# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Atsuhiro Osuka' _publ_contact_author_email OSUKA@KUCHEM.KYOTO-U.AC.JP _publ_section_title ; Muliple conformational changes of beta-tetraphenyl meso-hexakis(pentafluorophenyl) substituted [26] and [28]hexaphyrins(1.1.1.1.1.1) ; loop_ _publ_author_name 'Atsuhiro Osuka' 'Taro Koide' 'Shohei Saito' 'Katsuyuki Youfu' # Attachment '3A_SQ.cif' data_3A_SQ _database_code_depnum_ccdc_archive 'CCDC 728271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C90 H30 F30 N6), 2(C H Cl3)' _chemical_formula_sum 'C272 H92 Cl6 F90 N18' _chemical_formula_weight 5534.34 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' Cl Cl 0.3639 0.7018 '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' N N 0.0311 0.0180 '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 18.209(3) _cell_length_b 18.259(3) _cell_length_c 19.016(3) _cell_angle_alpha 98.298(11) _cell_angle_beta 105.095(10) _cell_angle_gamma 94.010(11) _cell_volume 6002.0(17) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13275 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 68.16 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2762 _exptl_absorpt_coefficient_mu 1.831 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50467 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.1582 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 64.00 _reflns_number_total 18798 _reflns_number_gt 5336 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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. Though some electron density was properly assigned as a molecule of chloroform, other electron density due to severely disordered solvents still remained. All attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to this solvent molecule were removed by use of the utility SQUEEZE in PLATON software packate, SQUEEZE-PLATON. ; _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^)+(0.1080P)^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 18798 _refine_ls_number_parameters 1738 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1963 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2453 _refine_ls_wR_factor_gt 0.1958 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_restrained_S_all 0.800 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F 0.78314(18) 0.12101(18) 0.41811(18) 0.0569(10) Uani 1 1 d . . . F2 F 0.7317(2) 0.1127(2) 0.53754(19) 0.0761(12) Uani 1 1 d . . . F3 F 0.7325(2) 0.2386(2) 0.63386(19) 0.0805(13) Uani 1 1 d . . . F4 F 0.7914(2) 0.3727(2) 0.6119(2) 0.0965(15) Uani 1 1 d . . . F5 F 0.8481(2) 0.3788(2) 0.49534(19) 0.0746(12) Uani 1 1 d . . . F6 F 1.1158(2) 0.44712(18) 0.48255(17) 0.0632(11) Uani 1 1 d . . . F7 F 1.2440(2) 0.5146(2) 0.58363(19) 0.0786(12) Uani 1 1 d . . . F8 F 1.3789(2) 0.4555(2) 0.59381(19) 0.0726(12) Uani 1 1 d . . . F9 F 1.3828(2) 0.3269(2) 0.50372(18) 0.0709(11) Uani 1 1 d . . . F10 F 1.25522(17) 0.25889(19) 0.40310(17) 0.0539(10) Uani 1 1 d . . . F11 F 1.33417(16) 0.3519(2) 0.32077(16) 0.0544(10) Uani 1 1 d . . . F12 F 1.44586(18) 0.4367(2) 0.42767(17) 0.0688(12) Uani 1 1 d . . . F13 F 1.46094(19) 0.5868(2) 0.43362(18) 0.0641(11) Uani 1 1 d . . . F14 F 1.3614(2) 0.6501(2) 0.33346(18) 0.0688(12) Uani 1 1 d . . . F15 F 1.24741(19) 0.56509(19) 0.22669(18) 0.0574(10) Uani 1 1 d . . . F16 F 1.1506(2) 0.2863(2) -0.16174(18) 0.0733(12) Uani 1 1 d . . . F17 F 1.2086(2) 0.2948(2) -0.2784(2) 0.0861(13) Uani 1 1 d . . . F18 F 1.2666(2) 0.4279(2) -0.2995(2) 0.0823(13) Uani 1 1 d . . . F19 F 1.2693(2) 0.5532(2) -0.20437(18) 0.0743(12) Uani 1 1 d . . . F20 F 1.21773(18) 0.54603(19) -0.08439(17) 0.0564(10) Uani 1 1 d . . . F21 F 0.88461(19) 0.21940(19) -0.14993(17) 0.0635(11) Uani 1 1 d . . . F22 F 0.7556(2) 0.1523(2) -0.25019(18) 0.0721(12) Uani 1 1 d . . . F23 F 0.6220(2) 0.2112(2) -0.26001(19) 0.0745(12) Uani 1 1 d . . . F24 F 0.61681(19) 0.3391(2) -0.17030(18) 0.0674(11) Uani 1 1 d . . . F25 F 0.74482(16) 0.4075(2) -0.07044(17) 0.0545(10) Uani 1 1 d . . . F26 F 0.75102(18) 0.10335(18) 0.10584(17) 0.0546(10) Uani 1 1 d . . . F27 F 0.63847(19) 0.0170(2) -0.00064(18) 0.0658(11) Uani 1 1 d . . . F28 F 0.53924(19) 0.0806(2) -0.10034(17) 0.0671(11) Uani 1 1 d . . . F29 F 0.55489(19) 0.2300(2) -0.09355(19) 0.0666(11) Uani 1 1 d . . . F30 F 0.66564(18) 0.3165(2) 0.01204(17) 0.0549(10) Uani 1 1 d . . . N1 N 0.8298(3) 0.2633(2) 0.2580(3) 0.0409(13) Uani 1 1 d . . . H1 H 0.8782 0.2715 0.2587 0.049 Uiso 1 1 calc R . . N2 N 0.9726(3) 0.2752(3) 0.3576(3) 0.0442(14) Uani 1 1 d . . . N3 N 1.1735(3) 0.3752(3) 0.3029(3) 0.0411(14) Uani 1 1 d . . . N4 N 1.1697(3) 0.4021(3) 0.0734(3) 0.0442(14) Uani 1 1 d . . . H2 H 1.1212 0.3934 0.0721 0.053 Uiso 1 1 calc R . . N5 N 1.0254(3) 0.3905(2) -0.0268(2) 0.0415(14) Uani 1 1 d . . . N6 N 0.8266(2) 0.2916(3) 0.0303(2) 0.0385(13) Uani 1 1 d . . . C1 C 0.7701(4) 0.2553(3) 0.1976(4) 0.050(2) Uani 1 1 d . . . C2 C 0.6991(4) 0.2449(3) 0.2176(3) 0.0432(17) Uani 1 1 d . . . C3 C 0.7201(3) 0.2495(3) 0.2940(3) 0.0326(15) Uani 1 1 d . . . C4 C 0.8032(3) 0.2564(3) 0.3190(4) 0.0383(17) Uani 1 1 d . . . C5 C 0.8495(3) 0.2546(3) 0.3899(4) 0.0436(18) Uani 1 1 d . . . C6 C 0.9295(4) 0.2608(3) 0.4044(3) 0.0406(17) Uani 1 1 d . . . C7 C 0.9810(4) 0.2554(3) 0.4771(3) 0.0525(19) Uani 1 1 d . . . H3 H 0.9662 0.2423 0.5184 0.063 Uiso 1 1 calc R . . C8 C 1.0538(4) 0.2729(3) 0.4736(3) 0.0458(18) Uani 1 1 d . . . H4 H 1.0995 0.2754 0.5123 0.055 Uiso 1 1 calc R . . C9 C 1.0480(4) 0.2869(3) 0.4002(4) 0.0462(18) Uani 1 1 d . . . C10 C 1.1107(3) 0.3159(3) 0.3787(3) 0.0385(16) Uani 1 1 d . . . C11 C 1.1143(4) 0.3280(3) 0.3078(3) 0.0378(16) Uani 1 1 d . . . C12 C 1.0676(3) 0.2942(3) 0.2335(3) 0.0453(18) Uani 1 1 d . . . H5 H 1.0220 0.2610 0.2220 0.054 Uiso 1 1 calc R . . C13 C 1.1013(3) 0.3188(4) 0.1840(4) 0.0523(19) Uani 1 1 d . . . H6 H 1.0858 0.3051 0.1318 0.063 Uiso 1 1 calc R . . C14 C 1.1678(4) 0.3718(3) 0.2299(3) 0.0410(17) Uani 1 1 d . . . C15 C 1.2238(3) 0.4084(3) 0.2079(4) 0.0410(18) Uani 1 1 d . . . C16 C 1.2306(4) 0.4119(3) 0.1342(3) 0.0373(16) Uani 1 1 d . . . C17 C 1.3008(4) 0.4208(3) 0.1134(4) 0.0458(18) Uani 1 1 d . . . C18 C 1.2808(3) 0.4170(3) 0.0373(4) 0.0453(18) Uani 1 1 d . . . C19 C 1.1988(4) 0.4086(3) 0.0140(4) 0.0489(19) Uani 1 1 d . . . C20 C 1.1493(4) 0.4101(3) -0.0539(3) 0.0407(17) Uani 1 1 d . . . C21 C 1.0688(4) 0.4052(3) -0.0747(4) 0.0418(17) Uani 1 1 d . . . C22 C 1.0169(3) 0.4095(3) -0.1448(3) 0.0431(17) Uani 1 1 d . . . H7 H 1.0311 0.4221 -0.1866 0.052 Uiso 1 1 calc R . . C23 C 0.9447(3) 0.3928(3) -0.1414(3) 0.0389(16) Uani 1 1 d . . . H8 H 0.8992 0.3902 -0.1804 0.047 Uiso 1 1 calc R . . C24 C 0.9497(4) 0.3795(3) -0.0670(4) 0.0451(18) Uani 1 1 d . . . C25 C 0.8873(4) 0.3479(3) -0.0468(4) 0.0381(17) Uani 1 1 d . . . C26 C 0.8854(3) 0.3395(4) 0.0263(4) 0.0471(19) Uani 1 1 d . . . C27 C 0.9341(3) 0.3740(3) 0.1003(3) 0.0429(17) Uani 1 1 d . . . H9 H 0.9796 0.4074 0.1123 0.052 Uiso 1 1 calc R . . C28 C 0.8992(3) 0.3471(3) 0.1463(3) 0.0442(17) Uani 1 1 d . . . H10 H 0.9156 0.3600 0.1986 0.053 Uiso 1 1 calc R . . C29 C 0.8323(3) 0.2950(3) 0.1050(4) 0.0398(17) Uani 1 1 d . . . C30 C 0.7740(3) 0.2571(3) 0.1245(3) 0.0373(16) Uani 1 1 d . . . C31 C 0.8175(3) 0.2508(4) 0.4539(4) 0.052(2) Uani 1 1 d . . . C32 C 0.7869(3) 0.1840(4) 0.4670(3) 0.0461(18) Uani 1 1 d . . . C33 C 0.7599(4) 0.1792(5) 0.5270(3) 0.054(2) Uani 1 1 d . . . C34 C 0.7601(4) 0.2426(5) 0.5753(4) 0.063(2) Uani 1 1 d . . . C35 C 0.7915(4) 0.3113(5) 0.5658(4) 0.064(2) Uani 1 1 d . . . C36 C 0.8175(4) 0.3130(4) 0.5044(4) 0.0487(19) Uani 1 1 d . . . C37 C 1.1807(4) 0.3509(4) 0.4369(3) 0.0411(17) Uani 1 1 d . . . C38 C 1.1821(4) 0.4154(4) 0.4868(4) 0.0435(18) Uani 1 1 d . . . C39 C 1.2460(4) 0.4505(4) 0.5379(4) 0.0498(19) Uani 1 1 d . . . C40 C 1.3137(4) 0.4231(4) 0.5445(4) 0.057(2) Uani 1 1 d . . . C41 C 1.3162(4) 0.3554(5) 0.4981(4) 0.057(2) Uani 1 1 d . . . C42 C 1.2509(4) 0.3224(4) 0.4460(3) 0.0492(19) Uani 1 1 d . . . C43 C 1.2864(3) 0.4574(4) 0.2687(3) 0.0432(19) Uani 1 1 d . . . C44 C 1.3363(4) 0.4266(3) 0.3212(4) 0.044(2) Uani 1 1 d . . . C45 C 1.3955(3) 0.4671(4) 0.3771(3) 0.0410(17) Uani 1 1 d . . . C46 C 1.4055(4) 0.5432(5) 0.3814(4) 0.055(2) Uani 1 1 d . . . C47 C 1.3548(4) 0.5758(4) 0.3316(4) 0.053(2) Uani 1 1 d . . . C48 C 1.2964(4) 0.5334(4) 0.2759(4) 0.048(2) Uani 1 1 d . . . C49 C 1.1823(3) 0.4182(4) -0.1188(3) 0.0393(17) Uani 1 1 d . . . C50 C 1.1808(3) 0.3524(4) -0.1688(4) 0.051(2) Uani 1 1 d . . . C51 C 1.2089(4) 0.3570(4) -0.2279(4) 0.056(2) Uani 1 1 d . . . C52 C 1.2388(4) 0.4222(5) -0.2417(4) 0.054(2) Uani 1 1 d . . . C53 C 1.2395(4) 0.4867(4) -0.1944(4) 0.054(2) Uani 1 1 d . . . C54 C 1.2129(4) 0.4848(4) -0.1338(4) 0.053(2) Uani 1 1 d . . . C55 C 0.8171(4) 0.3144(4) -0.1072(3) 0.0422(17) Uani 1 1 d . . . C56 C 0.8179(4) 0.2492(4) -0.1542(4) 0.0507(19) Uani 1 1 d . . . C57 C 0.7528(4) 0.2148(4) -0.2055(4) 0.055(2) Uani 1 1 d . . . C58 C 0.6855(4) 0.2443(4) -0.2110(4) 0.053(2) Uani 1 1 d . . . C59 C 0.6830(4) 0.3080(4) -0.1648(4) 0.053(2) Uani 1 1 d . . . C60 C 0.7481(4) 0.3427(4) -0.1139(4) 0.0478(19) Uani 1 1 d . . . C61 C 0.7106(3) 0.2145(4) 0.0622(3) 0.0373(17) Uani 1 1 d . . . C62 C 0.7035(3) 0.1385(5) 0.0577(3) 0.046(2) Uani 1 1 d . . . C63 C 0.6467(4) 0.0920(4) 0.0044(4) 0.053(2) Uani 1 1 d . . . C64 C 0.5958(4) 0.1216(5) -0.0474(4) 0.052(2) Uani 1 1 d . . . C65 C 0.6016(4) 0.1958(5) -0.0442(4) 0.048(2) Uani 1 1 d . . . C66 C 0.6598(3) 0.2439(4) 0.0087(3) 0.0405(18) Uani 1 1 d . . . C67 C 0.6189(4) 0.2432(4) 0.1696(3) 0.0409(17) Uani 1 1 d . . . C68 C 0.5692(4) 0.1777(4) 0.1546(3) 0.057(2) Uani 1 1 d . . . H11 H 0.5841 0.1357 0.1768 0.069 Uiso 1 1 calc R . . C69 C 0.4964(4) 0.1760(4) 0.1055(3) 0.056(2) Uani 1 1 d . . . H12 H 0.4622 0.1315 0.0938 0.067 Uiso 1 1 calc R . . C70 C 0.4730(4) 0.2359(4) 0.0742(3) 0.0499(19) Uani 1 1 d . . . H13 H 0.4231 0.2330 0.0417 0.060 Uiso 1 1 calc R . . C71 C 0.5221(3) 0.3011(4) 0.0899(3) 0.058(2) Uani 1 1 d . . . H14 H 0.5067 0.3433 0.0684 0.070 Uiso 1 1 calc R . . C72 C 0.5948(4) 0.3032(4) 0.1382(3) 0.0501(19) Uani 1 1 d . . . H15 H 0.6287 0.3479 0.1496 0.060 Uiso 1 1 calc R . . C73 C 0.6670(3) 0.2540(4) 0.3422(3) 0.0385(16) Uani 1 1 d . . . C74 C 0.6276(3) 0.1919(4) 0.3538(3) 0.0532(19) Uani 1 1 d . . . H16 H 0.6339 0.1441 0.3304 0.064 Uiso 1 1 calc R . . C75 C 0.5795(3) 0.1975(4) 0.3981(4) 0.059(2) Uani 1 1 d . . . H17 H 0.5536 0.1537 0.4060 0.071 Uiso 1 1 calc R . . C76 C 0.5679(3) 0.2682(5) 0.4325(3) 0.062(2) Uani 1 1 d . . . H18 H 0.5352 0.2725 0.4641 0.075 Uiso 1 1 calc R . . C77 C 0.6053(4) 0.3308(4) 0.4188(3) 0.061(2) Uani 1 1 d . . . H19 H 0.5968 0.3789 0.4396 0.073 Uiso 1 1 calc R . . C78 C 0.6550(4) 0.3237(4) 0.3751(3) 0.058(2) Uani 1 1 d . . . H20 H 0.6815 0.3672 0.3673 0.070 Uiso 1 1 calc R . . C79 C 1.3816(4) 0.4240(4) 0.1637(3) 0.0441(18) Uani 1 1 d . . . C80 C 1.4062(4) 0.3649(4) 0.1941(3) 0.0486(19) Uani 1 1 d . . . H21 H 1.3734 0.3194 0.1819 0.058 Uiso 1 1 calc R . . C81 C 1.4799(4) 0.3688(4) 0.2437(3) 0.057(2) Uani 1 1 d . . . H22 H 1.4962 0.3276 0.2667 0.068 Uiso 1 1 calc R . . C82 C 1.5273(4) 0.4349(4) 0.2575(3) 0.061(2) Uani 1 1 d . . . H23 H 1.5779 0.4388 0.2890 0.073 Uiso 1 1 calc R . . C83 C 1.5024(4) 0.4941(4) 0.2265(4) 0.056(2) Uani 1 1 d . . . H24 H 1.5352 0.5395 0.2378 0.067 Uiso 1 1 calc R . . C84 C 1.4293(4) 0.4895(4) 0.1784(3) 0.057(2) Uani 1 1 d . . . H25 H 1.4127 0.5309 0.1561 0.068 Uiso 1 1 calc R . . C85 C 1.3351(3) 0.4130(4) -0.0097(3) 0.0365(16) Uani 1 1 d . . . C86 C 1.3442(3) 0.3429(4) -0.0431(3) 0.056(2) Uani 1 1 d . . . H26 H 1.3159 0.2999 -0.0366 0.068 Uiso 1 1 calc R . . C87 C 1.3946(4) 0.3363(5) -0.0860(4) 0.070(2) Uani 1 1 d . . . H27 H 1.4031 0.2881 -0.1066 0.085 Uiso 1 1 calc R . . C88 C 1.4320(4) 0.3966(5) -0.0992(4) 0.066(2) Uani 1 1 d . . . H28 H 1.4653 0.3903 -0.1300 0.079 Uiso 1 1 calc R . . C89 C 1.4228(3) 0.4681(4) -0.0685(4) 0.061(2) Uani 1 1 d . . . H29 H 1.4491 0.5105 -0.0784 0.073 Uiso 1 1 calc R . . C90 C 1.3736(3) 0.4760(4) -0.0224(3) 0.0512(19) Uani 1 1 d . . . H30 H 1.3668 0.5242 -0.0002 0.061 Uiso 1 1 calc R . . F31 F 0.25473(16) -0.07430(19) 0.73654(16) 0.0532(10) Uani 1 1 d . . . F32 F 0.38310(19) -0.0064(2) 0.83756(18) 0.0659(11) Uani 1 1 d . . . F33 F 0.37886(19) 0.12202(19) 0.92727(18) 0.0712(12) Uani 1 1 d . . . F34 F 0.2444(2) 0.1802(2) 0.91657(19) 0.0780(12) Uani 1 1 d . . . F35 F 0.11548(19) 0.11375(18) 0.81587(17) 0.0595(10) Uani 1 1 d . . . F36 F 0.33388(18) 0.0163(2) 0.65495(18) 0.0577(10) Uani 1 1 d . . . F37 F 0.44564(19) 0.1033(2) 0.76047(18) 0.0657(11) Uani 1 1 d . . . F38 F 0.46057(19) 0.2534(2) 0.76729(18) 0.0647(11) Uani 1 1 d . . . F39 F 0.36178(19) 0.3168(2) 0.66689(18) 0.0669(11) Uani 1 1 d . . . F40 F 0.24828(18) 0.23161(18) 0.56154(17) 0.0545(10) Uani 1 1 d . . . F41 F -0.1519(2) 0.0462(2) 0.82828(18) 0.0704(12) Uani 1 1 d . . . F42 F -0.2082(2) 0.0389(2) 0.9450(2) 0.0950(15) Uani 1 1 d . . . F43 F -0.2671(2) -0.0942(2) 0.9659(2) 0.0842(13) Uani 1 1 d . . . F44 F -0.2677(2) -0.2194(2) 0.87140(19) 0.0769(12) Uani 1 1 d . . . F45 F -0.21698(18) -0.21244(19) 0.75123(18) 0.0599(10) Uani 1 1 d . . . N7 N -0.0249(3) -0.0570(3) 0.6923(2) 0.0404(13) Uani 1 1 d . . . N8 N 0.1743(3) 0.0422(3) 0.6357(3) 0.0414(14) Uani 1 1 d . . . N9 N 0.1700(3) 0.0704(3) 0.4077(3) 0.0438(14) Uani 1 1 d . . . H40 H 0.1216 0.0632 0.4074 0.053 Uiso 1 1 calc R . . C91 C -0.0673(4) -0.0732(3) 0.7380(4) 0.0436(18) Uani 1 1 d . . . C92 C -0.0185(3) -0.0767(3) 0.8106(3) 0.0459(18) Uani 1 1 d . . . H31 H -0.0346 -0.0883 0.8518 0.055 Uiso 1 1 calc R . . C93 C 0.0546(3) -0.0603(3) 0.8087(3) 0.0462(18) Uani 1 1 d . . . H32 H 0.0997 -0.0595 0.8478 0.055 Uiso 1 1 calc R . . C94 C 0.0505(3) -0.0442(3) 0.7348(3) 0.0354(16) Uani 1 1 d . . . C95 C 0.1109(3) -0.0144(3) 0.7114(3) 0.0360(16) Uani 1 1 d . . . C96 C 0.1160(4) -0.0049(4) 0.6400(4) 0.0429(17) Uani 1 1 d . . . C97 C 0.0675(3) -0.0399(3) 0.5664(3) 0.0512(19) Uani 1 1 d . . . H33 H 0.0223 -0.0737 0.5555 0.061 Uiso 1 1 calc R . . C98 C 0.1007(3) -0.0139(3) 0.5179(3) 0.0406(16) Uani 1 1 d . . . H34 H 0.0842 -0.0270 0.4656 0.049 Uiso 1 1 calc R . . C99 C 0.1658(4) 0.0373(3) 0.5607(4) 0.0425(17) Uani 1 1 d . . . C100 C 0.2264(3) 0.0757(3) 0.5426(4) 0.0428(18) Uani 1 1 d . . . C101 C 0.2293(3) 0.0770(3) 0.4672(4) 0.0409(17) Uani 1 1 d . . . C102 C 0.3009(3) 0.0884(3) 0.4470(4) 0.0381(16) Uani 1 1 d . . . C103 C 0.2792(4) 0.0837(3) 0.3704(4) 0.0518(19) Uani 1 1 d . . . C104 C 0.1957(4) 0.0765(3) 0.3473(4) 0.0441(18) Uani 1 1 d . . . C105 C -0.1482(4) -0.0777(3) 0.7224(3) 0.0461(19) Uani 1 1 d . . . C106 C 0.1822(4) 0.0172(3) 0.7726(3) 0.0384(17) Uani 1 1 d . . . C107 C 0.2507(4) -0.0112(4) 0.7795(3) 0.0403(17) Uani 1 1 d . . . C108 C 0.3170(4) 0.0246(4) 0.8311(3) 0.0457(18) Uani 1 1 d . . . C109 C 0.3149(4) 0.0880(4) 0.8760(4) 0.057(2) Uani 1 1 d . . . C110 C 0.2476(5) 0.1174(4) 0.8719(4) 0.060(2) Uani 1 1 d . . . C111 C 0.1815(4) 0.0805(4) 0.8197(4) 0.0402(17) Uani 1 1 d . . . C112 C 0.2882(4) 0.1218(4) 0.6033(3) 0.0402(17) Uani 1 1 d . . . C113 C 0.3390(4) 0.0887(4) 0.6565(3) 0.0452(18) Uani 1 1 d . . . C114 C 0.3952(4) 0.1342(4) 0.7112(4) 0.0469(19) Uani 1 1 d . . . C115 C 0.4042(3) 0.2085(4) 0.7143(3) 0.0420(18) Uani 1 1 d . . . C116 C 0.3560(4) 0.2432(4) 0.6642(4) 0.0424(18) Uani 1 1 d . . . C117 C 0.2985(3) 0.1980(4) 0.6096(3) 0.0387(17) Uani 1 1 d . . . C118 C -0.1808(3) -0.0819(4) 0.7854(4) 0.053(2) Uani 1 1 d . . . C119 C -0.1808(4) -0.0197(4) 0.8388(4) 0.052(2) Uani 1 1 d . . . C120 C -0.2098(4) -0.0240(5) 0.8979(4) 0.063(2) Uani 1 1 d . . . C121 C -0.2394(4) -0.0918(5) 0.9079(4) 0.057(2) Uani 1 1 d . . . C122 C -0.2397(4) -0.1554(4) 0.8564(5) 0.059(2) Uani 1 1 d . . . C123 C -0.2110(3) -0.1477(5) 0.7988(4) 0.051(2) Uani 1 1 d . . . C124 C 0.3789(4) 0.0929(4) 0.4954(3) 0.0466(19) Uani 1 1 d . . . C125 C 0.4039(4) 0.0320(4) 0.5260(3) 0.057(2) Uani 1 1 d . . . H35 H 0.3704 -0.0131 0.5126 0.068 Uiso 1 1 calc R . . C126 C 0.4757(4) 0.0331(4) 0.5755(4) 0.063(2) Uani 1 1 d . . . H36 H 0.4902 -0.0093 0.5973 0.075 Uiso 1 1 calc R . . C127 C 0.5259(4) 0.0992(5) 0.5919(3) 0.063(2) Uani 1 1 d . . . H37 H 0.5753 0.1020 0.6253 0.076 Uiso 1 1 calc R . . C128 C 0.5038(4) 0.1598(4) 0.5599(4) 0.064(2) Uani 1 1 d . . . H38 H 0.5381 0.2041 0.5702 0.077 Uiso 1 1 calc R . . C129 C 0.4310(4) 0.1558(4) 0.5125(3) 0.053(2) Uani 1 1 d . . . H39 H 0.4163 0.1982 0.4908 0.064 Uiso 1 1 calc R . . C130 C 0.3333(3) 0.0798(4) 0.3248(3) 0.0454(18) Uani 1 1 d . . . C131 C 0.3446(3) 0.0104(4) 0.2922(3) 0.0433(17) Uani 1 1 d . . . H41 H 0.3173 -0.0324 0.3003 0.052 Uiso 1 1 calc R . . C132 C 0.3947(4) 0.0007(4) 0.2479(3) 0.059(2) Uani 1 1 d . . . H42 H 0.4024 -0.0477 0.2270 0.071 Uiso 1 1 calc R . . C133 C 0.4331(3) 0.0641(5) 0.2351(3) 0.059(2) Uani 1 1 d . . . H43 H 0.4676 0.0592 0.2052 0.071 Uiso 1 1 calc R . . C134 C 0.4211(4) 0.1335(4) 0.2655(3) 0.058(2) Uani 1 1 d . . . H44 H 0.4454 0.1764 0.2543 0.069 Uiso 1 1 calc R . . C135 C 0.3740(3) 0.1424(4) 0.3126(3) 0.0487(18) Uani 1 1 d . . . H45 H 0.3696 0.1908 0.3362 0.058 Uiso 1 1 calc R . . C1S C 0.0155(4) 0.4822(4) 0.6280(4) 0.076(2) Uani 1 1 d . . . H46 H -0.0163 0.4763 0.5756 0.091 Uiso 1 1 calc R . . Cl1S Cl -0.04300(12) 0.50063(12) 0.68636(11) 0.1130(8) Uani 1 1 d . . . Cl2S Cl 0.08712(17) 0.55214(13) 0.64301(14) 0.1590(12) Uani 1 1 d . . . Cl3S Cl 0.05344(15) 0.39926(13) 0.64244(14) 0.1555(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.069(3) 0.046(2) 0.058(2) 0.0030(19) 0.028(2) -0.005(2) F2 0.092(3) 0.064(3) 0.081(3) 0.012(2) 0.047(2) -0.023(2) F3 0.099(3) 0.107(3) 0.053(3) 0.016(2) 0.051(2) 0.012(2) F4 0.142(4) 0.084(3) 0.073(3) -0.019(2) 0.065(3) 0.008(3) F5 0.109(3) 0.054(3) 0.070(3) 0.003(2) 0.047(2) -0.003(2) F6 0.075(3) 0.058(3) 0.056(2) 0.0114(19) 0.013(2) 0.019(2) F7 0.085(3) 0.060(3) 0.069(3) -0.011(2) -0.002(2) -0.007(2) F8 0.056(3) 0.076(3) 0.065(3) 0.010(2) -0.009(2) -0.024(2) F9 0.049(3) 0.096(3) 0.065(3) 0.023(2) 0.004(2) 0.006(2) F10 0.045(2) 0.065(3) 0.050(2) 0.0017(19) 0.0143(19) 0.0023(19) F11 0.038(2) 0.075(3) 0.044(2) 0.016(2) 0.0002(17) 0.001(2) F12 0.045(2) 0.105(3) 0.039(2) 0.011(2) -0.0161(18) 0.002(2) F13 0.045(2) 0.081(3) 0.054(2) 0.002(2) 0.003(2) -0.011(2) F14 0.073(3) 0.062(3) 0.063(3) 0.003(2) 0.011(2) -0.004(2) F15 0.049(3) 0.071(3) 0.051(3) 0.027(2) 0.0051(19) 0.002(2) F16 0.100(3) 0.058(3) 0.066(3) 0.000(2) 0.039(2) -0.011(2) F17 0.119(3) 0.074(3) 0.077(3) 0.000(2) 0.055(3) 0.009(3) F18 0.096(3) 0.106(3) 0.060(3) 0.016(2) 0.047(2) 0.012(3) F19 0.081(3) 0.076(3) 0.069(3) 0.020(2) 0.030(2) -0.022(2) F20 0.061(2) 0.050(2) 0.052(2) -0.0009(19) 0.0135(19) -0.0128(19) F21 0.046(2) 0.070(3) 0.064(3) -0.004(2) 0.003(2) 0.010(2) F22 0.090(3) 0.058(3) 0.052(2) -0.006(2) 0.002(2) -0.006(2) F23 0.055(3) 0.090(3) 0.057(3) 0.006(2) -0.012(2) -0.024(2) F24 0.035(2) 0.092(3) 0.069(3) 0.010(2) 0.007(2) 0.004(2) F25 0.039(2) 0.070(3) 0.054(2) 0.015(2) 0.0107(18) 0.0029(19) F26 0.047(2) 0.065(3) 0.046(2) 0.0036(19) 0.0071(19) -0.0012(19) F27 0.059(3) 0.058(3) 0.069(3) 0.000(2) 0.009(2) -0.015(2) F28 0.048(2) 0.088(3) 0.045(2) -0.007(2) -0.0064(19) -0.015(2) F29 0.059(3) 0.077(3) 0.056(3) 0.021(2) 0.000(2) -0.001(2) F30 0.050(2) 0.059(3) 0.053(2) 0.016(2) 0.0080(18) -0.008(2) N1 0.025(3) 0.069(4) 0.034(3) 0.019(3) 0.012(3) 0.003(3) N2 0.028(3) 0.061(4) 0.041(4) 0.002(3) 0.011(3) -0.004(3) N3 0.035(3) 0.057(4) 0.030(3) -0.001(3) 0.018(3) -0.015(3) N4 0.022(3) 0.073(4) 0.026(3) -0.001(3) -0.005(3) -0.006(3) N5 0.037(3) 0.048(3) 0.035(3) 0.004(3) 0.006(3) 0.000(3) N6 0.024(3) 0.066(4) 0.025(3) 0.003(3) 0.010(3) 0.005(3) C1 0.025(4) 0.068(5) 0.042(5) 0.003(4) -0.013(4) 0.000(4) C2 0.032(4) 0.063(5) 0.034(4) 0.010(4) 0.010(4) -0.002(4) C3 0.034(4) 0.042(4) 0.023(4) 0.003(3) 0.012(3) -0.001(3) C4 0.017(4) 0.041(4) 0.048(5) 0.005(3) -0.003(3) -0.003(3) C5 0.014(4) 0.062(5) 0.049(5) 0.002(4) 0.004(3) -0.009(3) C6 0.035(4) 0.052(4) 0.025(4) 0.005(3) -0.006(3) -0.005(3) C7 0.058(5) 0.065(5) 0.039(5) 0.011(4) 0.024(4) -0.005(4) C8 0.071(5) 0.043(4) 0.030(4) 0.013(3) 0.024(4) -0.006(4) C9 0.049(5) 0.053(5) 0.043(5) 0.016(4) 0.020(4) 0.000(4) C10 0.030(4) 0.056(5) 0.024(4) 0.011(3) 0.001(3) -0.009(3) C11 0.042(4) 0.038(4) 0.034(4) 0.008(3) 0.010(4) 0.005(3) C12 0.019(4) 0.065(5) 0.036(4) -0.005(4) -0.011(3) 0.000(3) C13 0.034(4) 0.082(6) 0.045(5) 0.022(4) 0.011(4) 0.011(4) C14 0.041(5) 0.054(5) 0.027(4) 0.013(4) 0.003(4) 0.006(4) C15 0.028(4) 0.037(4) 0.053(5) -0.008(3) 0.017(4) -0.018(3) C16 0.038(4) 0.050(4) 0.030(4) 0.008(3) 0.019(4) 0.001(3) C17 0.044(5) 0.045(4) 0.048(5) -0.001(4) 0.018(4) -0.003(4) C18 0.027(4) 0.044(4) 0.047(5) 0.005(4) -0.014(4) -0.018(3) C19 0.042(5) 0.059(5) 0.035(5) -0.007(4) 0.005(4) -0.017(4) C20 0.043(5) 0.041(4) 0.030(4) -0.005(3) 0.006(4) -0.007(3) C21 0.031(4) 0.060(5) 0.039(5) 0.013(4) 0.018(4) -0.005(4) C22 0.031(4) 0.062(5) 0.034(4) 0.016(3) 0.003(3) -0.007(3) C23 0.024(4) 0.059(4) 0.032(4) 0.006(3) 0.010(3) -0.011(3) C24 0.059(5) 0.040(4) 0.040(5) 0.010(3) 0.016(4) 0.008(4) C25 0.046(5) 0.038(4) 0.042(5) 0.013(3) 0.028(4) 0.007(3) C26 0.018(4) 0.063(5) 0.051(5) -0.010(4) 0.006(4) -0.001(3) C27 0.026(4) 0.053(4) 0.046(5) 0.006(4) 0.006(3) -0.004(3) C28 0.045(4) 0.047(4) 0.038(4) -0.002(3) 0.016(4) -0.012(3) C29 0.027(4) 0.048(4) 0.050(5) 0.001(4) 0.026(4) -0.007(3) C30 0.039(4) 0.055(5) 0.016(4) 0.016(3) -0.001(3) 0.006(3) C31 0.021(4) 0.089(6) 0.044(5) 0.002(4) 0.015(3) -0.016(4) C32 0.032(4) 0.066(5) 0.036(4) -0.006(4) 0.011(3) -0.001(4) C33 0.051(5) 0.096(6) 0.018(4) 0.008(4) 0.021(3) -0.007(4) C34 0.061(5) 0.098(7) 0.025(5) -0.003(5) 0.014(4) -0.008(5) C35 0.072(6) 0.077(6) 0.032(5) -0.020(5) 0.011(4) 0.012(5) C36 0.061(5) 0.048(5) 0.027(4) -0.017(4) 0.011(4) -0.013(4) C37 0.029(4) 0.058(5) 0.033(4) 0.013(4) 0.002(3) -0.006(4) C38 0.035(5) 0.055(5) 0.042(5) 0.022(4) 0.005(4) 0.005(4) C39 0.056(5) 0.058(5) 0.031(4) 0.003(4) 0.005(4) 0.013(5) C40 0.037(5) 0.044(5) 0.076(6) 0.010(4) -0.006(4) -0.018(4) C41 0.035(5) 0.079(6) 0.068(6) 0.051(5) 0.013(4) 0.016(5) C42 0.034(5) 0.064(5) 0.036(5) -0.004(4) -0.008(4) -0.001(4) C43 0.023(4) 0.091(6) 0.025(4) 0.030(4) 0.010(3) 0.017(4) C44 0.034(4) 0.023(4) 0.070(6) -0.014(4) 0.023(4) -0.022(3) C45 0.014(4) 0.068(5) 0.033(4) 0.014(4) -0.007(3) -0.008(4) C46 0.028(5) 0.078(6) 0.050(5) 0.006(5) 0.000(4) -0.007(4) C47 0.037(5) 0.064(6) 0.054(5) -0.006(5) 0.018(4) -0.010(5) C48 0.069(6) 0.037(5) 0.048(5) 0.009(4) 0.034(4) 0.003(4) C49 0.040(4) 0.052(5) 0.014(3) -0.017(3) -0.003(3) 0.009(3) C50 0.029(4) 0.084(6) 0.047(5) 0.022(5) 0.022(4) -0.012(4) C51 0.073(5) 0.029(4) 0.076(6) 0.012(4) 0.032(5) 0.008(4) C52 0.043(5) 0.082(6) 0.040(5) 0.012(5) 0.015(4) 0.010(4) C53 0.040(4) 0.061(6) 0.065(6) 0.013(5) 0.023(4) -0.016(4) C54 0.047(5) 0.032(4) 0.077(6) 0.010(4) 0.016(4) -0.022(4) C55 0.032(4) 0.061(5) 0.025(4) 0.007(3) -0.004(3) -0.016(4) C56 0.058(6) 0.053(5) 0.037(5) -0.002(4) 0.012(4) 0.001(4) C57 0.038(5) 0.063(6) 0.058(6) 0.004(4) 0.004(4) 0.006(4) C58 0.055(6) 0.056(5) 0.039(5) 0.000(4) 0.004(4) -0.012(5) C59 0.031(5) 0.082(6) 0.045(5) 0.020(4) 0.003(4) -0.002(4) C60 0.036(5) 0.052(5) 0.060(5) 0.008(4) 0.022(4) 0.006(4) C61 0.030(4) 0.046(4) 0.033(4) 0.012(4) 0.004(3) -0.007(4) C62 0.026(4) 0.096(6) 0.011(4) 0.015(4) -0.007(3) 0.008(4) C63 0.041(5) 0.063(6) 0.050(5) 0.003(5) 0.012(4) -0.005(5) C64 0.027(4) 0.075(6) 0.038(5) -0.017(5) 0.002(3) -0.025(4) C65 0.028(4) 0.084(6) 0.029(5) 0.020(5) -0.002(3) -0.003(4) C66 0.018(4) 0.088(6) 0.022(4) 0.033(4) 0.003(3) 0.009(4) C67 0.032(4) 0.049(5) 0.039(4) 0.005(4) 0.008(4) 0.000(4) C68 0.060(5) 0.062(5) 0.049(5) 0.013(4) 0.013(4) -0.002(4) C69 0.043(5) 0.090(6) 0.032(4) 0.012(4) 0.011(4) -0.022(4) C70 0.041(4) 0.073(5) 0.041(4) 0.037(4) 0.009(3) -0.003(4) C71 0.017(4) 0.079(6) 0.066(5) 0.004(4) -0.002(4) -0.016(4) C72 0.053(5) 0.050(5) 0.042(5) -0.006(4) 0.009(4) 0.009(4) C73 0.033(4) 0.045(5) 0.035(4) 0.008(4) 0.008(3) -0.010(4) C74 0.045(5) 0.057(5) 0.062(5) 0.020(4) 0.017(4) 0.003(4) C75 0.045(5) 0.073(6) 0.051(5) 0.002(4) 0.013(4) -0.030(4) C76 0.032(4) 0.120(7) 0.033(4) 0.008(5) 0.015(3) -0.021(4) C77 0.059(5) 0.072(6) 0.060(5) -0.003(4) 0.039(4) -0.003(4) C78 0.057(5) 0.065(5) 0.050(5) 0.005(4) 0.016(4) -0.008(4) C79 0.020(4) 0.061(5) 0.040(4) 0.003(4) -0.005(3) -0.006(4) C80 0.032(4) 0.057(5) 0.056(5) 0.009(4) 0.011(4) 0.003(4) C81 0.041(5) 0.080(6) 0.046(5) 0.004(4) 0.006(4) 0.018(4) C82 0.039(5) 0.080(6) 0.052(5) -0.006(5) 0.007(4) -0.018(5) C83 0.047(5) 0.049(5) 0.064(5) 0.002(4) 0.009(4) -0.012(4) C84 0.033(5) 0.095(6) 0.036(4) 0.004(4) 0.004(4) -0.006(4) C85 0.020(4) 0.066(5) 0.024(4) 0.011(4) 0.007(3) -0.004(3) C86 0.051(5) 0.063(5) 0.051(5) -0.001(4) 0.016(4) -0.006(4) C87 0.059(6) 0.099(7) 0.053(5) -0.005(5) 0.023(4) 0.006(5) C88 0.069(6) 0.084(7) 0.048(5) 0.006(5) 0.024(4) 0.002(5) C89 0.046(5) 0.083(6) 0.060(5) 0.023(4) 0.023(4) -0.015(4) C90 0.041(4) 0.061(5) 0.049(5) 0.008(4) 0.014(4) -0.015(4) F31 0.047(2) 0.071(3) 0.035(2) -0.0035(19) 0.0047(17) 0.014(2) F32 0.031(2) 0.088(3) 0.071(3) 0.018(2) 0.000(2) 0.004(2) F33 0.053(3) 0.080(3) 0.055(3) 0.004(2) -0.021(2) -0.019(2) F34 0.098(3) 0.052(3) 0.063(3) -0.008(2) -0.003(2) -0.003(2) F35 0.064(3) 0.057(3) 0.051(2) 0.0006(18) 0.007(2) 0.017(2) F36 0.049(2) 0.051(2) 0.072(3) 0.015(2) 0.0134(19) 0.002(2) F37 0.047(2) 0.090(3) 0.051(2) 0.014(2) -0.0025(19) 0.001(2) F38 0.053(3) 0.081(3) 0.048(2) 0.004(2) 0.002(2) -0.010(2) F39 0.068(3) 0.057(3) 0.072(3) 0.004(2) 0.019(2) -0.006(2) F40 0.045(2) 0.061(3) 0.055(2) 0.0159(19) 0.0068(19) 0.0038(19) F41 0.101(3) 0.049(3) 0.061(3) 0.002(2) 0.028(2) -0.004(2) F42 0.148(4) 0.081(3) 0.067(3) -0.012(2) 0.062(3) 0.014(3) F43 0.092(3) 0.110(3) 0.068(3) 0.018(2) 0.054(3) 0.001(2) F44 0.090(3) 0.081(3) 0.066(3) 0.012(2) 0.040(2) -0.017(3) F45 0.062(2) 0.059(3) 0.051(2) -0.002(2) 0.012(2) -0.004(2) N7 0.032(3) 0.056(4) 0.034(3) 0.010(3) 0.010(3) -0.001(3) N8 0.036(3) 0.042(3) 0.043(4) 0.011(3) 0.006(3) 0.000(3) N9 0.022(3) 0.071(4) 0.041(4) 0.016(3) 0.014(3) -0.006(3) C91 0.033(4) 0.054(4) 0.034(5) -0.003(3) 0.001(4) -0.008(4) C92 0.031(4) 0.073(5) 0.028(4) 0.014(3) -0.001(3) 0.000(4) C93 0.023(4) 0.081(5) 0.024(4) 0.006(3) -0.010(3) 0.005(3) C94 0.018(4) 0.037(4) 0.039(4) -0.010(3) -0.001(3) -0.011(3) C95 0.017(4) 0.054(4) 0.032(4) 0.000(3) 0.003(3) -0.004(3) C96 0.046(5) 0.053(5) 0.030(4) 0.009(4) 0.007(4) 0.014(4) C97 0.037(4) 0.077(5) 0.037(4) 0.011(4) 0.009(4) -0.012(4) C98 0.032(4) 0.056(5) 0.027(4) 0.002(3) 0.002(3) -0.008(3) C99 0.031(4) 0.055(5) 0.033(4) 0.004(4) -0.004(3) 0.007(3) C100 0.029(4) 0.061(5) 0.044(5) 0.010(4) 0.022(4) -0.003(3) C101 0.023(4) 0.055(4) 0.046(5) 0.004(4) 0.015(4) -0.004(3) C102 0.025(4) 0.049(4) 0.039(4) 0.010(3) 0.006(4) -0.003(3) C103 0.047(5) 0.074(5) 0.036(5) 0.001(4) 0.018(4) 0.007(4) C104 0.037(5) 0.052(4) 0.046(5) -0.008(4) 0.031(4) -0.014(3) C105 0.057(5) 0.060(5) 0.018(4) 0.006(3) 0.007(4) -0.002(4) C106 0.052(5) 0.036(4) 0.032(4) 0.004(3) 0.020(4) 0.006(4) C107 0.039(5) 0.046(5) 0.033(4) -0.001(3) 0.011(4) -0.008(4) C108 0.031(5) 0.068(5) 0.031(4) -0.003(4) 0.006(4) -0.005(4) C109 0.040(5) 0.086(6) 0.029(4) 0.001(4) -0.009(4) -0.008(5) C110 0.077(6) 0.034(5) 0.057(5) -0.013(4) 0.018(5) -0.024(4) C111 0.033(4) 0.036(4) 0.050(5) 0.010(4) 0.007(4) 0.003(4) C112 0.042(4) 0.049(5) 0.026(4) 0.005(4) 0.009(3) -0.019(4) C113 0.070(5) 0.051(5) 0.014(4) 0.011(4) 0.008(4) 0.002(5) C114 0.049(5) 0.047(5) 0.037(5) -0.003(4) 0.004(4) 0.009(4) C115 0.027(4) 0.064(6) 0.026(4) -0.005(4) 0.002(3) -0.009(4) C116 0.042(5) 0.039(5) 0.044(5) 0.008(4) 0.011(4) -0.009(4) C117 0.016(4) 0.050(5) 0.046(5) 0.010(4) 0.001(3) -0.001(3) C118 0.036(4) 0.061(5) 0.058(5) 0.011(4) 0.012(4) -0.023(4) C119 0.066(5) 0.024(4) 0.063(6) 0.002(4) 0.017(4) 0.005(4) C120 0.059(5) 0.082(7) 0.053(5) -0.005(5) 0.035(4) -0.005(5) C121 0.046(5) 0.086(7) 0.049(5) 0.021(5) 0.023(4) 0.003(5) C122 0.046(5) 0.047(5) 0.075(6) 0.005(5) 0.009(4) -0.009(4) C123 0.023(4) 0.097(7) 0.028(4) -0.003(4) 0.003(3) 0.007(4) C124 0.041(5) 0.076(6) 0.029(4) 0.007(4) 0.025(4) -0.005(4) C125 0.035(5) 0.074(6) 0.047(5) 0.008(4) -0.006(4) -0.015(4) C126 0.061(6) 0.064(6) 0.059(5) 0.007(4) 0.014(4) -0.005(5) C127 0.034(5) 0.115(7) 0.030(4) 0.001(5) -0.001(3) 0.005(5) C128 0.033(5) 0.104(7) 0.045(5) 0.015(4) 0.001(4) -0.024(5) C129 0.031(4) 0.075(5) 0.045(5) 0.008(4) 0.003(3) -0.022(4) C130 0.027(4) 0.056(5) 0.044(5) 0.002(4) 0.000(3) -0.001(4) C131 0.030(4) 0.060(5) 0.048(4) 0.017(4) 0.023(3) -0.002(3) C132 0.036(4) 0.079(6) 0.054(5) -0.003(4) 0.008(4) -0.005(4) C133 0.028(4) 0.094(6) 0.057(5) 0.004(5) 0.016(4) 0.017(4) C134 0.057(5) 0.072(6) 0.049(5) 0.014(4) 0.024(4) 0.000(4) C135 0.033(4) 0.064(5) 0.042(4) 0.004(4) 0.003(3) -0.009(4) C1S 0.100(6) 0.072(5) 0.082(5) 0.031(4) 0.042(5) 0.080(5) Cl1S 0.1274(19) 0.136(2) 0.1092(17) 0.0474(15) 0.0661(15) 0.0536(16) Cl2S 0.247(3) 0.0709(16) 0.206(3) 0.0048(17) 0.160(3) -0.0086(19) Cl3S 0.175(3) 0.100(2) 0.174(2) -0.0219(17) 0.034(2) 0.0429(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 C32 1.355(6) . ? F2 C33 1.347(7) . ? F3 C34 1.344(7) . ? F4 C35 1.319(7) . ? F5 C36 1.341(7) . ? F6 C38 1.365(6) . ? F7 C39 1.363(6) . ? F8 C40 1.341(6) . ? F9 C41 1.339(6) . ? F10 C42 1.338(6) . ? F11 C44 1.360(6) . ? F12 C45 1.357(6) . ? F13 C46 1.333(7) . ? F14 C47 1.348(7) . ? F15 C48 1.342(7) . ? F16 C50 1.330(7) . ? F17 C51 1.376(7) . ? F18 C52 1.338(6) . ? F19 C53 1.353(7) . ? F20 C54 1.334(7) . ? F21 C56 1.354(7) . ? F22 C57 1.333(7) . ? F23 C58 1.322(6) . ? F24 C59 1.353(7) . ? F25 C60 1.356(6) . ? F26 C62 1.354(6) . ? F27 C63 1.354(7) . ? F28 C64 1.329(6) . ? F29 C65 1.350(6) . ? F30 C66 1.313(7) . ? N1 C1 1.343(6) . ? N1 C4 1.388(6) . ? N1 H1 0.8800 . ? N2 C6 1.370(6) . ? N2 C9 1.384(7) . ? N3 C14 1.357(6) . ? N3 C11 1.363(6) . ? N4 C16 1.357(6) . ? N4 C19 1.382(7) . ? N4 H2 0.8800 . ? N5 C24 1.376(7) . ? N5 C21 1.392(6) . ? N6 C26 1.360(6) . ? N6 C29 1.387(6) . ? C1 C30 1.415(7) . ? C1 C2 1.447(7) . ? C2 C3 1.390(7) . ? C2 C67 1.503(7) . ? C3 C4 1.452(7) . ? C3 C73 1.496(7) . ? C4 C5 1.398(7) . ? C5 C6 1.403(7) . ? C5 C31 1.489(7) . ? C6 C7 1.476(7) . ? C7 C8 1.362(7) . ? C7 H3 0.9500 . ? C8 C9 1.434(7) . ? C8 H4 0.9500 . ? C9 C10 1.406(7) . ? C10 C11 1.415(7) . ? C10 C37 1.484(7) . ? C11 C12 1.466(7) . ? C12 C13 1.359(7) . ? C12 H5 0.9500 . ? C13 C14 1.485(7) . ? C13 H6 0.9500 . ? C14 C15 1.368(7) . ? C15 C16 1.448(7) . ? C15 C43 1.520(7) . ? C16 C17 1.439(7) . ? C17 C18 1.385(7) . ? C17 C79 1.524(8) . ? C18 C19 1.433(7) . ? C18 C85 1.495(8) . ? C19 C20 1.375(7) . ? C20 C21 1.408(7) . ? C20 C49 1.529(7) . ? C21 C22 1.437(7) . ? C22 C23 1.348(6) . ? C22 H7 0.9500 . ? C23 C24 1.451(7) . ? C23 H8 0.9500 . ? C24 C25 1.405(7) . ? C25 C26 1.430(7) . ? C25 C55 1.500(7) . ? C26 C27 1.476(7) . ? C27 C28 1.334(7) . ? C27 H9 0.9500 . ? C28 C29 1.460(7) . ? C28 H10 0.9500 . ? C29 C30 1.385(7) . ? C30 C61 1.495(7) . ? C31 C36 1.378(8) . ? C31 C32 1.387(8) . ? C32 C33 1.367(7) . ? C33 C34 1.370(8) . ? C34 C35 1.397(9) . ? C35 C36 1.373(8) . ? C37 C42 1.392(7) . ? C37 C38 1.395(8) . ? C38 C39 1.355(7) . ? C39 C40 1.346(8) . ? C40 C41 1.421(9) . ? C41 C42 1.367(8) . ? C43 C48 1.370(8) . ? C43 C44 1.378(8) . ? C44 C45 1.380(7) . ? C45 C46 1.375(8) . ? C46 C47 1.375(8) . ? C47 C48 1.383(8) . ? C49 C54 1.399(8) . ? C49 C50 1.415(8) . ? C50 C51 1.361(8) . ? C51 C52 1.362(8) . ? C52 C53 1.372(8) . ? C53 C54 1.366(8) . ? C55 C60 1.375(8) . ? C55 C56 1.385(8) . ? C56 C57 1.367(8) . ? C57 C58 1.359(8) . ? C58 C59 1.364(8) . ? C59 C60 1.365(8) . ? C61 C62 1.375(8) . ? C61 C66 1.384(7) . ? C62 C63 1.378(8) . ? C63 C64 1.367(8) . ? C64 C65 1.342(8) . ? C65 C66 1.402(8) . ? C67 C72 1.368(8) . ? C67 C68 1.396(7) . ? C68 C69 1.404(7) . ? C68 H11 0.9500 . ? C69 C70 1.361(8) . ? C69 H12 0.9500 . ? C70 C71 1.383(7) . ? C70 H13 0.9500 . ? C71 C72 1.394(7) . ? C71 H14 0.9500 . ? C72 H15 0.9500 . ? C73 C74 1.374(7) . ? C73 C78 1.393(7) . ? C74 C75 1.364(7) . ? C74 H16 0.9500 . ? C75 C76 1.415(8) . ? C75 H17 0.9500 . ? C76 C77 1.380(8) . ? C76 H18 0.9500 . ? C77 C78 1.379(7) . ? C77 H19 0.9500 . ? C78 H20 0.9500 . ? C79 C80 1.347(8) . ? C79 C84 1.376(8) . ? C80 C81 1.415(7) . ? C80 H21 0.9500 . ? C81 C82 1.385(8) . ? C81 H22 0.9500 . ? C82 C83 1.356(8) . ? C82 H23 0.9500 . ? C83 C84 1.394(7) . ? C83 H24 0.9500 . ? C84 H25 0.9500 . ? C85 C86 1.385(7) . ? C85 C90 1.390(7) . ? C86 C87 1.379(8) . ? C86 H26 0.9500 . ? C87 C88 1.342(8) . ? C87 H27 0.9500 . ? C88 C89 1.390(8) . ? C88 H28 0.9500 . ? C89 C90 1.408(7) . ? C89 H29 0.9500 . ? C90 H30 0.9500 . ? F31 C107 1.332(6) . ? F32 C108 1.350(6) . ? F33 C109 1.351(6) . ? F34 C110 1.340(7) . ? F35 C111 1.375(6) . ? F36 C113 1.314(6) . ? F37 C114 1.348(6) . ? F38 C115 1.360(6) . ? F39 C116 1.334(6) . ? F40 C117 1.361(6) . ? F41 C119 1.341(7) . ? F42 C120 1.343(7) . ? F43 C121 1.333(6) . ? F44 C122 1.340(7) . ? F45 C123 1.360(7) . ? N7 C91 1.353(7) . ? N7 C94 1.385(6) . ? N8 C96 1.345(7) . ? N8 C99 1.383(6) . ? N9 C101 1.329(6) . ? N9 C104 1.363(6) . ? N9 H40 0.8800 . ? C91 C105 1.419(7) . ? C91 C92 1.447(7) . ? C92 C93 1.355(7) . ? C92 H31 0.9500 . ? C93 C94 1.462(7) . ? C93 H32 0.9500 . ? C94 C95 1.394(7) . ? C95 C96 1.419(7) . ? C95 C106 1.512(7) . ? C96 C97 1.472(7) . ? C97 C98 1.349(7) . ? C97 H33 0.9500 . ? C98 C99 1.437(7) . ? C98 H34 0.9500 . ? C99 C100 1.410(7) . ? C100 C101 1.452(7) . ? C100 C112 1.490(7) . ? C101 C102 1.461(7) . ? C102 C103 1.396(7) . ? C102 C124 1.467(7) . ? C103 C104 1.460(7) . ? C103 C130 1.470(8) . ? C104 C105 1.385(7) 2_556 ? C105 C104 1.385(7) 2_556 ? C105 C118 1.478(8) . ? C106 C111 1.359(7) . ? C106 C107 1.365(7) . ? C107 C108 1.391(7) . ? C108 C109 1.345(8) . ? C109 C110 1.360(8) . ? C110 C111 1.400(8) . ? C112 C117 1.375(7) . ? C112 C113 1.418(7) . ? C113 C114 1.377(8) . ? C114 C115 1.345(8) . ? C115 C116 1.376(8) . ? C116 C117 1.387(7) . ? C118 C123 1.371(8) . ? C118 C119 1.409(8) . ? C119 C120 1.371(8) . ? C120 C121 1.374(9) . ? C121 C122 1.406(8) . ? C122 C123 1.350(8) . ? C124 C125 1.378(8) . ? C124 C129 1.381(7) . ? C125 C126 1.396(7) . ? C125 H35 0.9500 . ? C126 C127 1.407(8) . ? C126 H36 0.9500 . ? C127 C128 1.374(8) . ? C127 H37 0.9500 . ? C128 C129 1.385(7) . ? C128 H38 0.9500 . ? C129 H39 0.9500 . ? C130 C131 1.382(7) . ? C130 C135 1.400(7) . ? C131 C132 1.399(7) . ? C131 H41 0.9500 . ? C132 C133 1.395(8) . ? C132 H42 0.9500 . ? C133 C134 1.372(8) . ? C133 H43 0.9500 . ? C134 C135 1.392(7) . ? C134 H44 0.9500 . ? C135 H45 0.9500 . ? C1S Cl2S 1.696(7) . ? C1S Cl3S 1.736(6) . ? C1S Cl1S 1.744(6) . ? C1S H46 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 109.2(5) . . ? C1 N1 H1 125.4 . . ? C4 N1 H1 125.4 . . ? C6 N2 C9 106.1(5) . . ? C14 N3 C11 106.8(5) . . ? C16 N4 C19 106.6(5) . . ? C16 N4 H2 126.7 . . ? C19 N4 H2 126.7 . . ? C24 N5 C21 107.4(5) . . ? C26 N6 C29 106.2(5) . . ? N1 C1 C30 126.2(6) . . ? N1 C1 C2 110.0(6) . . ? C30 C1 C2 123.8(6) . . ? C3 C2 C1 105.6(6) . . ? C3 C2 C67 125.6(6) . . ? C1 C2 C67 128.0(6) . . ? C2 C3 C4 107.8(6) . . ? C2 C3 C73 125.9(6) . . ? C4 C3 C73 126.1(5) . . ? N1 C4 C5 124.9(6) . . ? N1 C4 C3 107.0(5) . . ? C5 C4 C3 128.1(6) . . ? C4 C5 C6 120.7(6) . . ? C4 C5 C31 122.2(5) . . ? C6 C5 C31 116.9(6) . . ? N2 C6 C5 127.8(6) . . ? N2 C6 C7 109.2(5) . . ? C5 C6 C7 123.0(6) . . ? C8 C7 C6 106.8(6) . . ? C8 C7 H3 126.6 . . ? C6 C7 H3 126.6 . . ? C7 C8 C9 106.7(6) . . ? C7 C8 H4 126.6 . . ? C9 C8 H4 126.6 . . ? N2 C9 C10 125.9(6) . . ? N2 C9 C8 110.9(6) . . ? C10 C9 C8 122.9(7) . . ? C9 C10 C11 128.8(6) . . ? C9 C10 C37 118.7(6) . . ? C11 C10 C37 111.6(6) . . ? N3 C11 C10 118.4(6) . . ? N3 C11 C12 109.8(5) . . ? C10 C11 C12 131.7(6) . . ? C13 C12 C11 107.7(6) . . ? C13 C12 H5 126.1 . . ? C11 C12 H5 126.1 . . ? C12 C13 C14 104.7(6) . . ? C12 C13 H6 127.7 . . ? C14 C13 H6 127.7 . . ? N3 C14 C15 120.1(6) . . ? N3 C14 C13 111.0(6) . . ? C15 C14 C13 128.6(6) . . ? C14 C15 C16 129.8(6) . . ? C14 C15 C43 116.2(6) . . ? C16 C15 C43 113.8(5) . . ? N4 C16 C17 110.1(5) . . ? N4 C16 C15 123.5(6) . . ? C17 C16 C15 126.2(6) . . ? C18 C17 C16 107.0(6) . . ? C18 C17 C79 126.2(6) . . ? C16 C17 C79 126.5(6) . . ? C17 C18 C19 105.8(6) . . ? C17 C18 C85 125.6(6) . . ? C19 C18 C85 128.2(6) . . ? C20 C19 N4 119.3(6) . . ? C20 C19 C18 130.4(7) . . ? N4 C19 C18 110.3(6) . . ? C19 C20 C21 129.3(6) . . ? C19 C20 C49 118.7(6) . . ? C21 C20 C49 112.0(5) . . ? N5 C21 C20 122.5(6) . . ? N5 C21 C22 108.0(5) . . ? C20 C21 C22 129.5(6) . . ? C23 C22 C21 108.6(6) . . ? C23 C22 H7 125.7 . . ? C21 C22 H7 125.7 . . ? C22 C23 C24 107.1(6) . . ? C22 C23 H8 126.5 . . ? C24 C23 H8 126.5 . . ? N5 C24 C25 127.5(6) . . ? N5 C24 C23 108.7(6) . . ? C25 C24 C23 122.9(6) . . ? C24 C25 C26 126.3(6) . . ? C24 C25 C55 118.0(6) . . ? C26 C25 C55 115.6(5) . . ? N6 C26 C25 115.3(6) . . ? N6 C26 C27 111.9(6) . . ? C25 C26 C27 132.9(6) . . ? C28 C27 C26 103.7(6) . . ? C28 C27 H9 128.2 . . ? C26 C27 H9 128.2 . . ? C27 C28 C29 110.5(6) . . ? C27 C28 H10 124.7 . . ? C29 C28 H10 124.7 . . ? C30 C29 N6 118.1(6) . . ? C30 C29 C28 133.9(6) . . ? N6 C29 C28 107.7(5) . . ? C29 C30 C1 125.6(6) . . ? C29 C30 C61 116.2(6) . . ? C1 C30 C61 118.2(6) . . ? C36 C31 C32 116.0(6) . . ? C36 C31 C5 122.2(7) . . ? C32 C31 C5 121.8(6) . . ? F1 C32 C33 118.6(7) . . ? F1 C32 C31 118.9(6) . . ? C33 C32 C31 122.5(7) . . ? F2 C33 C32 120.1(7) . . ? F2 C33 C34 120.3(6) . . ? C32 C33 C34 119.6(8) . . ? F3 C34 C33 120.0(8) . . ? F3 C34 C35 119.6(7) . . ? C33 C34 C35 120.4(7) . . ? F4 C35 C36 121.6(8) . . ? F4 C35 C34 120.7(7) . . ? C36 C35 C34 117.5(7) . . ? F5 C36 C35 117.7(6) . . ? F5 C36 C31 118.3(6) . . ? C35 C36 C31 123.9(7) . . ? C42 C37 C38 114.1(6) . . ? C42 C37 C10 122.8(6) . . ? C38 C37 C10 123.1(6) . . ? C39 C38 F6 117.3(7) . . ? C39 C38 C37 124.2(7) . . ? F6 C38 C37 118.4(6) . . ? C40 C39 C38 120.7(7) . . ? C40 C39 F7 118.0(7) . . ? C38 C39 F7 121.3(7) . . ? F8 C40 C39 123.4(7) . . ? F8 C40 C41 118.2(7) . . ? C39 C40 C41 118.4(7) . . ? F9 C41 C42 121.1(8) . . ? F9 C41 C40 119.6(7) . . ? C42 C41 C40 119.3(7) . . ? F10 C42 C41 117.8(7) . . ? F10 C42 C37 119.0(6) . . ? C41 C42 C37 123.2(7) . . ? C48 C43 C44 116.0(7) . . ? C48 C43 C15 123.2(6) . . ? C44 C43 C15 120.8(7) . . ? F11 C44 C43 122.8(6) . . ? F11 C44 C45 113.0(7) . . ? C43 C44 C45 124.1(7) . . ? F12 C45 C46 117.4(6) . . ? F12 C45 C44 124.2(7) . . ? C46 C45 C44 118.4(7) . . ? F13 C46 C45 122.6(7) . . ? F13 C46 C47 118.5(8) . . ? C45 C46 C47 118.8(7) . . ? F14 C47 C46 121.5(7) . . ? F14 C47 C48 117.3(7) . . ? C46 C47 C48 121.2(8) . . ? F15 C48 C43 117.3(7) . . ? F15 C48 C47 121.3(7) . . ? C43 C48 C47 121.3(8) . . ? C54 C49 C50 117.2(6) . . ? C54 C49 C20 126.0(6) . . ? C50 C49 C20 116.8(6) . . ? F16 C50 C51 118.5(7) . . ? F16 C50 C49 122.6(6) . . ? C51 C50 C49 118.9(7) . . ? C50 C51 C52 123.3(7) . . ? C50 C51 F17 121.4(7) . . ? C52 C51 F17 115.3(7) . . ? F18 C52 C51 124.2(7) . . ? F18 C52 C53 117.3(7) . . ? C51 C52 C53 118.5(7) . . ? F19 C53 C54 118.1(7) . . ? F19 C53 C52 121.5(7) . . ? C54 C53 C52 120.3(7) . . ? F20 C54 C53 121.5(6) . . ? F20 C54 C49 116.8(6) . . ? C53 C54 C49 121.7(7) . . ? C60 C55 C56 117.3(6) . . ? C60 C55 C25 121.7(6) . . ? C56 C55 C25 120.7(6) . . ? F21 C56 C57 119.3(6) . . ? F21 C56 C55 119.4(6) . . ? C57 C56 C55 121.3(7) . . ? F22 C57 C58 120.2(7) . . ? F22 C57 C56 119.8(7) . . ? C58 C57 C56 120.0(7) . . ? F23 C58 C57 120.5(7) . . ? F23 C58 C59 119.6(7) . . ? C57 C58 C59 119.8(7) . . ? F24 C59 C58 120.7(7) . . ? F24 C59 C60 119.1(7) . . ? C58 C59 C60 120.2(7) . . ? F25 C60 C59 119.1(7) . . ? F25 C60 C55 119.4(6) . . ? C59 C60 C55 121.4(7) . . ? C62 C61 C66 117.4(6) . . ? C62 C61 C30 115.9(6) . . ? C66 C61 C30 126.7(6) . . ? F26 C62 C61 122.6(6) . . ? F26 C62 C63 114.8(7) . . ? C61 C62 C63 122.6(7) . . ? F27 C63 C64 117.0(7) . . ? F27 C63 C62 123.4(7) . . ? C64 C63 C62 119.6(7) . . ? F28 C64 C65 117.8(8) . . ? F28 C64 C63 123.2(8) . . ? C65 C64 C63 118.9(7) . . ? C64 C65 F29 123.2(7) . . ? C64 C65 C66 122.4(7) . . ? F29 C65 C66 114.3(7) . . ? F30 C66 C61 118.3(6) . . ? F30 C66 C65 122.6(6) . . ? C61 C66 C65 119.0(7) . . ? C72 C67 C68 119.6(6) . . ? C72 C67 C2 121.5(6) . . ? C68 C67 C2 118.9(7) . . ? C67 C68 C69 117.7(7) . . ? C67 C68 H11 121.2 . . ? C69 C68 H11 121.2 . . ? C70 C69 C68 122.3(7) . . ? C70 C69 H12 118.8 . . ? C68 C69 H12 118.8 . . ? C69 C70 C71 119.8(7) . . ? C69 C70 H13 120.1 . . ? C71 C70 H13 120.1 . . ? C70 C71 C72 118.4(7) . . ? C70 C71 H14 120.8 . . ? C72 C71 H14 120.8 . . ? C67 C72 C71 122.2(7) . . ? C67 C72 H15 118.9 . . ? C71 C72 H15 118.9 . . ? C74 C73 C78 118.4(6) . . ? C74 C73 C3 122.5(6) . . ? C78 C73 C3 119.0(6) . . ? C75 C74 C73 121.4(7) . . ? C75 C74 H16 119.3 . . ? C73 C74 H16 119.3 . . ? C74 C75 C76 120.4(6) . . ? C74 C75 H17 119.8 . . ? C76 C75 H17 119.8 . . ? C77 C76 C75 118.4(6) . . ? C77 C76 H18 120.8 . . ? C75 C76 H18 120.8 . . ? C78 C77 C76 120.2(7) . . ? C78 C77 H19 119.9 . . ? C76 C77 H19 119.9 . . ? C77 C78 C73 121.2(7) . . ? C77 C78 H20 119.4 . . ? C73 C78 H20 119.4 . . ? C80 C79 C84 120.1(6) . . ? C80 C79 C17 121.4(6) . . ? C84 C79 C17 118.4(7) . . ? C79 C80 C81 121.6(7) . . ? C79 C80 H21 119.2 . . ? C81 C80 H21 119.2 . . ? C82 C81 C80 117.5(7) . . ? C82 C81 H22 121.3 . . ? C80 C81 H22 121.3 . . ? C83 C82 C81 120.6(7) . . ? C83 C82 H23 119.7 . . ? C81 C82 H23 119.7 . . ? C82 C83 C84 121.0(7) . . ? C82 C83 H24 119.5 . . ? C84 C83 H24 119.5 . . ? C79 C84 C83 119.1(7) . . ? C79 C84 H25 120.5 . . ? C83 C84 H25 120.5 . . ? C86 C85 C90 120.1(6) . . ? C86 C85 C18 117.1(6) . . ? C90 C85 C18 122.7(6) . . ? C87 C86 C85 119.3(7) . . ? C87 C86 H26 120.4 . . ? C85 C86 H26 120.4 . . ? C88 C87 C86 121.2(8) . . ? C88 C87 H27 119.4 . . ? C86 C87 H27 119.4 . . ? C87 C88 C89 121.3(7) . . ? C87 C88 H28 119.3 . . ? C89 C88 H28 119.3 . . ? C88 C89 C90 118.3(7) . . ? C88 C89 H29 120.8 . . ? C90 C89 H29 120.8 . . ? C85 C90 C89 119.6(6) . . ? C85 C90 H30 120.2 . . ? C89 C90 H30 120.2 . . ? C91 N7 C94 106.4(5) . . ? C96 N8 C99 104.2(5) . . ? C101 N9 C104 109.5(5) . . ? C101 N9 H40 125.2 . . ? C104 N9 H40 125.2 . . ? N7 C91 C105 126.4(6) . . ? N7 C91 C92 110.6(6) . . ? C105 C91 C92 122.6(6) . . ? C93 C92 C91 107.0(6) . . ? C93 C92 H31 126.5 . . ? C91 C92 H31 126.5 . . ? C92 C93 C94 106.5(5) . . ? C92 C93 H32 126.8 . . ? C94 C93 H32 126.8 . . ? N7 C94 C95 124.3(6) . . ? N7 C94 C93 109.2(5) . . ? C95 C94 C93 126.3(6) . . ? C94 C95 C96 131.1(6) . . ? C94 C95 C106 115.0(5) . . ? C96 C95 C106 113.8(5) . . ? N8 C96 C95 117.7(6) . . ? N8 C96 C97 111.9(6) . . ? C95 C96 C97 130.4(6) . . ? C98 C97 C96 105.4(6) . . ? C98 C97 H33 127.3 . . ? C96 C97 H33 127.3 . . ? C97 C98 C99 106.7(6) . . ? C97 C98 H34 126.7 . . ? C99 C98 H34 126.7 . . ? N8 C99 C100 114.5(6) . . ? N8 C99 C98 111.7(6) . . ? C100 C99 C98 133.3(6) . . ? C99 C100 C101 123.4(6) . . ? C99 C100 C112 118.7(6) . . ? C101 C100 C112 117.7(5) . . ? N9 C101 C100 126.8(6) . . ? N9 C101 C102 110.1(6) . . ? C100 C101 C102 123.1(6) . . ? C103 C102 C101 105.2(6) . . ? C103 C102 C124 127.1(6) . . ? C101 C102 C124 127.2(6) . . ? C102 C103 C104 106.6(6) . . ? C102 C103 C130 123.9(6) . . ? C104 C103 C130 129.3(6) . . ? N9 C104 C105 123.9(6) . 2_556 ? N9 C104 C103 108.2(6) . . ? C105 C104 C103 127.8(6) 2_556 . ? C104 C105 C91 123.1(6) 2_556 . ? C104 C105 C118 120.4(6) 2_556 . ? C91 C105 C118 116.5(6) . . ? C111 C106 C107 117.0(6) . . ? C111 C106 C95 119.7(6) . . ? C107 C106 C95 123.0(6) . . ? F31 C107 C106 120.0(6) . . ? F31 C107 C108 118.8(6) . . ? C106 C107 C108 121.2(6) . . ? C109 C108 F32 120.1(6) . . ? C109 C108 C107 120.5(7) . . ? F32 C108 C107 119.4(6) . . ? C108 C109 F33 120.6(7) . . ? C108 C109 C110 120.2(7) . . ? F33 C109 C110 119.1(7) . . ? F34 C110 C109 121.0(7) . . ? F34 C110 C111 120.6(7) . . ? C109 C110 C111 118.4(7) . . ? C106 C111 F35 121.1(6) . . ? C106 C111 C110 122.6(6) . . ? F35 C111 C110 116.2(6) . . ? C117 C112 C113 117.5(6) . . ? C117 C112 C100 121.2(6) . . ? C113 C112 C100 121.3(6) . . ? F36 C113 C114 119.5(7) . . ? F36 C113 C112 121.9(6) . . ? C114 C113 C112 118.6(7) . . ? C115 C114 F37 118.8(7) . . ? C115 C114 C113 121.9(7) . . ? F37 C114 C113 119.2(7) . . ? C114 C115 F38 122.0(7) . . ? C114 C115 C116 121.7(6) . . ? F38 C115 C116 116.3(7) . . ? F39 C116 C115 123.3(6) . . ? F39 C116 C117 119.7(6) . . ? C115 C116 C117 116.9(6) . . ? F40 C117 C112 118.8(6) . . ? F40 C117 C116 117.8(6) . . ? C112 C117 C116 123.4(6) . . ? C123 C118 C119 113.9(7) . . ? C123 C118 C105 122.6(7) . . ? C119 C118 C105 123.4(7) . . ? F41 C119 C120 120.3(7) . . ? F41 C119 C118 116.4(7) . . ? C120 C119 C118 123.3(7) . . ? F42 C120 C119 118.7(7) . . ? F42 C120 C121 121.6(7) . . ? C119 C120 C121 119.7(7) . . ? F43 C121 C120 118.3(7) . . ? F43 C121 C122 122.9(8) . . ? C120 C121 C122 118.8(7) . . ? F44 C122 C123 126.3(8) . . ? F44 C122 C121 114.8(8) . . ? C123 C122 C121 118.9(7) . . ? C122 C123 F45 113.6(7) . . ? C122 C123 C118 125.4(7) . . ? F45 C123 C118 120.9(7) . . ? C125 C124 C129 116.4(7) . . ? C125 C124 C102 120.1(7) . . ? C129 C124 C102 123.5(7) . . ? C124 C125 C126 123.5(7) . . ? C124 C125 H35 118.2 . . ? C126 C125 H35 118.2 . . ? C125 C126 C127 117.4(7) . . ? C125 C126 H36 121.3 . . ? C127 C126 H36 121.3 . . ? C128 C127 C126 120.3(7) . . ? C128 C127 H37 119.8 . . ? C126 C127 H37 119.8 . . ? C127 C128 C129 119.5(7) . . ? C127 C128 H38 120.3 . . ? C129 C128 H38 120.3 . . ? C124 C129 C128 122.8(7) . . ? C124 C129 H39 118.6 . . ? C128 C129 H39 118.6 . . ? C131 C130 C135 118.1(6) . . ? C131 C130 C103 118.1(6) . . ? C135 C130 C103 123.8(6) . . ? C130 C131 C132 122.6(6) . . ? C130 C131 H41 118.7 . . ? C132 C131 H41 118.7 . . ? C133 C132 C131 118.2(7) . . ? C133 C132 H42 120.9 . . ? C131 C132 H42 120.9 . . ? C134 C133 C132 120.0(7) . . ? C134 C133 H43 120.0 . . ? C132 C133 H43 120.0 . . ? C133 C134 C135 121.4(7) . . ? C133 C134 H44 119.3 . . ? C135 C134 H44 119.3 . . ? C134 C135 C130 119.7(6) . . ? C134 C135 H45 120.2 . . ? C130 C135 H45 120.2 . . ? Cl2S C1S Cl3S 110.1(4) . . ? Cl2S C1S Cl1S 111.7(4) . . ? Cl3S C1S Cl1S 108.5(4) . . ? Cl2S C1S H46 108.8 . . ? Cl3S C1S H46 108.8 . . ? Cl1S C1S H46 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C30 -178.5(6) . . . . ? C4 N1 C1 C2 1.9(7) . . . . ? N1 C1 C2 C3 1.8(7) . . . . ? C30 C1 C2 C3 -177.8(6) . . . . ? N1 C1 C2 C67 171.8(6) . . . . ? C30 C1 C2 C67 -7.8(10) . . . . ? C1 C2 C3 C4 -4.6(7) . . . . ? C67 C2 C3 C4 -174.9(6) . . . . ? C1 C2 C3 C73 170.0(5) . . . . ? C67 C2 C3 C73 -0.3(10) . . . . ? C1 N1 C4 C5 173.6(6) . . . . ? C1 N1 C4 C3 -4.7(6) . . . . ? C2 C3 C4 N1 5.8(6) . . . . ? C73 C3 C4 N1 -168.7(5) . . . . ? C2 C3 C4 C5 -172.4(6) . . . . ? C73 C3 C4 C5 13.1(10) . . . . ? N1 C4 C5 C6 0.9(9) . . . . ? C3 C4 C5 C6 178.8(6) . . . . ? N1 C4 C5 C31 177.0(6) . . . . ? C3 C4 C5 C31 -5.1(10) . . . . ? C9 N2 C6 C5 171.3(6) . . . . ? C9 N2 C6 C7 -6.3(6) . . . . ? C4 C5 C6 N2 5.9(10) . . . . ? C31 C5 C6 N2 -170.4(6) . . . . ? C4 C5 C6 C7 -176.8(5) . . . . ? C31 C5 C6 C7 6.9(9) . . . . ? N2 C6 C7 C8 4.9(7) . . . . ? C5 C6 C7 C8 -172.7(6) . . . . ? C6 C7 C8 C9 -1.4(6) . . . . ? C6 N2 C9 C10 -168.3(6) . . . . ? C6 N2 C9 C8 5.5(7) . . . . ? C7 C8 C9 N2 -2.4(7) . . . . ? C7 C8 C9 C10 171.6(6) . . . . ? N2 C9 C10 C11 -11.2(10) . . . . ? C8 C9 C10 C11 175.7(6) . . . . ? N2 C9 C10 C37 157.6(6) . . . . ? C8 C9 C10 C37 -15.5(9) . . . . ? C14 N3 C11 C10 174.4(5) . . . . ? C14 N3 C11 C12 -1.4(6) . . . . ? C9 C10 C11 N3 161.7(6) . . . . ? C37 C10 C11 N3 -7.7(8) . . . . ? C9 C10 C11 C12 -23.6(10) . . . . ? C37 C10 C11 C12 167.0(6) . . . . ? N3 C11 C12 C13 2.8(7) . . . . ? C10 C11 C12 C13 -172.2(6) . . . . ? C11 C12 C13 C14 -2.8(6) . . . . ? C11 N3 C14 C15 -174.1(5) . . . . ? C11 N3 C14 C13 -0.4(7) . . . . ? C12 C13 C14 N3 2.1(7) . . . . ? C12 C13 C14 C15 175.2(6) . . . . ? N3 C14 C15 C16 179.1(6) . . . . ? C13 C14 C15 C16 6.5(11) . . . . ? N3 C14 C15 C43 -5.4(8) . . . . ? C13 C14 C15 C43 -177.9(6) . . . . ? C19 N4 C16 C17 -3.2(7) . . . . ? C19 N4 C16 C15 -179.4(5) . . . . ? C14 C15 C16 N4 25.7(10) . . . . ? C43 C15 C16 N4 -149.9(6) . . . . ? C14 C15 C16 C17 -149.9(6) . . . . ? C43 C15 C16 C17 34.5(8) . . . . ? N4 C16 C17 C18 0.6(7) . . . . ? C15 C16 C17 C18 176.7(5) . . . . ? N4 C16 C17 C79 -172.3(6) . . . . ? C15 C16 C17 C79 3.7(10) . . . . ? C16 C17 C18 C19 2.1(7) . . . . ? C79 C17 C18 C19 175.1(6) . . . . ? C16 C17 C18 C85 -171.1(6) . . . . ? C79 C17 C18 C85 1.8(10) . . . . ? C16 N4 C19 C20 -172.2(5) . . . . ? C16 N4 C19 C18 4.6(7) . . . . ? C17 C18 C19 C20 172.0(6) . . . . ? C85 C18 C19 C20 -14.9(11) . . . . ? C17 C18 C19 N4 -4.2(7) . . . . ? C85 C18 C19 N4 168.8(6) . . . . ? N4 C19 C20 C21 -0.7(10) . . . . ? C18 C19 C20 C21 -176.7(6) . . . . ? N4 C19 C20 C49 179.2(5) . . . . ? C18 C19 C20 C49 3.3(10) . . . . ? C24 N5 C21 C20 -172.0(5) . . . . ? C24 N5 C21 C22 5.1(6) . . . . ? C19 C20 C21 N5 -6.2(10) . . . . ? C49 C20 C21 N5 173.9(5) . . . . ? C19 C20 C21 C22 177.4(6) . . . . ? C49 C20 C21 C22 -2.6(9) . . . . ? N5 C21 C22 C23 -4.3(7) . . . . ? C20 C21 C22 C23 172.6(6) . . . . ? C21 C22 C23 C24 1.7(7) . . . . ? C21 N5 C24 C25 165.1(6) . . . . ? C21 N5 C24 C23 -4.1(6) . . . . ? C22 C23 C24 N5 1.5(7) . . . . ? C22 C23 C24 C25 -168.3(5) . . . . ? N5 C24 C25 C26 18.5(10) . . . . ? C23 C24 C25 C26 -173.7(5) . . . . ? N5 C24 C25 C55 -156.8(6) . . . . ? C23 C24 C25 C55 11.0(8) . . . . ? C29 N6 C26 C25 -176.3(5) . . . . ? C29 N6 C26 C27 2.4(6) . . . . ? C24 C25 C26 N6 -164.4(5) . . . . ? C55 C25 C26 N6 11.0(8) . . . . ? C24 C25 C26 C27 17.1(10) . . . . ? C55 C25 C26 C27 -167.4(6) . . . . ? N6 C26 C27 C28 -2.9(7) . . . . ? C25 C26 C27 C28 175.5(6) . . . . ? C26 C27 C28 C29 2.1(7) . . . . ? C26 N6 C29 C30 173.3(5) . . . . ? C26 N6 C29 C28 -1.1(6) . . . . ? C27 C28 C29 C30 -173.9(6) . . . . ? C27 C28 C29 N6 -0.8(7) . . . . ? N6 C29 C30 C1 -179.2(5) . . . . ? C28 C29 C30 C1 -6.7(11) . . . . ? N6 C29 C30 C61 1.0(8) . . . . ? C28 C29 C30 C61 173.5(6) . . . . ? N1 C1 C30 C29 -27.5(10) . . . . ? C2 C1 C30 C29 152.0(6) . . . . ? N1 C1 C30 C61 152.2(6) . . . . ? C2 C1 C30 C61 -28.2(9) . . . . ? C4 C5 C31 C36 -98.9(7) . . . . ? C6 C5 C31 C36 77.3(8) . . . . ? C4 C5 C31 C32 82.2(8) . . . . ? C6 C5 C31 C32 -101.6(7) . . . . ? C36 C31 C32 F1 178.0(5) . . . . ? C5 C31 C32 F1 -3.0(9) . . . . ? C36 C31 C32 C33 -1.4(9) . . . . ? C5 C31 C32 C33 177.6(6) . . . . ? F1 C32 C33 F2 1.4(9) . . . . ? C31 C32 C33 F2 -179.1(6) . . . . ? F1 C32 C33 C34 -177.2(6) . . . . ? C31 C32 C33 C34 2.3(10) . . . . ? F2 C33 C34 F3 0.4(10) . . . . ? C32 C33 C34 F3 179.0(6) . . . . ? F2 C33 C34 C35 178.0(6) . . . . ? C32 C33 C34 C35 -3.4(11) . . . . ? F3 C34 C35 F4 -2.9(11) . . . . ? C33 C34 C35 F4 179.5(6) . . . . ? F3 C34 C35 C36 -178.6(6) . . . . ? C33 C34 C35 C36 3.7(11) . . . . ? F4 C35 C36 F5 4.7(10) . . . . ? C34 C35 C36 F5 -179.6(6) . . . . ? F4 C35 C36 C31 -178.8(6) . . . . ? C34 C35 C36 C31 -3.0(10) . . . . ? C32 C31 C36 F5 178.4(5) . . . . ? C5 C31 C36 F5 -0.6(9) . . . . ? C32 C31 C36 C35 1.9(10) . . . . ? C5 C31 C36 C35 -177.1(6) . . . . ? C9 C10 C37 C42 116.3(7) . . . . ? C11 C10 C37 C42 -73.0(8) . . . . ? C9 C10 C37 C38 -64.2(8) . . . . ? C11 C10 C37 C38 106.5(6) . . . . ? C42 C37 C38 C39 3.1(10) . . . . ? C10 C37 C38 C39 -176.5(6) . . . . ? C42 C37 C38 F6 -179.5(5) . . . . ? C10 C37 C38 F6 0.9(9) . . . . ? F6 C38 C39 C40 -178.9(6) . . . . ? C37 C38 C39 C40 -1.5(11) . . . . ? F6 C38 C39 F7 0.5(9) . . . . ? C37 C38 C39 F7 178.0(6) . . . . ? C38 C39 C40 F8 179.7(6) . . . . ? F7 C39 C40 F8 0.3(10) . . . . ? C38 C39 C40 C41 -1.8(11) . . . . ? F7 C39 C40 C41 178.8(6) . . . . ? F8 C40 C41 F9 -1.2(10) . . . . ? C39 C40 C41 F9 -179.8(6) . . . . ? F8 C40 C41 C42 -178.2(6) . . . . ? C39 C40 C41 C42 3.2(10) . . . . ? F9 C41 C42 F10 2.9(10) . . . . ? C40 C41 C42 F10 179.9(6) . . . . ? F9 C41 C42 C37 -178.5(6) . . . . ? C40 C41 C42 C37 -1.5(10) . . . . ? C38 C37 C42 F10 177.1(5) . . . . ? C10 C37 C42 F10 -3.3(10) . . . . ? C38 C37 C42 C41 -1.5(10) . . . . ? C10 C37 C42 C41 178.1(6) . . . . ? C14 C15 C43 C48 -113.1(7) . . . . ? C16 C15 C43 C48 63.1(7) . . . . ? C14 C15 C43 C44 65.9(7) . . . . ? C16 C15 C43 C44 -117.8(6) . . . . ? C48 C43 C44 F11 -179.0(5) . . . . ? C15 C43 C44 F11 1.8(8) . . . . ? C48 C43 C44 C45 -2.4(9) . . . . ? C15 C43 C44 C45 178.5(6) . . . . ? F11 C44 C45 F12 -1.3(8) . . . . ? C43 C44 C45 F12 -178.3(5) . . . . ? F11 C44 C45 C46 177.4(5) . . . . ? C43 C44 C45 C46 0.5(9) . . . . ? F12 C45 C46 F13 -1.4(9) . . . . ? C44 C45 C46 F13 179.8(5) . . . . ? F12 C45 C46 C47 -179.1(5) . . . . ? C44 C45 C46 C47 2.1(9) . . . . ? F13 C46 C47 F14 1.8(9) . . . . ? C45 C46 C47 F14 179.6(5) . . . . ? F13 C46 C47 C48 179.5(5) . . . . ? C45 C46 C47 C48 -2.7(10) . . . . ? C44 C43 C48 F15 -178.3(5) . . . . ? C15 C43 C48 F15 0.8(8) . . . . ? C44 C43 C48 C47 1.7(9) . . . . ? C15 C43 C48 C47 -179.2(6) . . . . ? F14 C47 C48 F15 -1.4(9) . . . . ? C46 C47 C48 F15 -179.2(5) . . . . ? F14 C47 C48 C43 178.5(5) . . . . ? C46 C47 C48 C43 0.8(10) . . . . ? C19 C20 C49 C54 -80.7(8) . . . . ? C21 C20 C49 C54 99.3(7) . . . . ? C19 C20 C49 C50 100.1(7) . . . . ? C21 C20 C49 C50 -79.9(6) . . . . ? C54 C49 C50 F16 -177.5(6) . . . . ? C20 C49 C50 F16 1.7(9) . . . . ? C54 C49 C50 C51 0.0(9) . . . . ? C20 C49 C50 C51 179.3(6) . . . . ? F16 C50 C51 C52 177.9(6) . . . . ? C49 C50 C51 C52 0.2(10) . . . . ? F16 C50 C51 F17 -2.1(9) . . . . ? C49 C50 C51 F17 -179.8(5) . . . . ? C50 C51 C52 F18 180.0(6) . . . . ? F17 C51 C52 F18 -0.1(10) . . . . ? C50 C51 C52 C53 -1.2(11) . . . . ? F17 C51 C52 C53 178.8(5) . . . . ? F18 C52 C53 F19 -1.9(9) . . . . ? C51 C52 C53 F19 179.1(6) . . . . ? F18 C52 C53 C54 -179.1(6) . . . . ? C51 C52 C53 C54 1.9(10) . . . . ? F19 C53 C54 F20 -1.8(9) . . . . ? C52 C53 C54 F20 175.5(6) . . . . ? F19 C53 C54 C49 -179.0(6) . . . . ? C52 C53 C54 C49 -1.8(10) . . . . ? C50 C49 C54 F20 -176.6(5) . . . . ? C20 C49 C54 F20 4.2(9) . . . . ? C50 C49 C54 C53 0.7(9) . . . . ? C20 C49 C54 C53 -178.4(6) . . . . ? C24 C25 C55 C60 -116.3(7) . . . . ? C26 C25 C55 C60 67.9(8) . . . . ? C24 C25 C55 C56 69.9(8) . . . . ? C26 C25 C55 C56 -105.9(7) . . . . ? C60 C55 C56 F21 179.7(6) . . . . ? C25 C55 C56 F21 -6.3(9) . . . . ? C60 C55 C56 C57 0.5(10) . . . . ? C25 C55 C56 C57 174.5(6) . . . . ? F21 C56 C57 F22 0.5(10) . . . . ? C55 C56 C57 F22 179.6(6) . . . . ? F21 C56 C57 C58 -179.4(6) . . . . ? C55 C56 C57 C58 -0.3(11) . . . . ? F22 C57 C58 F23 0.7(10) . . . . ? C56 C57 C58 F23 -179.5(6) . . . . ? F22 C57 C58 C59 179.6(6) . . . . ? C56 C57 C58 C59 -0.5(11) . . . . ? F23 C58 C59 F24 -2.4(10) . . . . ? C57 C58 C59 F24 178.7(6) . . . . ? F23 C58 C59 C60 180.0(6) . . . . ? C57 C58 C59 C60 1.1(11) . . . . ? F24 C59 C60 F25 -0.2(9) . . . . ? C58 C59 C60 F25 177.5(6) . . . . ? F24 C59 C60 C55 -178.4(6) . . . . ? C58 C59 C60 C55 -0.8(11) . . . . ? C56 C55 C60 F25 -178.3(5) . . . . ? C25 C55 C60 F25 7.8(9) . . . . ? C56 C55 C60 C59 0.0(10) . . . . ? C25 C55 C60 C59 -174.0(6) . . . . ? C29 C30 C61 C62 114.9(6) . . . . ? C1 C30 C61 C62 -64.9(7) . . . . ? C29 C30 C61 C66 -64.2(8) . . . . ? C1 C30 C61 C66 116.0(7) . . . . ? C66 C61 C62 F26 178.4(5) . . . . ? C30 C61 C62 F26 -0.8(8) . . . . ? C66 C61 C62 C63 -2.4(9) . . . . ? C30 C61 C62 C63 178.3(5) . . . . ? F26 C62 C63 F27 -0.5(9) . . . . ? C61 C62 C63 F27 -179.7(5) . . . . ? F26 C62 C63 C64 -179.5(5) . . . . ? C61 C62 C63 C64 1.3(10) . . . . ? F27 C63 C64 F28 1.3(9) . . . . ? C62 C63 C64 F28 -179.7(5) . . . . ? F27 C63 C64 C65 179.6(6) . . . . ? C62 C63 C64 C65 -1.3(9) . . . . ? F28 C64 C65 F29 -2.7(9) . . . . ? C63 C64 C65 F29 178.9(5) . . . . ? F28 C64 C65 C66 -179.0(5) . . . . ? C63 C64 C65 C66 2.5(10) . . . . ? C62 C61 C66 F30 179.9(5) . . . . ? C30 C61 C66 F30 -0.9(9) . . . . ? C62 C61 C66 C65 3.5(8) . . . . ? C30 C61 C66 C65 -177.4(6) . . . . ? C64 C65 C66 F30 -180.0(6) . . . . ? F29 C65 C66 F30 3.3(8) . . . . ? C64 C65 C66 C61 -3.7(9) . . . . ? F29 C65 C66 C61 179.7(5) . . . . ? C3 C2 C67 C72 107.2(7) . . . . ? C1 C2 C67 C72 -60.9(9) . . . . ? C3 C2 C67 C68 -75.5(8) . . . . ? C1 C2 C67 C68 116.4(7) . . . . ? C72 C67 C68 C69 1.7(9) . . . . ? C2 C67 C68 C69 -175.7(5) . . . . ? C67 C68 C69 C70 -1.4(9) . . . . ? C68 C69 C70 C71 0.7(10) . . . . ? C69 C70 C71 C72 -0.2(9) . . . . ? C68 C67 C72 C71 -1.3(9) . . . . ? C2 C67 C72 C71 176.0(5) . . . . ? C70 C71 C72 C67 0.6(9) . . . . ? C2 C3 C73 C74 84.1(8) . . . . ? C4 C3 C73 C74 -102.3(7) . . . . ? C2 C3 C73 C78 -93.9(7) . . . . ? C4 C3 C73 C78 79.7(8) . . . . ? C78 C73 C74 C75 -2.0(9) . . . . ? C3 C73 C74 C75 179.9(5) . . . . ? C73 C74 C75 C76 1.2(10) . . . . ? C74 C75 C76 C77 1.1(9) . . . . ? C75 C76 C77 C78 -2.6(10) . . . . ? C76 C77 C78 C73 1.8(10) . . . . ? C74 C73 C78 C77 0.5(9) . . . . ? C3 C73 C78 C77 178.7(5) . . . . ? C18 C17 C79 C80 -106.6(8) . . . . ? C16 C17 C79 C80 65.0(8) . . . . ? C18 C17 C79 C84 74.1(8) . . . . ? C16 C17 C79 C84 -114.3(7) . . . . ? C84 C79 C80 C81 2.4(9) . . . . ? C17 C79 C80 C81 -176.8(5) . . . . ? C79 C80 C81 C82 -2.8(9) . . . . ? C80 C81 C82 C83 2.5(9) . . . . ? C81 C82 C83 C84 -1.9(10) . . . . ? C80 C79 C84 C83 -1.7(9) . . . . ? C17 C79 C84 C83 177.6(5) . . . . ? C82 C83 C84 C79 1.4(9) . . . . ? C17 C18 C85 C86 95.7(7) . . . . ? C19 C18 C85 C86 -76.1(8) . . . . ? C17 C18 C85 C90 -86.5(8) . . . . ? C19 C18 C85 C90 101.7(8) . . . . ? C90 C85 C86 C87 3.3(9) . . . . ? C18 C85 C86 C87 -178.9(5) . . . . ? C85 C86 C87 C88 -3.7(10) . . . . ? C86 C87 C88 C89 1.7(11) . . . . ? C87 C88 C89 C90 0.5(10) . . . . ? C86 C85 C90 C89 -1.1(9) . . . . ? C18 C85 C90 C89 -178.8(5) . . . . ? C88 C89 C90 C85 -0.8(9) . . . . ? C94 N7 C91 C105 168.4(6) . . . . ? C94 N7 C91 C92 -4.3(6) . . . . ? N7 C91 C92 C93 1.5(7) . . . . ? C105 C91 C92 C93 -171.6(6) . . . . ? C91 C92 C93 C94 1.8(6) . . . . ? C91 N7 C94 C95 -169.3(5) . . . . ? C91 N7 C94 C93 5.4(6) . . . . ? C92 C93 C94 N7 -4.5(6) . . . . ? C92 C93 C94 C95 170.1(5) . . . . ? N7 C94 C95 C96 -14.8(10) . . . . ? C93 C94 C95 C96 171.3(6) . . . . ? N7 C94 C95 C106 161.5(5) . . . . ? C93 C94 C95 C106 -12.4(8) . . . . ? C99 N8 C96 C95 177.6(5) . . . . ? C99 N8 C96 C97 -1.2(6) . . . . ? C94 C95 C96 N8 163.5(6) . . . . ? C106 C95 C96 N8 -12.8(8) . . . . ? C94 C95 C96 C97 -17.9(11) . . . . ? C106 C95 C96 C97 165.8(6) . . . . ? N8 C96 C97 C98 2.1(7) . . . . ? C95 C96 C97 C98 -176.6(6) . . . . ? C96 C97 C98 C99 -1.9(7) . . . . ? C96 N8 C99 C100 -172.9(5) . . . . ? C96 N8 C99 C98 0.0(6) . . . . ? C97 C98 C99 N8 1.3(7) . . . . ? C97 C98 C99 C100 172.3(6) . . . . ? N8 C99 C100 C101 179.2(5) . . . . ? C98 C99 C100 C101 8.4(10) . . . . ? N8 C99 C100 C112 -5.2(8) . . . . ? C98 C99 C100 C112 -176.1(6) . . . . ? C104 N9 C101 C100 178.3(6) . . . . ? C104 N9 C101 C102 0.0(7) . . . . ? C99 C100 C101 N9 28.0(10) . . . . ? C112 C100 C101 N9 -147.6(6) . . . . ? C99 C100 C101 C102 -153.9(6) . . . . ? C112 C100 C101 C102 30.5(9) . . . . ? N9 C101 C102 C103 -3.3(7) . . . . ? C100 C101 C102 C103 178.3(6) . . . . ? N9 C101 C102 C124 -175.3(6) . . . . ? C100 C101 C102 C124 6.3(10) . . . . ? C101 C102 C103 C104 5.0(7) . . . . ? C124 C102 C103 C104 177.0(6) . . . . ? C101 C102 C103 C130 -169.8(6) . . . . ? C124 C102 C103 C130 2.2(11) . . . . ? C101 N9 C104 C105 -174.9(6) . . . 2_556 ? C101 N9 C104 C103 3.2(7) . . . . ? C102 C103 C104 N9 -5.3(7) . . . . ? C130 C103 C104 N9 169.1(6) . . . . ? C102 C103 C104 C105 172.7(6) . . . 2_556 ? C130 C103 C104 C105 -12.9(11) . . . 2_556 ? N7 C91 C105 C104 9.8(10) . . . 2_556 ? C92 C91 C105 C104 -178.2(6) . . . 2_556 ? N7 C91 C105 C118 -168.5(6) . . . . ? C92 C91 C105 C118 3.4(9) . . . . ? C94 C95 C106 C111 -69.5(7) . . . . ? C96 C95 C106 C111 107.4(6) . . . . ? C94 C95 C106 C107 116.5(6) . . . . ? C96 C95 C106 C107 -66.5(8) . . . . ? C111 C106 C107 F31 178.0(5) . . . . ? C95 C106 C107 F31 -7.9(9) . . . . ? C111 C106 C107 C108 -1.8(9) . . . . ? C95 C106 C107 C108 172.3(6) . . . . ? F31 C107 C108 C109 -179.3(6) . . . . ? C106 C107 C108 C109 0.6(10) . . . . ? F31 C107 C108 F32 -1.7(9) . . . . ? C106 C107 C108 F32 178.2(5) . . . . ? F32 C108 C109 F33 1.0(10) . . . . ? C107 C108 C109 F33 178.5(6) . . . . ? F32 C108 C109 C110 -176.9(6) . . . . ? C107 C108 C109 C110 0.7(11) . . . . ? C108 C109 C110 F34 179.5(6) . . . . ? F33 C109 C110 F34 1.6(11) . . . . ? C108 C109 C110 C111 -0.6(11) . . . . ? F33 C109 C110 C111 -178.5(6) . . . . ? C107 C106 C111 F35 178.8(5) . . . . ? C95 C106 C111 F35 4.5(9) . . . . ? C107 C106 C111 C110 1.9(9) . . . . ? C95 C106 C111 C110 -172.4(6) . . . . ? F34 C110 C111 C106 179.1(6) . . . . ? C109 C110 C111 C106 -0.7(10) . . . . ? F34 C110 C111 F35 2.1(9) . . . . ? C109 C110 C111 F35 -177.8(6) . . . . ? C99 C100 C112 C117 -113.5(7) . . . . ? C101 C100 C112 C117 62.3(8) . . . . ? C99 C100 C112 C113 66.8(7) . . . . ? C101 C100 C112 C113 -117.3(6) . . . . ? C117 C112 C113 F36 -179.8(5) . . . . ? C100 C112 C113 F36 -0.2(9) . . . . ? C117 C112 C113 C114 0.2(8) . . . . ? C100 C112 C113 C114 179.8(5) . . . . ? F36 C113 C114 C115 178.3(5) . . . . ? C112 C113 C114 C115 -1.7(9) . . . . ? F36 C113 C114 F37 2.5(9) . . . . ? C112 C113 C114 F37 -177.5(5) . . . . ? F37 C114 C115 F38 -2.8(9) . . . . ? C113 C114 C115 F38 -178.6(5) . . . . ? F37 C114 C115 C116 178.0(5) . . . . ? C113 C114 C115 C116 2.2(10) . . . . ? C114 C115 C116 F39 177.9(5) . . . . ? F38 C115 C116 F39 -1.3(8) . . . . ? C114 C115 C116 C117 -1.1(9) . . . . ? F38 C115 C116 C117 179.6(5) . . . . ? C113 C112 C117 F40 -176.8(5) . . . . ? C100 C112 C117 F40 3.6(8) . . . . ? C113 C112 C117 C116 0.8(9) . . . . ? C100 C112 C117 C116 -178.8(5) . . . . ? F39 C116 C117 F40 -1.9(8) . . . . ? C115 C116 C117 F40 177.2(5) . . . . ? F39 C116 C117 C112 -179.5(5) . . . . ? C115 C116 C117 C112 -0.4(9) . . . . ? C104 C105 C118 C123 82.0(8) 2_556 . . . ? C91 C105 C118 C123 -99.6(7) . . . . ? C104 C105 C118 C119 -100.8(8) 2_556 . . . ? C91 C105 C118 C119 77.6(8) . . . . ? C123 C118 C119 F41 -179.9(5) . . . . ? C105 C118 C119 F41 2.7(10) . . . . ? C123 C118 C119 C120 -1.4(10) . . . . ? C105 C118 C119 C120 -178.7(7) . . . . ? F41 C119 C120 F42 -0.3(10) . . . . ? C118 C119 C120 F42 -178.8(6) . . . . ? F41 C119 C120 C121 179.7(6) . . . . ? C118 C119 C120 C121 1.2(11) . . . . ? F42 C120 C121 F43 0.0(10) . . . . ? C119 C120 C121 F43 179.9(6) . . . . ? F42 C120 C121 C122 179.7(6) . . . . ? C119 C120 C121 C122 -0.4(11) . . . . ? F43 C121 C122 F44 -2.0(9) . . . . ? C120 C121 C122 F44 178.3(6) . . . . ? F43 C121 C122 C123 179.5(6) . . . . ? C120 C121 C122 C123 -0.2(10) . . . . ? F44 C122 C123 F45 4.1(9) . . . . ? C121 C122 C123 F45 -177.6(5) . . . . ? F44 C122 C123 C118 -178.3(6) . . . . ? C121 C122 C123 C118 0.0(10) . . . . ? C119 C118 C123 C122 0.8(10) . . . . ? C105 C118 C123 C122 178.1(6) . . . . ? C119 C118 C123 F45 178.2(5) . . . . ? C105 C118 C123 F45 -4.5(10) . . . . ? C103 C102 C124 C125 -106.3(8) . . . . ? C101 C102 C124 C125 64.0(8) . . . . ? C103 C102 C124 C129 73.2(9) . . . . ? C101 C102 C124 C129 -116.5(7) . . . . ? C129 C124 C125 C126 4.0(9) . . . . ? C102 C124 C125 C126 -176.5(6) . . . . ? C124 C125 C126 C127 -2.9(10) . . . . ? C125 C126 C127 C128 0.1(10) . . . . ? C126 C127 C128 C129 1.3(10) . . . . ? C125 C124 C129 C128 -2.4(9) . . . . ? C102 C124 C129 C128 178.1(6) . . . . ? C127 C128 C129 C124 -0.2(10) . . . . ? C102 C103 C130 C131 95.3(7) . . . . ? C104 C103 C130 C131 -78.2(9) . . . . ? C102 C103 C130 C135 -84.7(8) . . . . ? C104 C103 C130 C135 101.8(8) . . . . ? C135 C130 C131 C132 -0.1(9) . . . . ? C103 C130 C131 C132 179.9(5) . . . . ? C130 C131 C132 C133 -1.5(9) . . . . ? C131 C132 C133 C134 -0.2(9) . . . . ? C132 C133 C134 C135 3.4(10) . . . . ? C133 C134 C135 C130 -5.0(9) . . . . ? C131 C130 C135 C134 3.3(8) . . . . ? C103 C130 C135 C134 -176.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 64.00 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.563 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.071 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 255 108 ' ' 2 -0.025 0.181 0.677 122 57 ' ' 3 0.025 0.819 0.323 124 57 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT026_3A_SQ ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 28 Perc. RESPONSE: Tiny crystal gave the very weak reflections. Though we tried to make a fine crystal, it was difficult to make a better one. ; # end Validation Reply Form # Attachment '4-TFA2-B.cif' data_4-TFA2-B _database_code_depnum_ccdc_archive 'CCDC 728272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H34 F30 N6, 2(C2 H F3 O2), 2(C2 F3 O2), 3(C H2 Cl2) ' _chemical_formula_sum 'C101 H42 Cl6 F42 N6 O8' _chemical_formula_weight 2478.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.8248(14) _cell_length_b 21.260(2) _cell_length_c 34.396(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.059(2) _cell_angle_gamma 90.00 _cell_volume 9953.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5339 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 24.04 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4936 _exptl_absorpt_coefficient_mu 0.313 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8849 _exptl_absorpt_correction_T_max 0.9693 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60223 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 22188 _reflns_number_gt 13754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Though some electron density was properly assigned as molecules of dichloromethane, TFA and TFA anion, other electron density around the solvents are still remained. All attempts to model the disorder were unsatisfactory as well as to remove the residual density by use of the utility SQUEEZE in PLATON software packate, SQUEEZE-PLATON. ; _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^)+(0.1244P)^2^+23.6299P] 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 22188 _refine_ls_number_parameters 1468 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1268 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2445 _refine_ls_wR_factor_gt 0.2072 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.034 _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 0.6690(3) 0.67594(18) 0.24345(11) 0.0161(7) Uani 1 1 d . . . C2 C 0.7731(3) 0.68563(18) 0.24720(12) 0.0188(8) Uani 1 1 d . . . C3 C 0.8040(3) 0.65464(19) 0.21614(12) 0.0193(8) Uani 1 1 d . . . C4 C 0.7197(3) 0.62312(19) 0.19375(12) 0.0180(8) Uani 1 1 d . . . C5 C 0.7164(3) 0.57853(18) 0.16335(12) 0.0183(8) Uani 1 1 d . . . C6 C 0.6310(3) 0.55525(18) 0.13988(12) 0.0186(8) Uani 1 1 d . . . C7 C 0.6183(3) 0.49528(19) 0.12108(13) 0.0225(9) Uani 1 1 d . . . H7 H 0.6687 0.4655 0.1196 0.027 Uiso 1 1 calc R . . C8 C 0.5214(3) 0.48828(19) 0.10567(12) 0.0217(8) Uani 1 1 d . . . H8 H 0.4920 0.4520 0.0925 0.026 Uiso 1 1 calc R . . C9 C 0.4716(3) 0.54475(18) 0.11272(11) 0.0174(8) Uani 1 1 d . . . C10 C 0.3717(3) 0.55747(18) 0.10085(11) 0.0173(8) Uani 1 1 d . . . C11 C 0.3229(3) 0.61528(18) 0.10161(12) 0.0171(8) Uani 1 1 d . . . C12 C 0.2203(3) 0.62323(19) 0.10024(13) 0.0212(8) Uani 1 1 d . . . H12 H 0.1738 0.5903 0.1002 0.025 Uiso 1 1 calc R . . C13 C 0.1998(3) 0.68600(19) 0.09902(12) 0.0202(8) Uani 1 1 d . . . H13 H 0.1371 0.7045 0.0987 0.024 Uiso 1 1 calc R . . C14 C 0.2890(3) 0.71894(18) 0.09825(11) 0.0173(8) Uani 1 1 d . . . C15 C 0.2993(3) 0.78280(18) 0.08854(11) 0.0163(8) Uani 1 1 d . . . C16 C 0.2310(3) 0.82737(18) 0.09751(11) 0.0162(8) Uani 1 1 d . . . C17 C 0.1987(3) 0.88579(17) 0.07971(11) 0.0159(7) Uani 1 1 d . . . C18 C 0.1287(3) 0.91018(18) 0.09993(11) 0.0162(8) Uani 1 1 d . . . C19 C 0.1194(3) 0.86871(17) 0.13122(11) 0.0156(7) Uani 1 1 d . . . C20 C 0.0630(3) 0.87356(18) 0.16187(12) 0.0166(8) Uani 1 1 d . . . C21 C 0.0886(3) 0.84335(18) 0.19795(12) 0.0185(8) Uani 1 1 d . . . C22 C 0.0337(3) 0.8327(2) 0.22869(13) 0.0245(9) Uani 1 1 d . . . H22 H -0.0328 0.8446 0.2281 0.029 Uiso 1 1 calc R . . C23 C 0.0920(3) 0.8026(2) 0.25905(13) 0.0245(9) Uani 1 1 d . . . H23 H 0.0734 0.7904 0.2833 0.029 Uiso 1 1 calc R . . C24 C 0.1857(3) 0.79256(19) 0.24832(12) 0.0205(8) Uani 1 1 d . . . C25 C 0.2697(3) 0.76393(19) 0.26977(12) 0.0193(8) Uani 1 1 d . . . C26 C 0.3508(3) 0.74554(19) 0.25284(12) 0.0190(8) Uani 1 1 d . . . C27 C 0.3671(3) 0.7443(2) 0.21271(12) 0.0246(9) Uani 1 1 d . . . H27 H 0.3203 0.7559 0.1902 0.030 Uiso 1 1 calc R . . C28 C 0.4595(3) 0.72407(19) 0.21199(12) 0.0216(8) Uani 1 1 d . . . H28 H 0.4887 0.7187 0.1892 0.026 Uiso 1 1 calc R . . C29 C 0.5049(3) 0.71231(18) 0.25167(12) 0.0177(8) Uani 1 1 d . . . C30 C 0.6043(3) 0.69978(17) 0.26725(11) 0.0164(8) Uani 1 1 d . . . C31 C 0.8111(3) 0.54907(19) 0.15716(12) 0.0214(8) Uani 1 1 d . . . C32 C 0.8678(3) 0.5132(2) 0.18602(13) 0.0280(10) Uani 1 1 d . . . C33 C 0.9574(3) 0.4887(2) 0.18141(14) 0.0335(11) Uani 1 1 d . . . C34 C 0.9919(3) 0.5001(2) 0.14716(14) 0.0306(10) Uani 1 1 d . . . C35 C 0.9385(3) 0.5354(2) 0.11792(13) 0.0294(10) Uani 1 1 d . . . C36 C 0.8479(3) 0.5588(2) 0.12269(13) 0.0262(9) Uani 1 1 d . . . C37 C 0.3059(3) 0.50567(18) 0.08338(12) 0.0191(8) Uani 1 1 d . . . C38 C 0.2804(3) 0.45513(19) 0.10483(13) 0.0231(9) Uani 1 1 d . . . C39 C 0.2128(3) 0.4104(2) 0.08760(15) 0.0305(10) Uani 1 1 d . . . C40 C 0.1691(4) 0.4160(2) 0.04953(16) 0.0379(12) Uani 1 1 d . . . C41 C 0.1913(4) 0.4657(2) 0.02699(16) 0.0410(12) Uani 1 1 d . . . C42 C 0.2597(3) 0.5101(2) 0.04402(14) 0.0274(9) Uani 1 1 d . . . C43 C 0.3787(3) 0.80070(18) 0.06733(12) 0.0169(8) Uani 1 1 d . . . C44 C 0.4375(3) 0.85350(18) 0.07786(12) 0.0188(8) Uani 1 1 d . . . C45 C 0.5088(3) 0.8718(2) 0.05674(14) 0.0258(9) Uani 1 1 d . . . C46 C 0.5265(3) 0.8362(2) 0.02534(13) 0.0256(9) Uani 1 1 d . . . C47 C 0.4701(3) 0.7836(2) 0.01400(12) 0.0227(9) Uani 1 1 d . . . C48 C 0.3964(3) 0.76750(18) 0.03458(12) 0.0188(8) Uani 1 1 d . . . C49 C -0.0274(3) 0.91210(19) 0.15503(12) 0.0207(8) Uani 1 1 d . . . C50 C -0.0430(3) 0.9619(2) 0.17857(16) 0.0331(11) Uani 1 1 d . . . C51 C -0.1276(5) 0.9983(3) 0.1694(2) 0.0561(17) Uani 1 1 d U . . C52 C -0.1959(4) 0.9835(3) 0.1359(2) 0.0613(19) Uani 1 1 d U . . C53 C -0.1824(3) 0.9349(3) 0.11271(19) 0.0514(16) Uani 1 1 d U . . C54 C -0.1000(3) 0.8992(3) 0.12219(15) 0.0347(12) Uani 1 1 d . . . F16 F 0.0264(2) 0.97859(14) 0.20876(9) 0.0461(8) Uani 1 1 d . . . F17 F -0.1383(4) 1.04726(18) 0.19277(17) 0.0924(15) Uani 1 1 d U . . F18 F -0.2761(3) 1.0209(2) 0.12814(17) 0.1037(18) Uani 1 1 d U . . F19 F -0.2483(2) 0.9212(2) 0.08088(13) 0.0875(15) Uani 1 1 d U . . F20 F -0.0897(2) 0.85041(17) 0.09871(9) 0.0496(8) Uani 1 1 d . . . C56 C 0.3335(3) 0.7945(2) 0.34002(13) 0.0244(9) Uani 1 1 d . . . C57 C 0.3396(3) 0.7888(2) 0.38024(13) 0.0269(9) Uani 1 1 d . . . C58 C 0.2850(3) 0.7432(2) 0.39501(12) 0.0254(9) Uani 1 1 d . . . C59 C 0.2259(3) 0.7042(2) 0.36936(12) 0.0217(8) Uani 1 1 d . . . C60 C 0.2214(3) 0.7109(2) 0.32915(12) 0.0211(8) Uani 1 1 d . . . C61 C 0.6386(3) 0.71238(18) 0.30977(12) 0.0174(8) Uani 1 1 d . . . C62 C 0.6157(3) 0.76931(19) 0.32683(12) 0.0203(8) Uani 1 1 d . . . C63 C 0.6355(3) 0.7787(2) 0.36696(14) 0.0269(9) Uani 1 1 d . . . C64 C 0.6838(3) 0.7328(2) 0.39124(13) 0.0303(10) Uani 1 1 d . . . C65 C 0.7118(3) 0.6777(2) 0.37536(13) 0.0266(9) Uani 1 1 d . . . C66 C 0.6881(3) 0.66807(19) 0.33528(12) 0.0206(8) Uani 1 1 d . . . C67 C 0.8311(3) 0.7277(2) 0.27693(12) 0.0206(8) Uani 1 1 d . . . C68 C 0.9038(3) 0.7037(2) 0.30658(12) 0.0231(9) Uani 1 1 d . . . H68 H 0.9193 0.6601 0.3070 0.028 Uiso 1 1 calc R . . C69 C 0.9535(3) 0.7431(2) 0.33542(13) 0.0283(10) Uani 1 1 d . . . H69 H 1.0023 0.7264 0.3557 0.034 Uiso 1 1 calc R . . C70 C 0.9326(3) 0.8061(2) 0.33488(14) 0.0300(10) Uani 1 1 d . . . H70 H 0.9675 0.8328 0.3546 0.036 Uiso 1 1 calc R . . C71 C 0.8609(3) 0.8311(2) 0.30574(14) 0.0297(10) Uani 1 1 d . . . H71 H 0.8467 0.8748 0.3054 0.036 Uiso 1 1 calc R . . C72 C 0.8098(3) 0.7915(2) 0.27690(13) 0.0238(9) Uani 1 1 d . . . H72 H 0.7600 0.8083 0.2571 0.029 Uiso 1 1 calc R . . C73 C 0.9022(3) 0.6600(2) 0.20488(12) 0.0227(9) Uani 1 1 d . . . C74 C 0.9846(3) 0.6352(2) 0.22879(14) 0.0289(10) Uani 1 1 d . . . H74 H 0.9783 0.6149 0.2528 0.035 Uiso 1 1 calc R . . C75 C 1.0764(3) 0.6401(3) 0.21765(14) 0.0345(11) Uani 1 1 d . . . H75 H 1.1327 0.6226 0.2339 0.041 Uiso 1 1 calc R . . C76 C 1.0856(3) 0.6706(2) 0.18270(14) 0.0342(11) Uani 1 1 d . . . H76 H 1.1482 0.6738 0.1750 0.041 Uiso 1 1 calc R . . C77 C 1.0045(3) 0.6961(2) 0.15933(14) 0.0312(10) Uani 1 1 d . . . H77 H 1.0112 0.7177 0.1358 0.037 Uiso 1 1 calc R . . C78 C 0.9128(3) 0.6904(2) 0.17004(13) 0.0256(9) Uani 1 1 d . . . H78 H 0.8567 0.7074 0.1535 0.031 Uiso 1 1 calc R . . C79 C 0.2331(3) 0.91456(18) 0.04555(12) 0.0176(8) Uani 1 1 d . . . C80 C 0.2344(3) 0.88010(19) 0.01094(12) 0.0194(8) Uani 1 1 d . . . H80 H 0.2078 0.8388 0.0086 0.023 Uiso 1 1 calc R . . C81 C 0.2737(3) 0.9054(2) -0.01983(12) 0.0243(9) Uani 1 1 d . . . H81 H 0.2755 0.8812 -0.0429 0.029 Uiso 1 1 calc R . . C82 C 0.3106(3) 0.9663(2) -0.01700(13) 0.0269(9) Uani 1 1 d . . . H82 H 0.3381 0.9837 -0.0381 0.032 Uiso 1 1 calc R . . C83 C 0.3071(3) 1.0017(2) 0.01664(14) 0.0285(10) Uani 1 1 d . . . H83 H 0.3312 1.0437 0.0183 0.034 Uiso 1 1 calc R . . C84 C 0.2688(3) 0.97619(19) 0.04774(13) 0.0224(9) Uani 1 1 d . . . H84 H 0.2668 1.0007 0.0707 0.027 Uiso 1 1 calc R . . C85 C 0.0741(3) 0.97048(18) 0.09039(11) 0.0165(8) Uani 1 1 d . . . C86 C 0.0080(3) 0.97450(19) 0.05476(12) 0.0208(8) Uani 1 1 d . . . H86 H -0.0019 0.9396 0.0373 0.025 Uiso 1 1 calc R . . C87 C -0.0431(3) 1.0303(2) 0.04520(13) 0.0251(9) Uani 1 1 d . . . H87 H -0.0881 1.0335 0.0210 0.030 Uiso 1 1 calc R . . C88 C -0.0290(3) 1.0811(2) 0.07039(13) 0.0255(9) Uani 1 1 d . . . H88 H -0.0646 1.1189 0.0637 0.031 Uiso 1 1 calc R . . C89 C 0.0373(3) 1.0769(2) 0.10557(14) 0.0262(9) Uani 1 1 d . . . H89 H 0.0473 1.1120 0.1229 0.031 Uiso 1 1 calc R . . C90 C 0.0889(3) 1.02170(19) 0.11551(13) 0.0225(9) Uani 1 1 d . . . H90 H 0.1344 1.0190 0.1396 0.027 Uiso 1 1 calc R . . C91 C 0.5706(5) 0.6037(3) -0.00102(18) 0.0475(14) Uani 1 1 d . . . C92 C 0.5762(4) 0.6460(2) 0.03535(16) 0.0358(11) Uani 1 1 d . . . C93 C 0.3421(4) 0.5441(3) 0.2454(2) 0.0510(15) Uani 1 1 d . . . C94 C 0.4473(3) 0.5642(2) 0.24158(14) 0.0284(10) Uani 1 1 d . . . C95 C 0.4858(3) 0.6004(2) 0.40607(15) 0.0314(10) Uani 1 1 d . . . C96 C 0.4732(3) 0.6096(2) 0.36114(13) 0.0241(9) Uani 1 1 d . . . C99 C 0.3088(5) 0.5236(3) 0.72187(18) 0.0522(15) Uani 1 1 d . . . H99A H 0.3379 0.4810 0.7223 0.063 Uiso 1 1 calc R . . H99B H 0.2371 0.5189 0.7206 0.063 Uiso 1 1 calc R . . C100 C 0.1545(6) 0.2667(3) 0.4766(2) 0.0681(19) Uani 1 1 d . . . H10A H 0.1904 0.2846 0.4566 0.082 Uiso 1 1 calc R . . H10B H 0.2016 0.2407 0.4948 0.082 Uiso 1 1 calc R . . C101 C 0.1370(6) 0.6571(4) 0.9602(2) 0.087(3) Uani 1 1 d . . . H10C H 0.1020 0.6302 0.9767 0.104 Uiso 1 1 calc R . . H10D H 0.2033 0.6663 0.9752 0.104 Uiso 1 1 calc R . . Cl1 Cl 0.33117(11) 0.56417(8) 0.67999(5) 0.0535(4) Uani 1 1 d . . . Cl2 Cl 0.35995(16) 0.56439(9) 0.76558(6) 0.0754(5) Uani 1 1 d . . . Cl3 Cl 0.1158(2) 0.32937(12) 0.50375(7) 0.1069(9) Uani 1 1 d . . . Cl4 Cl 0.0638(3) 0.21884(16) 0.45297(8) 0.1339(13) Uani 1 1 d . . . Cl5 Cl 0.07366(16) 0.72555(11) 0.94880(8) 0.0912(7) Uani 1 1 d . . . Cl6 Cl 0.14744(16) 0.61557(9) 0.91339(8) 0.0978(8) Uani 1 1 d . . . F1 F 0.8379(2) 0.50313(17) 0.22037(9) 0.0517(9) Uani 1 1 d . . . F2 F 1.0117(3) 0.45519(19) 0.21051(10) 0.0644(11) Uani 1 1 d . . . F3 F 1.08008(19) 0.47740(15) 0.14265(9) 0.0434(7) Uani 1 1 d . . . F4 F 0.9748(2) 0.54757(18) 0.08519(9) 0.0501(8) Uani 1 1 d . . . F5 F 0.7986(2) 0.59434(17) 0.09420(8) 0.0468(8) Uani 1 1 d . . . F6 F 0.3187(2) 0.44954(12) 0.14294(8) 0.0343(6) Uani 1 1 d . . . F7 F 0.1890(2) 0.36234(13) 0.10945(10) 0.0418(7) Uani 1 1 d . . . F8 F 0.1040(3) 0.37300(16) 0.03316(12) 0.0632(10) Uani 1 1 d . . . F9 F 0.1488(3) 0.47186(18) -0.01086(11) 0.0705(12) Uani 1 1 d . . . F10 F 0.2799(2) 0.55811(13) 0.02190(8) 0.0394(7) Uani 1 1 d . . . F11 F 0.42512(17) 0.88799(11) 0.10909(7) 0.0270(5) Uani 1 1 d . . . F12 F 0.56135(18) 0.92372(12) 0.06692(9) 0.0352(6) Uani 1 1 d . . . F13 F 0.59840(18) 0.85229(14) 0.00589(9) 0.0377(7) Uani 1 1 d . . . F14 F 0.48593(18) 0.74938(13) -0.01699(7) 0.0304(6) Uani 1 1 d . . . F15 F 0.33767(17) 0.71918(11) 0.02070(7) 0.0231(5) Uani 1 1 d . . . F21 F 0.3881(2) 0.83979(13) 0.32710(8) 0.0380(7) Uani 1 1 d . . . F22 F 0.3973(2) 0.82704(15) 0.40521(8) 0.0424(7) Uani 1 1 d . . . F23 F 0.28975(19) 0.73709(13) 0.43388(7) 0.0331(6) Uani 1 1 d . . . F24 F 0.17286(19) 0.65947(12) 0.38349(8) 0.0319(6) Uani 1 1 d . . . F25 F 0.16154(18) 0.67240(12) 0.30506(7) 0.0281(6) Uani 1 1 d . . . F26 F 0.57575(18) 0.81615(11) 0.30415(8) 0.0279(6) Uani 1 1 d . . . F27 F 0.60902(19) 0.83231(13) 0.38265(8) 0.0354(6) Uani 1 1 d . . . F28 F 0.7041(2) 0.74282(16) 0.43037(8) 0.0462(8) Uani 1 1 d . . . F29 F 0.7586(2) 0.63330(15) 0.39895(8) 0.0404(7) Uani 1 1 d . . . F30 F 0.71336(17) 0.61256(11) 0.32120(7) 0.0259(5) Uani 1 1 d . . . F31 F 0.6151(3) 0.62763(17) -0.02906(10) 0.0649(11) Uani 1 1 d . . . F32 F 0.4788(3) 0.5924(2) -0.01785(13) 0.0853(14) Uani 1 1 d . . . F33 F 0.6123(4) 0.54824(17) 0.00941(13) 0.0860(15) Uani 1 1 d . . . F34 F 0.3056(2) 0.5856(2) 0.26900(12) 0.0798(13) Uani 1 1 d . . . F35 F 0.3409(4) 0.4912(3) 0.2634(3) 0.147(3) Uani 1 1 d . . . F36 F 0.2801(2) 0.5435(3) 0.21242(13) 0.0861(15) Uani 1 1 d . . . F37 F 0.5737(3) 0.6199(2) 0.42268(10) 0.0796(14) Uani 1 1 d . . . F38 F 0.4784(3) 0.54259(16) 0.41730(11) 0.0633(10) Uani 1 1 d . . . F39 F 0.4218(3) 0.6336(2) 0.42117(10) 0.0848(16) Uani 1 1 d . . . N1 N 0.6403(2) 0.63911(15) 0.21083(10) 0.0175(7) Uani 1 1 d . . . H1 H 0.5794 0.6273 0.2020 0.021 Uiso 1 1 calc R . . N2 N 0.5411(2) 0.58399(16) 0.13360(10) 0.0185(7) Uani 1 1 d . . . H2 H 0.5294 0.6220 0.1417 0.022 Uiso 1 1 calc R . . N3 N 0.3622(2) 0.67455(14) 0.10135(9) 0.0158(6) Uani 1 1 d . . . H3 H 0.4252 0.6829 0.1029 0.019 Uiso 1 1 calc R . . N4 N 0.1808(2) 0.81891(15) 0.12846(10) 0.0171(7) Uani 1 1 d . . . H4 H 0.1873 0.7860 0.1443 0.021 Uiso 1 1 calc R . . N5 N 0.1809(2) 0.81695(16) 0.21082(10) 0.0193(7) Uani 1 1 d . . . H5 H 0.2289 0.8160 0.1971 0.023 Uiso 1 1 calc R . . N6 N 0.4362(2) 0.72375(15) 0.27495(10) 0.0178(7) Uani 1 1 d . . . H6 H 0.4456 0.7179 0.3007 0.021 Uiso 1 1 calc R . . O1 O 0.5084(2) 0.64481(16) 0.05316(10) 0.0351(8) Uani 1 1 d . . . O2 O 0.6553(3) 0.6779(2) 0.04236(11) 0.0480(10) Uani 1 1 d . . . H2A H 0.6551 0.7004 0.0624 0.072 Uiso 1 1 calc R . . O3 O 0.5069(2) 0.56819(15) 0.27348(10) 0.0305(7) Uani 1 1 d . . . O4 O 0.4620(2) 0.57581(16) 0.20819(10) 0.0317(7) Uani 1 1 d . . . O5 O 0.4917(3) 0.55939(15) 0.34341(11) 0.0396(8) Uani 1 1 d . . . H5A H 0.4840 0.5662 0.3190 0.059 Uiso 1 1 calc R . . O6 O 0.4512(2) 0.66151(14) 0.34809(9) 0.0265(7) Uani 1 1 d . . . C55 C 0.2743(3) 0.75654(19) 0.31317(12) 0.0194(8) Uani 1 1 d . . . O7 O 0.5580(2) 0.72241(14) 0.13324(9) 0.0251(6) Uani 1 1 d . . . F42 F 0.6384(2) 0.86281(13) 0.14057(9) 0.0458(8) Uani 1 1 d . . . F40 F 0.6255(3) 0.80471(15) 0.18983(9) 0.0498(8) Uani 1 1 d . . . F41 F 0.7612(2) 0.80874(15) 0.16897(11) 0.0521(9) Uani 1 1 d . . . O8 O 0.6827(2) 0.7469(2) 0.10184(11) 0.0443(9) Uani 1 1 d . . . C97 C 0.6307(3) 0.7526(2) 0.12823(12) 0.0240(9) Uani 1 1 d . . . C98 C 0.6643(3) 0.8073(2) 0.15694(14) 0.0294(10) 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 0.0155(17) 0.0177(18) 0.0154(19) 0.0007(15) 0.0031(14) 0.0011(14) C2 0.0153(17) 0.0214(19) 0.019(2) -0.0008(16) 0.0022(15) -0.0011(15) C3 0.0144(17) 0.023(2) 0.020(2) -0.0022(16) 0.0019(15) -0.0006(15) C4 0.0140(17) 0.0223(19) 0.0177(19) -0.0017(16) 0.0025(15) 0.0026(15) C5 0.0148(17) 0.0198(19) 0.020(2) -0.0011(16) 0.0040(15) 0.0027(15) C6 0.0168(18) 0.0204(19) 0.019(2) -0.0017(16) 0.0042(15) 0.0026(15) C7 0.0186(19) 0.023(2) 0.026(2) -0.0052(17) 0.0051(16) 0.0050(16) C8 0.023(2) 0.020(2) 0.022(2) -0.0056(17) 0.0019(16) 0.0014(16) C9 0.0197(18) 0.0186(19) 0.0146(19) -0.0010(15) 0.0047(15) -0.0002(15) C10 0.0174(18) 0.0188(19) 0.0164(19) -0.0022(15) 0.0051(15) -0.0035(15) C11 0.0147(17) 0.0180(18) 0.019(2) -0.0008(16) 0.0029(14) -0.0010(14) C12 0.0153(18) 0.022(2) 0.028(2) 0.0007(17) 0.0070(16) -0.0030(15) C13 0.0158(18) 0.0202(19) 0.026(2) -0.0030(17) 0.0085(16) -0.0010(15) C14 0.0149(17) 0.0214(19) 0.0163(19) -0.0019(16) 0.0044(14) 0.0016(15) C15 0.0153(17) 0.0173(18) 0.0164(19) -0.0007(15) 0.0030(14) 0.0010(14) C16 0.0141(17) 0.0190(18) 0.0157(19) -0.0014(15) 0.0027(14) -0.0008(14) C17 0.0139(16) 0.0160(18) 0.0175(19) -0.0016(15) 0.0018(14) 0.0001(14) C18 0.0123(16) 0.0181(18) 0.0176(19) -0.0001(15) 0.0014(14) -0.0008(14) C19 0.0134(16) 0.0153(17) 0.0180(19) 0.0018(15) 0.0023(14) 0.0022(14) C20 0.0142(17) 0.0170(18) 0.0185(19) 0.0006(15) 0.0027(14) 0.0006(14) C21 0.0145(17) 0.0191(19) 0.023(2) 0.0019(16) 0.0056(15) 0.0046(15) C22 0.0181(19) 0.031(2) 0.027(2) 0.0054(19) 0.0108(17) 0.0080(17) C23 0.023(2) 0.029(2) 0.024(2) 0.0075(18) 0.0125(17) 0.0074(17) C24 0.0204(19) 0.023(2) 0.019(2) 0.0046(17) 0.0065(16) 0.0060(16) C25 0.0174(18) 0.024(2) 0.018(2) 0.0029(16) 0.0062(15) 0.0045(15) C26 0.0169(18) 0.0222(19) 0.018(2) 0.0039(16) 0.0040(15) 0.0020(15) C27 0.0201(19) 0.036(2) 0.018(2) 0.0043(18) 0.0054(16) 0.0080(18) C28 0.0222(19) 0.025(2) 0.019(2) 0.0022(17) 0.0076(16) 0.0081(16) C29 0.0169(18) 0.0169(18) 0.020(2) 0.0009(16) 0.0065(15) 0.0009(14) C30 0.0172(17) 0.0159(18) 0.0163(19) 0.0002(15) 0.0032(14) -0.0015(14) C31 0.0178(18) 0.024(2) 0.022(2) -0.0066(17) 0.0030(16) 0.0012(16) C32 0.026(2) 0.034(2) 0.026(2) 0.0000(19) 0.0108(18) 0.0087(18) C33 0.031(2) 0.041(3) 0.029(3) 0.002(2) 0.0052(19) 0.018(2) C34 0.020(2) 0.039(3) 0.033(3) -0.009(2) 0.0053(18) 0.0096(19) C35 0.021(2) 0.047(3) 0.022(2) -0.006(2) 0.0090(17) -0.0022(19) C36 0.0177(19) 0.040(3) 0.021(2) -0.0032(19) 0.0031(16) 0.0039(18) C37 0.0155(17) 0.0160(18) 0.027(2) -0.0038(16) 0.0063(16) 0.0011(15) C38 0.0208(19) 0.022(2) 0.028(2) -0.0009(18) 0.0084(17) 0.0019(16) C39 0.025(2) 0.021(2) 0.049(3) 0.002(2) 0.015(2) -0.0016(17) C40 0.030(2) 0.031(3) 0.050(3) -0.009(2) -0.002(2) -0.013(2) C41 0.042(3) 0.038(3) 0.037(3) -0.003(2) -0.010(2) -0.006(2) C42 0.027(2) 0.023(2) 0.030(2) -0.0030(19) 0.0018(18) -0.0025(17) C43 0.0137(17) 0.0168(18) 0.020(2) 0.0030(15) 0.0019(15) 0.0021(14) C44 0.0179(18) 0.0180(19) 0.019(2) 0.0014(16) 0.0002(15) 0.0026(15) C45 0.0139(18) 0.026(2) 0.035(3) 0.0073(19) -0.0017(17) -0.0056(16) C46 0.0151(18) 0.033(2) 0.030(2) 0.0121(19) 0.0071(17) 0.0021(17) C47 0.0208(19) 0.030(2) 0.019(2) 0.0056(18) 0.0074(16) 0.0083(17) C48 0.0169(18) 0.0182(19) 0.021(2) 0.0029(16) 0.0028(15) 0.0020(15) C49 0.0156(18) 0.025(2) 0.022(2) 0.0083(17) 0.0064(15) 0.0040(16) C50 0.032(2) 0.026(2) 0.046(3) 0.006(2) 0.021(2) 0.0068(19) C51 0.060(3) 0.034(3) 0.089(4) 0.015(3) 0.054(3) 0.019(2) C52 0.025(2) 0.070(4) 0.093(5) 0.051(4) 0.019(3) 0.019(3) C53 0.017(2) 0.079(4) 0.058(3) 0.038(3) 0.005(2) 0.005(2) C54 0.0149(19) 0.056(3) 0.034(3) 0.021(2) 0.0059(18) -0.003(2) F16 0.0576(19) 0.0407(17) 0.0445(18) -0.0169(14) 0.0214(15) -0.0012(14) F17 0.100(3) 0.047(2) 0.152(4) 0.006(2) 0.081(3) 0.033(2) F18 0.049(2) 0.109(3) 0.163(4) 0.082(3) 0.044(2) 0.053(2) F19 0.0230(15) 0.153(4) 0.078(3) 0.063(3) -0.0136(16) -0.007(2) F20 0.0366(16) 0.078(2) 0.0324(16) -0.0069(16) 0.0001(13) -0.0266(16) C56 0.024(2) 0.025(2) 0.026(2) 0.0019(18) 0.0118(17) -0.0010(17) C57 0.026(2) 0.032(2) 0.024(2) -0.0052(19) 0.0065(18) -0.0043(18) C58 0.023(2) 0.037(2) 0.018(2) 0.0024(18) 0.0072(16) 0.0064(18) C59 0.0145(18) 0.030(2) 0.022(2) 0.0067(18) 0.0061(15) 0.0006(16) C60 0.0152(18) 0.026(2) 0.022(2) 0.0012(17) 0.0019(15) 0.0016(16) C61 0.0137(17) 0.0209(19) 0.019(2) -0.0026(16) 0.0061(15) -0.0040(15) C62 0.0167(18) 0.0202(19) 0.025(2) -0.0029(17) 0.0073(16) -0.0013(15) C63 0.021(2) 0.031(2) 0.030(2) -0.0103(19) 0.0064(18) -0.0035(17) C64 0.024(2) 0.048(3) 0.018(2) -0.009(2) 0.0023(17) -0.004(2) C65 0.020(2) 0.035(2) 0.024(2) 0.0033(19) 0.0038(17) 0.0052(18) C66 0.0128(17) 0.026(2) 0.025(2) -0.0018(17) 0.0080(15) 0.0006(15) C67 0.0133(17) 0.028(2) 0.021(2) -0.0040(17) 0.0061(15) -0.0051(15) C68 0.0171(18) 0.032(2) 0.021(2) -0.0012(18) 0.0056(16) -0.0008(17) C69 0.0168(19) 0.046(3) 0.022(2) -0.001(2) 0.0038(16) -0.0057(18) C70 0.020(2) 0.044(3) 0.028(2) -0.013(2) 0.0101(18) -0.0150(19) C71 0.030(2) 0.030(2) 0.031(2) -0.005(2) 0.0115(19) -0.0119(19) C72 0.0176(18) 0.032(2) 0.023(2) 0.0002(18) 0.0063(16) -0.0044(17) C73 0.0156(18) 0.033(2) 0.021(2) -0.0067(18) 0.0064(16) -0.0052(16) C74 0.0183(19) 0.044(3) 0.025(2) -0.005(2) 0.0064(17) 0.0012(18) C75 0.018(2) 0.055(3) 0.031(3) -0.013(2) 0.0071(18) 0.000(2) C76 0.019(2) 0.053(3) 0.034(3) -0.017(2) 0.0146(19) -0.011(2) C77 0.028(2) 0.041(3) 0.027(2) -0.006(2) 0.0129(19) -0.010(2) C78 0.0183(19) 0.033(2) 0.026(2) -0.0043(19) 0.0057(17) -0.0040(17) C79 0.0148(17) 0.0198(19) 0.018(2) 0.0031(16) 0.0038(15) 0.0035(15) C80 0.0184(18) 0.0183(19) 0.021(2) 0.0014(16) 0.0016(15) 0.0035(15) C81 0.023(2) 0.035(2) 0.014(2) 0.0016(18) 0.0033(16) 0.0103(18) C82 0.026(2) 0.033(2) 0.024(2) 0.0094(19) 0.0121(18) 0.0015(18) C83 0.029(2) 0.026(2) 0.031(2) 0.0076(19) 0.0071(19) -0.0044(18) C84 0.0216(19) 0.023(2) 0.023(2) 0.0018(17) 0.0045(16) -0.0014(16) C85 0.0145(17) 0.0176(18) 0.018(2) 0.0024(15) 0.0056(15) 0.0022(14) C86 0.0190(19) 0.022(2) 0.021(2) 0.0006(17) 0.0027(16) 0.0040(16) C87 0.025(2) 0.029(2) 0.021(2) 0.0064(18) 0.0037(17) 0.0093(17) C88 0.025(2) 0.024(2) 0.029(2) 0.0056(18) 0.0082(18) 0.0099(17) C89 0.027(2) 0.019(2) 0.034(2) -0.0040(18) 0.0089(18) 0.0023(17) C90 0.0225(19) 0.024(2) 0.021(2) 0.0002(17) 0.0027(16) 0.0003(16) C91 0.063(4) 0.040(3) 0.047(3) -0.002(3) 0.032(3) 0.005(3) C92 0.030(2) 0.036(3) 0.042(3) 0.012(2) 0.011(2) 0.010(2) C93 0.032(3) 0.061(4) 0.063(4) -0.006(3) 0.016(3) -0.011(3) C94 0.022(2) 0.029(2) 0.037(3) -0.008(2) 0.0127(19) -0.0033(17) C95 0.031(2) 0.030(2) 0.035(3) 0.013(2) 0.013(2) 0.0084(19) C96 0.0174(19) 0.029(2) 0.028(2) 0.0046(19) 0.0083(16) 0.0020(17) C99 0.064(4) 0.050(3) 0.047(3) -0.002(3) 0.021(3) 0.002(3) C100 0.080(5) 0.066(4) 0.053(4) 0.000(3) -0.005(4) 0.015(4) C101 0.087(5) 0.081(5) 0.074(5) 0.025(4) -0.039(4) -0.044(4) Cl1 0.0531(8) 0.0625(9) 0.0469(8) 0.0118(7) 0.0144(7) 0.0132(7) Cl2 0.0909(13) 0.0724(12) 0.0596(11) -0.0193(9) 0.0041(9) -0.0027(10) Cl3 0.149(2) 0.1007(16) 0.0650(13) -0.0006(12) 0.0014(13) 0.0679(16) Cl4 0.164(3) 0.149(3) 0.0696(15) 0.0215(16) -0.0317(16) -0.074(2) Cl5 0.0716(12) 0.0808(13) 0.128(2) -0.0096(13) 0.0370(13) -0.0212(10) Cl6 0.0781(13) 0.0579(11) 0.137(2) -0.0175(12) -0.0367(13) 0.0001(10) F1 0.0548(19) 0.071(2) 0.0361(17) 0.0229(16) 0.0260(15) 0.0369(17) F2 0.060(2) 0.090(3) 0.047(2) 0.0261(19) 0.0189(16) 0.057(2) F3 0.0231(13) 0.0616(19) 0.0475(18) -0.0071(15) 0.0116(12) 0.0204(13) F4 0.0317(15) 0.090(2) 0.0348(16) 0.0087(16) 0.0219(13) 0.0158(16) F5 0.0333(15) 0.079(2) 0.0303(15) 0.0182(15) 0.0115(12) 0.0224(15) F6 0.0469(16) 0.0291(14) 0.0273(14) 0.0052(11) 0.0075(12) -0.0055(12) F7 0.0388(15) 0.0264(14) 0.064(2) 0.0046(14) 0.0206(14) -0.0125(12) F8 0.052(2) 0.0482(19) 0.082(3) -0.0132(18) -0.0084(18) -0.0303(16) F9 0.086(3) 0.065(2) 0.045(2) 0.0000(18) -0.0311(19) -0.025(2) F10 0.0571(18) 0.0316(14) 0.0264(14) 0.0051(12) -0.0012(13) -0.0086(13) F11 0.0247(12) 0.0244(12) 0.0308(14) -0.0066(11) 0.0022(10) -0.0045(10) F12 0.0230(12) 0.0310(14) 0.0501(17) 0.0084(13) 0.0019(12) -0.0110(11) F13 0.0233(13) 0.0497(17) 0.0442(17) 0.0155(14) 0.0169(12) -0.0041(12) F14 0.0293(13) 0.0423(15) 0.0228(13) 0.0028(11) 0.0136(10) 0.0072(11) F15 0.0236(12) 0.0242(12) 0.0226(12) -0.0039(10) 0.0069(10) -0.0017(10) F21 0.0458(16) 0.0371(15) 0.0353(16) -0.0022(13) 0.0183(13) -0.0181(13) F22 0.0431(16) 0.0532(18) 0.0308(15) -0.0124(14) 0.0060(13) -0.0185(14) F23 0.0318(14) 0.0504(17) 0.0175(13) 0.0025(12) 0.0054(10) 0.0021(12) F24 0.0338(14) 0.0356(14) 0.0282(14) 0.0100(12) 0.0105(11) -0.0064(11) F25 0.0266(12) 0.0332(14) 0.0239(13) -0.0012(11) 0.0025(10) -0.0079(11) F26 0.0296(13) 0.0195(12) 0.0350(15) -0.0007(11) 0.0068(11) 0.0026(10) F27 0.0346(14) 0.0365(15) 0.0368(16) -0.0216(13) 0.0104(12) -0.0021(12) F28 0.0440(16) 0.072(2) 0.0201(14) -0.0143(14) -0.0006(12) 0.0074(15) F29 0.0360(15) 0.0591(19) 0.0243(14) 0.0089(13) 0.0005(12) 0.0215(14) F30 0.0228(12) 0.0260(12) 0.0286(13) 0.0003(11) 0.0040(10) 0.0070(10) F31 0.100(3) 0.060(2) 0.047(2) 0.0087(17) 0.049(2) 0.020(2) F32 0.090(3) 0.105(3) 0.064(3) -0.038(3) 0.024(2) -0.030(3) F33 0.157(4) 0.042(2) 0.078(3) 0.0091(19) 0.071(3) 0.035(2) F34 0.0357(18) 0.140(4) 0.071(3) -0.025(3) 0.0273(18) 0.006(2) F35 0.061(3) 0.089(4) 0.296(9) 0.084(5) 0.044(4) -0.025(3) F36 0.0293(17) 0.155(4) 0.077(3) -0.050(3) 0.0179(18) -0.031(2) F37 0.068(2) 0.137(4) 0.0291(18) 0.017(2) -0.0042(17) -0.046(3) F38 0.098(3) 0.0423(19) 0.053(2) 0.0243(16) 0.021(2) 0.0037(18) F39 0.114(3) 0.111(3) 0.040(2) 0.036(2) 0.046(2) 0.080(3) N1 0.0098(14) 0.0222(16) 0.0213(17) -0.0033(14) 0.0054(12) -0.0007(12) N2 0.0157(15) 0.0199(16) 0.0203(17) -0.0024(14) 0.0039(13) 0.0020(13) N3 0.0128(14) 0.0157(15) 0.0198(17) -0.0005(13) 0.0055(12) -0.0003(12) N4 0.0166(15) 0.0175(16) 0.0188(17) 0.0030(13) 0.0071(13) 0.0039(12) N5 0.0137(15) 0.0262(18) 0.0196(17) 0.0061(14) 0.0073(13) 0.0079(13) N6 0.0161(15) 0.0220(16) 0.0155(16) 0.0000(14) 0.0035(12) 0.0023(13) O1 0.0336(18) 0.0424(19) 0.0317(18) 0.0016(15) 0.0125(15) 0.0037(15) O2 0.0338(19) 0.073(3) 0.041(2) 0.004(2) 0.0164(16) 0.0044(18) O3 0.0290(16) 0.0309(17) 0.0334(18) -0.0024(14) 0.0103(14) -0.0019(13) O4 0.0235(15) 0.0405(19) 0.0325(18) -0.0092(15) 0.0086(13) -0.0081(14) O5 0.056(2) 0.0299(18) 0.037(2) 0.0036(15) 0.0186(17) 0.0070(16) O6 0.0278(15) 0.0290(16) 0.0233(16) 0.0073(13) 0.0065(12) 0.0061(13) C55 0.0173(18) 0.024(2) 0.018(2) 0.0066(16) 0.0056(15) 0.0060(15) O7 0.0231(14) 0.0264(15) 0.0269(16) -0.0011(13) 0.0076(12) -0.0043(12) F42 0.0572(19) 0.0314(15) 0.0420(18) 0.0066(13) -0.0099(15) -0.0024(14) F40 0.070(2) 0.0495(18) 0.0333(16) -0.0097(14) 0.0168(15) -0.0294(16) F41 0.0275(14) 0.0534(19) 0.069(2) -0.0113(17) -0.0095(14) -0.0057(14) O8 0.0304(18) 0.070(3) 0.035(2) -0.0085(19) 0.0134(15) -0.0141(17) C97 0.0214(19) 0.031(2) 0.019(2) 0.0074(18) 0.0023(16) -0.0004(17) C98 0.026(2) 0.031(2) 0.030(2) 0.009(2) 0.0008(18) -0.0076(18) _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 N1 1.369(5) . ? C1 C30 1.409(5) . ? C1 C2 1.437(5) . ? C2 C3 1.384(6) . ? C2 C67 1.484(5) . ? C3 C4 1.445(5) . ? C3 C73 1.480(5) . ? C4 N1 1.375(5) . ? C4 C5 1.406(6) . ? C5 C6 1.400(5) . ? C5 C31 1.499(5) . ? C6 N2 1.368(5) . ? C6 C7 1.426(6) . ? C7 C8 1.360(6) . ? C7 H7 0.9500 . ? C8 C9 1.426(5) . ? C8 H8 0.9500 . ? C9 N2 1.376(5) . ? C9 C10 1.396(5) . ? C10 C11 1.405(5) . ? C10 C37 1.487(5) . ? C11 N3 1.373(5) . ? C11 C12 1.420(5) . ? C12 C13 1.363(6) . ? C12 H12 0.9500 . ? C13 C14 1.422(5) . ? C13 H13 0.9500 . ? C14 N3 1.375(5) . ? C14 C15 1.411(5) . ? C15 C16 1.410(5) . ? C15 C43 1.470(5) . ? C16 N4 1.380(5) . ? C16 C17 1.422(5) . ? C17 C18 1.388(5) . ? C17 C79 1.475(5) . ? C18 C19 1.414(5) . ? C18 C85 1.495(5) . ? C19 N4 1.370(5) . ? C19 C20 1.420(5) . ? C20 C21 1.387(6) . ? C20 C49 1.479(5) . ? C21 N5 1.394(5) . ? C21 C22 1.423(6) . ? C22 C23 1.363(6) . ? C22 H22 0.9500 . ? C23 C24 1.423(6) . ? C23 H23 0.9500 . ? C24 N5 1.381(5) . ? C24 C25 1.402(5) . ? C25 C26 1.406(5) . ? C25 C55 1.491(5) . ? C26 N6 1.368(5) . ? C26 C27 1.437(6) . ? C27 C28 1.353(6) . ? C27 H27 0.9500 . ? C28 C29 1.421(6) . ? C28 H28 0.9500 . ? C29 N6 1.367(5) . ? C29 C30 1.410(5) . ? C30 C61 1.481(5) . ? C31 C32 1.382(6) . ? C31 C36 1.385(6) . ? C32 F1 1.335(5) . ? C32 C33 1.378(6) . ? C33 F2 1.345(5) . ? C33 C34 1.368(7) . ? C34 F3 1.345(5) . ? C34 C35 1.364(7) . ? C35 F4 1.336(5) . ? C35 C36 1.384(6) . ? C36 F5 1.328(5) . ? C37 C38 1.384(6) . ? C37 C42 1.395(6) . ? C38 F6 1.331(5) . ? C38 C39 1.391(6) . ? C39 F7 1.342(5) . ? C39 C40 1.349(7) . ? C40 F8 1.335(5) . ? C40 C41 1.378(8) . ? C41 F9 1.338(6) . ? C41 C42 1.390(6) . ? C42 F10 1.332(5) . ? C43 C48 1.387(6) . ? C43 C44 1.396(5) . ? C44 F11 1.336(5) . ? C44 C45 1.378(6) . ? C45 F12 1.335(5) . ? C45 C46 1.374(7) . ? C46 F13 1.336(5) . ? C46 C47 1.381(6) . ? C47 F14 1.340(5) . ? C47 C48 1.381(6) . ? C48 F15 1.344(5) . ? C49 C50 1.373(6) . ? C49 C54 1.401(6) . ? C50 F16 1.332(6) . ? C50 C51 1.392(7) . ? C51 F17 1.339(7) . ? C51 C52 1.392(10) . ? C52 C53 1.340(10) . ? C52 F18 1.353(6) . ? C53 F19 1.328(7) . ? C53 C54 1.359(7) . ? C54 F20 1.337(6) . ? C56 F21 1.346(5) . ? C56 C57 1.377(6) . ? C56 C55 1.382(6) . ? C57 F22 1.339(5) . ? C57 C58 1.379(6) . ? C58 F23 1.333(5) . ? C58 C59 1.372(6) . ? C59 F24 1.342(5) . ? C59 C60 1.381(6) . ? C60 F25 1.342(5) . ? C60 C55 1.386(6) . ? C61 C66 1.384(6) . ? C61 C62 1.405(5) . ? C62 F26 1.325(5) . ? C62 C63 1.374(6) . ? C63 F27 1.339(5) . ? C63 C64 1.378(7) . ? C64 F28 1.343(5) . ? C64 C65 1.377(7) . ? C65 F29 1.336(5) . ? C65 C66 1.375(6) . ? C66 F30 1.345(5) . ? C67 C72 1.388(6) . ? C67 C68 1.397(6) . ? C68 C69 1.386(6) . ? C68 H68 0.9500 . ? C69 C70 1.369(7) . ? C69 H69 0.9500 . ? C70 C71 1.386(7) . ? C70 H70 0.9500 . ? C71 C72 1.395(6) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.387(6) . ? C73 C78 1.392(6) . ? C74 C75 1.393(6) . ? C74 H74 0.9500 . ? C75 C76 1.392(7) . ? C75 H75 0.9500 . ? C76 C77 1.372(7) . ? C76 H76 0.9500 . ? C77 C78 1.387(6) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C84 1.398(6) . ? C79 C80 1.400(6) . ? C80 C81 1.381(6) . ? C80 H80 0.9500 . ? C81 C82 1.388(6) . ? C81 H81 0.9500 . ? C82 C83 1.389(7) . ? C82 H82 0.9500 . ? C83 C84 1.385(6) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C90 1.383(6) . ? C85 C86 1.398(5) . ? C86 C87 1.391(6) . ? C86 H86 0.9500 . ? C87 C88 1.377(6) . ? C87 H87 0.9500 . ? C88 C89 1.387(6) . ? C88 H88 0.9500 . ? C89 C90 1.385(6) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 F32 1.321(8) . ? C91 F33 1.333(7) . ? C91 F31 1.333(6) . ? C91 C92 1.533(8) . ? C92 O1 1.206(6) . ? C92 O2 1.273(6) . ? C93 F35 1.285(8) . ? C93 F36 1.297(7) . ? C93 F34 1.353(7) . ? C93 C94 1.543(7) . ? C94 O4 1.226(6) . ? C94 O3 1.255(6) . ? C95 F38 1.298(6) . ? C95 F39 1.309(6) . ? C95 F37 1.315(6) . ? C95 C96 1.537(6) . ? C96 O6 1.211(5) . ? C96 O5 1.277(5) . ? C99 Cl1 1.752(6) . ? C99 Cl2 1.772(6) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 Cl4 1.707(8) . ? C100 Cl3 1.764(7) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 Cl5 1.708(9) . ? C101 Cl6 1.863(10) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? N1 H1 0.8800 . ? N2 H2 0.8800 . ? N3 H3 0.8800 . ? N4 H4 0.8800 . ? N5 H5 0.8800 . ? N6 H6 0.8800 . ? O2 H2A 0.8400 . ? O5 H5A 0.8400 . ? O7 C97 1.229(5) . ? F42 C98 1.330(5) . ? F40 C98 1.335(6) . ? F41 C98 1.332(5) . ? O8 C97 1.258(5) . ? C97 C98 1.543(6) . ? 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 N1 C1 C30 124.0(3) . . ? N1 C1 C2 107.3(3) . . ? C30 C1 C2 128.6(4) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 C67 128.0(3) . . ? C1 C2 C67 124.1(4) . . ? C2 C3 C4 107.7(3) . . ? C2 C3 C73 125.9(4) . . ? C4 C3 C73 126.0(4) . . ? N1 C4 C5 124.1(3) . . ? N1 C4 C3 106.7(3) . . ? C5 C4 C3 128.8(3) . . ? C6 C5 C4 125.5(3) . . ? C6 C5 C31 116.1(3) . . ? C4 C5 C31 118.2(3) . . ? N2 C6 C5 125.8(4) . . ? N2 C6 C7 106.9(3) . . ? C5 C6 C7 127.0(4) . . ? C8 C7 C6 108.0(3) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? C7 C8 C9 108.3(4) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? N2 C9 C10 126.9(4) . . ? N2 C9 C8 106.6(3) . . ? C10 C9 C8 126.6(4) . . ? C9 C10 C11 128.2(4) . . ? C9 C10 C37 118.6(3) . . ? C11 C10 C37 113.2(3) . . ? N3 C11 C10 127.6(3) . . ? N3 C11 C12 106.6(3) . . ? C10 C11 C12 125.7(3) . . ? C13 C12 C11 108.6(3) . . ? C13 C12 H12 125.7 . . ? C11 C12 H12 125.7 . . ? C12 C13 C14 107.8(3) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? N3 C14 C15 125.1(3) . . ? N3 C14 C13 106.8(3) . . ? C15 C14 C13 127.0(3) . . ? C16 C15 C14 119.7(3) . . ? C16 C15 C43 121.4(3) . . ? C14 C15 C43 118.8(3) . . ? N4 C16 C15 121.8(3) . . ? N4 C16 C17 106.5(3) . . ? C15 C16 C17 131.7(4) . . ? C18 C17 C16 107.7(3) . . ? C18 C17 C79 126.5(3) . . ? C16 C17 C79 125.8(3) . . ? C17 C18 C19 108.2(3) . . ? C17 C18 C85 125.4(3) . . ? C19 C18 C85 126.3(3) . . ? N4 C19 C18 106.8(3) . . ? N4 C19 C20 122.3(3) . . ? C18 C19 C20 130.8(3) . . ? C21 C20 C19 122.9(3) . . ? C21 C20 C49 118.3(3) . . ? C19 C20 C49 118.7(3) . . ? C20 C21 N5 123.1(3) . . ? C20 C21 C22 130.8(4) . . ? N5 C21 C22 106.1(3) . . ? C23 C22 C21 108.8(4) . . ? C23 C22 H22 125.6 . . ? C21 C22 H22 125.6 . . ? C22 C23 C24 108.4(4) . . ? C22 C23 H23 125.8 . . ? C24 C23 H23 125.8 . . ? N5 C24 C25 123.7(4) . . ? N5 C24 C23 106.7(3) . . ? C25 C24 C23 129.5(4) . . ? C24 C25 C26 123.4(4) . . ? C24 C25 C55 117.3(3) . . ? C26 C25 C55 119.2(3) . . ? N6 C26 C25 122.4(4) . . ? N6 C26 C27 105.3(3) . . ? C25 C26 C27 132.3(4) . . ? C28 C27 C26 109.3(4) . . ? C28 C27 H27 125.4 . . ? C26 C27 H27 125.4 . . ? C27 C28 C29 107.4(4) . . ? C27 C28 H28 126.3 . . ? C29 C28 H28 126.3 . . ? N6 C29 C30 122.8(4) . . ? N6 C29 C28 107.2(3) . . ? C30 C29 C28 129.5(4) . . ? C1 C30 C29 121.5(4) . . ? C1 C30 C61 120.8(3) . . ? C29 C30 C61 117.7(3) . . ? C32 C31 C36 116.8(4) . . ? C32 C31 C5 121.9(4) . . ? C36 C31 C5 121.3(4) . . ? F1 C32 C33 117.7(4) . . ? F1 C32 C31 120.0(4) . . ? C33 C32 C31 122.3(4) . . ? F2 C33 C34 120.1(4) . . ? F2 C33 C32 120.7(4) . . ? C34 C33 C32 119.2(4) . . ? F3 C34 C35 119.8(4) . . ? F3 C34 C33 119.7(4) . . ? C35 C34 C33 120.5(4) . . ? F4 C35 C34 119.6(4) . . ? F4 C35 C36 120.7(4) . . ? C34 C35 C36 119.7(4) . . ? F5 C36 C35 118.4(4) . . ? F5 C36 C31 119.9(4) . . ? C35 C36 C31 121.5(4) . . ? C38 C37 C42 116.9(4) . . ? C38 C37 C10 123.7(4) . . ? C42 C37 C10 119.1(4) . . ? F6 C38 C37 120.0(4) . . ? F6 C38 C39 118.7(4) . . ? C37 C38 C39 121.3(4) . . ? F7 C39 C40 119.9(4) . . ? F7 C39 C38 119.6(4) . . ? C40 C39 C38 120.5(4) . . ? F8 C40 C39 120.3(5) . . ? F8 C40 C41 119.2(5) . . ? C39 C40 C41 120.5(4) . . ? F9 C41 C40 121.3(4) . . ? F9 C41 C42 119.7(5) . . ? C40 C41 C42 119.1(5) . . ? F10 C42 C41 118.3(4) . . ? F10 C42 C37 119.9(4) . . ? C41 C42 C37 121.7(4) . . ? C48 C43 C44 116.2(4) . . ? C48 C43 C15 121.6(3) . . ? C44 C43 C15 122.1(4) . . ? F11 C44 C45 118.2(4) . . ? F11 C44 C43 119.9(4) . . ? C45 C44 C43 121.9(4) . . ? F12 C45 C46 119.9(4) . . ? F12 C45 C44 120.1(4) . . ? C46 C45 C44 120.0(4) . . ? F13 C46 C45 120.2(4) . . ? F13 C46 C47 119.9(4) . . ? C45 C46 C47 119.9(4) . . ? F14 C47 C46 120.1(4) . . ? F14 C47 C48 120.7(4) . . ? C46 C47 C48 119.1(4) . . ? F15 C48 C47 117.5(4) . . ? F15 C48 C43 119.7(3) . . ? C47 C48 C43 122.8(4) . . ? C50 C49 C54 117.5(4) . . ? C50 C49 C20 123.3(4) . . ? C54 C49 C20 119.1(4) . . ? F16 C50 C49 119.9(4) . . ? F16 C50 C51 119.4(5) . . ? C49 C50 C51 120.5(5) . . ? F17 C51 C50 118.2(7) . . ? F17 C51 C52 122.8(6) . . ? C50 C51 C52 118.9(6) . . ? C53 C52 F18 122.1(7) . . ? C53 C52 C51 121.5(5) . . ? F18 C52 C51 116.4(7) . . ? F19 C53 C52 120.9(5) . . ? F19 C53 C54 120.1(7) . . ? C52 C53 C54 119.1(6) . . ? F20 C54 C53 117.4(5) . . ? F20 C54 C49 120.1(4) . . ? C53 C54 C49 122.4(6) . . ? F21 C56 C57 117.1(4) . . ? F21 C56 C55 119.8(4) . . ? C57 C56 C55 123.1(4) . . ? F22 C57 C56 121.1(4) . . ? F22 C57 C58 119.5(4) . . ? C56 C57 C58 119.4(4) . . ? F23 C58 C59 120.4(4) . . ? F23 C58 C57 120.2(4) . . ? C59 C58 C57 119.4(4) . . ? F24 C59 C58 119.8(4) . . ? F24 C59 C60 120.2(4) . . ? C58 C59 C60 120.0(4) . . ? F25 C60 C59 118.1(4) . . ? F25 C60 C55 119.6(4) . . ? C59 C60 C55 122.3(4) . . ? C66 C61 C62 116.4(4) . . ? C66 C61 C30 122.7(4) . . ? C62 C61 C30 120.8(4) . . ? F26 C62 C63 118.1(4) . . ? F26 C62 C61 120.2(4) . . ? C63 C62 C61 121.7(4) . . ? F27 C63 C62 120.5(4) . . ? F27 C63 C64 119.7(4) . . ? C62 C63 C64 119.8(4) . . ? F28 C64 C65 120.6(4) . . ? F28 C64 C63 119.3(4) . . ? C65 C64 C63 120.1(4) . . ? F29 C65 C66 120.6(4) . . ? F29 C65 C64 120.0(4) . . ? C66 C65 C64 119.4(4) . . ? F30 C66 C65 117.4(4) . . ? F30 C66 C61 120.0(4) . . ? C65 C66 C61 122.6(4) . . ? C72 C67 C68 118.9(4) . . ? C72 C67 C2 119.9(4) . . ? C68 C67 C2 121.1(4) . . ? C69 C68 C67 120.3(4) . . ? C69 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? C70 C69 C68 120.4(4) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? C69 C70 C71 120.4(4) . . ? C69 C70 H70 119.8 . . ? C71 C70 H70 119.8 . . ? C70 C71 C72 119.5(4) . . ? C70 C71 H71 120.3 . . ? C72 C71 H71 120.3 . . ? C67 C72 C71 120.5(4) . . ? C67 C72 H72 119.7 . . ? C71 C72 H72 119.7 . . ? C74 C73 C78 119.2(4) . . ? C74 C73 C3 120.8(4) . . ? C78 C73 C3 120.0(4) . . ? C73 C74 C75 120.2(4) . . ? C73 C74 H74 119.9 . . ? C75 C74 H74 119.9 . . ? C76 C75 C74 119.9(4) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C77 C76 C75 120.1(4) . . ? C77 C76 H76 119.9 . . ? C75 C76 H76 119.9 . . ? C76 C77 C78 120.1(4) . . ? C76 C77 H77 119.9 . . ? C78 C77 H77 119.9 . . ? C77 C78 C73 120.5(4) . . ? C77 C78 H78 119.7 . . ? C73 C78 H78 119.7 . . ? C84 C79 C80 118.7(4) . . ? C84 C79 C17 120.4(4) . . ? C80 C79 C17 120.9(4) . . ? C81 C80 C79 120.8(4) . . ? C81 C80 H80 119.6 . . ? C79 C80 H80 119.6 . . ? C80 C81 C82 119.9(4) . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C83 C82 C81 119.9(4) . . ? C83 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C84 C83 C82 120.3(4) . . ? C84 C83 H83 119.9 . . ? C82 C83 H83 119.9 . . ? C83 C84 C79 120.3(4) . . ? C83 C84 H84 119.8 . . ? C79 C84 H84 119.8 . . ? C90 C85 C86 120.2(4) . . ? C90 C85 C18 121.6(3) . . ? C86 C85 C18 118.2(3) . . ? C87 C86 C85 119.1(4) . . ? C87 C86 H86 120.4 . . ? C85 C86 H86 120.4 . . ? C88 C87 C86 120.7(4) . . ? C88 C87 H87 119.7 . . ? C86 C87 H87 119.7 . . ? C87 C88 C89 119.9(4) . . ? C87 C88 H88 120.1 . . ? C89 C88 H88 120.1 . . ? C90 C89 C88 120.2(4) . . ? C90 C89 H89 119.9 . . ? C88 C89 H89 119.9 . . ? C85 C90 C89 120.0(4) . . ? C85 C90 H90 120.0 . . ? C89 C90 H90 120.0 . . ? F32 C91 F33 107.2(5) . . ? F32 C91 F31 106.4(5) . . ? F33 C91 F31 107.4(4) . . ? F32 C91 C92 111.8(5) . . ? F33 C91 C92 110.0(5) . . ? F31 C91 C92 113.7(5) . . ? O1 C92 O2 129.3(5) . . ? O1 C92 C91 118.0(5) . . ? O2 C92 C91 112.7(5) . . ? F35 C93 F36 110.5(6) . . ? F35 C93 F34 104.2(6) . . ? F36 C93 F34 105.9(5) . . ? F35 C93 C94 112.0(5) . . ? F36 C93 C94 114.6(5) . . ? F34 C93 C94 109.0(5) . . ? O4 C94 O3 127.9(4) . . ? O4 C94 C93 116.7(4) . . ? O3 C94 C93 115.4(4) . . ? F38 C95 F39 107.3(4) . . ? F38 C95 F37 106.5(4) . . ? F39 C95 F37 107.2(5) . . ? F38 C95 C96 114.7(4) . . ? F39 C95 C96 111.4(4) . . ? F37 C95 C96 109.3(4) . . ? O6 C96 O5 130.0(4) . . ? O6 C96 C95 117.7(4) . . ? O5 C96 C95 112.2(4) . . ? Cl1 C99 Cl2 110.8(3) . . ? Cl1 C99 H99A 109.5 . . ? Cl2 C99 H99A 109.5 . . ? Cl1 C99 H99B 109.5 . . ? Cl2 C99 H99B 109.5 . . ? H99A C99 H99B 108.1 . . ? Cl4 C100 Cl3 115.9(5) . . ? Cl4 C100 H10A 108.3 . . ? Cl3 C100 H10A 108.3 . . ? Cl4 C100 H10B 108.3 . . ? Cl3 C100 H10B 108.3 . . ? H10A C100 H10B 107.4 . . ? Cl5 C101 Cl6 108.6(4) . . ? Cl5 C101 H10C 110.0 . . ? Cl6 C101 H10C 110.0 . . ? Cl5 C101 H10D 110.0 . . ? Cl6 C101 H10D 110.0 . . ? H10C C101 H10D 108.3 . . ? C1 N1 C4 110.7(3) . . ? C1 N1 H1 124.7 . . ? C4 N1 H1 124.7 . . ? C6 N2 C9 110.1(3) . . ? C6 N2 H2 124.9 . . ? C9 N2 H2 124.9 . . ? C11 N3 C14 110.1(3) . . ? C11 N3 H3 125.0 . . ? C14 N3 H3 125.0 . . ? C19 N4 C16 110.7(3) . . ? C19 N4 H4 124.6 . . ? C16 N4 H4 124.6 . . ? C24 N5 C21 109.9(3) . . ? C24 N5 H5 125.1 . . ? C21 N5 H5 125.1 . . ? C29 N6 C26 110.8(3) . . ? C29 N6 H6 124.6 . . ? C26 N6 H6 124.6 . . ? C92 O2 H2A 109.5 . . ? C96 O5 H5A 109.5 . . ? C56 C55 C60 115.8(4) . . ? C56 C55 C25 121.6(4) . . ? C60 C55 C25 122.5(4) . . ? O7 C97 O8 129.3(4) . . ? O7 C97 C98 117.8(4) . . ? O8 C97 C98 112.8(4) . . ? F42 C98 F41 107.1(4) . . ? F42 C98 F40 106.1(4) . . ? F41 C98 F40 105.6(4) . . ? F42 C98 C97 111.6(4) . . ? F41 C98 C97 113.0(4) . . ? F40 C98 C97 113.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.7(4) . . . . ? C30 C1 C2 C3 -177.8(4) . . . . ? N1 C1 C2 C67 174.5(4) . . . . ? C30 C1 C2 C67 -4.0(7) . . . . ? C1 C2 C3 C4 -2.4(5) . . . . ? C67 C2 C3 C4 -175.9(4) . . . . ? C1 C2 C3 C73 170.1(4) . . . . ? C67 C2 C3 C73 -3.4(7) . . . . ? C2 C3 C4 N1 3.3(5) . . . . ? C73 C3 C4 N1 -169.2(4) . . . . ? C2 C3 C4 C5 -169.7(4) . . . . ? C73 C3 C4 C5 17.8(7) . . . . ? N1 C4 C5 C6 15.9(7) . . . . ? C3 C4 C5 C6 -172.2(4) . . . . ? N1 C4 C5 C31 -158.9(4) . . . . ? C3 C4 C5 C31 12.9(6) . . . . ? C4 C5 C6 N2 21.5(7) . . . . ? C31 C5 C6 N2 -163.5(4) . . . . ? C4 C5 C6 C7 -152.2(4) . . . . ? C31 C5 C6 C7 22.7(6) . . . . ? N2 C6 C7 C8 -2.7(5) . . . . ? C5 C6 C7 C8 172.0(4) . . . . ? C6 C7 C8 C9 2.7(5) . . . . ? C7 C8 C9 N2 -1.8(5) . . . . ? C7 C8 C9 C10 178.5(4) . . . . ? N2 C9 C10 C11 11.3(7) . . . . ? C8 C9 C10 C11 -168.9(4) . . . . ? N2 C9 C10 C37 -171.6(4) . . . . ? C8 C9 C10 C37 8.1(6) . . . . ? C9 C10 C11 N3 23.6(7) . . . . ? C37 C10 C11 N3 -153.6(4) . . . . ? C9 C10 C11 C12 -160.7(4) . . . . ? C37 C10 C11 C12 22.1(6) . . . . ? N3 C11 C12 C13 0.3(5) . . . . ? C10 C11 C12 C13 -176.2(4) . . . . ? C11 C12 C13 C14 1.9(5) . . . . ? C12 C13 C14 N3 -3.4(5) . . . . ? C12 C13 C14 C15 165.3(4) . . . . ? N3 C14 C15 C16 -161.1(4) . . . . ? C13 C14 C15 C16 32.1(6) . . . . ? N3 C14 C15 C43 22.1(6) . . . . ? C13 C14 C15 C43 -144.8(4) . . . . ? C14 C15 C16 N4 27.5(6) . . . . ? C43 C15 C16 N4 -155.7(4) . . . . ? C14 C15 C16 C17 -152.6(4) . . . . ? C43 C15 C16 C17 24.2(6) . . . . ? N4 C16 C17 C18 -1.2(4) . . . . ? C15 C16 C17 C18 178.9(4) . . . . ? N4 C16 C17 C79 179.5(3) . . . . ? C15 C16 C17 C79 -0.5(7) . . . . ? C16 C17 C18 C19 2.2(4) . . . . ? C79 C17 C18 C19 -178.5(4) . . . . ? C16 C17 C18 C85 -178.7(3) . . . . ? C79 C17 C18 C85 0.6(6) . . . . ? C17 C18 C19 N4 -2.4(4) . . . . ? C85 C18 C19 N4 178.6(3) . . . . ? C17 C18 C19 C20 175.6(4) . . . . ? C85 C18 C19 C20 -3.5(7) . . . . ? N4 C19 C20 C21 23.6(6) . . . . ? C18 C19 C20 C21 -154.1(4) . . . . ? N4 C19 C20 C49 -155.9(4) . . . . ? C18 C19 C20 C49 26.4(6) . . . . ? C19 C20 C21 N5 14.2(6) . . . . ? C49 C20 C21 N5 -166.3(4) . . . . ? C19 C20 C21 C22 -166.5(4) . . . . ? C49 C20 C21 C22 13.0(7) . . . . ? C20 C21 C22 C23 -177.9(4) . . . . ? N5 C21 C22 C23 1.5(5) . . . . ? C21 C22 C23 C24 -0.6(5) . . . . ? C22 C23 C24 N5 -0.5(5) . . . . ? C22 C23 C24 C25 179.6(4) . . . . ? N5 C24 C25 C26 -13.3(7) . . . . ? C23 C24 C25 C26 166.5(4) . . . . ? N5 C24 C25 C55 162.9(4) . . . . ? C23 C24 C25 C55 -17.2(7) . . . . ? C24 C25 C26 N6 173.0(4) . . . . ? C55 C25 C26 N6 -3.2(6) . . . . ? C24 C25 C26 C27 -6.8(7) . . . . ? C55 C25 C26 C27 177.0(4) . . . . ? N6 C26 C27 C28 -1.5(5) . . . . ? C25 C26 C27 C28 178.3(4) . . . . ? C26 C27 C28 C29 -0.4(5) . . . . ? C27 C28 C29 N6 2.3(5) . . . . ? C27 C28 C29 C30 -169.4(4) . . . . ? N1 C1 C30 C29 -28.7(6) . . . . ? C2 C1 C30 C29 149.6(4) . . . . ? N1 C1 C30 C61 151.1(4) . . . . ? C2 C1 C30 C61 -30.5(6) . . . . ? N6 C29 C30 C1 167.1(4) . . . . ? C28 C29 C30 C1 -22.4(6) . . . . ? N6 C29 C30 C61 -12.7(6) . . . . ? C28 C29 C30 C61 157.8(4) . . . . ? C6 C5 C31 C32 -113.3(5) . . . . ? C4 C5 C31 C32 62.0(6) . . . . ? C6 C5 C31 C36 69.4(5) . . . . ? C4 C5 C31 C36 -115.3(5) . . . . ? C36 C31 C32 F1 178.4(4) . . . . ? C5 C31 C32 F1 1.0(7) . . . . ? C36 C31 C32 C33 0.9(7) . . . . ? C5 C31 C32 C33 -176.5(4) . . . . ? F1 C32 C33 F2 0.8(7) . . . . ? C31 C32 C33 F2 178.4(5) . . . . ? F1 C32 C33 C34 -177.5(5) . . . . ? C31 C32 C33 C34 0.0(8) . . . . ? F2 C33 C34 F3 0.4(7) . . . . ? C32 C33 C34 F3 178.8(4) . . . . ? F2 C33 C34 C35 -178.3(5) . . . . ? C32 C33 C34 C35 0.1(8) . . . . ? F3 C34 C35 F4 -0.6(7) . . . . ? C33 C34 C35 F4 178.0(5) . . . . ? F3 C34 C35 C36 -179.8(4) . . . . ? C33 C34 C35 C36 -1.2(7) . . . . ? F4 C35 C36 F5 -0.9(7) . . . . ? C34 C35 C36 F5 178.3(4) . . . . ? F4 C35 C36 C31 -177.0(4) . . . . ? C34 C35 C36 C31 2.2(7) . . . . ? C32 C31 C36 F5 -178.1(4) . . . . ? C5 C31 C36 F5 -0.7(6) . . . . ? C32 C31 C36 C35 -2.0(7) . . . . ? C5 C31 C36 C35 175.4(4) . . . . ? C9 C10 C37 C38 70.8(5) . . . . ? C11 C10 C37 C38 -111.7(4) . . . . ? C9 C10 C37 C42 -115.1(4) . . . . ? C11 C10 C37 C42 62.4(5) . . . . ? C42 C37 C38 F6 -177.2(4) . . . . ? C10 C37 C38 F6 -3.0(6) . . . . ? C42 C37 C38 C39 1.0(6) . . . . ? C10 C37 C38 C39 175.2(4) . . . . ? F6 C38 C39 F7 -1.0(6) . . . . ? C37 C38 C39 F7 -179.3(4) . . . . ? F6 C38 C39 C40 177.0(4) . . . . ? C37 C38 C39 C40 -1.2(7) . . . . ? F7 C39 C40 F8 -1.8(7) . . . . ? C38 C39 C40 F8 -179.8(4) . . . . ? F7 C39 C40 C41 178.7(5) . . . . ? C38 C39 C40 C41 0.7(8) . . . . ? F8 C40 C41 F9 0.3(8) . . . . ? C39 C40 C41 F9 179.8(5) . . . . ? F8 C40 C41 C42 -179.5(5) . . . . ? C39 C40 C41 C42 0.1(8) . . . . ? F9 C41 C42 F10 0.7(8) . . . . ? C40 C41 C42 F10 -179.5(5) . . . . ? F9 C41 C42 C37 179.9(5) . . . . ? C40 C41 C42 C37 -0.3(8) . . . . ? C38 C37 C42 F10 179.0(4) . . . . ? C10 C37 C42 F10 4.5(6) . . . . ? C38 C37 C42 C41 -0.2(7) . . . . ? C10 C37 C42 C41 -174.7(4) . . . . ? C16 C15 C43 C48 -130.0(4) . . . . ? C14 C15 C43 C48 46.8(5) . . . . ? C16 C15 C43 C44 47.2(5) . . . . ? C14 C15 C43 C44 -136.0(4) . . . . ? C48 C43 C44 F11 -179.9(3) . . . . ? C15 C43 C44 F11 2.8(6) . . . . ? C48 C43 C44 C45 0.4(6) . . . . ? C15 C43 C44 C45 -176.9(4) . . . . ? F11 C44 C45 F12 -2.0(6) . . . . ? C43 C44 C45 F12 177.7(3) . . . . ? F11 C44 C45 C46 177.5(4) . . . . ? C43 C44 C45 C46 -2.8(6) . . . . ? F12 C45 C46 F13 2.4(6) . . . . ? C44 C45 C46 F13 -177.1(4) . . . . ? F12 C45 C46 C47 -177.9(4) . . . . ? C44 C45 C46 C47 2.6(6) . . . . ? F13 C46 C47 F14 -1.5(6) . . . . ? C45 C46 C47 F14 178.9(4) . . . . ? F13 C46 C47 C48 179.6(4) . . . . ? C45 C46 C47 C48 0.0(6) . . . . ? F14 C47 C48 F15 -4.4(5) . . . . ? C46 C47 C48 F15 174.5(3) . . . . ? F14 C47 C48 C43 178.6(3) . . . . ? C46 C47 C48 C43 -2.5(6) . . . . ? C44 C43 C48 F15 -174.6(3) . . . . ? C15 C43 C48 F15 2.6(5) . . . . ? C44 C43 C48 C47 2.3(6) . . . . ? C15 C43 C48 C47 179.6(4) . . . . ? C21 C20 C49 C50 58.0(6) . . . . ? C19 C20 C49 C50 -122.4(5) . . . . ? C21 C20 C49 C54 -124.4(4) . . . . ? C19 C20 C49 C54 55.2(5) . . . . ? C54 C49 C50 F16 -175.9(4) . . . . ? C20 C49 C50 F16 1.7(7) . . . . ? C54 C49 C50 C51 -0.8(7) . . . . ? C20 C49 C50 C51 176.8(4) . . . . ? F16 C50 C51 F17 -3.3(7) . . . . ? C49 C50 C51 F17 -178.4(5) . . . . ? F16 C50 C51 C52 174.8(5) . . . . ? C49 C50 C51 C52 -0.3(8) . . . . ? F17 C51 C52 C53 178.7(5) . . . . ? C50 C51 C52 C53 0.7(9) . . . . ? F17 C51 C52 F18 -1.0(8) . . . . ? C50 C51 C52 F18 -179.0(5) . . . . ? F18 C52 C53 F19 -0.5(9) . . . . ? C51 C52 C53 F19 179.8(5) . . . . ? F18 C52 C53 C54 179.8(5) . . . . ? C51 C52 C53 C54 0.1(9) . . . . ? F19 C53 C54 F20 -0.8(7) . . . . ? C52 C53 C54 F20 178.9(5) . . . . ? F19 C53 C54 C49 178.9(4) . . . . ? C52 C53 C54 C49 -1.3(8) . . . . ? C50 C49 C54 F20 -178.6(4) . . . . ? C20 C49 C54 F20 3.7(6) . . . . ? C50 C49 C54 C53 1.7(7) . . . . ? C20 C49 C54 C53 -176.1(4) . . . . ? F21 C56 C57 F22 0.3(6) . . . . ? C55 C56 C57 F22 -179.4(4) . . . . ? F21 C56 C57 C58 180.0(4) . . . . ? C55 C56 C57 C58 0.3(7) . . . . ? F22 C57 C58 F23 -0.1(6) . . . . ? C56 C57 C58 F23 -179.8(4) . . . . ? F22 C57 C58 C59 179.9(4) . . . . ? C56 C57 C58 C59 0.2(6) . . . . ? F23 C58 C59 F24 -0.3(6) . . . . ? C57 C58 C59 F24 179.7(4) . . . . ? F23 C58 C59 C60 180.0(4) . . . . ? C57 C58 C59 C60 0.0(6) . . . . ? F24 C59 C60 F25 1.3(6) . . . . ? C58 C59 C60 F25 -179.1(4) . . . . ? F24 C59 C60 C55 179.7(4) . . . . ? C58 C59 C60 C55 -0.6(6) . . . . ? C1 C30 C61 C66 -51.7(5) . . . . ? C29 C30 C61 C66 128.1(4) . . . . ? C1 C30 C61 C62 133.0(4) . . . . ? C29 C30 C61 C62 -47.2(5) . . . . ? C66 C61 C62 F26 174.4(3) . . . . ? C30 C61 C62 F26 -10.0(5) . . . . ? C66 C61 C62 C63 -4.3(6) . . . . ? C30 C61 C62 C63 171.3(4) . . . . ? F26 C62 C63 F27 4.3(6) . . . . ? C61 C62 C63 F27 -177.0(3) . . . . ? F26 C62 C63 C64 -175.0(4) . . . . ? C61 C62 C63 C64 3.7(6) . . . . ? F27 C63 C64 F28 -0.3(6) . . . . ? C62 C63 C64 F28 179.0(4) . . . . ? F27 C63 C64 C65 -179.7(4) . . . . ? C62 C63 C64 C65 -0.4(7) . . . . ? F28 C64 C65 F29 0.6(7) . . . . ? C63 C64 C65 F29 -180.0(4) . . . . ? F28 C64 C65 C66 178.5(4) . . . . ? C63 C64 C65 C66 -2.1(7) . . . . ? F29 C65 C66 F30 0.4(6) . . . . ? C64 C65 C66 F30 -177.4(4) . . . . ? F29 C65 C66 C61 179.2(4) . . . . ? C64 C65 C66 C61 1.4(6) . . . . ? C62 C61 C66 F30 -179.5(3) . . . . ? C30 C61 C66 F30 5.0(6) . . . . ? C62 C61 C66 C65 1.8(6) . . . . ? C30 C61 C66 C65 -173.7(4) . . . . ? C3 C2 C67 C72 111.6(5) . . . . ? C1 C2 C67 C72 -60.9(6) . . . . ? C3 C2 C67 C68 -72.0(6) . . . . ? C1 C2 C67 C68 115.5(4) . . . . ? C72 C67 C68 C69 0.1(6) . . . . ? C2 C67 C68 C69 -176.4(4) . . . . ? C67 C68 C69 C70 -0.8(6) . . . . ? C68 C69 C70 C71 0.7(7) . . . . ? C69 C70 C71 C72 0.1(7) . . . . ? C68 C67 C72 C71 0.7(6) . . . . ? C2 C67 C72 C71 177.2(4) . . . . ? C70 C71 C72 C67 -0.8(6) . . . . ? C2 C3 C73 C74 69.4(6) . . . . ? C4 C3 C73 C74 -119.5(5) . . . . ? C2 C3 C73 C78 -110.2(5) . . . . ? C4 C3 C73 C78 60.9(6) . . . . ? C78 C73 C74 C75 -1.0(7) . . . . ? C3 C73 C74 C75 179.4(4) . . . . ? C73 C74 C75 C76 0.9(7) . . . . ? C74 C75 C76 C77 0.3(7) . . . . ? C75 C76 C77 C78 -1.3(7) . . . . ? C76 C77 C78 C73 1.3(7) . . . . ? C74 C73 C78 C77 -0.1(7) . . . . ? C3 C73 C78 C77 179.5(4) . . . . ? C18 C17 C79 C84 54.0(5) . . . . ? C16 C17 C79 C84 -126.8(4) . . . . ? C18 C17 C79 C80 -128.5(4) . . . . ? C16 C17 C79 C80 50.7(5) . . . . ? C84 C79 C80 C81 2.6(6) . . . . ? C17 C79 C80 C81 -174.9(3) . . . . ? C79 C80 C81 C82 -1.5(6) . . . . ? C80 C81 C82 C83 -0.5(6) . . . . ? C81 C82 C83 C84 1.3(6) . . . . ? C82 C83 C84 C79 -0.1(6) . . . . ? C80 C79 C84 C83 -1.8(6) . . . . ? C17 C79 C84 C83 175.7(4) . . . . ? C17 C18 C85 C90 -112.3(5) . . . . ? C19 C18 C85 C90 66.6(5) . . . . ? C17 C18 C85 C86 66.7(5) . . . . ? C19 C18 C85 C86 -114.4(4) . . . . ? C90 C85 C86 C87 -0.6(6) . . . . ? C18 C85 C86 C87 -179.6(4) . . . . ? C85 C86 C87 C88 0.0(6) . . . . ? C86 C87 C88 C89 0.5(7) . . . . ? C87 C88 C89 C90 -0.4(7) . . . . ? C86 C85 C90 C89 0.7(6) . . . . ? C18 C85 C90 C89 179.7(4) . . . . ? C88 C89 C90 C85 -0.2(6) . . . . ? F32 C91 C92 O1 27.4(7) . . . . ? F33 C91 C92 O1 -91.5(6) . . . . ? F31 C91 C92 O1 147.9(5) . . . . ? F32 C91 C92 O2 -153.1(5) . . . . ? F33 C91 C92 O2 88.0(6) . . . . ? F31 C91 C92 O2 -32.6(7) . . . . ? F35 C93 C94 O4 125.1(7) . . . . ? F36 C93 C94 O4 -1.8(7) . . . . ? F34 C93 C94 O4 -120.2(5) . . . . ? F35 C93 C94 O3 -56.6(8) . . . . ? F36 C93 C94 O3 176.6(5) . . . . ? F34 C93 C94 O3 58.1(6) . . . . ? F38 C95 C96 O6 159.3(4) . . . . ? F39 C95 C96 O6 37.1(6) . . . . ? F37 C95 C96 O6 -81.2(5) . . . . ? F38 C95 C96 O5 -23.1(6) . . . . ? F39 C95 C96 O5 -145.3(5) . . . . ? F37 C95 C96 O5 96.4(5) . . . . ? C30 C1 N1 C4 -180.0(4) . . . . ? C2 C1 N1 C4 1.4(4) . . . . ? C5 C4 N1 C1 170.5(4) . . . . ? C3 C4 N1 C1 -2.9(4) . . . . ? C5 C6 N2 C9 -173.2(4) . . . . ? C7 C6 N2 C9 1.6(5) . . . . ? C10 C9 N2 C6 179.8(4) . . . . ? C8 C9 N2 C6 0.1(4) . . . . ? C10 C11 N3 C14 173.9(4) . . . . ? C12 C11 N3 C14 -2.5(4) . . . . ? C15 C14 N3 C11 -165.4(4) . . . . ? C13 C14 N3 C11 3.6(4) . . . . ? C18 C19 N4 C16 1.6(4) . . . . ? C20 C19 N4 C16 -176.6(3) . . . . ? C15 C16 N4 C19 179.6(3) . . . . ? C17 C16 N4 C19 -0.3(4) . . . . ? C25 C24 N5 C21 -178.6(4) . . . . ? C23 C24 N5 C21 1.5(5) . . . . ? C20 C21 N5 C24 177.6(4) . . . . ? C22 C21 N5 C24 -1.8(5) . . . . ? C30 C29 N6 C26 169.0(4) . . . . ? C28 C29 N6 C26 -3.4(4) . . . . ? C25 C26 N6 C29 -176.8(4) . . . . ? C27 C26 N6 C29 3.0(4) . . . . ? F21 C56 C55 C60 179.4(4) . . . . ? C57 C56 C55 C60 -0.9(6) . . . . ? F21 C56 C55 C25 0.5(6) . . . . ? C57 C56 C55 C25 -179.8(4) . . . . ? F25 C60 C55 C56 179.4(3) . . . . ? C59 C60 C55 C56 1.1(6) . . . . ? F25 C60 C55 C25 -1.6(6) . . . . ? C59 C60 C55 C25 180.0(4) . . . . ? C24 C25 C55 C56 -105.1(5) . . . . ? C26 C25 C55 C56 71.3(5) . . . . ? C24 C25 C55 C60 76.0(5) . . . . ? C26 C25 C55 C60 -107.5(5) . . . . ? O7 C97 C98 F42 -103.0(5) . . . . ? O8 C97 C98 F42 75.3(5) . . . . ? O7 C97 C98 F41 136.3(4) . . . . ? O8 C97 C98 F41 -45.4(5) . . . . ? O7 C97 C98 F40 16.4(6) . . . . ? O8 C97 C98 F40 -165.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.978 _refine_diff_density_min -1.334 _refine_diff_density_rms 0.109 # Attachment '4A.CIF' data_4A _database_code_depnum_ccdc_archive 'CCDC 728273' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H32 F30 N6, 2.62(C H2 Cl2)' _chemical_formula_sum 'C92.62 H37.24 Cl5.24 F30 N6' _chemical_formula_weight 1989.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 13.6922(11) _cell_length_b 47.412(4) _cell_length_c 12.5608(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.791(2) _cell_angle_gamma 90.00 _cell_volume 8153.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9366 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.23 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3976 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42183 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14315 _reflns_number_gt 10638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Though almost all electron density was properly assigned, some electron density around the solvents are still remained. All attempts to model the disorder were unsatisfactory as well as to remove the residual density by use of the utility SQUEEZE in PLATON software packate, SQUEEZE-PLATON. ; _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^)+(0.0687P)^2^+27.8090P] 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 14315 _refine_ls_number_parameters 1245 _refine_ls_number_restraints 956 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0975 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.176 _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 F3 F 0.2574(2) 0.06732(7) 1.6250(3) 0.0203(8) Uani 1 1 d U . . F17 F 1.2092(2) -0.00575(7) 0.7798(3) 0.0265(8) Uani 1 1 d U . . F5 F 0.3979(2) 0.05565(6) 1.2901(2) 0.0185(7) Uani 1 1 d U . . F1 F 0.4445(2) 0.14034(6) 1.4823(3) 0.0211(8) Uani 1 1 d U . . F6 F 0.6435(2) 0.04692(7) 1.0624(3) 0.0239(8) Uani 1 1 d U . . F22 F 0.4214(2) 0.26965(7) 0.9756(3) 0.0245(8) Uani 1 1 d U . . F16 F 1.1027(2) 0.03542(7) 0.8730(3) 0.0189(7) Uani 1 1 d U . . F21 F 0.4789(2) 0.22275(6) 1.0781(2) 0.0188(7) Uani 1 1 d U . . F19 F 1.0780(2) 0.01933(7) 0.4462(3) 0.0229(8) Uani 1 1 d U . . F4 F 0.2894(2) 0.03549(7) 1.4497(3) 0.0209(8) Uani 1 1 d U . . F11 F 0.9788(2) 0.11382(7) 1.3263(3) 0.0247(8) Uani 1 1 d U . . F25 F 0.3757(2) 0.16827(7) 0.7825(3) 0.0216(8) Uani 1 1 d U . . F15 F 0.8518(2) 0.05059(7) 1.0703(3) 0.0227(8) Uani 1 1 d U . . F2 F 0.3340(3) 0.11998(7) 1.6398(3) 0.0235(8) Uani 1 1 d U . . F20 F 0.9703(2) 0.05995(7) 0.5370(3) 0.0248(8) Uani 1 1 d U . . F18 F 1.1966(2) -0.01376(7) 0.5671(3) 0.0253(8) Uani 1 1 d U . . F23 F 0.3455(3) 0.26651(7) 0.7765(3) 0.0300(9) Uani 1 1 d U . . F10 F 0.4543(2) 0.08011(8) 0.7722(3) 0.0278(9) Uani 1 1 d U . . F30 F 1.0070(2) 0.19900(6) 0.7584(2) 0.0194(7) Uani 1 1 d U . . F26 F 1.1154(2) 0.17830(7) 1.1080(2) 0.0213(8) Uani 1 1 d U . . F24 F 0.3187(3) 0.21535(8) 0.6820(3) 0.0311(9) Uani 1 1 d U . . F14 F 1.0097(2) 0.01730(7) 1.0977(3) 0.0257(8) Uani 1 1 d U . . F27 F 1.2096(2) 0.22777(7) 1.1156(3) 0.0291(9) Uani 1 1 d U . . F13 F 1.1533(2) 0.03227(7) 1.2383(3) 0.0263(8) Uani 1 1 d U . . F28 F 1.1970(3) 0.26417(7) 0.9494(3) 0.0350(10) Uani 1 1 d U . . F7 F 0.4892(3) 0.01756(7) 1.1309(3) 0.0313(9) Uani 1 1 d U . . F29 F 1.0981(3) 0.24910(7) 0.7701(3) 0.0344(9) Uani 1 1 d U . . F12 F 1.1349(2) 0.08014(8) 1.3547(3) 0.0313(9) Uani 1 1 d U . . N6 N 0.5544(3) 0.12368(9) 0.9410(3) 0.0094(9) Uani 1 1 d U . . H6 H 0.5236 0.1140 0.9900 0.011 Uiso 1 1 calc R . . N1 N 0.8119(3) 0.08156(9) 0.8342(3) 0.0101(9) Uani 1 1 d U . . H1 H 0.8239 0.0994 0.8482 0.012 Uiso 1 1 calc R . . C37 C 0.6025(4) 0.15895(11) 0.8370(4) 0.0108(11) Uani 1 1 d U . . F9 F 0.3007(3) 0.05049(9) 0.8418(4) 0.0429(11) Uani 1 1 d U . . N3 N 0.9123(3) 0.12864(9) 1.0498(4) 0.0117(10) Uani 1 1 d U . . H3 H 0.9401 0.1134 1.0243 0.014 Uiso 1 1 calc R . . N2 N 0.9692(3) 0.11464(9) 0.8556(4) 0.0109(9) Uani 1 1 d U . . C41 C 0.8242(4) 0.10224(10) 1.1844(4) 0.0086(10) Uani 1 1 d U . . N4 N 0.6482(3) 0.10856(9) 1.2126(3) 0.0089(9) Uani 1 1 d U . . H4 H 0.6376 0.1221 1.1658 0.011 Uiso 1 1 calc R . . F8 F 0.3184(3) 0.01863(8) 1.0206(4) 0.0428(11) Uani 1 1 d U . . C44 C 0.7230(4) 0.13196(11) 0.7185(4) 0.0099(11) Uani 1 1 d U . . C45 C 0.5418(4) 0.15179(11) 0.9231(4) 0.0087(10) Uani 1 1 d U . . C46 C 1.0569(4) 0.18704(11) 0.9327(4) 0.0104(11) Uani 1 1 d U . . C47 C 0.4732(4) 0.16805(11) 0.9846(4) 0.0097(11) Uani 1 1 d U . . C48 C 0.6517(4) 0.13407(11) 0.8052(4) 0.0125(11) Uani 1 1 d U . . C49 C 0.8739(4) 0.17375(10) 1.0770(4) 0.0075(10) Uani 1 1 d U . . C50 C 0.4471(4) 0.15941(11) 1.0849(4) 0.0102(11) Uani 1 1 d U . . C51 C 0.4247(4) 0.09889(11) 1.3802(4) 0.0105(11) Uani 1 1 d U . . C52 C 1.0013(4) 0.04116(11) 1.1552(5) 0.0159(12) Uani 1 1 d U . . C53 C 0.6211(4) 0.11230(11) 0.8731(4) 0.0106(11) Uani 1 1 d U . . N5 N 0.4953(3) 0.13710(9) 1.1337(3) 0.0093(9) Uani 1 1 d U . . C55 C 0.8457(4) 0.12856(11) 1.1295(4) 0.0081(10) Uani 1 1 d U . . C56 C 0.4511(4) 0.13186(11) 1.2244(4) 0.0109(11) Uani 1 1 d U . . C57 C 0.8015(4) 0.15041(12) 0.7128(4) 0.0145(12) Uani 1 1 d U . . H57 H 0.8060 0.1656 0.7619 0.017 Uiso 1 1 calc R . . C58 C 0.3285(4) 0.06154(11) 1.4563(4) 0.0114(11) Uani 1 1 d U . . C59 C 0.6688(4) 0.18217(10) 1.2003(4) 0.0093(11) Uani 1 1 d U . . H59 H 0.6607 0.1880 1.1284 0.011 Uiso 1 1 calc R . . C60 C 1.1008(4) 0.13793(11) 0.7812(4) 0.0134(11) Uani 1 1 d U . . H60 H 1.1471 0.1522 0.7653 0.016 Uiso 1 1 calc R . . C61 C 0.6018(4) 0.19096(11) 0.6795(4) 0.0127(11) Uani 1 1 d U . . H61 H 0.5862 0.1753 0.6354 0.015 Uiso 1 1 calc R . . C62 C 0.7175(4) 0.07270(11) 1.3035(4) 0.0111(11) Uani 1 1 d U . . H62 H 0.7627 0.0586 1.3257 0.013 Uiso 1 1 calc R . . C63 C 0.3588(4) 0.21691(13) 0.7802(5) 0.0186(12) Uani 1 1 d U . . C64 C 0.5790(4) 0.09843(10) 1.2802(4) 0.0099(11) Uani 1 1 d U . . C65 C 0.8788(4) 0.06340(11) 0.7935(4) 0.0132(11) Uani 1 1 d U . . C66 C 1.1446(4) 0.00672(11) 0.6136(5) 0.0171(12) Uani 1 1 d U . . C67 C 0.6382(4) 0.08186(11) 0.8765(4) 0.0108(11) Uani 1 1 d U . . C68 C 0.9306(4) 0.15550(11) 1.0141(4) 0.0083(10) Uani 1 1 d U . . C69 C 0.6363(4) 0.24057(12) 0.6980(5) 0.0161(12) Uani 1 1 d U . . H69 H 0.6450 0.2587 0.6671 0.019 Uiso 1 1 calc R . . C70 C 0.4289(4) 0.19359(11) 0.9342(4) 0.0104(11) Uani 1 1 d U . . C71 C 0.4865(4) 0.10998(11) 1.2930(4) 0.0097(11) Uani 1 1 d U . . C72 C 1.0013(4) 0.16033(11) 0.9318(4) 0.0095(11) Uani 1 1 d U . . C73 C 0.6934(4) 0.16590(11) 1.4103(4) 0.0144(12) Uani 1 1 d U . . H73 H 0.7021 0.1604 1.4826 0.017 Uiso 1 1 calc R . . C74 C 0.6253(4) 0.07545(11) 1.3375(4) 0.0121(11) Uani 1 1 d U . . H74 H 0.5955 0.0642 1.3904 0.015 Uiso 1 1 calc R . . C75 C 0.3841(4) 0.07209(11) 1.3761(4) 0.0101(11) Uani 1 1 d U . . C76 C 0.4366(4) 0.22017(11) 0.9819(4) 0.0124(11) Uani 1 1 d U . . C77 C 1.0960(4) 0.03163(11) 0.7672(4) 0.0129(11) Uani 1 1 d U . . C78 C 0.7623(4) 0.15895(11) 1.3373(4) 0.0126(11) Uani 1 1 d U . . H78 H 0.8189 0.1488 1.3596 0.015 Uiso 1 1 calc R . . C79 C 1.1569(4) 0.22111(12) 1.0294(5) 0.0185(12) Uani 1 1 d U . . C80 C 1.1097(4) 0.19552(12) 1.0235(4) 0.0147(12) Uani 1 1 d U . . C81 C 0.5992(4) 0.18929(10) 1.2742(4) 0.0109(11) Uani 1 1 d U . . H81 H 0.5435 0.1999 1.2528 0.013 Uiso 1 1 calc R . . C82 C 0.4061(4) 0.11433(11) 1.4713(4) 0.0141(11) Uani 1 1 d U . . C83 C 0.9196(4) 0.05814(11) 1.1421(4) 0.0134(11) Uani 1 1 d U . . C84 C 0.4091(4) 0.24458(11) 0.9295(5) 0.0156(12) Uani 1 1 d U . . C85 C 1.0224(4) 0.13959(11) 0.8582(4) 0.0097(11) Uani 1 1 d U . . C86 C 0.9717(4) 0.07060(11) 0.7623(4) 0.0111(11) Uani 1 1 d U . . C87 C 0.7362(4) 0.09503(10) 1.2269(4) 0.0083(10) Uani 1 1 d U . . C88 C 0.8661(4) 0.26398(12) 1.0681(5) 0.0225(13) Uani 1 1 d U . . H88 H 0.8640 0.2840 1.0667 0.027 Uiso 1 1 calc R . . C89 C 0.3680(4) 0.16823(11) 1.1532(4) 0.0107(11) Uani 1 1 d U . . H89 H 0.3239 0.1833 1.1402 0.013 Uiso 1 1 calc R . . C90 C 0.8205(4) 0.15667(11) 1.1485(4) 0.0091(10) Uani 1 1 d U . . C91 C 0.7508(4) 0.16647(10) 1.2301(4) 0.0086(10) Uani 1 1 d U . . C92 C 0.8710(4) 0.20500(11) 1.0723(4) 0.0101(11) Uani 1 1 d U . . C93 C 0.8829(4) 0.22064(11) 1.1660(5) 0.0157(12) Uani 1 1 d U . . H93 H 0.8934 0.2112 1.2319 0.019 Uiso 1 1 calc R . . C94 C 0.8557(4) 0.24858(11) 0.9746(5) 0.0155(12) Uani 1 1 d U . . H94 H 0.8468 0.2581 0.9086 0.019 Uiso 1 1 calc R . . C95 C 0.9089(4) 0.08292(10) 1.1997(4) 0.0079(10) Uani 1 1 d U . . C96 C 0.5540(4) 0.06442(11) 0.9135(4) 0.0101(11) Uani 1 1 d U . . C97 C 0.7876(4) 0.10686(12) 0.5684(5) 0.0208(13) Uani 1 1 d U . . H97 H 0.7827 0.0919 0.5185 0.025 Uiso 1 1 calc R . . C98 C 0.8669(4) 0.12510(12) 0.5655(5) 0.0182(12) Uani 1 1 d U . . H98 H 0.9165 0.1224 0.5144 0.022 Uiso 1 1 calc R . . C99 C 0.7393(4) 0.03940(12) 0.8248(5) 0.0173(12) Uani 1 1 d U . . H99 H 0.6933 0.0246 0.8334 0.021 Uiso 1 1 calc R . . C100 C 1.0328(4) 0.04875(11) 0.7082(4) 0.0114(11) Uani 1 1 d U . . C101 C 0.6367(4) 0.21068(11) 0.8519(4) 0.0127(11) Uani 1 1 d U . . H101 H 0.6463 0.2084 0.9264 0.015 Uiso 1 1 calc R . . C102 C 0.7234(4) 0.06868(11) 0.8510(4) 0.0129(11) Uani 1 1 d U . . C103 C 0.8733(4) 0.14724(12) 0.6374(4) 0.0148(12) Uani 1 1 d U . . H103 H 0.9264 0.1601 0.6349 0.018 Uiso 1 1 calc R . . C104 C 1.0113(4) 0.09798(11) 0.7844(4) 0.0104(11) Uani 1 1 d U . . C105 C 0.5613(4) 0.04796(11) 1.0065(5) 0.0147(12) Uani 1 1 d U . . C106 C 0.6128(4) 0.18716(11) 0.7883(4) 0.0105(11) Uani 1 1 d U . . C107 C 0.3708(4) 0.24277(12) 0.8277(4) 0.0155(12) Uani 1 1 d U . . C108 C 1.0845(4) 0.02364(11) 0.5521(5) 0.0149(12) Uani 1 1 d U . . C109 C 0.3502(4) 0.10417(11) 1.5532(4) 0.0143(12) Uani 1 1 d U . . C110 C 0.3112(4) 0.07747(11) 1.5465(4) 0.0134(11) Uani 1 1 d U . . C111 C 1.1508(4) 0.01067(11) 0.7214(5) 0.0138(12) Uani 1 1 d U . . C112 C 0.6465(4) 0.23710(12) 0.8069(4) 0.0153(12) Uani 1 1 d U . . H112 H 0.6602 0.2529 0.8509 0.018 Uiso 1 1 calc R . . C113 C 1.0565(4) 0.20543(11) 0.8472(4) 0.0138(11) Uani 1 1 d U . . C114 C 1.0295(4) 0.04426(11) 0.5999(5) 0.0153(12) Uani 1 1 d U . . C115 C 0.7157(4) 0.11035(12) 0.6435(4) 0.0159(12) Uani 1 1 d U . . H115 H 0.6612 0.0980 0.6440 0.019 Uiso 1 1 calc R . . C116 C 0.3879(4) 0.19299(11) 0.8323(4) 0.0140(12) Uani 1 1 d U . . C117 C 0.8581(4) 0.21943(11) 0.9771(4) 0.0109(11) Uani 1 1 d U . . H117 H 0.8508 0.2091 0.9126 0.013 Uiso 1 1 calc R . . C118 C 0.8795(4) 0.24976(12) 1.1629(5) 0.0211(13) Uani 1 1 d U . . H118 H 0.8865 0.2601 1.2273 0.025 Uiso 1 1 calc R . . C119 C 0.3688(4) 0.15112(11) 1.2380(4) 0.0120(11) Uani 1 1 d U . . H119 H 0.3246 0.1514 1.2956 0.014 Uiso 1 1 calc R . . C120 C 1.1030(4) 0.23164(11) 0.8525(5) 0.0174(12) Uani 1 1 d U . . C121 C 1.1530(4) 0.23912(12) 0.9442(5) 0.0198(13) Uani 1 1 d U . . C122 C 0.4652(4) 0.06473(12) 0.8613(5) 0.0163(12) Uani 1 1 d U . . C123 C 0.6134(4) 0.21750(11) 0.6340(5) 0.0158(12) Uani 1 1 d U . . H123 H 0.6057 0.2199 0.5592 0.019 Uiso 1 1 calc R . . C124 C 0.9840(4) 0.08976(11) 1.2701(4) 0.0143(12) Uani 1 1 d U . . C125 C 1.0943(4) 0.11204(11) 0.7369(4) 0.0140(11) Uani 1 1 d U . . H125 H 1.1362 0.1044 0.6845 0.017 Uiso 1 1 calc R . . C126 C 0.3940(5) 0.03357(12) 0.9866(5) 0.0255(14) Uani 1 1 d U . . C127 C 1.0647(4) 0.07293(12) 1.2846(5) 0.0165(12) Uani 1 1 d U . . C128 C 1.0734(4) 0.04855(12) 1.2257(5) 0.0153(12) Uani 1 1 d U . . C129 C 0.6104(4) 0.18102(11) 1.3792(4) 0.0127(11) Uani 1 1 d U . . H129 H 0.5619 0.1856 1.4297 0.015 Uiso 1 1 calc R . . C130 C 0.8294(4) 0.03645(11) 0.7866(5) 0.0149(12) Uani 1 1 d U . . H130 H 0.8564 0.0195 0.7595 0.018 Uiso 1 1 calc R . . C131 C 0.4810(4) 0.03297(12) 1.0416(5) 0.0205(13) Uani 1 1 d U . . C132 C 0.3862(4) 0.04959(13) 0.8951(5) 0.0242(13) Uani 1 1 d U . . Cl1 Cl 1.25850(14) 0.08518(4) 1.11682(15) 0.0429(5) Uani 1 1 d . . . Cl2 Cl 1.29854(13) 0.11843(4) 0.92831(16) 0.0462(5) Uani 1 1 d . . . Cl5 Cl 0.4157(2) 0.00687(7) 0.6548(3) 0.0462(10) Uani 0.619(5) 1 d PD A 3 Cl6 Cl 0.5778(3) 0.04143(7) 0.5949(2) 0.0503(11) Uani 0.619(5) 1 d PDU A 3 C133 C 1.2072(6) 0.1047(2) 1.0130(7) 0.054(2) Uani 1 1 d . . . H137 H 1.1687 0.1205 1.0426 0.065 Uiso 1 1 calc R . . H138 H 1.1622 0.0926 0.9710 0.065 Uiso 1 1 calc R . . C135 C 0.5392(8) 0.0093(3) 0.6365(10) 0.046(3) Uani 0.619(5) 1 d PDU A 3 H131 H 0.5729 0.0047 0.7046 0.055 Uiso 0.619(5) 1 calc PR A 3 H132 H 0.5587 -0.0050 0.5835 0.055 Uiso 0.619(5) 1 calc PR A 3 C134 C 0.107(2) 0.1736(10) 0.372(4) 0.035(5) Uani 0.51(4) 1 d PU B 1 H133 H 0.1538 0.1872 0.3419 0.042 Uiso 0.51(4) 1 calc PR B 1 H134 H 0.0808 0.1618 0.3128 0.042 Uiso 0.51(4) 1 calc PR B 1 Cl3 Cl 0.0131(18) 0.1915(5) 0.429(2) 0.046(3) Uani 0.51(4) 1 d PU B 1 Cl4 Cl 0.1681(13) 0.1515(5) 0.4677(16) 0.071(4) Uani 0.51(4) 1 d PU B 1 Cl7 Cl 0.1973(14) 0.1615(5) 0.4847(9) 0.061(4) Uani 0.49(4) 1 d PU B 2 Cl8 Cl 0.013(2) 0.1853(6) 0.409(2) 0.055(4) Uani 0.49(4) 1 d PU B 2 C137 C 0.133(2) 0.1720(11) 0.377(4) 0.039(5) Uani 0.49(4) 1 d PU B 2 H135 H 0.1253 0.1558 0.3274 0.046 Uiso 0.49(4) 1 calc PR B 2 H136 H 0.1695 0.1869 0.3395 0.046 Uiso 0.49(4) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F3 0.0243(18) 0.0213(18) 0.0157(18) 0.0053(14) 0.0143(14) -0.0038(14) F17 0.0270(19) 0.0198(18) 0.033(2) 0.0078(16) 0.0049(16) 0.0123(15) F5 0.0236(18) 0.0170(17) 0.0152(18) -0.0023(14) 0.0079(14) -0.0045(14) F1 0.033(2) 0.0128(17) 0.0171(18) -0.0030(14) 0.0075(15) -0.0110(15) F6 0.028(2) 0.0220(19) 0.022(2) 0.0059(15) -0.0042(16) 0.0001(15) F22 0.032(2) 0.0109(17) 0.031(2) -0.0006(14) -0.0045(16) 0.0024(15) F16 0.0214(18) 0.0200(18) 0.0155(18) 0.0042(14) 0.0020(14) 0.0039(14) F21 0.0259(18) 0.0174(17) 0.0129(18) 0.0011(13) -0.0096(14) 0.0003(14) F19 0.0245(19) 0.0227(19) 0.022(2) -0.0099(15) 0.0012(15) -0.0010(15) F4 0.0206(18) 0.0166(17) 0.026(2) -0.0001(14) 0.0076(15) -0.0075(14) F11 0.0260(19) 0.0215(19) 0.026(2) -0.0162(15) -0.0067(16) 0.0100(15) F25 0.0285(19) 0.0180(18) 0.0180(19) -0.0046(14) -0.0102(15) 0.0060(15) F15 0.0209(18) 0.0202(18) 0.027(2) -0.0071(15) -0.0071(15) -0.0008(14) F2 0.035(2) 0.0228(19) 0.0131(18) -0.0045(14) 0.0132(15) -0.0020(15) F20 0.0255(19) 0.0256(19) 0.023(2) -0.0013(15) -0.0050(15) 0.0121(15) F18 0.029(2) 0.0134(17) 0.034(2) -0.0041(15) 0.0115(16) 0.0090(15) F23 0.038(2) 0.0203(19) 0.032(2) 0.0129(16) -0.0037(17) 0.0119(16) F10 0.0196(18) 0.039(2) 0.025(2) 0.0125(17) -0.0077(15) -0.0031(16) F30 0.0290(19) 0.0169(17) 0.0123(18) 0.0066(13) -0.0021(15) -0.0055(14) F26 0.0261(19) 0.0263(19) 0.0113(17) 0.0028(14) -0.0052(14) -0.0020(15) F24 0.044(2) 0.035(2) 0.0135(19) 0.0011(16) -0.0126(17) 0.0137(18) F14 0.031(2) 0.0106(17) 0.036(2) -0.0107(15) -0.0014(17) 0.0066(15) F27 0.0177(18) 0.035(2) 0.034(2) -0.0185(17) -0.0074(16) -0.0041(16) F13 0.0243(19) 0.0193(18) 0.035(2) 0.0003(15) -0.0026(16) 0.0129(15) F28 0.026(2) 0.0159(19) 0.063(3) -0.0084(18) 0.0031(19) -0.0091(16) F7 0.047(2) 0.0200(19) 0.027(2) 0.0123(16) 0.0178(18) -0.0019(17) F29 0.041(2) 0.021(2) 0.041(2) 0.0159(17) 0.0057(19) -0.0094(17) F12 0.0188(18) 0.035(2) 0.040(2) -0.0126(17) -0.0186(17) 0.0109(16) N6 0.008(2) 0.009(2) 0.011(2) 0.0038(17) 0.0027(18) 0.0027(17) N1 0.009(2) 0.007(2) 0.014(2) -0.0030(18) -0.0017(18) -0.0008(17) C37 0.008(2) 0.013(3) 0.012(3) 0.000(2) -0.003(2) 0.000(2) F9 0.018(2) 0.055(3) 0.056(3) 0.006(2) -0.0086(19) -0.0123(18) N3 0.014(2) 0.007(2) 0.014(2) 0.0013(18) 0.0052(19) 0.0033(18) N2 0.008(2) 0.010(2) 0.015(2) -0.0015(18) 0.0014(18) 0.0017(17) C41 0.013(2) 0.007(2) 0.006(2) -0.0004(19) -0.003(2) 0.001(2) N4 0.009(2) 0.006(2) 0.012(2) 0.0028(17) 0.0006(18) -0.0017(17) F8 0.030(2) 0.036(2) 0.063(3) 0.007(2) 0.019(2) -0.0149(18) C44 0.011(2) 0.0077(19) 0.011(2) 0.0033(17) 0.0005(17) 0.0045(17) C45 0.006(2) 0.009(2) 0.011(3) 0.001(2) -0.003(2) 0.0021(19) C46 0.005(2) 0.014(3) 0.012(3) -0.001(2) 0.003(2) 0.000(2) C47 0.007(2) 0.007(2) 0.015(3) 0.000(2) -0.001(2) 0.000(2) C48 0.009(2) 0.014(3) 0.015(3) 0.001(2) -0.002(2) -0.001(2) C49 0.0072(19) 0.0082(19) 0.007(2) 0.0007(16) -0.0023(17) 0.0011(16) C50 0.006(2) 0.011(2) 0.014(3) 0.000(2) -0.002(2) 0.000(2) C51 0.008(2) 0.015(3) 0.008(2) 0.002(2) 0.000(2) 0.003(2) C52 0.020(3) 0.009(3) 0.019(3) 0.002(2) 0.004(2) 0.001(2) C53 0.010(2) 0.011(2) 0.011(3) 0.001(2) -0.001(2) 0.002(2) N5 0.014(2) 0.005(2) 0.009(2) 0.0018(17) 0.0014(18) 0.0041(17) C55 0.0086(19) 0.0103(19) 0.0055(19) 0.0017(16) -0.0010(17) 0.0010(17) C56 0.008(2) 0.015(3) 0.010(3) 0.001(2) 0.004(2) -0.002(2) C57 0.015(3) 0.017(3) 0.012(3) 0.002(2) 0.001(2) 0.004(2) C58 0.009(2) 0.008(2) 0.018(3) 0.004(2) -0.001(2) -0.002(2) C59 0.014(3) 0.006(2) 0.008(3) 0.001(2) -0.001(2) 0.000(2) C60 0.011(3) 0.016(3) 0.014(3) 0.005(2) 0.002(2) -0.004(2) C61 0.015(3) 0.014(3) 0.009(3) 0.000(2) 0.000(2) 0.001(2) C62 0.015(3) 0.009(3) 0.009(3) 0.000(2) -0.001(2) 0.000(2) C63 0.018(3) 0.026(3) 0.012(3) 0.004(2) -0.001(2) 0.007(2) C64 0.012(2) 0.005(2) 0.013(3) 0.000(2) 0.004(2) -0.003(2) C65 0.013(3) 0.009(2) 0.017(3) 0.003(2) -0.002(2) 0.003(2) C66 0.014(3) 0.005(2) 0.033(3) -0.003(2) 0.009(2) -0.001(2) C67 0.014(3) 0.010(2) 0.008(2) 0.002(2) -0.002(2) -0.001(2) C68 0.004(2) 0.013(2) 0.008(2) 0.004(2) -0.0041(19) -0.001(2) C69 0.019(3) 0.011(3) 0.018(3) 0.004(2) 0.000(2) 0.001(2) C70 0.012(2) 0.010(2) 0.010(3) 0.003(2) 0.003(2) 0.002(2) C71 0.012(2) 0.009(2) 0.008(2) 0.000(2) 0.002(2) -0.001(2) C72 0.005(2) 0.013(3) 0.010(3) 0.002(2) -0.004(2) -0.001(2) C73 0.018(3) 0.014(3) 0.011(3) 0.003(2) 0.003(2) 0.000(2) C74 0.014(2) 0.012(2) 0.010(2) 0.0051(17) 0.0023(18) -0.0033(17) C75 0.007(2) 0.013(3) 0.011(3) -0.001(2) -0.002(2) 0.002(2) C76 0.007(2) 0.015(3) 0.015(3) 0.004(2) -0.001(2) 0.003(2) C77 0.010(3) 0.013(3) 0.016(3) 0.004(2) 0.002(2) 0.000(2) C78 0.015(3) 0.009(3) 0.013(3) 0.003(2) -0.002(2) -0.001(2) C79 0.013(3) 0.019(3) 0.023(3) -0.012(2) -0.001(2) 0.000(2) C80 0.014(3) 0.016(3) 0.015(3) -0.002(2) 0.004(2) 0.000(2) C81 0.013(3) 0.005(2) 0.014(3) 0.000(2) 0.002(2) 0.002(2) C82 0.014(3) 0.014(3) 0.014(3) 0.002(2) -0.001(2) -0.003(2) C83 0.012(3) 0.012(3) 0.017(3) 0.008(2) -0.002(2) -0.001(2) C84 0.015(3) 0.011(3) 0.021(3) 0.000(2) 0.000(2) 0.003(2) C85 0.009(2) 0.011(2) 0.009(2) 0.003(2) -0.005(2) 0.000(2) C86 0.006(2) 0.013(3) 0.015(3) 0.001(2) -0.002(2) 0.004(2) C87 0.011(2) 0.007(2) 0.007(2) -0.0009(19) -0.003(2) 0.002(2) C88 0.027(3) 0.012(3) 0.028(3) 0.000(2) 0.006(3) -0.006(2) C89 0.006(2) 0.013(3) 0.013(3) 0.002(2) -0.001(2) 0.005(2) C90 0.010(2) 0.011(2) 0.006(2) -0.001(2) -0.004(2) 0.002(2) C91 0.009(2) 0.007(2) 0.009(3) -0.002(2) 0.002(2) -0.004(2) C92 0.004(2) 0.012(2) 0.014(2) 0.0010(19) 0.0002(19) -0.0026(18) C93 0.018(3) 0.014(3) 0.015(3) 0.003(2) 0.001(2) -0.002(2) C94 0.014(3) 0.013(3) 0.020(3) 0.006(2) 0.003(2) 0.001(2) C95 0.008(2) 0.008(2) 0.008(2) 0.0040(18) 0.0029(19) 0.0010(18) C96 0.012(2) 0.008(2) 0.011(3) -0.001(2) 0.003(2) -0.001(2) C97 0.031(3) 0.020(3) 0.011(3) -0.005(2) -0.005(2) 0.011(3) C98 0.014(3) 0.029(3) 0.012(3) 0.005(2) 0.003(2) 0.011(2) C99 0.014(3) 0.011(3) 0.027(3) 0.004(2) -0.002(2) -0.002(2) C100 0.008(2) 0.010(2) 0.016(3) -0.003(2) 0.007(2) 0.000(2) C101 0.014(3) 0.014(3) 0.010(3) -0.001(2) -0.001(2) 0.003(2) C102 0.013(3) 0.014(3) 0.012(3) 0.004(2) -0.001(2) -0.001(2) C103 0.010(3) 0.020(3) 0.015(3) 0.008(2) 0.001(2) 0.002(2) C104 0.007(2) 0.010(2) 0.014(3) 0.003(2) 0.001(2) 0.003(2) C105 0.014(3) 0.013(3) 0.017(3) -0.005(2) 0.002(2) 0.003(2) C106 0.010(2) 0.009(2) 0.013(3) 0.004(2) 0.002(2) 0.006(2) C107 0.015(3) 0.017(3) 0.015(3) 0.005(2) 0.003(2) 0.010(2) C108 0.014(3) 0.010(3) 0.021(3) -0.004(2) 0.003(2) -0.007(2) C109 0.017(3) 0.014(3) 0.011(3) -0.003(2) 0.002(2) 0.002(2) C110 0.012(3) 0.016(3) 0.012(3) 0.011(2) 0.003(2) 0.005(2) C111 0.007(2) 0.011(2) 0.023(3) 0.006(2) 0.004(2) 0.0030(19) C112 0.017(3) 0.014(3) 0.015(3) -0.002(2) 0.000(2) -0.002(2) C113 0.010(3) 0.016(3) 0.016(3) -0.002(2) 0.002(2) 0.000(2) C114 0.009(3) 0.012(3) 0.024(3) -0.001(2) 0.000(2) -0.003(2) C115 0.021(3) 0.012(3) 0.015(3) 0.000(2) -0.004(2) 0.004(2) C116 0.018(3) 0.012(3) 0.012(3) 0.001(2) 0.001(2) 0.004(2) C117 0.008(2) 0.013(3) 0.012(3) -0.001(2) 0.001(2) 0.002(2) C118 0.026(3) 0.017(3) 0.020(3) -0.008(2) 0.007(3) -0.005(2) C119 0.009(2) 0.015(3) 0.012(3) 0.001(2) 0.007(2) 0.001(2) C120 0.012(3) 0.013(3) 0.027(3) 0.007(2) 0.014(2) 0.001(2) C121 0.011(3) 0.011(3) 0.038(3) -0.005(2) 0.007(2) -0.007(2) C122 0.013(3) 0.018(3) 0.019(3) 0.003(2) 0.003(2) -0.003(2) C123 0.021(3) 0.016(3) 0.011(3) 0.008(2) 0.005(2) 0.004(2) C124 0.016(3) 0.011(3) 0.016(3) -0.001(2) 0.006(2) 0.003(2) C125 0.014(3) 0.013(3) 0.015(3) -0.003(2) 0.003(2) 0.003(2) C126 0.025(3) 0.014(3) 0.037(4) -0.001(3) 0.010(3) -0.010(2) C127 0.013(3) 0.019(3) 0.017(3) -0.003(2) -0.006(2) 0.004(2) C128 0.013(3) 0.015(3) 0.017(3) 0.005(2) -0.003(2) 0.006(2) C129 0.015(3) 0.009(3) 0.014(3) -0.005(2) 0.007(2) -0.002(2) C130 0.012(2) 0.009(2) 0.024(3) 0.002(2) 0.003(2) 0.005(2) C131 0.028(3) 0.011(3) 0.023(3) 0.002(2) 0.016(3) 0.003(2) C132 0.015(3) 0.025(3) 0.032(3) -0.001(3) -0.004(3) -0.005(2) Cl1 0.0433(11) 0.0462(11) 0.0393(11) 0.0108(9) 0.0018(9) -0.0018(9) Cl2 0.0345(10) 0.0570(13) 0.0468(12) 0.0201(10) -0.0102(9) -0.0152(9) Cl5 0.0338(17) 0.058(2) 0.046(2) 0.0048(16) -0.0075(14) -0.0042(15) Cl6 0.084(3) 0.0389(19) 0.0272(18) 0.0070(13) -0.0096(16) -0.0120(17) C133 0.036(4) 0.072(6) 0.053(6) 0.030(5) -0.011(4) 0.002(4) C135 0.032(6) 0.070(9) 0.035(7) 0.002(6) -0.002(5) -0.001(6) C134 0.031(12) 0.040(7) 0.034(7) 0.000(6) 0.004(10) 0.013(10) Cl3 0.025(3) 0.060(8) 0.052(8) 0.020(6) 0.010(4) 0.009(5) Cl4 0.049(5) 0.091(7) 0.072(6) 0.035(5) 0.008(5) 0.028(5) Cl7 0.045(6) 0.095(8) 0.041(3) 0.006(4) 0.005(4) 0.039(5) Cl8 0.040(4) 0.068(10) 0.058(9) 0.017(6) 0.006(5) 0.018(6) C137 0.032(11) 0.050(7) 0.035(7) 0.000(6) 0.009(10) 0.017(10) _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 F3 C110 1.329(6) . ? F17 C111 1.330(6) . ? F5 C75 1.347(6) . ? F1 C82 1.347(6) . ? F6 C105 1.320(6) . ? F22 C84 1.332(6) . ? F16 C77 1.343(6) . ? F21 C76 1.338(6) . ? F19 C108 1.347(6) . ? F4 C58 1.348(6) . ? F11 C124 1.344(6) . ? F25 C116 1.338(6) . ? F15 C83 1.334(6) . ? F2 C109 1.342(6) . ? F20 C114 1.348(6) . ? F18 C66 1.343(6) . ? F23 C107 1.340(6) . ? F10 C122 1.342(7) . ? F30 C113 1.332(6) . ? F26 C80 1.340(6) . ? F24 C63 1.346(6) . ? F14 C52 1.349(6) . ? F27 C79 1.331(7) . ? F13 C128 1.347(6) . ? F28 C121 1.333(6) . ? F7 C131 1.342(7) . ? F29 C120 1.327(7) . ? F12 C127 1.340(6) . ? N6 C45 1.362(6) . ? N6 C53 1.368(7) . ? N6 H6 0.8800 . ? N1 C65 1.362(7) . ? N1 C102 1.376(7) . ? N1 H1 0.8800 . ? C37 C45 1.414(7) . ? C37 C48 1.418(7) . ? C37 C106 1.479(7) . ? F9 C132 1.341(7) . ? N3 C55 1.363(7) . ? N3 C68 1.374(7) . ? N3 H3 0.8800 . ? N2 C104 1.330(7) . ? N2 C85 1.390(7) . ? C41 C87 1.368(7) . ? C41 C55 1.458(7) . ? C41 C95 1.488(7) . ? N4 C64 1.368(7) . ? N4 C87 1.375(6) . ? N4 H4 0.8800 . ? F8 C126 1.329(7) . ? C44 C57 1.389(8) . ? C44 C115 1.395(8) . ? C44 C48 1.476(8) . ? C45 C47 1.448(7) . ? C46 C113 1.383(8) . ? C46 C80 1.401(8) . ? C46 C72 1.478(7) . ? C47 C50 1.377(7) . ? C47 C70 1.492(7) . ? C48 C53 1.406(7) . ? C49 C68 1.411(7) . ? C49 C90 1.419(7) . ? C49 C92 1.483(7) . ? C50 N5 1.386(6) . ? C50 C89 1.452(7) . ? C51 C82 1.384(8) . ? C51 C75 1.388(7) . ? C51 C71 1.490(7) . ? C52 C128 1.363(8) . ? C52 C83 1.385(8) . ? C53 C67 1.462(7) . ? N5 C56 1.320(7) . ? C55 C90 1.398(7) . ? C56 C71 1.429(7) . ? C56 C119 1.462(7) . ? C57 C103 1.382(8) . ? C57 H57 0.9500 . ? C58 C75 1.366(7) . ? C58 C110 1.384(8) . ? C59 C81 1.381(7) . ? C59 C91 1.394(7) . ? C59 H59 0.9500 . ? C60 C125 1.350(8) . ? C60 C85 1.457(8) . ? C60 H60 0.9500 . ? C61 C106 1.384(8) . ? C61 C123 1.393(7) . ? C61 H61 0.9500 . ? C62 C74 1.345(7) . ? C62 C87 1.456(7) . ? C62 H62 0.9500 . ? C63 C116 1.366(8) . ? C63 C107 1.373(8) . ? C64 C71 1.390(7) . ? C64 C74 1.447(7) . ? C65 C86 1.379(7) . ? C65 C130 1.448(8) . ? C66 C111 1.368(8) . ? C66 C108 1.379(8) . ? C67 C102 1.365(8) . ? C67 C96 1.498(7) . ? C68 C72 1.445(7) . ? C69 C112 1.382(8) . ? C69 C123 1.391(8) . ? C69 H69 0.9500 . ? C70 C116 1.390(8) . ? C70 C76 1.399(8) . ? C72 C85 1.383(7) . ? C73 C78 1.364(8) . ? C73 C129 1.396(8) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C76 C84 1.381(8) . ? C77 C111 1.376(8) . ? C77 C100 1.392(7) . ? C78 C91 1.400(7) . ? C78 H78 0.9500 . ? C79 C121 1.369(9) . ? C79 C80 1.376(8) . ? C81 C129 1.382(8) . ? C81 H81 0.9500 . ? C82 C109 1.378(8) . ? C83 C95 1.388(7) . ? C84 C107 1.378(8) . ? C86 C104 1.433(7) . ? C86 C100 1.500(7) . ? C88 C118 1.379(9) . ? C88 C94 1.388(8) . ? C88 H88 0.9500 . ? C89 C119 1.338(8) . ? C89 H89 0.9500 . ? C90 C91 1.485(7) . ? C92 C117 1.387(8) . ? C92 C93 1.398(8) . ? C93 C118 1.382(8) . ? C93 H93 0.9500 . ? C94 C117 1.383(7) . ? C94 H94 0.9500 . ? C95 C124 1.386(8) . ? C96 C122 1.374(8) . ? C96 C105 1.406(8) . ? C97 C115 1.382(8) . ? C97 C98 1.388(8) . ? C97 H97 0.9500 . ? C98 C103 1.387(8) . ? C98 H98 0.9500 . ? C99 C130 1.336(8) . ? C99 C102 1.444(8) . ? C99 H99 0.9500 . ? C100 C114 1.377(8) . ? C101 C112 1.382(8) . ? C101 C106 1.408(7) . ? C101 H101 0.9500 . ? C103 H103 0.9500 . ? C104 C125 1.453(7) . ? C105 C131 1.386(8) . ? C108 C114 1.377(8) . ? C109 C110 1.376(8) . ? C112 H112 0.9500 . ? C113 C120 1.397(8) . ? C115 H115 0.9500 . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C119 H119 0.9500 . ? C120 C121 1.378(9) . ? C122 C132 1.370(8) . ? C123 H123 0.9500 . ? C124 C127 1.373(8) . ? C125 H125 0.9500 . ? C126 C131 1.369(9) . ? C126 C132 1.380(9) . ? C127 C128 1.378(8) . ? C129 H129 0.9500 . ? C130 H130 0.9500 . ? Cl1 C133 1.740(7) . ? Cl2 C133 1.776(8) . ? Cl5 C135 1.714(11) . ? Cl6 C135 1.697(12) . ? C133 H137 0.9900 . ? C133 H138 0.9900 . ? C135 H131 0.9900 . ? C135 H132 0.9900 . ? C134 Cl3 1.70(4) . ? C134 Cl4 1.80(4) . ? C134 H133 0.9900 . ? C134 H134 0.9900 . ? Cl7 C137 1.68(4) . ? Cl8 C137 1.81(4) . ? C137 H135 0.9900 . ? C137 H136 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C45 N6 C53 111.5(4) . . ? C45 N6 H6 124.2 . . ? C53 N6 H6 124.2 . . ? C65 N1 C102 112.0(4) . . ? C65 N1 H1 124.0 . . ? C102 N1 H1 124.0 . . ? C45 C37 C48 107.6(5) . . ? C45 C37 C106 126.5(5) . . ? C48 C37 C106 126.0(5) . . ? C55 N3 C68 111.7(4) . . ? C55 N3 H3 124.2 . . ? C68 N3 H3 124.2 . . ? C104 N2 C85 106.8(4) . . ? C87 C41 C55 125.7(5) . . ? C87 C41 C95 119.0(4) . . ? C55 C41 C95 115.2(4) . . ? C64 N4 C87 111.6(4) . . ? C64 N4 H4 124.2 . . ? C87 N4 H4 124.2 . . ? C57 C44 C115 118.4(5) . . ? C57 C44 C48 121.1(5) . . ? C115 C44 C48 120.4(5) . . ? N6 C45 C37 106.7(4) . . ? N6 C45 C47 121.0(5) . . ? C37 C45 C47 132.3(5) . . ? C113 C46 C80 116.6(5) . . ? C113 C46 C72 122.5(5) . . ? C80 C46 C72 120.8(5) . . ? C50 C47 C45 120.6(5) . . ? C50 C47 C70 121.4(5) . . ? C45 C47 C70 117.9(5) . . ? C53 C48 C37 107.1(5) . . ? C53 C48 C44 127.1(5) . . ? C37 C48 C44 125.8(5) . . ? C68 C49 C90 107.2(4) . . ? C68 C49 C92 127.2(5) . . ? C90 C49 C92 125.5(5) . . ? C47 C50 N5 120.3(5) . . ? C47 C50 C89 131.3(5) . . ? N5 C50 C89 108.2(4) . . ? C82 C51 C75 115.9(5) . . ? C82 C51 C71 122.3(5) . . ? C75 C51 C71 121.8(5) . . ? F14 C52 C128 119.8(5) . . ? F14 C52 C83 119.9(5) . . ? C128 C52 C83 120.3(5) . . ? N6 C53 C48 107.1(4) . . ? N6 C53 C67 118.6(5) . . ? C48 C53 C67 133.9(5) . . ? C56 N5 C50 107.7(4) . . ? N3 C55 C90 107.0(4) . . ? N3 C55 C41 119.4(4) . . ? C90 C55 C41 133.1(5) . . ? N5 C56 C71 120.0(5) . . ? N5 C56 C119 110.2(5) . . ? C71 C56 C119 129.7(5) . . ? C103 C57 C44 121.7(5) . . ? C103 C57 H57 119.2 . . ? C44 C57 H57 119.2 . . ? F4 C58 C75 121.0(5) . . ? F4 C58 C110 118.6(5) . . ? C75 C58 C110 120.5(5) . . ? C81 C59 C91 120.7(5) . . ? C81 C59 H59 119.6 . . ? C91 C59 H59 119.6 . . ? C125 C60 C85 106.1(5) . . ? C125 C60 H60 126.9 . . ? C85 C60 H60 126.9 . . ? C106 C61 C123 120.8(5) . . ? C106 C61 H61 119.6 . . ? C123 C61 H61 119.6 . . ? C74 C62 C87 108.2(5) . . ? C74 C62 H62 125.9 . . ? C87 C62 H62 125.9 . . ? F24 C63 C116 120.4(5) . . ? F24 C63 C107 119.5(5) . . ? C116 C63 C107 120.1(5) . . ? N4 C64 C71 124.9(5) . . ? N4 C64 C74 105.7(4) . . ? C71 C64 C74 129.3(5) . . ? N1 C65 C86 125.3(5) . . ? N1 C65 C130 105.3(5) . . ? C86 C65 C130 129.3(5) . . ? F18 C66 C111 120.3(5) . . ? F18 C66 C108 119.5(5) . . ? C111 C66 C108 120.2(5) . . ? C102 C67 C53 125.6(5) . . ? C102 C67 C96 118.9(5) . . ? C53 C67 C96 115.5(5) . . ? N3 C68 C49 106.3(4) . . ? N3 C68 C72 120.5(5) . . ? C49 C68 C72 133.0(5) . . ? C112 C69 C123 119.9(5) . . ? C112 C69 H69 120.1 . . ? C123 C69 H69 120.1 . . ? C116 C70 C76 116.1(5) . . ? C116 C70 C47 122.1(5) . . ? C76 C70 C47 121.4(5) . . ? C64 C71 C56 121.2(5) . . ? C64 C71 C51 118.2(5) . . ? C56 C71 C51 120.5(4) . . ? C85 C72 C68 120.9(5) . . ? C85 C72 C46 120.2(5) . . ? C68 C72 C46 118.7(5) . . ? C78 C73 C129 120.2(5) . . ? C78 C73 H73 119.9 . . ? C129 C73 H73 119.9 . . ? C62 C74 C64 108.8(5) . . ? C62 C74 H74 125.6 . . ? C64 C74 H74 125.6 . . ? F5 C75 C58 117.8(5) . . ? F5 C75 C51 119.9(5) . . ? C58 C75 C51 122.3(5) . . ? F21 C76 C84 117.8(5) . . ? F21 C76 C70 119.9(5) . . ? C84 C76 C70 122.1(5) . . ? F16 C77 C111 118.7(5) . . ? F16 C77 C100 118.8(5) . . ? C111 C77 C100 122.5(5) . . ? C73 C78 C91 121.0(5) . . ? C73 C78 H78 119.5 . . ? C91 C78 H78 119.5 . . ? F27 C79 C121 120.2(5) . . ? F27 C79 C80 120.1(6) . . ? C121 C79 C80 119.6(5) . . ? F26 C80 C79 118.2(5) . . ? F26 C80 C46 119.6(5) . . ? C79 C80 C46 122.2(5) . . ? C59 C81 C129 120.2(5) . . ? C59 C81 H81 119.9 . . ? C129 C81 H81 119.9 . . ? F1 C82 C109 117.6(5) . . ? F1 C82 C51 119.5(5) . . ? C109 C82 C51 122.8(5) . . ? F15 C83 C52 118.5(5) . . ? F15 C83 C95 120.1(5) . . ? C52 C83 C95 121.4(5) . . ? F22 C84 C107 120.2(5) . . ? F22 C84 C76 120.6(5) . . ? C107 C84 C76 119.2(5) . . ? C72 C85 N2 120.5(5) . . ? C72 C85 C60 130.2(5) . . ? N2 C85 C60 109.2(4) . . ? C65 C86 C104 121.1(5) . . ? C65 C86 C100 118.7(5) . . ? C104 C86 C100 120.1(4) . . ? C41 C87 N4 127.4(5) . . ? C41 C87 C62 127.1(5) . . ? N4 C87 C62 105.3(4) . . ? C118 C88 C94 119.0(5) . . ? C118 C88 H88 120.5 . . ? C94 C88 H88 120.5 . . ? C119 C89 C50 107.3(5) . . ? C119 C89 H89 126.3 . . ? C50 C89 H89 126.3 . . ? C55 C90 C49 107.8(5) . . ? C55 C90 C91 125.3(5) . . ? C49 C90 C91 126.9(5) . . ? C59 C91 C78 118.3(5) . . ? C59 C91 C90 120.3(5) . . ? C78 C91 C90 121.3(5) . . ? C117 C92 C93 118.4(5) . . ? C117 C92 C49 122.0(5) . . ? C93 C92 C49 119.6(5) . . ? C118 C93 C92 120.2(5) . . ? C118 C93 H93 119.9 . . ? C92 C93 H93 119.9 . . ? C117 C94 C88 120.3(5) . . ? C117 C94 H94 119.9 . . ? C88 C94 H94 119.9 . . ? C124 C95 C83 116.6(5) . . ? C124 C95 C41 120.5(5) . . ? C83 C95 C41 122.8(5) . . ? C122 C96 C105 117.0(5) . . ? C122 C96 C67 121.7(5) . . ? C105 C96 C67 121.2(5) . . ? C115 C97 C98 120.5(5) . . ? C115 C97 H97 119.8 . . ? C98 C97 H97 119.8 . . ? C103 C98 C97 119.8(5) . . ? C103 C98 H98 120.1 . . ? C97 C98 H98 120.1 . . ? C130 C99 C102 109.0(5) . . ? C130 C99 H99 125.5 . . ? C102 C99 H99 125.5 . . ? C114 C100 C77 116.5(5) . . ? C114 C100 C86 122.9(5) . . ? C77 C100 C86 120.5(5) . . ? C112 C101 C106 120.6(5) . . ? C112 C101 H101 119.7 . . ? C106 C101 H101 119.7 . . ? C67 C102 N1 126.2(5) . . ? C67 C102 C99 128.7(5) . . ? N1 C102 C99 104.8(4) . . ? C57 C103 C98 119.3(5) . . ? C57 C103 H103 120.4 . . ? C98 C103 H103 120.4 . . ? N2 C104 C86 120.1(5) . . ? N2 C104 C125 110.6(5) . . ? C86 C104 C125 129.2(5) . . ? F6 C105 C131 119.1(5) . . ? F6 C105 C96 120.8(5) . . ? C131 C105 C96 120.1(5) . . ? C61 C106 C101 118.6(5) . . ? C61 C106 C37 121.1(5) . . ? C101 C106 C37 120.3(5) . . ? F23 C107 C63 120.9(5) . . ? F23 C107 C84 119.1(5) . . ? C63 C107 C84 120.0(5) . . ? F19 C108 C114 120.6(5) . . ? F19 C108 C66 119.7(5) . . ? C114 C108 C66 119.6(5) . . ? F2 C109 C110 119.7(5) . . ? F2 C109 C82 120.7(5) . . ? C110 C109 C82 119.6(5) . . ? F3 C110 C109 120.4(5) . . ? F3 C110 C58 120.8(5) . . ? C109 C110 C58 118.8(5) . . ? F17 C111 C66 119.6(5) . . ? F17 C111 C77 121.3(5) . . ? C66 C111 C77 119.1(5) . . ? C101 C112 C69 120.2(5) . . ? C101 C112 H112 119.9 . . ? C69 C112 H112 119.9 . . ? F30 C113 C46 120.2(5) . . ? F30 C113 C120 118.0(5) . . ? C46 C113 C120 121.7(5) . . ? F20 C114 C108 117.6(5) . . ? F20 C114 C100 120.3(5) . . ? C108 C114 C100 122.0(5) . . ? C97 C115 C44 120.3(5) . . ? C97 C115 H115 119.9 . . ? C44 C115 H115 119.9 . . ? F25 C116 C63 118.0(5) . . ? F25 C116 C70 119.6(5) . . ? C63 C116 C70 122.4(5) . . ? C94 C117 C92 121.0(5) . . ? C94 C117 H117 119.5 . . ? C92 C117 H117 119.5 . . ? C88 C118 C93 121.1(6) . . ? C88 C118 H118 119.5 . . ? C93 C118 H118 119.5 . . ? C89 C119 C56 106.5(5) . . ? C89 C119 H119 126.8 . . ? C56 C119 H119 126.8 . . ? F29 C120 C121 120.7(5) . . ? F29 C120 C113 120.0(5) . . ? C121 C120 C113 119.3(5) . . ? F28 C121 C79 120.3(6) . . ? F28 C121 C120 119.3(6) . . ? C79 C121 C120 120.4(5) . . ? F10 C122 C132 117.7(5) . . ? F10 C122 C96 119.4(5) . . ? C132 C122 C96 122.9(5) . . ? C69 C123 C61 119.9(5) . . ? C69 C123 H123 120.0 . . ? C61 C123 H123 120.0 . . ? F11 C124 C127 118.1(5) . . ? F11 C124 C95 119.3(5) . . ? C127 C124 C95 122.5(5) . . ? C60 C125 C104 107.2(5) . . ? C60 C125 H125 126.4 . . ? C104 C125 H125 126.4 . . ? F8 C126 C131 120.2(6) . . ? F8 C126 C132 120.6(6) . . ? C131 C126 C132 119.2(6) . . ? F12 C127 C124 120.5(5) . . ? F12 C127 C128 120.0(5) . . ? C124 C127 C128 119.4(5) . . ? F13 C128 C52 120.6(5) . . ? F13 C128 C127 119.6(5) . . ? C52 C128 C127 119.8(5) . . ? C81 C129 C73 119.5(5) . . ? C81 C129 H129 120.3 . . ? C73 C129 H129 120.3 . . ? C99 C130 C65 108.6(5) . . ? C99 C130 H130 125.7 . . ? C65 C130 H130 125.7 . . ? F7 C131 C126 119.7(5) . . ? F7 C131 C105 119.1(6) . . ? C126 C131 C105 121.2(6) . . ? F9 C132 C122 121.1(6) . . ? F9 C132 C126 119.3(6) . . ? C122 C132 C126 119.6(6) . . ? Cl1 C133 Cl2 111.3(4) . . ? Cl1 C133 H137 109.4 . . ? Cl2 C133 H137 109.4 . . ? Cl1 C133 H138 109.4 . . ? Cl2 C133 H138 109.4 . . ? H137 C133 H138 108.0 . . ? Cl6 C135 Cl5 114.5(7) . . ? Cl6 C135 H131 108.6 . . ? Cl5 C135 H131 108.6 . . ? Cl6 C135 H132 108.6 . . ? Cl5 C135 H132 108.6 . . ? H131 C135 H132 107.6 . . ? Cl3 C134 Cl4 111(3) . . ? Cl3 C134 H133 109.4 . . ? Cl4 C134 H133 109.4 . . ? Cl3 C134 H134 109.4 . . ? Cl4 C134 H134 109.4 . . ? H133 C134 H134 108.0 . . ? Cl7 C137 Cl8 113(3) . . ? Cl7 C137 H135 108.9 . . ? Cl8 C137 H135 108.9 . . ? Cl7 C137 H136 108.9 . . ? Cl8 C137 H136 108.9 . . ? H135 C137 H136 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C53 N6 C45 C37 1.3(6) . . . . ? C53 N6 C45 C47 178.9(5) . . . . ? C48 C37 C45 N6 -0.3(6) . . . . ? C106 C37 C45 N6 179.5(5) . . . . ? C48 C37 C45 C47 -177.6(5) . . . . ? C106 C37 C45 C47 2.2(9) . . . . ? N6 C45 C47 C50 24.8(7) . . . . ? C37 C45 C47 C50 -158.3(5) . . . . ? N6 C45 C47 C70 -152.7(5) . . . . ? C37 C45 C47 C70 24.3(8) . . . . ? C45 C37 C48 C53 -0.7(6) . . . . ? C106 C37 C48 C53 179.5(5) . . . . ? C45 C37 C48 C44 -179.4(5) . . . . ? C106 C37 C48 C44 0.8(9) . . . . ? C57 C44 C48 C53 -127.9(6) . . . . ? C115 C44 C48 C53 48.7(8) . . . . ? C57 C44 C48 C37 50.6(8) . . . . ? C115 C44 C48 C37 -132.8(6) . . . . ? C45 C47 C50 N5 8.2(7) . . . . ? C70 C47 C50 N5 -174.4(5) . . . . ? C45 C47 C50 C89 -166.1(5) . . . . ? C70 C47 C50 C89 11.2(9) . . . . ? C45 N6 C53 C48 -1.7(6) . . . . ? C45 N6 C53 C67 -175.7(4) . . . . ? C37 C48 C53 N6 1.4(6) . . . . ? C44 C48 C53 N6 -179.9(5) . . . . ? C37 C48 C53 C67 174.2(6) . . . . ? C44 C48 C53 C67 -7.1(10) . . . . ? C47 C50 N5 C56 -175.1(5) . . . . ? C89 C50 N5 C56 0.4(6) . . . . ? C68 N3 C55 C90 -1.2(6) . . . . ? C68 N3 C55 C41 -174.1(4) . . . . ? C87 C41 C55 N3 -148.3(5) . . . . ? C95 C41 C55 N3 35.6(7) . . . . ? C87 C41 C55 C90 41.1(9) . . . . ? C95 C41 C55 C90 -135.0(6) . . . . ? C50 N5 C56 C71 -179.0(5) . . . . ? C50 N5 C56 C119 0.6(6) . . . . ? C115 C44 C57 C103 -2.2(8) . . . . ? C48 C44 C57 C103 174.5(5) . . . . ? C87 N4 C64 C71 172.4(5) . . . . ? C87 N4 C64 C74 -3.7(6) . . . . ? C102 N1 C65 C86 175.7(5) . . . . ? C102 N1 C65 C130 -1.8(6) . . . . ? N6 C53 C67 C102 -151.5(5) . . . . ? C48 C53 C67 C102 36.4(9) . . . . ? N6 C53 C67 C96 27.3(7) . . . . ? C48 C53 C67 C96 -144.8(6) . . . . ? C55 N3 C68 C49 1.6(6) . . . . ? C55 N3 C68 C72 178.1(4) . . . . ? C90 C49 C68 N3 -1.3(5) . . . . ? C92 C49 C68 N3 177.4(5) . . . . ? C90 C49 C68 C72 -177.2(5) . . . . ? C92 C49 C68 C72 1.5(9) . . . . ? C50 C47 C70 C116 -128.8(6) . . . . ? C45 C47 C70 C116 48.7(7) . . . . ? C50 C47 C70 C76 58.9(7) . . . . ? C45 C47 C70 C76 -123.7(6) . . . . ? N4 C64 C71 C56 8.3(8) . . . . ? C74 C64 C71 C56 -176.6(5) . . . . ? N4 C64 C71 C51 -171.8(5) . . . . ? C74 C64 C71 C51 3.3(8) . . . . ? N5 C56 C71 C64 15.4(8) . . . . ? C119 C56 C71 C64 -164.1(5) . . . . ? N5 C56 C71 C51 -164.4(5) . . . . ? C119 C56 C71 C51 16.1(8) . . . . ? C82 C51 C71 C64 107.9(6) . . . . ? C75 C51 C71 C64 -70.6(7) . . . . ? C82 C51 C71 C56 -72.2(7) . . . . ? C75 C51 C71 C56 109.3(6) . . . . ? N3 C68 C72 C85 26.6(7) . . . . ? C49 C68 C72 C85 -157.9(5) . . . . ? N3 C68 C72 C46 -148.5(5) . . . . ? C49 C68 C72 C46 27.0(8) . . . . ? C113 C46 C72 C85 62.0(7) . . . . ? C80 C46 C72 C85 -120.9(6) . . . . ? C113 C46 C72 C68 -122.8(6) . . . . ? C80 C46 C72 C68 54.3(7) . . . . ? C87 C62 C74 C64 3.3(6) . . . . ? N4 C64 C74 C62 0.1(6) . . . . ? C71 C64 C74 C62 -175.8(5) . . . . ? F4 C58 C75 F5 0.3(7) . . . . ? C110 C58 C75 F5 -179.7(5) . . . . ? F4 C58 C75 C51 179.5(5) . . . . ? C110 C58 C75 C51 -0.4(8) . . . . ? C82 C51 C75 F5 179.6(4) . . . . ? C71 C51 C75 F5 -1.8(7) . . . . ? C82 C51 C75 C58 0.4(8) . . . . ? C71 C51 C75 C58 179.0(5) . . . . ? C116 C70 C76 F21 -177.2(5) . . . . ? C47 C70 C76 F21 -4.4(8) . . . . ? C116 C70 C76 C84 -2.6(8) . . . . ? C47 C70 C76 C84 170.2(5) . . . . ? C129 C73 C78 C91 -0.7(8) . . . . ? F27 C79 C80 F26 2.6(8) . . . . ? C121 C79 C80 F26 179.6(5) . . . . ? F27 C79 C80 C46 -177.1(5) . . . . ? C121 C79 C80 C46 -0.1(8) . . . . ? C113 C46 C80 F26 -178.0(5) . . . . ? C72 C46 C80 F26 4.7(8) . . . . ? C113 C46 C80 C79 1.6(8) . . . . ? C72 C46 C80 C79 -175.6(5) . . . . ? C91 C59 C81 C129 0.3(8) . . . . ? C75 C51 C82 F1 178.8(5) . . . . ? C71 C51 C82 F1 0.2(8) . . . . ? C75 C51 C82 C109 -0.5(8) . . . . ? C71 C51 C82 C109 -179.1(5) . . . . ? F14 C52 C83 F15 -1.4(8) . . . . ? C128 C52 C83 F15 178.3(5) . . . . ? F14 C52 C83 C95 -179.6(5) . . . . ? C128 C52 C83 C95 0.0(8) . . . . ? F21 C76 C84 F22 -2.3(8) . . . . ? C70 C76 C84 F22 -177.0(5) . . . . ? F21 C76 C84 C107 176.1(5) . . . . ? C70 C76 C84 C107 1.4(8) . . . . ? C68 C72 C85 N2 6.2(7) . . . . ? C46 C72 C85 N2 -178.7(5) . . . . ? C68 C72 C85 C60 -168.6(5) . . . . ? C46 C72 C85 C60 6.5(8) . . . . ? C104 N2 C85 C72 -174.4(5) . . . . ? C104 N2 C85 C60 1.4(6) . . . . ? C125 C60 C85 C72 173.6(5) . . . . ? C125 C60 C85 N2 -1.6(6) . . . . ? N1 C65 C86 C104 8.7(9) . . . . ? C130 C65 C86 C104 -174.3(5) . . . . ? N1 C65 C86 C100 -173.6(5) . . . . ? C130 C65 C86 C100 3.3(9) . . . . ? C55 C41 C87 N4 10.9(9) . . . . ? C95 C41 C87 N4 -173.1(5) . . . . ? C55 C41 C87 C62 -163.7(5) . . . . ? C95 C41 C87 C62 12.2(8) . . . . ? C64 N4 C87 C41 -170.0(5) . . . . ? C64 N4 C87 C62 5.6(6) . . . . ? C74 C62 C87 C41 170.2(5) . . . . ? C74 C62 C87 N4 -5.4(6) . . . . ? C47 C50 C89 C119 173.5(6) . . . . ? N5 C50 C89 C119 -1.4(6) . . . . ? N3 C55 C90 C49 0.4(6) . . . . ? C41 C55 C90 C49 171.8(5) . . . . ? N3 C55 C90 C91 -179.2(5) . . . . ? C41 C55 C90 C91 -7.8(9) . . . . ? C68 C49 C90 C55 0.6(6) . . . . ? C92 C49 C90 C55 -178.2(5) . . . . ? C68 C49 C90 C91 -179.8(5) . . . . ? C92 C49 C90 C91 1.4(8) . . . . ? C81 C59 C91 C78 -2.1(7) . . . . ? C81 C59 C91 C90 174.4(5) . . . . ? C73 C78 C91 C59 2.3(8) . . . . ? C73 C78 C91 C90 -174.2(5) . . . . ? C55 C90 C91 C59 -121.7(6) . . . . ? C49 C90 C91 C59 58.8(7) . . . . ? C55 C90 C91 C78 54.6(7) . . . . ? C49 C90 C91 C78 -124.9(6) . . . . ? C68 C49 C92 C117 49.8(7) . . . . ? C90 C49 C92 C117 -131.6(6) . . . . ? C68 C49 C92 C93 -129.3(6) . . . . ? C90 C49 C92 C93 49.2(7) . . . . ? C117 C92 C93 C118 1.4(8) . . . . ? C49 C92 C93 C118 -179.4(5) . . . . ? C118 C88 C94 C117 0.4(9) . . . . ? F15 C83 C95 C124 -177.9(5) . . . . ? C52 C83 C95 C124 0.3(8) . . . . ? F15 C83 C95 C41 -0.8(8) . . . . ? C52 C83 C95 C41 177.4(5) . . . . ? C87 C41 C95 C124 -106.5(6) . . . . ? C55 C41 C95 C124 69.9(6) . . . . ? C87 C41 C95 C83 76.6(7) . . . . ? C55 C41 C95 C83 -107.1(6) . . . . ? C102 C67 C96 C122 -121.8(6) . . . . ? C53 C67 C96 C122 59.4(7) . . . . ? C102 C67 C96 C105 61.3(7) . . . . ? C53 C67 C96 C105 -117.6(6) . . . . ? C115 C97 C98 C103 -0.9(8) . . . . ? F16 C77 C100 C114 179.3(5) . . . . ? C111 C77 C100 C114 -1.8(8) . . . . ? F16 C77 C100 C86 -1.3(7) . . . . ? C111 C77 C100 C86 177.6(5) . . . . ? C65 C86 C100 C114 87.1(7) . . . . ? C104 C86 C100 C114 -95.2(6) . . . . ? C65 C86 C100 C77 -92.3(6) . . . . ? C104 C86 C100 C77 85.4(7) . . . . ? C53 C67 C102 N1 11.1(9) . . . . ? C96 C67 C102 N1 -167.7(5) . . . . ? C53 C67 C102 C99 -161.8(6) . . . . ? C96 C67 C102 C99 19.5(9) . . . . ? C65 N1 C102 C67 -170.1(5) . . . . ? C65 N1 C102 C99 4.2(6) . . . . ? C130 C99 C102 C67 169.0(6) . . . . ? C130 C99 C102 N1 -5.1(6) . . . . ? C44 C57 C103 C98 0.1(8) . . . . ? C97 C98 C103 C57 1.5(8) . . . . ? C85 N2 C104 C86 -179.1(5) . . . . ? C85 N2 C104 C125 -0.6(6) . . . . ? C65 C86 C104 N2 15.5(8) . . . . ? C100 C86 C104 N2 -162.1(5) . . . . ? C65 C86 C104 C125 -162.7(5) . . . . ? C100 C86 C104 C125 19.7(8) . . . . ? C122 C96 C105 F6 -178.8(5) . . . . ? C67 C96 C105 F6 -1.6(8) . . . . ? C122 C96 C105 C131 0.0(8) . . . . ? C67 C96 C105 C131 177.2(5) . . . . ? C123 C61 C106 C101 -0.5(8) . . . . ? C123 C61 C106 C37 -178.8(5) . . . . ? C112 C101 C106 C61 1.7(8) . . . . ? C112 C101 C106 C37 -180.0(5) . . . . ? C45 C37 C106 C61 -127.8(6) . . . . ? C48 C37 C106 C61 51.9(8) . . . . ? C45 C37 C106 C101 53.9(7) . . . . ? C48 C37 C106 C101 -126.4(6) . . . . ? F24 C63 C107 F23 -1.7(8) . . . . ? C116 C63 C107 F23 177.9(5) . . . . ? F24 C63 C107 C84 178.1(5) . . . . ? C116 C63 C107 C84 -2.3(9) . . . . ? F22 C84 C107 F23 -0.6(8) . . . . ? C76 C84 C107 F23 -179.0(5) . . . . ? F22 C84 C107 C63 179.6(5) . . . . ? C76 C84 C107 C63 1.2(8) . . . . ? F18 C66 C108 F19 0.5(7) . . . . ? C111 C66 C108 F19 -179.2(5) . . . . ? F18 C66 C108 C114 178.6(5) . . . . ? C111 C66 C108 C114 -1.0(8) . . . . ? F1 C82 C109 F2 0.9(8) . . . . ? C51 C82 C109 F2 -179.8(5) . . . . ? F1 C82 C109 C110 -178.7(5) . . . . ? C51 C82 C109 C110 0.7(8) . . . . ? F2 C109 C110 F3 0.2(8) . . . . ? C82 C109 C110 F3 179.8(5) . . . . ? F2 C109 C110 C58 179.8(5) . . . . ? C82 C109 C110 C58 -0.7(8) . . . . ? F4 C58 C110 F3 0.2(7) . . . . ? C75 C58 C110 F3 -179.9(5) . . . . ? F4 C58 C110 C109 -179.4(5) . . . . ? C75 C58 C110 C109 0.6(8) . . . . ? F18 C66 C111 F17 0.5(8) . . . . ? C108 C66 C111 F17 -179.9(5) . . . . ? F18 C66 C111 C77 -179.4(5) . . . . ? C108 C66 C111 C77 0.2(8) . . . . ? F16 C77 C111 F17 0.3(8) . . . . ? C100 C77 C111 F17 -178.7(5) . . . . ? F16 C77 C111 C66 -179.9(5) . . . . ? C100 C77 C111 C66 1.2(8) . . . . ? C106 C101 C112 C69 -2.4(8) . . . . ? C123 C69 C112 C101 1.9(8) . . . . ? C80 C46 C113 F30 -179.2(5) . . . . ? C72 C46 C113 F30 -2.0(8) . . . . ? C80 C46 C113 C120 -2.5(8) . . . . ? C72 C46 C113 C120 174.7(5) . . . . ? F19 C108 C114 F20 -0.6(7) . . . . ? C66 C108 C114 F20 -178.8(5) . . . . ? F19 C108 C114 C100 178.5(5) . . . . ? C66 C108 C114 C100 0.3(8) . . . . ? C77 C100 C114 F20 -179.9(5) . . . . ? C86 C100 C114 F20 0.7(8) . . . . ? C77 C100 C114 C108 1.0(8) . . . . ? C86 C100 C114 C108 -178.4(5) . . . . ? C98 C97 C115 C44 -1.2(8) . . . . ? C57 C44 C115 C97 2.7(8) . . . . ? C48 C44 C115 C97 -174.0(5) . . . . ? F24 C63 C116 F25 0.3(8) . . . . ? C107 C63 C116 F25 -179.3(5) . . . . ? F24 C63 C116 C70 -179.5(5) . . . . ? C107 C63 C116 C70 0.9(9) . . . . ? C76 C70 C116 F25 -178.3(5) . . . . ? C47 C70 C116 F25 9.0(8) . . . . ? C76 C70 C116 C63 1.5(8) . . . . ? C47 C70 C116 C63 -171.3(5) . . . . ? C88 C94 C117 C92 -0.1(8) . . . . ? C93 C92 C117 C94 -0.8(8) . . . . ? C49 C92 C117 C94 180.0(5) . . . . ? C94 C88 C118 C93 0.2(9) . . . . ? C92 C93 C118 C88 -1.1(9) . . . . ? C50 C89 C119 C56 1.7(6) . . . . ? N5 C56 C119 C89 -1.5(6) . . . . ? C71 C56 C119 C89 178.0(5) . . . . ? F30 C113 C120 F29 -0.9(8) . . . . ? C46 C113 C120 F29 -177.7(5) . . . . ? F30 C113 C120 C121 178.6(5) . . . . ? C46 C113 C120 C121 1.8(8) . . . . ? F27 C79 C121 F28 -4.1(8) . . . . ? C80 C79 C121 F28 178.9(5) . . . . ? F27 C79 C121 C120 176.3(5) . . . . ? C80 C79 C121 C120 -0.7(9) . . . . ? F29 C120 C121 F28 -0.3(8) . . . . ? C113 C120 C121 F28 -179.8(5) . . . . ? F29 C120 C121 C79 179.3(5) . . . . ? C113 C120 C121 C79 -0.2(8) . . . . ? C105 C96 C122 F10 179.9(5) . . . . ? C67 C96 C122 F10 2.8(8) . . . . ? C105 C96 C122 C132 -1.0(9) . . . . ? C67 C96 C122 C132 -178.1(5) . . . . ? C112 C69 C123 C61 -0.7(8) . . . . ? C106 C61 C123 C69 0.0(8) . . . . ? C83 C95 C124 F11 178.5(5) . . . . ? C41 C95 C124 F11 1.3(8) . . . . ? C83 C95 C124 C127 -1.1(8) . . . . ? C41 C95 C124 C127 -178.2(5) . . . . ? C85 C60 C125 C104 1.2(6) . . . . ? N2 C104 C125 C60 -0.5(6) . . . . ? C86 C104 C125 C60 177.9(5) . . . . ? F11 C124 C127 F12 1.5(8) . . . . ? C95 C124 C127 F12 -179.0(5) . . . . ? F11 C124 C127 C128 -178.1(5) . . . . ? C95 C124 C127 C128 1.5(9) . . . . ? F14 C52 C128 F13 0.2(8) . . . . ? C83 C52 C128 F13 -179.4(5) . . . . ? F14 C52 C128 C127 -180.0(5) . . . . ? C83 C52 C128 C127 0.4(9) . . . . ? F12 C127 C128 F13 -0.8(9) . . . . ? C124 C127 C128 F13 178.7(5) . . . . ? F12 C127 C128 C52 179.4(5) . . . . ? C124 C127 C128 C52 -1.1(9) . . . . ? C59 C81 C129 C73 1.3(8) . . . . ? C78 C73 C129 C81 -1.1(8) . . . . ? C102 C99 C130 C65 4.1(7) . . . . ? N1 C65 C130 C99 -1.6(6) . . . . ? C86 C65 C130 C99 -179.0(6) . . . . ? F8 C126 C131 F7 -1.0(9) . . . . ? C132 C126 C131 F7 179.7(5) . . . . ? F8 C126 C131 C105 178.8(5) . . . . ? C132 C126 C131 C105 -0.5(9) . . . . ? F6 C105 C131 F7 -0.7(8) . . . . ? C96 C105 C131 F7 -179.5(5) . . . . ? F6 C105 C131 C126 179.6(5) . . . . ? C96 C105 C131 C126 0.7(9) . . . . ? F10 C122 C132 F9 -1.0(9) . . . . ? C96 C122 C132 F9 180.0(6) . . . . ? F10 C122 C132 C126 -179.7(6) . . . . ? C96 C122 C132 C126 1.3(10) . . . . ? F8 C126 C132 F9 1.5(9) . . . . ? C131 C126 C132 F9 -179.2(6) . . . . ? F8 C126 C132 C122 -179.7(6) . . . . ? C131 C126 C132 C122 -0.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.711 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.102