# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email higashino@kuchem.kyoto-u.ac.jp _publ_contact_author_name 'Tomohiro Higashino' loop_ _publ_author_name 'Atsuhiro Osuka' 'Tomohiro Higashino' data_0412hi _database_code_depnum_ccdc_archive 'CCDC 827554' #TrackingRef 'PB-Eur.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H11 B F24 N5 P, 1.5(C6 H14), 0.5(C7 H8)' _chemical_formula_sum 'C67.50 H36 B F24 N5 P' _chemical_formula_weight 1414.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.1073(6) _cell_length_b 18.0820(3) _cell_length_c 22.4608(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.2569(10) _cell_angle_gamma 90.00 _cell_volume 11738.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 43042 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 68.385 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5696 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4554 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\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 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55183 _diffrn_reflns_av_R_equivalents 0.1381 _diffrn_reflns_av_sigmaI/netI 0.1279 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 68.24 _reflns_number_total 10540 _reflns_number_gt 5634 _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^)+(0.0400P)^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 10540 _refine_ls_number_parameters 912 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.91287(14) 0.6976(2) 0.87078(19) 0.0356(10) Uani 1 1 d . . . C2 C 0.86740(14) 0.6962(2) 0.83412(19) 0.0401(11) Uani 1 1 d . . . H1 H 0.8487 0.6532 0.8236 0.048 Uiso 1 1 calc R . . C3 C 0.85361(14) 0.7678(2) 0.81517(19) 0.0375(10) Uani 1 1 d . . . H2 H 0.8238 0.7820 0.7902 0.045 Uiso 1 1 calc R . . C4 C 0.88975(14) 0.8142(2) 0.83826(18) 0.0357(10) Uani 1 1 d . . . C5 C 0.89100(15) 0.8954(2) 0.83701(18) 0.0386(11) Uani 1 1 d . . . C6 C 0.93031(15) 0.9331(2) 0.86166(19) 0.0382(10) Uani 1 1 d . . . C7 C 0.93997(14) 1.0144(2) 0.8657(2) 0.0451(12) Uani 1 1 d . . . H3 H 0.9333 1.0362 0.9027 0.054 Uiso 1 1 calc R . . H4 H 0.9214 1.0404 0.8282 0.054 Uiso 1 1 calc R . . C8 C 0.99209(14) 1.0185(2) 0.8707(2) 0.0454(12) Uani 1 1 d . . . H5 H 0.9969 1.0355 0.8310 0.054 Uiso 1 1 calc R . . H6 H 1.0080 1.0531 0.9039 0.054 Uiso 1 1 calc R . . C9 C 1.01035(15) 0.9413(2) 0.88546(19) 0.0392(11) Uani 1 1 d . . . C10 C 1.05347(15) 0.9143(2) 0.89277(18) 0.0376(10) Uani 1 1 d . . . C11 C 1.06128(15) 0.8358(2) 0.89890(18) 0.0370(10) Uani 1 1 d . . . C12 C 1.02815(14) 0.7824(2) 0.90510(19) 0.0367(10) Uani 1 1 d . . . C13 C 1.04909(14) 0.7138(2) 0.90697(18) 0.0371(10) Uani 1 1 d . . . C14 C 1.09680(14) 0.7304(2) 0.90325(18) 0.0370(10) Uani 1 1 d . . . C15 C 1.13566(14) 0.6849(2) 0.90382(18) 0.0351(10) Uani 1 1 d . . . C16 C 1.13933(14) 0.6087(2) 0.91008(18) 0.0365(10) Uani 1 1 d . . . C17 C 1.17375(14) 0.5546(2) 0.91078(18) 0.0392(11) Uani 1 1 d . . . H7 H 1.2044 0.5651 0.9094 0.047 Uiso 1 1 calc R . . C18 C 1.15619(14) 0.4850(2) 0.91381(18) 0.0409(11) Uani 1 1 d . . . H8 H 1.1726 0.4399 0.9148 0.049 Uiso 1 1 calc R . . C19 C 1.10916(14) 0.4916(2) 0.91531(18) 0.0374(10) Uani 1 1 d . . . C20 C 1.06583(14) 0.4552(2) 0.91345(18) 0.0370(10) Uani 1 1 d . . . C21 C 1.03495(14) 0.5133(2) 0.91505(18) 0.0366(10) Uani 1 1 d . . . C22 C 1.05716(14) 0.5809(2) 0.91339(18) 0.0368(10) Uani 1 1 d . . . C23 C 1.03066(14) 0.6428(2) 0.90862(18) 0.0352(10) Uani 1 1 d . . . C24 C 0.98493(14) 0.6126(2) 0.90578(18) 0.0368(10) Uani 1 1 d . . . C25 C 0.93892(14) 0.6325(2) 0.89651(17) 0.0340(10) Uani 1 1 d . . . C26 C 0.84771(14) 0.9349(2) 0.8081(2) 0.0396(11) Uani 1 1 d . . . C27 C 0.82726(16) 0.9834(2) 0.8415(2) 0.0448(12) Uani 1 1 d . . . C28 C 0.78806(16) 1.0225(2) 0.8147(3) 0.0524(13) Uani 1 1 d . . . C29 C 0.76706(16) 1.0164(3) 0.7514(3) 0.0540(13) Uani 1 1 d . . . C30 C 0.78597(16) 0.9688(3) 0.7173(2) 0.0501(13) Uani 1 1 d . . . C31 C 0.82542(15) 0.9301(2) 0.7450(2) 0.0418(11) Uani 1 1 d . . . C32 C 1.09214(15) 0.9641(2) 0.8903(2) 0.0416(11) Uani 1 1 d . . . C33 C 1.09369(16) 1.0053(2) 0.8391(2) 0.0449(12) Uani 1 1 d . . . C34 C 1.13002(18) 1.0505(3) 0.8384(2) 0.0518(13) Uani 1 1 d . . . C35 C 1.16732(17) 1.0545(3) 0.8895(3) 0.0540(13) Uani 1 1 d . . . C36 C 1.16820(16) 1.0131(3) 0.9415(2) 0.0512(13) Uani 1 1 d . . . C37 C 1.13140(16) 0.9698(2) 0.9413(2) 0.0484(12) Uani 1 1 d . . . C38 C 1.17760(14) 0.7239(2) 0.89668(19) 0.0370(10) Uani 1 1 d . . . C39 C 1.20100(15) 0.7762(2) 0.9388(2) 0.0411(11) Uani 1 1 d . . . C40 C 1.23854(15) 0.8143(2) 0.9314(2) 0.0420(11) Uani 1 1 d . . . C41 C 1.25469(14) 0.7989(2) 0.8803(2) 0.0431(11) Uani 1 1 d . . . C42 C 1.23267(15) 0.7465(2) 0.8387(2) 0.0414(11) Uani 1 1 d . . . C43 C 1.19507(14) 0.7093(2) 0.8468(2) 0.0405(11) Uani 1 1 d . . . C44 C 1.05862(14) 0.3762(2) 0.89945(19) 0.0358(10) Uani 1 1 d . . . C45 C 1.09279(15) 0.3237(2) 0.9219(2) 0.0411(11) Uani 1 1 d . . . C46 C 1.08867(16) 0.2512(2) 0.9010(2) 0.0419(11) Uani 1 1 d . . . C47 C 1.04893(16) 0.2295(2) 0.8579(2) 0.0416(11) Uani 1 1 d . . . C48 C 1.01389(15) 0.2793(2) 0.8360(2) 0.0407(11) Uani 1 1 d . . . C49 C 1.01925(15) 0.3512(2) 0.85646(19) 0.0387(11) Uani 1 1 d . . . C50 C 0.91603(14) 0.5644(2) 0.90773(18) 0.0361(10) Uani 1 1 d . . . C51 C 0.87279(14) 0.5486(2) 0.91692(19) 0.0368(10) Uani 1 1 d . . . C52 C 0.86247(15) 0.4783(2) 0.93246(19) 0.0398(11) Uani 1 1 d . . . C53 C 0.89487(15) 0.4220(2) 0.94023(19) 0.0396(11) Uani 1 1 d . . . C54 C 0.93761(14) 0.4356(2) 0.93358(19) 0.0363(10) Uani 1 1 d . . . C55 C 0.94838(14) 0.5051(2) 0.91744(18) 0.0367(10) Uani 1 1 d . . . N1 N 0.92814(11) 0.77158(18) 0.87178(15) 0.0372(9) Uani 1 1 d . . . N2 N 0.97279(12) 0.89499(17) 0.88697(16) 0.0405(9) Uani 1 1 d . . . N3 N 1.10143(11) 0.80430(18) 0.89714(15) 0.0371(8) Uani 1 1 d . . . N4 N 1.10164(12) 0.56661(19) 0.91510(15) 0.0389(9) Uani 1 1 d . . . N5 N 0.98983(12) 0.53465(18) 0.91378(15) 0.0374(9) Uani 1 1 d . . . F1 F 0.84623(8) 0.98977(13) 0.90290(12) 0.0564(7) Uani 1 1 d . . . F2 F 0.76949(9) 1.06766(14) 0.84883(13) 0.0708(8) Uani 1 1 d . . . F3 F 0.72914(9) 1.05510(14) 0.72492(14) 0.0744(9) Uani 1 1 d . . . F4 F 0.76557(9) 0.96253(13) 0.65579(12) 0.0618(8) Uani 1 1 d . . . F5 F 0.84338(8) 0.88635(12) 0.70883(11) 0.0511(7) Uani 1 1 d . . . F6 F 1.05827(9) 1.00026(12) 0.78625(11) 0.0522(7) Uani 1 1 d . . . F7 F 1.12899(9) 1.08995(13) 0.78701(13) 0.0674(8) Uani 1 1 d . . . F8 F 1.20307(9) 1.09906(14) 0.88853(14) 0.0730(9) Uani 1 1 d . . . F9 F 1.20562(9) 1.01692(14) 0.99138(13) 0.0706(8) Uani 1 1 d . . . F10 F 1.13283(9) 0.93008(13) 0.99257(12) 0.0569(7) Uani 1 1 d . . . F11 F 1.18781(8) 0.79115(12) 0.99020(11) 0.0464(6) Uani 1 1 d . . . F12 F 1.26003(8) 0.86465(13) 0.97302(11) 0.0536(7) Uani 1 1 d . . . F13 F 1.29138(8) 0.83491(13) 0.87272(12) 0.0538(7) Uani 1 1 d . . . F14 F 1.24858(8) 0.73117(12) 0.78897(11) 0.0509(7) Uani 1 1 d . . . F15 F 1.17376(8) 0.65910(12) 0.80391(10) 0.0445(6) Uani 1 1 d . . . F16 F 1.13240(8) 0.34248(12) 0.96548(11) 0.0485(7) Uani 1 1 d . . . F17 F 1.12338(8) 0.20269(12) 0.92359(11) 0.0529(7) Uani 1 1 d . . . F18 F 1.04479(8) 0.15918(12) 0.83772(12) 0.0547(7) Uani 1 1 d . . . F19 F 0.97518(8) 0.25722(12) 0.79351(11) 0.0490(7) Uani 1 1 d . . . F20 F 0.98559(8) 0.39971(11) 0.83004(10) 0.0440(6) Uani 1 1 d . . . F21 F 0.84029(8) 0.60051(12) 0.91372(10) 0.0447(6) Uani 1 1 d . . . F22 F 0.82105(8) 0.46475(12) 0.94211(10) 0.0459(6) Uani 1 1 d . . . F23 F 0.88434(8) 0.35441(12) 0.95816(10) 0.0434(6) Uani 1 1 d . . . F24 F 0.97030(8) 0.38146(12) 0.94649(10) 0.0437(6) Uani 1 1 d . . . P1 P 0.97650(4) 0.81083(6) 0.92070(5) 0.0377(3) Uani 1 1 d . . . B1 B 0.97426(19) 0.8086(3) 1.0023(2) 0.0487(14) Uani 1 1 d . . . H1A H 1.0017 0.8332 1.0288 0.073 Uiso 1 1 calc R . . H1B H 0.9734 0.7572 1.0156 0.073 Uiso 1 1 calc R . . H1C H 0.9464 0.8344 1.0056 0.073 Uiso 1 1 calc R . . C60 C 1.3710(2) 0.6984(3) 0.8333(3) 0.0778(18) Uani 1 1 d . . . H9 H 1.3393 0.6803 0.8130 0.093 Uiso 1 1 calc R . . H10 H 1.3928 0.6675 0.8185 0.093 Uiso 1 1 calc R . . C61 C 1.3725(2) 0.8698(3) 0.7275(3) 0.0798(18) Uani 1 1 d . . . H11 H 1.4061 0.8799 0.7437 0.096 Uiso 1 1 calc R . . H12 H 1.3649 0.8713 0.6817 0.096 Uiso 1 1 calc R . . C62 C 1.37511(19) 0.7816(4) 0.8130(3) 0.098(2) Uani 1 1 d . . . H13 H 1.3539 0.8132 0.8286 0.117 Uiso 1 1 calc R . . H14 H 1.4071 0.7995 0.8315 0.117 Uiso 1 1 calc R . . C63 C 1.3637(2) 0.7871(4) 0.7470(3) 0.105(2) Uani 1 1 d . . . H15 H 1.3308 0.7738 0.7287 0.126 Uiso 1 1 calc R . . H16 H 1.3829 0.7522 0.7311 0.126 Uiso 1 1 calc R . . C64 C 1.3474(3) 0.9318(4) 0.7475(3) 0.144(3) Uani 1 1 d . . . H17 H 1.3151 0.9321 0.7221 0.216 Uiso 1 1 calc R . . H18 H 1.3621 0.9788 0.7423 0.216 Uiso 1 1 calc R . . H19 H 1.3486 0.9253 0.7912 0.216 Uiso 1 1 calc R . . C65 C 1.3807(3) 0.6890(3) 0.9010(3) 0.118(3) Uani 1 1 d . . . H20 H 1.4118 0.7075 0.9216 0.177 Uiso 1 1 calc R . . H21 H 1.3788 0.6364 0.9107 0.177 Uiso 1 1 calc R . . H22 H 1.3579 0.7168 0.9158 0.177 Uiso 1 1 calc R . . C66 C 0.75683(19) 0.7827(2) 0.9838(3) 0.0752(17) Uani 1 1 d . . . H25 H 0.7414 0.8271 0.9946 0.090 Uiso 1 1 calc R . . H26 H 0.7906 0.7901 1.0008 0.090 Uiso 1 1 calc R . . C67 C 0.76231(18) 0.8440(3) 0.8851(3) 0.0769(17) Uani 1 1 d . . . H27 H 0.7494 0.8897 0.8968 0.115 Uiso 1 1 calc R . . H28 H 0.7519 0.8381 0.8399 0.115 Uiso 1 1 calc R . . H29 H 0.7962 0.8464 0.8988 0.115 Uiso 1 1 calc R . . C68 C 0.7461(2) 0.7790(3) 0.9153(3) 0.092(2) Uani 1 1 d . . . H23 H 0.7122 0.7744 0.8979 0.110 Uiso 1 1 calc R . . H24 H 0.7603 0.7336 0.9042 0.110 Uiso 1 1 calc R . . C69 C 0.9974(5) 0.7391(4) 0.7508(11) 0.129(5) Uani 0.50 1 d PGU A -1 H30 H 0.9918 0.7909 0.7502 0.155 Uiso 0.50 1 calc PR A -1 C70 C 0.9615(3) 0.6897(5) 0.7481(8) 0.059(4) Uani 0.50 1 d PGU A -1 H31 H 0.9314 0.7076 0.7456 0.071 Uiso 0.50 1 calc PR A -1 C71 C 0.9697(3) 0.6140(4) 0.7489(7) 0.080(5) Uani 0.50 1 d PGU A -1 C72 C 1.0138(3) 0.5877(4) 0.7525(7) 0.089(6) Uani 0.50 1 d PGU A -1 H32 H 1.0194 0.5360 0.7530 0.106 Uiso 0.50 1 calc PR A -1 C73 C 1.0496(3) 0.6372(7) 0.7552(5) 0.104(7) Uani 0.50 1 d PGU A -1 H33 H 1.0798 0.6192 0.7576 0.125 Uiso 0.50 1 calc PR A -1 C74 C 1.0414(4) 0.7129(6) 0.7544(9) 0.127(7) Uani 0.50 1 d PGU A -1 H34 H 1.0660 0.7467 0.7562 0.152 Uiso 0.50 1 calc PR A -1 C75 C 0.9360(5) 0.5602(8) 0.7449(6) 0.126(6) Uani 0.50 1 d PU A -1 H35 H 0.9407 0.5199 0.7181 0.189 Uiso 0.50 1 calc PR A -1 H36 H 0.9053 0.5819 0.7274 0.189 Uiso 0.50 1 calc PR A -1 H37 H 0.9384 0.5407 0.7864 0.189 Uiso 0.50 1 calc PR A -1 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 0.038(2) 0.031(3) 0.040(3) -0.001(2) 0.014(2) 0.000(2) C2 0.046(3) 0.030(3) 0.047(3) -0.005(2) 0.018(2) -0.004(2) C3 0.035(2) 0.035(3) 0.042(3) -0.003(2) 0.009(2) 0.003(2) C4 0.040(3) 0.027(3) 0.039(3) 0.000(2) 0.008(2) 0.006(2) C5 0.048(3) 0.031(3) 0.037(3) 0.001(2) 0.013(2) 0.001(2) C6 0.047(3) 0.028(3) 0.039(3) 0.001(2) 0.011(2) 0.001(2) C7 0.048(3) 0.035(3) 0.052(3) 0.000(2) 0.015(2) -0.004(2) C8 0.049(3) 0.034(3) 0.056(3) -0.003(2) 0.020(2) 0.002(2) C9 0.047(3) 0.027(3) 0.042(3) -0.003(2) 0.011(2) -0.003(2) C10 0.045(3) 0.027(3) 0.040(3) -0.001(2) 0.010(2) -0.001(2) C11 0.045(3) 0.028(3) 0.039(3) -0.002(2) 0.013(2) -0.002(2) C12 0.038(3) 0.030(3) 0.044(3) 0.001(2) 0.015(2) 0.000(2) C13 0.039(3) 0.036(3) 0.037(3) 0.003(2) 0.012(2) 0.004(2) C14 0.043(3) 0.031(3) 0.035(2) 0.002(2) 0.007(2) -0.003(2) C15 0.043(3) 0.030(3) 0.033(2) 0.0004(19) 0.013(2) -0.001(2) C16 0.041(3) 0.032(3) 0.037(2) -0.004(2) 0.013(2) -0.001(2) C17 0.037(3) 0.038(3) 0.044(3) 0.001(2) 0.013(2) 0.002(2) C18 0.044(3) 0.038(3) 0.041(3) 0.001(2) 0.012(2) 0.005(2) C19 0.041(3) 0.032(3) 0.038(3) -0.008(2) 0.009(2) -0.001(2) C20 0.044(3) 0.029(3) 0.036(2) 0.002(2) 0.009(2) 0.001(2) C21 0.038(3) 0.033(3) 0.039(3) 0.001(2) 0.011(2) -0.003(2) C22 0.041(3) 0.034(3) 0.036(2) 0.002(2) 0.013(2) 0.000(2) C23 0.043(3) 0.029(3) 0.035(2) -0.0018(19) 0.013(2) -0.001(2) C24 0.044(3) 0.032(3) 0.032(2) -0.0016(19) 0.008(2) 0.001(2) C25 0.039(2) 0.032(3) 0.031(2) -0.0048(19) 0.0085(19) -0.004(2) C26 0.040(3) 0.027(3) 0.048(3) 0.004(2) 0.007(2) 0.000(2) C27 0.047(3) 0.039(3) 0.050(3) -0.003(2) 0.017(2) -0.001(2) C28 0.046(3) 0.035(3) 0.082(4) -0.008(3) 0.029(3) 0.004(2) C29 0.042(3) 0.038(3) 0.077(4) 0.012(3) 0.008(3) 0.007(2) C30 0.051(3) 0.041(3) 0.054(3) 0.008(2) 0.007(3) -0.002(2) C31 0.046(3) 0.027(3) 0.054(3) 0.000(2) 0.017(2) -0.001(2) C32 0.043(3) 0.031(3) 0.053(3) -0.005(2) 0.018(2) 0.000(2) C33 0.055(3) 0.034(3) 0.050(3) -0.002(2) 0.022(2) 0.006(2) C34 0.062(3) 0.036(3) 0.066(4) 0.005(3) 0.033(3) -0.001(3) C35 0.053(3) 0.035(3) 0.081(4) -0.013(3) 0.030(3) -0.013(2) C36 0.044(3) 0.048(3) 0.061(3) -0.015(3) 0.014(3) -0.008(2) C37 0.057(3) 0.041(3) 0.050(3) -0.003(2) 0.019(3) -0.007(2) C38 0.037(3) 0.034(3) 0.039(3) 0.000(2) 0.008(2) 0.002(2) C39 0.045(3) 0.037(3) 0.043(3) -0.001(2) 0.015(2) 0.003(2) C40 0.046(3) 0.032(3) 0.045(3) -0.001(2) 0.008(2) -0.006(2) C41 0.034(3) 0.037(3) 0.057(3) 0.006(2) 0.011(2) -0.005(2) C42 0.038(3) 0.040(3) 0.050(3) 0.005(2) 0.018(2) 0.001(2) C43 0.044(3) 0.030(3) 0.044(3) 0.000(2) 0.005(2) -0.006(2) C44 0.036(3) 0.029(3) 0.043(3) 0.000(2) 0.013(2) -0.004(2) C45 0.040(3) 0.038(3) 0.045(3) 0.001(2) 0.011(2) -0.006(2) C46 0.048(3) 0.027(3) 0.056(3) 0.002(2) 0.023(2) 0.003(2) C47 0.048(3) 0.029(3) 0.053(3) -0.005(2) 0.022(2) -0.007(2) C48 0.043(3) 0.034(3) 0.047(3) -0.006(2) 0.015(2) -0.006(2) C49 0.044(3) 0.029(3) 0.044(3) 0.004(2) 0.013(2) 0.002(2) C50 0.041(3) 0.031(3) 0.036(2) -0.001(2) 0.010(2) -0.004(2) C51 0.043(3) 0.027(3) 0.040(3) -0.003(2) 0.012(2) 0.001(2) C52 0.042(3) 0.041(3) 0.039(3) -0.004(2) 0.015(2) -0.007(2) C53 0.050(3) 0.029(3) 0.038(3) 0.001(2) 0.010(2) -0.006(2) C54 0.041(3) 0.026(3) 0.039(3) -0.0009(19) 0.006(2) 0.002(2) C55 0.038(3) 0.030(3) 0.041(3) -0.004(2) 0.009(2) -0.006(2) N1 0.040(2) 0.028(2) 0.044(2) -0.0002(17) 0.0111(17) -0.0029(17) N2 0.046(2) 0.026(2) 0.049(2) 0.0016(17) 0.0135(18) -0.0040(18) N3 0.040(2) 0.028(2) 0.042(2) 0.0021(17) 0.0108(17) 0.0000(17) N4 0.045(2) 0.031(2) 0.042(2) -0.0007(17) 0.0141(17) -0.0037(18) N5 0.045(2) 0.027(2) 0.041(2) -0.0008(16) 0.0139(17) -0.0045(17) F1 0.0614(18) 0.0547(18) 0.0554(17) -0.0092(14) 0.0201(14) 0.0027(14) F2 0.0670(19) 0.0572(19) 0.098(2) -0.0015(17) 0.0397(17) 0.0176(15) F3 0.0541(18) 0.063(2) 0.102(2) 0.0167(17) 0.0150(17) 0.0163(15) F4 0.0593(17) 0.0545(18) 0.0628(19) 0.0106(14) 0.0025(15) -0.0030(14) F5 0.0596(17) 0.0423(16) 0.0504(16) -0.0022(13) 0.0136(13) -0.0002(13) F6 0.0609(17) 0.0456(17) 0.0514(16) 0.0072(13) 0.0177(14) 0.0026(13) F7 0.081(2) 0.0492(18) 0.086(2) 0.0133(16) 0.0460(17) -0.0022(15) F8 0.0660(19) 0.0510(19) 0.113(2) -0.0157(17) 0.0429(18) -0.0239(15) F9 0.0579(18) 0.070(2) 0.079(2) -0.0155(16) 0.0115(16) -0.0180(15) F10 0.0615(17) 0.0542(18) 0.0505(17) -0.0018(14) 0.0083(14) -0.0081(14) F11 0.0494(15) 0.0447(16) 0.0467(15) -0.0034(12) 0.0159(13) -0.0029(12) F12 0.0494(16) 0.0492(17) 0.0604(17) -0.0080(13) 0.0125(13) -0.0140(13) F13 0.0461(16) 0.0478(17) 0.0723(18) -0.0019(13) 0.0243(14) -0.0126(13) F14 0.0541(16) 0.0528(17) 0.0520(16) 0.0008(13) 0.0249(13) -0.0001(13) F15 0.0464(15) 0.0439(16) 0.0447(15) -0.0063(12) 0.0154(12) -0.0060(12) F16 0.0474(15) 0.0346(15) 0.0581(16) 0.0018(12) 0.0060(13) 0.0024(12) F17 0.0554(17) 0.0370(16) 0.0666(18) 0.0010(13) 0.0175(14) 0.0073(13) F18 0.0611(17) 0.0315(15) 0.0757(19) -0.0127(13) 0.0261(15) -0.0034(13) F19 0.0500(16) 0.0398(16) 0.0574(16) -0.0125(12) 0.0151(13) -0.0080(12) F20 0.0443(15) 0.0363(15) 0.0494(15) -0.0006(12) 0.0100(12) 0.0018(12) F21 0.0458(15) 0.0370(15) 0.0541(16) 0.0011(12) 0.0188(12) 0.0014(12) F22 0.0452(15) 0.0421(16) 0.0529(16) -0.0038(12) 0.0179(12) -0.0085(12) F23 0.0513(15) 0.0296(14) 0.0510(15) 0.0020(12) 0.0169(12) -0.0061(12) F24 0.0483(15) 0.0335(15) 0.0509(15) 0.0041(12) 0.0163(12) 0.0001(12) P1 0.0412(7) 0.0289(7) 0.0435(7) -0.0012(5) 0.0125(5) -0.0019(5) B1 0.065(4) 0.042(4) 0.040(3) 0.001(3) 0.015(3) 0.006(3) C60 0.115(5) 0.044(4) 0.090(5) -0.006(3) 0.055(4) 0.003(3) C61 0.090(4) 0.085(5) 0.070(4) 0.015(4) 0.032(3) 0.029(4) C62 0.053(4) 0.167(7) 0.078(5) -0.030(5) 0.025(3) 0.009(4) C63 0.067(4) 0.158(7) 0.082(5) -0.031(5) 0.009(4) 0.028(4) C64 0.242(9) 0.126(6) 0.066(5) 0.018(4) 0.046(5) 0.087(6) C65 0.184(8) 0.074(5) 0.107(6) 0.003(4) 0.059(6) 0.021(5) C66 0.074(4) 0.070(4) 0.077(4) 0.003(3) 0.014(3) -0.015(3) C67 0.073(4) 0.075(4) 0.091(4) 0.012(3) 0.036(3) -0.012(3) C68 0.105(5) 0.086(5) 0.083(5) 0.010(4) 0.025(4) -0.026(4) C69 0.094(8) 0.266(13) 0.029(5) 0.004(16) 0.018(7) -0.100(14) C70 0.074(9) 0.054(8) 0.051(9) 0.000(7) 0.018(7) -0.036(6) C71 0.036(10) 0.159(13) 0.047(8) 0.001(11) 0.017(7) -0.021(10) C72 0.062(15) 0.163(11) 0.037(6) 0.015(10) 0.009(11) 0.026(8) C73 0.059(10) 0.212(18) 0.045(8) -0.012(13) 0.020(8) -0.016(13) C74 0.144(14) 0.204(16) 0.029(8) -0.016(12) 0.019(11) -0.068(14) C75 0.164(16) 0.157(14) 0.057(8) 0.018(10) 0.030(10) 0.064(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(5) . ? C1 N1 1.413(4) . ? C1 C25 1.443(5) . ? C2 C3 1.390(5) . ? C2 H1 0.9500 . ? C3 C4 1.356(5) . ? C3 H2 0.9500 . ? C4 N1 1.417(4) . ? C4 C5 1.470(5) . ? C5 C6 1.343(5) . ? C5 C26 1.469(5) . ? C6 N2 1.423(5) . ? C6 C7 1.496(5) . ? C7 C8 1.544(5) . ? C7 H3 0.9900 . ? C7 H4 0.9900 . ? C8 C9 1.503(5) . ? C8 H5 0.9900 . ? C8 H6 0.9900 . ? C9 C10 1.353(5) . ? C9 N2 1.415(5) . ? C10 C11 1.440(5) . ? C10 C32 1.485(5) . ? C11 N3 1.347(5) . ? C11 C12 1.423(5) . ? C12 C13 1.386(5) . ? C12 P1 1.764(4) . ? C13 C23 1.402(5) . ? C13 C14 1.492(5) . ? C14 N3 1.355(4) . ? C14 C15 1.427(5) . ? C15 C16 1.387(5) . ? C15 C38 1.494(5) . ? C16 N4 1.396(5) . ? C16 C17 1.421(5) . ? C17 C18 1.375(5) . ? C17 H7 0.9500 . ? C18 C19 1.431(5) . ? C18 H8 0.9500 . ? C19 N4 1.375(5) . ? C19 C20 1.451(5) . ? C20 C21 1.410(5) . ? C20 C44 1.466(5) . ? C21 C22 1.398(5) . ? C21 N5 1.405(5) . ? C22 N4 1.354(5) . ? C22 C23 1.362(5) . ? C23 C24 1.466(5) . ? C24 C25 1.389(5) . ? C24 N5 1.424(5) . ? C25 C50 1.467(5) . ? C26 C31 1.390(5) . ? C26 C27 1.404(5) . ? C27 F1 1.341(5) . ? C27 C28 1.363(6) . ? C28 F2 1.344(5) . ? C28 C29 1.388(6) . ? C29 F3 1.329(5) . ? C29 C30 1.377(6) . ? C30 F4 1.351(5) . ? C30 C31 1.368(5) . ? C31 F5 1.350(4) . ? C32 C33 1.383(6) . ? C32 C37 1.400(6) . ? C33 F6 1.358(5) . ? C33 C34 1.369(6) . ? C34 F7 1.350(5) . ? C34 C35 1.364(6) . ? C35 F8 1.350(5) . ? C35 C36 1.382(6) . ? C36 F9 1.349(5) . ? C36 C37 1.356(6) . ? C37 F10 1.348(5) . ? C38 C39 1.382(5) . ? C38 C43 1.389(5) . ? C39 F11 1.350(4) . ? C39 C40 1.372(5) . ? C40 F12 1.335(4) . ? C40 C41 1.395(6) . ? C41 F13 1.333(4) . ? C41 C42 1.365(5) . ? C42 F14 1.361(4) . ? C42 C43 1.372(5) . ? C43 F15 1.349(4) . ? C44 C49 1.379(5) . ? C44 C45 1.386(5) . ? C45 F16 1.357(4) . ? C45 C46 1.386(5) . ? C46 F17 1.350(4) . ? C46 C47 1.369(6) . ? C47 F18 1.344(4) . ? C47 C48 1.369(5) . ? C48 F19 1.344(4) . ? C48 C49 1.373(5) . ? C49 F20 1.346(4) . ? C50 C51 1.403(5) . ? C50 C55 1.424(5) . ? C51 F21 1.344(4) . ? C51 C52 1.377(5) . ? C52 F22 1.347(4) . ? C52 C53 1.387(5) . ? C53 F23 1.351(4) . ? C53 C54 1.359(5) . ? C54 F24 1.360(4) . ? C54 C55 1.372(5) . ? C55 N5 1.381(5) . ? N1 P1 1.713(3) . ? N2 P1 1.690(3) . ? P1 B1 1.853(5) . ? B1 H1A 0.9800 . ? B1 H1B 0.9800 . ? B1 H1C 0.9800 . ? C60 C65 1.476(7) . ? C60 C62 1.588(7) . ? C60 H9 0.9900 . ? C60 H10 0.9900 . ? C61 C64 1.490(7) . ? C61 C63 1.601(7) . ? C61 H11 0.9900 . ? C61 H12 0.9900 . ? C62 C63 1.428(7) . ? C62 H13 0.9900 . ? C62 H14 0.9900 . ? C63 H15 0.9900 . ? C63 H16 0.9900 . ? C64 H17 0.9800 . ? C64 H18 0.9800 . ? C64 H19 0.9800 . ? C65 H20 0.9800 . ? C65 H21 0.9800 . ? C65 H22 0.9800 . ? C66 C68 1.482(7) . ? C66 C66 1.505(8) 7_667 ? C66 H25 0.9900 . ? C66 H26 0.9900 . ? C67 C68 1.505(6) . ? C67 H27 0.9800 . ? C67 H28 0.9800 . ? C67 H29 0.9800 . ? C68 H23 0.9900 . ? C68 H24 0.9900 . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C69 H30 0.9500 . ? C70 C71 1.3900 . ? C70 H31 0.9500 . ? C71 C72 1.3900 . ? C71 C75 1.390(17) . ? C72 C73 1.3900 . ? C72 H32 0.9500 . ? C73 C74 1.3900 . ? C73 H33 0.9500 . ? C74 H34 0.9500 . ? C75 H35 0.9800 . ? C75 H36 0.9800 . ? C75 H37 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 106.9(4) . . ? C2 C1 C25 123.9(4) . . ? N1 C1 C25 128.9(4) . . ? C1 C2 C3 109.0(4) . . ? C1 C2 H1 125.5 . . ? C3 C2 H1 125.5 . . ? C4 C3 C2 108.7(4) . . ? C4 C3 H2 125.7 . . ? C2 C3 H2 125.7 . . ? C3 C4 N1 108.4(3) . . ? C3 C4 C5 129.2(4) . . ? N1 C4 C5 122.1(4) . . ? C6 C5 C26 120.4(4) . . ? C6 C5 C4 121.6(4) . . ? C26 C5 C4 118.0(4) . . ? C5 C6 N2 120.6(4) . . ? C5 C6 C7 131.1(4) . . ? N2 C6 C7 108.3(4) . . ? C6 C7 C8 103.2(3) . . ? C6 C7 H3 111.1 . . ? C8 C7 H3 111.1 . . ? C6 C7 H4 111.1 . . ? C8 C7 H4 111.1 . . ? H3 C7 H4 109.1 . . ? C9 C8 C7 105.8(3) . . ? C9 C8 H5 110.6 . . ? C7 C8 H5 110.6 . . ? C9 C8 H6 110.6 . . ? C7 C8 H6 110.6 . . ? H5 C8 H6 108.7 . . ? C10 C9 N2 122.0(4) . . ? C10 C9 C8 129.8(4) . . ? N2 C9 C8 108.0(4) . . ? C9 C10 C11 119.5(4) . . ? C9 C10 C32 120.8(4) . . ? C11 C10 C32 119.5(4) . . ? N3 C11 C12 112.1(4) . . ? N3 C11 C10 122.5(4) . . ? C12 C11 C10 125.3(4) . . ? C13 C12 C11 106.5(4) . . ? C13 C12 P1 132.3(3) . . ? C11 C12 P1 120.2(3) . . ? C12 C13 C23 129.7(4) . . ? C12 C13 C14 104.8(4) . . ? C23 C13 C14 125.4(4) . . ? N3 C14 C15 117.5(4) . . ? N3 C14 C13 109.4(4) . . ? C15 C14 C13 133.1(4) . . ? C16 C15 C14 128.0(4) . . ? C16 C15 C38 115.8(4) . . ? C14 C15 C38 116.2(4) . . ? C15 C16 N4 120.4(4) . . ? C15 C16 C17 136.2(4) . . ? N4 C16 C17 103.4(3) . . ? C18 C17 C16 109.9(4) . . ? C18 C17 H7 125.0 . . ? C16 C17 H7 125.0 . . ? C17 C18 C19 108.8(4) . . ? C17 C18 H8 125.6 . . ? C19 C18 H8 125.6 . . ? N4 C19 C18 104.2(4) . . ? N4 C19 C20 107.5(4) . . ? C18 C19 C20 148.1(4) . . ? C21 C20 C19 104.8(3) . . ? C21 C20 C44 132.3(4) . . ? C19 C20 C44 121.7(4) . . ? C22 C21 N5 103.1(3) . . ? C22 C21 C20 109.1(4) . . ? N5 C21 C20 147.6(4) . . ? N4 C22 C23 135.4(4) . . ? N4 C22 C21 108.0(4) . . ? C23 C22 C21 116.5(4) . . ? C22 C23 C13 121.8(4) . . ? C22 C23 C24 102.7(4) . . ? C13 C23 C24 135.5(4) . . ? C25 C24 N5 109.8(4) . . ? C25 C24 C23 142.7(4) . . ? N5 C24 C23 107.5(4) . . ? C24 C25 C1 132.7(4) . . ? C24 C25 C50 104.7(4) . . ? C1 C25 C50 121.7(4) . . ? C31 C26 C27 115.2(4) . . ? C31 C26 C5 122.4(4) . . ? C27 C26 C5 122.3(4) . . ? F1 C27 C28 118.5(4) . . ? F1 C27 C26 118.6(4) . . ? C28 C27 C26 122.8(5) . . ? F2 C28 C27 120.6(5) . . ? F2 C28 C29 119.3(5) . . ? C27 C28 C29 120.1(5) . . ? F3 C29 C30 121.1(5) . . ? F3 C29 C28 120.3(5) . . ? C30 C29 C28 118.6(5) . . ? F4 C30 C31 120.7(5) . . ? F4 C30 C29 118.7(4) . . ? C31 C30 C29 120.6(5) . . ? F5 C31 C30 118.0(4) . . ? F5 C31 C26 119.3(4) . . ? C30 C31 C26 122.7(4) . . ? C33 C32 C37 115.0(4) . . ? C33 C32 C10 124.6(4) . . ? C37 C32 C10 120.4(4) . . ? F6 C33 C34 117.7(4) . . ? F6 C33 C32 119.3(4) . . ? C34 C33 C32 123.0(5) . . ? F7 C34 C35 120.5(5) . . ? F7 C34 C33 119.9(5) . . ? C35 C34 C33 119.6(5) . . ? F8 C35 C34 119.4(5) . . ? F8 C35 C36 120.7(5) . . ? C34 C35 C36 120.0(5) . . ? F9 C36 C37 121.6(5) . . ? F9 C36 C35 119.2(4) . . ? C37 C36 C35 119.1(5) . . ? F10 C37 C36 118.3(5) . . ? F10 C37 C32 118.5(4) . . ? C36 C37 C32 123.2(5) . . ? C39 C38 C43 116.5(4) . . ? C39 C38 C15 122.3(4) . . ? C43 C38 C15 121.3(4) . . ? F11 C39 C40 116.8(4) . . ? F11 C39 C38 120.4(4) . . ? C40 C39 C38 122.7(4) . . ? F12 C40 C39 120.9(4) . . ? F12 C40 C41 119.9(4) . . ? C39 C40 C41 119.2(4) . . ? F13 C41 C42 120.8(4) . . ? F13 C41 C40 120.0(4) . . ? C42 C41 C40 119.2(4) . . ? F14 C42 C41 119.2(4) . . ? F14 C42 C43 120.2(4) . . ? C41 C42 C43 120.6(4) . . ? F15 C43 C42 118.6(4) . . ? F15 C43 C38 119.5(4) . . ? C42 C43 C38 121.8(4) . . ? C49 C44 C45 115.8(4) . . ? C49 C44 C20 121.1(4) . . ? C45 C44 C20 122.6(4) . . ? F16 C45 C46 117.2(4) . . ? F16 C45 C44 120.3(4) . . ? C46 C45 C44 122.5(4) . . ? F17 C46 C47 120.7(4) . . ? F17 C46 C45 120.1(4) . . ? C47 C46 C45 119.2(4) . . ? F18 C47 C46 119.4(4) . . ? F18 C47 C48 120.8(4) . . ? C46 C47 C48 119.9(4) . . ? F19 C48 C47 119.2(4) . . ? F19 C48 C49 121.1(4) . . ? C47 C48 C49 119.7(4) . . ? F20 C49 C48 117.8(4) . . ? F20 C49 C44 119.2(4) . . ? C48 C49 C44 122.8(4) . . ? C51 C50 C55 116.6(4) . . ? C51 C50 C25 134.1(4) . . ? C55 C50 C25 108.9(4) . . ? F21 C51 C52 116.5(4) . . ? F21 C51 C50 122.8(4) . . ? C52 C51 C50 120.6(4) . . ? F22 C52 C51 119.6(4) . . ? F22 C52 C53 119.8(4) . . ? C51 C52 C53 120.6(4) . . ? F23 C53 C54 120.3(4) . . ? F23 C53 C52 119.0(4) . . ? C54 C53 C52 120.5(4) . . ? C53 C54 F24 119.8(4) . . ? C53 C54 C55 119.7(4) . . ? F24 C54 C55 120.3(4) . . ? C54 C55 N5 130.9(4) . . ? C54 C55 C50 121.9(4) . . ? N5 C55 C50 106.9(4) . . ? C1 N1 C4 107.0(3) . . ? C1 N1 P1 128.1(3) . . ? C4 N1 P1 122.4(3) . . ? C9 N2 C6 109.8(3) . . ? C9 N2 P1 126.2(3) . . ? C6 N2 P1 123.6(3) . . ? C11 N3 C14 107.2(3) . . ? C22 N4 C19 110.4(4) . . ? C22 N4 C16 135.5(4) . . ? C19 N4 C16 113.6(4) . . ? C55 N5 C21 141.0(4) . . ? C55 N5 C24 109.1(3) . . ? C21 N5 C24 109.9(3) . . ? N2 P1 N1 98.51(17) . . ? N2 P1 C12 97.18(19) . . ? N1 P1 C12 112.96(18) . . ? N2 P1 B1 116.5(2) . . ? N1 P1 B1 111.4(2) . . ? C12 P1 B1 117.9(2) . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? C65 C60 C62 113.3(5) . . ? C65 C60 H9 108.9 . . ? C62 C60 H9 108.9 . . ? C65 C60 H10 108.9 . . ? C62 C60 H10 108.9 . . ? H9 C60 H10 107.7 . . ? C64 C61 C63 118.9(5) . . ? C64 C61 H11 107.6 . . ? C63 C61 H11 107.6 . . ? C64 C61 H12 107.6 . . ? C63 C61 H12 107.6 . . ? H11 C61 H12 107.0 . . ? C63 C62 C60 110.4(6) . . ? C63 C62 H13 109.6 . . ? C60 C62 H13 109.6 . . ? C63 C62 H14 109.6 . . ? C60 C62 H14 109.6 . . ? H13 C62 H14 108.1 . . ? C62 C63 C61 109.8(6) . . ? C62 C63 H15 109.7 . . ? C61 C63 H15 109.7 . . ? C62 C63 H16 109.7 . . ? C61 C63 H16 109.7 . . ? H15 C63 H16 108.2 . . ? C61 C64 H17 109.5 . . ? C61 C64 H18 109.5 . . ? H17 C64 H18 109.5 . . ? C61 C64 H19 109.5 . . ? H17 C64 H19 109.5 . . ? H18 C64 H19 109.5 . . ? C60 C65 H20 109.5 . . ? C60 C65 H21 109.5 . . ? H20 C65 H21 109.5 . . ? C60 C65 H22 109.5 . . ? H20 C65 H22 109.5 . . ? H21 C65 H22 109.5 . . ? C68 C66 C66 117.2(6) . 7_667 ? C68 C66 H25 108.0 . . ? C66 C66 H25 108.0 7_667 . ? C68 C66 H26 108.0 . . ? C66 C66 H26 108.0 7_667 . ? H25 C66 H26 107.2 . . ? C68 C67 H27 109.5 . . ? C68 C67 H28 109.5 . . ? H27 C67 H28 109.5 . . ? C68 C67 H29 109.5 . . ? H27 C67 H29 109.5 . . ? H28 C67 H29 109.5 . . ? C66 C68 C67 115.5(5) . . ? C66 C68 H23 108.4 . . ? C67 C68 H23 108.4 . . ? C66 C68 H24 108.4 . . ? C67 C68 H24 108.4 . . ? H23 C68 H24 107.5 . . ? C70 C69 C74 120.0 . . ? C70 C69 H30 120.0 . . ? C74 C69 H30 120.0 . . ? C69 C70 C71 120.0 . . ? C69 C70 H31 120.0 . . ? C71 C70 H31 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 C75 115.6(9) . . ? C70 C71 C75 124.4(9) . . ? C71 C72 C73 120.0 . . ? C71 C72 H32 120.0 . . ? C73 C72 H32 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H33 120.0 . . ? C72 C73 H33 120.0 . . ? C73 C74 C69 120.0 . . ? C73 C74 H34 120.0 . . ? C69 C74 H34 120.0 . . ? 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 N1 C1 C2 C3 -3.0(5) . . . . ? C25 C1 C2 C3 -177.5(4) . . . . ? C1 C2 C3 C4 1.1(5) . . . . ? C2 C3 C4 N1 1.3(5) . . . . ? C2 C3 C4 C5 -172.5(4) . . . . ? C3 C4 C5 C6 -179.1(4) . . . . ? N1 C4 C5 C6 7.8(6) . . . . ? C3 C4 C5 C26 1.1(7) . . . . ? N1 C4 C5 C26 -171.9(4) . . . . ? C26 C5 C6 N2 -176.9(4) . . . . ? C4 C5 C6 N2 3.4(6) . . . . ? C26 C5 C6 C7 -0.5(7) . . . . ? C4 C5 C6 C7 179.8(4) . . . . ? C5 C6 C7 C8 -154.9(5) . . . . ? N2 C6 C7 C8 21.8(4) . . . . ? C6 C7 C8 C9 -14.1(5) . . . . ? C7 C8 C9 C10 177.8(4) . . . . ? C7 C8 C9 N2 1.9(5) . . . . ? N2 C9 C10 C11 3.5(6) . . . . ? C8 C9 C10 C11 -171.9(4) . . . . ? N2 C9 C10 C32 179.3(4) . . . . ? C8 C9 C10 C32 4.0(7) . . . . ? C9 C10 C11 N3 170.0(4) . . . . ? C32 C10 C11 N3 -5.9(6) . . . . ? C9 C10 C11 C12 -7.6(6) . . . . ? C32 C10 C11 C12 176.5(4) . . . . ? N3 C11 C12 C13 -0.3(5) . . . . ? C10 C11 C12 C13 177.5(4) . . . . ? N3 C11 C12 P1 170.0(3) . . . . ? C10 C11 C12 P1 -12.3(6) . . . . ? C11 C12 C13 C23 -175.4(4) . . . . ? P1 C12 C13 C23 16.0(7) . . . . ? C11 C12 C13 C14 1.5(4) . . . . ? P1 C12 C13 C14 -167.1(3) . . . . ? C12 C13 C14 N3 -2.3(5) . . . . ? C23 C13 C14 N3 174.7(4) . . . . ? C12 C13 C14 C15 179.0(4) . . . . ? C23 C13 C14 C15 -4.0(8) . . . . ? N3 C14 C15 C16 179.3(4) . . . . ? C13 C14 C15 C16 -2.0(8) . . . . ? N3 C14 C15 C38 -0.8(5) . . . . ? C13 C14 C15 C38 177.8(4) . . . . ? C14 C15 C16 N4 1.8(6) . . . . ? C38 C15 C16 N4 -178.0(4) . . . . ? C14 C15 C16 C17 178.8(4) . . . . ? C38 C15 C16 C17 -1.1(7) . . . . ? C15 C16 C17 C18 -175.3(4) . . . . ? N4 C16 C17 C18 2.0(4) . . . . ? C16 C17 C18 C19 -0.1(5) . . . . ? C17 C18 C19 N4 -1.9(4) . . . . ? C17 C18 C19 C20 172.5(6) . . . . ? N4 C19 C20 C21 -2.6(4) . . . . ? C18 C19 C20 C21 -176.9(6) . . . . ? N4 C19 C20 C44 166.3(3) . . . . ? C18 C19 C20 C44 -8.0(10) . . . . ? C19 C20 C21 C22 4.0(5) . . . . ? C44 C20 C21 C22 -163.1(4) . . . . ? C19 C20 C21 N5 177.7(6) . . . . ? C44 C20 C21 N5 10.5(10) . . . . ? N5 C21 C22 N4 179.4(3) . . . . ? C20 C21 C22 N4 -4.1(5) . . . . ? N5 C21 C22 C23 -2.6(5) . . . . ? C20 C21 C22 C23 173.9(4) . . . . ? N4 C22 C23 C13 -3.2(8) . . . . ? C21 C22 C23 C13 179.5(4) . . . . ? N4 C22 C23 C24 176.3(5) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C12 C13 C23 C22 -176.8(4) . . . . ? C14 C13 C23 C22 7.0(6) . . . . ? C12 C13 C23 C24 3.9(8) . . . . ? C14 C13 C23 C24 -172.4(4) . . . . ? C22 C23 C24 C25 -173.4(5) . . . . ? C13 C23 C24 C25 6.0(9) . . . . ? C22 C23 C24 N5 4.2(4) . . . . ? C13 C23 C24 N5 -176.4(4) . . . . ? N5 C24 C25 C1 -161.2(4) . . . . ? C23 C24 C25 C1 16.3(9) . . . . ? N5 C24 C25 C50 7.7(4) . . . . ? C23 C24 C25 C50 -174.8(5) . . . . ? C2 C1 C25 C24 142.4(5) . . . . ? N1 C1 C25 C24 -30.9(7) . . . . ? C2 C1 C25 C50 -25.0(6) . . . . ? N1 C1 C25 C50 161.7(4) . . . . ? C6 C5 C26 C31 114.2(5) . . . . ? C4 C5 C26 C31 -66.0(5) . . . . ? C6 C5 C26 C27 -62.2(6) . . . . ? C4 C5 C26 C27 117.5(4) . . . . ? C31 C26 C27 F1 178.6(4) . . . . ? C5 C26 C27 F1 -4.8(6) . . . . ? C31 C26 C27 C28 0.7(6) . . . . ? C5 C26 C27 C28 177.4(4) . . . . ? F1 C27 C28 F2 1.5(6) . . . . ? C26 C27 C28 F2 179.3(4) . . . . ? F1 C27 C28 C29 -179.0(4) . . . . ? C26 C27 C28 C29 -1.2(7) . . . . ? F2 C28 C29 F3 0.3(7) . . . . ? C27 C28 C29 F3 -179.2(4) . . . . ? F2 C28 C29 C30 -178.7(4) . . . . ? C27 C28 C29 C30 1.8(7) . . . . ? F3 C29 C30 F4 0.8(7) . . . . ? C28 C29 C30 F4 179.8(4) . . . . ? F3 C29 C30 C31 179.0(4) . . . . ? C28 C29 C30 C31 -2.0(7) . . . . ? F4 C30 C31 F5 0.6(6) . . . . ? C29 C30 C31 F5 -177.5(4) . . . . ? F4 C30 C31 C26 179.8(4) . . . . ? C29 C30 C31 C26 1.6(7) . . . . ? C27 C26 C31 F5 178.2(4) . . . . ? C5 C26 C31 F5 1.5(6) . . . . ? C27 C26 C31 C30 -1.0(6) . . . . ? C5 C26 C31 C30 -177.6(4) . . . . ? C9 C10 C32 C33 -62.1(6) . . . . ? C11 C10 C32 C33 113.8(5) . . . . ? C9 C10 C32 C37 120.4(5) . . . . ? C11 C10 C32 C37 -63.7(6) . . . . ? C37 C32 C33 F6 176.5(4) . . . . ? C10 C32 C33 F6 -1.1(6) . . . . ? C37 C32 C33 C34 -2.2(6) . . . . ? C10 C32 C33 C34 -179.8(4) . . . . ? F6 C33 C34 F7 2.1(6) . . . . ? C32 C33 C34 F7 -179.1(4) . . . . ? F6 C33 C34 C35 -176.9(4) . . . . ? C32 C33 C34 C35 1.8(7) . . . . ? F7 C34 C35 F8 0.8(7) . . . . ? C33 C34 C35 F8 179.9(4) . . . . ? F7 C34 C35 C36 -179.2(4) . . . . ? C33 C34 C35 C36 -0.2(7) . . . . ? F8 C35 C36 F9 -0.9(7) . . . . ? C34 C35 C36 F9 179.1(4) . . . . ? F8 C35 C36 C37 179.0(4) . . . . ? C34 C35 C36 C37 -1.0(7) . . . . ? F9 C36 C37 F10 0.2(7) . . . . ? C35 C36 C37 F10 -179.7(4) . . . . ? F9 C36 C37 C32 -179.5(4) . . . . ? C35 C36 C37 C32 0.5(7) . . . . ? C33 C32 C37 F10 -178.7(4) . . . . ? C10 C32 C37 F10 -1.0(6) . . . . ? C33 C32 C37 C36 1.0(7) . . . . ? C10 C32 C37 C36 178.8(4) . . . . ? C16 C15 C38 C39 -118.8(4) . . . . ? C14 C15 C38 C39 61.3(5) . . . . ? C16 C15 C38 C43 61.2(5) . . . . ? C14 C15 C38 C43 -118.6(4) . . . . ? C43 C38 C39 F11 -176.7(4) . . . . ? C15 C38 C39 F11 3.4(6) . . . . ? C43 C38 C39 C40 2.3(6) . . . . ? C15 C38 C39 C40 -177.6(4) . . . . ? F11 C39 C40 F12 -1.3(6) . . . . ? C38 C39 C40 F12 179.6(4) . . . . ? F11 C39 C40 C41 177.6(4) . . . . ? C38 C39 C40 C41 -1.4(7) . . . . ? F12 C40 C41 F13 -0.4(6) . . . . ? C39 C40 C41 F13 -179.4(4) . . . . ? F12 C40 C41 C42 179.1(4) . . . . ? C39 C40 C41 C42 0.1(7) . . . . ? F13 C41 C42 F14 -0.1(6) . . . . ? C40 C41 C42 F14 -179.6(4) . . . . ? F13 C41 C42 C43 179.6(4) . . . . ? C40 C41 C42 C43 0.1(7) . . . . ? F14 C42 C43 F15 -1.7(6) . . . . ? C41 C42 C43 F15 178.6(4) . . . . ? F14 C42 C43 C38 -179.4(4) . . . . ? C41 C42 C43 C38 0.9(7) . . . . ? C39 C38 C43 F15 -179.7(3) . . . . ? C15 C38 C43 F15 0.2(6) . . . . ? C39 C38 C43 C42 -2.1(6) . . . . ? C15 C38 C43 C42 177.9(4) . . . . ? C21 C20 C44 C49 33.4(7) . . . . ? C19 C20 C44 C49 -131.9(4) . . . . ? C21 C20 C44 C45 -155.1(4) . . . . ? C19 C20 C44 C45 39.5(6) . . . . ? C49 C44 C45 F16 -178.4(4) . . . . ? C20 C44 C45 F16 9.7(6) . . . . ? C49 C44 C45 C46 2.3(6) . . . . ? C20 C44 C45 C46 -169.6(4) . . . . ? F16 C45 C46 F17 -0.6(6) . . . . ? C44 C45 C46 F17 178.7(4) . . . . ? F16 C45 C46 C47 178.8(4) . . . . ? C44 C45 C46 C47 -1.9(6) . . . . ? F17 C46 C47 F18 -0.5(6) . . . . ? C45 C46 C47 F18 -179.9(4) . . . . ? F17 C46 C47 C48 179.3(4) . . . . ? C45 C46 C47 C48 0.0(6) . . . . ? F18 C47 C48 F19 -0.5(6) . . . . ? C46 C47 C48 F19 179.7(4) . . . . ? F18 C47 C48 C49 -178.7(4) . . . . ? C46 C47 C48 C49 1.4(6) . . . . ? F19 C48 C49 F20 -3.6(6) . . . . ? C47 C48 C49 F20 174.7(4) . . . . ? F19 C48 C49 C44 -179.2(4) . . . . ? C47 C48 C49 C44 -1.0(7) . . . . ? C45 C44 C49 F20 -176.4(3) . . . . ? C20 C44 C49 F20 -4.4(6) . . . . ? C45 C44 C49 C48 -0.8(6) . . . . ? C20 C44 C49 C48 171.2(4) . . . . ? C24 C25 C50 C51 166.6(5) . . . . ? C1 C25 C50 C51 -22.9(7) . . . . ? C24 C25 C50 C55 -5.5(4) . . . . ? C1 C25 C50 C55 165.0(4) . . . . ? C55 C50 C51 F21 175.1(3) . . . . ? C25 C50 C51 F21 3.5(7) . . . . ? C55 C50 C51 C52 -2.1(6) . . . . ? C25 C50 C51 C52 -173.8(4) . . . . ? F21 C51 C52 F22 1.4(6) . . . . ? C50 C51 C52 F22 178.8(4) . . . . ? F21 C51 C52 C53 -176.4(4) . . . . ? C50 C51 C52 C53 1.0(6) . . . . ? F22 C52 C53 F23 -0.8(6) . . . . ? C51 C52 C53 F23 177.1(3) . . . . ? F22 C52 C53 C54 -176.8(4) . . . . ? C51 C52 C53 C54 1.0(6) . . . . ? F23 C53 C54 F24 -1.6(6) . . . . ? C52 C53 C54 F24 174.4(3) . . . . ? F23 C53 C54 C55 -177.7(3) . . . . ? C52 C53 C54 C55 -1.7(6) . . . . ? C53 C54 C55 N5 172.8(4) . . . . ? F24 C54 C55 N5 -3.3(7) . . . . ? C53 C54 C55 C50 0.5(6) . . . . ? F24 C54 C55 C50 -175.6(4) . . . . ? C51 C50 C55 C54 1.4(6) . . . . ? C25 C50 C55 C54 175.1(4) . . . . ? C51 C50 C55 N5 -172.5(4) . . . . ? C25 C50 C55 N5 1.2(4) . . . . ? C2 C1 N1 C4 3.7(4) . . . . ? C25 C1 N1 C4 177.9(4) . . . . ? C2 C1 N1 P1 165.9(3) . . . . ? C25 C1 N1 P1 -19.9(6) . . . . ? C3 C4 N1 C1 -3.1(4) . . . . ? C5 C4 N1 C1 171.2(4) . . . . ? C3 C4 N1 P1 -166.5(3) . . . . ? C5 C4 N1 P1 7.8(5) . . . . ? C10 C9 N2 C6 -164.1(4) . . . . ? C8 C9 N2 C6 12.1(4) . . . . ? C10 C9 N2 P1 22.4(6) . . . . ? C8 C9 N2 P1 -161.4(3) . . . . ? C5 C6 N2 C9 155.2(4) . . . . ? C7 C6 N2 C9 -21.9(4) . . . . ? C5 C6 N2 P1 -31.1(5) . . . . ? C7 C6 N2 P1 151.8(3) . . . . ? C12 C11 N3 C14 -1.2(5) . . . . ? C10 C11 N3 C14 -179.1(4) . . . . ? C15 C14 N3 C11 -178.9(4) . . . . ? C13 C14 N3 C11 2.1(4) . . . . ? C23 C22 N4 C19 -175.0(4) . . . . ? C21 C22 N4 C19 2.4(5) . . . . ? C23 C22 N4 C16 -3.4(9) . . . . ? C21 C22 N4 C16 174.1(4) . . . . ? C18 C19 N4 C22 177.0(3) . . . . ? C20 C19 N4 C22 0.1(5) . . . . ? C18 C19 N4 C16 3.4(5) . . . . ? C20 C19 N4 C16 -173.5(3) . . . . ? C15 C16 N4 C22 2.9(7) . . . . ? C17 C16 N4 C22 -174.9(4) . . . . ? C15 C16 N4 C19 174.4(4) . . . . ? C17 C16 N4 C19 -3.4(4) . . . . ? C54 C55 N5 C21 10.8(8) . . . . ? C50 C55 N5 C21 -176.0(5) . . . . ? C54 C55 N5 C24 -169.6(4) . . . . ? C50 C55 N5 C24 3.6(4) . . . . ? C22 C21 N5 C55 -175.2(5) . . . . ? C20 C21 N5 C55 11.0(11) . . . . ? C22 C21 N5 C24 5.2(4) . . . . ? C20 C21 N5 C24 -168.6(6) . . . . ? C25 C24 N5 C55 -7.4(5) . . . . ? C23 C24 N5 C55 174.2(3) . . . . ? C25 C24 N5 C21 172.3(3) . . . . ? C23 C24 N5 C21 -6.1(4) . . . . ? C9 N2 P1 N1 -149.0(3) . . . . ? C6 N2 P1 N1 38.4(3) . . . . ? C9 N2 P1 C12 -34.4(4) . . . . ? C6 N2 P1 C12 153.0(3) . . . . ? C9 N2 P1 B1 91.8(4) . . . . ? C6 N2 P1 B1 -80.8(4) . . . . ? C1 N1 P1 N2 174.0(3) . . . . ? C4 N1 P1 N2 -26.3(3) . . . . ? C1 N1 P1 C12 72.4(4) . . . . ? C4 N1 P1 C12 -127.9(3) . . . . ? C1 N1 P1 B1 -63.1(4) . . . . ? C4 N1 P1 B1 96.7(3) . . . . ? C13 C12 P1 N2 -164.7(4) . . . . ? C11 C12 P1 N2 27.9(4) . . . . ? C13 C12 P1 N1 -62.3(5) . . . . ? C11 C12 P1 N1 130.4(3) . . . . ? C13 C12 P1 B1 70.1(5) . . . . ? C11 C12 P1 B1 -97.3(4) . . . . ? C65 C60 C62 C63 -177.9(6) . . . . ? C60 C62 C63 C61 -174.8(4) . . . . ? C64 C61 C63 C62 -58.6(7) . . . . ? C66 C66 C68 C67 -177.3(6) 7_667 . . . ? C74 C69 C70 C71 0.0 . . . . ? C69 C70 C71 C72 0.0 . . . . ? C69 C70 C71 C75 -178.4(14) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C75 C71 C72 C73 178.6(13) . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C69 0.0 . . . . ? C70 C69 C74 C73 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.638 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.074 # Attachment 'PO-Eur.CIF' data_10215hi _database_code_depnum_ccdc_archive 'CCDC 827555' #TrackingRef 'PO-Eur.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C55 H6 F24 N5 O P),13(C6 H5 Cl)' _chemical_formula_sum 'C149 H44.50 Cl6.50 F48 N10 O2 P2' _chemical_formula_weight 3210.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 29.5322(5) _cell_length_b 10.3705(2) _cell_length_c 41.5808(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.1602(8) _cell_angle_gamma 90.00 _cell_volume 12572.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6388 _exptl_absorpt_coefficient_mu 2.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4872 _exptl_absorpt_correction_T_max 0.8727 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\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 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 114624 _diffrn_reflns_av_R_equivalents 0.1338 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 62.00 _reflns_number_total 19582 _reflns_number_gt 9906 _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^)+(0.1659P)^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 19582 _refine_ls_number_parameters 2085 _refine_ls_number_restraints 268 _refine_ls_R_factor_all 0.1505 _refine_ls_R_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.2961 _refine_ls_wR_factor_gt 0.2551 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4751(2) 0.7903(7) 0.35653(16) 0.0595(18) Uani 1 1 d . . . C2 C 0.5142(2) 0.7615(7) 0.34347(16) 0.0607(18) Uani 1 1 d . . . H1 H 0.5418 0.8102 0.3463 0.073 Uiso 1 1 calc R . . C3 C 0.50598(19) 0.6485(7) 0.32541(16) 0.0578(18) Uani 1 1 d . . . H2 H 0.5272 0.6076 0.3138 0.069 Uiso 1 1 calc R . . C4 C 0.4626(2) 0.6054(7) 0.32701(17) 0.0607(18) Uani 1 1 d . . . C5 C 0.4386(2) 0.4910(7) 0.31296(15) 0.0576(18) Uani 1 1 d . . . C6 C 0.3933(2) 0.4762(7) 0.31382(15) 0.0543(17) Uani 1 1 d . . . C7 C 0.3603(2) 0.3817(7) 0.29920(17) 0.0613(19) Uani 1 1 d . . . H3 H 0.3674 0.3042 0.2889 0.074 Uiso 1 1 calc R . . C8 C 0.3173(2) 0.4218(7) 0.30270(17) 0.0607(18) Uani 1 1 d . . . H4 H 0.2896 0.3778 0.2949 0.073 Uiso 1 1 calc R . . C9 C 0.3212(2) 0.5424(8) 0.32025(16) 0.0597(19) Uani 1 1 d . . . C10 C 0.2893(2) 0.6334(7) 0.32515(16) 0.0593(18) Uani 1 1 d . . . C11 C 0.30409(19) 0.7601(7) 0.33666(14) 0.0521(17) Uani 1 1 d . . . C12 C 0.35054(19) 0.7940(8) 0.34811(15) 0.0550(18) Uani 1 1 d . . . C13 C 0.34919(19) 0.9237(7) 0.35624(15) 0.0538(17) Uani 1 1 d . . . C14 C 0.30018(19) 0.9615(7) 0.34963(15) 0.0542(17) Uani 1 1 d . . . C15 C 0.27615(19) 1.0771(8) 0.35522(15) 0.0576(18) Uani 1 1 d . . . C16 C 0.2955(2) 1.1884(7) 0.37022(16) 0.0563(17) Uani 1 1 d . . . C17 C 0.2784(2) 1.3070(8) 0.38082(16) 0.065(2) Uani 1 1 d . . . H5 H 0.2472 1.3328 0.3767 0.077 Uiso 1 1 calc R . . C18 C 0.3139(2) 1.3797(8) 0.39796(17) 0.0648(19) Uani 1 1 d . . . H6 H 0.3112 1.4628 0.4071 0.078 Uiso 1 1 calc R . . C19 C 0.3548(2) 1.3064(8) 0.39915(17) 0.0640(19) Uani 1 1 d . . . C20 C 0.4030(2) 1.2996(8) 0.41178(16) 0.0614(19) Uani 1 1 d . . . C21 C 0.41715(19) 1.1809(7) 0.40100(15) 0.0544(17) Uani 1 1 d . . . C22 C 0.37924(19) 1.1213(7) 0.38174(16) 0.0545(17) Uani 1 1 d . . . C23 C 0.38625(19) 1.0010(7) 0.37052(15) 0.0562(18) Uani 1 1 d . . . C24 C 0.43566(19) 0.9815(7) 0.38130(15) 0.0528(17) Uani 1 1 d . . . C25 C 0.47111(19) 0.8986(7) 0.37902(15) 0.0541(17) Uani 1 1 d . . . C26 C 0.46493(19) 0.3953(8) 0.29735(17) 0.0590(18) Uani 1 1 d . . . C27 C 0.4847(2) 0.4262(9) 0.26937(18) 0.067(2) Uani 1 1 d . . . C28 C 0.5102(2) 0.3357(8) 0.25536(17) 0.0632(19) Uani 1 1 d . . . C29 C 0.5158(2) 0.2131(8) 0.26823(18) 0.0610(19) Uani 1 1 d . . . C30 C 0.4959(2) 0.1789(9) 0.2940(2) 0.068(2) Uani 1 1 d . . . C31 C 0.4712(2) 0.2704(8) 0.30835(17) 0.0604(18) Uani 1 1 d . . . C32 C 0.23871(19) 0.6055(7) 0.31872(16) 0.0545(17) Uani 1 1 d . . . C33 C 0.2141(2) 0.5897(7) 0.28876(18) 0.0656(19) Uani 1 1 d . . . C34 C 0.1667(2) 0.5724(7) 0.28323(18) 0.065(2) Uani 1 1 d . . . C35 C 0.1444(2) 0.5685(8) 0.3091(2) 0.068(2) Uani 1 1 d . . . C36 C 0.1675(2) 0.5847(7) 0.34009(18) 0.065(2) Uani 1 1 d . . . C37 C 0.2145(2) 0.6026(7) 0.34489(17) 0.0594(18) Uani 1 1 d . . . C38 C 0.22507(19) 1.0766(7) 0.34448(16) 0.0558(17) Uani 1 1 d . . . C39 C 0.1971(2) 0.9853(7) 0.35500(17) 0.0586(18) Uani 1 1 d . . . C40 C 0.1505(2) 0.9801(8) 0.34351(18) 0.0641(19) Uani 1 1 d . . . C41 C 0.1310(2) 1.0688(8) 0.32117(17) 0.0599(18) Uani 1 1 d . . . C42 C 0.1569(2) 1.1672(7) 0.31086(16) 0.0572(18) Uani 1 1 d . . . C43 C 0.20411(19) 1.1643(7) 0.32217(17) 0.0595(18) Uani 1 1 d . . . C44 C 0.4285(2) 1.4006(7) 0.43183(16) 0.0583(18) Uani 1 1 d . . . C45 C 0.4142(2) 1.4464(8) 0.46001(18) 0.068(2) Uani 1 1 d . . . C46 C 0.4367(3) 1.5448(9) 0.47837(19) 0.081(2) Uani 1 1 d . . . C47 C 0.4748(3) 1.5990(8) 0.46887(19) 0.076(2) Uani 1 1 d . . . C48 C 0.4894(2) 1.5564(9) 0.4407(2) 0.076(2) Uani 1 1 d . . . C49 C 0.4665(2) 1.4581(8) 0.42305(17) 0.0643(19) Uani 1 1 d . . . C50 C 0.51119(19) 0.9524(7) 0.39988(15) 0.0534(17) Uani 1 1 d . . . C51 C 0.5567(2) 0.9099(7) 0.41060(16) 0.0569(18) Uani 1 1 d . . . C52 C 0.5856(2) 0.9808(7) 0.43250(17) 0.0590(18) Uani 1 1 d . . . C53 C 0.5715(2) 1.0967(7) 0.44471(16) 0.0594(18) Uani 1 1 d . . . C54 C 0.5279(2) 1.1414(7) 0.43489(16) 0.0585(18) Uani 1 1 d . . . C55 C 0.49772(18) 1.0701(7) 0.41287(15) 0.0520(17) Uani 1 1 d . . . C56 C 0.0774(2) 0.2112(8) 0.11890(18) 0.066(2) Uani 1 1 d . . . C57 C 0.0391(2) 0.1902(8) 0.13355(17) 0.071(2) Uani 1 1 d . . . H7 H 0.0111 0.2369 0.1294 0.085 Uiso 1 1 calc R . . C58 C 0.0486(2) 0.0907(9) 0.15505(18) 0.074(2) Uani 1 1 d . . . H8 H 0.0278 0.0567 0.1682 0.089 Uiso 1 1 calc R . . C59 C 0.0925(2) 0.0466(8) 0.15501(18) 0.072(2) Uani 1 1 d . . . C60 C 0.1168(2) -0.0537(8) 0.17398(18) 0.069(2) Uani 1 1 d . . . C61 C 0.1624(2) -0.0738(8) 0.17323(18) 0.068(2) Uani 1 1 d . . . C62 C 0.1964(2) -0.1535(8) 0.19187(17) 0.070(2) Uani 1 1 d . . . H9 H 0.1900 -0.2246 0.2048 0.084 Uiso 1 1 calc R . . C63 C 0.2383(2) -0.1141(8) 0.18852(17) 0.072(2) Uani 1 1 d . . . H10 H 0.2663 -0.1502 0.1991 0.086 Uiso 1 1 calc R . . C64 C 0.2339(2) -0.0068(8) 0.16602(17) 0.067(2) Uani 1 1 d . . . C65 C 0.2646(2) 0.0876(8) 0.16133(16) 0.065(2) Uani 1 1 d . . . C66 C 0.2490(2) 0.2008(8) 0.14298(16) 0.0614(19) Uani 1 1 d . . . C67 C 0.2027(2) 0.2220(8) 0.12794(16) 0.066(2) Uani 1 1 d . . . C68 C 0.2020(2) 0.3457(9) 0.11497(17) 0.069(2) Uani 1 1 d . . . C69 C 0.2503(2) 0.3958(9) 0.12310(17) 0.068(2) Uani 1 1 d . . . C70 C 0.2716(2) 0.5156(8) 0.11701(18) 0.068(2) Uani 1 1 d . . . C71 C 0.2525(2) 0.6180(9) 0.09932(18) 0.073(2) Uani 1 1 d . . . C72 C 0.2664(3) 0.7418(8) 0.0907(2) 0.077(2) Uani 1 1 d . . . H11 H 0.2965 0.7753 0.0966 0.092 Uiso 1 1 calc R . . C73 C 0.2301(3) 0.8089(9) 0.07243(19) 0.082(2) Uani 1 1 d . . . H12 H 0.2314 0.8938 0.0640 0.099 Uiso 1 1 calc R . . C74 C 0.1912(2) 0.7282(8) 0.06863(18) 0.069(2) Uani 1 1 d . . . C75 C 0.1422(2) 0.7181(8) 0.05852(17) 0.067(2) Uani 1 1 d . . . C76 C 0.1305(2) 0.5939(9) 0.06806(18) 0.071(2) Uani 1 1 d . . . C77 C 0.1710(2) 0.5334(8) 0.08483(19) 0.071(2) Uani 1 1 d . . . C78 C 0.1644(2) 0.4124(9) 0.09788(18) 0.072(2) Uani 1 1 d . . . C79 C 0.1153(2) 0.3934(8) 0.08905(18) 0.071(2) Uani 1 1 d . . . C80 C 0.0792(2) 0.3121(8) 0.09445(18) 0.070(2) Uani 1 1 d . . . C81 C 0.0920(2) -0.1297(8) 0.19535(19) 0.070(2) Uani 1 1 d . . . C82 C 0.0556(2) -0.2077(10) 0.18389(19) 0.082(3) Uani 1 1 d . . . C83 C 0.0327(2) -0.2808(9) 0.2034(2) 0.082(2) Uani 1 1 d . . . C84 C 0.0444(3) -0.2714(9) 0.2364(2) 0.080(2) Uani 1 1 d . . . C85 C 0.0798(2) -0.1905(8) 0.25039(19) 0.069(2) Uani 1 1 d . . . C86 C 0.1037(2) -0.1221(8) 0.2292(2) 0.071(2) Uani 1 1 d . . . C87 C 0.3132(2) 0.0735(7) 0.17673(16) 0.0572(18) Uani 1 1 d . . . C88 C 0.3389(2) -0.0360(9) 0.17299(17) 0.069(2) Uani 1 1 d . . . C89 C 0.3831(2) -0.0530(8) 0.18808(18) 0.067(2) Uani 1 1 d . . . C90 C 0.4049(2) 0.0424(8) 0.20793(18) 0.067(2) Uani 1 1 d . . . C91 C 0.3799(2) 0.1542(8) 0.21213(17) 0.0643(19) Uani 1 1 d . . . C92 C 0.3358(2) 0.1645(8) 0.19741(17) 0.065(2) Uani 1 1 d . . . C93 C 0.3207(2) 0.5273(8) 0.1330(2) 0.076(2) Uani 1 1 d . . . C94 C 0.3323(2) 0.5371(8) 0.1661(2) 0.072(2) Uani 1 1 d . . . C95 C 0.3769(3) 0.5407(8) 0.1814(2) 0.082(2) Uani 1 1 d . . . C96 C 0.4114(2) 0.5390(9) 0.1627(3) 0.097(3) Uani 1 1 d . . . C97 C 0.4019(3) 0.5293(10) 0.1290(3) 0.098(3) Uani 1 1 d . . . C98 C 0.3573(3) 0.5238(10) 0.1151(2) 0.091(3) Uani 1 1 d . . . C99 C 0.11344(19) 0.8236(5) 0.04371(14) 0.075(2) Uani 1 1 d G . . C100 C 0.1249(2) 0.8912(8) 0.01729(15) 0.099(3) Uani 1 1 d G . . C101 C 0.0984(3) 0.9955(7) 0.00454(16) 0.129(4) Uani 1 1 d G . . C102 C 0.0604(3) 1.0322(5) 0.0182(2) 0.123(5) Uani 1 1 d G . . C103 C 0.0489(2) 0.9646(8) 0.0446(2) 0.126(4) Uani 1 1 d G . . C104 C 0.0754(2) 0.8603(7) 0.05737(14) 0.094(3) Uani 1 1 d G . . C105 C 0.0373(2) 0.3645(8) 0.07464(17) 0.066(2) Uani 1 1 d . . . C106 C -0.0071(2) 0.3210(9) 0.06592(18) 0.071(2) Uani 1 1 d . . . C107 C -0.0391(2) 0.3930(10) 0.04542(18) 0.075(2) Uani 1 1 d . . . C108 C -0.0267(2) 0.5093(9) 0.03356(17) 0.071(2) Uani 1 1 d . . . C109 C 0.0170(3) 0.5523(9) 0.03986(19) 0.076(2) Uani 1 1 d . . . C110 C 0.0491(2) 0.4825(9) 0.06106(16) 0.068(2) Uani 1 1 d . . . C111 C 0.3883(3) 0.0156(12) 0.4646(3) 0.108(7) Uani 0.632(9) 1 d PG A 5 C112 C 0.3929(3) -0.1092(12) 0.4534(3) 0.076(4) Uani 0.632(9) 1 d PG A 5 H28 H 0.4221 -0.1500 0.4568 0.091 Uiso 0.632(9) 1 calc PR A 5 C113 C 0.3549(4) -0.1743(11) 0.4372(3) 0.095(5) Uani 0.632(9) 1 d PG A 5 H29 H 0.3580 -0.2596 0.4295 0.115 Uiso 0.632(9) 1 calc PR A 5 C114 C 0.3122(3) -0.1146(14) 0.4322(4) 0.099(6) Uani 0.632(9) 1 d PG A 5 H30 H 0.2861 -0.1591 0.4212 0.119 Uiso 0.632(9) 1 calc PR A 5 C115 C 0.3076(3) 0.0102(14) 0.4435(4) 0.102(7) Uani 0.632(9) 1 d PG A 5 H31 H 0.2784 0.0510 0.4401 0.122 Uiso 0.632(9) 1 calc PR A 5 C116 C 0.3456(4) 0.0753(10) 0.4596(4) 0.112(7) Uani 0.632(9) 1 d PG A 5 H32 H 0.3425 0.1607 0.4673 0.135 Uiso 0.632(9) 1 calc PR A 5 C164 C 0.3671(5) 0.0795(16) 0.4698(4) 0.098(8) Uani 0.368(9) 1 d PGU A 6 H58 H 0.3814 0.1451 0.4838 0.117 Uiso 0.368(9) 1 calc PR A 6 C165 C 0.3206(5) 0.088(2) 0.4573(6) 0.110(8) Uani 0.368(9) 1 d PGU A 6 H59 H 0.3032 0.1592 0.4628 0.132 Uiso 0.368(9) 1 calc PR A 6 C166 C 0.2997(5) -0.008(3) 0.4368(6) 0.099(8) Uani 0.368(9) 1 d PGU A 6 H60 H 0.2680 -0.0024 0.4283 0.119 Uiso 0.368(9) 1 calc PR A 6 C167 C 0.3253(7) -0.112(3) 0.4288(7) 0.113(8) Uani 0.368(9) 1 d PGU A 6 H61 H 0.3110 -0.1781 0.4148 0.135 Uiso 0.368(9) 1 calc PR A 6 C168 C 0.3717(7) -0.121(2) 0.4413(6) 0.116(8) Uani 0.368(9) 1 d PGU A 6 H62 H 0.3892 -0.1921 0.4358 0.139 Uiso 0.368(9) 1 calc PR A 6 C169 C 0.3926(5) -0.0248(13) 0.4618(3) 0.112(9) Uani 0.368(9) 1 d PGU A 6 Cl9 Cl 0.4495(3) -0.0351(16) 0.4771(2) 0.169(7) Uani 0.368(9) 1 calc PR A 6 C117 C 0.3324(2) -0.0369(8) 0.27154(17) 0.068(2) Uani 1 1 d . . . C118 C 0.3800(2) -0.0201(9) 0.28113(18) 0.075(2) Uani 1 1 d . . . H13 H 0.3921 0.0602 0.2895 0.090 Uiso 1 1 calc R . . C119 C 0.4080(2) -0.1211(10) 0.27813(18) 0.079(2) Uani 1 1 d . . . H14 H 0.4402 -0.1120 0.2844 0.094 Uiso 1 1 calc R . . C120 C 0.3903(2) -0.2352(9) 0.26619(16) 0.069(2) Uani 1 1 d . . . H15 H 0.4106 -0.3033 0.2630 0.083 Uiso 1 1 calc R . . C121 C 0.3432(2) -0.2552(9) 0.25853(17) 0.071(2) Uani 1 1 d . . . H16 H 0.3314 -0.3372 0.2513 0.086 Uiso 1 1 calc R . . C122 C 0.3138(2) -0.1529(8) 0.26168(17) 0.066(2) Uani 1 1 d . . . H17 H 0.2814 -0.1639 0.2571 0.079 Uiso 1 1 calc R . . C123 C 0.1118(3) 0.2278(10) 0.38830(19) 0.080(2) Uani 1 1 d . . . C124 C 0.0962(3) 0.1102(10) 0.3977(2) 0.093(3) Uani 1 1 d . . . H18 H 0.0670 0.0784 0.3881 0.111 Uiso 1 1 calc R . . C125 C 0.1239(4) 0.0394(11) 0.4215(2) 0.106(3) Uani 1 1 d . . . H19 H 0.1127 -0.0389 0.4290 0.128 Uiso 1 1 calc R . . C126 C 0.1670(3) 0.0798(12) 0.4343(2) 0.104(3) Uani 1 1 d . . . H20 H 0.1858 0.0293 0.4502 0.125 Uiso 1 1 calc R . . C127 C 0.1830(3) 0.1949(12) 0.4238(2) 0.108(3) Uani 1 1 d . . . H21 H 0.2132 0.2228 0.4322 0.130 Uiso 1 1 calc R . . C128 C 0.1546(3) 0.2725(10) 0.40044(19) 0.086(3) Uani 1 1 d . . . H22 H 0.1651 0.3528 0.3935 0.103 Uiso 1 1 calc R . . C129 C 0.4516(7) -0.038(3) 0.1188(6) 0.131(11) Uani 0.422(16) 1 d PGU B 3 H33 H 0.4747 0.0013 0.1342 0.158 Uiso 0.422(16) 1 calc PR B 3 C130 C 0.4589(7) -0.160(3) 0.1065(7) 0.136(10) Uani 0.422(16) 1 d PGU B 3 H34 H 0.4870 -0.2033 0.1135 0.163 Uiso 0.422(16) 1 calc PR B 3 C131 C 0.4250(8) -0.217(2) 0.0840(6) 0.122(9) Uani 0.422(16) 1 d PGU B 3 H35 H 0.4300 -0.3002 0.0756 0.147 Uiso 0.422(16) 1 calc PR B 3 C132 C 0.3839(7) -0.153(2) 0.0739(5) 0.117(9) Uani 0.422(16) 1 d PGU B 3 H36 H 0.3607 -0.1924 0.0585 0.140 Uiso 0.422(16) 1 calc PR B 3 C133 C 0.3766(6) -0.032(2) 0.0862(6) 0.106(10) Uani 0.422(16) 1 d PGU B 3 H37 H 0.3485 0.0122 0.0793 0.127 Uiso 0.422(16) 1 calc PR B 3 C134 C 0.4105(9) 0.026(2) 0.1087(6) 0.108(9) Uani 0.422(16) 1 d PGDU B 3 C158 C 0.4537(4) -0.020(2) 0.1249(4) 0.122(8) Uani 0.578(16) 1 d PGU B 4 H38 H 0.4817 -0.0085 0.1393 0.147 Uiso 0.578(16) 1 calc PR B 4 C159 C 0.4464(5) -0.1316(18) 0.1062(5) 0.128(8) Uani 0.578(16) 1 d PGU B 4 H39 H 0.4695 -0.1961 0.1078 0.153 Uiso 0.578(16) 1 calc PR B 4 C160 C 0.4054(6) -0.1487(17) 0.0851(4) 0.133(8) Uani 0.578(16) 1 d PGU B 4 H40 H 0.4004 -0.2249 0.0723 0.159 Uiso 0.578(16) 1 calc PR B 4 C161 C 0.3716(4) -0.054(2) 0.0827(4) 0.122(9) Uani 0.578(16) 1 d PGU B 4 H41 H 0.3435 -0.0661 0.0683 0.147 Uiso 0.578(16) 1 calc PR B 4 C162 C 0.3788(4) 0.0570(18) 0.1014(4) 0.126(7) Uani 0.578(16) 1 d PGU B 4 H42 H 0.3557 0.1214 0.0998 0.152 Uiso 0.578(16) 1 calc PR B 4 C163 C 0.4199(5) 0.0741(17) 0.1225(4) 0.114(7) Uani 0.578(16) 1 d PGDU B 4 C135 C 0.2361(4) 0.2897(14) 0.0391(2) 0.108(4) Uani 1 1 d . . . C136 C 0.1911(3) 0.2449(12) 0.0313(2) 0.106(3) Uani 1 1 d . . . H23 H 0.1816 0.1619 0.0372 0.128 Uiso 1 1 calc R . . C137 C 0.1615(4) 0.3346(15) 0.0139(3) 0.125(4) Uani 1 1 d . . . H24 H 0.1302 0.3114 0.0079 0.150 Uiso 1 1 calc R . . C138 C 0.1755(4) 0.4582(13) 0.0047(2) 0.107(3) Uani 1 1 d . . . H25 H 0.1542 0.5155 -0.0074 0.128 Uiso 1 1 calc R . . C139 C 0.2214(4) 0.4936(13) 0.0138(2) 0.119(4) Uani 1 1 d . . . H26 H 0.2312 0.5776 0.0089 0.142 Uiso 1 1 calc R . . C140 C 0.2536(3) 0.4046(14) 0.0305(3) 0.109(4) Uani 1 1 d . . . H27 H 0.2854 0.4238 0.0354 0.130 Uiso 1 1 calc R . . C146 C 0.1844(7) 0.5296(18) 0.1775(6) 0.112(9) Uani 0.433(7) 1 d PGU C 1 H43 H 0.2052 0.5921 0.1717 0.135 Uiso 0.433(7) 1 calc PR C 1 C147 C 0.1375(8) 0.5440(18) 0.1672(5) 0.125(10) Uani 0.433(7) 1 d PGU C 1 H44 H 0.1263 0.6163 0.1544 0.151 Uiso 0.433(7) 1 calc PR C 1 C151 C 0.1071(5) 0.453(2) 0.1758(6) 0.140(10) Uani 0.433(7) 1 d PGU C 1 H45 H 0.0751 0.4623 0.1688 0.168 Uiso 0.433(7) 1 calc PR C 1 C148 C 0.1236(5) 0.347(2) 0.1946(6) 0.132(10) Uani 0.433(7) 1 d PGU C 1 H46 H 0.1029 0.2842 0.2004 0.158 Uiso 0.433(7) 1 calc PR C 1 C150 C 0.1705(6) 0.3324(17) 0.2049(5) 0.104(8) Uani 0.433(7) 1 d PGU C 1 C149 C 0.2009(4) 0.424(2) 0.1963(6) 0.097(9) Uani 0.433(7) 1 d PGU C 1 H47 H 0.2329 0.4140 0.2034 0.116 Uiso 0.433(7) 1 calc PR C 1 C152 C 0.1410(4) 0.4628(12) 0.1795(3) 0.085(5) Uani 0.567(7) 1 d PGU C 2 C153 C 0.1139(3) 0.3706(13) 0.1916(3) 0.087(5) Uani 0.567(7) 1 d PGU C 2 H48 H 0.0815 0.3741 0.1860 0.104 Uiso 0.567(7) 1 calc PR C 2 C154 C 0.1344(4) 0.2732(11) 0.2119(3) 0.077(4) Uani 0.567(7) 1 d PGU C 2 H49 H 0.1159 0.2102 0.2201 0.092 Uiso 0.567(7) 1 calc PR C 2 C155 C 0.1818(4) 0.2680(12) 0.2200(3) 0.104(8) Uani 0.567(7) 1 d PGU C 2 H50 H 0.1958 0.2015 0.2339 0.125 Uiso 0.567(7) 1 calc PR C 2 C156 C 0.2089(3) 0.3603(14) 0.2079(4) 0.097(6) Uani 0.567(7) 1 d PGU C 2 H51 H 0.2413 0.3567 0.2135 0.117 Uiso 0.567(7) 1 calc PR C 2 C157 C 0.1884(4) 0.4576(12) 0.1877(4) 0.083(6) Uani 0.567(7) 1 d PGU C 2 H52 H 0.2069 0.5206 0.1794 0.100 Uiso 0.567(7) 1 calc PR C 2 N1 N 0.44207(15) 0.6974(5) 0.34598(12) 0.0515(13) Uani 1 1 d . . . N2 N 0.36863(15) 0.5702(5) 0.32865(12) 0.0540(14) Uani 1 1 d . . . N3 N 0.27462(16) 0.8582(6) 0.33695(12) 0.0547(14) Uani 1 1 d . . . N4 N 0.34225(16) 1.1989(6) 0.38119(13) 0.0576(15) Uani 1 1 d . . . N5 N 0.45201(16) 1.0875(6) 0.40118(12) 0.0569(14) Uani 1 1 d . . . N6 N 0.11201(18) 0.1265(6) 0.13293(14) 0.0685(17) Uani 1 1 d . . . N7 N 0.18583(17) 0.0090(6) 0.15452(14) 0.0660(16) Uani 1 1 d . . . N8 N 0.27644(18) 0.3041(7) 0.13987(13) 0.0671(17) Uani 1 1 d . . . N9 N 0.20601(18) 0.6158(7) 0.08454(15) 0.0719(17) Uani 1 1 d . . . N10 N 0.09656(18) 0.4981(7) 0.06959(14) 0.0691(17) Uani 1 1 d . . . P1 P 0.39070(5) 0.67277(19) 0.35794(4) 0.0565(5) Uani 1 1 d . . . P2 P 0.16382(6) 0.0954(2) 0.12186(5) 0.0660(5) Uani 1 1 d . . . O1 O 0.39618(13) 0.6291(5) 0.39176(10) 0.0601(12) Uani 1 1 d . . . O2 O 0.15798(14) 0.0348(5) 0.08986(11) 0.0703(14) Uani 1 1 d . . . F1 F 0.47953(11) 0.5444(4) 0.25640(9) 0.0659(10) Uani 1 1 d . . . F2 F 0.52898(12) 0.3693(4) 0.22937(10) 0.0759(12) Uani 1 1 d . . . F3 F 0.54057(12) 0.1280(4) 0.25403(10) 0.0791(12) Uani 1 1 d . . . F4 F 0.50148(12) 0.0603(4) 0.30671(10) 0.0722(11) Uani 1 1 d . . . F5 F 0.45291(12) 0.2324(4) 0.33447(9) 0.0685(11) Uani 1 1 d . . . F6 F 0.23504(12) 0.5979(4) 0.26206(9) 0.0709(11) Uani 1 1 d . . . F7 F 0.14351(12) 0.5610(5) 0.25306(10) 0.0832(13) Uani 1 1 d . . . F8 F 0.09851(11) 0.5534(4) 0.30509(10) 0.0817(13) Uani 1 1 d . . . F9 F 0.14526(12) 0.5860(4) 0.36629(10) 0.0777(12) Uani 1 1 d . . . F10 F 0.23711(11) 0.6166(4) 0.37544(9) 0.0696(11) Uani 1 1 d . . . F11 F 0.21348(11) 0.9012(4) 0.37842(9) 0.0640(10) Uani 1 1 d . . . F12 F 0.12486(12) 0.8845(4) 0.35319(10) 0.0742(11) Uani 1 1 d . . . F13 F 0.08588(11) 1.0651(4) 0.30991(10) 0.0751(12) Uani 1 1 d . . . F14 F 0.13815(11) 1.2538(4) 0.28965(9) 0.0667(11) Uani 1 1 d . . . F15 F 0.22846(11) 1.2618(4) 0.31048(9) 0.0639(10) Uani 1 1 d . . . F16 F 0.37684(13) 1.3975(5) 0.46980(10) 0.0797(12) Uani 1 1 d . . . F17 F 0.42229(16) 1.5850(5) 0.50551(11) 0.1008(16) Uani 1 1 d . . . F18 F 0.49741(15) 1.6924(5) 0.48640(11) 0.0939(14) Uani 1 1 d . . . F19 F 0.52596(15) 1.6110(5) 0.43139(11) 0.0906(14) Uani 1 1 d . . . F20 F 0.48108(12) 1.4205(4) 0.39536(9) 0.0742(12) Uani 1 1 d . . . F21 F 0.57182(11) 0.7936(4) 0.40194(9) 0.0623(10) Uani 1 1 d . . . F22 F 0.62825(11) 0.9385(4) 0.44262(9) 0.0681(11) Uani 1 1 d . . . F23 F 0.60121(11) 1.1638(4) 0.46620(8) 0.0648(10) Uani 1 1 d . . . F24 F 0.51433(11) 1.2506(4) 0.44801(8) 0.0648(10) Uani 1 1 d . . . F25 F 0.04381(15) -0.2213(6) 0.15128(11) 0.1064(17) Uani 1 1 d . . . F26 F -0.00026(16) -0.3621(6) 0.19048(12) 0.1104(18) Uani 1 1 d . . . F27 F 0.02215(14) -0.3395(5) 0.25630(11) 0.0885(13) Uani 1 1 d . . . F28 F 0.09193(14) -0.1820(5) 0.28154(10) 0.0853(13) Uani 1 1 d . . . F29 F 0.13714(14) -0.0448(5) 0.24297(10) 0.0837(13) Uani 1 1 d . . . F30 F 0.32026(13) -0.1320(4) 0.15287(10) 0.0771(12) Uani 1 1 d . . . F31 F 0.40600(13) -0.1616(5) 0.18344(10) 0.0813(13) Uani 1 1 d . . . F32 F 0.44808(12) 0.0314(4) 0.22230(10) 0.0807(13) Uani 1 1 d . . . F33 F 0.40055(12) 0.2457(4) 0.23251(9) 0.0725(11) Uani 1 1 d . . . F34 F 0.31317(12) 0.2723(4) 0.20539(9) 0.0709(11) Uani 1 1 d . . . F35 F 0.29904(14) 0.5422(5) 0.18487(10) 0.0833(13) Uani 1 1 d . . . F36 F 0.38683(14) 0.5450(5) 0.21376(12) 0.0998(16) Uani 1 1 d . . . F37 F 0.45525(14) 0.5437(6) 0.17800(13) 0.1138(18) Uani 1 1 d . . . F38 F 0.43581(16) 0.5230(7) 0.11163(14) 0.137(2) Uani 1 1 d . . . F39 F 0.34775(15) 0.5138(6) 0.08243(13) 0.1156(19) Uani 1 1 d . . . F40 F 0.15996(18) 0.8579(7) 0.00415(14) 0.137(2) Uani 1 1 d . . . F41 F 0.1067(3) 1.0613(8) -0.0196(2) 0.198(4) Uani 1 1 d . . . F42 F 0.0342(2) 1.1306(6) 0.00754(19) 0.175(3) Uani 1 1 d . . . F43 F 0.0118(3) 0.9943(8) 0.05789(16) 0.177(3) Uani 1 1 d . . . F44 F 0.06438(16) 0.7979(6) 0.08291(12) 0.1130(19) Uani 1 1 d . . . F45 F -0.02164(13) 0.2060(5) 0.07521(10) 0.0828(13) Uani 1 1 d . . . F46 F -0.08149(12) 0.3497(5) 0.03660(10) 0.0807(13) Uani 1 1 d . . . F47 F -0.05778(13) 0.5765(5) 0.01310(10) 0.0826(13) Uani 1 1 d . . . F48 F 0.03011(13) 0.6608(5) 0.02591(10) 0.0826(13) Uani 1 1 d . . . Cl2 Cl 0.29565(6) 0.0961(2) 0.27337(5) 0.0791(6) Uani 1 1 d . . . Cl3 Cl 0.07758(6) 0.3191(2) 0.35898(5) 0.0873(6) Uani 1 1 d . . . Cl5 Cl 0.27435(10) 0.1768(4) 0.06146(7) 0.1418(12) Uani 1 1 d . . . Cl7 Cl 0.1942(3) 0.2045(9) 0.2252(2) 0.125(3) Uani 0.433(7) 1 d P C 1 Cl6 Cl 0.11417(17) 0.5834(5) 0.15450(11) 0.1017(19) Uani 0.567(7) 1 d P C 2 Cl4 Cl 0.3965(7) 0.1736(10) 0.1229(4) 0.175(8) Uani 0.422(16) 1 d PDU B 3 Cl8 Cl 0.4296(3) 0.2149(11) 0.1459(3) 0.176(5) Uani 0.578(16) 1 d PD B 4 Cl1 Cl 0.43258(17) 0.1021(6) 0.48653(9) 0.116(3) Uani 0.632(9) 1 d P A 5 C175 C 0.2875(8) 0.283(5) 0.5204(7) 0.37(3) Uani 0.50 1 d PGDU D -1 H63 H 0.3174 0.3195 0.5234 0.446 Uiso 0.50 1 calc PR D -1 C171 C 0.2791(12) 0.171(5) 0.5366(7) 0.40(3) Uani 0.50 1 d PGU D -1 H64 H 0.3034 0.1299 0.5507 0.477 Uiso 0.50 1 calc PR D -1 C170 C 0.2354(14) 0.118(4) 0.5321(7) 0.42(3) Uani 0.50 1 d PGU D -1 H65 H 0.2297 0.0407 0.5432 0.509 Uiso 0.50 1 calc PR D -1 C172 C 0.1999(11) 0.177(4) 0.5114(8) 0.47(3) Uani 0.50 1 d PGU D -1 H66 H 0.1700 0.1411 0.5084 0.564 Uiso 0.50 1 calc PR D -1 C174 C 0.2082(8) 0.290(4) 0.4952(7) 0.44(3) Uani 0.50 1 d PGDU D -1 H67 H 0.1840 0.3307 0.4811 0.525 Uiso 0.50 1 calc PR D -1 C173 C 0.2520(8) 0.343(4) 0.4997(7) 0.38(3) Uani 0.50 1 d PGDU D -1 Cl10 Cl 0.2610(7) 0.470(4) 0.4760(8) 0.69(4) Uani 0.50 1 d PD D -1 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 0.030(3) 0.079(5) 0.066(4) 0.002(4) -0.004(3) -0.001(3) C2 0.032(3) 0.077(5) 0.070(4) -0.001(4) -0.001(3) -0.002(3) C3 0.028(3) 0.079(5) 0.064(4) -0.004(4) 0.000(3) 0.004(3) C4 0.033(3) 0.073(5) 0.074(5) 0.008(4) 0.000(3) 0.005(3) C5 0.034(3) 0.075(5) 0.060(4) -0.002(4) -0.004(3) -0.001(3) C6 0.038(3) 0.059(5) 0.063(4) 0.006(3) -0.001(3) 0.000(3) C7 0.034(3) 0.070(5) 0.080(5) -0.017(4) 0.008(3) -0.004(3) C8 0.042(4) 0.061(5) 0.076(5) -0.005(4) -0.002(3) -0.007(3) C9 0.030(3) 0.084(6) 0.061(4) 0.001(4) -0.005(3) -0.004(3) C10 0.028(3) 0.076(5) 0.070(4) 0.003(4) -0.003(3) 0.002(3) C11 0.030(3) 0.072(5) 0.054(4) 0.000(3) 0.004(3) 0.000(3) C12 0.028(3) 0.080(6) 0.056(4) -0.002(4) 0.004(3) 0.005(3) C13 0.034(3) 0.072(5) 0.054(4) 0.002(4) 0.001(3) 0.002(3) C14 0.030(3) 0.075(5) 0.053(4) 0.006(3) -0.004(3) 0.009(3) C15 0.024(3) 0.086(6) 0.061(4) 0.003(4) 0.001(3) 0.001(3) C16 0.032(3) 0.066(5) 0.066(4) -0.009(4) -0.008(3) 0.005(3) C17 0.039(4) 0.086(6) 0.062(4) -0.010(4) -0.010(3) 0.009(4) C18 0.037(4) 0.079(5) 0.073(5) 0.002(4) -0.006(3) 0.007(3) C19 0.040(4) 0.078(6) 0.070(4) -0.013(4) -0.005(3) -0.003(4) C20 0.039(3) 0.082(6) 0.058(4) 0.007(4) -0.006(3) 0.001(4) C21 0.031(3) 0.067(5) 0.062(4) 0.002(4) -0.002(3) 0.002(3) C22 0.027(3) 0.071(5) 0.062(4) 0.001(4) -0.004(3) -0.006(3) C23 0.030(3) 0.076(5) 0.059(4) -0.002(4) -0.002(3) -0.004(3) C24 0.029(3) 0.067(5) 0.058(4) -0.003(3) -0.005(3) -0.002(3) C25 0.030(3) 0.070(5) 0.058(4) -0.001(4) -0.007(3) -0.004(3) C26 0.027(3) 0.079(6) 0.069(4) 0.000(4) -0.001(3) 0.002(3) C27 0.031(3) 0.099(7) 0.067(5) -0.005(5) -0.006(3) 0.009(4) C28 0.041(4) 0.087(6) 0.061(4) -0.004(4) 0.006(3) -0.002(4) C29 0.031(3) 0.071(6) 0.078(5) -0.007(4) 0.000(3) 0.003(3) C30 0.028(3) 0.082(6) 0.092(5) -0.003(5) 0.004(3) 0.002(4) C31 0.040(4) 0.080(6) 0.060(4) -0.004(4) 0.004(3) 0.000(4) C32 0.026(3) 0.065(5) 0.069(4) -0.008(4) -0.004(3) -0.001(3) C33 0.042(4) 0.077(6) 0.076(5) -0.010(4) 0.003(3) 0.000(4) C34 0.037(4) 0.072(5) 0.078(5) -0.011(4) -0.013(3) 0.000(3) C35 0.030(3) 0.083(6) 0.089(5) 0.000(4) -0.001(3) -0.005(3) C36 0.033(3) 0.081(6) 0.082(5) 0.003(4) 0.009(3) -0.005(3) C37 0.037(3) 0.069(5) 0.069(4) -0.002(4) 0.000(3) -0.002(3) C38 0.028(3) 0.074(5) 0.061(4) -0.004(4) -0.007(3) 0.004(3) C39 0.033(3) 0.075(5) 0.068(4) 0.001(4) 0.006(3) 0.005(3) C40 0.037(4) 0.075(5) 0.077(5) -0.008(4) -0.001(3) -0.008(4) C41 0.026(3) 0.079(5) 0.071(4) -0.002(4) -0.003(3) -0.003(3) C42 0.029(3) 0.068(5) 0.069(4) -0.001(4) -0.007(3) -0.001(3) C43 0.025(3) 0.075(5) 0.075(5) -0.003(4) -0.001(3) -0.004(3) C44 0.042(4) 0.070(5) 0.056(4) -0.002(4) -0.013(3) -0.002(3) C45 0.045(4) 0.080(6) 0.072(5) -0.008(4) -0.009(3) -0.001(4) C46 0.059(5) 0.109(7) 0.066(5) -0.012(5) -0.010(4) 0.003(5) C47 0.069(5) 0.077(6) 0.069(5) -0.016(4) -0.027(4) -0.002(4) C48 0.045(4) 0.098(7) 0.080(5) 0.011(5) -0.010(4) -0.010(4) C49 0.045(4) 0.083(6) 0.059(4) -0.007(4) -0.012(3) 0.005(4) C50 0.030(3) 0.064(5) 0.063(4) 0.005(3) -0.003(3) -0.001(3) C51 0.033(3) 0.065(5) 0.068(4) 0.011(4) -0.003(3) -0.001(3) C52 0.029(3) 0.073(5) 0.071(4) 0.005(4) -0.004(3) 0.000(3) C53 0.038(3) 0.071(5) 0.062(4) -0.001(4) -0.013(3) -0.010(3) C54 0.045(4) 0.063(5) 0.065(4) -0.005(4) 0.001(3) -0.003(3) C55 0.026(3) 0.068(5) 0.059(4) 0.000(3) -0.004(3) -0.001(3) C56 0.035(3) 0.078(6) 0.078(5) 0.002(4) -0.008(3) 0.008(3) C57 0.038(4) 0.101(7) 0.070(5) 0.003(4) -0.004(3) -0.004(4) C58 0.038(4) 0.108(7) 0.073(5) 0.011(5) -0.003(3) 0.004(4) C59 0.058(4) 0.091(6) 0.064(5) -0.008(4) 0.002(4) -0.012(4) C60 0.045(4) 0.081(6) 0.076(5) 0.006(4) -0.006(3) -0.004(4) C61 0.045(4) 0.080(6) 0.076(5) 0.006(4) 0.000(3) -0.012(4) C62 0.048(4) 0.089(6) 0.069(5) 0.018(4) -0.006(3) 0.003(4) C63 0.048(4) 0.096(6) 0.067(5) 0.008(4) -0.006(3) 0.008(4) C64 0.033(3) 0.091(6) 0.070(5) -0.001(4) -0.008(3) 0.010(4) C65 0.034(3) 0.104(6) 0.055(4) -0.001(4) -0.001(3) -0.002(4) C66 0.033(3) 0.089(6) 0.059(4) 0.000(4) -0.002(3) -0.004(4) C67 0.040(4) 0.096(6) 0.058(4) 0.005(4) -0.002(3) -0.005(4) C68 0.039(4) 0.108(7) 0.058(4) 0.001(4) 0.001(3) -0.006(4) C69 0.039(4) 0.097(6) 0.065(4) -0.008(4) 0.001(3) -0.007(4) C70 0.041(4) 0.086(6) 0.072(5) 0.003(4) -0.005(3) 0.001(4) C71 0.043(4) 0.095(7) 0.076(5) -0.003(5) -0.006(3) -0.011(4) C72 0.055(4) 0.077(6) 0.092(6) -0.006(5) -0.009(4) -0.008(4) C73 0.077(5) 0.091(7) 0.075(5) 0.004(5) 0.003(4) -0.017(5) C74 0.055(4) 0.084(6) 0.066(5) -0.004(4) 0.000(3) -0.005(4) C75 0.055(4) 0.079(6) 0.063(4) 0.002(4) -0.004(3) -0.005(4) C76 0.037(4) 0.094(7) 0.075(5) -0.008(4) -0.006(3) 0.000(4) C77 0.044(4) 0.082(6) 0.083(5) 0.001(5) 0.000(3) -0.003(4) C78 0.042(4) 0.097(7) 0.074(5) -0.001(5) -0.001(3) -0.002(4) C79 0.038(4) 0.099(6) 0.073(5) 0.002(4) -0.004(3) -0.002(4) C80 0.041(4) 0.093(6) 0.072(5) 0.000(4) -0.008(3) 0.004(4) C81 0.040(4) 0.093(6) 0.077(5) 0.001(4) 0.003(3) -0.006(4) C82 0.042(4) 0.133(8) 0.068(5) 0.007(5) 0.002(3) -0.008(5) C83 0.040(4) 0.108(7) 0.094(6) -0.003(5) -0.002(4) -0.018(4) C84 0.049(4) 0.109(7) 0.085(6) 0.015(5) 0.024(4) 0.006(4) C85 0.048(4) 0.092(6) 0.066(5) 0.003(4) 0.003(3) 0.003(4) C86 0.046(4) 0.082(6) 0.083(5) -0.002(4) 0.001(4) 0.001(4) C87 0.035(3) 0.072(5) 0.061(4) 0.000(4) -0.005(3) 0.008(3) C88 0.049(4) 0.094(6) 0.061(4) -0.005(4) -0.001(3) -0.014(4) C89 0.038(4) 0.077(6) 0.084(5) -0.006(4) 0.004(3) 0.008(4) C90 0.037(4) 0.080(6) 0.079(5) -0.002(4) -0.009(3) 0.002(4) C91 0.035(3) 0.082(6) 0.071(5) -0.002(4) -0.004(3) -0.003(4) C92 0.040(4) 0.086(6) 0.066(4) 0.011(4) 0.000(3) 0.015(4) C93 0.044(4) 0.087(6) 0.091(6) -0.003(5) -0.003(4) -0.005(4) C94 0.048(4) 0.069(6) 0.093(6) -0.008(4) -0.002(4) 0.007(4) C95 0.054(5) 0.086(6) 0.096(6) -0.008(5) -0.017(4) 0.001(4) C96 0.035(4) 0.102(7) 0.148(9) -0.033(6) -0.001(5) -0.011(4) C97 0.039(4) 0.138(9) 0.114(8) -0.008(6) 0.006(5) -0.011(5) C98 0.053(5) 0.131(8) 0.084(6) -0.006(6) 0.001(4) -0.013(5) C99 0.058(5) 0.087(6) 0.073(5) -0.009(5) -0.016(4) -0.004(4) C100 0.080(6) 0.105(8) 0.098(7) 0.031(6) -0.027(5) -0.013(6) C101 0.101(8) 0.116(10) 0.151(11) 0.034(9) -0.041(8) -0.028(8) C102 0.136(11) 0.075(8) 0.128(10) 0.018(7) -0.071(8) -0.005(8) C103 0.099(8) 0.130(11) 0.136(10) -0.057(8) -0.026(7) 0.032(8) C104 0.093(7) 0.106(8) 0.071(6) -0.001(5) -0.021(5) 0.022(6) C105 0.044(4) 0.085(6) 0.066(4) 0.000(4) -0.003(3) -0.001(4) C106 0.047(4) 0.095(7) 0.069(5) -0.006(5) 0.000(3) 0.001(4) C107 0.037(4) 0.115(8) 0.068(5) -0.010(5) -0.007(3) 0.000(4) C108 0.049(4) 0.097(7) 0.062(5) 0.000(4) -0.008(3) 0.016(4) C109 0.060(5) 0.087(7) 0.075(5) 0.007(5) -0.008(4) 0.000(4) C110 0.044(4) 0.098(7) 0.056(4) 0.001(4) -0.005(3) 0.003(4) C111 0.073(11) 0.17(2) 0.077(12) 0.029(12) 0.013(9) -0.012(13) C112 0.073(9) 0.073(10) 0.076(10) -0.003(8) -0.006(7) 0.008(8) C113 0.105(14) 0.106(14) 0.075(10) -0.014(10) 0.015(10) 0.001(11) C114 0.072(10) 0.143(17) 0.078(11) 0.001(11) -0.002(9) -0.043(11) C115 0.024(6) 0.142(17) 0.133(17) 0.025(14) -0.009(8) -0.001(9) C116 0.065(13) 0.172(19) 0.097(13) 0.018(12) 0.003(10) -0.054(12) C164 0.063(14) 0.158(18) 0.071(13) 0.041(12) 0.008(11) -0.037(13) C165 0.077(15) 0.161(17) 0.088(13) 0.026(12) -0.003(13) -0.058(13) C166 0.072(12) 0.153(17) 0.064(12) 0.009(12) -0.013(11) -0.036(11) C167 0.099(14) 0.157(16) 0.079(14) 0.018(12) 0.003(12) -0.039(12) C168 0.102(14) 0.169(18) 0.070(14) 0.024(13) -0.003(13) -0.026(14) C169 0.092(14) 0.148(17) 0.091(15) 0.035(14) 0.003(12) -0.046(12) Cl9 0.093(5) 0.268(18) 0.152(8) 0.106(9) 0.038(5) 0.017(7) C117 0.045(4) 0.092(6) 0.067(4) 0.013(4) 0.010(3) 0.005(4) C118 0.048(4) 0.092(6) 0.084(5) 0.008(5) 0.003(4) 0.005(4) C119 0.038(4) 0.123(8) 0.068(5) 0.010(5) -0.008(3) 0.004(5) C120 0.051(4) 0.089(6) 0.062(4) -0.001(4) -0.006(3) 0.008(4) C121 0.056(4) 0.090(6) 0.066(4) 0.002(4) 0.002(3) -0.003(4) C122 0.040(4) 0.087(6) 0.070(5) -0.003(4) 0.001(3) -0.004(4) C123 0.064(5) 0.106(8) 0.072(5) -0.001(5) 0.013(4) 0.010(5) C124 0.071(6) 0.113(8) 0.094(6) 0.008(6) 0.014(5) 0.014(6) C125 0.091(7) 0.130(9) 0.103(7) 0.016(7) 0.031(6) 0.016(7) C126 0.075(6) 0.138(10) 0.098(7) 0.031(7) 0.009(5) 0.031(7) C127 0.066(6) 0.148(10) 0.109(7) 0.020(7) 0.006(5) 0.026(6) C128 0.056(5) 0.124(8) 0.078(5) 0.011(5) 0.012(4) 0.011(5) C129 0.13(2) 0.19(2) 0.064(15) 0.010(17) -0.019(15) 0.00(2) C130 0.116(18) 0.21(2) 0.084(17) 0.008(18) 0.028(13) 0.032(18) C131 0.106(18) 0.18(2) 0.082(14) 0.027(16) 0.021(13) 0.023(16) C132 0.078(15) 0.18(2) 0.086(15) 0.025(16) 0.001(12) -0.010(16) C133 0.068(15) 0.15(2) 0.092(18) 0.021(18) -0.005(14) -0.023(17) C134 0.089(16) 0.16(2) 0.071(15) 0.008(14) -0.004(13) -0.028(16) C158 0.055(9) 0.22(2) 0.096(13) 0.064(13) 0.014(9) -0.022(11) C159 0.082(11) 0.200(19) 0.098(15) 0.070(13) 0.004(11) -0.006(13) C160 0.089(14) 0.189(19) 0.115(14) 0.075(14) 0.006(11) -0.006(12) C161 0.083(13) 0.17(2) 0.106(15) 0.040(15) 0.006(13) -0.017(13) C162 0.089(11) 0.176(19) 0.107(14) 0.039(13) -0.006(11) -0.047(12) C163 0.066(10) 0.19(2) 0.080(12) 0.038(13) 0.005(9) -0.025(12) C135 0.076(7) 0.179(12) 0.067(6) -0.021(7) 0.005(5) 0.022(7) C136 0.080(7) 0.157(10) 0.082(6) -0.005(6) 0.013(5) 0.020(7) C137 0.080(7) 0.192(14) 0.099(8) -0.026(9) -0.003(6) 0.029(9) C138 0.088(8) 0.126(10) 0.098(7) 0.008(7) -0.010(5) 0.022(7) C139 0.120(9) 0.166(11) 0.072(6) -0.004(7) 0.024(6) 0.003(8) C140 0.059(6) 0.168(12) 0.096(7) -0.030(8) 0.006(5) 0.006(7) C146 0.090(15) 0.111(19) 0.14(2) -0.036(16) 0.014(14) 0.009(15) C147 0.127(19) 0.095(19) 0.14(2) -0.060(17) -0.024(16) 0.042(17) C151 0.127(18) 0.11(2) 0.16(2) -0.052(17) -0.050(16) 0.029(16) C148 0.089(16) 0.12(2) 0.18(2) -0.058(19) -0.001(17) 0.020(17) C150 0.040(11) 0.113(19) 0.16(2) -0.049(15) 0.006(11) 0.005(12) C149 0.068(14) 0.090(18) 0.14(2) -0.040(16) 0.039(14) -0.019(14) C152 0.078(10) 0.079(12) 0.098(11) -0.028(10) 0.014(9) -0.001(10) C153 0.050(8) 0.111(14) 0.101(12) -0.032(11) 0.019(8) -0.020(9) C154 0.063(9) 0.076(11) 0.091(10) -0.024(8) 0.011(7) -0.007(8) C155 0.091(14) 0.085(16) 0.130(16) -0.036(13) -0.001(11) 0.027(12) C156 0.058(10) 0.102(16) 0.134(15) -0.022(12) 0.020(9) 0.016(10) C157 0.066(10) 0.073(12) 0.111(13) -0.042(11) 0.018(10) -0.009(10) N1 0.023(2) 0.067(4) 0.062(3) -0.002(3) -0.001(2) 0.002(2) N2 0.025(2) 0.068(4) 0.067(3) -0.001(3) 0.001(2) 0.003(2) N3 0.029(3) 0.070(4) 0.062(3) 0.001(3) -0.004(2) -0.003(3) N4 0.029(3) 0.071(4) 0.069(3) -0.013(3) -0.007(2) 0.006(3) N5 0.029(3) 0.077(4) 0.061(3) -0.005(3) -0.005(2) 0.003(3) N6 0.041(3) 0.091(5) 0.070(4) 0.002(3) -0.001(3) -0.003(3) N7 0.034(3) 0.091(5) 0.071(4) 0.004(3) 0.002(3) -0.004(3) N8 0.041(3) 0.096(5) 0.059(3) 0.004(3) -0.006(3) -0.001(3) N9 0.036(3) 0.097(5) 0.078(4) 0.006(4) -0.005(3) -0.005(3) N10 0.043(3) 0.089(5) 0.072(4) -0.001(3) -0.001(3) -0.003(3) P1 0.0290(8) 0.0731(13) 0.0644(11) 0.0000(9) -0.0012(7) 0.0022(8) P2 0.0395(9) 0.0871(16) 0.0667(12) 0.0011(10) -0.0057(8) -0.0037(9) O1 0.036(2) 0.083(4) 0.058(3) 0.007(2) -0.0015(19) -0.001(2) O2 0.049(3) 0.092(4) 0.066(3) -0.004(3) -0.001(2) -0.005(3) F1 0.046(2) 0.079(3) 0.071(2) 0.007(2) 0.0040(17) 0.008(2) F2 0.052(2) 0.094(3) 0.084(3) -0.006(2) 0.016(2) 0.003(2) F3 0.044(2) 0.094(3) 0.098(3) -0.019(3) 0.008(2) 0.008(2) F4 0.053(2) 0.067(3) 0.094(3) 0.002(2) 0.0039(19) 0.009(2) F5 0.050(2) 0.080(3) 0.074(3) 0.004(2) 0.0061(18) 0.000(2) F6 0.043(2) 0.104(3) 0.064(2) -0.006(2) 0.0003(17) -0.003(2) F7 0.046(2) 0.114(4) 0.082(3) -0.012(3) -0.0132(19) -0.001(2) F8 0.0279(19) 0.104(4) 0.108(3) 0.005(3) -0.0053(18) -0.006(2) F9 0.047(2) 0.094(3) 0.095(3) 0.003(2) 0.017(2) -0.007(2) F10 0.0383(19) 0.103(3) 0.066(2) 0.002(2) 0.0026(17) 0.002(2) F11 0.0412(19) 0.077(3) 0.071(2) 0.010(2) 0.0012(17) 0.0068(19) F12 0.037(2) 0.078(3) 0.107(3) 0.005(2) 0.0071(19) -0.006(2) F13 0.0252(18) 0.087(3) 0.108(3) -0.001(2) -0.0058(17) -0.0026(18) F14 0.0386(19) 0.079(3) 0.076(2) 0.014(2) -0.0091(17) 0.0035(19) F15 0.0359(19) 0.080(3) 0.074(2) 0.008(2) 0.0020(16) -0.0064(19) F16 0.053(2) 0.105(4) 0.079(3) -0.022(2) 0.0068(19) -0.010(2) F17 0.087(3) 0.135(5) 0.077(3) -0.039(3) 0.005(2) -0.007(3) F18 0.091(3) 0.087(3) 0.093(3) -0.020(3) -0.017(2) -0.011(3) F19 0.070(3) 0.100(4) 0.097(3) -0.009(3) -0.002(2) -0.030(3) F20 0.052(2) 0.102(3) 0.066(2) -0.008(2) -0.0004(18) -0.012(2) F21 0.0344(18) 0.070(3) 0.079(2) -0.002(2) -0.0031(16) 0.0031(18) F22 0.0313(18) 0.085(3) 0.082(3) -0.005(2) -0.0094(16) 0.0053(18) F23 0.0362(18) 0.086(3) 0.067(2) -0.008(2) -0.0084(16) -0.0068(18) F24 0.045(2) 0.080(3) 0.064(2) -0.007(2) -0.0084(16) 0.002(2) F25 0.076(3) 0.157(5) 0.080(3) 0.005(3) -0.006(2) -0.047(3) F26 0.077(3) 0.151(5) 0.097(3) 0.004(3) -0.004(2) -0.055(3) F27 0.062(3) 0.099(4) 0.107(3) 0.016(3) 0.019(2) -0.007(2) F28 0.080(3) 0.106(4) 0.069(3) 0.000(2) 0.009(2) -0.009(3) F29 0.076(3) 0.101(4) 0.072(3) -0.001(2) 0.002(2) -0.026(3) F30 0.052(2) 0.091(3) 0.084(3) -0.019(2) -0.0018(19) -0.011(2) F31 0.046(2) 0.094(4) 0.103(3) -0.008(3) 0.011(2) 0.003(2) F32 0.036(2) 0.101(3) 0.100(3) -0.007(3) -0.0063(19) 0.005(2) F33 0.045(2) 0.088(3) 0.078(3) -0.014(2) -0.0108(18) 0.001(2) F34 0.043(2) 0.091(3) 0.075(3) -0.006(2) -0.0026(17) 0.005(2) F35 0.057(2) 0.104(4) 0.081(3) -0.013(2) -0.011(2) 0.006(2) F36 0.067(3) 0.125(4) 0.096(3) -0.030(3) -0.026(2) 0.017(3) F37 0.045(2) 0.146(5) 0.140(4) -0.042(4) -0.016(2) 0.001(3) F38 0.046(3) 0.217(7) 0.148(5) -0.017(5) 0.019(3) -0.012(3) F39 0.062(3) 0.192(6) 0.093(4) 0.000(4) 0.015(2) -0.019(3) F40 0.068(3) 0.212(7) 0.128(5) 0.072(4) 0.005(3) -0.009(4) F41 0.156(6) 0.200(8) 0.209(8) 0.135(7) -0.059(5) -0.050(6) F42 0.167(6) 0.090(5) 0.222(7) 0.005(5) -0.104(6) 0.020(4) F43 0.152(6) 0.222(8) 0.140(5) -0.053(5) -0.030(4) 0.100(6) F44 0.087(3) 0.173(6) 0.076(3) -0.009(3) 0.004(2) 0.039(4) F45 0.047(2) 0.105(4) 0.091(3) -0.003(3) -0.005(2) -0.004(2) F46 0.041(2) 0.111(4) 0.083(3) -0.011(2) -0.0104(18) 0.000(2) F47 0.053(2) 0.110(4) 0.078(3) 0.003(3) -0.009(2) 0.017(2) F48 0.061(3) 0.104(4) 0.078(3) 0.012(3) -0.002(2) 0.007(2) Cl2 0.0651(11) 0.0876(15) 0.0852(13) 0.0035(11) 0.0135(9) 0.0131(10) Cl3 0.0627(12) 0.1099(18) 0.0852(13) -0.0038(12) -0.0007(9) 0.0160(11) Cl5 0.113(2) 0.199(3) 0.1050(19) -0.006(2) -0.0068(15) 0.062(2) Cl7 0.128(6) 0.131(7) 0.125(6) -0.018(5) 0.050(5) 0.000(5) Cl6 0.111(4) 0.107(4) 0.083(3) -0.010(2) 0.002(2) 0.020(3) Cl4 0.241(18) 0.158(9) 0.152(10) 0.014(7) 0.107(12) 0.005(9) Cl8 0.116(5) 0.253(10) 0.170(9) 0.074(7) 0.054(5) -0.004(5) Cl1 0.098(3) 0.153(6) 0.084(3) 0.023(3) -0.021(2) -0.048(3) C175 0.28(3) 0.69(8) 0.13(2) -0.08(3) 0.01(2) 0.31(4) C171 0.30(3) 0.73(8) 0.15(2) -0.09(3) -0.01(2) 0.31(4) C170 0.38(4) 0.73(8) 0.15(2) -0.12(3) -0.01(3) 0.30(5) C172 0.42(4) 0.76(8) 0.21(3) -0.12(4) -0.01(3) 0.24(5) C174 0.37(4) 0.74(8) 0.18(2) -0.09(3) -0.01(3) 0.24(5) C173 0.31(4) 0.73(8) 0.099(19) -0.12(3) 0.00(2) 0.23(4) Cl10 0.40(3) 1.05(9) 0.68(5) -0.69(6) 0.25(3) -0.16(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 1.386(9) . ? C1 N1 1.391(8) . ? C1 C25 1.478(10) . ? C2 C3 1.392(9) . ? C2 H1 0.9500 . ? C3 C4 1.369(8) . ? C3 H2 0.9500 . ? C4 N1 1.432(8) . ? C4 C5 1.456(10) . ? C5 C6 1.353(8) . ? C5 C26 1.474(9) . ? C6 N2 1.415(8) . ? C6 C7 1.446(9) . ? C7 C8 1.364(8) . ? C7 H3 0.9500 . ? C8 C9 1.444(10) . ? C8 H4 0.9500 . ? C9 C10 1.372(9) . ? C9 N2 1.417(7) . ? C10 C11 1.442(10) . ? C10 C32 1.504(8) . ? C11 N3 1.341(8) . ? C11 C12 1.423(8) . ? C12 C13 1.389(10) . ? C12 P1 1.732(7) . ? C13 C23 1.409(9) . ? C13 C14 1.482(8) . ? C14 N3 1.367(8) . ? C14 C15 1.431(9) . ? C15 C16 1.391(9) . ? C15 C38 1.504(8) . ? C16 N4 1.388(7) . ? C16 C17 1.425(9) . ? C17 C18 1.391(9) . ? C17 H5 0.9500 . ? C18 C19 1.422(9) . ? C18 H6 0.9500 . ? C19 N4 1.359(8) . ? C19 C20 1.440(8) . ? C20 C21 1.396(10) . ? C20 C44 1.470(10) . ? C21 C22 1.411(8) . ? C21 N5 1.412(8) . ? C22 N4 1.354(8) . ? C22 C23 1.360(9) . ? C23 C24 1.471(8) . ? C24 C25 1.369(9) . ? C24 N5 1.414(8) . ? C25 C50 1.462(8) . ? C26 C31 1.377(10) . ? C26 C27 1.419(10) . ? C27 F1 1.338(9) . ? C27 C28 1.388(10) . ? C28 F2 1.336(8) . ? C28 C29 1.379(10) . ? C29 F3 1.342(8) . ? C29 C30 1.351(10) . ? C30 F4 1.338(9) . ? C30 C31 1.388(10) . ? C31 F5 1.346(8) . ? C32 C33 1.349(9) . ? C32 C37 1.394(9) . ? C33 F6 1.357(8) . ? C33 C34 1.394(9) . ? C34 F7 1.335(7) . ? C34 C35 1.348(10) . ? C35 F8 1.347(7) . ? C35 C36 1.370(10) . ? C36 F9 1.358(8) . ? C36 C37 1.384(8) . ? C37 F10 1.346(7) . ? C38 C39 1.372(9) . ? C38 C43 1.374(9) . ? C39 F11 1.339(7) . ? C39 C40 1.385(8) . ? C40 F12 1.348(8) . ? C40 C41 1.367(9) . ? C41 F13 1.342(6) . ? C41 C42 1.384(9) . ? C42 F14 1.318(7) . ? C42 C43 1.398(8) . ? C43 F15 1.374(8) . ? C44 C49 1.370(9) . ? C44 C45 1.391(10) . ? C45 F16 1.335(8) . ? C45 C46 1.380(11) . ? C46 F17 1.334(9) . ? C46 C47 1.371(11) . ? C47 F18 1.327(8) . ? C47 C48 1.385(11) . ? C48 F19 1.330(8) . ? C48 C49 1.369(10) . ? C49 F20 1.349(8) . ? C50 C55 1.417(9) . ? C50 C51 1.418(8) . ? C51 F21 1.354(8) . ? C51 C52 1.359(9) . ? C52 F22 1.338(7) . ? C52 C53 1.395(10) . ? C53 F23 1.344(7) . ? C53 C54 1.367(9) . ? C54 F24 1.345(8) . ? C54 C55 1.386(9) . ? C55 N5 1.372(7) . ? C56 C57 1.386(9) . ? C56 N6 1.402(8) . ? C56 C80 1.466(10) . ? C57 C58 1.366(10) . ? C57 H7 0.9500 . ? C58 C59 1.375(10) . ? C58 H8 0.9500 . ? C59 N6 1.426(9) . ? C59 C60 1.428(10) . ? C60 C61 1.367(9) . ? C60 C81 1.468(10) . ? C61 N7 1.412(9) . ? C61 C62 1.431(9) . ? C62 C63 1.331(9) . ? C62 H9 0.9500 . ? C63 C64 1.446(10) . ? C63 H10 0.9500 . ? C64 C65 1.371(10) . ? C64 N7 1.433(7) . ? C65 C66 1.436(10) . ? C65 C87 1.483(8) . ? C66 N8 1.363(9) . ? C66 C67 1.427(8) . ? C67 C68 1.391(11) . ? C67 P2 1.735(8) . ? C68 C78 1.401(10) . ? C68 C69 1.505(9) . ? C69 N8 1.346(9) . ? C69 C70 1.432(11) . ? C70 C71 1.361(11) . ? C70 C93 1.500(9) . ? C71 C72 1.411(11) . ? C71 N9 1.413(8) . ? C72 C73 1.398(11) . ? C72 H11 0.9500 . ? C73 C74 1.410(10) . ? C73 H12 0.9500 . ? C74 N9 1.377(9) . ? C74 C75 1.443(9) . ? C75 C76 1.407(11) . ? C75 C99 1.461(9) . ? C76 N10 1.420(9) . ? C76 C77 1.431(10) . ? C77 N9 1.342(9) . ? C77 C78 1.393(11) . ? C78 C79 1.452(9) . ? C79 C80 1.405(10) . ? C79 N10 1.413(9) . ? C80 C105 1.476(9) . ? C81 C82 1.368(10) . ? C81 C86 1.398(10) . ? C82 F25 1.352(8) . ? C82 C83 1.365(11) . ? C83 F26 1.335(8) . ? C83 C84 1.365(11) . ? C84 F27 1.336(8) . ? C84 C85 1.395(11) . ? C85 F28 1.291(8) . ? C85 C86 1.403(11) . ? C86 F29 1.329(8) . ? C87 C92 1.375(10) . ? C87 C88 1.388(10) . ? C88 F30 1.360(8) . ? C88 C89 1.366(9) . ? C89 F31 1.343(8) . ? C89 C90 1.381(10) . ? C90 F32 1.324(7) . ? C90 C91 1.400(10) . ? C91 F33 1.350(8) . ? C91 C92 1.353(9) . ? C92 F34 1.371(8) . ? C93 C94 1.367(10) . ? C93 C98 1.408(11) . ? C94 F35 1.350(9) . ? C94 C95 1.369(10) . ? C95 F36 1.332(9) . ? C95 C96 1.378(12) . ? C96 F37 1.350(8) . ? C96 C97 1.389(12) . ? C97 F38 1.327(10) . ? C97 C98 1.351(10) . ? C98 F39 1.346(9) . ? C99 C100 1.3900 . ? C99 C104 1.3900 . ? C100 F40 1.291(8) . ? C100 C101 1.3900 . ? C101 F41 1.270(8) . ? C101 C102 1.3900 . ? C102 F42 1.315(7) . ? C102 C103 1.3900 . ? C103 F43 1.339(9) . ? C103 C104 1.3900 . ? C104 F44 1.328(7) . ? C105 C106 1.381(9) . ? C105 C110 1.415(10) . ? C106 F45 1.344(9) . ? C106 C107 1.385(11) . ? C107 F46 1.327(8) . ? C107 C108 1.374(11) . ? C108 F47 1.343(8) . ? C108 C109 1.352(10) . ? C109 F48 1.351(9) . ? C109 C110 1.390(10) . ? C110 N10 1.398(8) . ? C111 C112 1.3900 . ? C111 C116 1.3900 . ? C111 Cl1 1.722(8) . ? C112 C113 1.3900 . ? C112 H28 0.9500 . ? C113 C114 1.3900 . ? C113 H29 0.9500 . ? C114 C115 1.3900 . ? C114 H30 0.9500 . ? C115 C116 1.3900 . ? C115 H31 0.9500 . ? C116 H32 0.9500 . ? C164 C165 1.3900 . ? C164 C169 1.3900 . ? C164 H58 0.9500 . ? C165 C166 1.3900 . ? C165 H59 0.9500 . ? C166 C167 1.3900 . ? C166 H60 0.9500 . ? C167 C168 1.3900 . ? C167 H61 0.9500 . ? C168 C169 1.3900 . ? C168 H62 0.9500 . ? C169 Cl9 1.703(16) . ? C117 C122 1.359(10) . ? C117 C118 1.409(9) . ? C117 Cl2 1.764(8) . ? C118 C119 1.353(11) . ? C118 H13 0.9500 . ? C119 C120 1.354(11) . ? C119 H14 0.9500 . ? C120 C121 1.393(9) . ? C120 H15 0.9500 . ? C121 C122 1.391(10) . ? C121 H16 0.9500 . ? C122 H17 0.9500 . ? C123 C128 1.364(11) . ? C123 C124 1.382(12) . ? C123 Cl3 1.736(9) . ? C124 C125 1.388(12) . ? C124 H18 0.9500 . ? C125 C126 1.363(13) . ? C125 H19 0.9500 . ? C126 C127 1.379(14) . ? C126 H20 0.9500 . ? C127 C128 1.426(12) . ? C127 H21 0.9500 . ? C128 H22 0.9500 . ? C129 C130 1.3900 . ? C129 C134 1.3900 . ? C129 H33 0.9500 . ? C130 C131 1.3900 . ? C130 H34 0.9500 . ? C131 C132 1.3900 . ? C131 H35 0.9500 . ? C132 C133 1.3900 . ? C132 H36 0.9500 . ? C133 C134 1.3900 . ? C133 H37 0.9500 . ? C134 Cl4 1.715(19) . ? C158 C159 1.3900 . ? C158 C163 1.3900 . ? C158 H38 0.9500 . ? C159 C160 1.3900 . ? C159 H39 0.9500 . ? C160 C161 1.3900 . ? C160 H40 0.9500 . ? C161 C162 1.3900 . ? C161 H41 0.9500 . ? C162 C163 1.3900 . ? C162 H42 0.9500 . ? C163 Cl8 1.753(16) . ? C135 C140 1.369(15) . ? C135 C136 1.395(14) . ? C135 Cl5 1.782(12) . ? C136 C137 1.397(14) . ? C136 H23 0.9500 . ? C137 C138 1.418(15) . ? C137 H24 0.9500 . ? C138 C139 1.396(14) . ? C138 H25 0.9500 . ? C139 C140 1.424(15) . ? C139 H26 0.9500 . ? C140 H27 0.9500 . ? C146 C147 1.3900 . ? C146 C149 1.3900 . ? C146 H43 0.9500 . ? C147 C151 1.3900 . ? C147 H44 0.9500 . ? C151 C148 1.3900 . ? C151 H45 0.9500 . ? C148 C150 1.3900 . ? C148 H46 0.9500 . ? C150 C149 1.3900 . ? C150 Cl7 1.666(17) . ? C149 H47 0.9500 . ? C152 C153 1.3900 . ? C152 C157 1.3900 . ? C152 Cl6 1.734(11) . ? C153 C154 1.3900 . ? C153 H48 0.9500 . ? C154 C155 1.3900 . ? C154 H49 0.9500 . ? C155 C156 1.3900 . ? C155 H50 0.9500 . ? C156 C157 1.3900 . ? C156 H51 0.9500 . ? C157 H52 0.9500 . ? N1 P1 1.689(5) . ? N2 P1 1.670(5) . ? N6 P2 1.697(6) . ? N7 P2 1.670(6) . ? P1 O1 1.461(4) . ? P2 O2 1.457(5) . ? C175 C171 1.3900 . ? C175 C173 1.3900 . ? C175 H63 0.9500 . ? C171 C170 1.3900 . ? C171 H64 0.9500 . ? C170 C172 1.3900 . ? C170 H65 0.9500 . ? C172 C174 1.3900 . ? C172 H66 0.9500 . ? C174 C173 1.3900 . ? C174 H67 0.9500 . ? C173 Cl10 1.69(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 108.3(6) . . ? C2 C1 C25 124.6(6) . . ? N1 C1 C25 127.1(6) . . ? C1 C2 C3 107.9(6) . . ? C1 C2 H1 126.0 . . ? C3 C2 H1 126.0 . . ? C4 C3 C2 109.5(6) . . ? C4 C3 H2 125.3 . . ? C2 C3 H2 125.3 . . ? C3 C4 N1 106.9(6) . . ? C3 C4 C5 130.2(7) . . ? N1 C4 C5 122.9(5) . . ? C6 C5 C4 120.1(6) . . ? C6 C5 C26 121.9(6) . . ? C4 C5 C26 117.9(6) . . ? C5 C6 N2 120.9(6) . . ? C5 C6 C7 132.0(7) . . ? N2 C6 C7 106.9(5) . . ? C8 C7 C6 108.9(6) . . ? C8 C7 H3 125.5 . . ? C6 C7 H3 125.5 . . ? C7 C8 C9 108.5(6) . . ? C7 C8 H4 125.7 . . ? C9 C8 H4 125.7 . . ? C10 C9 N2 119.9(7) . . ? C10 C9 C8 132.0(6) . . ? N2 C9 C8 107.3(6) . . ? C9 C10 C11 119.8(6) . . ? C9 C10 C32 121.9(7) . . ? C11 C10 C32 118.3(6) . . ? N3 C11 C12 113.7(6) . . ? N3 C11 C10 122.2(5) . . ? C12 C11 C10 124.1(6) . . ? C13 C12 C11 104.9(6) . . ? C13 C12 P1 133.7(5) . . ? C11 C12 P1 119.1(6) . . ? C12 C13 C23 127.1(6) . . ? C12 C13 C14 106.0(6) . . ? C23 C13 C14 126.7(7) . . ? N3 C14 C15 117.5(5) . . ? N3 C14 C13 109.1(6) . . ? C15 C14 C13 133.4(6) . . ? C16 C15 C14 126.1(5) . . ? C16 C15 C38 117.2(6) . . ? C14 C15 C38 116.7(6) . . ? N4 C16 C15 121.9(6) . . ? N4 C16 C17 102.3(6) . . ? C15 C16 C17 135.6(6) . . ? C18 C17 C16 110.6(6) . . ? C18 C17 H5 124.7 . . ? C16 C17 H5 124.7 . . ? C17 C18 C19 107.1(7) . . ? C17 C18 H6 126.5 . . ? C19 C18 H6 126.5 . . ? N4 C19 C18 105.3(5) . . ? N4 C19 C20 109.1(6) . . ? C18 C19 C20 145.6(7) . . ? C21 C20 C19 104.8(6) . . ? C21 C20 C44 131.2(6) . . ? C19 C20 C44 124.0(7) . . ? C20 C21 C22 108.5(6) . . ? C20 C21 N5 149.0(6) . . ? C22 C21 N5 102.4(6) . . ? N4 C22 C23 134.9(6) . . ? N4 C22 C21 108.3(6) . . ? C23 C22 C21 116.5(6) . . ? C22 C23 C13 121.1(6) . . ? C22 C23 C24 102.7(6) . . ? C13 C23 C24 135.8(7) . . ? C25 C24 N5 109.6(5) . . ? C25 C24 C23 142.9(6) . . ? N5 C24 C23 107.5(6) . . ? C24 C25 C50 106.0(6) . . ? C24 C25 C1 131.2(5) . . ? C50 C25 C1 121.8(6) . . ? C31 C26 C27 115.7(7) . . ? C31 C26 C5 122.7(6) . . ? C27 C26 C5 121.6(7) . . ? F1 C27 C28 119.0(7) . . ? F1 C27 C26 120.1(7) . . ? C28 C27 C26 120.9(8) . . ? F2 C28 C29 120.9(7) . . ? F2 C28 C27 119.1(8) . . ? C29 C28 C27 120.0(7) . . ? F3 C29 C30 120.9(7) . . ? F3 C29 C28 118.4(7) . . ? C30 C29 C28 120.7(7) . . ? F4 C30 C29 120.8(7) . . ? F4 C30 C31 120.0(7) . . ? C29 C30 C31 119.1(8) . . ? F5 C31 C26 119.6(6) . . ? F5 C31 C30 116.9(7) . . ? C26 C31 C30 123.6(7) . . ? C33 C32 C37 116.8(6) . . ? C33 C32 C10 124.2(6) . . ? C37 C32 C10 118.9(6) . . ? C32 C33 F6 120.0(6) . . ? C32 C33 C34 123.2(7) . . ? F6 C33 C34 116.7(6) . . ? F7 C34 C35 120.3(6) . . ? F7 C34 C33 121.2(7) . . ? C35 C34 C33 118.6(6) . . ? F8 C35 C34 121.0(6) . . ? F8 C35 C36 118.1(7) . . ? C34 C35 C36 120.9(6) . . ? F9 C36 C35 121.6(6) . . ? F9 C36 C37 119.0(6) . . ? C35 C36 C37 119.4(7) . . ? F10 C37 C36 119.1(6) . . ? F10 C37 C32 119.7(5) . . ? C36 C37 C32 121.2(6) . . ? C39 C38 C43 116.3(6) . . ? C39 C38 C15 122.2(6) . . ? C43 C38 C15 121.4(6) . . ? F11 C39 C38 121.1(5) . . ? F11 C39 C40 116.7(6) . . ? C38 C39 C40 122.1(7) . . ? F12 C40 C41 120.2(5) . . ? F12 C40 C39 120.0(7) . . ? C41 C40 C39 119.7(7) . . ? F13 C41 C40 120.3(6) . . ? F13 C41 C42 118.8(6) . . ? C40 C41 C42 120.9(6) . . ? F14 C42 C41 121.0(5) . . ? F14 C42 C43 122.1(6) . . ? C41 C42 C43 116.7(6) . . ? C38 C43 F15 121.4(5) . . ? C38 C43 C42 124.0(7) . . ? F15 C43 C42 114.5(6) . . ? C49 C44 C45 116.6(7) . . ? C49 C44 C20 121.8(7) . . ? C45 C44 C20 121.6(7) . . ? F16 C45 C46 117.4(7) . . ? F16 C45 C44 120.3(6) . . ? C46 C45 C44 122.3(8) . . ? F17 C46 C47 120.1(8) . . ? F17 C46 C45 120.6(8) . . ? C47 C46 C45 119.2(8) . . ? F18 C47 C46 120.4(8) . . ? F18 C47 C48 120.0(8) . . ? C46 C47 C48 119.6(7) . . ? F19 C48 C49 121.1(8) . . ? F19 C48 C47 119.2(8) . . ? C49 C48 C47 119.8(8) . . ? F20 C49 C48 118.3(7) . . ? F20 C49 C44 119.2(6) . . ? C48 C49 C44 122.5(7) . . ? C55 C50 C51 117.2(6) . . ? C55 C50 C25 107.7(5) . . ? C51 C50 C25 134.9(7) . . ? F21 C51 C52 117.5(6) . . ? F21 C51 C50 121.9(6) . . ? C52 C51 C50 120.3(7) . . ? F22 C52 C51 119.5(7) . . ? F22 C52 C53 119.3(6) . . ? C51 C52 C53 121.2(6) . . ? F23 C53 C54 120.5(7) . . ? F23 C53 C52 119.2(6) . . ? C54 C53 C52 120.3(6) . . ? F24 C54 C53 119.4(6) . . ? F24 C54 C55 121.0(6) . . ? C53 C54 C55 119.5(7) . . ? N5 C55 C54 131.1(7) . . ? N5 C55 C50 107.4(5) . . ? C54 C55 C50 121.4(6) . . ? C57 C56 N6 108.1(7) . . ? C57 C56 C80 122.7(6) . . ? N6 C56 C80 129.1(6) . . ? C58 C57 C56 108.0(7) . . ? C58 C57 H7 126.0 . . ? C56 C57 H7 126.0 . . ? C57 C58 C59 110.2(7) . . ? C57 C58 H8 124.9 . . ? C59 C58 H8 124.9 . . ? C58 C59 N6 106.6(7) . . ? C58 C59 C60 129.3(8) . . ? N6 C59 C60 124.0(7) . . ? C61 C60 C59 120.6(7) . . ? C61 C60 C81 121.3(7) . . ? C59 C60 C81 118.0(7) . . ? C60 C61 N7 119.4(7) . . ? C60 C61 C62 133.3(7) . . ? N7 C61 C62 106.6(6) . . ? C63 C62 C61 110.6(7) . . ? C63 C62 H9 124.7 . . ? C61 C62 H9 124.7 . . ? C62 C63 C64 108.3(6) . . ? C62 C63 H10 125.9 . . ? C64 C63 H10 125.9 . . ? C65 C64 N7 121.0(7) . . ? C65 C64 C63 130.4(6) . . ? N7 C64 C63 106.7(6) . . ? C64 C65 C66 119.6(6) . . ? C64 C65 C87 119.1(7) . . ? C66 C65 C87 121.2(6) . . ? N8 C66 C67 112.4(7) . . ? N8 C66 C65 123.2(6) . . ? C67 C66 C65 124.3(7) . . ? C68 C67 C66 105.4(6) . . ? C68 C67 P2 132.3(5) . . ? C66 C67 P2 120.9(6) . . ? C67 C68 C78 127.8(7) . . ? C67 C68 C69 106.1(6) . . ? C78 C68 C69 126.1(8) . . ? N8 C69 C70 118.2(6) . . ? N8 C69 C68 108.5(7) . . ? C70 C69 C68 133.3(7) . . ? C71 C70 C69 128.1(6) . . ? C71 C70 C93 117.5(7) . . ? C69 C70 C93 114.3(7) . . ? C70 C71 C72 137.4(7) . . ? C70 C71 N9 120.8(7) . . ? C72 C71 N9 101.8(7) . . ? C73 C72 C71 111.3(7) . . ? C73 C72 H11 124.4 . . ? C71 C72 H11 124.4 . . ? C72 C73 C74 107.8(8) . . ? C72 C73 H12 126.1 . . ? C74 C73 H12 126.1 . . ? N9 C74 C73 104.9(6) . . ? N9 C74 C75 107.8(7) . . ? C73 C74 C75 146.8(8) . . ? C76 C75 C74 105.4(7) . . ? C76 C75 C99 130.7(6) . . ? C74 C75 C99 123.8(7) . . ? C75 C76 N10 149.3(7) . . ? C75 C76 C77 108.3(7) . . ? N10 C76 C77 102.3(7) . . ? N9 C77 C78 137.1(7) . . ? N9 C77 C76 107.6(7) . . ? C78 C77 C76 115.3(7) . . ? C77 C78 C68 119.6(7) . . ? C77 C78 C79 102.7(7) . . ? C68 C78 C79 137.7(8) . . ? C80 C79 N10 108.3(6) . . ? C80 C79 C78 142.5(8) . . ? N10 C79 C78 109.0(7) . . ? C79 C80 C56 130.7(6) . . ? C79 C80 C105 106.2(7) . . ? C56 C80 C105 122.0(6) . . ? C82 C81 C86 116.0(7) . . ? C82 C81 C60 123.1(7) . . ? C86 C81 C60 120.9(7) . . ? F25 C82 C83 117.7(7) . . ? F25 C82 C81 118.3(7) . . ? C83 C82 C81 123.8(8) . . ? F26 C83 C84 120.0(8) . . ? F26 C83 C82 120.7(8) . . ? C84 C83 C82 119.3(8) . . ? F27 C84 C83 121.0(8) . . ? F27 C84 C85 118.0(8) . . ? C83 C84 C85 120.9(8) . . ? F28 C85 C84 121.9(7) . . ? F28 C85 C86 120.6(7) . . ? C84 C85 C86 117.5(7) . . ? F29 C86 C81 121.0(7) . . ? F29 C86 C85 116.6(7) . . ? C81 C86 C85 122.4(7) . . ? C92 C87 C88 114.3(6) . . ? C92 C87 C65 122.9(7) . . ? C88 C87 C65 122.7(7) . . ? F30 C88 C89 116.8(7) . . ? F30 C88 C87 119.5(6) . . ? C89 C88 C87 123.6(7) . . ? F31 C89 C88 120.6(7) . . ? F31 C89 C90 119.3(6) . . ? C88 C89 C90 120.1(7) . . ? F32 C90 C89 122.1(7) . . ? F32 C90 C91 120.2(7) . . ? C89 C90 C91 117.6(6) . . ? F33 C91 C92 122.3(7) . . ? F33 C91 C90 117.8(6) . . ? C92 C91 C90 119.8(7) . . ? C91 C92 F34 115.2(7) . . ? C91 C92 C87 124.5(7) . . ? F34 C92 C87 120.3(6) . . ? C94 C93 C98 116.3(7) . . ? C94 C93 C70 121.4(7) . . ? C98 C93 C70 122.3(7) . . ? F35 C94 C93 119.8(6) . . ? F35 C94 C95 117.6(8) . . ? C93 C94 C95 122.6(8) . . ? F36 C95 C94 120.9(8) . . ? F36 C95 C96 120.4(7) . . ? C94 C95 C96 118.7(9) . . ? F37 C96 C95 118.3(9) . . ? F37 C96 C97 120.3(8) . . ? C95 C96 C97 121.4(7) . . ? F38 C97 C98 122.3(9) . . ? F38 C97 C96 120.2(7) . . ? C98 C97 C96 117.5(8) . . ? F39 C98 C97 117.9(8) . . ? F39 C98 C93 118.6(7) . . ? C97 C98 C93 123.4(9) . . ? C100 C99 C104 120.0 . . ? C100 C99 C75 120.8(6) . . ? C104 C99 C75 119.1(6) . . ? F40 C100 C101 119.2(6) . . ? F40 C100 C99 120.8(6) . . ? C101 C100 C99 120.0 . . ? F41 C101 C100 123.4(8) . . ? F41 C101 C102 116.6(8) . . ? C100 C101 C102 120.0 . . ? F42 C102 C103 116.9(9) . . ? F42 C102 C101 123.1(9) . . ? C103 C102 C101 120.0 . . ? F43 C103 C102 121.9(7) . . ? F43 C103 C104 118.1(7) . . ? C102 C103 C104 120.0 . . ? F44 C104 C103 119.3(6) . . ? F44 C104 C99 120.7(6) . . ? C103 C104 C99 120.0 . . ? C106 C105 C110 117.5(7) . . ? C106 C105 C80 134.7(8) . . ? C110 C105 C80 107.7(6) . . ? F45 C106 C105 123.2(7) . . ? F45 C106 C107 116.0(7) . . ? C105 C106 C107 120.8(9) . . ? F46 C107 C108 119.5(7) . . ? F46 C107 C106 120.5(9) . . ? C108 C107 C106 120.0(7) . . ? F47 C108 C109 119.1(8) . . ? F47 C108 C107 119.3(7) . . ? C109 C108 C107 121.4(7) . . ? F48 C109 C108 121.4(7) . . ? F48 C109 C110 119.6(7) . . ? C108 C109 C110 119.0(8) . . ? C109 C110 N10 130.9(8) . . ? C109 C110 C105 121.1(7) . . ? N10 C110 C105 107.4(6) . . ? C112 C111 C116 120.0 . . ? C112 C111 Cl1 123.8(8) . . ? C116 C111 Cl1 116.2(8) . . ? C111 C112 C113 120.0 . . ? C111 C112 H28 120.0 . . ? C113 C112 H28 120.0 . . ? C112 C113 C114 120.0 . . ? C112 C113 H29 120.0 . . ? C114 C113 H29 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H30 120.0 . . ? C115 C114 H30 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 H31 120.0 . . ? C114 C115 H31 120.0 . . ? C115 C116 C111 120.0 . . ? C115 C116 H32 120.0 . . ? C111 C116 H32 120.0 . . ? C165 C164 C169 120.0 . . ? C165 C164 H58 120.0 . . ? C169 C164 H58 120.0 . . ? C164 C165 C166 120.0 . . ? C164 C165 H59 120.0 . . ? C166 C165 H59 120.0 . . ? C167 C166 C165 120.0 . . ? C167 C166 H60 120.0 . . ? C165 C166 H60 120.0 . . ? C168 C167 C166 120.0 . . ? C168 C167 H61 120.0 . . ? C166 C167 H61 120.0 . . ? C167 C168 C169 120.0 . . ? C167 C168 H62 120.0 . . ? C169 C168 H62 120.0 . . ? C168 C169 C164 120.0 . . ? C168 C169 Cl9 120.0 . . ? C164 C169 Cl9 120.0 . . ? C122 C117 C118 122.2(7) . . ? C122 C117 Cl2 118.9(5) . . ? C118 C117 Cl2 118.9(7) . . ? C119 C118 C117 118.4(8) . . ? C119 C118 H13 120.8 . . ? C117 C118 H13 120.8 . . ? C118 C119 C120 120.3(7) . . ? C118 C119 H14 119.9 . . ? C120 C119 H14 119.9 . . ? C119 C120 C121 121.8(8) . . ? C119 C120 H15 119.1 . . ? C121 C120 H15 119.1 . . ? C122 C121 C120 118.8(8) . . ? C122 C121 H16 120.6 . . ? C120 C121 H16 120.6 . . ? C117 C122 C121 118.3(7) . . ? C117 C122 H17 120.8 . . ? C121 C122 H17 120.8 . . ? C128 C123 C124 121.7(9) . . ? C128 C123 Cl3 118.4(8) . . ? C124 C123 Cl3 119.8(7) . . ? C123 C124 C125 118.9(9) . . ? C123 C124 H18 120.6 . . ? C125 C124 H18 120.6 . . ? C126 C125 C124 121.5(11) . . ? C126 C125 H19 119.3 . . ? C124 C125 H19 119.3 . . ? C125 C126 C127 119.2(10) . . ? C125 C126 H20 120.4 . . ? C127 C126 H20 120.4 . . ? C126 C127 C128 120.6(10) . . ? C126 C127 H21 119.7 . . ? C128 C127 H21 119.7 . . ? C123 C128 C127 118.0(10) . . ? C123 C128 H22 121.0 . . ? C127 C128 H22 121.0 . . ? C130 C129 C134 120.0 . . ? C130 C129 H33 120.0 . . ? C134 C129 H33 120.0 . . ? C129 C130 C131 120.0 . . ? C129 C130 H34 120.0 . . ? C131 C130 H34 120.0 . . ? C132 C131 C130 120.0 . . ? C132 C131 H35 120.0 . . ? C130 C131 H35 120.0 . . ? C131 C132 C133 120.0 . . ? C131 C132 H36 120.0 . . ? C133 C132 H36 120.0 . . ? C132 C133 C134 120.0 . . ? C132 C133 H37 120.0 . . ? C134 C133 H37 120.0 . . ? C133 C134 C129 120.0 . . ? C133 C134 Cl4 115.4(16) . . ? C129 C134 Cl4 124.5(15) . . ? C159 C158 C163 120.0 . . ? C159 C158 H38 120.0 . . ? C163 C158 H38 120.0 . . ? C160 C159 C158 120.0 . . ? C160 C159 H39 120.0 . . ? C158 C159 H39 120.0 . . ? C159 C160 C161 120.0 . . ? C159 C160 H40 120.0 . . ? C161 C160 H40 120.0 . . ? C160 C161 C162 120.0 . . ? C160 C161 H41 120.0 . . ? C162 C161 H41 120.0 . . ? C161 C162 C163 120.0 . . ? C161 C162 H42 120.0 . . ? C163 C162 H42 120.0 . . ? C162 C163 C158 120.0 . . ? C162 C163 Cl8 120.4(11) . . ? C158 C163 Cl8 119.6(11) . . ? C140 C135 C136 127.9(11) . . ? C140 C135 Cl5 118.2(9) . . ? C136 C135 Cl5 113.8(11) . . ? C135 C136 C137 113.1(12) . . ? C135 C136 H23 123.4 . . ? C137 C136 H23 123.4 . . ? C136 C137 C138 123.8(11) . . ? C136 C137 H24 118.1 . . ? C138 C137 H24 118.1 . . ? C139 C138 C137 118.5(11) . . ? C139 C138 H25 120.8 . . ? C137 C138 H25 120.8 . . ? C138 C139 C140 120.3(12) . . ? C138 C139 H26 119.8 . . ? C140 C139 H26 119.8 . . ? C135 C140 C139 116.2(10) . . ? C135 C140 H27 121.9 . . ? C139 C140 H27 121.9 . . ? C147 C146 C149 120.0 . . ? C147 C146 H43 120.0 . . ? C149 C146 H43 120.0 . . ? C146 C147 C151 120.0 . . ? C146 C147 H44 120.0 . . ? C151 C147 H44 120.0 . . ? C148 C151 C147 120.0 . . ? C148 C151 H45 120.0 . . ? C147 C151 H45 120.0 . . ? C150 C148 C151 120.0 . . ? C150 C148 H46 120.0 . . ? C151 C148 H46 120.0 . . ? C149 C150 C148 120.0 . . ? C149 C150 Cl7 115.9(12) . . ? C148 C150 Cl7 124.0(12) . . ? C150 C149 C146 120.0 . . ? C150 C149 H47 120.0 . . ? C146 C149 H47 120.0 . . ? C153 C152 C157 120.0 . . ? C153 C152 Cl6 118.7(8) . . ? C157 C152 Cl6 121.3(8) . . ? C154 C153 C152 120.0 . . ? C154 C153 H48 120.0 . . ? C152 C153 H48 120.0 . . ? C153 C154 C155 120.0 . . ? C153 C154 H49 120.0 . . ? C155 C154 H49 120.0 . . ? C154 C155 C156 120.0 . . ? C154 C155 H50 120.0 . . ? C156 C155 H50 120.0 . . ? C157 C156 C155 120.0 . . ? C157 C156 H51 120.0 . . ? C155 C156 H51 120.0 . . ? C156 C157 C152 120.0 . . ? C156 C157 H52 120.0 . . ? C152 C157 H52 120.0 . . ? C1 N1 C4 107.4(5) . . ? C1 N1 P1 129.0(5) . . ? C4 N1 P1 122.7(4) . . ? C6 N2 C9 108.0(5) . . ? C6 N2 P1 126.0(4) . . ? C9 N2 P1 124.4(5) . . ? C11 N3 C14 106.2(5) . . ? C22 N4 C19 109.2(5) . . ? C22 N4 C16 135.8(6) . . ? C19 N4 C16 114.5(5) . . ? C55 N5 C21 140.1(6) . . ? C55 N5 C24 109.3(5) . . ? C21 N5 C24 110.5(5) . . ? C56 N6 C59 106.8(6) . . ? C56 N6 P2 129.4(5) . . ? C59 N6 P2 122.6(5) . . ? C61 N7 C64 107.1(6) . . ? C61 N7 P2 127.8(4) . . ? C64 N7 P2 124.7(5) . . ? C69 N8 C66 107.7(6) . . ? C77 N9 C74 110.9(6) . . ? C77 N9 C71 134.6(7) . . ? C74 N9 C71 114.1(7) . . ? C110 N10 C79 110.0(6) . . ? C110 N10 C76 139.1(7) . . ? C79 N10 C76 110.4(5) . . ? O1 P1 N2 118.4(3) . . ? O1 P1 N1 111.3(2) . . ? N2 P1 N1 98.4(3) . . ? O1 P1 C12 114.8(3) . . ? N2 P1 C12 96.7(3) . . ? N1 P1 C12 115.7(3) . . ? O2 P2 N7 119.0(3) . . ? O2 P2 N6 110.4(3) . . ? N7 P2 N6 97.6(3) . . ? O2 P2 C67 116.0(3) . . ? N7 P2 C67 97.2(3) . . ? N6 P2 C67 114.9(4) . . ? C171 C175 C173 120.0 . . ? C171 C175 H63 120.0 . . ? C173 C175 H63 120.0 . . ? C170 C171 C175 120.0 . . ? C170 C171 H64 120.0 . . ? C175 C171 H64 120.0 . . ? C172 C170 C171 120.0 . . ? C172 C170 H65 120.0 . . ? C171 C170 H65 120.0 . . ? C170 C172 C174 120.0 . . ? C170 C172 H66 120.0 . . ? C174 C172 H66 120.0 . . ? C173 C174 C172 120.0 . . ? C173 C174 H67 120.0 . . ? C172 C174 H67 120.0 . . ? C174 C173 C175 120.0 . . ? C174 C173 Cl10 117.3(11) . . ? C175 C173 Cl10 122.3(12) . . ? 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 N1 C1 C2 C3 -1.5(8) . . . . ? C25 C1 C2 C3 175.9(6) . . . . ? C1 C2 C3 C4 -0.3(8) . . . . ? C2 C3 C4 N1 1.9(7) . . . . ? C2 C3 C4 C5 -178.4(7) . . . . ? C3 C4 C5 C6 -170.8(7) . . . . ? N1 C4 C5 C6 8.8(10) . . . . ? C3 C4 C5 C26 7.8(11) . . . . ? N1 C4 C5 C26 -172.6(6) . . . . ? C4 C5 C6 N2 -0.8(9) . . . . ? C26 C5 C6 N2 -179.3(6) . . . . ? C4 C5 C6 C7 172.7(7) . . . . ? C26 C5 C6 C7 -5.9(11) . . . . ? C5 C6 C7 C8 -169.5(7) . . . . ? N2 C6 C7 C8 4.6(8) . . . . ? C6 C7 C8 C9 -1.1(8) . . . . ? C7 C8 C9 C10 166.8(7) . . . . ? C7 C8 C9 N2 -2.9(8) . . . . ? N2 C9 C10 C11 4.4(10) . . . . ? C8 C9 C10 C11 -164.2(7) . . . . ? N2 C9 C10 C32 -175.9(6) . . . . ? C8 C9 C10 C32 15.5(12) . . . . ? C9 C10 C11 N3 169.2(6) . . . . ? C32 C10 C11 N3 -10.5(9) . . . . ? C9 C10 C11 C12 -9.7(10) . . . . ? C32 C10 C11 C12 170.6(6) . . . . ? N3 C11 C12 C13 0.4(7) . . . . ? C10 C11 C12 C13 179.3(6) . . . . ? N3 C11 C12 P1 165.5(4) . . . . ? C10 C11 C12 P1 -15.5(9) . . . . ? C11 C12 C13 C23 176.1(6) . . . . ? P1 C12 C13 C23 14.1(11) . . . . ? C11 C12 C13 C14 1.1(7) . . . . ? P1 C12 C13 C14 -160.9(5) . . . . ? C12 C13 C14 N3 -2.3(7) . . . . ? C23 C13 C14 N3 -177.3(6) . . . . ? C12 C13 C14 C15 174.4(7) . . . . ? C23 C13 C14 C15 -0.7(11) . . . . ? N3 C14 C15 C16 174.6(6) . . . . ? C13 C14 C15 C16 -1.8(12) . . . . ? N3 C14 C15 C38 -3.9(9) . . . . ? C13 C14 C15 C38 179.6(6) . . . . ? C14 C15 C16 N4 1.2(11) . . . . ? C38 C15 C16 N4 179.7(6) . . . . ? C14 C15 C16 C17 -173.0(7) . . . . ? C38 C15 C16 C17 5.5(12) . . . . ? N4 C16 C17 C18 -1.8(8) . . . . ? C15 C16 C17 C18 173.1(8) . . . . ? C16 C17 C18 C19 -1.1(8) . . . . ? C17 C18 C19 N4 3.6(8) . . . . ? C17 C18 C19 C20 -175.3(11) . . . . ? N4 C19 C20 C21 -1.8(8) . . . . ? C18 C19 C20 C21 177.0(11) . . . . ? N4 C19 C20 C44 178.8(6) . . . . ? C18 C19 C20 C44 -2.3(16) . . . . ? C19 C20 C21 C22 2.0(8) . . . . ? C44 C20 C21 C22 -178.7(7) . . . . ? C19 C20 C21 N5 -174.2(10) . . . . ? C44 C20 C21 N5 5.1(17) . . . . ? C20 C21 C22 N4 -1.5(8) . . . . ? N5 C21 C22 N4 176.5(5) . . . . ? C20 C21 C22 C23 -176.7(6) . . . . ? N5 C21 C22 C23 1.3(8) . . . . ? N4 C22 C23 C13 -5.2(12) . . . . ? C21 C22 C23 C13 168.3(6) . . . . ? N4 C22 C23 C24 -178.5(7) . . . . ? C21 C22 C23 C24 -5.0(8) . . . . ? C12 C13 C23 C22 -170.0(7) . . . . ? C14 C13 C23 C22 4.0(10) . . . . ? C12 C13 C23 C24 0.6(12) . . . . ? C14 C13 C23 C24 174.6(7) . . . . ? C22 C23 C24 C25 -173.4(9) . . . . ? C13 C23 C24 C25 14.9(15) . . . . ? C22 C23 C24 N5 6.6(7) . . . . ? C13 C23 C24 N5 -165.2(7) . . . . ? N5 C24 C25 C50 2.9(7) . . . . ? C23 C24 C25 C50 -177.1(9) . . . . ? N5 C24 C25 C1 -165.6(7) . . . . ? C23 C24 C25 C1 14.4(15) . . . . ? C2 C1 C25 C24 141.3(8) . . . . ? N1 C1 C25 C24 -41.8(12) . . . . ? C2 C1 C25 C50 -25.7(10) . . . . ? N1 C1 C25 C50 151.2(6) . . . . ? C6 C5 C26 C31 -63.4(9) . . . . ? C4 C5 C26 C31 118.1(7) . . . . ? C6 C5 C26 C27 115.2(8) . . . . ? C4 C5 C26 C27 -63.3(8) . . . . ? C31 C26 C27 F1 178.4(5) . . . . ? C5 C26 C27 F1 -0.3(9) . . . . ? C31 C26 C27 C28 -2.6(9) . . . . ? C5 C26 C27 C28 178.7(6) . . . . ? F1 C27 C28 F2 0.2(9) . . . . ? C26 C27 C28 F2 -178.8(6) . . . . ? F1 C27 C28 C29 -179.7(6) . . . . ? C26 C27 C28 C29 1.3(10) . . . . ? F2 C28 C29 F3 0.0(9) . . . . ? C27 C28 C29 F3 179.8(6) . . . . ? F2 C28 C29 C30 -178.5(6) . . . . ? C27 C28 C29 C30 1.4(10) . . . . ? F3 C29 C30 F4 2.0(10) . . . . ? C28 C29 C30 F4 -179.6(6) . . . . ? F3 C29 C30 C31 179.0(6) . . . . ? C28 C29 C30 C31 -2.6(10) . . . . ? C27 C26 C31 F5 -179.0(5) . . . . ? C5 C26 C31 F5 -0.3(9) . . . . ? C27 C26 C31 C30 1.4(10) . . . . ? C5 C26 C31 C30 -179.9(6) . . . . ? F4 C30 C31 F5 -1.4(9) . . . . ? C29 C30 C31 F5 -178.5(6) . . . . ? F4 C30 C31 C26 178.2(6) . . . . ? C29 C30 C31 C26 1.2(10) . . . . ? C9 C10 C32 C33 -70.4(10) . . . . ? C11 C10 C32 C33 109.3(8) . . . . ? C9 C10 C32 C37 113.5(8) . . . . ? C11 C10 C32 C37 -66.8(9) . . . . ? C37 C32 C33 F6 176.7(6) . . . . ? C10 C32 C33 F6 0.5(11) . . . . ? C37 C32 C33 C34 0.6(12) . . . . ? C10 C32 C33 C34 -175.6(7) . . . . ? C32 C33 C34 F7 178.0(7) . . . . ? F6 C33 C34 F7 1.8(11) . . . . ? C32 C33 C34 C35 -1.4(12) . . . . ? F6 C33 C34 C35 -177.6(7) . . . . ? F7 C34 C35 F8 -0.1(12) . . . . ? C33 C34 C35 F8 179.3(7) . . . . ? F7 C34 C35 C36 -177.7(7) . . . . ? C33 C34 C35 C36 1.7(12) . . . . ? F8 C35 C36 F9 -0.1(11) . . . . ? C34 C35 C36 F9 177.4(7) . . . . ? F8 C35 C36 C37 -178.9(7) . . . . ? C34 C35 C36 C37 -1.3(12) . . . . ? F9 C36 C37 F10 2.1(11) . . . . ? C35 C36 C37 F10 -179.1(7) . . . . ? F9 C36 C37 C32 -178.3(6) . . . . ? C35 C36 C37 C32 0.5(12) . . . . ? C33 C32 C37 F10 179.4(6) . . . . ? C10 C32 C37 F10 -4.2(10) . . . . ? C33 C32 C37 C36 -0.1(11) . . . . ? C10 C32 C37 C36 176.3(7) . . . . ? C16 C15 C38 C39 -123.1(8) . . . . ? C14 C15 C38 C39 55.6(9) . . . . ? C16 C15 C38 C43 60.3(9) . . . . ? C14 C15 C38 C43 -121.0(7) . . . . ? C43 C38 C39 F11 -175.2(6) . . . . ? C15 C38 C39 F11 8.1(10) . . . . ? C43 C38 C39 C40 0.9(10) . . . . ? C15 C38 C39 C40 -175.9(7) . . . . ? F11 C39 C40 F12 -7.4(10) . . . . ? C38 C39 C40 F12 176.3(6) . . . . ? F11 C39 C40 C41 175.6(6) . . . . ? C38 C39 C40 C41 -0.6(11) . . . . ? F12 C40 C41 F13 3.2(10) . . . . ? C39 C40 C41 F13 -179.9(6) . . . . ? F12 C40 C41 C42 -179.7(6) . . . . ? C39 C40 C41 C42 -2.7(11) . . . . ? F13 C41 C42 F14 -2.0(10) . . . . ? C40 C41 C42 F14 -179.1(6) . . . . ? F13 C41 C42 C43 -177.4(6) . . . . ? C40 C41 C42 C43 5.4(10) . . . . ? C39 C38 C43 F15 178.5(6) . . . . ? C15 C38 C43 F15 -4.7(10) . . . . ? C39 C38 C43 C42 2.1(11) . . . . ? C15 C38 C43 C42 178.9(7) . . . . ? F14 C42 C43 C38 179.3(6) . . . . ? C41 C42 C43 C38 -5.2(11) . . . . ? F14 C42 C43 F15 2.8(10) . . . . ? C41 C42 C43 F15 178.2(6) . . . . ? C21 C20 C44 C49 57.1(11) . . . . ? C19 C20 C44 C49 -123.7(8) . . . . ? C21 C20 C44 C45 -125.5(8) . . . . ? C19 C20 C44 C45 53.6(10) . . . . ? C49 C44 C45 F16 178.4(6) . . . . ? C20 C44 C45 F16 0.9(10) . . . . ? C49 C44 C45 C46 0.2(11) . . . . ? C20 C44 C45 C46 -177.3(7) . . . . ? F16 C45 C46 F17 2.7(11) . . . . ? C44 C45 C46 F17 -179.1(7) . . . . ? F16 C45 C46 C47 -179.0(7) . . . . ? C44 C45 C46 C47 -0.8(12) . . . . ? F17 C46 C47 F18 -0.6(12) . . . . ? C45 C46 C47 F18 -178.9(7) . . . . ? F17 C46 C47 C48 179.9(7) . . . . ? C45 C46 C47 C48 1.6(12) . . . . ? F18 C47 C48 F19 -0.5(11) . . . . ? C46 C47 C48 F19 178.9(7) . . . . ? F18 C47 C48 C49 178.6(6) . . . . ? C46 C47 C48 C49 -1.9(12) . . . . ? F19 C48 C49 F20 -2.1(10) . . . . ? C47 C48 C49 F20 178.8(7) . . . . ? F19 C48 C49 C44 -179.5(7) . . . . ? C47 C48 C49 C44 1.4(11) . . . . ? C45 C44 C49 F20 -177.9(6) . . . . ? C20 C44 C49 F20 -0.4(10) . . . . ? C45 C44 C49 C48 -0.5(11) . . . . ? C20 C44 C49 C48 176.9(7) . . . . ? C24 C25 C50 C55 -2.3(7) . . . . ? C1 C25 C50 C55 167.6(6) . . . . ? C24 C25 C50 C51 173.2(7) . . . . ? C1 C25 C50 C51 -16.9(12) . . . . ? C55 C50 C51 F21 174.1(6) . . . . ? C25 C50 C51 F21 -1.1(12) . . . . ? C55 C50 C51 C52 0.2(10) . . . . ? C25 C50 C51 C52 -175.0(7) . . . . ? F21 C51 C52 F22 5.0(10) . . . . ? C50 C51 C52 F22 179.2(6) . . . . ? F21 C51 C52 C53 -174.8(6) . . . . ? C50 C51 C52 C53 -0.6(10) . . . . ? F22 C52 C53 F23 0.5(10) . . . . ? C51 C52 C53 F23 -179.7(6) . . . . ? F22 C52 C53 C54 -179.6(6) . . . . ? C51 C52 C53 C54 0.3(11) . . . . ? F23 C53 C54 F24 -3.0(10) . . . . ? C52 C53 C54 F24 177.1(6) . . . . ? F23 C53 C54 C55 -179.6(6) . . . . ? C52 C53 C54 C55 0.5(11) . . . . ? F24 C54 C55 N5 -2.2(11) . . . . ? C53 C54 C55 N5 174.3(7) . . . . ? F24 C54 C55 C50 -177.5(6) . . . . ? C53 C54 C55 C50 -0.9(10) . . . . ? C51 C50 C55 N5 -175.7(6) . . . . ? C25 C50 C55 N5 0.8(7) . . . . ? C51 C50 C55 C54 0.6(10) . . . . ? C25 C50 C55 C54 177.0(6) . . . . ? N6 C56 C57 C58 -2.9(9) . . . . ? C80 C56 C57 C58 -179.8(7) . . . . ? C56 C57 C58 C59 0.5(9) . . . . ? C57 C58 C59 N6 2.1(9) . . . . ? C57 C58 C59 C60 178.7(8) . . . . ? C58 C59 C60 C61 -172.3(8) . . . . ? N6 C59 C60 C61 3.8(12) . . . . ? C58 C59 C60 C81 4.8(12) . . . . ? N6 C59 C60 C81 -179.1(7) . . . . ? C59 C60 C61 N7 2.6(11) . . . . ? C81 C60 C61 N7 -174.4(7) . . . . ? C59 C60 C61 C62 171.2(8) . . . . ? C81 C60 C61 C62 -5.8(14) . . . . ? C60 C61 C62 C63 -162.4(9) . . . . ? N7 C61 C62 C63 7.3(9) . . . . ? C61 C62 C63 C64 -2.1(9) . . . . ? C62 C63 C64 C65 159.9(8) . . . . ? C62 C63 C64 N7 -3.8(9) . . . . ? N7 C64 C65 C66 -3.7(11) . . . . ? C63 C64 C65 C66 -165.4(7) . . . . ? N7 C64 C65 C87 173.4(6) . . . . ? C63 C64 C65 C87 11.7(12) . . . . ? C64 C65 C66 N8 173.5(6) . . . . ? C87 C65 C66 N8 -3.5(11) . . . . ? C64 C65 C66 C67 -2.0(11) . . . . ? C87 C65 C66 C67 -179.0(7) . . . . ? N8 C66 C67 C68 -0.1(8) . . . . ? C65 C66 C67 C68 175.8(7) . . . . ? N8 C66 C67 P2 167.7(5) . . . . ? C65 C66 C67 P2 -16.3(10) . . . . ? C66 C67 C68 C78 -179.5(7) . . . . ? P2 C67 C68 C78 14.6(13) . . . . ? C66 C67 C68 C69 0.2(8) . . . . ? P2 C67 C68 C69 -165.7(6) . . . . ? C67 C68 C69 N8 -0.2(8) . . . . ? C78 C68 C69 N8 179.5(7) . . . . ? C67 C68 C69 C70 -179.1(8) . . . . ? C78 C68 C69 C70 0.6(13) . . . . ? N8 C69 C70 C71 176.2(8) . . . . ? C68 C69 C70 C71 -4.9(14) . . . . ? N8 C69 C70 C93 -4.9(10) . . . . ? C68 C69 C70 C93 173.9(8) . . . . ? C69 C70 C71 C72 179.0(9) . . . . ? C93 C70 C71 C72 0.2(15) . . . . ? C69 C70 C71 N9 1.1(13) . . . . ? C93 C70 C71 N9 -177.7(7) . . . . ? C70 C71 C72 C73 -177.4(10) . . . . ? N9 C71 C72 C73 0.7(9) . . . . ? C71 C72 C73 C74 -0.1(10) . . . . ? C72 C73 C74 N9 -0.6(9) . . . . ? C72 C73 C74 C75 168.8(11) . . . . ? N9 C74 C75 C76 -2.5(8) . . . . ? C73 C74 C75 C76 -171.8(11) . . . . ? N9 C74 C75 C99 173.7(7) . . . . ? C73 C74 C75 C99 4.4(17) . . . . ? C74 C75 C76 N10 -180(100) . . . . ? C99 C75 C76 N10 4.6(19) . . . . ? C74 C75 C76 C77 2.6(8) . . . . ? C99 C75 C76 C77 -173.2(7) . . . . ? C75 C76 C77 N9 -1.8(9) . . . . ? N10 C76 C77 N9 179.3(6) . . . . ? C75 C76 C77 C78 175.7(7) . . . . ? N10 C76 C77 C78 -3.2(9) . . . . ? N9 C77 C78 C68 -3.0(15) . . . . ? C76 C77 C78 C68 -179.6(7) . . . . ? N9 C77 C78 C79 176.0(9) . . . . ? C76 C77 C78 C79 -0.6(9) . . . . ? C67 C68 C78 C77 -175.8(7) . . . . ? C69 C68 C78 C77 4.5(12) . . . . ? C67 C68 C78 C79 5.6(15) . . . . ? C69 C68 C78 C79 -174.0(8) . . . . ? C77 C78 C79 C80 -170.6(11) . . . . ? C68 C78 C79 C80 8.1(19) . . . . ? C77 C78 C79 N10 4.2(8) . . . . ? C68 C78 C79 N10 -177.1(9) . . . . ? N10 C79 C80 C56 -162.4(8) . . . . ? C78 C79 C80 C56 12.4(17) . . . . ? N10 C79 C80 C105 5.5(8) . . . . ? C78 C79 C80 C105 -179.7(10) . . . . ? C57 C56 C80 C79 142.5(9) . . . . ? N6 C56 C80 C79 -33.7(14) . . . . ? C57 C56 C80 C105 -23.7(12) . . . . ? N6 C56 C80 C105 160.1(7) . . . . ? C61 C60 C81 C82 -118.2(9) . . . . ? C59 C60 C81 C82 64.7(11) . . . . ? C61 C60 C81 C86 64.0(11) . . . . ? C59 C60 C81 C86 -113.0(8) . . . . ? C86 C81 C82 F25 -178.1(7) . . . . ? C60 C81 C82 F25 4.0(13) . . . . ? C86 C81 C82 C83 -3.3(13) . . . . ? C60 C81 C82 C83 178.8(8) . . . . ? F25 C82 C83 F26 -0.2(13) . . . . ? C81 C82 C83 F26 -175.0(8) . . . . ? F25 C82 C83 C84 178.8(8) . . . . ? C81 C82 C83 C84 4.0(14) . . . . ? F26 C83 C84 F27 -2.3(13) . . . . ? C82 C83 C84 F27 178.7(8) . . . . ? F26 C83 C84 C85 177.6(8) . . . . ? C82 C83 C84 C85 -1.3(13) . . . . ? F27 C84 C85 F28 1.2(12) . . . . ? C83 C84 C85 F28 -178.8(8) . . . . ? F27 C84 C85 C86 178.4(7) . . . . ? C83 C84 C85 C86 -1.5(12) . . . . ? C82 C81 C86 F29 -177.0(7) . . . . ? C60 C81 C86 F29 0.9(11) . . . . ? C82 C81 C86 C85 0.2(12) . . . . ? C60 C81 C86 C85 178.1(8) . . . . ? F28 C85 C86 F29 -3.3(11) . . . . ? C84 C85 C86 F29 179.5(7) . . . . ? F28 C85 C86 C81 179.4(7) . . . . ? C84 C85 C86 C81 2.1(12) . . . . ? C64 C65 C87 C92 -123.4(8) . . . . ? C66 C65 C87 C92 53.6(10) . . . . ? C64 C65 C87 C88 52.8(10) . . . . ? C66 C65 C87 C88 -130.2(8) . . . . ? C92 C87 C88 F30 -179.4(6) . . . . ? C65 C87 C88 F30 4.2(10) . . . . ? C92 C87 C88 C89 -0.7(11) . . . . ? C65 C87 C88 C89 -177.1(7) . . . . ? F30 C88 C89 F31 -1.4(10) . . . . ? C87 C88 C89 F31 179.9(7) . . . . ? F30 C88 C89 C90 177.6(7) . . . . ? C87 C88 C89 C90 -1.1(12) . . . . ? F31 C89 C90 F32 1.0(11) . . . . ? C88 C89 C90 F32 -178.1(7) . . . . ? F31 C89 C90 C91 179.9(6) . . . . ? C88 C89 C90 C91 0.8(11) . . . . ? F32 C90 C91 F33 -3.5(10) . . . . ? C89 C90 C91 F33 177.5(7) . . . . ? F32 C90 C91 C92 -179.9(7) . . . . ? C89 C90 C91 C92 1.2(11) . . . . ? F33 C91 C92 F34 -1.9(10) . . . . ? C90 C91 C92 F34 174.3(6) . . . . ? F33 C91 C92 C87 -179.4(7) . . . . ? C90 C91 C92 C87 -3.2(12) . . . . ? C88 C87 C92 C91 2.9(11) . . . . ? C65 C87 C92 C91 179.3(7) . . . . ? C88 C87 C92 F34 -174.5(6) . . . . ? C65 C87 C92 F34 1.9(11) . . . . ? C71 C70 C93 C94 110.2(9) . . . . ? C69 C70 C93 C94 -68.8(10) . . . . ? C71 C70 C93 C98 -72.4(11) . . . . ? C69 C70 C93 C98 108.6(9) . . . . ? C98 C93 C94 F35 179.4(8) . . . . ? C70 C93 C94 F35 -3.0(12) . . . . ? C98 C93 C94 C95 -1.3(13) . . . . ? C70 C93 C94 C95 176.3(8) . . . . ? F35 C94 C95 F36 2.1(12) . . . . ? C93 C94 C95 F36 -177.2(8) . . . . ? F35 C94 C95 C96 -178.4(8) . . . . ? C93 C94 C95 C96 2.3(14) . . . . ? F36 C95 C96 F37 -1.1(14) . . . . ? C94 C95 C96 F37 179.4(8) . . . . ? F36 C95 C96 C97 177.4(9) . . . . ? C94 C95 C96 C97 -2.2(15) . . . . ? F37 C96 C97 F38 0.9(16) . . . . ? C95 C96 C97 F38 -177.5(9) . . . . ? F37 C96 C97 C98 179.4(9) . . . . ? C95 C96 C97 C98 1.0(16) . . . . ? F38 C97 C98 F39 -1.2(16) . . . . ? C96 C97 C98 F39 -179.7(9) . . . . ? F38 C97 C98 C93 178.5(9) . . . . ? C96 C97 C98 C93 0.0(16) . . . . ? C94 C93 C98 F39 179.8(8) . . . . ? C70 C93 C98 F39 2.3(14) . . . . ? C94 C93 C98 C97 0.1(15) . . . . ? C70 C93 C98 C97 -177.4(9) . . . . ? C76 C75 C99 C100 -134.0(7) . . . . ? C74 C75 C99 C100 50.8(8) . . . . ? C76 C75 C99 C104 49.2(10) . . . . ? C74 C75 C99 C104 -126.0(7) . . . . ? C104 C99 C100 F40 -179.5(7) . . . . ? C75 C99 C100 F40 3.7(7) . . . . ? C104 C99 C100 C101 0.0 . . . . ? C75 C99 C100 C101 -176.8(5) . . . . ? F40 C100 C101 F41 -0.1(7) . . . . ? C99 C100 C101 F41 -179.7(8) . . . . ? F40 C100 C101 C102 179.5(7) . . . . ? C99 C100 C101 C102 0.0 . . . . ? F41 C101 C102 F42 -1.0(8) . . . . ? C100 C101 C102 F42 179.3(6) . . . . ? F41 C101 C102 C103 179.7(7) . . . . ? C100 C101 C102 C103 0.0 . . . . ? F42 C102 C103 F43 2.7(7) . . . . ? C101 C102 C103 F43 -178.0(7) . . . . ? F42 C102 C103 C104 -179.3(6) . . . . ? C101 C102 C103 C104 0.0 . . . . ? F43 C103 C104 F44 -2.9(6) . . . . ? C102 C103 C104 F44 179.0(6) . . . . ? F43 C103 C104 C99 178.1(7) . . . . ? C102 C103 C104 C99 0.0 . . . . ? C100 C99 C104 F44 -179.0(6) . . . . ? C75 C99 C104 F44 -2.2(7) . . . . ? C100 C99 C104 C103 0.0 . . . . ? C75 C99 C104 C103 176.8(5) . . . . ? C79 C80 C105 C106 169.6(8) . . . . ? C56 C80 C105 C106 -21.2(13) . . . . ? C79 C80 C105 C110 -6.3(9) . . . . ? C56 C80 C105 C110 162.9(7) . . . . ? C110 C105 C106 F45 174.9(7) . . . . ? C80 C105 C106 F45 -0.7(14) . . . . ? C110 C105 C106 C107 -2.0(11) . . . . ? C80 C105 C106 C107 -177.6(8) . . . . ? F45 C106 C107 F46 1.5(11) . . . . ? C105 C106 C107 F46 178.7(7) . . . . ? F45 C106 C107 C108 -177.2(7) . . . . ? C105 C106 C107 C108 -0.1(12) . . . . ? F46 C107 C108 F47 -0.3(11) . . . . ? C106 C107 C108 F47 178.4(7) . . . . ? F46 C107 C108 C109 -174.8(7) . . . . ? C106 C107 C108 C109 4.0(12) . . . . ? F47 C108 C109 F48 -0.3(12) . . . . ? C107 C108 C109 F48 174.1(7) . . . . ? F47 C108 C109 C110 180.0(7) . . . . ? C107 C108 C109 C110 -5.6(12) . . . . ? F48 C109 C110 N10 -5.9(13) . . . . ? C108 C109 C110 N10 173.8(8) . . . . ? F48 C109 C110 C105 -176.3(7) . . . . ? C108 C109 C110 C105 3.4(12) . . . . ? C106 C105 C110 C109 0.3(11) . . . . ? C80 C105 C110 C109 177.1(7) . . . . ? C106 C105 C110 N10 -172.1(6) . . . . ? C80 C105 C110 N10 4.6(8) . . . . ? C116 C111 C112 C113 0.0 . . . . ? Cl1 C111 C112 C113 176.9(10) . . . . ? C111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 C111 0.0 . . . . ? C112 C111 C116 C115 0.0 . . . . ? Cl1 C111 C116 C115 -177.1(9) . . . . ? C169 C164 C165 C166 0.0 . . . . ? C164 C165 C166 C167 0.0 . . . . ? C165 C166 C167 C168 0.0 . . . . ? C166 C167 C168 C169 0.0 . . . . ? C167 C168 C169 C164 0.0 . . . . ? C167 C168 C169 Cl9 180.0 . . . . ? C165 C164 C169 C168 0.0 . . . . ? C165 C164 C169 Cl9 180.0 . . . . ? C122 C117 C118 C119 4.8(11) . . . . ? Cl2 C117 C118 C119 -176.8(6) . . . . ? C117 C118 C119 C120 0.0(11) . . . . ? C118 C119 C120 C121 -4.0(12) . . . . ? C119 C120 C121 C122 3.4(11) . . . . ? C118 C117 C122 C121 -5.3(11) . . . . ? Cl2 C117 C122 C121 176.3(5) . . . . ? C120 C121 C122 C117 1.2(10) . . . . ? C128 C123 C124 C125 3.6(13) . . . . ? Cl3 C123 C124 C125 -179.3(7) . . . . ? C123 C124 C125 C126 -3.8(14) . . . . ? C124 C125 C126 C127 1.4(16) . . . . ? C125 C126 C127 C128 1.3(16) . . . . ? C124 C123 C128 C127 -1.0(13) . . . . ? Cl3 C123 C128 C127 -178.2(7) . . . . ? C126 C127 C128 C123 -1.5(14) . . . . ? C134 C129 C130 C131 0.0 . . . . ? C129 C130 C131 C132 0.0 . . . . ? C130 C131 C132 C133 0.0 . . . . ? C131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C129 0.0 . . . . ? C132 C133 C134 Cl4 -178.0(18) . . . . ? C130 C129 C134 C133 0.0 . . . . ? C130 C129 C134 Cl4 178(2) . . . . ? C163 C158 C159 C160 0.0 . . . . ? C158 C159 C160 C161 0.0 . . . . ? C159 C160 C161 C162 0.0 . . . . ? C160 C161 C162 C163 0.0 . . . . ? C161 C162 C163 C158 0.0 . . . . ? C161 C162 C163 Cl8 179.4(12) . . . . ? C159 C158 C163 C162 0.0 . . . . ? C159 C158 C163 Cl8 -179.4(12) . . . . ? C140 C135 C136 C137 -3.2(15) . . . . ? Cl5 C135 C136 C137 179.8(7) . . . . ? C135 C136 C137 C138 0.6(15) . . . . ? C136 C137 C138 C139 -0.9(16) . . . . ? C137 C138 C139 C140 3.3(15) . . . . ? C136 C135 C140 C139 5.5(16) . . . . ? Cl5 C135 C140 C139 -177.6(7) . . . . ? C138 C139 C140 C135 -5.3(14) . . . . ? C149 C146 C147 C151 0.0 . . . . ? C146 C147 C151 C148 0.0 . . . . ? C147 C151 C148 C150 0.0 . . . . ? C151 C148 C150 C149 0.0 . . . . ? C151 C148 C150 Cl7 -175.5(17) . . . . ? C148 C150 C149 C146 0.0 . . . . ? Cl7 C150 C149 C146 175.8(16) . . . . ? C147 C146 C149 C150 0.0 . . . . ? C157 C152 C153 C154 0.0 . . . . ? Cl6 C152 C153 C154 -179.6(11) . . . . ? C152 C153 C154 C155 0.0 . . . . ? C153 C154 C155 C156 0.0 . . . . ? C154 C155 C156 C157 0.0 . . . . ? C155 C156 C157 C152 0.0 . . . . ? C153 C152 C157 C156 0.0 . . . . ? Cl6 C152 C157 C156 179.6(11) . . . . ? C2 C1 N1 C4 2.6(7) . . . . ? C25 C1 N1 C4 -174.6(6) . . . . ? C2 C1 N1 P1 171.3(5) . . . . ? C25 C1 N1 P1 -6.0(10) . . . . ? C3 C4 N1 C1 -2.8(7) . . . . ? C5 C4 N1 C1 177.5(6) . . . . ? C3 C4 N1 P1 -172.4(4) . . . . ? C5 C4 N1 P1 8.0(9) . . . . ? C5 C6 N2 C9 168.5(6) . . . . ? C7 C6 N2 C9 -6.4(7) . . . . ? C5 C6 N2 P1 -25.3(9) . . . . ? C7 C6 N2 P1 159.8(5) . . . . ? C10 C9 N2 C6 -165.4(6) . . . . ? C8 C9 N2 C6 5.8(7) . . . . ? C10 C9 N2 P1 28.1(9) . . . . ? C8 C9 N2 P1 -160.7(5) . . . . ? C12 C11 N3 C14 -1.8(7) . . . . ? C10 C11 N3 C14 179.2(6) . . . . ? C15 C14 N3 C11 -174.8(5) . . . . ? C13 C14 N3 C11 2.5(7) . . . . ? C23 C22 N4 C19 174.2(8) . . . . ? C21 C22 N4 C19 0.3(8) . . . . ? C23 C22 N4 C16 3.0(14) . . . . ? C21 C22 N4 C16 -170.8(7) . . . . ? C18 C19 N4 C22 -178.4(6) . . . . ? C20 C19 N4 C22 1.0(8) . . . . ? C18 C19 N4 C16 -5.1(8) . . . . ? C20 C19 N4 C16 174.2(6) . . . . ? C15 C16 N4 C22 -0.6(12) . . . . ? C17 C16 N4 C22 175.2(7) . . . . ? C15 C16 N4 C19 -171.5(7) . . . . ? C17 C16 N4 C19 4.4(8) . . . . ? C54 C55 N5 C21 10.8(13) . . . . ? C50 C55 N5 C21 -173.5(7) . . . . ? C54 C55 N5 C24 -174.7(7) . . . . ? C50 C55 N5 C24 1.0(7) . . . . ? C20 C21 N5 C55 -6.0(17) . . . . ? C22 C21 N5 C55 177.7(8) . . . . ? C20 C21 N5 C24 180(100) . . . . ? C22 C21 N5 C24 3.2(7) . . . . ? C25 C24 N5 C55 -2.6(7) . . . . ? C23 C24 N5 C55 177.5(5) . . . . ? C25 C24 N5 C21 173.7(5) . . . . ? C23 C24 N5 C21 -6.3(7) . . . . ? C57 C56 N6 C59 4.1(8) . . . . ? C80 C56 N6 C59 -179.3(7) . . . . ? C57 C56 N6 P2 171.8(5) . . . . ? C80 C56 N6 P2 -11.5(11) . . . . ? C58 C59 N6 C56 -3.7(8) . . . . ? C60 C59 N6 C56 179.4(7) . . . . ? C58 C59 N6 P2 -172.5(5) . . . . ? C60 C59 N6 P2 10.6(10) . . . . ? C60 C61 N7 C64 162.0(7) . . . . ? C62 C61 N7 C64 -9.4(8) . . . . ? C60 C61 N7 P2 -25.5(10) . . . . ? C62 C61 N7 P2 163.1(5) . . . . ? C65 C64 N7 C61 -157.3(7) . . . . ? C63 C64 N7 C61 8.2(8) . . . . ? C65 C64 N7 P2 29.9(10) . . . . ? C63 C64 N7 P2 -164.6(5) . . . . ? C70 C69 N8 C66 179.2(6) . . . . ? C68 C69 N8 C66 0.1(8) . . . . ? C67 C66 N8 C69 0.0(8) . . . . ? C65 C66 N8 C69 -176.0(7) . . . . ? C78 C77 N9 C74 -176.5(9) . . . . ? C76 C77 N9 C74 0.2(9) . . . . ? C78 C77 N9 C71 -3.9(16) . . . . ? C76 C77 N9 C71 172.8(8) . . . . ? C73 C74 N9 C77 175.4(6) . . . . ? C75 C74 N9 C77 1.5(9) . . . . ? C73 C74 N9 C71 1.1(9) . . . . ? C75 C74 N9 C71 -172.8(6) . . . . ? C70 C71 N9 C77 5.0(13) . . . . ? C72 C71 N9 C77 -173.6(8) . . . . ? C70 C71 N9 C74 177.4(7) . . . . ? C72 C71 N9 C74 -1.2(9) . . . . ? C109 C110 N10 C79 -172.7(8) . . . . ? C105 C110 N10 C79 -1.3(8) . . . . ? C109 C110 N10 C76 17.5(15) . . . . ? C105 C110 N10 C76 -171.1(8) . . . . ? C80 C79 N10 C110 -2.8(8) . . . . ? C78 C79 N10 C110 -179.4(6) . . . . ? C80 C79 N10 C76 170.1(6) . . . . ? C78 C79 N10 C76 -6.5(8) . . . . ? C75 C76 N10 C110 -2.3(19) . . . . ? C77 C76 N10 C110 175.6(8) . . . . ? C75 C76 N10 C79 -172.2(12) . . . . ? C77 C76 N10 C79 5.7(8) . . . . ? C6 N2 P1 O1 -85.2(6) . . . . ? C9 N2 P1 O1 78.9(6) . . . . ? C6 N2 P1 N1 34.6(6) . . . . ? C9 N2 P1 N1 -161.4(5) . . . . ? C6 N2 P1 C12 151.9(6) . . . . ? C9 N2 P1 C12 -44.0(6) . . . . ? C1 N1 P1 O1 -67.1(6) . . . . ? C4 N1 P1 O1 100.0(5) . . . . ? C1 N1 P1 N2 167.9(5) . . . . ? C4 N1 P1 N2 -25.0(5) . . . . ? C1 N1 P1 C12 66.2(6) . . . . ? C4 N1 P1 C12 -126.6(5) . . . . ? C13 C12 P1 O1 70.4(7) . . . . ? C11 C12 P1 O1 -89.6(5) . . . . ? C13 C12 P1 N2 -164.1(7) . . . . ? C11 C12 P1 N2 35.9(5) . . . . ? C13 C12 P1 N1 -61.4(7) . . . . ? C11 C12 P1 N1 138.6(5) . . . . ? C61 N7 P2 O2 -85.5(7) . . . . ? C64 N7 P2 O2 85.7(6) . . . . ? C61 N7 P2 N6 32.9(7) . . . . ? C64 N7 P2 N6 -155.8(6) . . . . ? C61 N7 P2 C67 149.3(7) . . . . ? C64 N7 P2 C67 -39.4(7) . . . . ? C56 N6 P2 O2 -65.3(7) . . . . ? C59 N6 P2 O2 100.8(6) . . . . ? C56 N6 P2 N7 169.9(6) . . . . ? C59 N6 P2 N7 -24.1(6) . . . . ? C56 N6 P2 C67 68.3(7) . . . . ? C59 N6 P2 C67 -125.7(6) . . . . ? C68 C67 P2 O2 68.5(8) . . . . ? C66 C67 P2 O2 -95.6(6) . . . . ? C68 C67 P2 N7 -164.2(7) . . . . ? C66 C67 P2 N7 31.7(6) . . . . ? C68 C67 P2 N6 -62.4(8) . . . . ? C66 C67 P2 N6 133.5(6) . . . . ? C173 C175 C171 C170 0.0 . . . . ? C175 C171 C170 C172 0.0 . . . . ? C171 C170 C172 C174 0.0 . . . . ? C170 C172 C174 C173 0.0 . . . . ? C172 C174 C173 C175 0.0 . . . . ? C172 C174 C173 Cl10 173(2) . . . . ? C171 C175 C173 C174 0.0 . . . . ? C171 C175 C173 Cl10 -173(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 62.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.757 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.090 # Attachment 'PS-Eur.CIF' data_1125hi _database_code_depnum_ccdc_archive 'CCDC 827556' #TrackingRef 'PS-Eur.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H6 F24 N5 P S, 3(C7 H8)' _chemical_formula_sum 'C76 H30 F24 N5 P S' _chemical_formula_weight 1532.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.4591(5) _cell_length_b 8.6913(2) _cell_length_c 37.1609(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.5998(18) _cell_angle_gamma 90.00 _cell_volume 6264.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 25344 _cell_measurement_theta_min 3.165 _cell_measurement_theta_max 68.215 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7274 _exptl_absorpt_correction_T_max 0.7274 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\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 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60930 _diffrn_reflns_av_R_equivalents 0.1115 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 68.25 _reflns_number_total 11391 _reflns_number_gt 7915 _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^)+(0.0229P)^2^+7.4531P] 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 11391 _refine_ls_number_parameters 1028 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.057 _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 0.30860(18) 0.3587(4) 0.42313(9) 0.0257(8) Uani 1 1 d . . . C2 C 0.35530(18) 0.3445(4) 0.45285(10) 0.0274(8) Uani 1 1 d . . . H1 H 0.3492 0.3829 0.4763 0.033 Uiso 1 1 calc R . . C3 C 0.41317(18) 0.2645(4) 0.44286(9) 0.0263(8) Uani 1 1 d . . . H2 H 0.4527 0.2391 0.4584 0.032 Uiso 1 1 calc R . . C4 C 0.40342(17) 0.2286(4) 0.40683(9) 0.0235(8) Uani 1 1 d . . . C5 C 0.44584(17) 0.1388(4) 0.38461(9) 0.0236(8) Uani 1 1 d . . . C6 C 0.42837(17) 0.1181(4) 0.34899(10) 0.0244(8) Uani 1 1 d . . . C7 C 0.46004(18) 0.0399(4) 0.32002(10) 0.0280(8) Uani 1 1 d . . . H3 H 0.5001 -0.0227 0.3229 0.034 Uiso 1 1 calc R . . C8 C 0.42370(18) 0.0700(4) 0.28847(10) 0.0265(8) Uani 1 1 d . . . H4 H 0.4337 0.0306 0.2656 0.032 Uiso 1 1 calc R . . C9 C 0.36718(17) 0.1714(4) 0.29482(9) 0.0237(8) Uani 1 1 d . . . C10 C 0.32307(17) 0.2568(4) 0.27209(9) 0.0239(8) Uani 1 1 d . . . C11 C 0.28359(17) 0.3765(4) 0.28801(9) 0.0238(8) Uani 1 1 d . . . C12 C 0.27362(17) 0.3902(4) 0.32518(9) 0.0242(8) Uani 1 1 d . . . C13 C 0.23485(17) 0.5226(4) 0.32867(9) 0.0227(8) Uani 1 1 d . . . C14 C 0.22355(17) 0.5860(4) 0.29157(9) 0.0227(8) Uani 1 1 d . . . C15 C 0.18652(17) 0.7154(4) 0.27696(9) 0.0242(8) Uani 1 1 d . . . C16 C 0.14151(18) 0.8089(4) 0.29434(10) 0.0248(8) Uani 1 1 d . . . C17 C 0.09340(18) 0.9277(4) 0.28380(10) 0.0276(8) Uani 1 1 d . . . H5 H 0.0876 0.9732 0.2605 0.033 Uiso 1 1 calc R . . C18 C 0.05650(18) 0.9661(4) 0.31286(10) 0.0279(8) Uani 1 1 d . . . H6 H 0.0208 1.0406 0.3127 0.033 Uiso 1 1 calc R . . C19 C 0.08104(17) 0.8754(4) 0.34286(10) 0.0247(8) Uani 1 1 d . . . C20 C 0.07725(17) 0.8412(4) 0.38097(10) 0.0246(8) Uani 1 1 d . . . C21 C 0.12701(18) 0.7279(4) 0.38873(10) 0.0249(8) Uani 1 1 d . . . C22 C 0.16102(18) 0.6966(4) 0.35745(9) 0.0241(8) Uani 1 1 d . . . C23 C 0.20856(17) 0.5831(4) 0.35973(9) 0.0228(8) Uani 1 1 d . . . C24 C 0.21003(18) 0.5365(4) 0.39784(10) 0.0250(8) Uani 1 1 d . . . C25 C 0.24284(18) 0.4382(4) 0.42258(9) 0.0250(8) Uani 1 1 d . . . C26 C 0.51148(18) 0.0734(4) 0.40154(9) 0.0242(8) Uani 1 1 d . . . C27 C 0.51390(19) -0.0277(4) 0.43074(10) 0.0279(8) Uani 1 1 d . . . C28 C 0.5747(2) -0.0879(4) 0.44588(10) 0.0327(9) Uani 1 1 d . . . C29 C 0.6362(2) -0.0489(4) 0.43241(10) 0.0348(9) Uani 1 1 d . . . C30 C 0.63625(19) 0.0503(4) 0.40375(10) 0.0328(9) Uani 1 1 d . . . C31 C 0.57461(19) 0.1117(4) 0.38916(10) 0.0280(8) Uani 1 1 d . . . C32 C 0.31594(18) 0.2403(4) 0.23238(10) 0.0244(8) Uani 1 1 d . . . C33 C 0.36846(18) 0.2693(4) 0.21035(10) 0.0262(8) Uani 1 1 d . . . C34 C 0.35843(19) 0.2631(4) 0.17296(10) 0.0286(8) Uani 1 1 d . . . C35 C 0.2943(2) 0.2286(4) 0.15690(10) 0.0287(8) Uani 1 1 d . . . C36 C 0.24087(18) 0.1996(4) 0.17780(10) 0.0277(8) Uani 1 1 d . . . C37 C 0.25205(18) 0.2054(4) 0.21490(10) 0.0275(8) Uani 1 1 d . . . C38 C 0.19254(18) 0.7467(4) 0.23778(9) 0.0246(8) Uani 1 1 d . . . C39 C 0.25254(18) 0.8038(4) 0.22535(10) 0.0267(8) Uani 1 1 d . . . C40 C 0.2600(2) 0.8257(4) 0.18918(11) 0.0327(9) Uani 1 1 d . . . C41 C 0.2058(2) 0.7926(4) 0.16406(10) 0.0343(9) Uani 1 1 d . . . C42 C 0.1460(2) 0.7343(4) 0.17531(10) 0.0298(9) Uani 1 1 d . . . C43 C 0.13964(19) 0.7129(4) 0.21166(10) 0.0268(8) Uani 1 1 d . . . C44 C 0.02965(18) 0.9199(4) 0.40368(9) 0.0250(8) Uani 1 1 d . . . C45 C -0.04034(19) 0.9283(4) 0.39445(10) 0.0297(8) Uani 1 1 d . . . C46 C -0.08505(19) 1.0019(4) 0.41541(11) 0.0330(9) Uani 1 1 d . . . C47 C -0.0600(2) 1.0733(4) 0.44647(11) 0.0331(9) Uani 1 1 d . . . C48 C 0.0099(2) 1.0715(4) 0.45634(10) 0.0336(9) Uani 1 1 d . . . C49 C 0.05310(19) 0.9940(4) 0.43536(10) 0.0296(8) Uani 1 1 d . . . C50 C 0.20329(18) 0.4492(4) 0.45436(9) 0.0257(8) Uani 1 1 d . . . C51 C 0.20138(19) 0.3608(4) 0.48587(10) 0.0292(8) Uani 1 1 d . . . C52 C 0.1535(2) 0.3915(4) 0.51007(10) 0.0319(9) Uani 1 1 d . . . C53 C 0.10509(19) 0.5074(4) 0.50341(10) 0.0318(9) Uani 1 1 d . . . C54 C 0.10406(18) 0.5934(4) 0.47236(10) 0.0289(8) Uani 1 1 d . . . C55 C 0.15210(18) 0.5638(4) 0.44815(10) 0.0264(8) Uani 1 1 d . . . C56 C 0.4547(2) 0.5652(4) 0.33252(11) 0.0352(9) Uani 1 1 d . . . C57 C 0.4034(2) 0.6672(4) 0.31917(12) 0.0388(10) Uani 1 1 d . . . H7 H 0.3948 0.6790 0.2938 0.047 Uiso 1 1 calc R . . C58 C 0.3651(2) 0.7508(5) 0.34172(13) 0.0428(11) Uani 1 1 d . . . H8 H 0.3305 0.8194 0.3319 0.051 Uiso 1 1 calc R . . C59 C 0.3772(2) 0.7348(5) 0.37850(13) 0.0462(11) Uani 1 1 d . . . H9 H 0.3508 0.7926 0.3942 0.055 Uiso 1 1 calc R . . C60 C 0.4277(2) 0.6345(5) 0.39274(12) 0.0447(11) Uani 1 1 d . . . H10 H 0.4360 0.6235 0.4181 0.054 Uiso 1 1 calc R . . C61 C 0.4660(2) 0.5507(4) 0.36982(11) 0.0408(10) Uani 1 1 d . . . H11 H 0.5006 0.4821 0.3797 0.049 Uiso 1 1 calc R . . C62 C 0.4959(2) 0.4756(5) 0.30739(12) 0.0466(11) Uani 1 1 d . . . H12 H 0.5293 0.4105 0.3214 0.070 Uiso 1 1 calc R . . H13 H 0.5204 0.5468 0.2925 0.070 Uiso 1 1 calc R . . H14 H 0.4649 0.4107 0.2918 0.070 Uiso 1 1 calc R . . C63 C 0.3217(2) 0.7543(5) 0.00715(11) 0.0409(10) Uani 1 1 d . . . C64 C 0.2774(2) 0.8105(5) 0.03179(12) 0.0475(11) Uani 1 1 d . . . H15 H 0.2314 0.7735 0.0310 0.057 Uiso 1 1 calc R . . C65 C 0.2992(2) 0.9191(5) 0.05737(12) 0.0491(12) Uani 1 1 d . . . H16 H 0.2679 0.9562 0.0737 0.059 Uiso 1 1 calc R . . C66 C 0.3660(2) 0.9743(5) 0.05952(12) 0.0486(12) Uani 1 1 d . . . H17 H 0.3808 1.0495 0.0770 0.058 Uiso 1 1 calc R . . C67 C 0.4107(2) 0.9177(5) 0.03565(12) 0.0479(11) Uani 1 1 d . . . H18 H 0.4569 0.9536 0.0369 0.058 Uiso 1 1 calc R . . C68 C 0.3889(2) 0.8099(5) 0.01006(12) 0.0418(10) Uani 1 1 d . . . H19 H 0.4207 0.7725 -0.0060 0.050 Uiso 1 1 calc R . . C69 C 0.2976(2) 0.6408(5) -0.02125(13) 0.0571(13) Uani 1 1 d . . . H20 H 0.2491 0.6158 -0.0189 0.086 Uiso 1 1 calc R . . H21 H 0.3254 0.5469 -0.0184 0.086 Uiso 1 1 calc R . . H22 H 0.3025 0.6851 -0.0452 0.086 Uiso 1 1 calc R . . C70A C 0.0165(4) 0.4460(9) 0.3582(2) 0.039(2) Uani 0.583(7) 1 d P A 1 C71A C 0.0671(13) 0.344(3) 0.3507(8) 0.038(6) Uani 0.583(7) 1 d P A 1 H23 H 0.0867 0.2793 0.3694 0.045 Uiso 0.583(7) 1 calc PR A 1 C72A C 0.0904(3) 0.3340(8) 0.3169(2) 0.0346(19) Uani 0.583(7) 1 d P A 1 H24 H 0.1253 0.2614 0.3126 0.042 Uiso 0.583(7) 1 calc PR A 1 C73A C 0.0651(6) 0.4228(15) 0.2901(3) 0.028(3) Uani 0.583(7) 1 d P A 1 H25 H 0.0818 0.4138 0.2669 0.033 Uiso 0.583(7) 1 calc PR A 1 C74A C 0.0114(4) 0.5347(8) 0.2963(2) 0.037(2) Uani 0.583(7) 1 d P A 1 H26 H -0.0070 0.6004 0.2775 0.045 Uiso 0.583(7) 1 calc PR A 1 C75A C -0.0114(7) 0.5419(13) 0.3300(3) 0.037(3) Uani 0.583(7) 1 d P A 1 H27 H -0.0467 0.6130 0.3347 0.045 Uiso 0.583(7) 1 calc PR A 1 C76A C -0.0103(6) 0.4548(13) 0.3952(3) 0.053(3) Uani 0.583(7) 1 d P A 1 H28 H -0.0471 0.5318 0.3950 0.079 Uiso 0.583(7) 1 calc PR A 1 H29 H 0.0273 0.4842 0.4130 0.079 Uiso 0.583(7) 1 calc PR A 1 H30 H -0.0285 0.3541 0.4016 0.079 Uiso 0.583(7) 1 calc PR A 1 C70B C 0.0371(5) 0.4278(12) 0.3266(3) 0.043(3) Uani 0.417(7) 1 d PU A 2 C71B C -0.0148(11) 0.508(2) 0.3428(6) 0.044(3) Uani 0.417(7) 1 d PU A 2 H31 H -0.0437 0.5757 0.3284 0.053 Uiso 0.417(7) 1 calc PR A 2 C72B C -0.0251(8) 0.4927(15) 0.3779(4) 0.047(3) Uani 0.417(7) 1 d PU A 2 H32 H -0.0617 0.5473 0.3876 0.056 Uiso 0.417(7) 1 calc PR A 2 C73B C 0.0189(6) 0.3938(14) 0.4010(4) 0.041(3) Uani 0.417(7) 1 d PU A 2 H33 H 0.0124 0.3822 0.4259 0.049 Uiso 0.417(7) 1 calc PR A 2 C74B C 0.0702(5) 0.3179(11) 0.3854(3) 0.040(3) Uani 0.417(7) 1 d PU A 2 H34 H 0.1007 0.2544 0.4000 0.048 Uiso 0.417(7) 1 calc PR A 2 C75B C 0.079(2) 0.330(6) 0.3489(13) 0.036(4) Uani 0.417(7) 1 d PU A 2 H35 H 0.1142 0.2721 0.3388 0.044 Uiso 0.417(7) 1 calc PR A 2 C76B C 0.0437(9) 0.450(3) 0.2867(6) 0.043(5) Uani 0.417(7) 1 d PU A 2 H36 H 0.0812 0.3848 0.2791 0.065 Uiso 0.417(7) 1 calc PR A 2 H37 H 0.0539 0.5578 0.2819 0.065 Uiso 0.417(7) 1 calc PR A 2 H38 H 0.0004 0.4204 0.2731 0.065 Uiso 0.417(7) 1 calc PR A 2 F1 F 0.45524(11) -0.0705(2) 0.44472(5) 0.0348(5) Uani 1 1 d . . . F2 F 0.57425(12) -0.1843(3) 0.47418(6) 0.0458(6) Uani 1 1 d . . . F3 F 0.69587(11) -0.1069(3) 0.44687(6) 0.0488(6) Uani 1 1 d . . . F4 F 0.69541(10) 0.0876(3) 0.38972(6) 0.0426(6) Uani 1 1 d . . . F5 F 0.57775(10) 0.2100(2) 0.36128(6) 0.0351(5) Uani 1 1 d . . . F6 F 0.43176(10) 0.3088(2) 0.22484(5) 0.0319(5) Uani 1 1 d . . . F7 F 0.41125(11) 0.2910(2) 0.15257(5) 0.0355(5) Uani 1 1 d . . . F8 F 0.28490(11) 0.2205(2) 0.12077(6) 0.0389(5) Uani 1 1 d . . . F9 F 0.17864(10) 0.1622(3) 0.16211(6) 0.0385(5) Uani 1 1 d . . . F10 F 0.19836(10) 0.1748(2) 0.23439(6) 0.0354(5) Uani 1 1 d . . . F11 F 0.30650(10) 0.8382(2) 0.24906(6) 0.0377(5) Uani 1 1 d . . . F12 F 0.31963(11) 0.8816(3) 0.17816(6) 0.0450(6) Uani 1 1 d . . . F13 F 0.21186(13) 0.8196(3) 0.12896(6) 0.0495(7) Uani 1 1 d . . . F14 F 0.09356(12) 0.6966(3) 0.15129(6) 0.0430(6) Uani 1 1 d . . . F15 F 0.08018(10) 0.6537(2) 0.22176(5) 0.0345(5) Uani 1 1 d . . . F16 F -0.06708(10) 0.8625(2) 0.36349(6) 0.0369(5) Uani 1 1 d . . . F17 F -0.15313(11) 1.0041(3) 0.40577(6) 0.0431(6) Uani 1 1 d . . . F18 F -0.10288(12) 1.1443(3) 0.46772(6) 0.0469(6) Uani 1 1 d . . . F19 F 0.03504(11) 1.1430(3) 0.48677(6) 0.0424(6) Uani 1 1 d . . . F20 F 0.12110(10) 0.9905(2) 0.44601(6) 0.0365(5) Uani 1 1 d . . . F21 F 0.24429(11) 0.2421(2) 0.49269(6) 0.0372(5) Uani 1 1 d . . . F22 F 0.15191(12) 0.3070(3) 0.54048(6) 0.0417(6) Uani 1 1 d . . . F23 F 0.05830(11) 0.5326(3) 0.52749(6) 0.0396(6) Uani 1 1 d . . . F24 F 0.05390(10) 0.6987(2) 0.46519(5) 0.0333(5) Uani 1 1 d . . . N1 N 0.33920(14) 0.2913(3) 0.39358(7) 0.0230(6) Uani 1 1 d . . . N2 N 0.36893(14) 0.1908(3) 0.33256(8) 0.0241(7) Uani 1 1 d . . . N3 N 0.25440(14) 0.4933(3) 0.26809(8) 0.0247(7) Uani 1 1 d . . . N4 N 0.13089(14) 0.7842(3) 0.33035(8) 0.0233(6) Uani 1 1 d . . . N5 N 0.15806(14) 0.6203(3) 0.41382(8) 0.0248(7) Uani 1 1 d . . . P1 P 0.29817(5) 0.23528(10) 0.35386(2) 0.0231(2) Uani 1 1 d . . . S1 S 0.23060(5) 0.07847(10) 0.35987(3) 0.0299(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 0.028(2) 0.0226(17) 0.027(2) 0.0016(14) 0.0052(16) 0.0024(15) C2 0.032(2) 0.0282(19) 0.022(2) -0.0014(15) 0.0041(16) 0.0009(15) C3 0.022(2) 0.0299(19) 0.026(2) 0.0022(15) 0.0010(16) 0.0000(15) C4 0.0180(19) 0.0229(17) 0.030(2) 0.0025(14) 0.0022(15) 0.0033(14) C5 0.0213(19) 0.0225(17) 0.027(2) 0.0018(14) 0.0028(15) 0.0032(14) C6 0.0190(19) 0.0245(18) 0.030(2) 0.0024(15) 0.0048(16) 0.0039(14) C7 0.025(2) 0.0262(18) 0.033(2) 0.0009(15) 0.0053(17) 0.0046(15) C8 0.028(2) 0.0256(18) 0.027(2) -0.0051(15) 0.0063(16) 0.0002(15) C9 0.0205(19) 0.0240(17) 0.027(2) -0.0021(14) 0.0023(15) -0.0011(14) C10 0.0215(19) 0.0267(18) 0.024(2) -0.0007(14) 0.0046(15) 0.0001(14) C11 0.0202(19) 0.0259(18) 0.0251(19) 0.0004(14) 0.0002(15) -0.0007(14) C12 0.022(2) 0.0261(18) 0.0241(19) 0.0013(14) 0.0017(15) 0.0013(14) C13 0.0224(19) 0.0212(17) 0.025(2) -0.0008(14) 0.0048(15) -0.0004(14) C14 0.0205(19) 0.0224(17) 0.0253(19) 0.0008(14) 0.0034(15) 0.0007(14) C15 0.0213(19) 0.0237(17) 0.028(2) -0.0005(14) 0.0021(15) -0.0040(14) C16 0.021(2) 0.0262(18) 0.027(2) 0.0003(15) 0.0018(16) -0.0033(14) C17 0.025(2) 0.0261(18) 0.032(2) 0.0024(15) -0.0011(16) 0.0052(15) C18 0.023(2) 0.0261(18) 0.034(2) 0.0002(15) 0.0027(17) 0.0035(15) C19 0.0203(19) 0.0253(18) 0.029(2) 0.0001(15) 0.0064(16) 0.0051(14) C20 0.0184(19) 0.0256(18) 0.030(2) -0.0027(15) 0.0039(15) -0.0001(14) C21 0.023(2) 0.0215(17) 0.030(2) -0.0025(14) 0.0021(16) -0.0031(14) C22 0.023(2) 0.0228(18) 0.027(2) -0.0001(14) 0.0025(15) -0.0011(14) C23 0.0197(19) 0.0239(17) 0.0249(19) 0.0006(14) 0.0019(15) -0.0013(14) C24 0.022(2) 0.0232(17) 0.030(2) -0.0005(14) 0.0048(16) 0.0030(14) C25 0.024(2) 0.0243(18) 0.027(2) -0.0024(14) 0.0066(16) 0.0020(14) C26 0.024(2) 0.0203(17) 0.028(2) -0.0030(14) 0.0015(16) 0.0014(14) C27 0.028(2) 0.0257(18) 0.031(2) -0.0014(15) 0.0066(17) 0.0023(15) C28 0.040(2) 0.031(2) 0.026(2) 0.0035(16) 0.0006(18) 0.0074(17) C29 0.032(2) 0.041(2) 0.030(2) -0.0019(17) -0.0063(18) 0.0145(18) C30 0.025(2) 0.036(2) 0.037(2) -0.0049(17) 0.0022(18) 0.0019(16) C31 0.028(2) 0.0261(18) 0.030(2) 0.0030(15) 0.0029(17) 0.0007(15) C32 0.023(2) 0.0214(17) 0.029(2) 0.0012(14) 0.0055(16) 0.0031(14) C33 0.025(2) 0.0223(17) 0.031(2) 0.0002(15) 0.0017(16) 0.0024(14) C34 0.031(2) 0.0266(18) 0.029(2) 0.0033(15) 0.0117(17) 0.0001(15) C35 0.035(2) 0.0277(19) 0.023(2) -0.0016(15) -0.0009(17) 0.0016(16) C36 0.021(2) 0.0273(19) 0.034(2) 0.0003(15) -0.0017(17) 0.0015(15) C37 0.024(2) 0.0253(18) 0.034(2) -0.0007(15) 0.0083(17) 0.0020(15) C38 0.026(2) 0.0210(17) 0.027(2) 0.0026(14) 0.0019(16) 0.0036(14) C39 0.024(2) 0.0233(18) 0.033(2) -0.0005(15) 0.0017(17) -0.0007(14) C40 0.034(2) 0.0242(19) 0.043(2) 0.0058(16) 0.0178(19) 0.0050(16) C41 0.046(3) 0.034(2) 0.025(2) 0.0043(16) 0.0118(19) 0.0109(18) C42 0.033(2) 0.0298(19) 0.025(2) -0.0020(15) -0.0022(17) 0.0078(16) C43 0.027(2) 0.0264(18) 0.028(2) 0.0018(15) 0.0069(16) 0.0051(15) C44 0.025(2) 0.0204(17) 0.030(2) 0.0017(14) 0.0027(16) 0.0012(14) C45 0.027(2) 0.0281(19) 0.034(2) -0.0037(16) 0.0020(17) 0.0009(15) C46 0.022(2) 0.036(2) 0.041(2) 0.0025(17) 0.0041(18) 0.0061(16) C47 0.031(2) 0.033(2) 0.038(2) -0.0027(17) 0.0125(18) 0.0097(16) C48 0.042(3) 0.029(2) 0.030(2) -0.0057(16) 0.0034(18) 0.0039(17) C49 0.023(2) 0.033(2) 0.034(2) -0.0010(16) 0.0039(17) 0.0035(15) C50 0.028(2) 0.0249(18) 0.024(2) -0.0020(14) 0.0020(16) -0.0007(15) C51 0.028(2) 0.0301(19) 0.029(2) 0.0016(16) 0.0015(17) 0.0032(16) C52 0.035(2) 0.038(2) 0.024(2) 0.0054(16) 0.0069(17) 0.0003(17) C53 0.029(2) 0.039(2) 0.029(2) -0.0019(17) 0.0114(17) -0.0006(17) C54 0.026(2) 0.0306(19) 0.031(2) -0.0025(16) 0.0032(17) 0.0055(15) C55 0.025(2) 0.0275(18) 0.027(2) -0.0017(15) 0.0053(16) -0.0004(15) C56 0.039(2) 0.027(2) 0.040(2) 0.0001(17) 0.0065(19) -0.0104(17) C57 0.038(2) 0.032(2) 0.045(3) 0.0060(18) -0.005(2) -0.0074(18) C58 0.034(2) 0.033(2) 0.061(3) -0.002(2) -0.002(2) -0.0068(18) C59 0.042(3) 0.033(2) 0.065(3) -0.008(2) 0.011(2) -0.0103(19) C60 0.056(3) 0.036(2) 0.042(3) -0.0001(19) 0.004(2) -0.012(2) C61 0.046(3) 0.031(2) 0.045(3) 0.0075(18) 0.000(2) -0.0085(19) C62 0.049(3) 0.034(2) 0.057(3) 0.005(2) 0.009(2) -0.003(2) C63 0.040(3) 0.039(2) 0.044(3) 0.0099(19) 0.007(2) 0.0076(19) C64 0.038(3) 0.052(3) 0.053(3) 0.010(2) 0.011(2) 0.008(2) C65 0.053(3) 0.054(3) 0.042(3) 0.005(2) 0.014(2) 0.012(2) C66 0.057(3) 0.042(2) 0.045(3) 0.002(2) -0.001(2) 0.010(2) C67 0.041(3) 0.044(3) 0.059(3) 0.004(2) 0.000(2) 0.005(2) C68 0.039(3) 0.038(2) 0.049(3) 0.0078(19) 0.008(2) 0.0084(19) C69 0.053(3) 0.054(3) 0.063(3) 0.000(2) -0.001(3) -0.001(2) C70A 0.039(5) 0.037(4) 0.041(5) -0.008(4) 0.009(4) -0.019(4) C71A 0.038(13) 0.029(8) 0.044(9) 0.006(7) -0.010(9) -0.009(8) C72A 0.027(4) 0.031(4) 0.046(5) -0.005(3) 0.003(3) -0.004(3) C73A 0.024(7) 0.030(5) 0.029(6) 0.000(4) 0.003(5) 0.006(4) C74A 0.033(5) 0.025(4) 0.052(5) -0.002(3) -0.008(4) 0.001(3) C75A 0.026(5) 0.033(6) 0.054(7) -0.014(5) 0.009(5) -0.003(4) C76A 0.068(10) 0.054(8) 0.037(6) -0.013(6) 0.012(6) -0.026(6) C70B 0.030(5) 0.039(5) 0.057(6) 0.002(4) -0.003(5) -0.010(4) C71B 0.030(6) 0.036(6) 0.066(8) 0.002(6) -0.002(7) -0.008(5) C72B 0.033(6) 0.036(5) 0.072(7) -0.003(6) 0.008(7) -0.002(4) C73B 0.030(6) 0.036(6) 0.057(6) -0.004(5) 0.003(5) -0.009(4) C74B 0.034(5) 0.044(5) 0.043(6) 0.001(4) 0.001(4) -0.004(4) C75B 0.026(7) 0.039(7) 0.045(8) -0.005(6) 0.007(6) 0.000(6) C76B 0.018(10) 0.054(11) 0.055(8) 0.032(7) -0.021(7) -0.003(8) F1 0.0339(13) 0.0341(12) 0.0371(13) 0.0079(9) 0.0079(10) 0.0014(9) F2 0.0579(16) 0.0478(14) 0.0317(13) 0.0122(11) 0.0025(12) 0.0167(12) F3 0.0365(14) 0.0642(16) 0.0438(15) -0.0004(12) -0.0080(11) 0.0227(12) F4 0.0223(12) 0.0554(15) 0.0505(15) 0.0003(11) 0.0055(11) 0.0007(10) F5 0.0300(12) 0.0364(12) 0.0395(13) 0.0105(10) 0.0066(10) 0.0004(9) F6 0.0241(12) 0.0392(12) 0.0322(12) 0.0005(9) 0.0016(9) -0.0054(9) F7 0.0341(13) 0.0431(13) 0.0306(12) 0.0013(10) 0.0099(10) -0.0049(10) F8 0.0443(14) 0.0454(13) 0.0263(12) -0.0016(10) -0.0016(10) -0.0021(10) F9 0.0249(12) 0.0501(14) 0.0392(14) -0.0038(10) -0.0059(10) -0.0042(10) F10 0.0247(12) 0.0453(13) 0.0370(13) -0.0019(10) 0.0073(10) -0.0031(9) F11 0.0270(12) 0.0395(12) 0.0465(14) 0.0014(10) 0.0028(10) -0.0051(9) F12 0.0422(15) 0.0421(13) 0.0542(16) 0.0075(11) 0.0259(12) 0.0008(11) F13 0.0679(17) 0.0538(15) 0.0290(13) 0.0104(11) 0.0177(12) 0.0168(13) F14 0.0472(15) 0.0525(14) 0.0278(13) -0.0032(10) -0.0073(11) 0.0096(11) F15 0.0272(12) 0.0425(12) 0.0335(13) 0.0005(10) 0.0006(10) -0.0049(10) F16 0.0286(12) 0.0402(12) 0.0413(14) -0.0090(10) -0.0007(10) 0.0019(10) F17 0.0244(13) 0.0526(15) 0.0530(16) -0.0036(11) 0.0076(11) 0.0075(10) F18 0.0417(15) 0.0518(15) 0.0490(15) -0.0092(11) 0.0152(12) 0.0141(11) F19 0.0445(14) 0.0472(14) 0.0356(14) -0.0126(11) 0.0036(11) 0.0060(11) F20 0.0283(13) 0.0435(13) 0.0375(13) -0.0065(10) 0.0010(10) 0.0041(10) F21 0.0390(13) 0.0370(12) 0.0363(13) 0.0105(10) 0.0071(10) 0.0112(10) F22 0.0470(15) 0.0492(14) 0.0305(13) 0.0124(10) 0.0121(11) 0.0053(11) F23 0.0366(13) 0.0486(14) 0.0358(13) 0.0024(10) 0.0173(11) 0.0051(10) F24 0.0303(12) 0.0335(11) 0.0370(13) 0.0007(9) 0.0088(10) 0.0078(9) N1 0.0217(16) 0.0244(15) 0.0230(16) -0.0015(12) 0.0026(13) 0.0033(12) N2 0.0216(16) 0.0235(15) 0.0271(17) -0.0002(12) 0.0016(13) 0.0049(12) N3 0.0217(16) 0.0243(15) 0.0282(17) 0.0004(12) 0.0030(13) 0.0017(12) N4 0.0211(16) 0.0237(15) 0.0254(17) 0.0012(12) 0.0033(13) 0.0044(12) N5 0.0233(16) 0.0240(15) 0.0278(17) -0.0001(12) 0.0060(13) 0.0088(12) P1 0.0221(5) 0.0219(4) 0.0256(5) 0.0003(4) 0.0029(4) 0.0020(4) S1 0.0274(5) 0.0258(5) 0.0367(6) 0.0018(4) 0.0033(4) -0.0024(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 1.378(5) . ? C1 N1 1.417(4) . ? C1 C25 1.453(5) . ? C2 C3 1.399(5) . ? C2 H1 0.9500 . ? C3 C4 1.373(5) . ? C3 H2 0.9500 . ? C4 N1 1.415(4) . ? C4 C5 1.443(5) . ? C5 C6 1.352(5) . ? C5 C26 1.491(4) . ? C6 N2 1.413(4) . ? C6 C7 1.452(5) . ? C7 C8 1.345(5) . ? C7 H3 0.9500 . ? C8 C9 1.444(5) . ? C8 H4 0.9500 . ? C9 C10 1.373(5) . ? C9 N2 1.410(4) . ? C10 C11 1.447(5) . ? C10 C32 1.478(5) . ? C11 N3 1.354(4) . ? C11 C12 1.415(4) . ? C12 C13 1.388(4) . ? C12 P1 1.759(3) . ? C13 C23 1.402(4) . ? C13 C14 1.484(4) . ? C14 N3 1.362(4) . ? C14 C15 1.420(4) . ? C15 C16 1.391(5) . ? C15 C38 1.495(5) . ? C16 N4 1.387(4) . ? C16 C17 1.427(5) . ? C17 C18 1.385(5) . ? C17 H5 0.9500 . ? C18 C19 1.416(5) . ? C18 H6 0.9500 . ? C19 N4 1.363(4) . ? C19 C20 1.455(5) . ? C20 C21 1.395(5) . ? C20 C44 1.471(5) . ? C21 C22 1.409(5) . ? C21 N5 1.421(4) . ? C22 C23 1.350(5) . ? C22 N4 1.357(4) . ? C23 C24 1.471(5) . ? C24 C25 1.374(5) . ? C24 N5 1.415(4) . ? C25 C50 1.463(5) . ? C26 C31 1.386(5) . ? C26 C27 1.394(5) . ? C27 F1 1.344(4) . ? C27 C28 1.373(5) . ? C28 F2 1.345(4) . ? C28 C29 1.375(5) . ? C29 F3 1.339(4) . ? C29 C30 1.370(5) . ? C30 F4 1.341(4) . ? C30 C31 1.383(5) . ? C31 F5 1.348(4) . ? C32 C33 1.383(5) . ? C32 C37 1.389(5) . ? C33 F6 1.349(4) . ? C33 C34 1.388(5) . ? C34 F7 1.347(4) . ? C34 C35 1.372(5) . ? C35 F8 1.342(4) . ? C35 C36 1.371(5) . ? C36 F9 1.341(4) . ? C36 C37 1.379(5) . ? C37 F10 1.345(4) . ? C38 C39 1.382(5) . ? C38 C43 1.388(5) . ? C39 F11 1.349(4) . ? C39 C40 1.377(5) . ? C40 F12 1.351(4) . ? C40 C41 1.382(5) . ? C41 F13 1.340(4) . ? C41 C42 1.365(5) . ? C42 F14 1.341(4) . ? C42 C43 1.379(5) . ? C43 F15 1.347(4) . ? C44 C45 1.380(5) . ? C44 C49 1.387(5) . ? C45 F16 1.351(4) . ? C45 C46 1.371(5) . ? C46 F17 1.345(4) . ? C46 C47 1.366(5) . ? C47 F18 1.344(4) . ? C47 C48 1.380(5) . ? C48 F19 1.347(4) . ? C48 C49 1.368(5) . ? C49 F20 1.351(4) . ? C50 C51 1.403(5) . ? C50 C55 1.415(5) . ? C51 F21 1.339(4) . ? C51 C52 1.372(5) . ? C52 F22 1.351(4) . ? C52 C53 1.388(5) . ? C53 F23 1.344(4) . ? C53 C54 1.374(5) . ? C54 F24 1.349(4) . ? C54 C55 1.373(5) . ? C55 N5 1.380(4) . ? C56 C61 1.392(5) . ? C56 C57 1.396(5) . ? C56 C62 1.497(5) . ? C57 C58 1.373(6) . ? C57 H7 0.9500 . ? C58 C59 1.375(6) . ? C58 H8 0.9500 . ? C59 C60 1.387(6) . ? C59 H9 0.9500 . ? C60 C61 1.384(6) . ? C60 H10 0.9500 . ? C61 H11 0.9500 . ? C62 H12 0.9800 . ? C62 H13 0.9800 . ? C62 H14 0.9800 . ? C63 C68 1.390(6) . ? C63 C64 1.395(6) . ? C63 C69 1.493(6) . ? C64 C65 1.382(6) . ? C64 H15 0.9500 . ? C65 C66 1.381(6) . ? C65 H16 0.9500 . ? C66 C67 1.382(6) . ? C66 H17 0.9500 . ? C67 C68 1.377(6) . ? C67 H18 0.9500 . ? C68 H19 0.9500 . ? C69 H20 0.9800 . ? C69 H21 0.9800 . ? C69 H22 0.9800 . ? C70A C71A 1.37(3) . ? C70A C75A 1.412(13) . ? C70A C76A 1.508(12) . ? C71A C72A 1.37(3) . ? C71A H23 0.9500 . ? C72A C73A 1.323(14) . ? C72A H24 0.9500 . ? C73A C74A 1.459(11) . ? C73A H25 0.9500 . ? C74A C75A 1.364(12) . ? C74A H26 0.9500 . ? C75A H27 0.9500 . ? C76A H28 0.9800 . ? C76A H29 0.9800 . ? C76A H30 0.9800 . ? C70B C71B 1.40(2) . ? C70B C75B 1.40(4) . ? C70B C76B 1.51(2) . ? C71B C72B 1.34(2) . ? C71B H31 0.9500 . ? C72B C73B 1.446(18) . ? C72B H32 0.9500 . ? C73B C74B 1.365(15) . ? C73B H33 0.9500 . ? C74B C75B 1.39(5) . ? C74B H34 0.9500 . ? C75B H35 0.9500 . ? C76B H36 0.9800 . ? C76B H37 0.9800 . ? C76B H38 0.9800 . ? N1 P1 1.693(3) . ? N2 P1 1.687(3) . ? P1 S1 1.9192(13) . ? 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 N1 107.0(3) . . ? C2 C1 C25 125.2(3) . . ? N1 C1 C25 127.6(3) . . ? C1 C2 C3 108.9(3) . . ? C1 C2 H1 125.5 . . ? C3 C2 H1 125.5 . . ? C4 C3 C2 108.7(3) . . ? C4 C3 H2 125.7 . . ? C2 C3 H2 125.7 . . ? C3 C4 N1 107.5(3) . . ? C3 C4 C5 129.8(3) . . ? N1 C4 C5 122.6(3) . . ? C6 C5 C4 121.5(3) . . ? C6 C5 C26 120.1(3) . . ? C4 C5 C26 118.4(3) . . ? C5 C6 N2 119.8(3) . . ? C5 C6 C7 134.4(3) . . ? N2 C6 C7 105.7(3) . . ? C8 C7 C6 109.3(3) . . ? C8 C7 H3 125.4 . . ? C6 C7 H3 125.4 . . ? C7 C8 C9 109.3(3) . . ? C7 C8 H4 125.3 . . ? C9 C8 H4 125.3 . . ? C10 C9 N2 120.7(3) . . ? C10 C9 C8 132.6(3) . . ? N2 C9 C8 106.1(3) . . ? C9 C10 C11 117.6(3) . . ? C9 C10 C32 124.4(3) . . ? C11 C10 C32 117.9(3) . . ? N3 C11 C12 112.7(3) . . ? N3 C11 C10 121.9(3) . . ? C12 C11 C10 125.3(3) . . ? C13 C12 C11 106.2(3) . . ? C13 C12 P1 134.5(3) . . ? C11 C12 P1 118.4(2) . . ? C12 C13 C23 128.7(3) . . ? C12 C13 C14 105.2(3) . . ? C23 C13 C14 126.1(3) . . ? N3 C14 C15 117.4(3) . . ? N3 C14 C13 109.6(3) . . ? C15 C14 C13 133.0(3) . . ? C16 C15 C14 127.2(3) . . ? C16 C15 C38 116.6(3) . . ? C14 C15 C38 116.1(3) . . ? N4 C16 C15 120.4(3) . . ? N4 C16 C17 103.4(3) . . ? C15 C16 C17 135.9(3) . . ? C18 C17 C16 109.3(3) . . ? C18 C17 H5 125.4 . . ? C16 C17 H5 125.4 . . ? C17 C18 C19 108.4(3) . . ? C17 C18 H6 125.8 . . ? C19 C18 H6 125.8 . . ? N4 C19 C18 105.1(3) . . ? N4 C19 C20 107.8(3) . . ? C18 C19 C20 147.1(3) . . ? C21 C20 C19 104.9(3) . . ? C21 C20 C44 131.9(3) . . ? C19 C20 C44 123.1(3) . . ? C20 C21 C22 109.3(3) . . ? C20 C21 N5 148.4(3) . . ? C22 C21 N5 102.2(3) . . ? C23 C22 N4 135.2(3) . . ? C23 C22 C21 117.0(3) . . ? N4 C22 C21 107.5(3) . . ? C22 C23 C13 121.0(3) . . ? C22 C23 C24 102.8(3) . . ? C13 C23 C24 135.2(3) . . ? C25 C24 N5 110.4(3) . . ? C25 C24 C23 142.0(3) . . ? N5 C24 C23 107.6(3) . . ? C24 C25 C1 131.8(3) . . ? C24 C25 C50 104.7(3) . . ? C1 C25 C50 122.6(3) . . ? C31 C26 C27 115.7(3) . . ? C31 C26 C5 121.4(3) . . ? C27 C26 C5 122.9(3) . . ? F1 C27 C28 117.8(3) . . ? F1 C27 C26 119.9(3) . . ? C28 C27 C26 122.2(3) . . ? F2 C28 C27 119.9(4) . . ? F2 C28 C29 119.9(3) . . ? C27 C28 C29 120.2(3) . . ? F3 C29 C30 119.6(4) . . ? F3 C29 C28 120.8(3) . . ? C30 C29 C28 119.6(3) . . ? F4 C30 C29 120.6(3) . . ? F4 C30 C31 119.9(3) . . ? C29 C30 C31 119.5(4) . . ? F5 C31 C30 117.0(3) . . ? F5 C31 C26 120.2(3) . . ? C30 C31 C26 122.8(3) . . ? C33 C32 C37 116.0(3) . . ? C33 C32 C10 124.0(3) . . ? C37 C32 C10 119.8(3) . . ? F6 C33 C32 120.3(3) . . ? F6 C33 C34 117.4(3) . . ? C32 C33 C34 122.3(3) . . ? F7 C34 C35 120.2(3) . . ? F7 C34 C33 120.2(3) . . ? C35 C34 C33 119.6(3) . . ? F8 C35 C36 120.6(3) . . ? F8 C35 C34 119.6(3) . . ? C36 C35 C34 119.9(3) . . ? F9 C36 C35 119.9(3) . . ? F9 C36 C37 120.5(3) . . ? C35 C36 C37 119.6(3) . . ? F10 C37 C36 117.7(3) . . ? F10 C37 C32 119.7(3) . . ? C36 C37 C32 122.6(3) . . ? C39 C38 C43 116.2(3) . . ? C39 C38 C15 121.7(3) . . ? C43 C38 C15 122.1(3) . . ? F11 C39 C40 118.0(3) . . ? F11 C39 C38 119.7(3) . . ? C40 C39 C38 122.3(3) . . ? F12 C40 C39 120.4(4) . . ? F12 C40 C41 119.8(4) . . ? C39 C40 C41 119.7(3) . . ? F13 C41 C42 120.5(4) . . ? F13 C41 C40 119.9(4) . . ? C42 C41 C40 119.6(3) . . ? F14 C42 C41 120.6(3) . . ? F14 C42 C43 119.7(3) . . ? C41 C42 C43 119.7(3) . . ? F15 C43 C42 118.1(3) . . ? F15 C43 C38 119.4(3) . . ? C42 C43 C38 122.5(3) . . ? C45 C44 C49 115.9(3) . . ? C45 C44 C20 122.5(3) . . ? C49 C44 C20 121.6(3) . . ? F16 C45 C46 117.6(3) . . ? F16 C45 C44 119.6(3) . . ? C46 C45 C44 122.8(3) . . ? F17 C46 C47 119.7(3) . . ? F17 C46 C45 120.8(3) . . ? C47 C46 C45 119.5(4) . . ? F18 C47 C46 120.6(4) . . ? F18 C47 C48 119.6(3) . . ? C46 C47 C48 119.8(3) . . ? F19 C48 C49 120.5(3) . . ? F19 C48 C47 120.1(3) . . ? C49 C48 C47 119.4(4) . . ? F20 C49 C48 118.4(3) . . ? F20 C49 C44 119.1(3) . . ? C48 C49 C44 122.5(4) . . ? C51 C50 C55 117.1(3) . . ? C51 C50 C25 133.5(3) . . ? C55 C50 C25 108.9(3) . . ? F21 C51 C52 118.1(3) . . ? F21 C51 C50 121.4(3) . . ? C52 C51 C50 120.4(3) . . ? F22 C52 C51 120.4(3) . . ? F22 C52 C53 118.9(3) . . ? C51 C52 C53 120.7(3) . . ? F23 C53 C54 120.4(3) . . ? F23 C53 C52 119.1(3) . . ? C54 C53 C52 120.6(3) . . ? F24 C54 C55 121.2(3) . . ? F24 C54 C53 119.8(3) . . ? C55 C54 C53 119.0(3) . . ? C54 C55 N5 130.6(3) . . ? C54 C55 C50 122.2(3) . . ? N5 C55 C50 106.9(3) . . ? C61 C56 C57 117.6(4) . . ? C61 C56 C62 121.6(4) . . ? C57 C56 C62 120.8(4) . . ? C58 C57 C56 121.8(4) . . ? C58 C57 H7 119.1 . . ? C56 C57 H7 119.1 . . ? C57 C58 C59 119.7(4) . . ? C57 C58 H8 120.1 . . ? C59 C58 H8 120.1 . . ? C58 C59 C60 120.1(4) . . ? C58 C59 H9 120.0 . . ? C60 C59 H9 120.0 . . ? C61 C60 C59 119.8(4) . . ? C61 C60 H10 120.1 . . ? C59 C60 H10 120.1 . . ? C60 C61 C56 121.0(4) . . ? C60 C61 H11 119.5 . . ? C56 C61 H11 119.5 . . ? C56 C62 H12 109.5 . . ? C56 C62 H13 109.5 . . ? H12 C62 H13 109.5 . . ? C56 C62 H14 109.5 . . ? H12 C62 H14 109.5 . . ? H13 C62 H14 109.5 . . ? C68 C63 C64 117.0(4) . . ? C68 C63 C69 121.7(4) . . ? C64 C63 C69 121.3(4) . . ? C65 C64 C63 121.3(4) . . ? C65 C64 H15 119.4 . . ? C63 C64 H15 119.4 . . ? C66 C65 C64 120.8(4) . . ? C66 C65 H16 119.6 . . ? C64 C65 H16 119.6 . . ? C65 C66 C67 118.5(4) . . ? C65 C66 H17 120.8 . . ? C67 C66 H17 120.8 . . ? C68 C67 C66 120.7(4) . . ? C68 C67 H18 119.6 . . ? C66 C67 H18 119.6 . . ? C67 C68 C63 121.7(4) . . ? C67 C68 H19 119.2 . . ? C63 C68 H19 119.2 . . ? C63 C69 H20 109.5 . . ? C63 C69 H21 109.5 . . ? H20 C69 H21 109.5 . . ? C63 C69 H22 109.5 . . ? H20 C69 H22 109.5 . . ? H21 C69 H22 109.5 . . ? C71A C70A C75A 118.0(14) . . ? C71A C70A C76A 121.6(14) . . ? C75A C70A C76A 120.4(9) . . ? C70A C71A C72A 122(2) . . ? C70A C71A H23 119.2 . . ? C72A C71A H23 119.2 . . ? C73A C72A C71A 121.4(13) . . ? C73A C72A H24 119.3 . . ? C71A C72A H24 119.3 . . ? C72A C73A C74A 119.8(11) . . ? C72A C73A H25 120.1 . . ? C74A C73A H25 120.1 . . ? C75A C74A C73A 117.8(9) . . ? C75A C74A H26 121.1 . . ? C73A C74A H26 121.1 . . ? C74A C75A C70A 121.4(10) . . ? C74A C75A H27 119.3 . . ? C70A C75A H27 119.3 . . ? C70A C76A H28 109.5 . . ? C70A C76A H29 109.5 . . ? H28 C76A H29 109.5 . . ? C70A C76A H30 109.5 . . ? H28 C76A H30 109.5 . . ? H29 C76A H30 109.5 . . ? C71B C70B C75B 117(2) . . ? C71B C70B C76B 118.7(13) . . ? C75B C70B C76B 124(2) . . ? C72B C71B C70B 122.5(17) . . ? C72B C71B H31 118.7 . . ? C70B C71B H31 118.7 . . ? C71B C72B C73B 120.5(16) . . ? C71B C72B H32 119.7 . . ? C73B C72B H32 119.7 . . ? C74B C73B C72B 116.9(13) . . ? C74B C73B H33 121.5 . . ? C72B C73B H33 121.5 . . ? C73B C74B C75B 122(2) . . ? C73B C74B H34 118.9 . . ? C75B C74B H34 118.9 . . ? C74B C75B C70B 121(4) . . ? C74B C75B H35 119.6 . . ? C70B C75B H35 119.6 . . ? C70B C76B H36 109.5 . . ? C70B C76B H37 109.5 . . ? H36 C76B H37 109.5 . . ? C70B C76B H38 109.5 . . ? H36 C76B H38 109.5 . . ? H37 C76B H38 109.5 . . ? C4 N1 C1 107.7(3) . . ? C4 N1 P1 122.3(2) . . ? C1 N1 P1 126.6(2) . . ? C9 N2 C6 109.3(3) . . ? C9 N2 P1 122.6(2) . . ? C6 N2 P1 124.8(2) . . ? C11 N3 C14 106.3(3) . . ? C22 N4 C19 110.5(3) . . ? C22 N4 C16 135.5(3) . . ? C19 N4 C16 113.8(3) . . ? C55 N5 C24 108.7(3) . . ? C55 N5 C21 141.0(3) . . ? C24 N5 C21 110.1(3) . . ? N2 P1 N1 97.44(14) . . ? N2 P1 C12 94.78(15) . . ? N1 P1 C12 113.22(15) . . ? N2 P1 S1 118.98(11) . . ? N1 P1 S1 112.49(11) . . ? C12 P1 S1 117.30(12) . . ? 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 N1 C1 C2 C3 -2.4(4) . . . . ? C25 C1 C2 C3 -178.4(3) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C2 C3 C4 N1 1.8(4) . . . . ? C2 C3 C4 C5 -175.5(3) . . . . ? C3 C4 C5 C6 -178.6(4) . . . . ? N1 C4 C5 C6 4.4(5) . . . . ? C3 C4 C5 C26 -1.0(5) . . . . ? N1 C4 C5 C26 -177.9(3) . . . . ? C4 C5 C6 N2 2.7(5) . . . . ? C26 C5 C6 N2 -174.9(3) . . . . ? C4 C5 C6 C7 178.1(4) . . . . ? C26 C5 C6 C7 0.5(6) . . . . ? C5 C6 C7 C8 -173.2(4) . . . . ? N2 C6 C7 C8 2.6(4) . . . . ? C6 C7 C8 C9 1.1(4) . . . . ? C7 C8 C9 C10 166.8(4) . . . . ? C7 C8 C9 N2 -4.3(4) . . . . ? N2 C9 C10 C11 5.7(5) . . . . ? C8 C9 C10 C11 -164.4(3) . . . . ? N2 C9 C10 C32 -177.7(3) . . . . ? C8 C9 C10 C32 12.2(6) . . . . ? C9 C10 C11 N3 160.9(3) . . . . ? C32 C10 C11 N3 -16.0(5) . . . . ? C9 C10 C11 C12 -16.0(5) . . . . ? C32 C10 C11 C12 167.1(3) . . . . ? N3 C11 C12 C13 0.9(4) . . . . ? C10 C11 C12 C13 178.1(3) . . . . ? N3 C11 C12 P1 171.6(2) . . . . ? C10 C11 C12 P1 -11.2(5) . . . . ? C11 C12 C13 C23 176.8(3) . . . . ? P1 C12 C13 C23 8.3(6) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? P1 C12 C13 C14 -169.1(3) . . . . ? C12 C13 C14 N3 0.2(4) . . . . ? C23 C13 C14 N3 -177.3(3) . . . . ? C12 C13 C14 C15 177.7(4) . . . . ? C23 C13 C14 C15 0.2(6) . . . . ? N3 C14 C15 C16 167.7(3) . . . . ? C13 C14 C15 C16 -9.7(6) . . . . ? N3 C14 C15 C38 -7.2(5) . . . . ? C13 C14 C15 C38 175.4(3) . . . . ? C14 C15 C16 N4 2.7(5) . . . . ? C38 C15 C16 N4 177.6(3) . . . . ? C14 C15 C16 C17 -169.8(4) . . . . ? C38 C15 C16 C17 5.1(6) . . . . ? N4 C16 C17 C18 -0.9(4) . . . . ? C15 C16 C17 C18 172.5(4) . . . . ? C16 C17 C18 C19 1.2(4) . . . . ? C17 C18 C19 N4 -1.1(4) . . . . ? C17 C18 C19 C20 176.4(5) . . . . ? N4 C19 C20 C21 0.1(4) . . . . ? C18 C19 C20 C21 -177.3(5) . . . . ? N4 C19 C20 C44 179.0(3) . . . . ? C18 C19 C20 C44 1.6(8) . . . . ? C19 C20 C21 C22 1.5(4) . . . . ? C44 C20 C21 C22 -177.3(3) . . . . ? C19 C20 C21 N5 -173.1(5) . . . . ? C44 C20 C21 N5 8.1(9) . . . . ? C20 C21 C22 C23 -176.5(3) . . . . ? N5 C21 C22 C23 0.5(4) . . . . ? C20 C21 C22 N4 -2.5(4) . . . . ? N5 C21 C22 N4 174.6(3) . . . . ? N4 C22 C23 C13 -4.9(6) . . . . ? C21 C22 C23 C13 167.0(3) . . . . ? N4 C22 C23 C24 -175.3(4) . . . . ? C21 C22 C23 C24 -3.4(4) . . . . ? C12 C13 C23 C22 -167.3(3) . . . . ? C14 C13 C23 C22 9.6(5) . . . . ? C12 C13 C23 C24 -0.7(7) . . . . ? C14 C13 C23 C24 176.2(4) . . . . ? C22 C23 C24 C25 -177.5(5) . . . . ? C13 C23 C24 C25 14.2(8) . . . . ? C22 C23 C24 N5 4.8(4) . . . . ? C13 C23 C24 N5 -163.5(4) . . . . ? N5 C24 C25 C1 -162.0(3) . . . . ? C23 C24 C25 C1 20.3(8) . . . . ? N5 C24 C25 C50 6.9(4) . . . . ? C23 C24 C25 C50 -170.8(4) . . . . ? C2 C1 C25 C24 137.4(4) . . . . ? N1 C1 C25 C24 -37.9(6) . . . . ? C2 C1 C25 C50 -29.9(5) . . . . ? N1 C1 C25 C50 154.9(3) . . . . ? C6 C5 C26 C31 57.7(5) . . . . ? C4 C5 C26 C31 -120.0(4) . . . . ? C6 C5 C26 C27 -123.0(4) . . . . ? C4 C5 C26 C27 59.3(5) . . . . ? C31 C26 C27 F1 179.6(3) . . . . ? C5 C26 C27 F1 0.3(5) . . . . ? C31 C26 C27 C28 -1.2(5) . . . . ? C5 C26 C27 C28 179.5(3) . . . . ? F1 C27 C28 F2 -1.1(5) . . . . ? C26 C27 C28 F2 179.6(3) . . . . ? F1 C27 C28 C29 179.5(3) . . . . ? C26 C27 C28 C29 0.2(6) . . . . ? F2 C28 C29 F3 0.7(6) . . . . ? C27 C28 C29 F3 -179.9(3) . . . . ? F2 C28 C29 C30 -179.5(3) . . . . ? C27 C28 C29 C30 -0.1(6) . . . . ? F3 C29 C30 F4 1.2(6) . . . . ? C28 C29 C30 F4 -178.7(3) . . . . ? F3 C29 C30 C31 -179.2(3) . . . . ? C28 C29 C30 C31 1.0(6) . . . . ? F4 C30 C31 F5 -1.1(5) . . . . ? C29 C30 C31 F5 179.2(3) . . . . ? F4 C30 C31 C26 177.5(3) . . . . ? C29 C30 C31 C26 -2.1(6) . . . . ? C27 C26 C31 F5 -179.3(3) . . . . ? C5 C26 C31 F5 0.1(5) . . . . ? C27 C26 C31 C30 2.2(5) . . . . ? C5 C26 C31 C30 -178.5(3) . . . . ? C9 C10 C32 C33 -63.2(5) . . . . ? C11 C10 C32 C33 113.4(4) . . . . ? C9 C10 C32 C37 122.1(4) . . . . ? C11 C10 C32 C37 -61.2(4) . . . . ? C37 C32 C33 F6 177.9(3) . . . . ? C10 C32 C33 F6 3.1(5) . . . . ? C37 C32 C33 C34 -0.4(5) . . . . ? C10 C32 C33 C34 -175.3(3) . . . . ? F6 C33 C34 F7 2.1(5) . . . . ? C32 C33 C34 F7 -179.5(3) . . . . ? F6 C33 C34 C35 -177.8(3) . . . . ? C32 C33 C34 C35 0.6(5) . . . . ? F7 C34 C35 F8 1.0(5) . . . . ? C33 C34 C35 F8 -179.1(3) . . . . ? F7 C34 C35 C36 179.7(3) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? F8 C35 C36 F9 0.3(5) . . . . ? C34 C35 C36 F9 -178.4(3) . . . . ? F8 C35 C36 C37 178.6(3) . . . . ? C34 C35 C36 C37 0.0(5) . . . . ? F9 C36 C37 F10 -1.1(5) . . . . ? C35 C36 C37 F10 -179.4(3) . . . . ? F9 C36 C37 C32 178.6(3) . . . . ? C35 C36 C37 C32 0.2(5) . . . . ? C33 C32 C37 F10 179.6(3) . . . . ? C10 C32 C37 F10 -5.3(5) . . . . ? C33 C32 C37 C36 0.0(5) . . . . ? C10 C32 C37 C36 175.1(3) . . . . ? C16 C15 C38 C39 112.5(4) . . . . ? C14 C15 C38 C39 -72.1(4) . . . . ? C16 C15 C38 C43 -70.9(4) . . . . ? C14 C15 C38 C43 104.6(4) . . . . ? C43 C38 C39 F11 -179.5(3) . . . . ? C15 C38 C39 F11 -2.6(5) . . . . ? C43 C38 C39 C40 -0.2(5) . . . . ? C15 C38 C39 C40 176.6(3) . . . . ? F11 C39 C40 F12 -0.7(5) . . . . ? C38 C39 C40 F12 -179.9(3) . . . . ? F11 C39 C40 C41 -179.7(3) . . . . ? C38 C39 C40 C41 1.1(5) . . . . ? F12 C40 C41 F13 -1.7(5) . . . . ? C39 C40 C41 F13 177.3(3) . . . . ? F12 C40 C41 C42 179.2(3) . . . . ? C39 C40 C41 C42 -1.8(5) . . . . ? F13 C41 C42 F14 3.0(5) . . . . ? C40 C41 C42 F14 -177.8(3) . . . . ? F13 C41 C42 C43 -177.5(3) . . . . ? C40 C41 C42 C43 1.7(5) . . . . ? F14 C42 C43 F15 0.2(5) . . . . ? C41 C42 C43 F15 -179.3(3) . . . . ? F14 C42 C43 C38 178.7(3) . . . . ? C41 C42 C43 C38 -0.9(5) . . . . ? C39 C38 C43 F15 178.6(3) . . . . ? C15 C38 C43 F15 1.8(5) . . . . ? C39 C38 C43 C42 0.1(5) . . . . ? C15 C38 C43 C42 -176.7(3) . . . . ? C21 C20 C44 C45 -127.9(4) . . . . ? C19 C20 C44 C45 53.5(5) . . . . ? C21 C20 C44 C49 53.9(5) . . . . ? C19 C20 C44 C49 -124.7(4) . . . . ? C49 C44 C45 F16 178.3(3) . . . . ? C20 C44 C45 F16 0.0(5) . . . . ? C49 C44 C45 C46 -1.5(5) . . . . ? C20 C44 C45 C46 -179.8(3) . . . . ? F16 C45 C46 F17 1.8(5) . . . . ? C44 C45 C46 F17 -178.4(3) . . . . ? F16 C45 C46 C47 -178.4(3) . . . . ? C44 C45 C46 C47 1.5(6) . . . . ? F17 C46 C47 F18 0.8(6) . . . . ? C45 C46 C47 F18 -179.0(3) . . . . ? F17 C46 C47 C48 -179.9(3) . . . . ? C45 C46 C47 C48 0.3(6) . . . . ? F18 C47 C48 F19 -1.3(6) . . . . ? C46 C47 C48 F19 179.4(3) . . . . ? F18 C47 C48 C49 177.5(3) . . . . ? C46 C47 C48 C49 -1.9(6) . . . . ? F19 C48 C49 F20 0.3(5) . . . . ? C47 C48 C49 F20 -178.4(3) . . . . ? F19 C48 C49 C44 -179.4(3) . . . . ? C47 C48 C49 C44 1.8(6) . . . . ? C45 C44 C49 F20 -179.9(3) . . . . ? C20 C44 C49 F20 -1.6(5) . . . . ? C45 C44 C49 C48 -0.2(5) . . . . ? C20 C44 C49 C48 178.1(3) . . . . ? C24 C25 C50 C51 166.5(4) . . . . ? C1 C25 C50 C51 -23.3(6) . . . . ? C24 C25 C50 C55 -5.0(4) . . . . ? C1 C25 C50 C55 165.2(3) . . . . ? C55 C50 C51 F21 174.8(3) . . . . ? C25 C50 C51 F21 3.9(6) . . . . ? C55 C50 C51 C52 -3.0(5) . . . . ? C25 C50 C51 C52 -174.0(4) . . . . ? F21 C51 C52 F22 2.4(5) . . . . ? C50 C51 C52 F22 -179.7(3) . . . . ? F21 C51 C52 C53 -176.2(3) . . . . ? C50 C51 C52 C53 1.7(6) . . . . ? F22 C52 C53 F23 0.3(5) . . . . ? C51 C52 C53 F23 179.0(3) . . . . ? F22 C52 C53 C54 -178.5(3) . . . . ? C51 C52 C53 C54 0.2(6) . . . . ? F23 C53 C54 F24 -3.1(5) . . . . ? C52 C53 C54 F24 175.7(3) . . . . ? F23 C53 C54 C55 -179.4(3) . . . . ? C52 C53 C54 C55 -0.6(6) . . . . ? F24 C54 C55 N5 -4.0(6) . . . . ? C53 C54 C55 N5 172.2(4) . . . . ? F24 C54 C55 C50 -177.1(3) . . . . ? C53 C54 C55 C50 -0.9(6) . . . . ? C51 C50 C55 C54 2.7(5) . . . . ? C25 C50 C55 C54 175.8(3) . . . . ? C51 C50 C55 N5 -171.9(3) . . . . ? C25 C50 C55 N5 1.2(4) . . . . ? C61 C56 C57 C58 0.0(6) . . . . ? C62 C56 C57 C58 -179.9(4) . . . . ? C56 C57 C58 C59 0.1(6) . . . . ? C57 C58 C59 C60 -0.1(6) . . . . ? C58 C59 C60 C61 0.0(6) . . . . ? C59 C60 C61 C56 0.0(6) . . . . ? C57 C56 C61 C60 0.0(5) . . . . ? C62 C56 C61 C60 179.8(4) . . . . ? C68 C63 C64 C65 1.4(6) . . . . ? C69 C63 C64 C65 -178.0(4) . . . . ? C63 C64 C65 C66 -0.6(7) . . . . ? C64 C65 C66 C67 -0.5(7) . . . . ? C65 C66 C67 C68 0.7(6) . . . . ? C66 C67 C68 C63 0.2(6) . . . . ? C64 C63 C68 C67 -1.2(6) . . . . ? C69 C63 C68 C67 178.3(4) . . . . ? C75A C70A C71A C72A 0(3) . . . . ? C76A C70A C71A C72A 178.5(16) . . . . ? C70A C71A C72A C73A 1(3) . . . . ? C71A C72A C73A C74A 0(2) . . . . ? C72A C73A C74A C75A -0.7(16) . . . . ? C73A C74A C75A C70A 0.8(15) . . . . ? C71A C70A C75A C74A 0(2) . . . . ? C76A C70A C75A C74A -179.2(9) . . . . ? C75B C70B C71B C72B -1(3) . . . . ? C76B C70B C71B C72B 178.6(17) . . . . ? C70B C71B C72B C73B 2(3) . . . . ? C71B C72B C73B C74B 0(2) . . . . ? C72B C73B C74B C75B -2(3) . . . . ? C73B C74B C75B C70B 3(5) . . . . ? C71B C70B C75B C74B -1(5) . . . . ? C76B C70B C75B C74B 179(2) . . . . ? C3 C4 N1 C1 -3.2(4) . . . . ? C5 C4 N1 C1 174.3(3) . . . . ? C3 C4 N1 P1 -163.7(2) . . . . ? C5 C4 N1 P1 13.8(4) . . . . ? C2 C1 N1 C4 3.4(4) . . . . ? C25 C1 N1 C4 179.4(3) . . . . ? C2 C1 N1 P1 162.8(2) . . . . ? C25 C1 N1 P1 -21.3(5) . . . . ? C10 C9 N2 C6 -166.4(3) . . . . ? C8 C9 N2 C6 6.0(3) . . . . ? C10 C9 N2 P1 33.5(4) . . . . ? C8 C9 N2 P1 -154.1(2) . . . . ? C5 C6 N2 C9 171.2(3) . . . . ? C7 C6 N2 C9 -5.4(4) . . . . ? C5 C6 N2 P1 -29.2(4) . . . . ? C7 C6 N2 P1 154.2(2) . . . . ? C12 C11 N3 C14 -0.8(4) . . . . ? C10 C11 N3 C14 -178.1(3) . . . . ? C15 C14 N3 C11 -177.6(3) . . . . ? C13 C14 N3 C11 0.4(4) . . . . ? C23 C22 N4 C19 175.0(4) . . . . ? C21 C22 N4 C19 2.6(4) . . . . ? C23 C22 N4 C16 -9.7(7) . . . . ? C21 C22 N4 C16 177.8(3) . . . . ? C18 C19 N4 C22 176.9(3) . . . . ? C20 C19 N4 C22 -1.7(4) . . . . ? C18 C19 N4 C16 0.5(4) . . . . ? C20 C19 N4 C16 -178.0(3) . . . . ? C15 C16 N4 C22 10.4(6) . . . . ? C17 C16 N4 C22 -174.9(4) . . . . ? C15 C16 N4 C19 -174.5(3) . . . . ? C17 C16 N4 C19 0.2(4) . . . . ? C54 C55 N5 C24 -170.9(4) . . . . ? C50 C55 N5 C24 3.0(4) . . . . ? C54 C55 N5 C21 4.4(7) . . . . ? C50 C55 N5 C21 178.3(4) . . . . ? C25 C24 N5 C55 -6.5(4) . . . . ? C23 C24 N5 C55 172.0(3) . . . . ? C25 C24 N5 C21 176.7(3) . . . . ? C23 C24 N5 C21 -4.8(4) . . . . ? C20 C21 N5 C55 2.3(9) . . . . ? C22 C21 N5 C55 -172.5(4) . . . . ? C20 C21 N5 C24 177.5(5) . . . . ? C22 C21 N5 C24 2.7(4) . . . . ? C9 N2 P1 N1 -164.2(3) . . . . ? C6 N2 P1 N1 38.8(3) . . . . ? C9 N2 P1 C12 -50.0(3) . . . . ? C6 N2 P1 C12 153.0(3) . . . . ? C9 N2 P1 S1 74.9(3) . . . . ? C6 N2 P1 S1 -82.0(3) . . . . ? C4 N1 P1 N2 -30.1(3) . . . . ? C1 N1 P1 N2 173.3(3) . . . . ? C4 N1 P1 C12 -128.6(3) . . . . ? C1 N1 P1 C12 74.9(3) . . . . ? C4 N1 P1 S1 95.6(3) . . . . ? C1 N1 P1 S1 -61.0(3) . . . . ? C13 C12 P1 N2 -155.3(4) . . . . ? C11 C12 P1 N2 37.3(3) . . . . ? C13 C12 P1 N1 -55.1(4) . . . . ? C11 C12 P1 N1 137.5(3) . . . . ? C13 C12 P1 S1 78.5(4) . . . . ? C11 C12 P1 S1 -88.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.396 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.076 data_0901hi _database_code_depnum_ccdc_archive 'CCDC 842955' #TrackingRef 'chlorinPO-ChemSci.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H8 F24 N5 O P, C2 H3 N, 0.75(C Cl4), 0.5(O) ' _chemical_formula_sum 'C57.75 H11 Cl3 F24 N6 O1.50 P' _chemical_formula_weight 1405.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 10.1849(5) _cell_length_b 14.9773(8) _cell_length_c 17.6759(10) _cell_angle_alpha 85.568(3) _cell_angle_beta 88.271(3) _cell_angle_gamma 76.766(3) _cell_volume 2616.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 11301 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 68.09 _exptl_crystal_description ? _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1387 _exptl_absorpt_coefficient_mu 3.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5714 _exptl_absorpt_correction_T_max 0.8584 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\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 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21103 _diffrn_reflns_av_R_equivalents 0.1076 _diffrn_reflns_av_sigmaI/netI 0.1437 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 59.99 _reflns_number_total 7529 _reflns_number_gt 3480 _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^)+(0.2000P)^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 7529 _refine_ls_number_parameters 857 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1922 _refine_ls_R_factor_gt 0.1190 _refine_ls_wR_factor_ref 0.3747 _refine_ls_wR_factor_gt 0.2902 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _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 0.2691(9) 0.8831(8) 0.2416(6) 0.063(3) Uani 1 1 d . . . C2 C 0.2114(10) 0.9643(8) 0.2762(6) 0.068(3) Uani 1 1 d . . . H2 H 0.2422 1.0197 0.2705 0.082 Uiso 1 1 calc R . . C3 C 0.1011(11) 0.9503(8) 0.3205(7) 0.071(3) Uani 1 1 d . . . H3 H 0.0465 0.9940 0.3512 0.085 Uiso 1 1 calc R . . C4 C 0.0845(10) 0.8651(8) 0.3126(6) 0.058(3) Uani 1 1 d . . . C5 C -0.0280(10) 0.8231(7) 0.3388(6) 0.056(3) Uani 1 1 d . . . C6 C -0.0237(10) 0.7336(8) 0.3279(6) 0.061(3) Uani 1 1 d . . . C7 C -0.1239(11) 0.6744(7) 0.3445(8) 0.081(4) Uani 1 1 d . . . H7 H -0.1896 0.6829 0.3029 0.097 Uiso 1 1 calc R . . H7A H -0.1736 0.6896 0.3926 0.097 Uiso 1 1 calc R . . C8 C -0.0371(9) 0.5743(7) 0.3510(7) 0.066(3) Uani 1 1 d . . . H8 H -0.0263 0.5497 0.4046 0.079 Uiso 1 1 calc R . . H8A H -0.0774 0.5331 0.3225 0.079 Uiso 1 1 calc R . . C9 C 0.0969(10) 0.5853(7) 0.3157(6) 0.059(3) Uani 1 1 d . . . C10 C 0.2129(9) 0.5188(7) 0.3076(6) 0.054(2) Uani 1 1 d . . . C11 C 0.3366(10) 0.5430(7) 0.2827(5) 0.054(2) Uani 1 1 d . . . C12 C 0.3448(9) 0.6337(7) 0.2580(6) 0.057(3) Uani 1 1 d . . . C13 C 0.4788(10) 0.6297(6) 0.2352(6) 0.056(3) Uani 1 1 d . . . C14 C 0.5496(10) 0.5303(7) 0.2494(6) 0.059(3) Uani 1 1 d . . . C15 C 0.6792(10) 0.4791(7) 0.2294(6) 0.061(3) Uani 1 1 d . . . C16 C 0.7814(9) 0.5152(7) 0.1950(6) 0.058(3) Uani 1 1 d . . . C17 C 0.9150(10) 0.4736(7) 0.1664(6) 0.067(3) Uani 1 1 d . . . H17 H 0.9601 0.4108 0.1746 0.080 Uiso 1 1 calc R . . C18 C 0.9657(11) 0.5415(7) 0.1247(7) 0.068(3) Uani 1 1 d . . . H18 H 1.0491 0.5324 0.0975 0.082 Uiso 1 1 calc R . . C19 C 0.8701(10) 0.6275(7) 0.1301(6) 0.063(3) Uani 1 1 d . . . C20 C 0.8322(9) 0.7235(7) 0.1036(6) 0.057(3) Uani 1 1 d . . . C21 C 0.7054(10) 0.7546(8) 0.1332(6) 0.067(3) Uani 1 1 d . . . C22 C 0.6657(12) 0.6815(8) 0.1771(7) 0.073(3) Uani 1 1 d . . . C23 C 0.5401(12) 0.6982(7) 0.2041(6) 0.066(3) Uani 1 1 d . . . C24 C 0.4867(10) 0.7991(8) 0.1791(6) 0.062(3) Uani 1 1 d . . . C25 C 0.3806(9) 0.8732(6) 0.1922(6) 0.057(3) Uani 1 1 d . . . C26 C -0.1481(9) 0.8830(6) 0.3711(5) 0.051(2) Uani 1 1 d . . . C27 C -0.1454(10) 0.9222(7) 0.4373(6) 0.057(3) Uani 1 1 d . . . C28 C -0.2549(11) 0.9842(7) 0.4642(6) 0.060(3) Uani 1 1 d . . . C29 C -0.3727(11) 1.0084(7) 0.4236(6) 0.061(3) Uani 1 1 d . . . C30 C -0.3805(9) 0.9672(8) 0.3598(7) 0.066(3) Uani 1 1 d . . . C31 C -0.2718(9) 0.9071(7) 0.3312(6) 0.057(3) Uani 1 1 d . . . C32 C 0.2143(9) 0.4202(7) 0.3258(6) 0.059(3) Uani 1 1 d . . . C33 C 0.2377(11) 0.3577(9) 0.2690(7) 0.070(3) Uani 1 1 d . . . C34 C 0.2470(12) 0.2641(9) 0.2851(8) 0.080(3) Uani 1 1 d . . . C35 C 0.2256(11) 0.2309(8) 0.3567(8) 0.071(3) Uani 1 1 d . . . C36 C 0.1996(12) 0.2901(9) 0.4139(8) 0.076(3) Uani 1 1 d . . . C37 C 0.1938(12) 0.3830(8) 0.3983(7) 0.074(3) Uani 1 1 d . . . C38 C 0.7070(11) 0.3773(7) 0.2470(6) 0.059(3) Uani 1 1 d . . . C39 C 0.6402(10) 0.3233(7) 0.2124(6) 0.059(3) Uani 1 1 d . . . C40 C 0.6660(12) 0.2297(9) 0.2264(7) 0.074(3) Uani 1 1 d . . . C41 C 0.7628(11) 0.1870(7) 0.2779(7) 0.066(3) Uani 1 1 d . . . C42 C 0.8325(11) 0.2381(8) 0.3140(7) 0.074(3) Uani 1 1 d . . . C43 C 0.8049(11) 0.3313(8) 0.2994(7) 0.067(3) Uani 1 1 d . . . C44 C 0.9187(9) 0.7678(7) 0.0516(6) 0.055(3) Uani 1 1 d . . . C45 C 0.9475(10) 0.7380(7) -0.0205(6) 0.060(3) Uani 1 1 d . . . C46 C 1.0234(11) 0.7819(7) -0.0741(7) 0.063(3) Uani 1 1 d . . . C47 C 1.0781(10) 0.8495(7) -0.0482(6) 0.060(3) Uani 1 1 d . . . C48 C 1.0527(10) 0.8790(7) 0.0240(7) 0.061(3) Uani 1 1 d . . . C49 C 0.9739(10) 0.8360(7) 0.0723(6) 0.059(3) Uani 1 1 d . . . C50 C 0.4178(10) 0.9502(7) 0.1478(6) 0.057(3) Uani 1 1 d . . . C51 C 0.3490(12) 1.0413(8) 0.1267(7) 0.069(3) Uani 1 1 d . . . C52 C 0.4127(11) 1.1010(8) 0.0858(7) 0.069(3) Uani 1 1 d . . . C53 C 0.5438(11) 1.0709(7) 0.0620(6) 0.064(3) Uani 1 1 d . . . C54 C 0.6141(10) 0.9815(8) 0.0753(6) 0.058(3) Uani 1 1 d . . . C55 C 0.5472(10) 0.9213(7) 0.1178(6) 0.057(3) Uani 1 1 d . . . N1 N 0.1883(8) 0.8204(6) 0.2658(5) 0.058(2) Uani 1 1 d . . . N2 N 0.0912(7) 0.6772(5) 0.2952(5) 0.060(2) Uani 1 1 d . . . N3 N 0.4570(8) 0.4819(6) 0.2774(5) 0.058(2) Uani 1 1 d . . . N4 N 0.7642(8) 0.6065(6) 0.1737(5) 0.063(2) Uani 1 1 d . . . N5 N 0.5916(8) 0.8264(5) 0.1354(5) 0.059(2) Uani 1 1 d . . . F1 F -0.0324(5) 0.9011(4) 0.4792(3) 0.0716(17) Uani 1 1 d . . . F2 F -0.2493(6) 1.0238(4) 0.5298(3) 0.0737(17) Uani 1 1 d . . . F3 F -0.4795(6) 1.0717(4) 0.4492(4) 0.0785(19) Uani 1 1 d . . . F4 F -0.4958(6) 0.9929(4) 0.3175(4) 0.086(2) Uani 1 1 d . . . F5 F -0.2819(6) 0.8722(4) 0.2655(3) 0.0742(17) Uani 1 1 d . . . F6 F 0.2543(6) 0.3896(4) 0.1972(4) 0.0759(17) Uani 1 1 d . . . F7 F 0.2710(7) 0.2089(4) 0.2278(4) 0.088(2) Uani 1 1 d . . . F8 F 0.2329(7) 0.1415(5) 0.3714(4) 0.092(2) Uani 1 1 d . . . F9 F 0.1779(9) 0.2582(5) 0.4846(4) 0.107(2) Uani 1 1 d . . . F10 F 0.1675(7) 0.4374(4) 0.4567(4) 0.0855(19) Uani 1 1 d . . . F11 F 0.5490(6) 0.3600(4) 0.1594(3) 0.0731(17) Uani 1 1 d . . . F12 F 0.5985(6) 0.1780(4) 0.1920(4) 0.0828(19) Uani 1 1 d . . . F13 F 0.7928(6) 0.0944(4) 0.2911(4) 0.088(2) Uani 1 1 d . . . F14 F 0.9308(7) 0.1964(5) 0.3647(4) 0.100(2) Uani 1 1 d . . . F15 F 0.8745(6) 0.3796(4) 0.3373(4) 0.0837(19) Uani 1 1 d . . . F16 F 0.8968(5) 0.6716(4) -0.0458(3) 0.0635(15) Uani 1 1 d . . . F17 F 1.0450(6) 0.7566(4) -0.1442(3) 0.0700(16) Uani 1 1 d . . . F18 F 1.1509(6) 0.8939(4) -0.0985(3) 0.0702(16) Uani 1 1 d . . . F19 F 1.1086(5) 0.9449(4) 0.0460(3) 0.0676(16) Uani 1 1 d . . . F20 F 0.9456(5) 0.8687(4) 0.1420(3) 0.0639(15) Uani 1 1 d . . . F21 F 0.2173(5) 1.0716(4) 0.1443(4) 0.0711(17) Uani 1 1 d . . . F22 F 0.3483(6) 1.1869(4) 0.0659(4) 0.0744(17) Uani 1 1 d . . . F23 F 0.6026(6) 1.1309(4) 0.0189(4) 0.0708(16) Uani 1 1 d . . . F24 F 0.7370(5) 0.9515(4) 0.0451(3) 0.0682(16) Uani 1 1 d . . . P1 P 0.1985(3) 0.71529(19) 0.23289(17) 0.0625(8) Uani 1 1 d . . . O1 O 0.1696(7) 0.7201(5) 0.1521(4) 0.0673(19) Uani 1 1 d . . . Cl1 Cl 0.5363(6) 0.5911(4) 0.4300(3) 0.129(3) Uani 0.749(8) 1 d P A 1 Cl2 Cl 0.4662(5) 0.6769(5) 0.5686(3) 0.128(3) Uani 0.749(8) 1 d P A 1 C60 C 0.438(2) 0.6865(10) 0.4626(12) 0.113(8) Uani 0.749(8) 1 d P A 1 Cl3 Cl 0.4418(9) 0.7809(5) 0.4126(5) 0.160(3) Uani 0.749(8) 1 d P A 1 Cl4 Cl 0.2654(6) 0.6682(8) 0.4650(4) 0.214(5) Uani 0.749(8) 1 d P A 1 O2 O 0.248(3) 0.769(2) 0.505(2) 0.089(10) Uiso 0.251(8) 1 d P A 2 O3 O 0.527(3) 0.769(2) 0.447(2) 0.077(10) Uiso 0.251(8) 1 d P A 2 C56 C 0.415(5) 0.627(2) 0.018(3) 0.27(2) Uani 1 1 d DU . . C57 C 0.558(5) 0.594(2) 0.0325(13) 0.378(12) Uani 1 1 d D . . H19 H 0.5734 0.5871 0.0873 0.568 Uiso 1 1 calc R . . H20 H 0.6071 0.6379 0.0085 0.568 Uiso 1 1 calc R . . H21 H 0.5903 0.5340 0.0111 0.568 Uiso 1 1 calc R . . N6 N 0.316(3) 0.605(3) 0.006(2) 0.64(6) Uani 1 1 d 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 0.038(5) 0.067(7) 0.081(8) -0.009(6) 0.000(5) -0.005(5) C2 0.057(7) 0.066(7) 0.075(8) -0.003(6) 0.000(5) 0.001(6) C3 0.071(7) 0.051(7) 0.091(9) -0.019(6) -0.003(6) -0.009(6) C4 0.049(6) 0.067(7) 0.057(6) -0.010(5) -0.002(5) -0.007(5) C5 0.053(6) 0.046(6) 0.067(7) -0.012(5) -0.012(5) -0.004(5) C6 0.059(6) 0.065(7) 0.066(7) -0.010(6) -0.007(5) -0.024(6) C7 0.052(6) 0.058(7) 0.126(11) -0.023(7) 0.004(6) 0.003(6) C8 0.048(6) 0.062(7) 0.086(8) -0.013(6) 0.015(5) -0.008(5) C9 0.062(6) 0.046(6) 0.071(7) -0.014(5) 0.013(5) -0.015(5) C10 0.048(5) 0.048(6) 0.064(7) -0.008(5) 0.003(5) -0.008(5) C11 0.057(6) 0.044(6) 0.056(6) 0.002(5) -0.001(5) -0.005(5) C12 0.032(5) 0.059(7) 0.072(7) 0.005(5) -0.009(4) 0.001(5) C13 0.067(7) 0.034(5) 0.059(6) 0.003(5) -0.011(5) 0.002(5) C14 0.050(6) 0.053(7) 0.070(7) -0.008(5) 0.000(5) -0.006(5) C15 0.047(6) 0.046(6) 0.082(7) -0.004(5) 0.000(5) 0.003(5) C16 0.044(6) 0.060(7) 0.066(7) 0.001(5) -0.006(5) -0.005(5) C17 0.069(7) 0.038(6) 0.083(8) 0.001(5) 0.001(6) 0.007(5) C18 0.073(7) 0.049(7) 0.079(8) 0.002(6) -0.006(6) -0.008(6) C19 0.057(6) 0.058(7) 0.070(7) 0.003(6) -0.011(5) -0.008(5) C20 0.047(6) 0.051(6) 0.071(7) 0.002(5) 0.000(5) -0.010(5) C21 0.049(6) 0.074(8) 0.075(8) -0.021(6) -0.002(5) -0.006(6) C22 0.066(7) 0.060(8) 0.088(9) 0.000(6) 0.006(6) -0.010(6) C23 0.082(8) 0.038(6) 0.082(8) -0.006(5) 0.022(6) -0.023(6) C24 0.050(6) 0.073(8) 0.065(7) -0.008(6) -0.002(5) -0.016(6) C25 0.045(6) 0.038(6) 0.085(8) 0.000(5) -0.011(5) 0.001(4) C26 0.057(6) 0.040(6) 0.057(6) -0.004(5) -0.005(5) -0.015(5) C27 0.056(6) 0.048(6) 0.063(7) -0.012(5) -0.013(5) -0.001(5) C28 0.076(7) 0.059(7) 0.043(6) -0.010(5) -0.005(5) -0.010(6) C29 0.066(7) 0.046(6) 0.065(7) -0.014(5) 0.004(5) -0.001(5) C30 0.030(5) 0.076(8) 0.088(8) -0.015(7) -0.012(5) -0.001(5) C31 0.048(6) 0.062(7) 0.058(6) -0.016(5) -0.015(5) -0.003(5) C32 0.049(6) 0.053(7) 0.070(7) -0.003(6) 0.000(5) 0.000(5) C33 0.059(7) 0.070(9) 0.077(9) 0.000(7) -0.006(6) -0.006(6) C34 0.079(8) 0.063(9) 0.095(10) -0.024(8) 0.001(7) -0.005(6) C35 0.071(7) 0.059(8) 0.079(9) 0.000(7) -0.013(6) -0.005(6) C36 0.085(8) 0.067(8) 0.079(9) 0.012(7) -0.022(6) -0.028(7) C37 0.092(9) 0.066(8) 0.069(8) -0.009(7) -0.019(6) -0.028(7) C38 0.071(7) 0.044(6) 0.061(7) -0.012(5) -0.009(5) -0.008(5) C39 0.049(6) 0.046(7) 0.076(8) 0.002(6) -0.011(5) 0.001(5) C40 0.074(8) 0.078(9) 0.076(8) -0.034(7) -0.003(6) -0.019(7) C41 0.075(8) 0.043(7) 0.077(8) -0.007(6) -0.005(6) -0.003(6) C42 0.060(7) 0.069(8) 0.087(9) 0.010(7) -0.019(6) -0.007(6) C43 0.072(7) 0.054(7) 0.077(8) -0.002(6) -0.009(6) -0.019(6) C44 0.045(5) 0.052(6) 0.067(7) -0.008(5) -0.004(5) -0.005(5) C45 0.050(6) 0.050(6) 0.078(8) -0.012(6) -0.013(5) -0.003(5) C46 0.067(7) 0.048(7) 0.072(8) -0.012(6) -0.008(6) -0.004(5) C47 0.051(6) 0.062(7) 0.061(7) -0.002(6) -0.005(5) -0.006(5) C48 0.054(6) 0.052(6) 0.087(8) -0.020(6) -0.010(5) -0.029(5) C49 0.055(6) 0.050(6) 0.072(8) -0.009(6) -0.011(5) -0.006(5) C50 0.056(6) 0.054(7) 0.059(6) 0.004(5) -0.005(5) -0.009(5) C51 0.068(7) 0.055(7) 0.082(8) -0.005(6) -0.012(6) -0.006(6) C52 0.060(7) 0.069(8) 0.074(8) -0.008(6) -0.011(6) -0.003(6) C53 0.065(7) 0.052(7) 0.075(8) -0.004(6) -0.004(6) -0.015(6) C54 0.046(6) 0.068(7) 0.061(7) -0.009(6) -0.005(5) -0.012(5) C55 0.064(7) 0.061(7) 0.053(6) -0.014(5) -0.003(5) -0.023(6) N1 0.048(5) 0.065(6) 0.063(5) -0.012(4) -0.003(4) -0.010(4) N2 0.042(5) 0.039(5) 0.097(7) -0.015(4) 0.020(4) -0.003(4) N3 0.046(5) 0.055(5) 0.065(5) -0.006(4) -0.002(4) 0.006(4) N4 0.062(6) 0.045(5) 0.078(6) -0.004(4) 0.008(5) -0.008(4) N5 0.049(5) 0.043(5) 0.077(6) -0.010(4) 0.002(4) 0.009(4) F1 0.063(4) 0.068(4) 0.081(4) -0.020(3) -0.015(3) -0.003(3) F2 0.067(4) 0.073(4) 0.078(4) -0.019(3) -0.007(3) -0.006(3) F3 0.061(4) 0.069(4) 0.099(5) -0.018(4) 0.010(3) 0.001(3) F4 0.060(4) 0.078(4) 0.113(5) -0.025(4) -0.020(3) 0.002(3) F5 0.069(4) 0.073(4) 0.078(4) -0.026(3) -0.011(3) -0.004(3) F6 0.086(4) 0.058(4) 0.080(5) -0.013(3) 0.002(3) -0.009(3) F7 0.092(5) 0.067(4) 0.104(5) -0.025(4) 0.003(4) -0.011(3) F8 0.093(5) 0.056(4) 0.122(6) -0.005(4) -0.007(4) -0.008(4) F9 0.177(8) 0.077(5) 0.076(5) 0.012(4) -0.017(5) -0.053(5) F10 0.117(5) 0.075(4) 0.070(4) -0.016(4) 0.003(4) -0.029(4) F11 0.065(4) 0.073(4) 0.079(4) -0.015(3) -0.012(3) -0.007(3) F12 0.076(4) 0.069(4) 0.109(5) -0.029(4) 0.000(4) -0.022(3) F13 0.082(4) 0.056(4) 0.126(6) -0.003(4) -0.005(4) -0.014(3) F14 0.090(5) 0.074(5) 0.132(6) 0.020(4) -0.048(4) -0.013(4) F15 0.080(4) 0.062(4) 0.107(5) 0.001(4) -0.031(4) -0.011(3) F16 0.062(3) 0.058(4) 0.072(4) -0.014(3) 0.006(3) -0.015(3) F17 0.076(4) 0.063(4) 0.069(4) -0.014(3) 0.001(3) -0.008(3) F18 0.065(4) 0.065(4) 0.079(4) 0.000(3) 0.003(3) -0.012(3) F19 0.058(3) 0.072(4) 0.075(4) -0.014(3) -0.002(3) -0.015(3) F20 0.066(4) 0.069(4) 0.059(4) -0.011(3) -0.001(3) -0.018(3) F21 0.053(3) 0.058(4) 0.098(5) -0.005(3) -0.006(3) -0.004(3) F22 0.070(4) 0.053(4) 0.092(5) 0.009(3) -0.015(3) -0.001(3) F23 0.069(4) 0.054(4) 0.086(4) 0.006(3) -0.007(3) -0.010(3) F24 0.062(4) 0.066(4) 0.074(4) -0.002(3) 0.001(3) -0.010(3) P1 0.0567(16) 0.0522(17) 0.076(2) -0.0095(14) -0.0069(13) -0.0050(13) O1 0.067(4) 0.072(5) 0.061(5) -0.012(4) -0.010(3) -0.008(4) Cl1 0.175(5) 0.095(4) 0.096(4) -0.016(3) -0.039(3) 0.021(4) Cl2 0.077(3) 0.213(7) 0.094(4) -0.071(4) -0.015(2) -0.010(3) C60 0.162(18) 0.029(9) 0.145(17) -0.025(9) -0.115(14) 0.004(9) Cl3 0.223(8) 0.107(5) 0.155(6) -0.033(4) -0.025(6) -0.035(5) Cl4 0.099(4) 0.452(16) 0.099(5) -0.036(7) -0.013(3) -0.075(6) C56 0.35(3) 0.29(3) 0.21(3) -0.11(2) -0.01(2) -0.08(3) C57 0.85(5) 0.40(3) 0.071(14) -0.07(2) 0.06(3) -0.501 N6 0.29(4) 1.02(12) 0.28(4) 0.31(6) 0.11(3) 0.39(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C25 1.399(14) . ? C1 C2 1.402(14) . ? C1 N1 1.419(13) . ? C2 C3 1.395(15) . ? C2 H2 0.9500 . ? C3 C4 1.343(14) . ? C3 H3 0.9500 . ? C4 N1 1.400(12) . ? C4 C5 1.475(14) . ? C5 C6 1.360(13) . ? C5 C26 1.471(13) . ? C6 N2 1.414(12) . ? C6 C7 1.506(15) . ? C7 C8 1.555(14) . ? C7 H7 0.9900 . ? C7 H7A 0.9900 . ? C8 C9 1.521(13) . ? C8 H8 0.9900 . ? C8 H8A 0.9900 . ? C9 C10 1.371(13) . ? C9 N2 1.385(12) . ? C10 C11 1.437(13) . ? C10 C32 1.484(14) . ? C11 N3 1.357(11) . ? C11 C12 1.414(13) . ? C12 C13 1.400(13) . ? C12 P1 1.742(9) . ? C13 C23 1.390(14) . ? C13 C14 1.504(13) . ? C14 N3 1.374(13) . ? C14 C15 1.416(13) . ? C15 C16 1.383(14) . ? C15 C38 1.496(14) . ? C16 N4 1.363(12) . ? C16 C17 1.454(13) . ? C17 C18 1.395(15) . ? C17 H17 0.9500 . ? C18 C19 1.434(13) . ? C18 H18 0.9500 . ? C19 N4 1.388(13) . ? C19 C20 1.445(14) . ? C20 C21 1.371(13) . ? C20 C44 1.478(14) . ? C21 N5 1.391(12) . ? C21 C22 1.421(15) . ? C22 N4 1.327(13) . ? C22 C23 1.327(14) . ? C23 C24 1.519(14) . ? C24 C25 1.389(13) . ? C24 N5 1.417(13) . ? C25 C50 1.460(14) . ? C26 C27 1.352(12) . ? C26 C31 1.422(12) . ? C27 F1 1.350(10) . ? C27 C28 1.377(13) . ? C28 F2 1.350(11) . ? C28 C29 1.378(14) . ? C29 C30 1.340(14) . ? C29 F3 1.361(10) . ? C30 C31 1.368(13) . ? C30 F4 1.375(11) . ? C31 F5 1.325(10) . ? C32 C37 1.387(15) . ? C32 C33 1.404(15) . ? C33 F6 1.342(13) . ? C33 C34 1.390(16) . ? C34 F7 1.338(13) . ? C34 C35 1.353(17) . ? C35 F8 1.330(13) . ? C35 C36 1.377(16) . ? C36 F9 1.333(13) . ? C36 C37 1.386(15) . ? C37 F10 1.348(12) . ? C38 C39 1.358(14) . ? C38 C43 1.404(14) . ? C39 F11 1.336(11) . ? C39 C40 1.371(15) . ? C40 F12 1.335(12) . ? C40 C41 1.372(15) . ? C41 F13 1.353(12) . ? C41 C42 1.359(15) . ? C42 C43 1.364(15) . ? C42 F14 1.370(12) . ? C43 F15 1.346(11) . ? C44 C49 1.352(13) . ? C44 C45 1.384(14) . ? C45 F16 1.332(11) . ? C45 C46 1.421(15) . ? C46 F17 1.322(12) . ? C46 C47 1.374(14) . ? C47 F18 1.369(12) . ? C47 C48 1.381(14) . ? C48 F19 1.334(10) . ? C48 C49 1.378(15) . ? C49 F20 1.358(11) . ? C50 C55 1.392(13) . ? C50 C51 1.411(14) . ? C51 F21 1.350(12) . ? C51 C52 1.372(16) . ? C52 F22 1.329(12) . ? C52 C53 1.372(14) . ? C53 F23 1.363(12) . ? C53 C54 1.373(14) . ? C54 F24 1.339(11) . ? C54 C55 1.410(14) . ? C55 N5 1.402(12) . ? N1 P1 1.700(9) . ? N2 P1 1.687(8) . ? P1 O1 1.460(7) . ? Cl1 C60 1.677(17) . ? Cl2 C60 1.894(19) . ? C60 Cl3 1.61(2) . ? C60 Cl4 1.84(2) . ? C56 N6 1.161(5) . ? C56 C57 1.452(5) . ? C57 H19 0.9800 . ? C57 H20 0.9800 . ? C57 H21 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C25 C1 C2 124.1(10) . . ? C25 C1 N1 130.5(10) . . ? C2 C1 N1 105.3(9) . . ? C3 C2 C1 108.8(10) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? C4 C3 C2 109.0(10) . . ? C4 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? C3 C4 N1 108.5(10) . . ? C3 C4 C5 129.3(9) . . ? N1 C4 C5 121.9(9) . . ? C6 C5 C26 121.6(9) . . ? C6 C5 C4 120.5(9) . . ? C26 C5 C4 117.7(8) . . ? C5 C6 N2 121.1(9) . . ? C5 C6 C7 132.3(10) . . ? N2 C6 C7 106.6(9) . . ? C6 C7 C8 104.6(8) . . ? C6 C7 H7 110.8 . . ? C8 C7 H7 110.8 . . ? C6 C7 H7A 110.8 . . ? C8 C7 H7A 110.8 . . ? H7 C7 H7A 108.9 . . ? C9 C8 C7 102.6(9) . . ? C9 C8 H8 111.2 . . ? C7 C8 H8 111.2 . . ? C9 C8 H8A 111.2 . . ? C7 C8 H8A 111.2 . . ? H8 C8 H8A 109.2 . . ? C10 C9 N2 121.8(9) . . ? C10 C9 C8 128.2(9) . . ? N2 C9 C8 109.9(8) . . ? C9 C10 C11 120.8(9) . . ? C9 C10 C32 120.8(9) . . ? C11 C10 C32 118.4(8) . . ? N3 C11 C12 112.4(9) . . ? N3 C11 C10 124.4(9) . . ? C12 C11 C10 123.2(8) . . ? C13 C12 C11 106.8(8) . . ? C13 C12 P1 129.8(8) . . ? C11 C12 P1 119.7(7) . . ? C23 C13 C12 130.6(9) . . ? C23 C13 C14 124.5(10) . . ? C12 C13 C14 104.9(9) . . ? N3 C14 C15 117.5(9) . . ? N3 C14 C13 108.5(8) . . ? C15 C14 C13 133.1(10) . . ? C16 C15 C14 125.7(10) . . ? C16 C15 C38 117.6(9) . . ? C14 C15 C38 116.8(9) . . ? N4 C16 C15 122.0(9) . . ? N4 C16 C17 104.5(9) . . ? C15 C16 C17 133.1(10) . . ? C18 C17 C16 108.5(9) . . ? C18 C17 H17 125.8 . . ? C16 C17 H17 125.8 . . ? C17 C18 C19 108.0(10) . . ? C17 C18 H18 126.0 . . ? C19 C18 H18 126.0 . . ? N4 C19 C18 105.1(9) . . ? N4 C19 C20 108.0(9) . . ? C18 C19 C20 146.4(10) . . ? C21 C20 C19 104.9(10) . . ? C21 C20 C44 132.5(10) . . ? C19 C20 C44 122.5(9) . . ? C20 C21 N5 147.1(12) . . ? C20 C21 C22 109.4(10) . . ? N5 C21 C22 103.3(9) . . ? N4 C22 C23 134.4(11) . . ? N4 C22 C21 108.3(10) . . ? C23 C22 C21 116.7(10) . . ? C22 C23 C13 123.2(10) . . ? C22 C23 C24 102.8(9) . . ? C13 C23 C24 133.1(10) . . ? C25 C24 N5 111.9(9) . . ? C25 C24 C23 141.5(10) . . ? N5 C24 C23 105.9(8) . . ? C24 C25 C1 132.4(10) . . ? C24 C25 C50 103.7(9) . . ? C1 C25 C50 123.5(9) . . ? C27 C26 C31 116.6(9) . . ? C27 C26 C5 122.5(9) . . ? C31 C26 C5 120.8(9) . . ? F1 C27 C26 120.0(9) . . ? F1 C27 C28 117.8(9) . . ? C26 C27 C28 122.3(9) . . ? F2 C28 C27 121.3(9) . . ? F2 C28 C29 118.4(9) . . ? C27 C28 C29 120.2(10) . . ? C30 C29 F3 121.0(10) . . ? C30 C29 C28 118.8(9) . . ? F3 C29 C28 120.2(9) . . ? C29 C30 C31 121.7(9) . . ? C29 C30 F4 119.3(9) . . ? C31 C30 F4 118.6(10) . . ? F5 C31 C30 119.6(8) . . ? F5 C31 C26 120.1(8) . . ? C30 C31 C26 120.3(9) . . ? C37 C32 C33 115.4(11) . . ? C37 C32 C10 123.6(10) . . ? C33 C32 C10 121.1(10) . . ? F6 C33 C34 119.3(11) . . ? F6 C33 C32 118.5(11) . . ? C34 C33 C32 122.2(12) . . ? F7 C34 C35 121.1(12) . . ? F7 C34 C33 118.5(13) . . ? C35 C34 C33 120.3(12) . . ? F8 C35 C34 119.9(12) . . ? F8 C35 C36 120.7(12) . . ? C34 C35 C36 119.4(12) . . ? F9 C36 C35 119.9(11) . . ? F9 C36 C37 119.7(12) . . ? C35 C36 C37 120.4(12) . . ? F10 C37 C36 117.6(11) . . ? F10 C37 C32 120.2(11) . . ? C36 C37 C32 122.3(11) . . ? C39 C38 C43 115.8(10) . . ? C39 C38 C15 122.0(10) . . ? C43 C38 C15 122.2(9) . . ? F11 C39 C38 120.4(10) . . ? F11 C39 C40 116.5(10) . . ? C38 C39 C40 123.0(10) . . ? F12 C40 C39 122.0(11) . . ? F12 C40 C41 118.4(11) . . ? C39 C40 C41 119.6(11) . . ? F13 C41 C42 119.7(11) . . ? F13 C41 C40 120.7(11) . . ? C42 C41 C40 119.6(11) . . ? C41 C42 C43 119.9(11) . . ? C41 C42 F14 120.3(11) . . ? C43 C42 F14 119.8(11) . . ? F15 C43 C42 118.1(10) . . ? F15 C43 C38 119.7(10) . . ? C42 C43 C38 122.2(11) . . ? C49 C44 C45 118.0(10) . . ? C49 C44 C20 122.3(10) . . ? C45 C44 C20 119.7(10) . . ? F16 C45 C44 122.0(10) . . ? F16 C45 C46 116.1(10) . . ? C44 C45 C46 121.7(10) . . ? F17 C46 C47 121.7(11) . . ? F17 C46 C45 121.7(10) . . ? C47 C46 C45 116.5(10) . . ? F18 C47 C46 118.1(10) . . ? F18 C47 C48 119.3(10) . . ? C46 C47 C48 122.4(11) . . ? F19 C48 C49 122.0(10) . . ? F19 C48 C47 119.8(10) . . ? C49 C48 C47 118.2(9) . . ? C44 C49 F20 119.8(10) . . ? C44 C49 C48 122.9(10) . . ? F20 C49 C48 117.2(9) . . ? C55 C50 C51 116.7(10) . . ? C55 C50 C25 109.2(9) . . ? C51 C50 C25 133.9(10) . . ? F21 C51 C52 117.9(10) . . ? F21 C51 C50 121.0(11) . . ? C52 C51 C50 121.1(11) . . ? F22 C52 C53 118.9(11) . . ? F22 C52 C51 121.3(10) . . ? C53 C52 C51 119.7(11) . . ? F23 C53 C52 118.3(10) . . ? F23 C53 C54 118.9(10) . . ? C52 C53 C54 122.5(11) . . ? F24 C54 C53 121.5(10) . . ? F24 C54 C55 121.5(9) . . ? C53 C54 C55 116.9(10) . . ? C50 C55 N5 108.7(9) . . ? C50 C55 C54 122.6(10) . . ? N5 C55 C54 128.7(9) . . ? C4 N1 C1 108.3(8) . . ? C4 N1 P1 124.8(7) . . ? C1 N1 P1 126.2(7) . . ? C9 N2 C6 110.7(8) . . ? C9 N2 P1 124.3(6) . . ? C6 N2 P1 124.8(7) . . ? C11 N3 C14 107.3(8) . . ? C22 N4 C16 136.7(9) . . ? C22 N4 C19 109.3(9) . . ? C16 N4 C19 113.6(8) . . ? C21 N5 C55 142.2(9) . . ? C21 N5 C24 111.1(9) . . ? C55 N5 C24 106.1(8) . . ? O1 P1 N2 118.2(4) . . ? O1 P1 N1 112.9(4) . . ? N2 P1 N1 98.8(4) . . ? O1 P1 C12 112.8(4) . . ? N2 P1 C12 98.2(5) . . ? N1 P1 C12 114.5(5) . . ? Cl3 C60 Cl1 115.3(15) . . ? Cl3 C60 Cl4 109.4(9) . . ? Cl1 C60 Cl4 105.7(9) . . ? Cl3 C60 Cl2 120.4(8) . . ? Cl1 C60 Cl2 105.8(8) . . ? Cl4 C60 Cl2 98.0(12) . . ? N6 C56 C57 144(4) . . ? C56 C57 H19 109.5 . . ? C56 C57 H20 109.5 . . ? H19 C57 H20 109.5 . . ? C56 C57 H21 109.5 . . ? H19 C57 H21 109.5 . . ? H20 C57 H21 109.5 . . ? 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 C25 C1 C2 C3 178.9(10) . . . . ? N1 C1 C2 C3 0.8(12) . . . . ? C1 C2 C3 C4 -2.3(13) . . . . ? C2 C3 C4 N1 2.9(12) . . . . ? C2 C3 C4 C5 -170.4(10) . . . . ? C3 C4 C5 C6 -177.3(11) . . . . ? N1 C4 C5 C6 10.2(15) . . . . ? C3 C4 C5 C26 7.5(16) . . . . ? N1 C4 C5 C26 -165.0(9) . . . . ? C26 C5 C6 N2 178.6(9) . . . . ? C4 C5 C6 N2 3.6(15) . . . . ? C26 C5 C6 C7 -1.5(18) . . . . ? C4 C5 C6 C7 -176.5(11) . . . . ? C5 C6 C7 C8 -156.5(12) . . . . ? N2 C6 C7 C8 23.5(12) . . . . ? C6 C7 C8 C9 -15.4(12) . . . . ? C7 C8 C9 C10 178.6(11) . . . . ? C7 C8 C9 N2 2.3(12) . . . . ? N2 C9 C10 C11 4.8(15) . . . . ? C8 C9 C10 C11 -171.1(10) . . . . ? N2 C9 C10 C32 -176.4(9) . . . . ? C8 C9 C10 C32 7.8(17) . . . . ? C9 C10 C11 N3 176.2(10) . . . . ? C32 C10 C11 N3 -2.8(14) . . . . ? C9 C10 C11 C12 -6.4(15) . . . . ? C32 C10 C11 C12 174.7(10) . . . . ? N3 C11 C12 C13 0.3(12) . . . . ? C10 C11 C12 C13 -177.4(9) . . . . ? N3 C11 C12 P1 160.7(7) . . . . ? C10 C11 C12 P1 -17.0(14) . . . . ? C11 C12 C13 C23 177.6(11) . . . . ? P1 C12 C13 C23 19.9(17) . . . . ? C11 C12 C13 C14 -0.8(11) . . . . ? P1 C12 C13 C14 -158.5(9) . . . . ? C23 C13 C14 N3 -177.4(10) . . . . ? C12 C13 C14 N3 1.1(11) . . . . ? C23 C13 C14 C15 -8.4(19) . . . . ? C12 C13 C14 C15 170.1(11) . . . . ? N3 C14 C15 C16 174.6(10) . . . . ? C13 C14 C15 C16 6.4(19) . . . . ? N3 C14 C15 C38 -5.1(14) . . . . ? C13 C14 C15 C38 -173.3(10) . . . . ? C14 C15 C16 N4 -2.6(17) . . . . ? C38 C15 C16 N4 177.1(9) . . . . ? C14 C15 C16 C17 -175.2(11) . . . . ? C38 C15 C16 C17 4.5(17) . . . . ? N4 C16 C17 C18 -4.4(12) . . . . ? C15 C16 C17 C18 169.1(11) . . . . ? C16 C17 C18 C19 3.5(13) . . . . ? C17 C18 C19 N4 -1.3(12) . . . . ? C17 C18 C19 C20 -172.0(15) . . . . ? N4 C19 C20 C21 0.1(11) . . . . ? C18 C19 C20 C21 170.8(15) . . . . ? N4 C19 C20 C44 -176.3(9) . . . . ? C18 C19 C20 C44 -6(2) . . . . ? C19 C20 C21 N5 -172.5(16) . . . . ? C44 C20 C21 N5 3(3) . . . . ? C19 C20 C21 C22 0.5(12) . . . . ? C44 C20 C21 C22 176.5(11) . . . . ? C20 C21 C22 N4 -1.1(13) . . . . ? N5 C21 C22 N4 175.1(9) . . . . ? C20 C21 C22 C23 -174.0(10) . . . . ? N5 C21 C22 C23 2.2(14) . . . . ? N4 C22 C23 C13 -3(2) . . . . ? C21 C22 C23 C13 167.3(11) . . . . ? N4 C22 C23 C24 -174.0(13) . . . . ? C21 C22 C23 C24 -3.5(14) . . . . ? C12 C13 C23 C22 -171.9(11) . . . . ? C14 C13 C23 C22 6.2(18) . . . . ? C12 C13 C23 C24 -4(2) . . . . ? C14 C13 C23 C24 173.9(10) . . . . ? C22 C23 C24 C25 -165.7(14) . . . . ? C13 C23 C24 C25 25(2) . . . . ? C22 C23 C24 N5 3.4(12) . . . . ? C13 C23 C24 N5 -166.1(12) . . . . ? N5 C24 C25 C1 -167.3(11) . . . . ? C23 C24 C25 C1 1(2) . . . . ? N5 C24 C25 C50 5.2(11) . . . . ? C23 C24 C25 C50 173.9(13) . . . . ? C2 C1 C25 C24 146.3(12) . . . . ? N1 C1 C25 C24 -36(2) . . . . ? C2 C1 C25 C50 -24.8(17) . . . . ? N1 C1 C25 C50 152.7(10) . . . . ? C6 C5 C26 C27 118.2(12) . . . . ? C4 C5 C26 C27 -66.6(13) . . . . ? C6 C5 C26 C31 -65.8(13) . . . . ? C4 C5 C26 C31 109.4(11) . . . . ? C31 C26 C27 F1 178.6(9) . . . . ? C5 C26 C27 F1 -5.2(15) . . . . ? C31 C26 C27 C28 -1.7(15) . . . . ? C5 C26 C27 C28 174.5(10) . . . . ? F1 C27 C28 F2 0.9(15) . . . . ? C26 C27 C28 F2 -178.7(9) . . . . ? F1 C27 C28 C29 179.8(10) . . . . ? C26 C27 C28 C29 0.1(16) . . . . ? F2 C28 C29 C30 -177.9(10) . . . . ? C27 C28 C29 C30 3.3(16) . . . . ? F2 C28 C29 F3 0.7(15) . . . . ? C27 C28 C29 F3 -178.1(9) . . . . ? F3 C29 C30 C31 176.5(10) . . . . ? C28 C29 C30 C31 -4.9(17) . . . . ? F3 C29 C30 F4 3.4(17) . . . . ? C28 C29 C30 F4 -177.9(10) . . . . ? C29 C30 C31 F5 -176.0(10) . . . . ? F4 C30 C31 F5 -2.9(16) . . . . ? C29 C30 C31 C26 3.3(17) . . . . ? F4 C30 C31 C26 176.3(9) . . . . ? C27 C26 C31 F5 179.4(9) . . . . ? C5 C26 C31 F5 3.1(15) . . . . ? C27 C26 C31 C30 0.1(15) . . . . ? C5 C26 C31 C30 -176.1(10) . . . . ? C9 C10 C32 C37 -65.6(15) . . . . ? C11 C10 C32 C37 113.3(11) . . . . ? C9 C10 C32 C33 114.7(11) . . . . ? C11 C10 C32 C33 -66.4(13) . . . . ? C37 C32 C33 F6 178.0(9) . . . . ? C10 C32 C33 F6 -2.3(15) . . . . ? C37 C32 C33 C34 -3.3(16) . . . . ? C10 C32 C33 C34 176.4(10) . . . . ? F6 C33 C34 F7 -0.6(16) . . . . ? C32 C33 C34 F7 -179.2(9) . . . . ? F6 C33 C34 C35 -177.5(10) . . . . ? C32 C33 C34 C35 3.9(18) . . . . ? F7 C34 C35 F8 2.3(17) . . . . ? C33 C34 C35 F8 179.1(10) . . . . ? F7 C34 C35 C36 -179.2(10) . . . . ? C33 C34 C35 C36 -2.4(18) . . . . ? F8 C35 C36 F9 -1.8(17) . . . . ? C34 C35 C36 F9 179.7(11) . . . . ? F8 C35 C36 C37 179.2(10) . . . . ? C34 C35 C36 C37 0.7(18) . . . . ? F9 C36 C37 F10 0.7(17) . . . . ? C35 C36 C37 F10 179.8(10) . . . . ? F9 C36 C37 C32 -179.4(10) . . . . ? C35 C36 C37 C32 -0.3(18) . . . . ? C33 C32 C37 F10 -178.5(9) . . . . ? C10 C32 C37 F10 1.8(16) . . . . ? C33 C32 C37 C36 1.6(16) . . . . ? C10 C32 C37 C36 -178.1(10) . . . . ? C16 C15 C38 C39 -114.4(12) . . . . ? C14 C15 C38 C39 65.3(14) . . . . ? C16 C15 C38 C43 64.7(14) . . . . ? C14 C15 C38 C43 -115.5(12) . . . . ? C43 C38 C39 F11 -177.3(9) . . . . ? C15 C38 C39 F11 1.9(15) . . . . ? C43 C38 C39 C40 -0.7(16) . . . . ? C15 C38 C39 C40 178.5(11) . . . . ? F11 C39 C40 F12 -3.6(16) . . . . ? C38 C39 C40 F12 179.6(10) . . . . ? F11 C39 C40 C41 177.2(10) . . . . ? C38 C39 C40 C41 0.5(18) . . . . ? F12 C40 C41 F13 2.7(17) . . . . ? C39 C40 C41 F13 -178.1(10) . . . . ? F12 C40 C41 C42 -179.7(10) . . . . ? C39 C40 C41 C42 -0.5(18) . . . . ? F13 C41 C42 C43 178.3(11) . . . . ? C40 C41 C42 C43 0.7(18) . . . . ? F13 C41 C42 F14 -1.4(17) . . . . ? C40 C41 C42 F14 -179.0(10) . . . . ? C41 C42 C43 F15 178.9(11) . . . . ? F14 C42 C43 F15 -1.3(17) . . . . ? C41 C42 C43 C38 -1.0(18) . . . . ? F14 C42 C43 C38 178.8(10) . . . . ? C39 C38 C43 F15 -178.9(9) . . . . ? C15 C38 C43 F15 1.9(16) . . . . ? C39 C38 C43 C42 0.9(17) . . . . ? C15 C38 C43 C42 -178.3(11) . . . . ? C21 C20 C44 C49 68.8(16) . . . . ? C19 C20 C44 C49 -115.8(11) . . . . ? C21 C20 C44 C45 -112.6(13) . . . . ? C19 C20 C44 C45 62.8(13) . . . . ? C49 C44 C45 F16 -179.6(8) . . . . ? C20 C44 C45 F16 1.7(14) . . . . ? C49 C44 C45 C46 -5.1(14) . . . . ? C20 C44 C45 C46 176.2(9) . . . . ? F16 C45 C46 F17 -1.7(14) . . . . ? C44 C45 C46 F17 -176.4(8) . . . . ? F16 C45 C46 C47 -178.9(8) . . . . ? C44 C45 C46 C47 6.3(15) . . . . ? F17 C46 C47 F18 3.3(14) . . . . ? C45 C46 C47 F18 -179.4(8) . . . . ? F17 C46 C47 C48 177.7(9) . . . . ? C45 C46 C47 C48 -5.1(15) . . . . ? F18 C47 C48 F19 -5.7(14) . . . . ? C46 C47 C48 F19 -180.0(9) . . . . ? F18 C47 C48 C49 177.0(9) . . . . ? C46 C47 C48 C49 2.7(16) . . . . ? C45 C44 C49 F20 178.4(8) . . . . ? C20 C44 C49 F20 -2.9(14) . . . . ? C45 C44 C49 C48 2.6(15) . . . . ? C20 C44 C49 C48 -178.8(9) . . . . ? F19 C48 C49 C44 -178.6(8) . . . . ? C47 C48 C49 C44 -1.3(16) . . . . ? F19 C48 C49 F20 5.4(15) . . . . ? C47 C48 C49 F20 -177.3(8) . . . . ? C24 C25 C50 C55 -6.2(11) . . . . ? C1 C25 C50 C55 167.1(10) . . . . ? C24 C25 C50 C51 169.4(11) . . . . ? C1 C25 C50 C51 -17.3(19) . . . . ? C55 C50 C51 F21 170.9(9) . . . . ? C25 C50 C51 F21 -4.4(19) . . . . ? C55 C50 C51 C52 -7.1(16) . . . . ? C25 C50 C51 C52 177.6(11) . . . . ? F21 C51 C52 F22 2.0(16) . . . . ? C50 C51 C52 F22 -179.9(9) . . . . ? F21 C51 C52 C53 -175.3(9) . . . . ? C50 C51 C52 C53 2.8(17) . . . . ? F22 C52 C53 F23 0.2(15) . . . . ? C51 C52 C53 F23 177.5(10) . . . . ? F22 C52 C53 C54 -175.1(10) . . . . ? C51 C52 C53 C54 2.2(17) . . . . ? F23 C53 C54 F24 -2.0(15) . . . . ? C52 C53 C54 F24 173.3(9) . . . . ? F23 C53 C54 C55 -177.8(9) . . . . ? C52 C53 C54 C55 -2.5(16) . . . . ? C51 C50 C55 N5 -171.4(9) . . . . ? C25 C50 C55 N5 5.0(11) . . . . ? C51 C50 C55 C54 6.8(15) . . . . ? C25 C50 C55 C54 -176.7(9) . . . . ? F24 C54 C55 C50 -178.0(8) . . . . ? C53 C54 C55 C50 -2.2(15) . . . . ? F24 C54 C55 N5 -0.1(16) . . . . ? C53 C54 C55 N5 175.6(10) . . . . ? C3 C4 N1 C1 -2.4(11) . . . . ? C5 C4 N1 C1 171.5(9) . . . . ? C3 C4 N1 P1 -173.3(8) . . . . ? C5 C4 N1 P1 0.6(13) . . . . ? C25 C1 N1 C4 -177.0(11) . . . . ? C2 C1 N1 C4 0.9(11) . . . . ? C25 C1 N1 P1 -6.2(16) . . . . ? C2 C1 N1 P1 171.7(7) . . . . ? C10 C9 N2 C6 -163.5(9) . . . . ? C8 C9 N2 C6 13.0(12) . . . . ? C10 C9 N2 P1 22.0(15) . . . . ? C8 C9 N2 P1 -161.5(7) . . . . ? C5 C6 N2 C9 156.8(10) . . . . ? C7 C6 N2 C9 -23.2(12) . . . . ? C5 C6 N2 P1 -28.8(14) . . . . ? C7 C6 N2 P1 151.3(8) . . . . ? C12 C11 N3 C14 0.4(11) . . . . ? C10 C11 N3 C14 178.1(9) . . . . ? C15 C14 N3 C11 -171.9(9) . . . . ? C13 C14 N3 C11 -0.9(11) . . . . ? C23 C22 N4 C16 1(2) . . . . ? C21 C22 N4 C16 -170.6(11) . . . . ? C23 C22 N4 C19 172.3(14) . . . . ? C21 C22 N4 C19 1.2(13) . . . . ? C15 C16 N4 C22 1(2) . . . . ? C17 C16 N4 C22 175.2(12) . . . . ? C15 C16 N4 C19 -170.7(9) . . . . ? C17 C16 N4 C19 3.7(12) . . . . ? C18 C19 N4 C22 -175.5(9) . . . . ? C20 C19 N4 C22 -0.8(12) . . . . ? C18 C19 N4 C16 -1.6(12) . . . . ? C20 C19 N4 C16 173.0(9) . . . . ? C20 C21 N5 C55 -18(3) . . . . ? C22 C21 N5 C55 168.9(12) . . . . ? C20 C21 N5 C24 173.7(16) . . . . ? C22 C21 N5 C24 0.4(11) . . . . ? C50 C55 N5 C21 -170.7(12) . . . . ? C54 C55 N5 C21 11(2) . . . . ? C50 C55 N5 C24 -1.8(11) . . . . ? C54 C55 N5 C24 -179.9(10) . . . . ? C25 C24 N5 C21 170.4(9) . . . . ? C23 C24 N5 C21 -2.3(11) . . . . ? C25 C24 N5 C55 -2.3(11) . . . . ? C23 C24 N5 C55 -175.0(8) . . . . ? C9 N2 P1 O1 84.4(9) . . . . ? C6 N2 P1 O1 -89.4(9) . . . . ? C9 N2 P1 N1 -153.6(9) . . . . ? C6 N2 P1 N1 32.6(9) . . . . ? C9 N2 P1 C12 -37.1(10) . . . . ? C6 N2 P1 C12 149.2(9) . . . . ? C4 N1 P1 O1 107.4(8) . . . . ? C1 N1 P1 O1 -61.9(9) . . . . ? C4 N1 P1 N2 -18.4(9) . . . . ? C1 N1 P1 N2 172.3(8) . . . . ? C4 N1 P1 C12 -121.7(8) . . . . ? C1 N1 P1 C12 69.0(9) . . . . ? C13 C12 P1 O1 63.2(11) . . . . ? C11 C12 P1 O1 -92.0(9) . . . . ? C13 C12 P1 N2 -171.4(10) . . . . ? C11 C12 P1 N2 33.3(9) . . . . ? C13 C12 P1 N1 -67.7(11) . . . . ? C11 C12 P1 N1 137.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.615 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.114