# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email maedahir@ph.ritsumei.ac.jp _publ_contact_author_name 'Hiromitsu Maeda' loop_ _publ_author_name Y.Haketa M.Takayama H.Maeda data_90525 _database_code_depnum_ccdc_archive 'CCDC 845953' #TrackingRef '1-TATACl.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H50 B2 Cl3 F4 N7 O4' _chemical_formula_weight 1028.95 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P - 1' _symmetry_space_group_name_Hall '- P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.553(2) _cell_length_b 13.788(4) _cell_length_c 20.858(8) _cell_angle_alpha 88.838(14) _cell_angle_beta 86.545(14) _cell_angle_gamma 73.382(12) _cell_volume 2352.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.267 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8250 _exptl_absorpt_correction_T_max 0.9486 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22626 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10176 _reflns_number_gt 7205 _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^)+(0.0921P)^2^+2.3903P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10176 _refine_ls_number_parameters 653 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 C1 C 1.2609(4) 0.6288(3) 0.05205(17) 0.0457(8) Uani 1 1 d . . . H1 H 1.3222 0.5595 0.0504 0.055 Uiso 1 1 calc R . . C2 C 1.2764(4) 0.7020(3) 0.00922(16) 0.0444(8) Uani 1 1 d . . . H2 H 1.3507 0.6921 -0.0274 0.053 Uiso 1 1 calc R . . C3 C 1.1698(3) 0.7903(2) 0.02722(12) 0.0258(6) Uani 1 1 d . . . H3 H 1.1568 0.8531 0.0054 0.031 Uiso 1 1 calc R . . C4 C 1.0824(3) 0.7758(2) 0.08206(13) 0.0298(6) Uani 1 1 d . . . C5 C 0.9562(3) 0.8552(2) 0.11111(13) 0.0291(6) Uani 1 1 d . . . C6 C 0.8618(3) 0.8404(2) 0.16496(13) 0.0290(6) Uani 1 1 d . . . H4 H 0.8775 0.7745 0.1827 0.035 Uiso 1 1 calc R . . C7 C 0.7446(3) 0.9223(2) 0.19258(13) 0.0265(6) Uani 1 1 d . . . C8 C 0.6514(3) 0.9147(2) 0.25043(13) 0.0255(6) Uani 1 1 d . . . C9 C 0.5255(3) 0.9879(2) 0.28207(14) 0.0296(6) Uani 1 1 d . . . H5 H 0.4835 1.0566 0.2693 0.036 Uiso 1 1 calc R . . C10 C 0.4723(3) 0.9423(2) 0.33561(13) 0.0304(6) Uani 1 1 d . . . H6 H 0.3873 0.9739 0.3663 0.036 Uiso 1 1 calc R . . C11 C 0.5653(3) 0.8428(2) 0.33594(13) 0.0292(6) Uani 1 1 d . . . H7 H 0.5548 0.7936 0.3671 0.035 Uiso 1 1 calc R . . C12 C 0.3908(5) 0.3816(4) 0.16151(19) 0.0618(12) Uani 1 1 d . . . H8 H 0.3862 0.4217 0.1237 0.074 Uiso 1 1 calc R . . C13 C 0.5149(5) 0.2991(3) 0.17559(15) 0.0473(9) Uani 1 1 d . . . H9 H 0.6133 0.2729 0.1500 0.057 Uiso 1 1 calc R . . C14 C 0.4743(3) 0.2604(2) 0.23262(12) 0.0235(5) Uani 1 1 d . . . H10 H 0.5385 0.2016 0.2533 0.028 Uiso 1 1 calc R . . C15 C 0.3244(3) 0.3208(2) 0.25531(13) 0.0260(6) Uani 1 1 d . . . C16 C 0.2411(3) 0.3083(2) 0.31525(13) 0.0260(6) Uani 1 1 d . . . C17 C 0.1113(3) 0.3842(2) 0.34086(14) 0.0302(6) Uani 1 1 d . . . H11 H 0.0760 0.4471 0.3190 0.036 Uiso 1 1 calc R . . C18 C 0.0325(3) 0.3689(2) 0.39843(13) 0.0274(6) Uani 1 1 d . . . C19 C -0.1006(3) 0.4440(2) 0.42851(13) 0.0269(6) Uani 1 1 d . . . C20 C -0.1884(4) 0.4385(2) 0.48601(14) 0.0366(7) Uani 1 1 d . . . H12 H -0.1760 0.3806 0.5129 0.044 Uiso 1 1 calc R . . C21 C -0.2983(4) 0.5341(3) 0.49701(15) 0.0387(7) Uani 1 1 d . . . H13 H -0.3743 0.5533 0.5328 0.046 Uiso 1 1 calc R . . C22 C -0.2765(4) 0.5950(2) 0.44683(15) 0.0343(7) Uani 1 1 d . . . H14 H -0.3351 0.6643 0.4420 0.041 Uiso 1 1 calc R . . C23 C 1.3820(3) 0.9163(2) 0.12557(13) 0.0284(6) Uani 1 1 d . . . H15 H 1.4126 0.9532 0.0904 0.034 Uiso 1 1 calc R . . C24 C 1.4543(3) 0.8142(2) 0.13141(13) 0.0299(6) Uani 1 1 d . . . H16 H 1.5375 0.7821 0.1002 0.036 Uiso 1 1 calc R . . C25 C 1.4128(3) 0.7561(2) 0.18007(13) 0.0273(6) Uani 1 1 d . . . H17 H 1.4696 0.6862 0.1832 0.033 Uiso 1 1 calc R . . C26 C 1.2863(3) 0.8006(2) 0.22486(12) 0.0226(5) Uani 1 1 d . . . C27 C 1.1145(3) 0.7906(2) 0.32015(12) 0.0227(5) Uani 1 1 d . . . C28 C 1.0669(3) 0.7351(2) 0.37053(13) 0.0265(6) Uani 1 1 d . . . H18 H 1.1133 0.6639 0.3729 0.032 Uiso 1 1 calc R . . C29 C 0.9512(3) 0.7854(2) 0.41702(13) 0.0273(6) Uani 1 1 d . . . H19 H 0.9205 0.7470 0.4513 0.033 Uiso 1 1 calc R . . C30 C 0.8789(3) 0.8877(2) 0.41596(12) 0.0259(6) Uani 1 1 d . . . H20 H 0.8014 0.9190 0.4493 0.031 Uiso 1 1 calc R . . C31 C 0.9200(3) 0.9459(2) 0.36551(12) 0.0217(5) Uani 1 1 d . . . C32 C 0.8962(3) 1.1078(2) 0.31301(12) 0.0225(5) Uani 1 1 d . . . C33 C 0.8319(3) 1.2125(2) 0.31065(13) 0.0282(6) Uani 1 1 d . . . H21 H 0.7537 1.2468 0.3430 0.034 Uiso 1 1 calc R . . C34 C 0.8824(4) 1.2663(2) 0.26119(14) 0.0310(6) Uani 1 1 d . . . H22 H 0.8351 1.3375 0.2597 0.037 Uiso 1 1 calc R . . C35 C 0.9989(4) 1.2212(2) 0.21359(14) 0.0303(6) Uani 1 1 d . . . H23 H 1.0283 1.2605 0.1795 0.036 Uiso 1 1 calc R . . C36 C 1.0719(3) 1.1177(2) 0.21644(13) 0.0272(6) Uani 1 1 d . . . C37 C 1.2631(3) 0.9650(2) 0.17201(13) 0.0264(6) Uani 1 1 d . . . C38 C 1.2121(3) 0.9061(2) 0.22116(12) 0.0228(5) Uani 1 1 d . . . C39 C 1.0894(3) 0.9540(2) 0.26790(12) 0.0210(5) Uani 1 1 d . . . C40 C 1.0185(3) 1.0593(2) 0.26532(12) 0.0230(5) Uani 1 1 d . . . C41 C 1.0422(3) 0.8961(2) 0.31779(11) 0.0207(5) Uani 1 1 d . . . C42 C 0.7201(3) 1.0980(2) 0.40912(12) 0.0248(6) Uani 1 1 d . . . H24 H 0.6562 1.0508 0.4229 0.030 Uiso 1 1 calc R . . H25 H 0.6446 1.1584 0.3900 0.030 Uiso 1 1 calc R . . C43 C 0.7922(3) 1.1297(2) 0.46745(13) 0.0288(6) Uani 1 1 d . . . H26 H 0.8649 1.0690 0.4874 0.035 Uiso 1 1 calc R . . H27 H 0.8590 1.1751 0.4535 0.035 Uiso 1 1 calc R . . C44 C 0.6598(4) 1.1836(3) 0.51660(15) 0.0445(9) Uani 1 1 d . . . H28 H 0.5961 1.2481 0.4987 0.067 Uiso 1 1 calc R . . H29 H 0.7100 1.1965 0.5553 0.067 Uiso 1 1 calc R . . H30 H 0.5876 1.1412 0.5276 0.067 Uiso 1 1 calc R . . C45 C 1.3037(3) 0.6349(2) 0.27502(13) 0.0248(5) Uani 1 1 d . . . H31 H 1.3390 0.6097 0.2309 0.030 Uiso 1 1 calc R . . H32 H 1.2193 0.6030 0.2917 0.030 Uiso 1 1 calc R . . C46 C 1.4497(3) 0.6029(2) 0.31704(14) 0.0289(6) Uani 1 1 d . . . H33 H 1.5388 0.6291 0.2982 0.035 Uiso 1 1 calc R . . H34 H 1.4176 0.6328 0.3603 0.035 Uiso 1 1 calc R . . C47 C 1.5116(4) 0.4881(2) 0.32298(16) 0.0369(7) Uani 1 1 d . . . H35 H 1.4250 0.4624 0.3433 0.055 Uiso 1 1 calc R . . H36 H 1.6069 0.4697 0.3493 0.055 Uiso 1 1 calc R . . H37 H 1.5425 0.4583 0.2802 0.055 Uiso 1 1 calc R . . C48 C 1.2726(4) 1.1314(2) 0.12845(14) 0.0332(7) Uani 1 1 d . . . H38 H 1.3904 1.0964 0.1205 0.040 Uiso 1 1 calc R . . H39 H 1.2626 1.1972 0.1489 0.040 Uiso 1 1 calc R . . C49 C 1.1920(4) 1.1496(3) 0.06531(15) 0.0374(7) Uani 1 1 d . . . H40 H 1.0776 1.1922 0.0719 0.045 Uiso 1 1 calc R . . H41 H 1.1913 1.0844 0.0465 0.045 Uiso 1 1 calc R . . C50 C 1.2891(4) 1.2035(3) 0.01977(15) 0.0404(8) Uani 1 1 d . . . H42 H 1.2952 1.2657 0.0400 0.061 Uiso 1 1 calc R . . H43 H 1.2340 1.2204 -0.0205 0.061 Uiso 1 1 calc R . . H44 H 1.3997 1.1588 0.0109 0.061 Uiso 1 1 calc R . . C51 C -0.1556(5) 0.5406(3) 0.0932(2) 0.0570(10) Uani 1 1 d . . . H45 H -0.1575 0.5564 0.1394 0.068 Uiso 1 1 calc R A 1 H46 H -0.1215 0.5946 0.0693 0.068 Uiso 1 1 calc R A 1 N1 N 1.1975(3) 1.06896(19) 0.17313(11) 0.0307(5) Uani 1 1 d . . . N2 N 0.8482(3) 1.04842(17) 0.36029(10) 0.0227(5) Uani 1 1 d . . . N3 N 1.2312(3) 0.74480(17) 0.27265(10) 0.0233(5) Uani 1 1 d . . . N4 N 0.6735(3) 0.82648(18) 0.28495(11) 0.0267(5) Uani 1 1 d . . . H47 H 0.7465 0.7686 0.2753 0.032 Uiso 1 1 calc R . . N5 N 1.1398(4) 0.6736(3) 0.09839(15) 0.0516(8) Uani 1 1 d . . . H48 H 1.1058 0.6434 0.1317 0.062 Uiso 1 1 calc R . . N6 N 0.2713(4) 0.3976(2) 0.21156(16) 0.0503(8) Uani 1 1 d . . . H49 H 0.1797 0.4472 0.2147 0.060 Uiso 1 1 calc R . . N7 N -0.1581(3) 0.54075(18) 0.40501(12) 0.0291(5) Uani 1 1 d . . . H50 H -0.1235 0.5637 0.3688 0.035 Uiso 1 1 calc R . . O1 O 0.0775(3) 0.28246(17) 0.42848(10) 0.0424(6) Uani 1 1 d . . . O2 O 0.2972(3) 0.22263(17) 0.34490(10) 0.0454(6) Uani 1 1 d . . . O3 O 0.7138(2) 1.01272(16) 0.16642(10) 0.0336(5) Uani 1 1 d . . . O4 O 0.9319(3) 0.94458(17) 0.08417(10) 0.0376(5) Uani 1 1 d . . . B1 B 0.2234(4) 0.2000(3) 0.40712(16) 0.0319(7) Uani 1 1 d . . . B2 B 0.7839(4) 1.0283(3) 0.10202(17) 0.0327(7) Uani 1 1 d . . . F1 F 0.1751(3) 0.11480(16) 0.40145(13) 0.0618(7) Uani 1 1 d . . . F2 F 0.3352(2) 0.1869(2) 0.45230(9) 0.0615(7) Uani 1 1 d . . . F3 F 0.8240(3) 1.11683(15) 0.10060(11) 0.0518(6) Uani 1 1 d . . . F4 F 0.6692(2) 1.02997(17) 0.05724(9) 0.0504(5) Uani 1 1 d . . . Cl1 Cl 0.90015(9) 0.60091(6) 0.25426(3) 0.03294(18) Uani 1 1 d . . . Cl2 Cl -0.34760(18) 0.55337(14) 0.07629(9) 0.0593(7) Uani 0.603(3) 1 d P B 1 Cl3 Cl 0.00019(13) 0.42907(8) 0.07967(5) 0.0633(3) Uani 1 1 d . B . Cl4 Cl -0.3250(3) 0.4866(2) 0.12618(14) 0.0595(10) Uani 0.397(3) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.049(2) 0.0402(19) 0.0401(18) -0.0072(15) 0.0030(15) -0.0017(16) C2 0.0422(19) 0.053(2) 0.0304(16) -0.0032(15) 0.0040(14) -0.0030(16) C3 0.0228(13) 0.0326(15) 0.0172(12) 0.0044(10) 0.0029(10) -0.0013(11) C4 0.0281(14) 0.0381(16) 0.0223(13) 0.0023(11) -0.0019(10) -0.0082(12) C5 0.0242(14) 0.0365(16) 0.0260(14) 0.0065(12) -0.0038(10) -0.0076(12) C6 0.0291(15) 0.0330(15) 0.0243(14) 0.0017(11) 0.0010(11) -0.0085(12) C7 0.0258(14) 0.0298(15) 0.0249(13) 0.0043(11) -0.0020(10) -0.0095(11) C8 0.0253(13) 0.0302(15) 0.0225(13) 0.0010(11) -0.0021(10) -0.0102(11) C9 0.0304(15) 0.0270(14) 0.0319(15) -0.0004(11) -0.0008(11) -0.0091(12) C10 0.0304(15) 0.0356(16) 0.0253(14) -0.0055(12) 0.0034(11) -0.0105(12) C11 0.0342(15) 0.0333(15) 0.0208(13) -0.0005(11) 0.0040(11) -0.0117(12) C12 0.075(3) 0.084(3) 0.045(2) 0.035(2) -0.0194(19) -0.051(3) C13 0.049(2) 0.075(3) 0.0251(15) -0.0057(16) 0.0089(14) -0.0310(19) C14 0.0223(13) 0.0252(13) 0.0219(12) -0.0029(10) 0.0036(10) -0.0057(11) C15 0.0251(13) 0.0263(14) 0.0266(13) -0.0026(11) -0.0006(10) -0.0073(11) C16 0.0271(14) 0.0244(14) 0.0263(13) -0.0001(11) -0.0035(10) -0.0068(11) C17 0.0257(14) 0.0266(14) 0.0355(15) 0.0032(12) 0.0033(11) -0.0040(11) C18 0.0261(14) 0.0266(14) 0.0284(14) -0.0007(11) -0.0023(11) -0.0056(11) C19 0.0259(14) 0.0274(14) 0.0251(13) -0.0003(11) 0.0001(10) -0.0045(11) C20 0.0389(17) 0.0364(17) 0.0285(15) 0.0057(13) 0.0049(12) -0.0028(13) C21 0.0348(17) 0.0422(18) 0.0313(16) 0.0008(13) 0.0050(12) -0.0001(14) C22 0.0288(15) 0.0309(15) 0.0366(16) -0.0018(12) 0.0048(12) 0.0005(12) C23 0.0307(14) 0.0350(15) 0.0193(13) -0.0032(11) 0.0074(10) -0.0109(12) C24 0.0258(14) 0.0387(16) 0.0227(13) -0.0078(12) 0.0091(10) -0.0067(12) C25 0.0249(13) 0.0298(15) 0.0239(13) -0.0058(11) 0.0044(10) -0.0033(11) C26 0.0235(13) 0.0274(14) 0.0174(12) -0.0047(10) 0.0008(9) -0.0081(11) C27 0.0199(12) 0.0300(14) 0.0174(12) -0.0036(10) 0.0005(9) -0.0060(11) C28 0.0277(14) 0.0279(14) 0.0238(13) 0.0011(11) 0.0013(10) -0.0086(11) C29 0.0280(14) 0.0364(16) 0.0189(12) 0.0016(11) 0.0017(10) -0.0120(12) C30 0.0249(13) 0.0355(15) 0.0180(12) -0.0030(11) 0.0043(10) -0.0104(11) C31 0.0195(12) 0.0292(14) 0.0160(11) -0.0051(10) 0.0009(9) -0.0065(10) C32 0.0223(13) 0.0275(14) 0.0167(12) -0.0041(10) 0.0024(9) -0.0061(11) C33 0.0248(13) 0.0326(15) 0.0234(13) -0.0054(11) 0.0040(10) -0.0030(11) C34 0.0310(15) 0.0275(15) 0.0298(14) -0.0021(11) -0.0005(11) -0.0009(12) C35 0.0358(16) 0.0280(15) 0.0247(14) 0.0015(11) 0.0051(11) -0.0069(12) C36 0.0287(14) 0.0305(15) 0.0197(12) -0.0032(11) 0.0052(10) -0.0054(12) C37 0.0266(14) 0.0283(14) 0.0218(13) -0.0020(11) 0.0045(10) -0.0048(11) C38 0.0213(12) 0.0284(14) 0.0174(12) -0.0041(10) 0.0028(9) -0.0052(11) C39 0.0185(12) 0.0279(14) 0.0158(11) -0.0039(10) 0.0011(9) -0.0056(10) C40 0.0221(13) 0.0281(14) 0.0165(12) -0.0029(10) 0.0022(9) -0.0042(11) C41 0.0174(12) 0.0288(14) 0.0158(11) -0.0029(10) 0.0004(9) -0.0064(10) C42 0.0219(13) 0.0317(14) 0.0184(12) -0.0069(10) 0.0066(10) -0.0051(11) C43 0.0240(13) 0.0399(16) 0.0217(13) -0.0090(11) 0.0034(10) -0.0081(12) C44 0.0345(17) 0.071(2) 0.0289(16) -0.0246(16) 0.0096(13) -0.0167(16) C45 0.0262(13) 0.0234(13) 0.0251(13) -0.0034(10) 0.0014(10) -0.0080(11) C46 0.0275(14) 0.0279(14) 0.0307(14) -0.0057(11) -0.0006(11) -0.0067(11) C47 0.0360(17) 0.0277(16) 0.0454(18) -0.0020(13) -0.0083(13) -0.0051(13) C48 0.0351(16) 0.0359(16) 0.0300(15) -0.0028(12) 0.0036(12) -0.0133(13) C49 0.0353(16) 0.0437(18) 0.0327(16) -0.0047(13) 0.0005(12) -0.0110(14) C50 0.0411(18) 0.0470(19) 0.0299(16) 0.0075(14) 0.0071(13) -0.0096(15) C51 0.059(2) 0.058(2) 0.050(2) -0.0056(19) 0.0003(18) -0.010(2) N1 0.0376(14) 0.0295(13) 0.0212(11) 0.0002(9) 0.0103(10) -0.0059(11) N2 0.0211(11) 0.0286(12) 0.0164(10) -0.0046(9) 0.0044(8) -0.0047(9) N3 0.0223(11) 0.0259(12) 0.0210(11) -0.0035(9) 0.0040(8) -0.0063(9) N4 0.0341(13) 0.0265(12) 0.0204(11) -0.0024(9) 0.0031(9) -0.0108(10) N5 0.058(2) 0.0541(19) 0.0437(17) 0.0028(14) -0.0028(14) -0.0180(16) N6 0.0486(18) 0.0454(18) 0.059(2) 0.0117(15) -0.0132(14) -0.0152(14) N7 0.0266(12) 0.0277(12) 0.0299(12) 0.0022(10) 0.0040(9) -0.0038(10) O1 0.0521(14) 0.0326(12) 0.0286(11) 0.0056(9) 0.0132(10) 0.0066(10) O2 0.0535(14) 0.0359(12) 0.0293(11) 0.0057(9) 0.0121(10) 0.0120(11) O3 0.0338(11) 0.0304(11) 0.0335(11) 0.0085(9) 0.0065(8) -0.0065(9) O4 0.0308(11) 0.0392(12) 0.0369(12) 0.0146(10) 0.0089(9) -0.0040(9) B1 0.0296(17) 0.0321(17) 0.0274(16) 0.0005(13) 0.0038(13) 0.0006(14) B2 0.0277(17) 0.0329(18) 0.0325(17) 0.0134(14) 0.0043(13) -0.0026(14) F1 0.0444(12) 0.0458(12) 0.0940(18) -0.0263(12) 0.0279(11) -0.0157(10) F2 0.0285(10) 0.118(2) 0.0299(10) 0.0019(11) -0.0017(8) -0.0085(11) F3 0.0528(12) 0.0382(11) 0.0622(13) 0.0095(10) 0.0218(10) -0.0154(9) F4 0.0358(10) 0.0681(14) 0.0345(10) 0.0081(9) 0.0013(8) 0.0043(10) Cl1 0.0413(4) 0.0332(4) 0.0245(3) -0.0001(3) 0.0017(3) -0.0117(3) Cl2 0.0393(8) 0.0593(11) 0.0737(13) -0.0299(9) 0.0056(7) -0.0048(7) Cl3 0.0607(6) 0.0616(6) 0.0522(6) 0.0071(5) -0.0007(4) 0.0062(5) Cl4 0.0465(14) 0.0620(18) 0.074(2) -0.0256(14) 0.0112(12) -0.0221(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 C1 C2 1.364(5) . ? C1 N5 1.388(5) . ? C1 H1 0.9500 . ? C2 C3 1.341(4) . ? C2 H2 0.9500 . ? C3 C4 1.371(4) . ? C3 H3 0.9500 . ? C4 N5 1.395(4) . ? C4 C5 1.415(4) . ? C5 O4 1.311(4) . ? C5 C6 1.390(4) . ? C6 C7 1.387(4) . ? C6 H4 0.9500 . ? C7 O3 1.313(3) . ? C7 C8 1.424(4) . ? C8 N4 1.373(4) . ? C8 C9 1.391(4) . ? C9 C10 1.387(4) . ? C9 H5 0.9500 . ? C10 C11 1.375(4) . ? C10 H6 0.9500 . ? C11 N4 1.345(3) . ? C11 H7 0.9500 . ? C12 C13 1.357(6) . ? C12 N6 1.391(5) . ? C12 H8 0.9500 . ? C13 C14 1.361(4) . ? C13 H9 0.9500 . ? C14 C15 1.377(4) . ? C14 H10 0.9500 . ? C15 N6 1.377(4) . ? C15 C16 1.433(4) . ? C16 O2 1.300(3) . ? C16 C17 1.379(4) . ? C17 C18 1.383(4) . ? C17 H11 0.9500 . ? C18 O1 1.303(4) . ? C18 C19 1.424(4) . ? C19 N7 1.375(4) . ? C19 C20 1.388(4) . ? C20 C21 1.397(4) . ? C20 H12 0.9500 . ? C21 C22 1.366(4) . ? C21 H13 0.9500 . ? C22 N7 1.354(4) . ? C22 H14 0.9500 . ? C23 C24 1.372(4) . ? C23 C37 1.393(4) . ? C23 H15 0.9500 . ? C24 C25 1.373(4) . ? C24 H16 0.9500 . ? C25 C26 1.394(3) . ? C25 H17 0.9500 . ? C26 N3 1.388(3) . ? C26 C38 1.413(4) . ? C27 N3 1.387(3) . ? C27 C28 1.396(4) . ? C27 C41 1.410(4) . ? C28 C29 1.385(4) . ? C28 H18 0.9500 . ? C29 C30 1.369(4) . ? C29 H19 0.9500 . ? C30 C31 1.399(4) . ? C30 H20 0.9500 . ? C31 N2 1.376(3) . ? C31 C41 1.430(3) . ? C32 N2 1.386(3) . ? C32 C33 1.392(4) . ? C32 C40 1.426(3) . ? C33 C34 1.378(4) . ? C33 H21 0.9500 . ? C34 C35 1.384(4) . ? C34 H22 0.9500 . ? C35 C36 1.386(4) . ? C35 H23 0.9500 . ? C36 N1 1.385(3) . ? C36 C40 1.421(4) . ? C37 N1 1.383(4) . ? C37 C38 1.419(4) . ? C38 C39 1.412(3) . ? C39 C41 1.408(4) . ? C39 C40 1.405(4) . ? C42 N2 1.473(3) . ? C42 C43 1.523(4) . ? C42 H24 0.9900 . ? C42 H25 0.9900 . ? C43 C44 1.515(4) . ? C43 H26 0.9900 . ? C43 H27 0.9900 . ? C44 H28 0.9800 . ? C44 H29 0.9800 . ? C44 H30 0.9800 . ? C45 N3 1.465(3) . ? C45 C46 1.524(4) . ? C45 H31 0.9900 . ? C45 H32 0.9900 . ? C46 C47 1.524(4) . ? C46 H33 0.9900 . ? C46 H34 0.9900 . ? C47 H35 0.9800 . ? C47 H36 0.9800 . ? C47 H37 0.9800 . ? C48 N1 1.494(4) . ? C48 C49 1.506(4) . ? C48 H38 0.9900 . ? C48 H39 0.9900 . ? C49 C50 1.540(4) . ? C49 H40 0.9900 . ? C49 H41 0.9900 . ? C50 H42 0.9800 . ? C50 H43 0.9800 . ? C50 H44 0.9800 . ? C51 Cl2 1.660(5) . ? C51 Cl3 1.738(4) . ? C51 Cl4 1.898(5) . ? C51 H45 0.9900 . ? C51 H46 0.9900 . ? N4 H47 0.8800 . ? N5 H48 0.8800 . ? N6 H49 0.8800 . ? N7 H50 0.8800 . ? O1 B1 1.480(4) . ? O2 B1 1.475(4) . ? O3 B2 1.475(4) . ? O4 B2 1.482(4) . ? B1 F2 1.355(4) . ? B1 F1 1.362(4) . ? B2 F3 1.359(4) . ? B2 F4 1.390(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 C2 C1 N5 107.9(3) . . ? C2 C1 H1 126.1 . . ? N5 C1 H1 126.1 . . ? C3 C2 C1 108.9(3) . . ? C3 C2 H2 125.5 . . ? C1 C2 H2 125.5 . . ? C2 C3 C4 109.2(3) . . ? C2 C3 H3 125.4 . . ? C4 C3 H3 125.4 . . ? C3 C4 N5 107.1(3) . . ? C3 C4 C5 122.0(3) . . ? N5 C4 C5 130.9(3) . . ? O4 C5 C6 121.2(3) . . ? O4 C5 C4 116.2(2) . . ? C6 C5 C4 122.5(3) . . ? C5 C6 C7 119.6(3) . . ? C5 C6 H4 120.2 . . ? C7 C6 H4 120.2 . . ? O3 C7 C6 121.2(2) . . ? O3 C7 C8 115.9(2) . . ? C6 C7 C8 122.9(3) . . ? N4 C8 C9 107.3(2) . . ? N4 C8 C7 123.0(2) . . ? C9 C8 C7 129.7(3) . . ? C10 C9 C8 107.5(3) . . ? C10 C9 H5 126.3 . . ? C8 C9 H5 126.3 . . ? C11 C10 C9 107.3(2) . . ? C11 C10 H6 126.4 . . ? C9 C10 H6 126.4 . . ? N4 C11 C10 109.0(3) . . ? N4 C11 H7 125.5 . . ? C10 C11 H7 125.5 . . ? C13 C12 N6 108.7(3) . . ? C13 C12 H8 125.7 . . ? N6 C12 H8 125.7 . . ? C14 C13 C12 108.3(3) . . ? C14 C13 H9 125.9 . . ? C12 C13 H9 125.9 . . ? C13 C14 C15 108.3(3) . . ? C13 C14 H10 125.8 . . ? C15 C14 H10 125.8 . . ? C14 C15 N6 108.1(3) . . ? C14 C15 C16 125.9(3) . . ? N6 C15 C16 126.0(3) . . ? O2 C16 C17 121.8(3) . . ? O2 C16 C15 116.5(2) . . ? C17 C16 C15 121.7(3) . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H11 120.0 . . ? C18 C17 H11 120.0 . . ? O1 C18 C17 120.7(3) . . ? O1 C18 C19 115.8(2) . . ? C17 C18 C19 123.5(3) . . ? N7 C19 C20 107.5(2) . . ? N7 C19 C18 123.3(2) . . ? C20 C19 C18 129.1(3) . . ? C19 C20 C21 107.2(3) . . ? C19 C20 H12 126.4 . . ? C21 C20 H12 126.4 . . ? C22 C21 C20 107.5(3) . . ? C22 C21 H13 126.2 . . ? C20 C21 H13 126.2 . . ? N7 C22 C21 109.0(3) . . ? N7 C22 H14 125.5 . . ? C21 C22 H14 125.5 . . ? C24 C23 C37 118.9(3) . . ? C24 C23 H15 120.5 . . ? C37 C23 H15 120.5 . . ? C25 C24 C23 123.4(2) . . ? C25 C24 H16 118.3 . . ? C23 C24 H16 118.3 . . ? C24 C25 C26 119.3(3) . . ? C24 C25 H17 120.3 . . ? C26 C25 H17 120.3 . . ? N3 C26 C25 122.1(2) . . ? N3 C26 C38 119.3(2) . . ? C25 C26 C38 118.6(2) . . ? N3 C27 C28 121.8(3) . . ? N3 C27 C41 119.2(2) . . ? C28 C27 C41 119.0(2) . . ? C29 C28 C27 119.1(3) . . ? C29 C28 H18 120.4 . . ? C27 C28 H18 120.4 . . ? C30 C29 C28 123.2(3) . . ? C30 C29 H19 118.4 . . ? C28 C29 H19 118.4 . . ? C29 C30 C31 119.6(2) . . ? C29 C30 H20 120.2 . . ? C31 C30 H20 120.2 . . ? N2 C31 C30 122.7(2) . . ? N2 C31 C41 119.1(2) . . ? C30 C31 C41 118.2(2) . . ? N2 C32 C33 122.9(2) . . ? N2 C32 C40 118.4(2) . . ? C33 C32 C40 118.7(2) . . ? C34 C33 C32 119.6(2) . . ? C34 C33 H21 120.2 . . ? C32 C33 H21 120.2 . . ? C33 C34 C35 123.0(3) . . ? C33 C34 H22 118.5 . . ? C35 C34 H22 118.5 . . ? C36 C35 C34 118.9(3) . . ? C36 C35 H23 120.6 . . ? C34 C35 H23 120.6 . . ? C35 C36 N1 121.9(3) . . ? C35 C36 C40 119.7(2) . . ? N1 C36 C40 118.5(2) . . ? N1 C37 C23 122.1(3) . . ? N1 C37 C38 118.9(2) . . ? C23 C37 C38 118.9(3) . . ? C26 C38 C39 119.7(2) . . ? C26 C38 C37 120.7(2) . . ? C39 C38 C37 119.6(2) . . ? C41 C39 C40 120.5(2) . . ? C41 C39 C38 119.6(2) . . ? C40 C39 C38 119.8(2) . . ? C39 C40 C36 120.2(2) . . ? C39 C40 C32 119.8(2) . . ? C36 C40 C32 120.0(2) . . ? C39 C41 C27 120.1(2) . . ? C39 C41 C31 119.0(2) . . ? C27 C41 C31 120.9(2) . . ? N2 C42 C43 111.7(2) . . ? N2 C42 H24 109.3 . . ? C43 C42 H24 109.3 . . ? N2 C42 H25 109.3 . . ? C43 C42 H25 109.3 . . ? H24 C42 H25 107.9 . . ? C44 C43 C42 111.5(2) . . ? C44 C43 H26 109.3 . . ? C42 C43 H26 109.3 . . ? C44 C43 H27 109.3 . . ? C42 C43 H27 109.3 . . ? H26 C43 H27 108.0 . . ? C43 C44 H28 109.5 . . ? C43 C44 H29 109.5 . . ? H28 C44 H29 109.5 . . ? C43 C44 H30 109.5 . . ? H28 C44 H30 109.5 . . ? H29 C44 H30 109.5 . . ? N3 C45 C46 113.1(2) . . ? N3 C45 H31 109.0 . . ? C46 C45 H31 109.0 . . ? N3 C45 H32 109.0 . . ? C46 C45 H32 109.0 . . ? H31 C45 H32 107.8 . . ? C47 C46 C45 111.3(2) . . ? C47 C46 H33 109.4 . . ? C45 C46 H33 109.4 . . ? C47 C46 H34 109.4 . . ? C45 C46 H34 109.4 . . ? H33 C46 H34 108.0 . . ? C46 C47 H35 109.5 . . ? C46 C47 H36 109.5 . . ? H35 C47 H36 109.5 . . ? C46 C47 H37 109.5 . . ? H35 C47 H37 109.5 . . ? H36 C47 H37 109.5 . . ? N1 C48 C49 111.9(3) . . ? N1 C48 H38 109.2 . . ? C49 C48 H38 109.2 . . ? N1 C48 H39 109.2 . . ? C49 C48 H39 109.2 . . ? H38 C48 H39 107.9 . . ? C48 C49 C50 108.3(3) . . ? C48 C49 H40 110.0 . . ? C50 C49 H40 110.0 . . ? C48 C49 H41 110.0 . . ? C50 C49 H41 110.0 . . ? H40 C49 H41 108.4 . . ? C49 C50 H42 109.5 . . ? C49 C50 H43 109.5 . . ? H42 C50 H43 109.5 . . ? C49 C50 H44 109.5 . . ? H42 C50 H44 109.5 . . ? H43 C50 H44 109.5 . . ? Cl2 C51 Cl3 122.7(3) . . ? Cl2 C51 Cl4 44.34(16) . . ? Cl3 C51 Cl4 99.8(2) . . ? Cl2 C51 H45 106.6 . . ? Cl3 C51 H45 106.6 . . ? Cl4 C51 H45 79.5 . . ? Cl2 C51 H46 106.6 . . ? Cl3 C51 H46 106.6 . . ? Cl4 C51 H46 149.4 . . ? H45 C51 H46 106.6 . . ? C37 N1 C36 122.7(2) . . ? C37 N1 C48 118.4(2) . . ? C36 N1 C48 118.8(2) . . ? C31 N2 C32 123.0(2) . . ? C31 N2 C42 118.4(2) . . ? C32 N2 C42 118.6(2) . . ? C26 N3 C27 121.8(2) . . ? C26 N3 C45 119.3(2) . . ? C27 N3 C45 118.8(2) . . ? C11 N4 C8 109.0(2) . . ? C11 N4 H47 125.5 . . ? C8 N4 H47 125.5 . . ? C1 N5 C4 106.9(3) . . ? C1 N5 H48 126.6 . . ? C4 N5 H48 126.6 . . ? C15 N6 C12 106.6(3) . . ? C15 N6 H49 126.7 . . ? C12 N6 H49 126.7 . . ? C22 N7 C19 108.7(2) . . ? C22 N7 H50 125.6 . . ? C19 N7 H50 125.6 . . ? C18 O1 B1 122.6(2) . . ? C16 O2 B1 122.1(2) . . ? C7 O3 B2 121.3(2) . . ? C5 O4 B2 120.8(2) . . ? F2 B1 F1 110.5(3) . . ? F2 B1 O2 109.0(3) . . ? F1 B1 O2 109.3(3) . . ? F2 B1 O1 108.3(3) . . ? F1 B1 O1 107.4(3) . . ? O2 B1 O1 112.3(2) . . ? F3 B2 F4 110.5(3) . . ? F3 B2 O3 109.7(3) . . ? F4 B2 O3 108.7(2) . . ? F3 B2 O4 109.0(2) . . ? F4 B2 O4 107.4(3) . . ? O3 B2 O4 111.6(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 N5 C1 C2 C3 0.0(4) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 N5 0.5(4) . . . . ? C2 C3 C4 C5 -177.7(3) . . . . ? C3 C4 C5 O4 -2.7(4) . . . . ? N5 C4 C5 O4 179.6(3) . . . . ? C3 C4 C5 C6 177.0(3) . . . . ? N5 C4 C5 C6 -0.7(5) . . . . ? O4 C5 C6 C7 -3.0(4) . . . . ? C4 C5 C6 C7 177.4(3) . . . . ? C5 C6 C7 O3 4.4(4) . . . . ? C5 C6 C7 C8 -175.2(3) . . . . ? O3 C7 C8 N4 -177.4(2) . . . . ? C6 C7 C8 N4 2.3(4) . . . . ? O3 C7 C8 C9 3.8(4) . . . . ? C6 C7 C8 C9 -176.5(3) . . . . ? N4 C8 C9 C10 -0.2(3) . . . . ? C7 C8 C9 C10 178.7(3) . . . . ? C8 C9 C10 C11 -0.1(3) . . . . ? C9 C10 C11 N4 0.4(3) . . . . ? N6 C12 C13 C14 2.0(4) . . . . ? C12 C13 C14 C15 -1.4(4) . . . . ? C13 C14 C15 N6 0.3(4) . . . . ? C13 C14 C15 C16 -177.4(3) . . . . ? C14 C15 C16 O2 -13.5(4) . . . . ? N6 C15 C16 O2 169.2(3) . . . . ? C14 C15 C16 C17 164.8(3) . . . . ? N6 C15 C16 C17 -12.5(5) . . . . ? O2 C16 C17 C18 -2.7(5) . . . . ? C15 C16 C17 C18 179.2(3) . . . . ? C16 C17 C18 O1 -1.3(5) . . . . ? C16 C17 C18 C19 179.0(3) . . . . ? O1 C18 C19 N7 176.6(3) . . . . ? C17 C18 C19 N7 -3.6(5) . . . . ? O1 C18 C19 C20 1.0(5) . . . . ? C17 C18 C19 C20 -179.3(3) . . . . ? N7 C19 C20 C21 -0.7(4) . . . . ? C18 C19 C20 C21 175.5(3) . . . . ? C19 C20 C21 C22 0.2(4) . . . . ? C20 C21 C22 N7 0.3(4) . . . . ? C37 C23 C24 C25 1.8(5) . . . . ? C23 C24 C25 C26 2.8(5) . . . . ? C24 C25 C26 N3 175.7(3) . . . . ? C24 C25 C26 C38 -4.2(4) . . . . ? N3 C27 C28 C29 179.1(2) . . . . ? C41 C27 C28 C29 -0.5(4) . . . . ? C27 C28 C29 C30 0.6(4) . . . . ? C28 C29 C30 C31 1.0(4) . . . . ? C29 C30 C31 N2 177.7(2) . . . . ? C29 C30 C31 C41 -2.4(4) . . . . ? N2 C32 C33 C34 -178.3(3) . . . . ? C40 C32 C33 C34 2.7(4) . . . . ? C32 C33 C34 C35 -1.7(5) . . . . ? C33 C34 C35 C36 -1.8(5) . . . . ? C34 C35 C36 N1 -175.2(3) . . . . ? C34 C35 C36 C40 4.2(4) . . . . ? C24 C23 C37 N1 173.0(3) . . . . ? C24 C23 C37 C38 -4.6(4) . . . . ? N3 C26 C38 C39 3.2(4) . . . . ? C25 C26 C38 C39 -176.8(2) . . . . ? N3 C26 C38 C37 -178.6(2) . . . . ? C25 C26 C38 C37 1.4(4) . . . . ? N1 C37 C38 C26 -174.6(3) . . . . ? C23 C37 C38 C26 3.1(4) . . . . ? N1 C37 C38 C39 3.6(4) . . . . ? C23 C37 C38 C39 -178.8(3) . . . . ? C26 C38 C39 C41 0.1(4) . . . . ? C37 C38 C39 C41 -178.1(2) . . . . ? C26 C38 C39 C40 178.3(2) . . . . ? C37 C38 C39 C40 0.1(4) . . . . ? C41 C39 C40 C36 177.2(2) . . . . ? C38 C39 C40 C36 -1.0(4) . . . . ? C41 C39 C40 C32 -1.0(4) . . . . ? C38 C39 C40 C32 -179.2(2) . . . . ? C35 C36 C40 C39 178.7(3) . . . . ? N1 C36 C40 C39 -1.9(4) . . . . ? C35 C36 C40 C32 -3.1(4) . . . . ? N1 C36 C40 C32 176.3(3) . . . . ? N2 C32 C40 C39 -1.2(4) . . . . ? C33 C32 C40 C39 177.8(2) . . . . ? N2 C32 C40 C36 -179.4(2) . . . . ? C33 C32 C40 C36 -0.4(4) . . . . ? C40 C39 C41 C27 -179.7(2) . . . . ? C38 C39 C41 C27 -1.5(4) . . . . ? C40 C39 C41 C31 0.6(4) . . . . ? C38 C39 C41 C31 178.8(2) . . . . ? N3 C27 C41 C39 -0.4(4) . . . . ? C28 C27 C41 C39 179.3(2) . . . . ? N3 C27 C41 C31 179.3(2) . . . . ? C28 C27 C41 C31 -1.0(4) . . . . ? N2 C31 C41 C39 2.0(4) . . . . ? C30 C31 C41 C39 -177.8(2) . . . . ? N2 C31 C41 C27 -177.7(2) . . . . ? C30 C31 C41 C27 2.5(4) . . . . ? N2 C42 C43 C44 178.2(3) . . . . ? N3 C45 C46 C47 174.9(2) . . . . ? N1 C48 C49 C50 -173.6(3) . . . . ? C23 C37 N1 C36 175.7(3) . . . . ? C38 C37 N1 C36 -6.7(4) . . . . ? C23 C37 N1 C48 -8.2(4) . . . . ? C38 C37 N1 C48 169.4(3) . . . . ? C35 C36 N1 C37 -174.8(3) . . . . ? C40 C36 N1 C37 5.8(4) . . . . ? C35 C36 N1 C48 9.2(4) . . . . ? C40 C36 N1 C48 -170.2(2) . . . . ? C49 C48 N1 C37 91.0(3) . . . . ? C49 C48 N1 C36 -92.8(3) . . . . ? C30 C31 N2 C32 175.4(2) . . . . ? C41 C31 N2 C32 -4.4(4) . . . . ? C30 C31 N2 C42 -1.5(4) . . . . ? C41 C31 N2 C42 178.7(2) . . . . ? C33 C32 N2 C31 -175.0(3) . . . . ? C40 C32 N2 C31 4.0(4) . . . . ? C33 C32 N2 C42 1.9(4) . . . . ? C40 C32 N2 C42 -179.1(2) . . . . ? C43 C42 N2 C31 86.5(3) . . . . ? C43 C42 N2 C32 -90.5(3) . . . . ? C25 C26 N3 C27 174.7(2) . . . . ? C38 C26 N3 C27 -5.3(4) . . . . ? C25 C26 N3 C45 -2.3(4) . . . . ? C38 C26 N3 C45 177.7(2) . . . . ? C28 C27 N3 C26 -175.8(2) . . . . ? C41 C27 N3 C26 3.9(4) . . . . ? C28 C27 N3 C45 1.3(4) . . . . ? C41 C27 N3 C45 -179.1(2) . . . . ? C46 C45 N3 C26 91.0(3) . . . . ? C46 C45 N3 C27 -86.1(3) . . . . ? C10 C11 N4 C8 -0.6(3) . . . . ? C9 C8 N4 C11 0.5(3) . . . . ? C7 C8 N4 C11 -178.5(3) . . . . ? C2 C1 N5 C4 0.3(4) . . . . ? C3 C4 N5 C1 -0.5(4) . . . . ? C5 C4 N5 C1 177.5(3) . . . . ? C14 C15 N6 C12 0.9(4) . . . . ? C16 C15 N6 C12 178.6(3) . . . . ? C13 C12 N6 C15 -1.8(4) . . . . ? C21 C22 N7 C19 -0.7(4) . . . . ? C20 C19 N7 C22 0.9(3) . . . . ? C18 C19 N7 C22 -175.6(3) . . . . ? C17 C18 O1 B1 6.3(5) . . . . ? C19 C18 O1 B1 -173.9(3) . . . . ? C17 C16 O2 B1 1.5(5) . . . . ? C15 C16 O2 B1 179.7(3) . . . . ? C6 C7 O3 B2 9.2(4) . . . . ? C8 C7 O3 B2 -171.1(3) . . . . ? C6 C5 O4 B2 -11.9(4) . . . . ? C4 C5 O4 B2 167.8(3) . . . . ? C16 O2 B1 F2 -117.0(3) . . . . ? C16 O2 B1 F1 122.1(3) . . . . ? C16 O2 B1 O1 3.0(4) . . . . ? C18 O1 B1 F2 113.5(3) . . . . ? C18 O1 B1 F1 -127.2(3) . . . . ? C18 O1 B1 O2 -7.0(4) . . . . ? C7 O3 B2 F3 -142.7(3) . . . . ? C7 O3 B2 F4 96.4(3) . . . . ? C7 O3 B2 O4 -21.8(4) . . . . ? C5 O4 B2 F3 144.4(3) . . . . ? C5 O4 B2 F4 -95.9(3) . . . . ? C5 O4 B2 O3 23.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.849 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.076 # Attachment '2-TATACl.CIF' data_90408mae _database_code_depnum_ccdc_archive 'CCDC 845954' #TrackingRef '2-TATACl.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H49 B Cl F6 N5 O2' _chemical_formula_weight 852.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P - 1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.341(3) _cell_length_b 12.445(6) _cell_length_c 20.303(8) _cell_angle_alpha 79.279(15) _cell_angle_beta 85.683(13) _cell_angle_gamma 80.571(15) _cell_volume 2040.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.167 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9362 _exptl_absorpt_correction_T_max 0.9835 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19971 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9212 _reflns_number_gt 5909 _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^)+(0.1149P)^2^+0.2854P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9212 _refine_ls_number_parameters 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1902 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.16275(8) 0.56711(6) 0.07309(3) 0.0356(2) Uani 1 1 d . . . F1 F 0.25741(18) 0.23090(14) 0.36531(9) 0.0393(4) Uani 1 1 d . . . F2 F 0.0228(2) 0.29182(16) 0.41948(8) 0.0403(4) Uani 1 1 d . . . O1 O 0.0208(2) 0.28353(16) 0.30630(9) 0.0305(4) Uani 1 1 d . . . O2 O 0.1550(2) 0.41929(16) 0.34652(9) 0.0305(4) Uani 1 1 d . . . N1 N -0.0038(3) 0.3448(2) 0.12584(11) 0.0294(5) Uani 1 1 d . . . H13 H 0.0407 0.4048 0.1113 0.035 Uiso 1 1 calc R . . N2 N 0.2621(3) 0.6294(2) 0.20948(12) 0.0321(5) Uani 1 1 d . . . H14 H 0.2306 0.6137 0.1724 0.039 Uiso 1 1 calc R . . C11 C 0.3082(3) 0.6213(2) 0.31575(14) 0.0290(6) Uani 1 1 d . . . C12 C -0.0900(3) 0.2028(2) 0.19286(14) 0.0318(6) Uani 1 1 d . . . C13 C 0.1350(3) 0.4219(2) 0.23155(13) 0.0297(6) Uani 1 1 d . . . H15 H 0.1635 0.4526 0.1866 0.036 Uiso 1 1 calc R . . C14 C -0.0129(3) 0.2934(2) 0.19187(13) 0.0280(6) Uani 1 1 d . . . C15 C 0.0514(3) 0.3326(2) 0.24443(13) 0.0266(5) Uani 1 1 d . . . C16 C 0.1771(3) 0.4666(2) 0.28382(13) 0.0266(6) Uani 1 1 d . . . C17 C 0.3652(3) 0.7130(2) 0.27828(16) 0.0336(6) Uani 1 1 d . . . C18 C 0.3351(3) 0.7176(2) 0.21227(15) 0.0340(6) Uani 1 1 d . . . H16 H 0.3606 0.7724 0.1755 0.041 Uiso 1 1 calc R . . C19 C -0.0727(3) 0.2904(3) 0.08665(15) 0.0346(6) Uani 1 1 d . . . H17 H -0.0821 0.3099 0.0394 0.042 Uiso 1 1 calc R . . C20 C -0.1267(3) 0.2018(3) 0.12763(15) 0.0343(6) Uani 1 1 d . . . C21 C 0.2438(3) 0.5674(2) 0.27230(13) 0.0288(6) Uani 1 1 d . . . B1 B 0.1148(4) 0.3038(3) 0.36124(15) 0.0294(7) Uani 1 1 d . . . N3 N 0.6414(3) 0.41743(19) 0.36943(11) 0.0291(5) Uani 1 1 d . . . C31 C 0.6903(3) 0.5096(2) 0.25598(13) 0.0251(5) Uani 1 1 d . . . N4 N 0.7327(3) 0.60758(19) 0.14312(11) 0.0287(5) Uani 1 1 d . . . C33 C 0.6017(3) 0.4429(2) 0.16208(14) 0.0309(6) Uani 1 1 d . . . H18 H 0.5869 0.4498 0.1155 0.037 Uiso 1 1 calc R . . C34 C 0.5657(3) 0.3430(2) 0.27539(14) 0.0304(6) Uani 1 1 d . . . H19 H 0.5309 0.2814 0.3046 0.036 Uiso 1 1 calc R . . C35 C 0.7727(3) 0.5798(2) 0.35076(13) 0.0284(6) Uani 1 1 d . . . C36 C 0.6750(3) 0.5205(2) 0.18574(13) 0.0267(5) Uani 1 1 d . . . C37 C 0.8084(3) 0.6804(2) 0.23677(13) 0.0278(6) Uani 1 1 d . . . C38 C 0.6326(3) 0.4217(2) 0.30123(13) 0.0276(6) Uani 1 1 d . . . C39 C 0.7917(3) 0.6904(2) 0.16694(14) 0.0297(6) Uani 1 1 d . . . C40 C 0.5509(3) 0.3558(2) 0.20720(15) 0.0317(6) Uani 1 1 d . . . H20 H 0.5037 0.3025 0.1904 0.038 Uiso 1 1 calc R . . C41 C 0.7378(3) 0.4802(3) 0.46373(14) 0.0340(6) Uani 1 1 d . . . H21 H 0.7040 0.4197 0.4944 0.041 Uiso 1 1 calc R . . C42 C 0.7255(3) 0.6149(2) 0.06986(13) 0.0306(6) Uani 1 1 d . . . H22 H 0.7369 0.5393 0.0596 0.037 Uiso 1 1 calc R . . H23 H 0.8183 0.6496 0.0470 0.037 Uiso 1 1 calc R . . C43 C 0.7588(3) 0.5897(2) 0.28106(13) 0.0263(5) Uani 1 1 d . . . C44 C 0.8431(3) 0.6606(3) 0.37577(14) 0.0338(6) Uani 1 1 d . A . C45 C 0.8363(4) 0.7832(3) 0.12405(15) 0.0364(7) Uani 1 1 d . . . H24 H 0.8268 0.7912 0.0770 0.044 Uiso 1 1 calc R . . N5 N 0.8937(4) 0.7478(2) 0.33132(13) 0.0454(7) Uani 1 1 d . . . C47 C 0.7166(3) 0.4908(2) 0.39519(13) 0.0289(6) Uani 1 1 d . . . C48 C 0.5683(3) 0.6814(3) 0.04242(14) 0.0345(6) Uani 1 1 d . . . H25 H 0.4756 0.6446 0.0631 0.041 Uiso 1 1 calc R . . H26 H 0.5537 0.7560 0.0545 0.041 Uiso 1 1 calc R . . C49 C 0.8596(3) 0.6477(3) 0.44482(15) 0.0366(7) Uani 1 1 d . . . H27 H 0.9060 0.7002 0.4628 0.044 Uiso 1 1 calc R A . C50 C 0.8083(3) 0.5585(3) 0.48655(14) 0.0353(6) Uani 1 1 d . A . H28 H 0.8220 0.5503 0.5333 0.042 Uiso 1 1 calc R . . C51 C 0.8729(3) 0.7623(2) 0.26279(14) 0.0326(6) Uani 1 1 d . A . C52 C 0.8941(4) 0.8629(3) 0.15037(15) 0.0391(7) Uani 1 1 d . A . H29 H 0.9215 0.9264 0.1206 0.047 Uiso 1 1 calc R . . C53 C 0.9142(4) 0.8547(3) 0.21852(15) 0.0381(7) Uani 1 1 d . . . H30 H 0.9555 0.9112 0.2348 0.046 Uiso 1 1 calc R A . C54 C 0.5553(3) 0.3378(3) 0.41655(14) 0.0345(6) Uani 1 1 d . . . H31 H 0.4582 0.3266 0.3950 0.041 Uiso 1 1 calc R . . H32 H 0.5171 0.3703 0.4569 0.041 Uiso 1 1 calc R . . C55 C 0.6578(4) 0.2261(3) 0.43827(17) 0.0432(8) Uani 1 1 d . . . H33 H 0.7571 0.2361 0.4588 0.052 Uiso 1 1 calc R . . H34 H 0.6916 0.1905 0.3987 0.052 Uiso 1 1 calc R . . C56 C 0.5691(4) 0.6925(3) -0.03322(16) 0.0457(8) Uani 1 1 d . . . H35 H 0.6542 0.7353 -0.0539 0.069 Uiso 1 1 calc R . . H36 H 0.4630 0.7305 -0.0491 0.069 Uiso 1 1 calc R . . H37 H 0.5905 0.6187 -0.0455 0.069 Uiso 1 1 calc R . . C57 C 1.0005(5) 0.8161(4) 0.3568(2) 0.0333(13) Uani 0.716(9) 1 d P A 1 H38 H 1.0777 0.8429 0.3204 0.040 Uiso 0.716(9) 1 calc PR A 1 H39 H 1.0642 0.7701 0.3940 0.040 Uiso 0.716(9) 1 calc PR A 1 C58 C 1.0063(13) 0.9830(12) 0.4075(9) 0.051(2) Uani 0.716(9) 1 d P A 1 H69 H 1.0671 0.9374 0.4450 0.076 Uiso 0.716(9) 1 calc PR A 1 H70 H 0.9389 1.0467 0.4229 0.076 Uiso 0.716(9) 1 calc PR A 1 H71 H 1.0827 1.0092 0.3714 0.076 Uiso 0.716(9) 1 calc PR A 1 C69 C 1.063(3) 0.966(3) 0.402(2) 0.050(7) Uani 0.284(9) 1 d P A 2 H72 H 1.0040 1.0332 0.3758 0.075 Uiso 0.284(9) 1 calc PR A 2 H73 H 1.1772 0.9746 0.4035 0.075 Uiso 0.284(9) 1 calc PR A 2 H74 H 1.0144 0.9556 0.4481 0.075 Uiso 0.284(9) 1 calc PR A 2 C59 C 0.5603(4) 0.1519(4) 0.4891(2) 0.0661(12) Uani 1 1 d . . . H43 H 0.5315 0.1857 0.5291 0.099 Uiso 1 1 calc R . . H44 H 0.6262 0.0791 0.5016 0.099 Uiso 1 1 calc R . . H45 H 0.4609 0.1435 0.4690 0.099 Uiso 1 1 calc R . . C60 C 0.8969(5) 0.9137(4) 0.3814(2) 0.0367(13) Uani 0.716(9) 1 d P A 1 H46 H 0.8195 0.8871 0.4178 0.044 Uiso 0.716(9) 1 calc PR A 1 H47 H 0.8334 0.9600 0.3442 0.044 Uiso 0.716(9) 1 calc PR A 1 C61 C 0.3677(4) 0.0608(3) 0.2543(2) 0.0582(10) Uani 1 1 d . . . H48 H 0.3229 0.1406 0.2465 0.070 Uiso 1 1 calc R . . H49 H 0.2789 0.0188 0.2733 0.070 Uiso 1 1 calc R . . C62 C 0.2980(4) 0.0231(3) 0.1428(2) 0.0649(12) Uani 1 1 d . . . H50 H 0.2334 -0.0351 0.1643 0.078 Uiso 1 1 calc R . . H51 H 0.2248 0.0949 0.1374 0.078 Uiso 1 1 calc R . . C63 C 0.4344(5) 0.0263(4) 0.1885(2) 0.0669(11) Uani 1 1 d . . . H52 H 0.5010 -0.0479 0.1978 0.080 Uiso 1 1 calc R . . H53 H 0.5057 0.0790 0.1651 0.080 Uiso 1 1 calc R . . C64 C 0.5002(6) 0.0386(4) 0.3021(4) 0.120(3) Uani 1 1 d . . . H54 H 0.5185 -0.0403 0.3215 0.180 Uiso 1 1 calc R . . H55 H 0.4694 0.0821 0.3379 0.180 Uiso 1 1 calc R . . H56 H 0.6003 0.0595 0.2783 0.180 Uiso 1 1 calc R . . C65 C 0.3609(7) 0.0006(4) 0.0758(3) 0.0906(15) Uani 1 1 d . . . H57 H 0.4417 -0.0678 0.0821 0.109 Uiso 1 1 calc R . . H58 H 0.4189 0.0619 0.0536 0.109 Uiso 1 1 calc R . . C66 C 0.2366(8) -0.0126(6) 0.0295(3) 0.110(2) Uani 1 1 d . . . H59 H 0.1965 -0.0831 0.0454 0.165 Uiso 1 1 calc R . . H60 H 0.2863 -0.0117 -0.0158 0.165 Uiso 1 1 calc R . . H61 H 0.1457 0.0484 0.0288 0.165 Uiso 1 1 calc R . . F3 F 0.3175(2) 0.59031(15) 0.38199(8) 0.0382(4) Uani 1 1 d . . . F4 F -0.1224(2) 0.12843(15) 0.24671(9) 0.0419(4) Uani 1 1 d . . . F5 F 0.4372(2) 0.78532(15) 0.30326(9) 0.0434(4) Uani 1 1 d . . . F6 F -0.2049(2) 0.12742(16) 0.10806(9) 0.0477(5) Uani 1 1 d . . . C67 C 1.0509(13) 0.8677(9) 0.3708(5) 0.032(3) Uani 0.284(9) 1 d P A 2 H65 H 1.0976 0.7993 0.4008 0.038 Uiso 0.284(9) 1 calc PR A 2 H66 H 1.1159 0.8727 0.3278 0.038 Uiso 0.284(9) 1 calc PR A 2 C70 C 0.8777(12) 0.8605(9) 0.3581(5) 0.027(3) Uani 0.284(9) 1 d P A 2 H67 H 0.8316 0.9236 0.3241 0.032 Uiso 0.284(9) 1 calc PR A 2 H68 H 0.8083 0.8588 0.3999 0.032 Uiso 0.284(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0379(4) 0.0411(4) 0.0282(4) 0.0001(3) -0.0057(3) -0.0127(3) F1 0.0343(8) 0.0334(10) 0.0506(11) -0.0006(8) -0.0132(7) -0.0093(7) F2 0.0461(9) 0.0513(12) 0.0288(9) -0.0060(8) 0.0014(7) -0.0255(8) O1 0.0347(10) 0.0314(11) 0.0277(10) -0.0018(8) -0.0055(8) -0.0138(8) O2 0.0354(10) 0.0321(11) 0.0262(10) -0.0029(8) -0.0041(7) -0.0134(8) N1 0.0307(11) 0.0308(13) 0.0277(12) -0.0036(10) -0.0036(9) -0.0078(9) N2 0.0386(12) 0.0291(13) 0.0287(12) -0.0023(10) -0.0020(9) -0.0086(10) C11 0.0311(13) 0.0264(14) 0.0304(14) -0.0059(11) -0.0037(11) -0.0045(10) C12 0.0356(14) 0.0288(15) 0.0316(14) -0.0028(12) -0.0071(11) -0.0067(11) C13 0.0332(14) 0.0331(16) 0.0243(13) -0.0032(11) -0.0014(10) -0.0116(11) C14 0.0270(13) 0.0299(15) 0.0278(14) -0.0046(11) -0.0022(10) -0.0059(10) C15 0.0236(12) 0.0278(14) 0.0281(13) -0.0043(11) -0.0030(10) -0.0026(10) C16 0.0228(12) 0.0279(14) 0.0289(14) -0.0030(11) -0.0019(10) -0.0053(10) C17 0.0320(14) 0.0253(15) 0.0465(17) -0.0117(13) 0.0015(12) -0.0084(11) C18 0.0389(15) 0.0260(15) 0.0369(16) -0.0028(12) 0.0008(12) -0.0086(12) C19 0.0376(15) 0.0367(17) 0.0314(15) -0.0093(13) -0.0057(11) -0.0058(12) C20 0.0385(15) 0.0299(16) 0.0381(16) -0.0091(13) -0.0103(12) -0.0079(12) C21 0.0286(13) 0.0291(15) 0.0289(14) -0.0041(11) -0.0017(10) -0.0064(11) B1 0.0325(15) 0.0294(17) 0.0277(15) -0.0010(13) -0.0046(12) -0.0122(12) N3 0.0291(11) 0.0294(13) 0.0299(12) -0.0044(10) -0.0016(9) -0.0088(9) C31 0.0226(12) 0.0238(14) 0.0301(14) -0.0071(11) -0.0035(10) -0.0034(10) N4 0.0325(11) 0.0296(13) 0.0261(11) -0.0067(10) -0.0039(9) -0.0080(9) C33 0.0319(13) 0.0334(16) 0.0299(14) -0.0087(12) -0.0059(11) -0.0067(11) C34 0.0291(13) 0.0280(15) 0.0359(15) -0.0060(12) -0.0039(11) -0.0080(11) C35 0.0261(13) 0.0305(15) 0.0302(14) -0.0088(12) -0.0035(10) -0.0042(10) C36 0.0264(12) 0.0240(14) 0.0306(14) -0.0066(11) -0.0042(10) -0.0028(10) C37 0.0298(13) 0.0262(14) 0.0291(14) -0.0078(11) -0.0026(10) -0.0058(10) C38 0.0247(12) 0.0280(15) 0.0308(14) -0.0057(11) -0.0032(10) -0.0044(10) C39 0.0319(13) 0.0278(15) 0.0309(14) -0.0067(11) -0.0037(11) -0.0064(11) C40 0.0288(13) 0.0297(15) 0.0399(16) -0.0100(12) -0.0066(11) -0.0071(11) C41 0.0370(15) 0.0359(17) 0.0301(15) -0.0028(12) -0.0043(11) -0.0104(12) C42 0.0331(14) 0.0338(16) 0.0266(13) -0.0077(12) -0.0026(11) -0.0071(11) C43 0.0237(12) 0.0264(14) 0.0298(14) -0.0068(11) -0.0033(10) -0.0033(10) C44 0.0394(15) 0.0327(16) 0.0329(15) -0.0082(12) -0.0027(11) -0.0128(12) C45 0.0460(16) 0.0341(17) 0.0300(15) -0.0034(13) -0.0051(12) -0.0102(13) N5 0.0730(18) 0.0405(16) 0.0313(13) -0.0093(12) -0.0040(12) -0.0298(14) C47 0.0268(13) 0.0309(15) 0.0300(14) -0.0052(12) -0.0035(10) -0.0068(10) C48 0.0373(15) 0.0335(16) 0.0323(15) -0.0050(12) -0.0041(11) -0.0038(12) C49 0.0446(16) 0.0374(17) 0.0329(15) -0.0104(13) -0.0070(12) -0.0138(13) C50 0.0365(15) 0.0440(18) 0.0273(14) -0.0074(13) -0.0053(11) -0.0092(12) C51 0.0415(15) 0.0289(15) 0.0302(14) -0.0073(12) -0.0021(11) -0.0107(12) C52 0.0526(17) 0.0300(17) 0.0361(16) -0.0016(13) -0.0013(13) -0.0160(13) C53 0.0500(17) 0.0303(16) 0.0382(16) -0.0084(13) -0.0034(13) -0.0147(13) C54 0.0343(14) 0.0383(17) 0.0326(15) -0.0012(13) -0.0026(11) -0.0160(12) C55 0.0423(16) 0.0376(18) 0.0490(19) 0.0043(15) -0.0111(14) -0.0133(13) C56 0.0499(18) 0.051(2) 0.0357(17) -0.0098(15) -0.0148(14) 0.0009(15) C57 0.035(2) 0.035(3) 0.035(2) -0.0109(19) -0.0038(17) -0.014(2) C58 0.063(7) 0.040(6) 0.057(4) -0.024(4) -0.018(6) -0.006(5) C69 0.058(16) 0.031(11) 0.065(16) -0.015(8) -0.035(17) 0.000(12) C59 0.057(2) 0.062(3) 0.073(3) 0.031(2) -0.0208(19) -0.0318(19) C60 0.041(2) 0.035(3) 0.036(2) -0.011(2) -0.0076(17) -0.0045(18) C61 0.0422(19) 0.059(3) 0.074(3) -0.028(2) 0.0107(17) 0.0045(16) C62 0.048(2) 0.035(2) 0.107(4) 0.012(2) -0.025(2) -0.0102(15) C63 0.071(3) 0.047(2) 0.082(3) -0.004(2) 0.001(2) -0.0154(19) C64 0.072(3) 0.051(3) 0.257(8) -0.062(4) -0.068(4) 0.003(2) C65 0.106(4) 0.056(3) 0.111(4) -0.020(3) -0.009(3) -0.008(3) C66 0.161(6) 0.120(5) 0.060(3) -0.019(3) -0.007(3) -0.051(4) F3 0.0491(10) 0.0371(10) 0.0318(9) -0.0066(7) -0.0073(7) -0.0133(7) F4 0.0575(10) 0.0339(10) 0.0368(10) 0.0026(8) -0.0111(8) -0.0201(8) F5 0.0507(10) 0.0313(10) 0.0541(11) -0.0136(8) -0.0009(8) -0.0173(8) F6 0.0646(12) 0.0367(11) 0.0489(11) -0.0102(9) -0.0196(9) -0.0180(9) C67 0.042(6) 0.031(6) 0.028(5) -0.008(4) -0.014(4) -0.012(5) C70 0.032(6) 0.018(5) 0.033(5) -0.009(4) -0.003(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 B1 1.370(4) . ? F2 B1 1.358(3) . ? O1 C15 1.317(3) . ? O1 B1 1.491(3) . ? O2 C16 1.312(3) . ? O2 B1 1.501(4) . ? N1 C19 1.349(4) . ? N1 C14 1.376(3) . ? N1 H13 0.8800 . ? N2 C18 1.351(4) . ? N2 C21 1.374(4) . ? N2 H14 0.8800 . ? C11 F3 1.333(3) . ? C11 C17 1.382(4) . ? C11 C21 1.388(4) . ? C12 F4 1.337(3) . ? C12 C14 1.382(4) . ? C12 C20 1.384(4) . ? C13 C16 1.378(4) . ? C13 C15 1.382(4) . ? C13 H15 0.9500 . ? C14 C15 1.425(4) . ? C16 C21 1.427(4) . ? C17 F5 1.349(3) . ? C17 C18 1.371(4) . ? C18 H16 0.9500 . ? C19 C20 1.370(4) . ? C19 H17 0.9500 . ? C20 F6 1.347(3) . ? N3 C38 1.383(3) . ? N3 C47 1.384(3) . ? N3 C54 1.480(3) . ? C31 C43 1.413(4) . ? C31 C38 1.415(4) . ? C31 C36 1.421(4) . ? N4 C36 1.384(4) . ? N4 C39 1.388(3) . ? N4 C42 1.478(3) . ? C33 C40 1.385(4) . ? C33 C36 1.395(4) . ? C33 H18 0.9500 . ? C34 C40 1.376(4) . ? C34 C38 1.400(4) . ? C34 H19 0.9500 . ? C35 C43 1.410(4) . ? C35 C47 1.413(4) . ? C35 C44 1.428(4) . ? C37 C43 1.405(4) . ? C37 C39 1.415(4) . ? C37 C51 1.425(4) . ? C39 C45 1.395(4) . ? C40 H20 0.9500 . ? C41 C50 1.382(4) . ? C41 C47 1.395(4) . ? C41 H21 0.9500 . ? C42 C48 1.516(4) . ? C42 H22 0.9900 . ? C42 H23 0.9900 . ? C44 N5 1.378(4) . ? C44 C49 1.396(4) . ? C45 C52 1.377(4) . ? C45 H24 0.9500 . ? N5 C51 1.390(4) . ? N5 C57 1.506(5) . ? N5 C70 1.578(11) . ? C48 C56 1.516(4) . ? C48 H25 0.9900 . ? C48 H26 0.9900 . ? C49 C50 1.372(4) . ? C49 H27 0.9500 . ? C50 H28 0.9500 . ? C51 C53 1.396(4) . ? C52 C53 1.389(4) . ? C52 H29 0.9500 . ? C53 H30 0.9500 . ? C54 C55 1.515(4) . ? C54 H31 0.9900 . ? C54 H32 0.9900 . ? C55 C59 1.530(5) . ? C55 H33 0.9900 . ? C55 H34 0.9900 . ? C56 H35 0.9800 . ? C56 H36 0.9800 . ? C56 H37 0.9800 . ? C57 C60 1.512(7) . ? C57 H38 0.9900 . ? C57 H39 0.9900 . ? C58 C60 1.536(15) . ? C58 H69 0.9800 . ? C58 H70 0.9800 . ? C58 H71 0.9800 . ? C69 C67 1.51(4) . ? C69 H72 0.9800 . ? C69 H73 0.9800 . ? C69 H74 0.9800 . ? C59 H43 0.9800 . ? C59 H44 0.9800 . ? C59 H45 0.9800 . ? C60 H46 0.9900 . ? C60 H47 0.9900 . ? C61 C64 1.483(6) . ? C61 C63 1.517(6) . ? C61 H48 0.9900 . ? C61 H49 0.9900 . ? C62 C65 1.479(7) . ? C62 C63 1.530(6) . ? C62 H50 0.9900 . ? C62 H51 0.9900 . ? C63 H52 0.9900 . ? C63 H53 0.9900 . ? C64 H54 0.9800 . ? C64 H55 0.9800 . ? C64 H56 0.9800 . ? C65 C66 1.498(7) . ? C65 H57 0.9900 . ? C65 H58 0.9900 . ? C66 H59 0.9800 . ? C66 H60 0.9800 . ? C66 H61 0.9800 . ? C67 C70 1.507(15) . ? C67 H65 0.9900 . ? C67 H66 0.9900 . ? C70 H67 0.9900 . ? C70 H68 0.9900 . ? 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 C15 O1 B1 118.7(2) . . ? C16 O2 B1 119.0(2) . . ? C19 N1 C14 110.4(2) . . ? C19 N1 H13 124.8 . . ? C14 N1 H13 124.8 . . ? C18 N2 C21 110.9(2) . . ? C18 N2 H14 124.6 . . ? C21 N2 H14 124.6 . . ? F3 C11 C17 125.1(2) . . ? F3 C11 C21 126.8(2) . . ? C17 C11 C21 108.1(2) . . ? F4 C12 C14 126.6(2) . . ? F4 C12 C20 125.7(3) . . ? C14 C12 C20 107.8(3) . . ? C16 C13 C15 120.1(2) . . ? C16 C13 H15 120.0 . . ? C15 C13 H15 120.0 . . ? N1 C14 C12 106.2(2) . . ? N1 C14 C15 122.6(2) . . ? C12 C14 C15 131.2(3) . . ? O1 C15 C13 121.2(2) . . ? O1 C15 C14 117.1(2) . . ? C13 C15 C14 121.7(2) . . ? O2 C16 C13 121.4(2) . . ? O2 C16 C21 117.0(2) . . ? C13 C16 C21 121.5(2) . . ? F5 C17 C18 126.5(3) . . ? F5 C17 C11 125.2(3) . . ? C18 C17 C11 108.3(3) . . ? N2 C18 C17 107.0(3) . . ? N2 C18 H16 126.5 . . ? C17 C18 H16 126.5 . . ? N1 C19 C20 107.2(3) . . ? N1 C19 H17 126.4 . . ? C20 C19 H17 126.4 . . ? F6 C20 C19 125.9(3) . . ? F6 C20 C12 125.8(3) . . ? C19 C20 C12 108.4(3) . . ? N2 C21 C11 105.7(2) . . ? N2 C21 C16 122.9(2) . . ? C11 C21 C16 131.4(3) . . ? F2 B1 F1 111.9(2) . . ? F2 B1 O1 109.0(2) . . ? F1 B1 O1 108.5(2) . . ? F2 B1 O2 108.4(2) . . ? F1 B1 O2 108.5(2) . . ? O1 B1 O2 110.5(2) . . ? C38 N3 C47 122.4(2) . . ? C38 N3 C54 118.8(2) . . ? C47 N3 C54 118.6(2) . . ? C43 C31 C38 119.7(2) . . ? C43 C31 C36 119.5(2) . . ? C38 C31 C36 120.8(2) . . ? C36 N4 C39 122.1(2) . . ? C36 N4 C42 118.9(2) . . ? C39 N4 C42 118.9(2) . . ? C40 C33 C36 119.4(3) . . ? C40 C33 H18 120.3 . . ? C36 C33 H18 120.3 . . ? C40 C34 C38 119.4(3) . . ? C40 C34 H19 120.3 . . ? C38 C34 H19 120.3 . . ? C43 C35 C47 119.9(2) . . ? C43 C35 C44 119.5(3) . . ? C47 C35 C44 120.6(2) . . ? N4 C36 C33 122.2(2) . . ? N4 C36 C31 119.1(2) . . ? C33 C36 C31 118.7(2) . . ? C43 C37 C39 119.8(2) . . ? C43 C37 C51 119.5(2) . . ? C39 C37 C51 120.6(3) . . ? N3 C38 C34 122.1(2) . . ? N3 C38 C31 119.1(2) . . ? C34 C38 C31 118.8(2) . . ? N4 C39 C45 122.0(3) . . ? N4 C39 C37 119.1(3) . . ? C45 C39 C37 118.9(3) . . ? C34 C40 C33 122.9(3) . . ? C34 C40 H20 118.6 . . ? C33 C40 H20 118.6 . . ? C50 C41 C47 119.3(3) . . ? C50 C41 H21 120.3 . . ? C47 C41 H21 120.3 . . ? N4 C42 C48 112.7(2) . . ? N4 C42 H22 109.0 . . ? C48 C42 H22 109.0 . . ? N4 C42 H23 109.0 . . ? C48 C42 H23 109.0 . . ? H22 C42 H23 107.8 . . ? C37 C43 C35 120.2(2) . . ? C37 C43 C31 120.0(2) . . ? C35 C43 C31 119.7(2) . . ? N5 C44 C49 122.1(3) . . ? N5 C44 C35 119.3(3) . . ? C49 C44 C35 118.6(3) . . ? C52 C45 C39 119.6(3) . . ? C52 C45 H24 120.2 . . ? C39 C45 H24 120.2 . . ? C44 N5 C51 122.1(2) . . ? C44 N5 C57 117.8(3) . . ? C51 N5 C57 119.2(3) . . ? C44 N5 C70 115.9(4) . . ? C51 N5 C70 113.1(4) . . ? C57 N5 C70 41.0(4) . . ? N3 C47 C41 122.1(3) . . ? N3 C47 C35 119.0(2) . . ? C41 C47 C35 118.9(2) . . ? C56 C48 C42 111.2(2) . . ? C56 C48 H25 109.4 . . ? C42 C48 H25 109.4 . . ? C56 C48 H26 109.4 . . ? C42 C48 H26 109.4 . . ? H25 C48 H26 108.0 . . ? C50 C49 C44 119.5(3) . . ? C50 C49 H27 120.3 . . ? C44 C49 H27 120.3 . . ? C49 C50 C41 123.1(3) . . ? C49 C50 H28 118.4 . . ? C41 C50 H28 118.4 . . ? N5 C51 C53 121.8(3) . . ? N5 C51 C37 119.2(3) . . ? C53 C51 C37 118.9(3) . . ? C45 C52 C53 123.0(3) . . ? C45 C52 H29 118.5 . . ? C53 C52 H29 118.5 . . ? C52 C53 C51 119.0(3) . . ? C52 C53 H30 120.5 . . ? C51 C53 H30 120.5 . . ? N3 C54 C55 114.2(2) . . ? N3 C54 H31 108.7 . . ? C55 C54 H31 108.7 . . ? N3 C54 H32 108.7 . . ? C55 C54 H32 108.7 . . ? H31 C54 H32 107.6 . . ? C54 C55 C59 110.1(3) . . ? C54 C55 H33 109.6 . . ? C59 C55 H33 109.6 . . ? C54 C55 H34 109.6 . . ? C59 C55 H34 109.6 . . ? H33 C55 H34 108.2 . . ? C48 C56 H35 109.5 . . ? C48 C56 H36 109.5 . . ? H35 C56 H36 109.5 . . ? C48 C56 H37 109.5 . . ? H35 C56 H37 109.5 . . ? H36 C56 H37 109.5 . . ? N5 C57 C60 109.9(4) . . ? N5 C57 H38 109.7 . . ? C60 C57 H38 109.7 . . ? N5 C57 H39 109.7 . . ? C60 C57 H39 109.7 . . ? H38 C57 H39 108.2 . . ? C67 C69 H72 109.5 . . ? C67 C69 H73 109.5 . . ? H72 C69 H73 109.5 . . ? C67 C69 H74 109.5 . . ? H72 C69 H74 109.5 . . ? H73 C69 H74 109.5 . . ? C55 C59 H43 109.5 . . ? C55 C59 H44 109.5 . . ? H43 C59 H44 109.5 . . ? C55 C59 H45 109.5 . . ? H43 C59 H45 109.5 . . ? H44 C59 H45 109.5 . . ? C57 C60 C58 109.7(5) . . ? C57 C60 H46 109.7 . . ? C58 C60 H46 109.7 . . ? C57 C60 H47 109.7 . . ? C58 C60 H47 109.7 . . ? H46 C60 H47 108.2 . . ? C64 C61 C63 109.4(4) . . ? C64 C61 H48 109.8 . . ? C63 C61 H48 109.8 . . ? C64 C61 H49 109.8 . . ? C63 C61 H49 109.8 . . ? H48 C61 H49 108.2 . . ? C65 C62 C63 112.4(4) . . ? C65 C62 H50 109.1 . . ? C63 C62 H50 109.1 . . ? C65 C62 H51 109.1 . . ? C63 C62 H51 109.1 . . ? H50 C62 H51 107.9 . . ? C61 C63 C62 111.7(4) . . ? C61 C63 H52 109.3 . . ? C62 C63 H52 109.3 . . ? C61 C63 H53 109.3 . . ? C62 C63 H53 109.3 . . ? H52 C63 H53 107.9 . . ? C61 C64 H54 109.5 . . ? C61 C64 H55 109.5 . . ? H54 C64 H55 109.5 . . ? C61 C64 H56 109.5 . . ? H54 C64 H56 109.5 . . ? H55 C64 H56 109.5 . . ? C62 C65 C66 116.0(5) . . ? C62 C65 H57 108.3 . . ? C66 C65 H57 108.3 . . ? C62 C65 H58 108.3 . . ? C66 C65 H58 108.3 . . ? H57 C65 H58 107.4 . . ? C65 C66 H59 109.5 . . ? C65 C66 H60 109.5 . . ? H59 C66 H60 109.5 . . ? C65 C66 H61 109.5 . . ? H59 C66 H61 109.5 . . ? H60 C66 H61 109.5 . . ? C69 C67 C70 112.0(13) . . ? C69 C67 H65 109.2 . . ? C70 C67 H65 109.2 . . ? C69 C67 H66 109.2 . . ? C70 C67 H66 109.2 . . ? H65 C67 H66 107.9 . . ? C67 C70 N5 103.0(7) . . ? C67 C70 H67 111.2 . . ? N5 C70 H67 111.2 . . ? C67 C70 H68 111.2 . . ? N5 C70 H68 111.2 . . ? H67 C70 H68 109.1 . . ? 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 C19 N1 C14 C12 0.4(3) . . . . ? C19 N1 C14 C15 179.6(2) . . . . ? F4 C12 C14 N1 179.0(2) . . . . ? C20 C12 C14 N1 -0.3(3) . . . . ? F4 C12 C14 C15 0.0(5) . . . . ? C20 C12 C14 C15 -179.4(3) . . . . ? B1 O1 C15 C13 -16.8(4) . . . . ? B1 O1 C15 C14 166.5(2) . . . . ? C16 C13 C15 O1 -5.0(4) . . . . ? C16 C13 C15 C14 171.6(2) . . . . ? N1 C14 C15 O1 173.2(2) . . . . ? C12 C14 C15 O1 -7.9(4) . . . . ? N1 C14 C15 C13 -3.6(4) . . . . ? C12 C14 C15 C13 175.3(3) . . . . ? B1 O2 C16 C13 12.3(4) . . . . ? B1 O2 C16 C21 -168.8(2) . . . . ? C15 C13 C16 O2 7.3(4) . . . . ? C15 C13 C16 C21 -171.5(2) . . . . ? F3 C11 C17 F5 -0.7(4) . . . . ? C21 C11 C17 F5 -179.5(2) . . . . ? F3 C11 C17 C18 179.7(2) . . . . ? C21 C11 C17 C18 0.8(3) . . . . ? C21 N2 C18 C17 0.1(3) . . . . ? F5 C17 C18 N2 179.8(2) . . . . ? C11 C17 C18 N2 -0.6(3) . . . . ? C14 N1 C19 C20 -0.4(3) . . . . ? N1 C19 C20 F6 179.0(3) . . . . ? N1 C19 C20 C12 0.1(3) . . . . ? F4 C12 C20 F6 1.9(5) . . . . ? C14 C12 C20 F6 -178.7(3) . . . . ? F4 C12 C20 C19 -179.2(3) . . . . ? C14 C12 C20 C19 0.1(3) . . . . ? C18 N2 C21 C11 0.4(3) . . . . ? C18 N2 C21 C16 -177.1(2) . . . . ? F3 C11 C21 N2 -179.6(2) . . . . ? C17 C11 C21 N2 -0.7(3) . . . . ? F3 C11 C21 C16 -2.4(5) . . . . ? C17 C11 C21 C16 176.5(3) . . . . ? O2 C16 C21 N2 -175.2(2) . . . . ? C13 C16 C21 N2 3.7(4) . . . . ? O2 C16 C21 C11 8.0(4) . . . . ? C13 C16 C21 C11 -173.1(3) . . . . ? C15 O1 B1 F2 152.1(2) . . . . ? C15 O1 B1 F1 -85.7(3) . . . . ? C15 O1 B1 O2 33.1(3) . . . . ? C16 O2 B1 F2 -150.4(2) . . . . ? C16 O2 B1 F1 87.9(3) . . . . ? C16 O2 B1 O1 -30.9(3) . . . . ? C39 N4 C36 C33 173.9(2) . . . . ? C42 N4 C36 C33 -3.8(4) . . . . ? C39 N4 C36 C31 -6.0(4) . . . . ? C42 N4 C36 C31 176.4(2) . . . . ? C40 C33 C36 N4 178.1(2) . . . . ? C40 C33 C36 C31 -2.1(4) . . . . ? C43 C31 C36 N4 2.1(4) . . . . ? C38 C31 C36 N4 179.9(2) . . . . ? C43 C31 C36 C33 -177.7(2) . . . . ? C38 C31 C36 C33 0.1(4) . . . . ? C47 N3 C38 C34 175.8(2) . . . . ? C54 N3 C38 C34 -9.5(4) . . . . ? C47 N3 C38 C31 -5.4(4) . . . . ? C54 N3 C38 C31 169.3(2) . . . . ? C40 C34 C38 N3 175.9(2) . . . . ? C40 C34 C38 C31 -3.0(4) . . . . ? C43 C31 C38 N3 1.4(4) . . . . ? C36 C31 C38 N3 -176.4(2) . . . . ? C43 C31 C38 C34 -179.8(2) . . . . ? C36 C31 C38 C34 2.4(4) . . . . ? C36 N4 C39 C45 -174.2(2) . . . . ? C42 N4 C39 C45 3.4(4) . . . . ? C36 N4 C39 C37 6.3(4) . . . . ? C42 N4 C39 C37 -176.1(2) . . . . ? C43 C37 C39 N4 -2.7(4) . . . . ? C51 C37 C39 N4 178.2(2) . . . . ? C43 C37 C39 C45 177.7(2) . . . . ? C51 C37 C39 C45 -1.4(4) . . . . ? C38 C34 C40 C33 1.0(4) . . . . ? C36 C33 C40 C34 1.6(4) . . . . ? C36 N4 C42 C48 90.3(3) . . . . ? C39 N4 C42 C48 -87.4(3) . . . . ? C39 C37 C43 C35 -179.1(2) . . . . ? C51 C37 C43 C35 0.0(4) . . . . ? C39 C37 C43 C31 -0.9(4) . . . . ? C51 C37 C43 C31 178.2(2) . . . . ? C47 C35 C43 C37 177.5(2) . . . . ? C44 C35 C43 C37 -2.3(4) . . . . ? C47 C35 C43 C31 -0.7(4) . . . . ? C44 C35 C43 C31 179.6(2) . . . . ? C38 C31 C43 C37 -176.6(2) . . . . ? C36 C31 C43 C37 1.2(4) . . . . ? C38 C31 C43 C35 1.6(4) . . . . ? C36 C31 C43 C35 179.4(2) . . . . ? C43 C35 C44 N5 1.1(4) . . . . ? C47 C35 C44 N5 -178.7(3) . . . . ? C43 C35 C44 C49 -178.4(3) . . . . ? C47 C35 C44 C49 1.9(4) . . . . ? N4 C39 C45 C52 180.0(3) . . . . ? C37 C39 C45 C52 -0.5(4) . . . . ? C49 C44 N5 C51 -178.1(3) . . . . ? C35 C44 N5 C51 2.5(5) . . . . ? C49 C44 N5 C57 13.0(5) . . . . ? C35 C44 N5 C57 -166.4(3) . . . . ? C49 C44 N5 C70 -33.1(6) . . . . ? C35 C44 N5 C70 147.5(5) . . . . ? C38 N3 C47 C41 -174.3(2) . . . . ? C54 N3 C47 C41 11.1(4) . . . . ? C38 N3 C47 C35 6.3(4) . . . . ? C54 N3 C47 C35 -168.4(2) . . . . ? C50 C41 C47 N3 -177.6(3) . . . . ? C50 C41 C47 C35 1.9(4) . . . . ? C43 C35 C47 N3 -3.1(4) . . . . ? C44 C35 C47 N3 176.6(2) . . . . ? C43 C35 C47 C41 177.4(2) . . . . ? C44 C35 C47 C41 -2.9(4) . . . . ? N4 C42 C48 C56 176.9(3) . . . . ? N5 C44 C49 C50 -179.4(3) . . . . ? C35 C44 C49 C50 0.0(4) . . . . ? C44 C49 C50 C41 -1.0(5) . . . . ? C47 C41 C50 C49 0.0(4) . . . . ? C44 N5 C51 C53 175.6(3) . . . . ? C57 N5 C51 C53 -15.7(5) . . . . ? C70 N5 C51 C53 29.7(5) . . . . ? C44 N5 C51 C37 -4.8(5) . . . . ? C57 N5 C51 C37 164.0(3) . . . . ? C70 N5 C51 C37 -150.6(5) . . . . ? C43 C37 C51 N5 3.4(4) . . . . ? C39 C37 C51 N5 -177.5(3) . . . . ? C43 C37 C51 C53 -176.9(3) . . . . ? C39 C37 C51 C53 2.2(4) . . . . ? C39 C45 C52 C53 1.5(5) . . . . ? C45 C52 C53 C51 -0.6(5) . . . . ? N5 C51 C53 C52 178.4(3) . . . . ? C37 C51 C53 C52 -1.2(4) . . . . ? C38 N3 C54 C55 91.4(3) . . . . ? C47 N3 C54 C55 -93.8(3) . . . . ? N3 C54 C55 C59 177.5(3) . . . . ? C44 N5 C57 C60 -92.5(4) . . . . ? C51 N5 C57 C60 98.3(4) . . . . ? C70 N5 C57 C60 5.9(6) . . . . ? N5 C57 C60 C58 179.8(8) . . . . ? C64 C61 C63 C62 167.5(4) . . . . ? C65 C62 C63 C61 174.2(4) . . . . ? C63 C62 C65 C66 175.5(4) . . . . ? C69 C67 C70 N5 -175(2) . . . . ? C44 N5 C70 C67 105.3(7) . . . . ? C51 N5 C70 C67 -106.6(6) . . . . ? C57 N5 C70 C67 1.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.418 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.074 # Attachment '3-TATACl.CIF' data_90603mae _database_code_depnum_ccdc_archive 'CCDC 845955' #TrackingRef '3-TATACl.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H57 B Cl3 F2 N5 O2' _chemical_formula_weight 891.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P - 1' _symmetry_space_group_name_Hall '- P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.092(4) _cell_length_b 11.957(4) _cell_length_c 19.330(6) _cell_angle_alpha 77.243(10) _cell_angle_beta 82.685(13) _cell_angle_gamma 63.623(12) _cell_volume 2238.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9265 _exptl_absorpt_correction_T_max 0.9501 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22208 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10173 _reflns_number_gt 6228 _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^)+(0.0787P)^2^+2.3966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10173 _refine_ls_number_parameters 557 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1972 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 C1 C 1.6334(4) 0.1835(4) 0.0329(2) 0.0571(11) Uani 1 1 d . . . H1 H 1.6832 0.1172 0.0721 0.086 Uiso 1 1 calc R . . H2 H 1.6970 0.1977 -0.0040 0.086 Uiso 1 1 calc R . . H3 H 1.5758 0.1567 0.0129 0.086 Uiso 1 1 calc R . . C2 C 1.5480(4) 0.3041(3) 0.05982(18) 0.0372(8) Uani 1 1 d . . . H4 H 1.5052 0.3726 0.0191 0.045 Uiso 1 1 calc R . . H5 H 1.6066 0.3282 0.0820 0.045 Uiso 1 1 calc R . . C3 C 1.4402(3) 0.2952(3) 0.11283(16) 0.0307(7) Uani 1 1 d . . . C4 C 1.2032(4) 0.5854(3) 0.04389(19) 0.0413(8) Uani 1 1 d . . . H6 H 1.2508 0.5386 0.0056 0.062 Uiso 1 1 calc R . . H7 H 1.1811 0.6757 0.0275 0.062 Uiso 1 1 calc R . . H8 H 1.1201 0.5750 0.0575 0.062 Uiso 1 1 calc R . . C5 C 1.2925(3) 0.5340(3) 0.10758(16) 0.0304(7) Uani 1 1 d . . . H9 H 1.3764 0.5448 0.0937 0.036 Uiso 1 1 calc R . . H10 H 1.2454 0.5833 0.1456 0.036 Uiso 1 1 calc R . . C6 C 1.3271(3) 0.3969(3) 0.13514(15) 0.0279(7) Uani 1 1 d . . . C7 C 1.2497(3) 0.3446(3) 0.18146(15) 0.0274(6) Uani 1 1 d . . . N1 N 1.3166(3) 0.2142(3) 0.18776(14) 0.0319(6) Uani 1 1 d . . . H11 H 1.2891 0.1594 0.2142 0.038 Uiso 1 1 calc R . . C8 C 1.4307(3) 0.1842(3) 0.14698(17) 0.0330(7) Uani 1 1 d . . . H12 H 1.4943 0.1005 0.1424 0.040 Uiso 1 1 calc R . . C9 C 1.1220(3) 0.4025(3) 0.21696(15) 0.0273(6) Uani 1 1 d . . . C10 C 1.0562(3) 0.3323(3) 0.25513(16) 0.0301(7) Uani 1 1 d . . . H13 H 1.0916 0.2443 0.2539 0.036 Uiso 1 1 calc R . . C11 C 0.9408(3) 0.3873(3) 0.29461(15) 0.0271(6) Uani 1 1 d . . . C12 C 0.8796(3) 0.3148(3) 0.34156(16) 0.0285(7) Uani 1 1 d . . . N2 N 0.9386(3) 0.1839(3) 0.34876(13) 0.0312(6) Uani 1 1 d . . . H14 H 1.0139 0.1382 0.3273 0.037 Uiso 1 1 calc R . . C13 C 0.8610(4) 0.1380(3) 0.39430(17) 0.0359(8) Uani 1 1 d . . . H15 H 0.8792 0.0508 0.4081 0.043 Uiso 1 1 calc R . . C14 C 0.7515(4) 0.2371(3) 0.41758(16) 0.0337(7) Uani 1 1 d . . . C15 C 0.6438(4) 0.2237(4) 0.46988(18) 0.0422(9) Uani 1 1 d . . . H16 H 0.6414 0.1420 0.4698 0.051 Uiso 1 1 calc R . . H17 H 0.5553 0.2929 0.4546 0.051 Uiso 1 1 calc R . . C16 C 0.6664(5) 0.2283(4) 0.54488(19) 0.0534(11) Uani 1 1 d . . . H18 H 0.7516 0.1572 0.5613 0.080 Uiso 1 1 calc R . . H19 H 0.5923 0.2221 0.5764 0.080 Uiso 1 1 calc R . . H20 H 0.6700 0.3086 0.5453 0.080 Uiso 1 1 calc R . . C17 C 0.7620(3) 0.3501(3) 0.38454(15) 0.0308(7) Uani 1 1 d . . . C18 C 0.6669(3) 0.4817(3) 0.39523(17) 0.0348(7) Uani 1 1 d . . . H21 H 0.5796 0.4821 0.4145 0.042 Uiso 1 1 calc R . . H22 H 0.6507 0.5398 0.3486 0.042 Uiso 1 1 calc R . . C19 C 0.7181(4) 0.5313(4) 0.44503(19) 0.0433(9) Uani 1 1 d . . . H23 H 0.7388 0.4721 0.4905 0.065 Uiso 1 1 calc R . . H24 H 0.6490 0.6147 0.4527 0.065 Uiso 1 1 calc R . . H25 H 0.7998 0.5393 0.4241 0.065 Uiso 1 1 calc R . . O1 O 1.0695(2) 0.5263(2) 0.21362(12) 0.0359(6) Uani 1 1 d . . . O2 O 0.8829(2) 0.5108(2) 0.29237(12) 0.0342(5) Uani 1 1 d . . . B1 B 0.9329(4) 0.5966(4) 0.2434(2) 0.0317(8) Uani 1 1 d . . . F1 F 0.93711(19) 0.67930(17) 0.28119(10) 0.0359(4) Uani 1 1 d . . . F2 F 0.8463(2) 0.6622(2) 0.18812(11) 0.0505(6) Uani 1 1 d . . . C20 C -0.3210(3) -0.0520(3) 0.30650(17) 0.0329(7) Uani 1 1 d . . . H26 H -0.2452 -0.1223 0.2924 0.040 Uiso 1 1 calc R . . C21 C -0.4241(4) -0.0688(3) 0.34805(19) 0.0379(8) Uani 1 1 d . . . H27 H -0.4172 -0.1527 0.3621 0.045 Uiso 1 1 calc R . . C22 C -0.5369(4) 0.0286(3) 0.37063(18) 0.0357(8) Uani 1 1 d . . . H28 H -0.6036 0.0111 0.4007 0.043 Uiso 1 1 calc R . . C23 C -0.5516(3) 0.1535(3) 0.34859(16) 0.0288(7) Uani 1 1 d . . . N3 N -0.6642(3) 0.2569(3) 0.36629(13) 0.0298(6) Uani 1 1 d . . . C24 C -0.6756(3) 0.3802(3) 0.34810(15) 0.0281(7) Uani 1 1 d . . . C25 C -0.7836(3) 0.4827(3) 0.37073(17) 0.0341(7) Uani 1 1 d . . . H29 H -0.8518 0.4698 0.4018 0.041 Uiso 1 1 calc R . . C26 C -0.7912(3) 0.6035(3) 0.34783(17) 0.0370(8) Uani 1 1 d . . . H30 H -0.8657 0.6723 0.3640 0.044 Uiso 1 1 calc R . . C27 C -0.6961(3) 0.6294(3) 0.30263(17) 0.0335(7) Uani 1 1 d . . . H31 H -0.7060 0.7142 0.2876 0.040 Uiso 1 1 calc R . . C28 C -0.5855(3) 0.5287(3) 0.27963(15) 0.0291(7) Uani 1 1 d . . . N4 N -0.4850(3) 0.5474(2) 0.23472(14) 0.0372(7) Uani 1 1 d . . . C29 C -0.3750(3) 0.4480(3) 0.21057(15) 0.0286(7) Uani 1 1 d . . . C30 C -0.2774(3) 0.4681(3) 0.16365(16) 0.0296(7) Uani 1 1 d . . . H32 H -0.2872 0.5519 0.1447 0.035 Uiso 1 1 calc R . . C31 C -0.1664(3) 0.3650(3) 0.14500(16) 0.0293(7) Uani 1 1 d . . . H33 H -0.1007 0.3800 0.1127 0.035 Uiso 1 1 calc R . . C32 C -0.1461(3) 0.2409(3) 0.17106(16) 0.0277(6) Uani 1 1 d . . . H34 H -0.0670 0.1724 0.1578 0.033 Uiso 1 1 calc R . . C33 C -0.2436(3) 0.2173(3) 0.21720(15) 0.0251(6) Uani 1 1 d . . . N5 N -0.2283(3) 0.0954(2) 0.24576(13) 0.0263(5) Uani 1 1 d . . . C34 C -0.3306(3) 0.0715(3) 0.28558(16) 0.0268(6) Uani 1 1 d . . . C35 C -0.4467(3) 0.1748(3) 0.30546(15) 0.0249(6) Uani 1 1 d . . . C36 C -0.3604(3) 0.3221(3) 0.23613(15) 0.0242(6) Uani 1 1 d . . . C37 C -0.4603(3) 0.3001(3) 0.28158(15) 0.0238(6) Uani 1 1 d . . . C38 C -0.5737(3) 0.4032(3) 0.30289(15) 0.0259(6) Uani 1 1 d . . . C39 C -0.0975(3) -0.0118(3) 0.23441(17) 0.0297(7) Uani 1 1 d . . . H35 H -0.0844 -0.0839 0.2742 0.036 Uiso 1 1 calc R . . H36 H -0.0246 0.0142 0.2353 0.036 Uiso 1 1 calc R . . C40 C -0.0852(3) -0.0565(3) 0.16536(17) 0.0336(7) Uani 1 1 d . . . H37 H -0.1104 0.0171 0.1256 0.040 Uiso 1 1 calc R . . H38 H -0.1475 -0.0959 0.1670 0.040 Uiso 1 1 calc R . . C41 C 0.0583(4) -0.1523(3) 0.1530(2) 0.0423(9) Uani 1 1 d . . . H39 H 0.1204 -0.1147 0.1543 0.063 Uiso 1 1 calc R . . H40 H 0.0667 -0.1758 0.1066 0.063 Uiso 1 1 calc R . . H41 H 0.0804 -0.2282 0.1902 0.063 Uiso 1 1 calc R . . C42 C -0.7780(3) 0.2354(3) 0.40499(16) 0.0345(7) Uani 1 1 d . . . H42 H -0.7819 0.1628 0.3904 0.041 Uiso 1 1 calc R . . H43 H -0.8629 0.3115 0.3912 0.041 Uiso 1 1 calc R . . C43 C -0.7688(4) 0.2085(4) 0.48547(17) 0.0410(8) Uani 1 1 d . . . H44 H -0.6925 0.1252 0.5007 0.049 Uiso 1 1 calc R . . H45 H -0.7524 0.2746 0.5002 0.049 Uiso 1 1 calc R . . C44 C -0.8988(4) 0.2074(4) 0.5204(2) 0.0579(12) Uani 1 1 d . . . H46 H -0.9724 0.2927 0.5095 0.087 Uiso 1 1 calc R . . H47 H -0.8890 0.1815 0.5719 0.087 Uiso 1 1 calc R . . H48 H -0.9189 0.1473 0.5024 0.087 Uiso 1 1 calc R . . C45 C -0.4834(5) 0.6789(4) 0.2173(2) 0.0703(15) Uani 1 1 d . . . H49 H -0.5333 0.7273 0.2554 0.084 Uiso 1 1 calc R . . H50 H -0.3893 0.6681 0.2156 0.084 Uiso 1 1 calc R . . C46 C -0.5442(5) 0.7496(4) 0.1500(3) 0.0631(12) Uani 1 1 d . . . H51 H -0.6407 0.7678 0.1517 0.076 Uiso 1 1 calc R . . H52 H -0.4975 0.7021 0.1112 0.076 Uiso 1 1 calc R . . C47 C -0.5263(7) 0.8752(4) 0.1394(4) 0.106(3) Uani 1 1 d . . . H53 H -0.6050 0.9393 0.1600 0.159 Uiso 1 1 calc R . . H54 H -0.5175 0.9066 0.0886 0.159 Uiso 1 1 calc R . . H55 H -0.4451 0.8582 0.1630 0.159 Uiso 1 1 calc R . . C48 C 0.1757(5) 0.1919(4) -0.0300(2) 0.0616(12) Uani 1 1 d . . . H56 H 0.2671 0.1353 -0.0457 0.074 Uiso 1 1 calc R . . H57 H 0.1198 0.2332 -0.0724 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.10723(14) 0.09973(11) 0.02876(7) 0.0786(4) Uani 1 1 d . . . Cl2 Cl 0.1862(2) 0.30787(19) 0.00566(8) 0.1051(6) Uani 1 1 d . . . Cl3 Cl 0.21249(8) -0.00008(7) 0.27965(5) 0.0360(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 C1 0.047(2) 0.046(2) 0.066(3) -0.012(2) 0.023(2) -0.0141(19) C2 0.0345(19) 0.0443(19) 0.0377(18) -0.0104(16) 0.0090(15) -0.0227(16) C3 0.0339(18) 0.0389(17) 0.0280(15) -0.0087(14) 0.0005(13) -0.0227(15) C4 0.044(2) 0.0383(18) 0.0380(19) -0.0011(16) -0.0039(16) -0.0168(17) C5 0.0346(18) 0.0353(17) 0.0290(15) -0.0077(14) 0.0069(13) -0.0231(15) C6 0.0314(17) 0.0357(16) 0.0234(14) -0.0080(13) 0.0019(12) -0.0202(14) C7 0.0344(18) 0.0331(16) 0.0238(14) -0.0077(13) 0.0006(12) -0.0218(14) N1 0.0370(16) 0.0331(14) 0.0321(14) -0.0057(12) 0.0042(12) -0.0223(13) C8 0.0335(18) 0.0356(17) 0.0355(17) -0.0130(14) 0.0042(14) -0.0182(15) C9 0.0330(17) 0.0350(16) 0.0207(14) -0.0022(13) -0.0032(12) -0.0213(14) C10 0.0320(18) 0.0329(16) 0.0293(15) -0.0006(13) -0.0003(13) -0.0199(14) C11 0.0316(17) 0.0338(16) 0.0217(14) -0.0001(13) -0.0057(12) -0.0204(14) C12 0.0333(17) 0.0344(16) 0.0232(14) -0.0015(13) -0.0018(12) -0.0209(14) N2 0.0378(16) 0.0347(14) 0.0274(13) -0.0028(11) 0.0019(11) -0.0234(13) C13 0.050(2) 0.0409(18) 0.0273(16) 0.0017(14) -0.0008(15) -0.0324(18) C14 0.041(2) 0.0471(19) 0.0225(14) 0.0008(14) -0.0011(13) -0.0312(17) C15 0.049(2) 0.057(2) 0.0328(17) -0.0012(16) 0.0037(16) -0.039(2) C16 0.066(3) 0.077(3) 0.0297(18) -0.0033(19) 0.0094(18) -0.049(2) C17 0.0349(18) 0.0454(18) 0.0210(14) -0.0026(14) -0.0014(12) -0.0265(16) C18 0.0331(18) 0.0424(19) 0.0287(16) -0.0017(15) 0.0015(14) -0.0188(16) C19 0.048(2) 0.044(2) 0.0398(19) -0.0105(17) 0.0034(17) -0.0204(18) O1 0.0451(14) 0.0320(12) 0.0376(12) -0.0109(10) 0.0154(11) -0.0251(11) O2 0.0404(14) 0.0333(12) 0.0324(12) -0.0070(10) 0.0110(10) -0.0217(11) B1 0.035(2) 0.0352(19) 0.0315(18) -0.0034(16) 0.0022(15) -0.0231(17) F1 0.0332(11) 0.0324(10) 0.0464(11) -0.0137(9) 0.0066(9) -0.0170(9) F2 0.0516(14) 0.0715(15) 0.0374(11) 0.0150(10) -0.0110(9) -0.0433(12) C20 0.0330(18) 0.0295(16) 0.0385(18) -0.0074(14) 0.0017(14) -0.0157(14) C21 0.047(2) 0.0296(16) 0.0434(19) -0.0053(15) 0.0025(16) -0.0243(16) C22 0.0378(19) 0.0409(18) 0.0370(17) -0.0071(15) 0.0042(15) -0.0261(16) C23 0.0292(17) 0.0373(17) 0.0254(14) -0.0076(13) 0.0008(12) -0.0190(14) N3 0.0248(14) 0.0412(15) 0.0260(13) -0.0063(12) 0.0018(10) -0.0171(12) C24 0.0272(17) 0.0367(17) 0.0208(14) -0.0046(13) -0.0037(12) -0.0138(14) C25 0.0256(17) 0.0431(19) 0.0277(15) -0.0082(14) 0.0020(13) -0.0095(15) C26 0.0286(18) 0.0399(18) 0.0321(17) -0.0102(15) -0.0022(14) -0.0036(15) C27 0.0336(18) 0.0320(16) 0.0281(16) -0.0070(14) -0.0041(13) -0.0066(14) C28 0.0310(17) 0.0284(15) 0.0225(14) -0.0025(13) -0.0015(12) -0.0088(14) N4 0.0439(18) 0.0262(13) 0.0319(14) -0.0026(12) 0.0099(13) -0.0106(13) C29 0.0336(18) 0.0272(15) 0.0231(14) -0.0045(13) 0.0015(13) -0.0120(14) C30 0.0371(18) 0.0287(15) 0.0244(14) -0.0032(13) 0.0023(13) -0.0172(14) C31 0.0322(17) 0.0365(17) 0.0260(15) -0.0082(13) 0.0038(13) -0.0209(15) C32 0.0259(16) 0.0306(15) 0.0287(15) -0.0096(13) 0.0029(12) -0.0131(13) C33 0.0279(16) 0.0275(15) 0.0233(14) -0.0046(12) -0.0016(12) -0.0147(13) N5 0.0249(14) 0.0241(12) 0.0307(13) -0.0063(11) 0.0014(11) -0.0113(11) C34 0.0279(16) 0.0284(15) 0.0275(15) -0.0055(13) 0.0000(12) -0.0152(13) C35 0.0253(16) 0.0283(15) 0.0234(14) -0.0061(12) -0.0020(12) -0.0127(13) C36 0.0274(16) 0.0265(14) 0.0202(13) -0.0039(12) -0.0005(11) -0.0133(13) C37 0.0242(15) 0.0274(14) 0.0200(13) -0.0041(12) -0.0034(11) -0.0108(13) C38 0.0246(16) 0.0307(15) 0.0207(14) -0.0061(12) -0.0012(12) -0.0096(13) C39 0.0265(16) 0.0292(15) 0.0337(16) -0.0055(13) -0.0007(13) -0.0126(13) C40 0.0357(19) 0.0318(16) 0.0358(17) -0.0102(14) 0.0032(14) -0.0159(15) C41 0.040(2) 0.0328(17) 0.049(2) -0.0114(16) 0.0091(17) -0.0121(16) C42 0.0269(17) 0.053(2) 0.0287(16) -0.0075(15) 0.0037(13) -0.0224(16) C43 0.042(2) 0.049(2) 0.0305(17) -0.0046(16) 0.0025(15) -0.0207(18) C44 0.051(3) 0.071(3) 0.042(2) 0.001(2) 0.0152(19) -0.028(2) C45 0.063(3) 0.052(2) 0.054(3) 0.004(2) 0.031(2) -0.003(2) C46 0.056(3) 0.058(3) 0.072(3) -0.018(2) -0.005(2) -0.019(2) C47 0.122(5) 0.038(2) 0.147(6) -0.032(3) 0.081(4) -0.041(3) C48 0.077(3) 0.056(3) 0.048(2) -0.007(2) 0.019(2) -0.032(2) Cl1 0.0893(9) 0.0503(6) 0.0667(7) 0.0013(6) 0.0346(7) -0.0191(6) Cl2 0.1470(16) 0.1557(15) 0.0731(9) -0.0291(9) -0.0153(9) -0.1119(14) Cl3 0.0342(4) 0.0323(4) 0.0438(5) -0.0029(3) -0.0004(3) -0.0185(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.497(5) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 C3 1.498(4) . ? C2 H4 0.9900 . ? C2 H5 0.9900 . ? C3 C8 1.388(4) . ? C3 C6 1.406(5) . ? C4 C5 1.520(5) . ? C4 H6 0.9800 . ? C4 H7 0.9800 . ? C4 H8 0.9800 . ? C5 C6 1.492(4) . ? C5 H9 0.9900 . ? C5 H10 0.9900 . ? C6 C7 1.401(4) . ? C7 N1 1.381(4) . ? C7 C9 1.431(4) . ? N1 C8 1.349(4) . ? N1 H11 0.8800 . ? C8 H12 0.9500 . ? C9 O1 1.318(4) . ? C9 C10 1.385(4) . ? C10 C11 1.370(4) . ? C10 H13 0.9500 . ? C11 O2 1.316(4) . ? C11 C12 1.433(4) . ? C12 N2 1.383(4) . ? C12 C17 1.400(4) . ? N2 C13 1.352(4) . ? N2 H14 0.8800 . ? C13 C14 1.378(5) . ? C13 H15 0.9500 . ? C14 C17 1.410(4) . ? C14 C15 1.505(4) . ? C15 C16 1.519(5) . ? C15 H16 0.9900 . ? C15 H17 0.9900 . ? C16 H18 0.9800 . ? C16 H19 0.9800 . ? C16 H20 0.9800 . ? C17 C18 1.498(5) . ? C18 C19 1.514(5) . ? C18 H21 0.9900 . ? C18 H22 0.9900 . ? C19 H23 0.9800 . ? C19 H24 0.9800 . ? C19 H25 0.9800 . ? O1 B1 1.481(4) . ? O2 B1 1.483(4) . ? B1 F1 1.373(4) . ? B1 F2 1.378(4) . ? C20 C21 1.376(4) . ? C20 C34 1.401(4) . ? C20 H26 0.9500 . ? C21 C22 1.379(5) . ? C21 H27 0.9500 . ? C22 C23 1.400(4) . ? C22 H28 0.9500 . ? C23 N3 1.382(4) . ? C23 C35 1.427(4) . ? N3 C24 1.390(4) . ? N3 C42 1.477(4) . ? C24 C25 1.388(5) . ? C24 C38 1.426(4) . ? C25 C26 1.381(5) . ? C25 H29 0.9500 . ? C26 C27 1.382(5) . ? C26 H30 0.9500 . ? C27 C28 1.392(4) . ? C27 H31 0.9500 . ? C28 N4 1.391(4) . ? C28 C38 1.419(4) . ? N4 C29 1.389(4) . ? N4 C45 1.542(5) . ? C29 C30 1.392(4) . ? C29 C36 1.418(4) . ? C30 C31 1.379(5) . ? C30 H32 0.9500 . ? C31 C32 1.381(4) . ? C31 H33 0.9500 . ? C32 C33 1.399(4) . ? C32 H34 0.9500 . ? C33 N5 1.381(4) . ? C33 C36 1.422(4) . ? N5 C34 1.389(4) . ? N5 C39 1.478(4) . ? C34 C35 1.415(4) . ? C35 C37 1.411(4) . ? C36 C37 1.407(4) . ? C37 C38 1.409(4) . ? C39 C40 1.513(4) . ? C39 H35 0.9900 . ? C39 H36 0.9900 . ? C40 C41 1.519(5) . ? C40 H37 0.9900 . ? C40 H38 0.9900 . ? C41 H39 0.9800 . ? C41 H40 0.9800 . ? C41 H41 0.9800 . ? C42 C43 1.525(4) . ? C42 H42 0.9900 . ? C42 H43 0.9900 . ? C43 C44 1.516(5) . ? C43 H44 0.9900 . ? C43 H45 0.9900 . ? C44 H46 0.9800 . ? C44 H47 0.9800 . ? C44 H48 0.9800 . ? C45 C46 1.448(6) . ? C45 H49 0.9900 . ? C45 H50 0.9900 . ? C46 C47 1.567(6) . ? C46 H51 0.9900 . ? C46 H52 0.9900 . ? C47 H53 0.9800 . ? C47 H54 0.9800 . ? C47 H55 0.9800 . ? C48 Cl2 1.731(5) . ? C48 Cl1 1.747(4) . ? C48 H56 0.9900 . ? C48 H57 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C1 C2 C3 113.7(3) . . ? C1 C2 H4 108.8 . . ? C3 C2 H4 108.8 . . ? C1 C2 H5 108.8 . . ? C3 C2 H5 108.8 . . ? H4 C2 H5 107.7 . . ? C8 C3 C6 107.1(3) . . ? C8 C3 C2 126.1(3) . . ? C6 C3 C2 126.8(3) . . ? C5 C4 H6 109.5 . . ? C5 C4 H7 109.5 . . ? H6 C4 H7 109.5 . . ? C5 C4 H8 109.5 . . ? H6 C4 H8 109.5 . . ? H7 C4 H8 109.5 . . ? C6 C5 C4 111.3(3) . . ? C6 C5 H9 109.4 . . ? C4 C5 H9 109.4 . . ? C6 C5 H10 109.4 . . ? C4 C5 H10 109.4 . . ? H9 C5 H10 108.0 . . ? C7 C6 C3 107.1(3) . . ? C7 C6 C5 127.7(3) . . ? C3 C6 C5 124.9(3) . . ? N1 C7 C6 107.5(3) . . ? N1 C7 C9 120.8(3) . . ? C6 C7 C9 131.6(3) . . ? C8 N1 C7 109.3(3) . . ? C8 N1 H11 125.4 . . ? C7 N1 H11 125.4 . . ? N1 C8 C3 109.0(3) . . ? N1 C8 H12 125.5 . . ? C3 C8 H12 125.5 . . ? O1 C9 C10 120.4(3) . . ? O1 C9 C7 117.5(2) . . ? C10 C9 C7 122.1(3) . . ? C11 C10 C9 121.2(3) . . ? C11 C10 H13 119.4 . . ? C9 C10 H13 119.4 . . ? O2 C11 C10 120.7(3) . . ? O2 C11 C12 116.7(3) . . ? C10 C11 C12 122.6(3) . . ? N2 C12 C17 108.0(3) . . ? N2 C12 C11 119.7(3) . . ? C17 C12 C11 132.3(3) . . ? C13 N2 C12 108.5(3) . . ? C13 N2 H14 125.7 . . ? C12 N2 H14 125.7 . . ? N2 C13 C14 109.6(3) . . ? N2 C13 H15 125.2 . . ? C14 C13 H15 125.2 . . ? C13 C14 C17 107.3(3) . . ? C13 C14 C15 125.2(3) . . ? C17 C14 C15 127.5(3) . . ? C14 C15 C16 112.7(3) . . ? C14 C15 H16 109.0 . . ? C16 C15 H16 109.1 . . ? C14 C15 H17 109.0 . . ? C16 C15 H17 109.0 . . ? H16 C15 H17 107.8 . . ? C15 C16 H18 109.5 . . ? C15 C16 H19 109.5 . . ? H18 C16 H19 109.5 . . ? C15 C16 H20 109.5 . . ? H18 C16 H20 109.5 . . ? H19 C16 H20 109.5 . . ? C12 C17 C14 106.7(3) . . ? C12 C17 C18 127.1(3) . . ? C14 C17 C18 126.2(3) . . ? C17 C18 C19 113.3(3) . . ? C17 C18 H21 108.9 . . ? C19 C18 H21 108.9 . . ? C17 C18 H22 108.9 . . ? C19 C18 H22 108.9 . . ? H21 C18 H22 107.7 . . ? C18 C19 H23 109.5 . . ? C18 C19 H24 109.5 . . ? H23 C19 H24 109.5 . . ? C18 C19 H25 109.5 . . ? H23 C19 H25 109.5 . . ? H24 C19 H25 109.5 . . ? C9 O1 B1 121.6(2) . . ? C11 O2 B1 121.7(3) . . ? F1 B1 F2 110.3(3) . . ? F1 B1 O1 108.8(3) . . ? F2 B1 O1 108.6(3) . . ? F1 B1 O2 107.7(3) . . ? F2 B1 O2 109.3(3) . . ? O1 B1 O2 112.2(3) . . ? C21 C20 C34 118.3(3) . . ? C21 C20 H26 120.9 . . ? C34 C20 H26 120.9 . . ? C20 C21 C22 124.1(3) . . ? C20 C21 H27 118.0 . . ? C22 C21 H27 118.0 . . ? C21 C22 C23 119.0(3) . . ? C21 C22 H28 120.5 . . ? C23 C22 H28 120.5 . . ? N3 C23 C22 122.6(3) . . ? N3 C23 C35 118.9(3) . . ? C22 C23 C35 118.5(3) . . ? C23 N3 C24 122.7(2) . . ? C23 N3 C42 118.6(3) . . ? C24 N3 C42 118.7(3) . . ? C25 C24 N3 122.8(3) . . ? C25 C24 C38 118.5(3) . . ? N3 C24 C38 118.7(3) . . ? C26 C25 C24 119.5(3) . . ? C26 C25 H29 120.2 . . ? C24 C25 H29 120.2 . . ? C25 C26 C27 123.4(3) . . ? C25 C26 H30 118.3 . . ? C27 C26 H30 118.3 . . ? C26 C27 C28 118.6(3) . . ? C26 C27 H31 120.7 . . ? C28 C27 H31 120.7 . . ? N4 C28 C27 121.8(3) . . ? N4 C28 C38 118.8(3) . . ? C27 C28 C38 119.4(3) . . ? C29 N4 C28 122.4(3) . . ? C29 N4 C45 117.1(3) . . ? C28 N4 C45 120.1(3) . . ? N4 C29 C30 122.0(3) . . ? N4 C29 C36 118.7(3) . . ? C30 C29 C36 119.2(3) . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H32 120.4 . . ? C29 C30 H32 120.4 . . ? C30 C31 C32 123.1(3) . . ? C30 C31 H33 118.5 . . ? C32 C31 H33 118.5 . . ? C31 C32 C33 119.1(3) . . ? C31 C32 H34 120.4 . . ? C33 C32 H34 120.4 . . ? N5 C33 C32 121.9(3) . . ? N5 C33 C36 119.2(2) . . ? C32 C33 C36 118.9(3) . . ? C33 N5 C34 122.0(3) . . ? C33 N5 C39 118.3(2) . . ? C34 N5 C39 119.7(2) . . ? N5 C34 C20 121.5(3) . . ? N5 C34 C35 118.9(3) . . ? C20 C34 C35 119.5(3) . . ? C37 C35 C34 119.9(3) . . ? C37 C35 C23 119.5(3) . . ? C34 C35 C23 120.5(3) . . ? C37 C36 C29 120.1(3) . . ? C37 C36 C33 119.6(3) . . ? C29 C36 C33 120.3(3) . . ? C36 C37 C38 119.9(3) . . ? C36 C37 C35 119.8(3) . . ? C38 C37 C35 120.3(3) . . ? C37 C38 C28 119.9(3) . . ? C37 C38 C24 119.5(3) . . ? C28 C38 C24 120.6(3) . . ? N5 C39 C40 113.9(3) . . ? N5 C39 H35 108.8 . . ? C40 C39 H35 108.8 . . ? N5 C39 H36 108.8 . . ? C40 C39 H36 108.8 . . ? H35 C39 H36 107.7 . . ? C39 C40 C41 110.2(3) . . ? C39 C40 H37 109.6 . . ? C41 C40 H37 109.6 . . ? C39 C40 H38 109.6 . . ? C41 C40 H38 109.6 . . ? H37 C40 H38 108.1 . . ? C40 C41 H39 109.5 . . ? C40 C41 H40 109.5 . . ? H39 C41 H40 109.5 . . ? C40 C41 H41 109.5 . . ? H39 C41 H41 109.5 . . ? H40 C41 H41 109.5 . . ? N3 C42 C43 113.7(3) . . ? N3 C42 H42 108.8 . . ? C43 C42 H42 108.8 . . ? N3 C42 H43 108.8 . . ? C43 C42 H43 108.8 . . ? H42 C42 H43 107.7 . . ? C44 C43 C42 109.8(3) . . ? C44 C43 H44 109.7 . . ? C42 C43 H44 109.7 . . ? C44 C43 H45 109.7 . . ? C42 C43 H45 109.7 . . ? H44 C43 H45 108.2 . . ? C43 C44 H46 109.5 . . ? C43 C44 H47 109.5 . . ? H46 C44 H47 109.5 . . ? C43 C44 H48 109.5 . . ? H46 C44 H48 109.5 . . ? H47 C44 H48 109.5 . . ? C46 C45 N4 111.0(4) . . ? C46 C45 H49 109.4 . . ? N4 C45 H49 109.4 . . ? C46 C45 H50 109.4 . . ? N4 C45 H50 109.4 . . ? H49 C45 H50 108.0 . . ? C45 C46 C47 103.8(5) . . ? C45 C46 H51 111.0 . . ? C47 C46 H51 111.0 . . ? C45 C46 H52 111.0 . . ? C47 C46 H52 111.0 . . ? H51 C46 H52 109.0 . . ? C46 C47 H53 109.5 . . ? C46 C47 H54 109.5 . . ? H53 C47 H54 109.5 . . ? C46 C47 H55 109.5 . . ? H53 C47 H55 109.5 . . ? H54 C47 H55 109.5 . . ? Cl2 C48 Cl1 114.0(2) . . ? Cl2 C48 H56 108.8 . . ? Cl1 C48 H56 108.8 . . ? Cl2 C48 H57 108.8 . . ? Cl1 C48 H57 108.8 . . ? H56 C48 H57 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C8 12.7(5) . . . . ? C1 C2 C3 C6 -164.4(4) . . . . ? C8 C3 C6 C7 -1.3(4) . . . . ? C2 C3 C6 C7 176.2(3) . . . . ? C8 C3 C6 C5 -175.6(3) . . . . ? C2 C3 C6 C5 1.9(5) . . . . ? C4 C5 C6 C7 -82.9(4) . . . . ? C4 C5 C6 C3 90.2(4) . . . . ? C3 C6 C7 N1 1.1(3) . . . . ? C5 C6 C7 N1 175.3(3) . . . . ? C3 C6 C7 C9 -176.3(3) . . . . ? C5 C6 C7 C9 -2.2(5) . . . . ? C6 C7 N1 C8 -0.6(4) . . . . ? C9 C7 N1 C8 177.2(3) . . . . ? C7 N1 C8 C3 -0.2(4) . . . . ? C6 C3 C8 N1 0.9(4) . . . . ? C2 C3 C8 N1 -176.6(3) . . . . ? N1 C7 C9 O1 174.3(3) . . . . ? C6 C7 C9 O1 -8.5(5) . . . . ? N1 C7 C9 C10 -4.2(5) . . . . ? C6 C7 C9 C10 173.0(3) . . . . ? O1 C9 C10 C11 -5.0(5) . . . . ? C7 C9 C10 C11 173.4(3) . . . . ? C9 C10 C11 O2 6.0(5) . . . . ? C9 C10 C11 C12 -172.0(3) . . . . ? O2 C11 C12 N2 -177.3(3) . . . . ? C10 C11 C12 N2 0.8(5) . . . . ? O2 C11 C12 C17 4.2(5) . . . . ? C10 C11 C12 C17 -177.7(3) . . . . ? C17 C12 N2 C13 0.3(4) . . . . ? C11 C12 N2 C13 -178.6(3) . . . . ? C12 N2 C13 C14 -0.2(4) . . . . ? N2 C13 C14 C17 0.1(4) . . . . ? N2 C13 C14 C15 -178.8(3) . . . . ? C13 C14 C15 C16 98.2(4) . . . . ? C17 C14 C15 C16 -80.4(5) . . . . ? N2 C12 C17 C14 -0.2(3) . . . . ? C11 C12 C17 C14 178.5(3) . . . . ? N2 C12 C17 C18 178.4(3) . . . . ? C11 C12 C17 C18 -2.9(6) . . . . ? C13 C14 C17 C12 0.1(4) . . . . ? C15 C14 C17 C12 178.9(3) . . . . ? C13 C14 C17 C18 -178.5(3) . . . . ? C15 C14 C17 C18 0.3(5) . . . . ? C12 C17 C18 C19 -77.5(4) . . . . ? C14 C17 C18 C19 100.8(4) . . . . ? C10 C9 O1 B1 -6.8(4) . . . . ? C7 C9 O1 B1 174.8(3) . . . . ? C10 C11 O2 B1 4.8(4) . . . . ? C12 C11 O2 B1 -177.1(3) . . . . ? C9 O1 B1 F1 134.9(3) . . . . ? C9 O1 B1 F2 -105.0(3) . . . . ? C9 O1 B1 O2 15.8(4) . . . . ? C11 O2 B1 F1 -134.6(3) . . . . ? C11 O2 B1 F2 105.6(3) . . . . ? C11 O2 B1 O1 -14.9(4) . . . . ? C34 C20 C21 C22 -0.1(5) . . . . ? C20 C21 C22 C23 2.2(6) . . . . ? C21 C22 C23 N3 177.1(3) . . . . ? C21 C22 C23 C35 -2.1(5) . . . . ? C22 C23 N3 C24 176.0(3) . . . . ? C35 C23 N3 C24 -4.7(4) . . . . ? C22 C23 N3 C42 -5.1(4) . . . . ? C35 C23 N3 C42 174.1(3) . . . . ? C23 N3 C24 C25 -174.6(3) . . . . ? C42 N3 C24 C25 6.6(4) . . . . ? C23 N3 C24 C38 6.9(4) . . . . ? C42 N3 C24 C38 -171.9(3) . . . . ? N3 C24 C25 C26 -177.0(3) . . . . ? C38 C24 C25 C26 1.5(5) . . . . ? C24 C25 C26 C27 0.2(5) . . . . ? C25 C26 C27 C28 -1.0(5) . . . . ? C26 C27 C28 N4 -179.3(3) . . . . ? C26 C27 C28 C38 0.2(5) . . . . ? C27 C28 N4 C29 -179.1(3) . . . . ? C38 C28 N4 C29 1.4(5) . . . . ? C27 C28 N4 C45 8.5(5) . . . . ? C38 C28 N4 C45 -171.0(3) . . . . ? C28 N4 C29 C30 177.7(3) . . . . ? C45 N4 C29 C30 -9.7(5) . . . . ? C28 N4 C29 C36 -4.0(5) . . . . ? C45 N4 C29 C36 168.6(3) . . . . ? N4 C29 C30 C31 176.1(3) . . . . ? C36 C29 C30 C31 -2.3(5) . . . . ? C29 C30 C31 C32 -0.3(5) . . . . ? C30 C31 C32 C33 1.7(5) . . . . ? C31 C32 C33 N5 -179.1(3) . . . . ? C31 C32 C33 C36 -0.3(4) . . . . ? C32 C33 N5 C34 -173.2(3) . . . . ? C36 C33 N5 C34 8.0(4) . . . . ? C32 C33 N5 C39 8.1(4) . . . . ? C36 C33 N5 C39 -170.7(3) . . . . ? C33 N5 C34 C20 171.6(3) . . . . ? C39 N5 C34 C20 -9.8(4) . . . . ? C33 N5 C34 C35 -8.6(4) . . . . ? C39 N5 C34 C35 170.1(3) . . . . ? C21 C20 C34 N5 177.7(3) . . . . ? C21 C20 C34 C35 -2.1(5) . . . . ? N5 C34 C35 C37 3.4(4) . . . . ? C20 C34 C35 C37 -176.8(3) . . . . ? N5 C34 C35 C23 -177.6(3) . . . . ? C20 C34 C35 C23 2.2(5) . . . . ? N3 C23 C35 C37 -0.3(4) . . . . ? C22 C23 C35 C37 178.9(3) . . . . ? N3 C23 C35 C34 -179.3(3) . . . . ? C22 C23 C35 C34 0.0(4) . . . . ? N4 C29 C36 C37 3.9(4) . . . . ? C30 C29 C36 C37 -177.7(3) . . . . ? N4 C29 C36 C33 -174.8(3) . . . . ? C30 C29 C36 C33 3.6(4) . . . . ? N5 C33 C36 C37 -2.2(4) . . . . ? C32 C33 C36 C37 179.0(3) . . . . ? N5 C33 C36 C29 176.6(3) . . . . ? C32 C33 C36 C29 -2.2(4) . . . . ? C29 C36 C37 C38 -1.3(4) . . . . ? C33 C36 C37 C38 177.4(3) . . . . ? C29 C36 C37 C35 178.5(3) . . . . ? C33 C36 C37 C35 -2.8(4) . . . . ? C34 C35 C37 C36 2.1(4) . . . . ? C23 C35 C37 C36 -176.8(3) . . . . ? C34 C35 C37 C38 -178.1(3) . . . . ? C23 C35 C37 C38 3.0(4) . . . . ? C36 C37 C38 C28 -1.3(4) . . . . ? C35 C37 C38 C28 178.9(3) . . . . ? C36 C37 C38 C24 179.0(3) . . . . ? C35 C37 C38 C24 -0.8(4) . . . . ? N4 C28 C38 C37 1.3(4) . . . . ? C27 C28 C38 C37 -178.2(3) . . . . ? N4 C28 C38 C24 -179.0(3) . . . . ? C27 C28 C38 C24 1.4(5) . . . . ? C25 C24 C38 C37 177.4(3) . . . . ? N3 C24 C38 C37 -4.1(4) . . . . ? C25 C24 C38 C28 -2.3(4) . . . . ? N3 C24 C38 C28 176.3(3) . . . . ? C33 N5 C39 C40 -85.9(3) . . . . ? C34 N5 C39 C40 95.4(3) . . . . ? N5 C39 C40 C41 171.5(2) . . . . ? C23 N3 C42 C43 89.8(4) . . . . ? C24 N3 C42 C43 -91.3(4) . . . . ? N3 C42 C43 C44 171.6(3) . . . . ? C29 N4 C45 C46 89.4(4) . . . . ? C28 N4 C45 C46 -97.8(4) . . . . ? N4 C45 C46 C47 -176.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.406 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.070 # Attachment '4-TATACl.CIF' data_90513mae _database_code_depnum_ccdc_archive 'CCDC 845956' #TrackingRef '4-TATACl.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H100 B2 Cl N7 O4' _chemical_formula_weight 1400.84 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P - 1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.754(5) _cell_length_b 17.148(7) _cell_length_c 17.170(5) _cell_angle_alpha 116.501(12) _cell_angle_beta 108.051(10) _cell_angle_gamma 91.068(14) _cell_volume 3879(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9440 _exptl_absorpt_correction_T_max 0.9588 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36354 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.47 _reflns_number_total 17214 _reflns_number_gt 8285 _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^)+(0.1241P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17214 _refine_ls_number_parameters 989 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1546 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2435 _refine_ls_wR_factor_gt 0.2066 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 C1 C 0.1138(4) 0.9662(3) 0.7459(3) 0.107(2) Uani 1 1 d . . . H18 H 0.0731 0.9489 0.7708 0.160 Uiso 1 1 calc R . . H19 H 0.1389 1.0298 0.7846 0.160 Uiso 1 1 calc R . . H20 H 0.1634 0.9326 0.7464 0.160 Uiso 1 1 calc R . . C2 C 0.0615(3) 0.9469(3) 0.6474(3) 0.0832(15) Uani 1 1 d . . . H21 H 0.0128 0.9826 0.6481 0.100 Uiso 1 1 calc R . . H22 H 0.1030 0.9662 0.6236 0.100 Uiso 1 1 calc R . . C3 C 0.0194(3) 0.8508(2) 0.5813(2) 0.0599(11) Uani 1 1 d . . . C4 C 0.0311(2) 0.7806(3) 0.5992(2) 0.0581(10) Uani 1 1 d . . . H23 H 0.0661 0.7849 0.6576 0.070 Uiso 1 1 calc R . . C5 C -0.1594(3) 0.8936(3) 0.4440(3) 0.0773(13) Uani 1 1 d . . . H24 H -0.2061 0.8399 0.4110 0.116 Uiso 1 1 calc R . . H25 H -0.1767 0.9321 0.4155 0.116 Uiso 1 1 calc R . . H26 H -0.1540 0.9251 0.5095 0.116 Uiso 1 1 calc R . . C6 C -0.0691(3) 0.8684(2) 0.4378(2) 0.0586(10) Uani 1 1 d . . . H27 H -0.0758 0.8335 0.3715 0.070 Uiso 1 1 calc R . . H28 H -0.0236 0.9229 0.4659 0.070 Uiso 1 1 calc R . . C7 C -0.0360(2) 0.8152(2) 0.4867(2) 0.0490(9) Uani 1 1 d . . . C8 C -0.0573(2) 0.7241(2) 0.45087(19) 0.0411(8) Uani 1 1 d . . . C9 C -0.11170(19) 0.6559(2) 0.36018(19) 0.0367(7) Uani 1 1 d . . . C10 C -0.1163(2) 0.5671(2) 0.33399(19) 0.0383(7) Uani 1 1 d . . . H29 H -0.0754 0.5486 0.3734 0.046 Uiso 1 1 calc R . . C11 C -0.18096(19) 0.5039(2) 0.24934(19) 0.0348(7) Uani 1 1 d . . . C12 C -0.20340(19) 0.4146(2) 0.2283(2) 0.0361(7) Uani 1 1 d . . . C13 C -0.26079(19) 0.3400(2) 0.1483(2) 0.0429(8) Uani 1 1 d . . . C14 C -0.2566(2) 0.2696(2) 0.1683(3) 0.0540(9) Uani 1 1 d . . . C15 C -0.1983(2) 0.3018(2) 0.2594(3) 0.0530(9) Uani 1 1 d . . . H1 H -0.1834 0.2681 0.2915 0.064 Uiso 1 1 calc R . . C16 C -0.3047(3) 0.1750(3) 0.1046(3) 0.0781(13) Uani 1 1 d . . . H2 H -0.3246 0.1525 0.1414 0.094 Uiso 1 1 calc R . . H3 H -0.3600 0.1741 0.0566 0.094 Uiso 1 1 calc R . . C17 C -0.2537(4) 0.1163(4) 0.0592(4) 0.131(3) Uani 1 1 d . . . H4 H -0.2363 0.1358 0.0198 0.197 Uiso 1 1 calc R . . H5 H -0.2904 0.0565 0.0206 0.197 Uiso 1 1 calc R . . H6 H -0.1990 0.1159 0.1057 0.197 Uiso 1 1 calc R . . C18 C -0.3193(2) 0.3357(2) 0.0583(2) 0.0575(10) Uani 1 1 d . . . H7 H -0.3442 0.3910 0.0724 0.069 Uiso 1 1 calc R . . H8 H -0.3712 0.2859 0.0272 0.069 Uiso 1 1 calc R . . C19 C -0.2710(3) 0.3237(3) -0.0084(3) 0.0768(13) Uani 1 1 d . . . H9 H -0.2218 0.3745 0.0201 0.115 Uiso 1 1 calc R . . H10 H -0.3141 0.3195 -0.0659 0.115 Uiso 1 1 calc R . . H11 H -0.2458 0.2692 -0.0228 0.115 Uiso 1 1 calc R . . C20 C -0.2758(2) 0.6471(2) 0.14544(19) 0.0382(7) Uani 1 1 d . . . C21 C -0.2802(2) 0.7367(2) 0.1765(2) 0.0465(8) Uani 1 1 d . . . H12 H -0.2338 0.7795 0.2318 0.056 Uiso 1 1 calc R . . C22 C -0.3498(2) 0.7653(3) 0.1293(2) 0.0555(10) Uani 1 1 d . . . H13 H -0.3511 0.8268 0.1523 0.067 Uiso 1 1 calc R . . C23 C -0.4177(2) 0.7030(3) 0.0483(2) 0.0546(10) Uani 1 1 d . . . H14 H -0.4653 0.7218 0.0148 0.065 Uiso 1 1 calc R . . C24 C -0.4159(2) 0.6147(3) 0.0167(2) 0.0521(9) Uani 1 1 d . . . H15 H -0.4627 0.5721 -0.0383 0.063 Uiso 1 1 calc R . . C25 C -0.3458(2) 0.5871(2) 0.0648(2) 0.0431(8) Uani 1 1 d . . . H16 H -0.3457 0.5255 0.0419 0.052 Uiso 1 1 calc R . . C26 C -0.10511(19) 0.6124(2) 0.16741(18) 0.0382(7) Uani 1 1 d . . . C27 C -0.0658(2) 0.5374(2) 0.13636(19) 0.0428(8) Uani 1 1 d . . . H30 H -0.0925 0.4844 0.1312 0.051 Uiso 1 1 calc R . . C28 C 0.0105(2) 0.5371(3) 0.1128(2) 0.0492(9) Uani 1 1 d . . . H31 H 0.0351 0.4846 0.0919 0.059 Uiso 1 1 calc R . . C29 C 0.0506(2) 0.6124(3) 0.1194(2) 0.0554(9) Uani 1 1 d . . . H32 H 0.1032 0.6127 0.1036 0.067 Uiso 1 1 calc R . . C30 C 0.0133(2) 0.6882(3) 0.1494(3) 0.0570(10) Uani 1 1 d . . . H33 H 0.0405 0.7408 0.1542 0.068 Uiso 1 1 calc R . . C31 C -0.0629(2) 0.6878(2) 0.1723(2) 0.0483(8) Uani 1 1 d . . . H34 H -0.0876 0.7403 0.1920 0.058 Uiso 1 1 calc R . . C32 C 0.2342(3) 0.4789(3) 0.0937(2) 0.0588(10) Uani 1 1 d . . . H35 H 0.2141 0.5124 0.1460 0.088 Uiso 1 1 calc R . . H36 H 0.1990 0.4864 0.0402 0.088 Uiso 1 1 calc R . . H37 H 0.2989 0.5008 0.1117 0.088 Uiso 1 1 calc R . . C33 C 0.2199(2) 0.3817(3) 0.0676(2) 0.0524(9) Uani 1 1 d . . . H38 H 0.1541 0.3596 0.0464 0.063 Uiso 1 1 calc R . . H39 H 0.2403 0.3485 0.0146 0.063 Uiso 1 1 calc R . . C34 C 0.2695(2) 0.3628(2) 0.14606(19) 0.0403(8) Uani 1 1 d . . . C35 C 0.3280(2) 0.4250(2) 0.23253(19) 0.0385(7) Uani 1 1 d . . . H40 H 0.3449 0.4860 0.2516 0.046 Uiso 1 1 calc R . . C36 C 0.2628(2) 0.2822(2) 0.14703(19) 0.0436(8) Uani 1 1 d . . . C37 C 0.2039(3) 0.1969(3) 0.0665(2) 0.0721(13) Uani 1 1 d . . . H41 H 0.1856 0.1596 0.0911 0.086 Uiso 1 1 calc R . . H42 H 0.1480 0.2104 0.0325 0.086 Uiso 1 1 calc R . . C38 C 0.2488(4) 0.1461(3) 0.0007(3) 0.1050(19) Uani 1 1 d . . . H43 H 0.2653 0.1818 -0.0256 0.157 Uiso 1 1 calc R . . H44 H 0.2072 0.0913 -0.0496 0.157 Uiso 1 1 calc R . . H45 H 0.3037 0.1315 0.0335 0.157 Uiso 1 1 calc R . . C39 C 0.3187(2) 0.2968(2) 0.23490(19) 0.0379(7) Uani 1 1 d . . . C40 C 0.3397(2) 0.2395(2) 0.2755(2) 0.0398(7) Uani 1 1 d . . . C41 C 0.4108(2) 0.2649(2) 0.35872(19) 0.0396(7) Uani 1 1 d . . . H46 H 0.4535 0.3178 0.3852 0.047 Uiso 1 1 calc R . . C42 C 0.4202(2) 0.2142(2) 0.4035(2) 0.0443(8) Uani 1 1 d . . . C43 C 0.4908(2) 0.2410(2) 0.4914(2) 0.0443(8) Uani 1 1 d . B . C44 C 0.5214(3) 0.1941(2) 0.5397(2) 0.0547(10) Uani 1 1 d . B . C45 C 0.4799(3) 0.1049(3) 0.5183(3) 0.0753(13) Uani 1 1 d . . . H47 H 0.5272 0.0786 0.5468 0.090 Uiso 1 1 calc R . . H48 H 0.4568 0.0659 0.4501 0.090 Uiso 1 1 calc R . . C46 C 0.4022(4) 0.1088(3) 0.5546(3) 0.0904(15) Uani 1 1 d . . . H49 H 0.4251 0.1461 0.6224 0.136 Uiso 1 1 calc R . . H50 H 0.3768 0.0488 0.5389 0.136 Uiso 1 1 calc R . . H51 H 0.3547 0.1338 0.5259 0.136 Uiso 1 1 calc R . . C47 C 0.6024(3) 0.2469(3) 0.6137(3) 0.0646(12) Uani 1 1 d . . . C50 C 0.6176(3) 0.3239(3) 0.6099(2) 0.0544(10) Uani 1 1 d . B . H57 H 0.6673 0.3716 0.6520 0.065 Uiso 1 1 calc R . . O1 O -0.22615(13) 0.52679(14) 0.18644(13) 0.0372(5) Uani 1 1 d . . . O2 O -0.16071(13) 0.68282(14) 0.30261(12) 0.0384(5) Uani 1 1 d . . . O3 O 0.28735(15) 0.16124(14) 0.23086(15) 0.0518(6) Uani 1 1 d . . . O4 O 0.36475(18) 0.13811(15) 0.36596(15) 0.0561(6) Uani 1 1 d . . . N1 N -0.01425(19) 0.70474(19) 0.52182(17) 0.0494(7) Uani 1 1 d . . . H98 H -0.0163 0.6514 0.5170 0.059 Uiso 1 1 calc R . . N2 N -0.16633(16) 0.38775(18) 0.29472(18) 0.0408(6) Uani 1 1 d . . . H17 H -0.1277 0.4221 0.3515 0.049 Uiso 1 1 calc R . . N3 N 0.35776(16) 0.38520(16) 0.28608(15) 0.0358(6) Uani 1 1 d . . . H99 H 0.3958 0.4116 0.3441 0.043 Uiso 1 1 calc R . . N4 N 0.55034(18) 0.32048(18) 0.53640(16) 0.0444(7) Uani 1 1 d . . . H100 H 0.5453 0.3624 0.5199 0.053 Uiso 1 1 calc R B . B1 B -0.1921(2) 0.6160(2) 0.1988(2) 0.0378(8) Uani 1 1 d . . . B2 B 0.3131(3) 0.0917(3) 0.2610(3) 0.0567(11) Uani 1 1 d . . . Cl1 Cl 0.0000 0.5000 0.5000 0.0538(3) Uani 1 2 d S . . C51 C 0.2210(3) 0.0309(2) 0.2350(3) 0.0715(12) Uani 1 1 d . . . C52 C 0.2036(4) 0.0007(3) 0.2925(4) 0.1004(18) Uani 1 1 d . . . H58 H 0.2486 0.0182 0.3518 0.121 Uiso 1 1 calc R . . C53 C 0.1214(5) -0.0548(4) 0.2659(5) 0.122(2) Uani 1 1 d . . . H59 H 0.1115 -0.0752 0.3061 0.146 Uiso 1 1 calc R . . C54 C 0.0554(5) -0.0788(4) 0.1800(6) 0.125(2) Uani 1 1 d . . . H60 H 0.0002 -0.1171 0.1605 0.151 Uiso 1 1 calc R . . C55 C 0.0686(4) -0.0490(4) 0.1242(5) 0.112(2) Uani 1 1 d . . . H61 H 0.0220 -0.0642 0.0664 0.134 Uiso 1 1 calc R . . C56 C 0.1502(3) 0.0040(3) 0.1505(4) 0.0910(15) Uani 1 1 d . . . H62 H 0.1583 0.0232 0.1088 0.109 Uiso 1 1 calc R . . C57 C 0.3809(3) 0.0373(2) 0.2102(2) 0.0525(9) Uani 1 1 d . . . C58 C 0.4014(3) -0.0410(3) 0.2121(3) 0.0652(11) Uani 1 1 d . . . H63 H 0.3758 -0.0618 0.2442 0.078 Uiso 1 1 calc R . . C59 C 0.4576(3) -0.0892(3) 0.1688(3) 0.0746(13) Uani 1 1 d . . . H64 H 0.4688 -0.1428 0.1704 0.090 Uiso 1 1 calc R . . C60 C 0.4973(3) -0.0603(3) 0.1235(3) 0.0656(11) Uani 1 1 d . . . H65 H 0.5370 -0.0928 0.0949 0.079 Uiso 1 1 calc R . . C61 C 0.4789(3) 0.0164(3) 0.1202(2) 0.0582(10) Uani 1 1 d . . . H66 H 0.5057 0.0371 0.0887 0.070 Uiso 1 1 calc R . . C62 C 0.4211(2) 0.0637(2) 0.1628(2) 0.0531(9) Uani 1 1 d . . . H67 H 0.4088 0.1162 0.1592 0.064 Uiso 1 1 calc R . . C63 C 0.7808(2) 0.7420(2) 0.5540(3) 0.0609(10) Uani 1 1 d . . . H68 H 0.7927 0.8038 0.5747 0.073 Uiso 1 1 calc R . . C64 C 0.8235(2) 0.7109(3) 0.6144(3) 0.0601(10) Uani 1 1 d . . . H69 H 0.8637 0.7509 0.6755 0.072 Uiso 1 1 calc R . . C65 C 0.8077(2) 0.6211(2) 0.5854(2) 0.0535(9) Uani 1 1 d . A . C66 C 0.8371(2) 0.4945(3) 0.6122(2) 0.0535(9) Uani 1 1 d . A . C67 C 0.8851(3) 0.4583(3) 0.6668(3) 0.0645(11) Uani 1 1 d . . . H70 H 0.9278 0.4959 0.7274 0.077 Uiso 1 1 calc R . . C68 C 0.8709(3) 0.3696(3) 0.6334(2) 0.0608(10) Uani 1 1 d . . . H71 H 0.9066 0.3461 0.6706 0.073 Uiso 1 1 calc R . . C69 C 0.8068(3) 0.3110(3) 0.5475(2) 0.0588(10) Uani 1 1 d . . . H72 H 0.7980 0.2491 0.5272 0.071 Uiso 1 1 calc R . . C70 C 0.7556(2) 0.3445(2) 0.4917(2) 0.0494(9) Uani 1 1 d . A . C71 C 0.6404(2) 0.3236(2) 0.3480(2) 0.0444(8) Uani 1 1 d . A . C72 C 0.5740(2) 0.2688(2) 0.2620(2) 0.0508(9) Uani 1 1 d . . . H73 H 0.5580 0.2075 0.2421 0.061 Uiso 1 1 calc R . . C73 C 0.5314(2) 0.3046(2) 0.2058(2) 0.0462(8) Uani 1 1 d . . . H74 H 0.4859 0.2665 0.1472 0.055 Uiso 1 1 calc R . . C74 C 0.5515(2) 0.3923(2) 0.2302(2) 0.0449(8) Uani 1 1 d . . . H75 H 0.5205 0.4141 0.1892 0.054 Uiso 1 1 calc R . . C75 C 0.6185(2) 0.4494(2) 0.3165(2) 0.0405(7) Uani 1 1 d . A . C76 C 0.7025(2) 0.5970(2) 0.4333(2) 0.0465(8) Uani 1 1 d . A . C77 C 0.7209(2) 0.6873(2) 0.4642(3) 0.0579(10) Uani 1 1 d . . . H76 H 0.6929 0.7114 0.4245 0.069 Uiso 1 1 calc R . . C78 C 0.6139(2) 0.5704(3) 0.2712(3) 0.0596(10) Uani 1 1 d . . . H77 H 0.6624 0.6172 0.2848 0.072 Uiso 1 1 calc R . . H78 H 0.6035 0.5207 0.2085 0.072 Uiso 1 1 calc R . . C79 C 0.5298(3) 0.6061(3) 0.2728(3) 0.0661(11) Uani 1 1 d . . . H79 H 0.5396 0.6545 0.3361 0.079 Uiso 1 1 calc R . . H80 H 0.4807 0.5588 0.2570 0.079 Uiso 1 1 calc R . . C80 C 0.5021(3) 0.6411(3) 0.2039(2) 0.0596(10) Uani 1 1 d . . . H81 H 0.5490 0.6904 0.2220 0.089 Uiso 1 1 calc R . . H82 H 0.4444 0.6618 0.2033 0.089 Uiso 1 1 calc R . . H83 H 0.4947 0.5937 0.1417 0.089 Uiso 1 1 calc R . . C81 C 0.6499(3) 0.1993(4) 0.3892(3) 0.0820(15) Uani 1 1 d . . . H84 H 0.6570 0.1998 0.4488 0.098 Uiso 1 1 calc R . . H85 H 0.5845 0.1810 0.3503 0.098 Uiso 1 1 calc R . . C82 C 0.7000(3) 0.1381(4) 0.3424(3) 0.0892(16) Uani 1 1 d . . . H86 H 0.7658 0.1634 0.3722 0.107 Uiso 1 1 calc R . . H87 H 0.6801 0.1243 0.2763 0.107 Uiso 1 1 calc R . . C83 C 0.6802(3) 0.0507(3) 0.3503(3) 0.0812(14) Uani 1 1 d . . . H88 H 0.7127 0.0619 0.4141 0.122 Uiso 1 1 calc R . . H89 H 0.7009 0.0020 0.3071 0.122 Uiso 1 1 calc R . . H90 H 0.6148 0.0345 0.3345 0.122 Uiso 1 1 calc R . . C95 C 1.0282(3) 0.7267(4) 0.8803(3) 0.111(2) Uani 1 1 d . . . H107 H 1.0941 0.7449 0.9017 0.167 Uiso 0.588(12) 1 calc PR A 1 H108 H 1.0146 0.6910 0.9078 0.167 Uiso 0.588(12) 1 calc PR A 1 H109 H 1.0002 0.7795 0.8995 0.167 Uiso 0.588(12) 1 calc PR A 1 H110 H 1.0225 0.7549 0.9418 0.167 Uiso 0.412(12) 1 calc PR A 2 H111 H 1.0532 0.7721 0.8694 0.167 Uiso 0.412(12) 1 calc PR A 2 H112 H 1.0688 0.6838 0.8778 0.167 Uiso 0.412(12) 1 calc PR A 2 H101 H 1.0941 0.7449 0.9017 0.167 Uiso 0.588(12) 1 calc PR A 1 H102 H 1.0146 0.6910 0.9078 0.167 Uiso 0.588(12) 1 calc PR A 1 H103 H 1.0002 0.7795 0.8995 0.167 Uiso 0.588(12) 1 calc PR A 1 H104 H 1.0225 0.7549 0.9418 0.167 Uiso 0.412(12) 1 calc PR A 2 H105 H 1.0532 0.7721 0.8694 0.167 Uiso 0.412(12) 1 calc PR A 2 H106 H 1.0688 0.6838 0.8778 0.167 Uiso 0.412(12) 1 calc PR A 2 N5 N 0.6854(2) 0.2925(2) 0.4080(2) 0.0618(9) Uani 1 1 d . . . N6 N 0.8497(2) 0.5846(2) 0.6413(2) 0.0756(11) Uani 1 1 d . . . N7 N 0.64450(19) 0.53762(19) 0.34368(19) 0.0517(8) Uani 1 1 d . . . C87 C 0.72652(19) 0.4723(2) 0.4650(2) 0.0371(7) Uani 1 1 d . A . C88 C 0.7728(2) 0.4364(2) 0.5221(2) 0.0430(8) Uani 1 1 d . . . C89 C 0.7452(2) 0.5629(2) 0.4940(2) 0.0414(8) Uani 1 1 d . . . C90 C 0.66221(19) 0.4152(2) 0.37655(19) 0.0366(7) Uani 1 1 d . . . C91 C 0.8883(5) 0.6472(5) 0.7481(5) 0.054(2) Uani 0.588(12) 1 d P A 1 H113 H 0.8607 0.7011 0.7645 0.064 Uiso 0.588(12) 1 calc PR A 1 H114 H 0.8761 0.6168 0.7818 0.064 Uiso 0.588(12) 1 calc PR A 1 C92 C 0.9895(5) 0.6708(6) 0.7723(6) 0.064(2) Uani 0.588(12) 1 d P A 1 H115 H 1.0021 0.7059 0.7429 0.077 Uiso 0.588(12) 1 calc PR A 1 H116 H 1.0164 0.6167 0.7513 0.077 Uiso 0.588(12) 1 calc PR A 1 C93 C 0.9489(7) 0.6371(7) 0.7143(8) 0.048(3) Uani 0.412(12) 1 d P A 2 H117 H 0.9924 0.5960 0.7131 0.058 Uiso 0.412(12) 1 calc PR A 2 H118 H 0.9714 0.6823 0.7008 0.058 Uiso 0.412(12) 1 calc PR A 2 C94 C 0.9362(7) 0.6799(7) 0.8067(7) 0.061(3) Uani 0.412(12) 1 d P A 2 H119 H 0.9098 0.6344 0.8175 0.073 Uiso 0.412(12) 1 calc PR A 2 H120 H 0.8947 0.7227 0.8081 0.073 Uiso 0.412(12) 1 calc PR A 2 Cl2 Cl 0.5000 0.5000 0.5000 0.0400(3) Uani 1 2 d S . . C96 C 0.6495(10) 0.2053(9) 0.6760(12) 0.049(3) Uani 0.468(10) 1 d P B 3 H121 H 0.6087 0.1948 0.7054 0.059 Uiso 0.468(10) 1 calc PR B 3 H122 H 0.6645 0.1479 0.6381 0.059 Uiso 0.468(10) 1 calc PR B 3 C97 C 0.7321(7) 0.2675(7) 0.7470(7) 0.072(3) Uani 0.468(10) 1 d P B 3 H123 H 0.7701 0.2803 0.7170 0.109 Uiso 0.468(10) 1 calc PR B 3 H124 H 0.7655 0.2415 0.7851 0.109 Uiso 0.468(10) 1 calc PR B 3 H125 H 0.7161 0.3227 0.7867 0.109 Uiso 0.468(10) 1 calc PR B 3 C98 C 0.7390(5) 0.1822(6) 0.6641(6) 0.074(3) Uani 0.532(10) 1 d P B 4 H126 H 0.7047 0.1256 0.6101 0.111 Uiso 0.532(10) 1 calc PR B 4 H127 H 0.7752 0.1715 0.7150 0.111 Uiso 0.532(10) 1 calc PR B 4 H128 H 0.7793 0.2107 0.6471 0.111 Uiso 0.532(10) 1 calc PR B 4 C99 C 0.6760(11) 0.2397(9) 0.6942(12) 0.077(5) Uani 0.532(10) 1 d P B 4 H129 H 0.7111 0.2997 0.7416 0.092 Uiso 0.532(10) 1 calc PR B 4 H130 H 0.6452 0.2170 0.7242 0.092 Uiso 0.532(10) 1 calc PR B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.106(4) 0.079(4) 0.053(2) -0.007(2) -0.016(3) 0.018(3) C2 0.086(3) 0.053(3) 0.056(2) 0.0044(19) -0.010(2) 0.001(2) C3 0.065(2) 0.046(2) 0.0397(17) 0.0094(16) -0.0015(17) 0.0085(18) C4 0.064(2) 0.057(2) 0.0295(15) 0.0110(16) 0.0005(16) 0.0149(18) C5 0.098(3) 0.061(3) 0.067(2) 0.031(2) 0.020(2) 0.034(2) C6 0.076(3) 0.037(2) 0.0464(18) 0.0187(16) 0.0040(18) 0.0013(18) C7 0.0524(19) 0.037(2) 0.0405(17) 0.0132(15) 0.0027(16) 0.0045(15) C8 0.0459(17) 0.045(2) 0.0321(15) 0.0205(14) 0.0100(14) 0.0109(15) C9 0.0382(16) 0.0391(19) 0.0324(14) 0.0191(13) 0.0086(13) 0.0086(13) C10 0.0411(16) 0.0379(19) 0.0347(14) 0.0209(13) 0.0065(13) 0.0081(13) C11 0.0324(15) 0.0398(19) 0.0346(14) 0.0188(13) 0.0132(13) 0.0109(13) C12 0.0301(14) 0.0391(19) 0.0405(15) 0.0202(14) 0.0121(13) 0.0068(13) C13 0.0310(15) 0.041(2) 0.0503(18) 0.0187(15) 0.0111(14) 0.0069(14) C14 0.0386(17) 0.038(2) 0.077(2) 0.0254(18) 0.0137(18) 0.0004(15) C15 0.0449(19) 0.046(2) 0.073(2) 0.0381(19) 0.0128(18) 0.0025(16) C16 0.062(2) 0.040(2) 0.107(3) 0.027(2) 0.012(2) -0.0033(19) C17 0.089(4) 0.067(4) 0.124(4) -0.026(3) 0.005(3) -0.006(3) C18 0.0437(19) 0.046(2) 0.058(2) 0.0176(17) -0.0034(17) 0.0029(16) C19 0.075(3) 0.088(3) 0.054(2) 0.038(2) 0.000(2) 0.002(2) C20 0.0410(16) 0.044(2) 0.0338(15) 0.0209(14) 0.0145(14) 0.0122(14) C21 0.0443(18) 0.054(2) 0.0457(17) 0.0295(16) 0.0125(15) 0.0151(16) C22 0.051(2) 0.060(2) 0.059(2) 0.0341(19) 0.0146(18) 0.0239(18) C23 0.0427(18) 0.076(3) 0.056(2) 0.044(2) 0.0125(17) 0.0225(18) C24 0.0445(19) 0.063(3) 0.0445(18) 0.0281(18) 0.0068(16) 0.0122(17) C25 0.0432(17) 0.049(2) 0.0348(15) 0.0196(15) 0.0120(14) 0.0117(15) C26 0.0365(16) 0.045(2) 0.0259(13) 0.0179(13) -0.0001(13) 0.0095(14) C27 0.0398(17) 0.050(2) 0.0292(14) 0.0162(14) 0.0043(13) 0.0090(15) C28 0.0488(19) 0.060(2) 0.0397(16) 0.0248(16) 0.0156(15) 0.0191(17) C29 0.0449(19) 0.071(3) 0.060(2) 0.039(2) 0.0195(17) 0.0155(18) C30 0.051(2) 0.062(3) 0.067(2) 0.040(2) 0.0193(18) 0.0050(18) C31 0.0431(18) 0.052(2) 0.0516(18) 0.0284(17) 0.0138(16) 0.0127(16) C32 0.066(2) 0.073(3) 0.0477(19) 0.0381(19) 0.0167(18) 0.031(2) C33 0.050(2) 0.069(3) 0.0376(16) 0.0286(17) 0.0097(15) 0.0109(18) C34 0.0389(16) 0.045(2) 0.0326(14) 0.0170(14) 0.0098(13) 0.0061(14) C35 0.0396(16) 0.0347(18) 0.0376(15) 0.0178(14) 0.0082(14) 0.0074(13) C36 0.0447(18) 0.042(2) 0.0305(14) 0.0106(14) 0.0064(14) 0.0004(14) C37 0.102(3) 0.047(2) 0.0352(17) 0.0122(17) -0.002(2) -0.019(2) C38 0.137(5) 0.065(3) 0.052(2) -0.003(2) 0.005(3) 0.014(3) C39 0.0391(16) 0.0296(17) 0.0328(14) 0.0086(13) 0.0074(13) 0.0017(13) C40 0.0453(17) 0.0278(17) 0.0365(15) 0.0072(13) 0.0149(14) 0.0036(13) C41 0.0483(18) 0.0271(17) 0.0380(15) 0.0153(13) 0.0094(14) 0.0010(13) C42 0.068(2) 0.0231(17) 0.0402(16) 0.0115(13) 0.0226(16) 0.0100(15) C43 0.067(2) 0.0297(18) 0.0428(16) 0.0188(14) 0.0246(16) 0.0188(16) C44 0.085(3) 0.049(2) 0.052(2) 0.0328(18) 0.037(2) 0.034(2) C45 0.129(4) 0.055(3) 0.086(3) 0.053(2) 0.061(3) 0.047(3) C46 0.128(4) 0.074(3) 0.101(3) 0.056(3) 0.059(3) 0.023(3) C47 0.086(3) 0.075(3) 0.055(2) 0.042(2) 0.035(2) 0.054(2) C50 0.064(2) 0.060(3) 0.0374(17) 0.0224(16) 0.0158(17) 0.0343(19) O1 0.0353(10) 0.0394(13) 0.0331(10) 0.0179(9) 0.0061(9) 0.0091(9) O2 0.0425(11) 0.0380(13) 0.0321(10) 0.0177(9) 0.0081(9) 0.0113(9) O3 0.0592(14) 0.0262(13) 0.0481(12) 0.0065(10) 0.0094(11) -0.0047(10) O4 0.0900(18) 0.0242(13) 0.0522(13) 0.0134(10) 0.0305(13) 0.0033(12) N1 0.0599(17) 0.0462(18) 0.0340(13) 0.0188(12) 0.0064(13) 0.0156(14) N2 0.0343(13) 0.0437(17) 0.0501(14) 0.0293(13) 0.0116(12) 0.0051(12) N3 0.0383(13) 0.0293(14) 0.0292(11) 0.0115(10) 0.0028(11) 0.0022(11) N4 0.0580(16) 0.0376(17) 0.0373(13) 0.0188(12) 0.0145(13) 0.0206(13) B1 0.0369(18) 0.041(2) 0.0312(16) 0.0182(15) 0.0058(15) 0.0083(15) B2 0.081(3) 0.025(2) 0.051(2) 0.0107(17) 0.019(2) -0.002(2) Cl1 0.0706(8) 0.0543(8) 0.0382(6) 0.0285(5) 0.0110(6) 0.0195(6) C51 0.101(3) 0.025(2) 0.080(3) 0.0088(19) 0.046(3) 0.000(2) C52 0.147(5) 0.043(3) 0.102(4) 0.015(3) 0.063(3) -0.016(3) C53 0.182(6) 0.056(3) 0.134(5) 0.022(3) 0.103(5) -0.020(4) C54 0.147(6) 0.041(3) 0.148(6) -0.001(4) 0.074(5) -0.018(3) C55 0.104(4) 0.059(4) 0.137(5) 0.019(3) 0.041(4) -0.018(3) C56 0.093(3) 0.053(3) 0.094(3) 0.012(2) 0.029(3) -0.022(2) C57 0.067(2) 0.033(2) 0.0402(17) 0.0077(15) 0.0128(17) -0.0009(16) C58 0.094(3) 0.038(2) 0.059(2) 0.0213(18) 0.024(2) 0.011(2) C59 0.086(3) 0.050(3) 0.066(2) 0.018(2) 0.014(2) 0.024(2) C60 0.063(2) 0.059(3) 0.054(2) 0.015(2) 0.014(2) 0.019(2) C61 0.066(2) 0.047(2) 0.0449(18) 0.0127(16) 0.0119(18) 0.0039(18) C62 0.057(2) 0.036(2) 0.0459(18) 0.0086(15) 0.0102(17) 0.0023(16) C63 0.053(2) 0.036(2) 0.075(2) 0.0166(19) 0.014(2) 0.0078(17) C64 0.051(2) 0.047(2) 0.058(2) 0.0121(18) 0.0071(18) 0.0029(17) C65 0.054(2) 0.043(2) 0.0515(19) 0.0181(17) 0.0099(17) 0.0075(16) C66 0.052(2) 0.056(2) 0.0430(17) 0.0233(17) 0.0052(16) 0.0015(17) C67 0.063(2) 0.068(3) 0.049(2) 0.032(2) -0.0013(19) 0.001(2) C68 0.056(2) 0.071(3) 0.056(2) 0.041(2) 0.0052(19) 0.006(2) C69 0.064(2) 0.060(3) 0.060(2) 0.041(2) 0.0123(19) 0.0092(19) C70 0.055(2) 0.048(2) 0.0422(17) 0.0253(16) 0.0082(16) 0.0031(16) C71 0.0492(18) 0.045(2) 0.0406(16) 0.0239(15) 0.0123(15) 0.0059(15) C72 0.059(2) 0.040(2) 0.0437(17) 0.0178(15) 0.0097(17) 0.0015(16) C73 0.0420(17) 0.050(2) 0.0375(16) 0.0177(15) 0.0075(14) 0.0051(15) C74 0.0433(17) 0.049(2) 0.0402(16) 0.0221(15) 0.0100(15) 0.0111(15) C75 0.0363(16) 0.0384(19) 0.0443(16) 0.0199(14) 0.0108(14) 0.0072(14) C76 0.0410(17) 0.038(2) 0.0537(19) 0.0209(16) 0.0102(16) 0.0089(14) C77 0.051(2) 0.044(2) 0.066(2) 0.0250(18) 0.0073(18) 0.0079(17) C78 0.060(2) 0.059(3) 0.064(2) 0.0279(19) 0.0282(19) 0.0077(19) C79 0.068(2) 0.057(3) 0.071(2) 0.030(2) 0.022(2) 0.012(2) C80 0.068(2) 0.066(3) 0.059(2) 0.039(2) 0.0256(19) 0.030(2) C81 0.065(3) 0.118(4) 0.061(2) 0.043(3) 0.019(2) 0.009(3) C82 0.073(3) 0.123(5) 0.068(3) 0.045(3) 0.019(2) 0.028(3) C83 0.096(3) 0.047(3) 0.089(3) 0.041(2) 0.005(3) 0.007(2) C95 0.054(3) 0.137(5) 0.069(3) 0.007(3) -0.006(2) -0.001(3) N5 0.076(2) 0.0403(18) 0.0556(17) 0.0295(15) -0.0030(16) -0.0075(15) N6 0.087(2) 0.050(2) 0.0493(17) 0.0176(16) -0.0168(17) -0.0076(17) N7 0.0515(16) 0.0433(18) 0.0500(16) 0.0239(14) 0.0025(14) 0.0080(13) C87 0.0322(15) 0.042(2) 0.0387(15) 0.0184(14) 0.0162(13) 0.0098(13) C88 0.0431(17) 0.046(2) 0.0414(16) 0.0233(15) 0.0136(15) 0.0078(15) C89 0.0373(16) 0.042(2) 0.0416(16) 0.0171(14) 0.0134(14) 0.0100(14) C90 0.0350(15) 0.0407(19) 0.0375(15) 0.0194(14) 0.0157(13) 0.0087(13) C91 0.041(4) 0.061(5) 0.046(5) 0.013(4) 0.018(4) 0.012(3) C92 0.036(4) 0.083(6) 0.052(5) 0.016(4) 0.011(4) 0.004(4) C93 0.037(5) 0.051(6) 0.044(6) 0.018(5) 0.007(5) -0.003(4) C94 0.038(6) 0.067(7) 0.038(6) 0.003(5) -0.002(5) -0.005(5) Cl2 0.0462(6) 0.0284(6) 0.0324(5) 0.0098(4) 0.0049(5) 0.0031(4) C96 0.048(6) 0.055(9) 0.062(7) 0.040(7) 0.022(6) 0.025(6) C97 0.061(6) 0.086(8) 0.057(6) 0.037(5) -0.001(5) 0.025(5) C98 0.068(5) 0.081(7) 0.094(6) 0.061(5) 0.023(5) 0.035(5) C99 0.106(13) 0.054(9) 0.076(9) 0.051(8) 0.009(10) 0.025(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.509(6) . ? C1 H18 0.9800 . ? C1 H19 0.9800 . ? C1 H20 0.9800 . ? C2 C3 1.506(5) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C3 C4 1.372(5) . ? C3 C7 1.411(4) . ? C4 N1 1.342(4) . ? C4 H23 0.9500 . ? C5 C6 1.516(6) . ? C5 H24 0.9800 . ? C5 H25 0.9800 . ? C5 H26 0.9800 . ? C6 C7 1.497(5) . ? C6 H27 0.9900 . ? C6 H28 0.9900 . ? C7 C8 1.387(5) . ? C8 N1 1.383(4) . ? C8 C9 1.427(4) . ? C9 O2 1.317(3) . ? C9 C10 1.374(4) . ? C10 C11 1.400(4) . ? C10 H29 0.9500 . ? C11 O1 1.319(3) . ? C11 C12 1.416(4) . ? C12 N2 1.386(4) . ? C12 C13 1.400(4) . ? C13 C14 1.393(5) . ? C13 C18 1.502(4) . ? C14 C15 1.383(5) . ? C14 C16 1.504(5) . ? C15 N2 1.334(4) . ? C15 H1 0.9500 . ? C16 C17 1.408(7) . ? C16 H2 0.9900 . ? C16 H3 0.9900 . ? C17 H4 0.9800 . ? C17 H5 0.9800 . ? C17 H6 0.9800 . ? C18 C19 1.505(6) . ? C18 H7 0.9900 . ? C18 H8 0.9900 . ? C19 H9 0.9800 . ? C19 H10 0.9800 . ? C19 H11 0.9800 . ? C20 C25 1.390(4) . ? C20 C21 1.393(5) . ? C20 B1 1.605(4) . ? C21 C22 1.387(4) . ? C21 H12 0.9500 . ? C22 C23 1.389(5) . ? C22 H13 0.9500 . ? C23 C24 1.366(5) . ? C23 H14 0.9500 . ? C24 C25 1.388(4) . ? C24 H15 0.9500 . ? C25 H16 0.9500 . ? C26 C27 1.395(4) . ? C26 C31 1.399(5) . ? C26 B1 1.614(5) . ? C27 C28 1.381(5) . ? C27 H30 0.9500 . ? C28 C29 1.369(5) . ? C28 H31 0.9500 . ? C29 C30 1.384(5) . ? C29 H32 0.9500 . ? C30 C31 1.374(5) . ? C30 H33 0.9500 . ? C31 H34 0.9500 . ? C32 C33 1.511(5) . ? C32 H35 0.9800 . ? C32 H36 0.9800 . ? C32 H37 0.9800 . ? C33 C34 1.510(4) . ? C33 H38 0.9900 . ? C33 H39 0.9900 . ? C34 C35 1.376(4) . ? C34 C36 1.391(5) . ? C35 N3 1.355(4) . ? C35 H40 0.9500 . ? C36 C39 1.395(4) . ? C36 C37 1.504(4) . ? C37 C38 1.475(7) . ? C37 H41 0.9900 . ? C37 H42 0.9900 . ? C38 H43 0.9800 . ? C38 H44 0.9800 . ? C38 H45 0.9800 . ? C39 N3 1.374(4) . ? C39 C40 1.429(4) . ? C40 O3 1.311(4) . ? C40 C41 1.386(4) . ? C41 C42 1.379(4) . ? C41 H46 0.9500 . ? C42 O4 1.318(4) . ? C42 C43 1.430(4) . ? C43 N4 1.377(4) . ? C43 C44 1.388(4) . ? C44 C47 1.410(6) . ? C44 C45 1.489(6) . ? C45 C46 1.527(6) . ? C45 H47 0.9900 . ? C45 H48 0.9900 . ? C46 H49 0.9800 . ? C46 H50 0.9800 . ? C46 H51 0.9800 . ? C47 C50 1.370(6) . ? C47 C96 1.552(18) . ? C47 C99 1.559(17) . ? C50 N4 1.351(4) . ? C50 H57 0.9500 . ? O1 B1 1.511(4) . ? O2 B1 1.531(4) . ? O3 B2 1.514(5) . ? O4 B2 1.527(5) . ? N1 H98 0.8800 . ? N2 H17 0.8800 . ? N3 H99 0.8800 . ? N4 H100 0.8800 . ? B2 C51 1.588(6) . ? B2 C57 1.630(6) . ? C51 C52 1.392(6) . ? C51 C56 1.395(6) . ? C52 C53 1.411(8) . ? C52 H58 0.9500 . ? C53 C54 1.385(9) . ? C53 H59 0.9500 . ? C54 C55 1.332(9) . ? C54 H60 0.9500 . ? C55 C56 1.384(7) . ? C55 H61 0.9500 . ? C56 H62 0.9500 . ? C57 C62 1.379(5) . ? C57 C58 1.400(5) . ? C58 C59 1.381(6) . ? C58 H63 0.9500 . ? C59 C60 1.368(6) . ? C59 H64 0.9500 . ? C60 C61 1.374(6) . ? C60 H65 0.9500 . ? C61 C62 1.391(5) . ? C61 H66 0.9500 . ? C62 H67 0.9500 . ? C63 C64 1.373(5) . ? C63 C77 1.386(5) . ? C63 H68 0.9500 . ? C64 C65 1.381(5) . ? C64 H69 0.9500 . ? C65 N6 1.382(5) . ? C65 C89 1.427(4) . ? C66 N6 1.383(5) . ? C66 C67 1.392(5) . ? C66 C88 1.423(4) . ? C67 C68 1.350(6) . ? C67 H70 0.9500 . ? C68 C69 1.385(5) . ? C68 H71 0.9500 . ? C69 C70 1.390(5) . ? C69 H72 0.9500 . ? C70 N5 1.384(4) . ? C70 C88 1.412(5) . ? C71 N5 1.378(4) . ? C71 C72 1.388(4) . ? C71 C90 1.421(5) . ? C72 C73 1.378(5) . ? C72 H73 0.9500 . ? C73 C74 1.370(5) . ? C73 H74 0.9500 . ? C74 C75 1.403(4) . ? C74 H75 0.9500 . ? C75 N7 1.378(4) . ? C75 C90 1.413(4) . ? C76 C77 1.385(5) . ? C76 N7 1.391(4) . ? C76 C89 1.416(4) . ? C77 H76 0.9500 . ? C78 C79 1.472(5) . ? C78 N7 1.536(5) . ? C78 H77 0.9900 . ? C78 H78 0.9900 . ? C79 C80 1.506(5) . ? C79 H79 0.9900 . ? C79 H80 0.9900 . ? C80 H81 0.9800 . ? C80 H82 0.9800 . ? C80 H83 0.9800 . ? C81 C82 1.429(6) . ? C81 N5 1.539(6) . ? C81 H84 0.9900 . ? C81 H85 0.9900 . ? C82 C83 1.598(7) . ? C82 H86 0.9900 . ? C82 H87 0.9900 . ? C83 H88 0.9800 . ? C83 H89 0.9800 . ? C83 H90 0.9800 . ? C95 C94 1.503(11) . ? C95 C92 1.556(10) . ? C95 H107 0.9800 . ? C95 H108 0.9800 . ? C95 H109 0.9800 . ? C95 H110 0.9800 . ? C95 H111 0.9800 . ? C95 H112 0.9800 . ? C95 H101 0.9800 . ? C95 H102 0.9800 . ? C95 H103 0.9800 . ? C95 H104 0.9800 . ? C95 H105 0.9800 . ? C95 H106 0.9800 . ? N6 C91 1.554(8) . ? N6 C93 1.597(11) . ? C87 C89 1.396(5) . ? C87 C90 1.405(4) . ? C87 C88 1.408(4) . ? C91 C92 1.515(12) . ? C91 H113 0.9900 . ? C91 H114 0.9900 . ? C92 H115 0.9900 . ? C92 H116 0.9900 . ? C93 C94 1.502(16) . ? C93 H117 0.9900 . ? C93 H118 0.9900 . ? C94 H119 0.9900 . ? C94 H120 0.9900 . ? C96 C97 1.457(17) . ? C96 H121 0.9900 . ? C96 H122 0.9900 . ? C97 H123 0.9800 . ? C97 H124 0.9800 . ? C97 H125 0.9800 . ? C98 C99 1.456(18) . ? C98 H126 0.9800 . ? C98 H127 0.9800 . ? C98 H128 0.9800 . ? C99 H129 0.9900 . ? C99 H130 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H18 109.5 . . ? C2 C1 H19 109.5 . . ? H18 C1 H19 109.5 . . ? C2 C1 H20 109.5 . . ? H18 C1 H20 109.5 . . ? H19 C1 H20 109.5 . . ? C3 C2 C1 114.3(4) . . ? C3 C2 H21 108.7 . . ? C1 C2 H21 108.7 . . ? C3 C2 H22 108.7 . . ? C1 C2 H22 108.7 . . ? H21 C2 H22 107.6 . . ? C4 C3 C7 106.6(3) . . ? C4 C3 C2 127.2(3) . . ? C7 C3 C2 126.1(4) . . ? N1 C4 C3 109.8(3) . . ? N1 C4 H23 125.1 . . ? C3 C4 H23 125.1 . . ? C6 C5 H24 109.5 . . ? C6 C5 H25 109.5 . . ? H24 C5 H25 109.5 . . ? C6 C5 H26 109.5 . . ? H24 C5 H26 109.5 . . ? H25 C5 H26 109.5 . . ? C7 C6 C5 111.7(3) . . ? C7 C6 H27 109.3 . . ? C5 C6 H27 109.3 . . ? C7 C6 H28 109.3 . . ? C5 C6 H28 109.3 . . ? H27 C6 H28 107.9 . . ? C8 C7 C3 107.3(3) . . ? C8 C7 C6 127.5(3) . . ? C3 C7 C6 125.1(3) . . ? N1 C8 C7 107.4(3) . . ? N1 C8 C9 121.3(3) . . ? C7 C8 C9 131.3(3) . . ? O2 C9 C10 121.0(2) . . ? O2 C9 C8 115.9(3) . . ? C10 C9 C8 123.0(3) . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H29 119.9 . . ? C11 C10 H29 119.9 . . ? O1 C11 C10 120.3(3) . . ? O1 C11 C12 117.0(2) . . ? C10 C11 C12 122.6(3) . . ? N2 C12 C13 106.8(3) . . ? N2 C12 C11 120.5(3) . . ? C13 C12 C11 132.7(3) . . ? C14 C13 C12 107.1(3) . . ? C14 C13 C18 125.5(3) . . ? C12 C13 C18 127.3(3) . . ? C15 C14 C13 107.6(3) . . ? C15 C14 C16 124.8(4) . . ? C13 C14 C16 127.7(4) . . ? N2 C15 C14 108.9(3) . . ? N2 C15 H1 125.5 . . ? C14 C15 H1 125.5 . . ? C17 C16 C14 115.7(4) . . ? C17 C16 H2 108.3 . . ? C14 C16 H2 108.3 . . ? C17 C16 H3 108.3 . . ? C14 C16 H3 108.3 . . ? H2 C16 H3 107.4 . . ? C16 C17 H4 109.5 . . ? C16 C17 H5 109.5 . . ? H4 C17 H5 109.5 . . ? C16 C17 H6 109.5 . . ? H4 C17 H6 109.5 . . ? H5 C17 H6 109.5 . . ? C13 C18 C19 114.5(3) . . ? C13 C18 H7 108.6 . . ? C19 C18 H7 108.6 . . ? C13 C18 H8 108.6 . . ? C19 C18 H8 108.6 . . ? H7 C18 H8 107.6 . . ? C18 C19 H9 109.5 . . ? C18 C19 H10 109.5 . . ? H9 C19 H10 109.5 . . ? C18 C19 H11 109.5 . . ? H9 C19 H11 109.5 . . ? H10 C19 H11 109.5 . . ? C25 C20 C21 116.6(3) . . ? C25 C20 B1 122.2(3) . . ? C21 C20 B1 121.2(3) . . ? C22 C21 C20 122.2(3) . . ? C22 C21 H12 118.9 . . ? C20 C21 H12 118.9 . . ? C21 C22 C23 119.3(4) . . ? C21 C22 H13 120.4 . . ? C23 C22 H13 120.4 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H14 120.1 . . ? C22 C23 H14 120.1 . . ? C23 C24 C25 120.2(3) . . ? C23 C24 H15 119.9 . . ? C25 C24 H15 119.9 . . ? C24 C25 C20 121.9(3) . . ? C24 C25 H16 119.1 . . ? C20 C25 H16 119.1 . . ? C27 C26 C31 115.7(3) . . ? C27 C26 B1 123.9(3) . . ? C31 C26 B1 120.4(3) . . ? C28 C27 C26 122.5(3) . . ? C28 C27 H30 118.7 . . ? C26 C27 H30 118.7 . . ? C29 C28 C27 120.1(3) . . ? C29 C28 H31 119.9 . . ? C27 C28 H31 119.9 . . ? C28 C29 C30 119.1(3) . . ? C28 C29 H32 120.5 . . ? C30 C29 H32 120.5 . . ? C31 C30 C29 120.5(4) . . ? C31 C30 H33 119.8 . . ? C29 C30 H33 119.8 . . ? C30 C31 C26 122.1(3) . . ? C30 C31 H34 118.9 . . ? C26 C31 H34 118.9 . . ? C33 C32 H35 109.5 . . ? C33 C32 H36 109.5 . . ? H35 C32 H36 109.5 . . ? C33 C32 H37 109.5 . . ? H35 C32 H37 109.5 . . ? H36 C32 H37 109.5 . . ? C34 C33 C32 113.9(3) . . ? C34 C33 H38 108.8 . . ? C32 C33 H38 108.8 . . ? C34 C33 H39 108.8 . . ? C32 C33 H39 108.8 . . ? H38 C33 H39 107.7 . . ? C35 C34 C36 107.3(3) . . ? C35 C34 C33 125.1(3) . . ? C36 C34 C33 127.6(3) . . ? N3 C35 C34 109.0(3) . . ? N3 C35 H40 125.5 . . ? C34 C35 H40 125.5 . . ? C34 C36 C39 107.5(3) . . ? C34 C36 C37 124.6(3) . . ? C39 C36 C37 127.9(3) . . ? C38 C37 C36 113.6(4) . . ? C38 C37 H41 108.9 . . ? C36 C37 H41 108.9 . . ? C38 C37 H42 108.9 . . ? C36 C37 H42 108.9 . . ? H41 C37 H42 107.7 . . ? C37 C38 H43 109.5 . . ? C37 C38 H44 109.5 . . ? H43 C38 H44 109.5 . . ? C37 C38 H45 109.5 . . ? H43 C38 H45 109.5 . . ? H44 C38 H45 109.5 . . ? N3 C39 C36 107.4(3) . . ? N3 C39 C40 120.0(2) . . ? C36 C39 C40 132.7(3) . . ? O3 C40 C41 120.9(3) . . ? O3 C40 C39 116.7(3) . . ? C41 C40 C39 122.3(3) . . ? C42 C41 C40 120.7(3) . . ? C42 C41 H46 119.6 . . ? C40 C41 H46 119.6 . . ? O4 C42 C41 120.9(3) . . ? O4 C42 C43 117.5(3) . . ? C41 C42 C43 121.7(3) . . ? N4 C43 C44 107.8(3) . . ? N4 C43 C42 121.1(3) . . ? C44 C43 C42 130.5(3) . . ? C43 C44 C47 106.5(3) . . ? C43 C44 C45 128.0(4) . . ? C47 C44 C45 125.5(3) . . ? C44 C45 C46 112.2(3) . . ? C44 C45 H47 109.2 . . ? C46 C45 H47 109.2 . . ? C44 C45 H48 109.2 . . ? C46 C45 H48 109.2 . . ? H47 C45 H48 107.9 . . ? C45 C46 H49 109.5 . . ? C45 C46 H50 109.5 . . ? H49 C46 H50 109.5 . . ? C45 C46 H51 109.5 . . ? H49 C46 H51 109.5 . . ? H50 C46 H51 109.5 . . ? C50 C47 C44 107.8(3) . . ? C50 C47 C96 137.3(6) . . ? C44 C47 C96 114.9(6) . . ? C50 C47 C99 114.9(6) . . ? C44 C47 C99 137.3(6) . . ? C96 C47 C99 22.4(6) . . ? N4 C50 C47 108.7(4) . . ? N4 C50 H57 125.7 . . ? C47 C50 H57 125.7 . . ? C11 O1 B1 117.9(2) . . ? C9 O2 B1 116.1(2) . . ? C40 O3 B2 119.9(3) . . ? C42 O4 B2 118.1(3) . . ? C4 N1 C8 108.9(3) . . ? C4 N1 H98 125.6 . . ? C8 N1 H98 125.6 . . ? C15 N2 C12 109.5(3) . . ? C15 N2 H17 125.2 . . ? C12 N2 H17 125.2 . . ? C35 N3 C39 108.8(2) . . ? C35 N3 H99 125.6 . . ? C39 N3 H99 125.6 . . ? C50 N4 C43 109.2(3) . . ? C50 N4 H100 125.4 . . ? C43 N4 H100 125.4 . . ? O1 B1 O2 108.0(2) . . ? O1 B1 C20 108.3(2) . . ? O2 B1 C20 107.5(2) . . ? O1 B1 C26 110.7(3) . . ? O2 B1 C26 107.2(2) . . ? C20 B1 C26 114.9(3) . . ? O3 B2 O4 108.8(3) . . ? O3 B2 C51 106.7(3) . . ? O4 B2 C51 110.7(3) . . ? O3 B2 C57 109.3(3) . . ? O4 B2 C57 107.9(3) . . ? C51 B2 C57 113.4(3) . . ? C52 C51 C56 114.8(5) . . ? C52 C51 B2 124.2(4) . . ? C56 C51 B2 121.0(4) . . ? C51 C52 C53 122.4(6) . . ? C51 C52 H58 118.8 . . ? C53 C52 H58 118.8 . . ? C54 C53 C52 118.6(6) . . ? C54 C53 H59 120.7 . . ? C52 C53 H59 120.7 . . ? C55 C54 C53 120.8(6) . . ? C55 C54 H60 119.6 . . ? C53 C54 H60 119.6 . . ? C54 C55 C56 120.0(7) . . ? C54 C55 H61 120.0 . . ? C56 C55 H61 120.0 . . ? C55 C56 C51 123.4(6) . . ? C55 C56 H62 118.3 . . ? C51 C56 H62 118.3 . . ? C62 C57 C58 115.6(4) . . ? C62 C57 B2 123.6(3) . . ? C58 C57 B2 120.9(4) . . ? C59 C58 C57 122.3(4) . . ? C59 C58 H63 118.9 . . ? C57 C58 H63 118.9 . . ? C60 C59 C58 120.5(4) . . ? C60 C59 H64 119.8 . . ? C58 C59 H64 119.8 . . ? C59 C60 C61 119.0(4) . . ? C59 C60 H65 120.5 . . ? C61 C60 H65 120.5 . . ? C60 C61 C62 120.0(4) . . ? C60 C61 H66 120.0 . . ? C62 C61 H66 120.0 . . ? C57 C62 C61 122.6(4) . . ? C57 C62 H67 118.7 . . ? C61 C62 H67 118.7 . . ? C64 C63 C77 123.1(4) . . ? C64 C63 H68 118.4 . . ? C77 C63 H68 118.4 . . ? C63 C64 C65 119.4(3) . . ? C63 C64 H69 120.3 . . ? C65 C64 H69 120.3 . . ? C64 C65 N6 122.9(3) . . ? C64 C65 C89 119.1(3) . . ? N6 C65 C89 118.0(3) . . ? N6 C66 C67 122.8(3) . . ? N6 C66 C88 118.5(3) . . ? C67 C66 C88 118.6(4) . . ? C68 C67 C66 119.8(3) . . ? C68 C67 H70 120.1 . . ? C66 C67 H70 120.1 . . ? C67 C68 C69 123.3(3) . . ? C67 C68 H71 118.3 . . ? C69 C68 H71 118.3 . . ? C68 C69 C70 118.8(4) . . ? C68 C69 H72 120.6 . . ? C70 C69 H72 120.6 . . ? N5 C70 C69 123.3(3) . . ? N5 C70 C88 117.5(3) . . ? C69 C70 C88 119.2(3) . . ? N5 C71 C72 122.3(3) . . ? N5 C71 C90 118.3(3) . . ? C72 C71 C90 119.3(3) . . ? C73 C72 C71 119.1(3) . . ? C73 C72 H73 120.4 . . ? C71 C72 H73 120.4 . . ? C74 C73 C72 123.3(3) . . ? C74 C73 H74 118.4 . . ? C72 C73 H74 118.4 . . ? C73 C74 C75 119.1(3) . . ? C73 C74 H75 120.5 . . ? C75 C74 H75 120.5 . . ? N7 C75 C74 122.0(3) . . ? N7 C75 C90 118.9(3) . . ? C74 C75 C90 119.1(3) . . ? C77 C76 N7 122.4(3) . . ? C77 C76 C89 119.3(3) . . ? N7 C76 C89 118.3(3) . . ? C76 C77 C63 119.0(3) . . ? C76 C77 H76 120.5 . . ? C63 C77 H76 120.5 . . ? C79 C78 N7 110.6(3) . . ? C79 C78 H77 109.5 . . ? N7 C78 H77 109.5 . . ? C79 C78 H78 109.5 . . ? N7 C78 H78 109.5 . . ? H77 C78 H78 108.1 . . ? C78 C79 C80 110.3(3) . . ? C78 C79 H79 109.6 . . ? C80 C79 H79 109.6 . . ? C78 C79 H80 109.6 . . ? C80 C79 H80 109.6 . . ? H79 C79 H80 108.1 . . ? C79 C80 H81 109.5 . . ? C79 C80 H82 109.5 . . ? H81 C80 H82 109.5 . . ? C79 C80 H83 109.5 . . ? H81 C80 H83 109.5 . . ? H82 C80 H83 109.5 . . ? C82 C81 N5 109.1(4) . . ? C82 C81 H84 109.9 . . ? N5 C81 H84 109.9 . . ? C82 C81 H85 109.9 . . ? N5 C81 H85 109.9 . . ? H84 C81 H85 108.3 . . ? C81 C82 C83 106.5(4) . . ? C81 C82 H86 110.4 . . ? C83 C82 H86 110.4 . . ? C81 C82 H87 110.4 . . ? C83 C82 H87 110.4 . . ? H86 C82 H87 108.6 . . ? C82 C83 H88 109.5 . . ? C82 C83 H89 109.5 . . ? H88 C83 H89 109.5 . . ? C82 C83 H90 109.5 . . ? H88 C83 H90 109.5 . . ? H89 C83 H90 109.5 . . ? C94 C95 C92 43.9(4) . . ? C94 C95 H107 153.3 . . ? C92 C95 H107 109.5 . . ? C94 C95 H108 84.6 . . ? C92 C95 H108 109.5 . . ? H107 C95 H108 109.5 . . ? C94 C95 H109 85.4 . . ? C92 C95 H109 109.5 . . ? H107 C95 H109 109.5 . . ? H108 C95 H109 109.5 . . ? C94 C95 H110 109.5 . . ? C92 C95 H110 153.4 . . ? H107 C95 H110 97.2 . . ? H108 C95 H110 59.1 . . ? H109 C95 H110 59.6 . . ? C94 C95 H111 109.5 . . ? C92 C95 H111 85.0 . . ? H107 C95 H111 60.0 . . ? H108 C95 H111 164.9 . . ? H109 C95 H111 67.7 . . ? H110 C95 H111 109.5 . . ? C94 C95 H112 109.5 . . ? C92 C95 H112 85.1 . . ? H107 C95 H112 58.8 . . ? H108 C95 H112 69.0 . . ? H109 C95 H112 164.5 . . ? H110 C95 H112 109.5 . . ? H111 C95 H112 109.5 . . ? C94 C95 H101 153.3 . . ? C92 C95 H101 109.5 . . ? H107 C95 H101 0.0 . . ? H108 C95 H101 109.5 . . ? H109 C95 H101 109.5 . . ? H110 C95 H101 97.2 . . ? H111 C95 H101 60.0 . . ? H112 C95 H101 58.8 . . ? C94 C95 H102 84.6 . . ? C92 C95 H102 109.5 . . ? H107 C95 H102 109.5 . . ? H108 C95 H102 0.0 . . ? H109 C95 H102 109.5 . . ? H110 C95 H102 59.1 . . ? H111 C95 H102 164.9 . . ? H112 C95 H102 69.0 . . ? H101 C95 H102 109.5 . . ? C94 C95 H103 85.4 . . ? C92 C95 H103 109.5 . . ? H107 C95 H103 109.5 . . ? H108 C95 H103 109.5 . . ? H109 C95 H103 0.0 . . ? H110 C95 H103 59.6 . . ? H111 C95 H103 67.7 . . ? H112 C95 H103 164.5 . . ? H101 C95 H103 109.5 . . ? H102 C95 H103 109.5 . . ? C94 C95 H104 109.5 . . ? C92 C95 H104 153.4 . . ? H107 C95 H104 97.2 . . ? H108 C95 H104 59.1 . . ? H109 C95 H104 59.6 . . ? H110 C95 H104 0.0 . . ? H111 C95 H104 109.5 . . ? H112 C95 H104 109.5 . . ? H101 C95 H104 97.2 . . ? H102 C95 H104 59.1 . . ? H103 C95 H104 59.6 . . ? C94 C95 H105 109.5 . . ? C92 C95 H105 85.0 . . ? H107 C95 H105 60.0 . . ? H108 C95 H105 164.9 . . ? H109 C95 H105 67.7 . . ? H110 C95 H105 109.5 . . ? H111 C95 H105 0.0 . . ? H112 C95 H105 109.5 . . ? H101 C95 H105 60.0 . . ? H102 C95 H105 164.9 . . ? H103 C95 H105 67.7 . . ? H104 C95 H105 109.5 . . ? C94 C95 H106 109.5 . . ? C92 C95 H106 85.1 . . ? H107 C95 H106 58.8 . . ? H108 C95 H106 69.0 . . ? H109 C95 H106 164.5 . . ? H110 C95 H106 109.5 . . ? H111 C95 H106 109.5 . . ? H112 C95 H106 0.0 . . ? H101 C95 H106 58.8 . . ? H102 C95 H106 69.0 . . ? H103 C95 H106 164.5 . . ? H104 C95 H106 109.5 . . ? H105 C95 H106 109.5 . . ? C71 N5 C70 123.5(3) . . ? C71 N5 C81 119.5(3) . . ? C70 N5 C81 116.5(3) . . ? C65 N6 C66 123.6(3) . . ? C65 N6 C91 117.1(4) . . ? C66 N6 C91 116.7(4) . . ? C65 N6 C93 114.8(5) . . ? C66 N6 C93 113.9(4) . . ? C91 N6 C93 46.3(4) . . ? C75 N7 C76 122.1(3) . . ? C75 N7 C78 119.2(3) . . ? C76 N7 C78 118.6(3) . . ? C89 C87 C90 119.8(3) . . ? C89 C87 C88 121.0(3) . . ? C90 C87 C88 119.1(3) . . ? C87 C88 C70 121.0(3) . . ? C87 C88 C66 119.0(3) . . ? C70 C88 C66 120.0(3) . . ? C87 C89 C76 120.3(3) . . ? C87 C89 C65 119.6(3) . . ? C76 C89 C65 120.0(3) . . ? C87 C90 C75 119.9(3) . . ? C87 C90 C71 120.1(3) . . ? C75 C90 C71 120.1(3) . . ? C92 C91 N6 105.1(5) . . ? C92 C91 H113 110.7 . . ? N6 C91 H113 110.7 . . ? C92 C91 H114 110.7 . . ? N6 C91 H114 110.7 . . ? H113 C91 H114 108.8 . . ? C91 C92 C95 104.5(6) . . ? C91 C92 H115 110.9 . . ? C95 C92 H115 110.9 . . ? C91 C92 H116 110.9 . . ? C95 C92 H116 110.9 . . ? H115 C92 H116 108.9 . . ? C94 C93 N6 104.0(7) . . ? C94 C93 H117 111.0 . . ? N6 C93 H117 111.0 . . ? C94 C93 H118 111.0 . . ? N6 C93 H118 111.0 . . ? H117 C93 H118 109.0 . . ? C93 C94 C95 107.3(9) . . ? C93 C94 H119 110.3 . . ? C95 C94 H119 110.3 . . ? C93 C94 H120 110.3 . . ? C95 C94 H120 110.3 . . ? H119 C94 H120 108.5 . . ? C97 C96 C47 107.4(10) . . ? C97 C96 H121 110.2 . . ? C47 C96 H121 110.2 . . ? C97 C96 H122 110.2 . . ? C47 C96 H122 110.2 . . ? H121 C96 H122 108.5 . . ? C98 C99 C47 114.0(12) . . ? C98 C99 H129 108.8 . . ? C47 C99 H129 108.8 . . ? C98 C99 H130 108.8 . . ? C47 C99 H130 108.8 . . ? H129 C99 H130 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -6.8(7) . . . . ? C1 C2 C3 C7 177.1(4) . . . . ? C7 C3 C4 N1 -0.6(5) . . . . ? C2 C3 C4 N1 -177.2(4) . . . . ? C4 C3 C7 C8 1.1(4) . . . . ? C2 C3 C7 C8 177.8(4) . . . . ? C4 C3 C7 C6 177.6(4) . . . . ? C2 C3 C7 C6 -5.7(7) . . . . ? C5 C6 C7 C8 86.0(5) . . . . ? C5 C6 C7 C3 -89.8(5) . . . . ? C3 C7 C8 N1 -1.2(4) . . . . ? C6 C7 C8 N1 -177.6(3) . . . . ? C3 C7 C8 C9 179.1(3) . . . . ? C6 C7 C8 C9 2.7(7) . . . . ? N1 C8 C9 O2 169.7(3) . . . . ? C7 C8 C9 O2 -10.6(5) . . . . ? N1 C8 C9 C10 -8.0(5) . . . . ? C7 C8 C9 C10 171.7(4) . . . . ? O2 C9 C10 C11 -7.4(5) . . . . ? C8 C9 C10 C11 170.3(3) . . . . ? C9 C10 C11 O1 12.8(5) . . . . ? C9 C10 C11 C12 -164.9(3) . . . . ? O1 C11 C12 N2 -172.8(2) . . . . ? C10 C11 C12 N2 4.9(4) . . . . ? O1 C11 C12 C13 6.3(5) . . . . ? C10 C11 C12 C13 -176.0(3) . . . . ? N2 C12 C13 C14 -0.3(3) . . . . ? C11 C12 C13 C14 -179.5(3) . . . . ? N2 C12 C13 C18 177.6(3) . . . . ? C11 C12 C13 C18 -1.6(6) . . . . ? C12 C13 C14 C15 0.7(4) . . . . ? C18 C13 C14 C15 -177.3(3) . . . . ? C12 C13 C14 C16 -178.9(4) . . . . ? C18 C13 C14 C16 3.2(6) . . . . ? C13 C14 C15 N2 -0.8(4) . . . . ? C16 C14 C15 N2 178.8(4) . . . . ? C15 C14 C16 C17 -82.7(6) . . . . ? C13 C14 C16 C17 96.7(6) . . . . ? C14 C13 C18 C19 -97.9(4) . . . . ? C12 C13 C18 C19 84.6(4) . . . . ? C25 C20 C21 C22 -0.7(5) . . . . ? B1 C20 C21 C22 177.2(3) . . . . ? C20 C21 C22 C23 -0.2(5) . . . . ? C21 C22 C23 C24 1.0(6) . . . . ? C22 C23 C24 C25 -0.8(6) . . . . ? C23 C24 C25 C20 -0.2(5) . . . . ? C21 C20 C25 C24 0.9(5) . . . . ? B1 C20 C25 C24 -177.0(3) . . . . ? C31 C26 C27 C28 0.7(4) . . . . ? B1 C26 C27 C28 -177.9(3) . . . . ? C26 C27 C28 C29 0.0(4) . . . . ? C27 C28 C29 C30 -0.4(5) . . . . ? C28 C29 C30 C31 0.0(5) . . . . ? C29 C30 C31 C26 0.7(5) . . . . ? C27 C26 C31 C30 -1.0(4) . . . . ? B1 C26 C31 C30 177.6(3) . . . . ? C32 C33 C34 C35 -4.2(5) . . . . ? C32 C33 C34 C36 172.9(3) . . . . ? C36 C34 C35 N3 0.4(4) . . . . ? C33 C34 C35 N3 178.0(3) . . . . ? C35 C34 C36 C39 -0.6(4) . . . . ? C33 C34 C36 C39 -178.1(3) . . . . ? C35 C34 C36 C37 178.7(3) . . . . ? C33 C34 C36 C37 1.1(6) . . . . ? C34 C36 C37 C38 87.3(5) . . . . ? C39 C36 C37 C38 -93.6(5) . . . . ? C34 C36 C39 N3 0.5(4) . . . . ? C37 C36 C39 N3 -178.7(3) . . . . ? C34 C36 C39 C40 -179.2(3) . . . . ? C37 C36 C39 C40 1.6(6) . . . . ? N3 C39 C40 O3 166.6(3) . . . . ? C36 C39 C40 O3 -13.7(5) . . . . ? N3 C39 C40 C41 -12.3(5) . . . . ? C36 C39 C40 C41 167.3(3) . . . . ? O3 C40 C41 C42 -9.5(5) . . . . ? C39 C40 C41 C42 169.4(3) . . . . ? C40 C41 C42 O4 3.6(5) . . . . ? C40 C41 C42 C43 -177.4(3) . . . . ? O4 C42 C43 N4 -178.5(3) . . . . ? C41 C42 C43 N4 2.4(5) . . . . ? O4 C42 C43 C44 11.4(5) . . . . ? C41 C42 C43 C44 -167.7(4) . . . . ? N4 C43 C44 C47 -1.5(4) . . . . ? C42 C43 C44 C47 169.7(3) . . . . ? N4 C43 C44 C45 179.8(3) . . . . ? C42 C43 C44 C45 -9.1(6) . . . . ? C43 C44 C45 C46 -81.8(5) . . . . ? C47 C44 C45 C46 99.6(5) . . . . ? C43 C44 C47 C50 1.3(4) . . . . ? C45 C44 C47 C50 -179.9(3) . . . . ? C43 C44 C47 C96 -178.8(7) . . . . ? C45 C44 C47 C96 0.0(8) . . . . ? C43 C44 C47 C99 -177.8(10) . . . . ? C45 C44 C47 C99 1.0(12) . . . . ? C44 C47 C50 N4 -0.7(4) . . . . ? C96 C47 C50 N4 179.4(9) . . . . ? C99 C47 C50 N4 178.7(8) . . . . ? C10 C11 O1 B1 13.3(4) . . . . ? C12 C11 O1 B1 -168.9(3) . . . . ? C10 C9 O2 B1 -22.9(4) . . . . ? C8 C9 O2 B1 159.4(3) . . . . ? C41 C40 O3 B2 -10.3(5) . . . . ? C39 C40 O3 B2 170.8(3) . . . . ? C41 C42 O4 B2 21.1(5) . . . . ? C43 C42 O4 B2 -158.0(3) . . . . ? C3 C4 N1 C8 -0.1(4) . . . . ? C7 C8 N1 C4 0.8(4) . . . . ? C9 C8 N1 C4 -179.4(3) . . . . ? C14 C15 N2 C12 0.6(4) . . . . ? C13 C12 N2 C15 -0.2(3) . . . . ? C11 C12 N2 C15 179.1(3) . . . . ? C34 C35 N3 C39 -0.1(3) . . . . ? C36 C39 N3 C35 -0.3(3) . . . . ? C40 C39 N3 C35 179.5(3) . . . . ? C47 C50 N4 C43 -0.2(4) . . . . ? C44 C43 N4 C50 1.1(4) . . . . ? C42 C43 N4 C50 -171.0(3) . . . . ? C11 O1 B1 O2 -39.5(3) . . . . ? C11 O1 B1 C20 -155.6(2) . . . . ? C11 O1 B1 C26 77.7(3) . . . . ? C9 O2 B1 O1 44.2(3) . . . . ? C9 O2 B1 C20 160.9(3) . . . . ? C9 O2 B1 C26 -75.1(3) . . . . ? C25 C20 B1 O1 -32.4(4) . . . . ? C21 C20 B1 O1 149.7(3) . . . . ? C25 C20 B1 O2 -148.9(3) . . . . ? C21 C20 B1 O2 33.2(4) . . . . ? C25 C20 B1 C26 91.8(4) . . . . ? C21 C20 B1 C26 -86.0(4) . . . . ? C27 C26 B1 O1 -2.0(4) . . . . ? C31 C26 B1 O1 179.5(2) . . . . ? C27 C26 B1 O2 115.6(3) . . . . ? C31 C26 B1 O2 -62.9(3) . . . . ? C27 C26 B1 C20 -125.0(3) . . . . ? C31 C26 B1 C20 56.5(4) . . . . ? C40 O3 B2 O4 31.3(5) . . . . ? C40 O3 B2 C51 150.7(3) . . . . ? C40 O3 B2 C57 -86.3(3) . . . . ? C42 O4 B2 O3 -36.5(5) . . . . ? C42 O4 B2 C51 -153.5(3) . . . . ? C42 O4 B2 C57 81.9(4) . . . . ? O3 B2 C51 C52 -137.8(4) . . . . ? O4 B2 C51 C52 -19.6(6) . . . . ? C57 B2 C51 C52 101.8(5) . . . . ? O3 B2 C51 C56 41.8(5) . . . . ? O4 B2 C51 C56 160.0(4) . . . . ? C57 B2 C51 C56 -78.6(5) . . . . ? C56 C51 C52 C53 1.7(8) . . . . ? B2 C51 C52 C53 -178.7(5) . . . . ? C51 C52 C53 C54 -1.0(9) . . . . ? C52 C53 C54 C55 -1.1(10) . . . . ? C53 C54 C55 C56 2.3(10) . . . . ? C54 C55 C56 C51 -1.5(9) . . . . ? C52 C51 C56 C55 -0.5(7) . . . . ? B2 C51 C56 C55 179.9(5) . . . . ? O3 B2 C57 C62 11.7(4) . . . . ? O4 B2 C57 C62 -106.5(4) . . . . ? C51 B2 C57 C62 130.6(4) . . . . ? O3 B2 C57 C58 -168.0(3) . . . . ? O4 B2 C57 C58 73.9(4) . . . . ? C51 B2 C57 C58 -49.1(5) . . . . ? C62 C57 C58 C59 -0.5(5) . . . . ? B2 C57 C58 C59 179.2(3) . . . . ? C57 C58 C59 C60 1.5(6) . . . . ? C58 C59 C60 C61 -1.4(6) . . . . ? C59 C60 C61 C62 0.4(5) . . . . ? C58 C57 C62 C61 -0.5(5) . . . . ? B2 C57 C62 C61 179.8(3) . . . . ? C60 C61 C62 C57 0.6(5) . . . . ? C77 C63 C64 C65 0.5(6) . . . . ? C63 C64 C65 N6 178.4(4) . . . . ? C63 C64 C65 C89 -1.6(6) . . . . ? N6 C66 C67 C68 -178.6(4) . . . . ? C88 C66 C67 C68 0.8(6) . . . . ? C66 C67 C68 C69 -3.1(7) . . . . ? C67 C68 C69 C70 1.4(6) . . . . ? C68 C69 C70 N5 -175.1(4) . . . . ? C68 C69 C70 C88 2.6(6) . . . . ? N5 C71 C72 C73 179.7(3) . . . . ? C90 C71 C72 C73 0.8(5) . . . . ? C71 C72 C73 C74 0.3(5) . . . . ? C72 C73 C74 C75 -0.1(5) . . . . ? C73 C74 C75 N7 177.4(3) . . . . ? C73 C74 C75 C90 -1.2(5) . . . . ? N7 C76 C77 C63 -178.8(3) . . . . ? C89 C76 C77 C63 0.0(6) . . . . ? C64 C63 C77 C76 0.3(6) . . . . ? N7 C78 C79 C80 178.0(3) . . . . ? N5 C81 C82 C83 164.6(3) . . . . ? C72 C71 N5 C70 176.1(3) . . . . ? C90 C71 N5 C70 -5.0(5) . . . . ? C72 C71 N5 C81 -12.0(5) . . . . ? C90 C71 N5 C81 166.9(3) . . . . ? C69 C70 N5 C71 -173.3(4) . . . . ? C88 C70 N5 C71 8.9(5) . . . . ? C69 C70 N5 C81 14.5(5) . . . . ? C88 C70 N5 C81 -163.2(3) . . . . ? C82 C81 N5 C71 97.4(4) . . . . ? C82 C81 N5 C70 -90.1(4) . . . . ? C64 C65 N6 C66 -177.5(4) . . . . ? C89 C65 N6 C66 2.6(6) . . . . ? C64 C65 N6 C91 21.6(6) . . . . ? C89 C65 N6 C91 -158.3(4) . . . . ? C64 C65 N6 C93 -30.2(6) . . . . ? C89 C65 N6 C93 149.9(5) . . . . ? C67 C66 N6 C65 175.0(4) . . . . ? C88 C66 N6 C65 -4.4(6) . . . . ? C67 C66 N6 C91 -24.0(6) . . . . ? C88 C66 N6 C91 156.5(4) . . . . ? C67 C66 N6 C93 27.5(7) . . . . ? C88 C66 N6 C93 -152.0(5) . . . . ? C74 C75 N7 C76 171.9(3) . . . . ? C90 C75 N7 C76 -9.5(5) . . . . ? C74 C75 N7 C78 -12.4(5) . . . . ? C90 C75 N7 C78 166.2(3) . . . . ? C77 C76 N7 C75 -172.7(3) . . . . ? C89 C76 N7 C75 8.5(5) . . . . ? C77 C76 N7 C78 11.6(5) . . . . ? C89 C76 N7 C78 -167.3(3) . . . . ? C79 C78 N7 C75 94.3(4) . . . . ? C79 C78 N7 C76 -89.8(4) . . . . ? C89 C87 C88 C70 -178.3(3) . . . . ? C90 C87 C88 C70 0.2(5) . . . . ? C89 C87 C88 C66 2.3(5) . . . . ? C90 C87 C88 C66 -179.2(3) . . . . ? N5 C70 C88 C87 -6.3(5) . . . . ? C69 C70 C88 C87 175.9(3) . . . . ? N5 C70 C88 C66 173.1(3) . . . . ? C69 C70 C88 C66 -4.8(5) . . . . ? N6 C66 C88 C87 2.0(5) . . . . ? C67 C66 C88 C87 -177.5(3) . . . . ? N6 C66 C88 C70 -177.4(4) . . . . ? C67 C66 C88 C70 3.1(5) . . . . ? C90 C87 C89 C76 -2.7(5) . . . . ? C88 C87 C89 C76 175.7(3) . . . . ? C90 C87 C89 C65 177.3(3) . . . . ? C88 C87 C89 C65 -4.2(5) . . . . ? C77 C76 C89 C87 178.9(3) . . . . ? N7 C76 C89 C87 -2.2(5) . . . . ? C77 C76 C89 C65 -1.2(5) . . . . ? N7 C76 C89 C65 177.7(3) . . . . ? C64 C65 C89 C87 -178.1(3) . . . . ? N6 C65 C89 C87 1.8(5) . . . . ? C64 C65 C89 C76 2.0(5) . . . . ? N6 C65 C89 C76 -178.1(3) . . . . ? C89 C87 C90 C75 1.7(4) . . . . ? C88 C87 C90 C75 -176.8(3) . . . . ? C89 C87 C90 C71 -177.6(3) . . . . ? C88 C87 C90 C71 3.9(4) . . . . ? N7 C75 C90 C87 4.3(4) . . . . ? C74 C75 C90 C87 -177.1(3) . . . . ? N7 C75 C90 C71 -176.4(3) . . . . ? C74 C75 C90 C71 2.2(5) . . . . ? N5 C71 C90 C87 -1.6(5) . . . . ? C72 C71 C90 C87 177.3(3) . . . . ? N5 C71 C90 C75 179.1(3) . . . . ? C72 C71 C90 C75 -2.0(5) . . . . ? C65 N6 C91 C92 -101.2(6) . . . . ? C66 N6 C91 C92 96.6(6) . . . . ? C93 N6 C91 C92 -1.9(6) . . . . ? N6 C91 C92 C95 -175.2(5) . . . . ? C94 C95 C92 C91 0.8(7) . . . . ? C65 N6 C93 C94 108.1(7) . . . . ? C66 N6 C93 C94 -101.3(7) . . . . ? C91 N6 C93 C94 3.5(6) . . . . ? N6 C93 C94 C95 176.8(7) . . . . ? C92 C95 C94 C93 0.8(7) . . . . ? C50 C47 C96 C97 -1.2(15) . . . . ? C44 C47 C96 C97 179.0(7) . . . . ? C99 C47 C96 C97 1(2) . . . . ? C50 C47 C99 C98 -103.1(9) . . . . ? C44 C47 C99 C98 76.0(15) . . . . ? C96 C47 C99 C98 78(3) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.861 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.060