 -4.5(4) . . . . ? C30 N8 B1 F2 -49.7(3) . . . . ? C33 N8 B1 F2 117.4(3) . . . . ? C30 N8 B1 F1 71.0(3) . . . . ? C33 N8 B1 F1 -121.9(2) . . . . ? C30 N8 B1 N1 -171.3(2) . . . . ? C33 N8 B1 N1 -4.2(3) . . . . ? C4 N1 B1 F2 62.0(4) . . . . ? C1 N1 B1 F2 -120.6(3) . . . . ? C4 N1 B1 F1 -58.6(3) . . . . ? C1 N1 B1 F1 118.8(3) . . . . ? C4 N1 B1 N8 -178.0(2) . . . . ? C1 N1 B1 N8 -0.6(3) . . . . ? C13 N4 B2 F3 -51.5(4) . . . . ? C16 N4 B2 F3 116.7(3) . . . . ? C13 N4 B2 F4 67.0(4) . . . . ? C16 N4 B2 F4 -124.7(3) . . . . ? C13 N4 B2 N5 -173.0(3) . . . . ? C16 N4 B2 N5 -4.7(4) . . . . ? C21 N5 B2 F3 63.9(4) . . . . ? C18 N5 B2 F3 -119.5(3) . . . . ? C21 N5 B2 F4 -55.7(4) . . . . ? C18 N5 B2 F4 120.9(3) . . . . ? C21 N5 B2 N4 -176.6(3) . . . . ? C18 N5 B2 N4 -0.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N F2 0.90 2.03 2.728(3) 133.3 . N3 H3N F4 0.90 2.21 2.819(3) 124.3 . N6 H6N F3 0.90 2.08 2.731(3) 128.7 . N7 H7N F1 0.90 2.29 2.814(3) 117.0 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.344 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.077