# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_0322hi _database_code_depnum_ccdc_archive 'CCDC 906719' #TrackingRef 'SO2_28-ChemSci.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H32 F30 N6 O8 S4, 0.5(C8 H18), 5(C6 H6)' _chemical_formula_sum 'C108 H71 F30 N6 O8 S4' _chemical_formula_weight 2278.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.2352(5) _cell_length_b 16.6412(7) _cell_length_c 25.9304(12) _cell_angle_alpha 76.808(3) _cell_angle_beta 80.972(3) _cell_angle_gamma 74.261(2) _cell_volume 4922.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 19325 _cell_measurement_theta_min 3.015 _cell_measurement_theta_max 68.21 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2318 _exptl_absorpt_coefficient_mu 1.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6962 _exptl_absorpt_correction_T_max 0.9087 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47536 _diffrn_reflns_av_R_equivalents 0.1746 _diffrn_reflns_av_sigmaI/netI 0.2584 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 61.00 _reflns_number_total 14648 _reflns_number_gt 3185 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^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 14648 _refine_ls_number_parameters 1428 _refine_ls_number_restraints 1074 _refine_ls_R_factor_all 0.3347 _refine_ls_R_factor_gt 0.1054 _refine_ls_wR_factor_ref 0.2861 _refine_ls_wR_factor_gt 0.1921 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 0.997 _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 0.9294(15) 0.1675(9) 0.3378(6) 0.109(4) Uani 1 1 d U . . C2 C 1.0385(13) 0.1111(8) 0.3541(5) 0.111(4) Uani 1 1 d U . . C3 C 1.1190(10) 0.1071(8) 0.3112(6) 0.105(4) Uani 1 1 d U . . C4 C 1.0659(13) 0.1592(8) 0.2664(6) 0.106(4) Uani 1 1 d U . . C5 C 1.1075(11) 0.1869(9) 0.2116(6) 0.100(4) Uani 1 1 d U . . C6 C 1.0592(12) 0.2630(10) 0.1815(6) 0.103(4) Uani 1 1 d U . . C7 C 1.0763(10) 0.2983(8) 0.1262(5) 0.105(4) Uani 1 1 d U . . H1 H 1.1309 0.2709 0.1014 0.126 Uiso 1 1 calc R . . C8 C 1.0038(11) 0.3771(9) 0.1137(6) 0.122(4) Uani 1 1 d U . . H2 H 0.9980 0.4140 0.0798 0.146 Uiso 1 1 calc R . . C9 C 0.9382(13) 0.3913(10) 0.1634(6) 0.109(4) Uani 1 1 d U . . C10 C 0.8398(12) 0.4581(9) 0.1708(6) 0.106(4) Uani 1 1 d U . . C11 C 0.7775(13) 0.4705(9) 0.2180(7) 0.105(4) Uani 1 1 d U . . C12 C 0.8050(12) 0.4459(8) 0.2706(6) 0.109(4) Uani 1 1 d U . . H3 H 0.8776 0.4124 0.2804 0.131 Uiso 1 1 calc R . . C13 C 0.7186(13) 0.4744(8) 0.3057(6) 0.117(4) Uani 1 1 d U . . H4 H 0.7182 0.4675 0.3431 0.141 Uiso 1 1 calc R . . C14 C 0.6249(15) 0.5188(8) 0.2728(7) 0.107(4) Uani 1 1 d U . . C15 C 0.5114(14) 0.5509(8) 0.2929(7) 0.119(4) Uani 1 1 d U . . C16 C 0.4238(14) 0.5757(9) 0.2532(7) 0.117(4) Uani 1 1 d U . . C17 C 0.3164(12) 0.6358(8) 0.2508(5) 0.102(4) Uani 1 1 d U . . C18 C 0.2720(10) 0.6233(8) 0.2077(6) 0.109(4) Uani 1 1 d U . . C19 C 0.3521(13) 0.5608(9) 0.1868(6) 0.110(4) Uani 1 1 d U . . C20 C 0.3587(11) 0.5171(9) 0.1422(6) 0.114(4) Uani 1 1 d U . . C21 C 0.4152(10) 0.4348(9) 0.1449(6) 0.100(4) Uani 1 1 d U . . C22 C 0.4397(9) 0.3830(8) 0.1036(5) 0.105(4) Uani 1 1 d U . . H5 H 0.4113 0.3995 0.0697 0.126 Uiso 1 1 calc R . . C23 C 0.5105(10) 0.3072(8) 0.1229(6) 0.109(4) Uani 1 1 d U . . H6 H 0.5405 0.2618 0.1041 0.131 Uiso 1 1 calc R . . C24 C 0.5333(12) 0.3058(9) 0.1759(6) 0.102(4) Uani 1 1 d U . . C25 C 0.6146(12) 0.2449(10) 0.2055(6) 0.110(4) Uani 1 1 d U . . C26 C 0.6328(13) 0.2532(7) 0.2550(7) 0.103(4) Uani 1 1 d U . . C27 C 0.5613(11) 0.2898(8) 0.2976(6) 0.115(4) Uani 1 1 d U . . H7 H 0.4844 0.3214 0.2949 0.137 Uiso 1 1 calc R . . C28 C 0.6147(12) 0.2745(7) 0.3417(5) 0.110(4) Uani 1 1 d U . . H8 H 0.5838 0.2928 0.3743 0.132 Uiso 1 1 calc R . . C29 C 0.7283(14) 0.2247(9) 0.3295(7) 0.111(4) Uani 1 1 d U . . C30 C 0.8171(14) 0.1966(8) 0.3604(7) 0.115(4) Uani 1 1 d U . . C31 C 1.1914(12) 0.1250(9) 0.1805(5) 0.105(4) Uani 1 1 d U . . C32 C 1.2917(14) 0.1432(9) 0.1532(6) 0.110(4) Uani 1 1 d U . . C33 C 1.3700(13) 0.0860(11) 0.1249(6) 0.111(4) Uani 1 1 d U . . C34 C 1.3526(15) 0.0129(11) 0.1219(6) 0.128(5) Uani 1 1 d U . . C35 C 1.2569(16) -0.0091(10) 0.1496(7) 0.133(5) Uani 1 1 d U . . C36 C 1.1830(12) 0.0461(10) 0.1764(6) 0.111(4) Uani 1 1 d U . . C37 C 0.7998(11) 0.5147(8) 0.1195(6) 0.106(4) Uani 1 1 d U . . C38 C 0.8513(12) 0.5739(9) 0.0918(7) 0.115(4) Uani 1 1 d U . . C39 C 0.8151(12) 0.6271(9) 0.0438(7) 0.119(5) Uani 1 1 d U . . C40 C 0.7226(12) 0.6160(8) 0.0251(6) 0.110(4) Uani 1 1 d U . . C41 C 0.6706(11) 0.5538(9) 0.0500(6) 0.108(4) Uani 1 1 d U . . C42 C 0.7109(12) 0.5034(8) 0.0976(6) 0.111(4) Uani 1 1 d U . . C43 C 0.4778(12) 0.5493(10) 0.3499(7) 0.114(4) Uani 1 1 d U . . C44 C 0.5050(13) 0.5966(10) 0.3797(9) 0.128(5) Uani 1 1 d U . . C45 C 0.4735(14) 0.5954(10) 0.4326(8) 0.121(5) Uani 1 1 d U . . C46 C 0.3975(16) 0.5435(13) 0.4553(7) 0.131(5) Uani 1 1 d U . . C47 C 0.3673(13) 0.4944(10) 0.4299(9) 0.124(5) Uani 1 1 d U . . C48 C 0.4056(15) 0.4986(10) 0.3765(8) 0.128(5) Uani 1 1 d U . . F11 F 0.5769(6) 0.6482(5) 0.3545(3) 0.145(3) Uani 1 1 d U . . F12 F 0.5016(7) 0.6430(5) 0.4595(3) 0.181(4) Uani 1 1 d U . . F13 F 0.3622(7) 0.5444(5) 0.5077(4) 0.165(3) Uani 1 1 d U . . F14 F 0.2949(7) 0.4467(5) 0.4546(3) 0.164(3) Uani 1 1 d U . . F15 F 0.3723(6) 0.4490(4) 0.3521(3) 0.141(3) Uani 1 1 d U . . C49 C 0.3049(10) 0.5631(8) 0.0934(6) 0.099(4) Uani 1 1 d U . . C50 C 0.3349(11) 0.6350(9) 0.0618(7) 0.112(4) Uani 1 1 d U . . C51 C 0.2823(13) 0.6778(9) 0.0153(7) 0.119(4) Uani 1 1 d U . . C52 C 0.2024(12) 0.6530(10) -0.0016(6) 0.112(4) Uani 1 1 d U . . C53 C 0.1773(11) 0.5814(9) 0.0272(6) 0.109(4) Uani 1 1 d U . . C54 C 0.2245(11) 0.5364(8) 0.0721(6) 0.105(4) Uani 1 1 d U . . C55 C 0.6872(12) 0.1735(10) 0.1799(5) 0.109(4) Uani 1 1 d U . . C56 C 0.6461(13) 0.1054(11) 0.1796(6) 0.117(4) Uani 1 1 d U . . C57 C 0.7178(15) 0.0365(10) 0.1573(6) 0.125(5) Uani 1 1 d U . . C58 C 0.8215(16) 0.0462(10) 0.1355(6) 0.132(5) Uani 1 1 d U . . C59 C 0.8644(15) 0.1091(11) 0.1324(6) 0.124(5) Uani 1 1 d U . . C60 C 0.7908(13) 0.1759(9) 0.1572(6) 0.108(4) Uani 1 1 d U . . C61 C 0.7909(12) 0.2068(10) 0.4146(8) 0.113(4) Uani 1 1 d U . . C62 C 0.8203(12) 0.2645(9) 0.4382(7) 0.109(5) Uani 1 1 d U . . C63 C 0.7967(14) 0.2730(10) 0.4888(8) 0.121(5) Uani 1 1 d U . . C64 C 0.7312(14) 0.2229(12) 0.5195(7) 0.125(5) Uani 1 1 d U . . C65 C 0.6973(13) 0.1626(10) 0.5030(8) 0.117(5) Uani 1 1 d U . . C66 C 0.7281(14) 0.1598(10) 0.4506(8) 0.119(5) Uani 1 1 d U . . F26 F 0.8831(5) 0.3159(4) 0.4040(3) 0.126(2) Uani 1 1 d U . . F27 F 0.8323(6) 0.3290(4) 0.5074(3) 0.149(3) Uani 1 1 d U . . F28 F 0.7040(6) 0.2280(4) 0.5737(3) 0.148(3) Uani 1 1 d U . . F29 F 0.6350(6) 0.1138(4) 0.5362(3) 0.138(3) Uani 1 1 d U . . F30 F 0.6919(5) 0.0984(4) 0.4341(3) 0.123(2) Uani 1 1 d U . . N1 N 0.9565(9) 0.1941(6) 0.2835(5) 0.108(3) Uani 1 1 d U . . N2 N 0.9752(9) 0.3250(8) 0.2038(4) 0.117(3) Uani 1 1 d U . . H83 H 0.9507 0.3219 0.2378 0.140 Uiso 1 1 calc R . . N3 N 0.6684(10) 0.5161(6) 0.2224(5) 0.117(4) Uani 1 1 d U . . H81 H 0.6296 0.5416 0.1949 0.140 Uiso 1 1 calc R . . N4 N 0.4451(9) 0.5340(6) 0.2134(5) 0.109(3) Uani 1 1 d U . . N5 N 0.4710(8) 0.3836(7) 0.1882(4) 0.105(3) Uani 1 1 d U . . H84 H 0.4673 0.3984 0.2190 0.126 Uiso 1 1 calc R . . N6 N 0.7330(9) 0.2149(6) 0.2777(5) 0.113(3) Uani 1 1 d U . . H82 H 0.7944 0.1868 0.2608 0.135 Uiso 1 1 calc R . . F1 F 1.3182(5) 0.2170(4) 0.1561(2) 0.125(2) Uani 1 1 d U . . F2 F 1.4653(6) 0.1126(4) 0.0989(3) 0.137(3) Uani 1 1 d U . . F3 F 1.4274(7) -0.0403(5) 0.0964(3) 0.162(3) Uani 1 1 d U . . F4 F 1.2323(6) -0.0804(5) 0.1470(3) 0.158(3) Uani 1 1 d U . . F5 F 1.0835(6) 0.0258(4) 0.2023(3) 0.130(2) Uani 1 1 d U . . F6 F 0.9402(5) 0.5903(4) 0.1083(3) 0.115(2) Uani 1 1 d U . . F7 F 0.8696(5) 0.6875(4) 0.0172(3) 0.125(2) Uani 1 1 d U . . F8 F 0.6877(5) 0.6689(4) -0.0214(3) 0.121(2) Uani 1 1 d U . . F9 F 0.5827(5) 0.5423(4) 0.0299(3) 0.119(2) Uani 1 1 d U . . F10 F 0.6563(5) 0.4428(4) 0.1217(3) 0.121(2) Uani 1 1 d U . . F16 F 0.4118(5) 0.6655(4) 0.0784(3) 0.126(2) Uani 1 1 d U . . F17 F 0.3190(6) 0.7492(4) -0.0116(3) 0.137(2) Uani 1 1 d U . . F18 F 0.1579(6) 0.6947(4) -0.0468(3) 0.136(3) Uani 1 1 d U . . F19 F 0.0932(5) 0.5533(4) 0.0104(3) 0.123(2) Uani 1 1 d U . . F20 F 0.1864(5) 0.4687(4) 0.0998(3) 0.120(2) Uani 1 1 d U . . F21 F 0.5439(6) 0.0977(4) 0.2040(3) 0.128(2) Uani 1 1 d U . . F22 F 0.6740(6) -0.0287(4) 0.1577(3) 0.152(3) Uani 1 1 d U . . F23 F 0.8874(7) -0.0208(5) 0.1136(3) 0.163(3) Uani 1 1 d U . . F24 F 0.9678(6) 0.1174(5) 0.1112(3) 0.146(3) Uani 1 1 d U . . F25 F 0.8351(5) 0.2434(4) 0.1562(2) 0.122(2) Uani 1 1 d U . . S1 S 1.0542(3) 0.0414(2) 0.41881(16) 0.1170(12) Uani 1 1 d U . . O1 O 0.9395(7) 0.0478(4) 0.4455(3) 0.119(3) Uani 1 1 d U . . O2 O 1.1189(6) -0.0431(5) 0.4091(3) 0.118(3) Uani 1 1 d U . . C67 C 1.1352(9) 0.0753(7) 0.4550(4) 0.110(4) Uani 1 1 d U . . H46 H 1.1537 0.0312 0.4873 0.132 Uiso 1 1 calc R . . H47 H 1.2081 0.0801 0.4332 0.132 Uiso 1 1 calc R . . C68 C 1.0773(9) 0.1615(7) 0.4722(4) 0.129(4) Uani 1 1 d U . . H48 H 1.0460 0.2034 0.4416 0.194 Uiso 1 1 calc R . . H49 H 1.1338 0.1817 0.4854 0.194 Uiso 1 1 calc R . . H50 H 1.0155 0.1540 0.5004 0.194 Uiso 1 1 calc R . . S2 S 1.2710(3) 0.0585(2) 0.31082(18) 0.1144(12) Uani 1 1 d U . . O3 O 1.3251(6) 0.1011(4) 0.2631(3) 0.115(3) Uani 1 1 d U . . O4 O 1.3095(6) 0.0602(4) 0.3611(3) 0.112(3) Uani 1 1 d U . . C69 C 1.2908(10) -0.0502(6) 0.3050(5) 0.124(4) Uani 1 1 d U . . H51 H 1.2514 -0.0811 0.3364 0.149 Uiso 1 1 calc R . . H52 H 1.2591 -0.0525 0.2726 0.149 Uiso 1 1 calc R . . C70 C 1.4200(9) -0.0908(7) 0.3014(5) 0.152(5) Uani 1 1 d U . . H53 H 1.4587 -0.0569 0.2719 0.227 Uiso 1 1 calc R . . H54 H 1.4344 -0.1488 0.2951 0.227 Uiso 1 1 calc R . . H55 H 1.4492 -0.0926 0.3348 0.227 Uiso 1 1 calc R . . S3 S 0.2614(3) 0.7178(2) 0.28800(17) 0.1219(12) Uani 1 1 d U . . O5 O 0.3529(6) 0.7230(4) 0.3160(3) 0.129(3) Uani 1 1 d U . . O6 O 0.2113(6) 0.7956(5) 0.2498(3) 0.125(3) Uani 1 1 d U . . C71 C 0.1574(10) 0.6820(8) 0.3372(5) 0.129(5) Uani 1 1 d U . . H56 H 0.1047 0.6618 0.3207 0.154 Uiso 1 1 calc R . . H57 H 0.1948 0.6345 0.3644 0.154 Uiso 1 1 calc R . . C72 C 0.0934(12) 0.7567(9) 0.3622(6) 0.188(6) Uani 1 1 d U . . H58 H 0.0564 0.7363 0.3972 0.283 Uiso 1 1 calc R . . H59 H 0.0354 0.7936 0.3394 0.283 Uiso 1 1 calc R . . H60 H 0.1467 0.7889 0.3662 0.283 Uiso 1 1 calc R . . S4 S 0.1303(3) 0.6685(2) 0.18926(18) 0.1178(12) Uani 1 1 d U . . O7 O 0.1094(6) 0.6119(5) 0.1588(3) 0.124(3) Uani 1 1 d U . . O8 O 0.0529(7) 0.6884(5) 0.2354(3) 0.124(3) Uani 1 1 d U . . C73 C 0.1386(10) 0.7660(7) 0.1448(4) 0.114(4) Uani 1 1 d U . . H61 H 0.1365 0.8099 0.1652 0.137 Uiso 1 1 calc R . . H62 H 0.2113 0.7578 0.1214 0.137 Uiso 1 1 calc R . . C74 C 0.0376(10) 0.7950(7) 0.1110(4) 0.134(4) Uani 1 1 d U . . H63 H 0.0380 0.7500 0.0922 0.201 Uiso 1 1 calc R . . H64 H 0.0442 0.8468 0.0850 0.201 Uiso 1 1 calc R . . H65 H -0.0339 0.8066 0.1342 0.201 Uiso 1 1 calc R . . C75A C 0.165(2) 0.4000(16) 0.2468(6) 0.117(6) Uani 0.69(2) 1 d PGU A 1 H21 H 0.1648 0.4192 0.2093 0.141 Uiso 0.69(2) 1 calc PR A 1 C76A C 0.1046(19) 0.4535(8) 0.2811(11) 0.126(7) Uani 0.69(2) 1 d PGU A 1 H22 H 0.0629 0.5094 0.2671 0.152 Uiso 0.69(2) 1 calc PR A 1 C77A C 0.1051(17) 0.4254(13) 0.3358(10) 0.131(7) Uani 0.69(2) 1 d PGU A 1 H23 H 0.0638 0.4620 0.3593 0.157 Uiso 0.69(2) 1 calc PR A 1 C78A C 0.166(2) 0.3437(15) 0.3562(5) 0.123(6) Uani 0.69(2) 1 d PGU A 1 H24 H 0.1666 0.3245 0.3937 0.147 Uiso 0.69(2) 1 calc PR A 1 C79A C 0.2268(18) 0.2901(8) 0.3219(9) 0.117(6) Uani 0.69(2) 1 d PGU A 1 H25 H 0.2685 0.2343 0.3359 0.141 Uiso 0.69(2) 1 calc PR A 1 C80A C 0.2262(17) 0.3183(14) 0.2672(8) 0.116(6) Uani 0.69(2) 1 d PGU A 1 H26 H 0.2676 0.2817 0.2437 0.139 Uiso 0.69(2) 1 calc PR A 1 C81 C 0.3652(14) 0.0983(11) 0.5315(8) 0.171(7) Uani 1 1 d U . . H27 H 0.3633 0.0475 0.5569 0.205 Uiso 1 1 calc R . . C82 C 0.3375(13) 0.1743(12) 0.5498(8) 0.180(6) Uani 1 1 d U . . H28 H 0.3166 0.1764 0.5865 0.216 Uiso 1 1 calc R . . C83 C 0.3422(14) 0.2462(12) 0.5117(8) 0.166(6) Uani 1 1 d U . . H29 H 0.3213 0.3001 0.5219 0.200 Uiso 1 1 calc R . . C84 C 0.3783(13) 0.2414(11) 0.4567(8) 0.161(6) Uani 1 1 d U . . H30 H 0.3844 0.2913 0.4312 0.193 Uiso 1 1 calc R . . C85 C 0.4038(12) 0.1644(11) 0.4414(7) 0.157(5) Uani 1 1 d U . . H31 H 0.4273 0.1610 0.4051 0.188 Uiso 1 1 calc R . . C86 C 0.3957(13) 0.0918(12) 0.4783(8) 0.159(6) Uani 1 1 d U . . H32 H 0.4105 0.0385 0.4678 0.191 Uiso 1 1 calc R . . C75B C 0.152(4) 0.444(2) 0.2518(18) 0.126(10) Uani 0.31(2) 1 d PGU A 2 H33 H 0.1312 0.4905 0.2233 0.151 Uiso 0.31(2) 1 calc PR A 2 C76B C 0.114(4) 0.453(2) 0.304(2) 0.133(10) Uani 0.31(2) 1 d PGU A 2 H34 H 0.0665 0.5053 0.3113 0.160 Uiso 0.31(2) 1 calc PR A 2 C77B C 0.144(5) 0.384(4) 0.3457(14) 0.124(9) Uani 0.31(2) 1 d PGU A 2 H35 H 0.1180 0.3905 0.3814 0.148 Uiso 0.31(2) 1 calc PR A 2 C78B C 0.213(5) 0.307(3) 0.3351(18) 0.127(10) Uani 0.31(2) 1 d PGU A 2 H36 H 0.2342 0.2609 0.3636 0.153 Uiso 0.31(2) 1 calc PR A 2 C79B C 0.252(4) 0.299(2) 0.283(2) 0.126(10) Uani 0.31(2) 1 d PGU A 2 H37 H 0.2989 0.2460 0.2756 0.151 Uiso 0.31(2) 1 calc PR A 2 C80B C 0.221(5) 0.367(3) 0.2412(14) 0.127(10) Uani 0.31(2) 1 d PGU A 2 H38 H 0.2474 0.3608 0.2055 0.152 Uiso 0.31(2) 1 calc PR A 2 C87 C 0.3022(15) 0.0382(10) 0.6864(7) 0.158(6) Uani 1 1 d U . . H9 H 0.3780 0.0219 0.6702 0.190 Uiso 1 1 calc R . . C88 C 0.2210(17) 0.0041(10) 0.6790(7) 0.175(6) Uani 1 1 d U . . H10 H 0.2379 -0.0363 0.6564 0.210 Uiso 1 1 calc R . . C89 C 0.1125(16) 0.0269(11) 0.7038(7) 0.172(6) Uani 1 1 d U . . H11 H 0.0580 -0.0021 0.7001 0.206 Uiso 1 1 calc R . . C90 C 0.0790(13) 0.0892(9) 0.7334(6) 0.140(5) Uani 1 1 d U . . H12 H 0.0021 0.1089 0.7473 0.168 Uiso 1 1 calc R . . C91 C 0.1652(15) 0.1202(9) 0.7412(6) 0.148(5) Uani 1 1 d U . . H13 H 0.1496 0.1602 0.7640 0.178 Uiso 1 1 calc R . . C92 C 0.2734(14) 0.0966(11) 0.7177(6) 0.149(5) Uani 1 1 d U . . H14 H 0.3300 0.1219 0.7235 0.179 Uiso 1 1 calc R . . C93 C 0.2031(15) -0.0452(11) 0.0066(7) 0.182(6) Uani 1 1 d U . . H39 H 0.1802 -0.0965 0.0098 0.219 Uiso 1 1 calc R . . C94 C 0.3118(17) -0.0415(12) -0.0158(7) 0.201(7) Uani 1 1 d U . . H40 H 0.3642 -0.0896 -0.0268 0.241 Uiso 1 1 calc R . . C95 C 0.3412(17) 0.0311(12) -0.0214(8) 0.225(8) Uani 1 1 d U . . H41 H 0.4145 0.0364 -0.0380 0.269 Uiso 1 1 calc R . . C96 C 0.2629(16) 0.1018(12) -0.0025(7) 0.192(6) Uani 1 1 d U . . H42 H 0.2869 0.1519 -0.0036 0.230 Uiso 1 1 calc R . . C97 C 0.1543(16) 0.0977(11) 0.0171(7) 0.180(6) Uani 1 1 d U . . H43 H 0.1004 0.1474 0.0252 0.216 Uiso 1 1 calc R . . C98 C 0.1228(15) 0.0256(12) 0.0251(7) 0.192(6) Uani 1 1 d U . . H44 H 0.0499 0.0207 0.0425 0.230 Uiso 1 1 calc R . . C99 C 0.4685(7) 0.2326(7) 0.8349(6) 0.192(7) Uani 1 1 d GU . . H75 H 0.5469 0.2203 0.8401 0.230 Uiso 1 1 calc R . . C100 C 0.4347(11) 0.2593(7) 0.7838(5) 0.202(7) Uani 1 1 d GU . . H76 H 0.4900 0.2653 0.7540 0.242 Uiso 1 1 calc R . . C101 C 0.3199(13) 0.2774(6) 0.7762(4) 0.200(7) Uani 1 1 d GU . . H77 H 0.2968 0.2957 0.7412 0.240 Uiso 1 1 calc R . . C102 C 0.2389(7) 0.2688(6) 0.8198(6) 0.179(6) Uani 1 1 d GU . . H78 H 0.1604 0.2811 0.8146 0.215 Uiso 1 1 calc R . . C103 C 0.2727(11) 0.2420(7) 0.8709(5) 0.200(7) Uani 1 1 d GU . . H79 H 0.2173 0.2361 0.9007 0.241 Uiso 1 1 calc R . . C104 C 0.3875(13) 0.2240(7) 0.8785(4) 0.201(6) Uani 1 1 d GU . . H80 H 0.4106 0.2057 0.9135 0.241 Uiso 1 1 calc R . . C105 C 0.1520(11) 0.3538(11) 0.6469(6) 0.251(10) Uani 1 1 d U . . H85 H 0.1918 0.3589 0.6756 0.377 Uiso 1 1 calc R . . H86 H 0.1951 0.3044 0.6316 0.377 Uiso 1 1 calc R . . H87 H 0.0755 0.3465 0.6613 0.377 Uiso 1 1 calc R . . C106 C 0.1419(11) 0.4346(10) 0.6036(7) 0.173(6) Uani 1 1 d U . . H69 H 0.2187 0.4434 0.5895 0.208 Uiso 1 1 calc R . . H70 H 0.0972 0.4847 0.6185 0.208 Uiso 1 1 calc R . . C107 C 0.0821(14) 0.4235(10) 0.5590(7) 0.197(6) Uani 1 1 d U . . H71 H 0.1357 0.3822 0.5391 0.237 Uiso 1 1 calc R . . H72 H 0.0161 0.3993 0.5751 0.237 Uiso 1 1 calc R . . C108 C 0.0426(15) 0.5019(12) 0.5224(6) 0.214(7) Uani 1 1 d U . . H73 H 0.1100 0.5208 0.5025 0.257 Uiso 1 1 calc R . . H74 H 0.0002 0.5456 0.5433 0.257 Uiso 1 1 calc R . . 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 0.121(11) 0.103(9) 0.106(11) 0.001(9) -0.024(11) -0.046(9) C2 0.120(12) 0.114(9) 0.108(12) -0.018(9) -0.019(9) -0.044(9) C3 0.082(10) 0.105(9) 0.127(12) -0.010(9) -0.015(8) -0.030(8) C4 0.114(10) 0.099(9) 0.107(11) 0.011(8) -0.038(10) -0.039(8) C5 0.091(9) 0.101(9) 0.107(11) 0.006(9) -0.038(8) -0.028(8) C6 0.111(10) 0.112(10) 0.092(10) 0.006(9) -0.048(9) -0.038(8) C7 0.100(9) 0.111(9) 0.117(11) -0.017(9) -0.015(9) -0.050(8) C8 0.106(11) 0.102(9) 0.155(13) -0.001(10) -0.028(10) -0.034(9) C9 0.101(10) 0.117(10) 0.118(11) -0.001(10) -0.028(9) -0.050(9) C10 0.095(10) 0.107(9) 0.113(11) -0.002(9) -0.034(9) -0.024(8) C11 0.100(10) 0.106(9) 0.098(11) -0.008(9) -0.014(10) -0.016(8) C12 0.100(10) 0.093(9) 0.134(14) -0.001(9) -0.030(10) -0.030(8) C13 0.124(12) 0.114(10) 0.116(12) -0.014(8) -0.039(10) -0.025(9) C14 0.116(11) 0.095(8) 0.114(11) -0.003(9) -0.046(11) -0.028(8) C15 0.119(11) 0.112(9) 0.128(12) -0.021(9) -0.029(11) -0.022(9) C16 0.112(11) 0.106(10) 0.140(12) -0.028(9) -0.015(10) -0.033(9) C17 0.092(10) 0.102(9) 0.127(11) -0.040(8) -0.006(9) -0.035(8) C18 0.062(8) 0.100(9) 0.162(12) 0.000(9) -0.056(8) -0.009(7) C19 0.092(10) 0.103(10) 0.140(12) -0.023(9) -0.015(9) -0.030(8) C20 0.108(9) 0.093(9) 0.130(11) -0.004(9) -0.032(9) -0.009(8) C21 0.086(8) 0.106(10) 0.119(11) -0.013(9) -0.029(8) -0.041(8) C22 0.081(8) 0.113(10) 0.133(11) 0.008(9) -0.056(8) -0.045(8) C23 0.081(8) 0.117(10) 0.136(12) 0.000(10) -0.030(8) -0.045(8) C24 0.101(9) 0.111(9) 0.111(11) -0.019(9) -0.036(8) -0.041(8) C25 0.097(10) 0.132(10) 0.112(11) -0.007(10) -0.044(9) -0.044(8) C26 0.110(10) 0.066(7) 0.134(13) -0.001(8) -0.045(10) -0.020(7) C27 0.103(10) 0.101(9) 0.134(13) -0.004(9) -0.049(9) -0.012(8) C28 0.110(10) 0.102(9) 0.119(11) -0.013(8) -0.046(9) -0.014(8) C29 0.110(10) 0.105(9) 0.122(11) -0.013(9) -0.039(11) -0.027(8) C30 0.097(10) 0.122(9) 0.110(12) -0.007(9) -0.004(10) -0.019(9) C31 0.094(9) 0.090(9) 0.124(10) 0.003(8) -0.027(8) -0.019(9) C32 0.109(11) 0.109(10) 0.134(12) -0.014(9) -0.041(9) -0.053(9) C33 0.105(11) 0.105(11) 0.122(11) -0.014(9) -0.024(9) -0.025(10) C34 0.136(13) 0.095(11) 0.146(13) -0.002(10) -0.023(10) -0.031(11) C35 0.134(14) 0.092(11) 0.175(14) -0.003(10) -0.030(11) -0.043(10) C36 0.082(10) 0.089(10) 0.159(12) -0.002(9) -0.026(9) -0.029(9) C37 0.086(9) 0.103(9) 0.135(11) 0.001(8) -0.029(8) -0.041(8) C38 0.092(10) 0.094(10) 0.167(13) -0.023(9) -0.029(10) -0.032(8) C39 0.092(10) 0.094(10) 0.175(13) -0.024(9) 0.006(10) -0.043(9) C40 0.101(10) 0.083(9) 0.145(12) -0.013(8) -0.028(9) -0.019(8) C41 0.097(10) 0.096(9) 0.140(12) -0.010(9) -0.040(9) -0.036(8) C42 0.098(10) 0.089(9) 0.150(12) -0.008(8) -0.024(9) -0.040(8) C43 0.093(9) 0.121(10) 0.131(13) -0.018(10) -0.050(10) -0.015(8) C44 0.116(11) 0.118(11) 0.149(15) -0.013(11) -0.050(12) -0.014(9) C45 0.115(12) 0.107(11) 0.137(14) -0.048(11) -0.048(12) 0.019(9) C46 0.122(12) 0.142(13) 0.119(14) -0.025(12) -0.058(11) 0.008(10) C47 0.098(11) 0.113(11) 0.157(15) -0.020(12) -0.033(11) -0.015(9) C48 0.126(12) 0.105(10) 0.147(15) 0.004(12) -0.040(12) -0.024(9) F11 0.117(6) 0.125(6) 0.208(8) -0.057(6) -0.059(5) -0.008(5) F12 0.172(7) 0.168(7) 0.219(9) -0.097(7) -0.115(6) 0.038(6) F13 0.158(7) 0.151(6) 0.153(7) -0.007(6) -0.046(7) 0.014(5) F14 0.141(7) 0.128(6) 0.194(9) 0.005(5) -0.003(6) -0.022(5) F15 0.135(6) 0.121(6) 0.171(8) -0.018(5) -0.029(5) -0.043(5) C49 0.079(8) 0.080(8) 0.138(11) -0.008(8) -0.031(8) -0.019(7) C50 0.077(9) 0.090(10) 0.159(13) -0.009(9) -0.024(9) -0.007(8) C51 0.105(11) 0.093(10) 0.152(13) -0.010(9) -0.017(10) -0.023(9) C52 0.101(10) 0.098(10) 0.132(12) 0.003(9) -0.035(9) -0.025(9) C53 0.090(9) 0.076(9) 0.157(13) -0.001(9) -0.048(9) -0.013(8) C54 0.087(9) 0.078(9) 0.141(12) -0.008(8) -0.032(9) -0.003(8) C55 0.078(9) 0.124(10) 0.119(10) -0.001(8) -0.015(8) -0.033(9) C56 0.088(11) 0.111(11) 0.147(11) 0.014(9) -0.032(9) -0.037(9) C57 0.108(12) 0.100(10) 0.169(13) -0.001(9) -0.053(10) -0.030(10) C58 0.126(13) 0.091(10) 0.178(13) -0.027(10) -0.029(11) -0.016(11) C59 0.117(12) 0.093(11) 0.158(12) -0.008(10) -0.058(10) -0.011(11) C60 0.084(10) 0.092(9) 0.151(11) 0.010(8) -0.034(9) -0.042(9) C61 0.103(10) 0.112(10) 0.134(13) -0.017(10) -0.035(10) -0.037(8) C62 0.103(9) 0.106(10) 0.109(12) 0.019(10) -0.032(10) -0.033(8) C63 0.122(11) 0.101(10) 0.147(15) -0.005(12) -0.057(12) -0.028(9) C64 0.114(11) 0.122(12) 0.125(13) -0.022(11) -0.031(11) 0.006(9) C65 0.110(11) 0.089(10) 0.143(14) -0.008(12) -0.040(11) -0.006(8) C66 0.122(12) 0.102(10) 0.132(14) -0.021(11) -0.054(12) -0.006(9) F26 0.112(5) 0.104(5) 0.164(7) -0.012(5) -0.049(5) -0.023(4) F27 0.144(6) 0.126(6) 0.191(8) -0.037(5) -0.053(5) -0.032(5) F28 0.130(6) 0.136(6) 0.161(7) -0.019(6) -0.050(6) 0.005(5) F29 0.121(6) 0.123(6) 0.150(7) 0.007(5) -0.028(5) -0.018(5) F30 0.118(5) 0.118(5) 0.126(6) 0.003(4) -0.038(4) -0.025(4) N1 0.092(7) 0.116(8) 0.120(9) -0.009(7) -0.034(8) -0.032(7) N2 0.119(9) 0.132(9) 0.108(9) -0.009(8) -0.035(7) -0.044(8) N3 0.125(10) 0.097(7) 0.117(9) -0.004(8) -0.031(9) -0.012(7) N4 0.094(8) 0.096(7) 0.151(10) -0.021(7) -0.032(7) -0.034(7) N5 0.107(8) 0.106(8) 0.101(8) 0.005(7) -0.048(6) -0.026(7) N6 0.108(8) 0.099(7) 0.125(10) -0.008(7) -0.026(8) -0.020(6) F1 0.100(5) 0.121(5) 0.158(6) -0.010(5) -0.041(4) -0.034(4) F2 0.109(5) 0.137(6) 0.166(7) -0.024(5) -0.015(5) -0.034(5) F3 0.150(7) 0.136(7) 0.201(9) -0.058(6) -0.013(6) -0.016(6) F4 0.169(7) 0.129(6) 0.187(8) -0.030(5) -0.030(5) -0.048(6) F5 0.118(5) 0.122(5) 0.153(6) -0.007(4) -0.038(5) -0.040(5) F6 0.094(5) 0.099(4) 0.154(6) -0.002(4) -0.035(4) -0.032(4) F7 0.110(5) 0.113(5) 0.158(6) -0.003(4) -0.034(4) -0.043(4) F8 0.113(5) 0.100(5) 0.149(6) 0.008(4) -0.047(5) -0.030(4) F9 0.094(5) 0.118(5) 0.155(6) -0.017(4) -0.048(4) -0.030(4) F10 0.109(5) 0.107(5) 0.152(6) -0.005(4) -0.037(4) -0.039(4) F16 0.113(5) 0.108(5) 0.164(7) -0.017(4) -0.030(5) -0.038(4) F17 0.134(6) 0.120(5) 0.152(7) -0.008(5) -0.019(5) -0.036(5) F18 0.133(6) 0.119(5) 0.149(7) 0.001(5) -0.053(5) -0.017(5) F19 0.097(5) 0.119(5) 0.153(6) -0.023(4) -0.037(4) -0.017(4) F20 0.105(5) 0.109(5) 0.149(6) -0.009(5) -0.036(4) -0.033(4) F21 0.119(6) 0.111(5) 0.157(7) -0.002(4) -0.040(5) -0.036(5) F22 0.144(6) 0.108(5) 0.216(8) -0.033(5) -0.051(5) -0.033(5) F23 0.163(7) 0.124(6) 0.198(8) -0.043(5) -0.040(6) -0.009(6) F24 0.111(6) 0.165(7) 0.168(7) -0.034(5) -0.027(5) -0.033(6) F25 0.101(5) 0.122(5) 0.146(6) -0.005(4) -0.027(4) -0.040(4) S1 0.106(3) 0.114(3) 0.132(4) 0.003(3) -0.035(3) -0.038(3) O1 0.112(6) 0.119(6) 0.125(7) 0.017(5) -0.028(6) -0.051(5) O2 0.107(6) 0.095(6) 0.152(7) -0.016(5) -0.037(5) -0.019(5) C67 0.092(9) 0.088(8) 0.148(11) 0.004(8) -0.059(8) -0.013(7) C68 0.123(10) 0.127(11) 0.153(12) -0.003(9) -0.068(9) -0.046(9) S2 0.094(3) 0.098(3) 0.148(4) 0.000(3) -0.033(3) -0.026(2) O3 0.104(6) 0.085(5) 0.154(7) -0.009(5) -0.021(6) -0.029(5) O4 0.102(6) 0.106(6) 0.124(7) 0.011(5) -0.048(5) -0.024(5) C69 0.112(10) 0.074(8) 0.185(12) -0.018(8) -0.039(9) -0.013(8) C70 0.100(10) 0.127(11) 0.228(15) -0.013(10) -0.041(10) -0.032(9) S3 0.105(3) 0.109(3) 0.157(4) -0.022(3) -0.036(3) -0.027(2) O5 0.103(6) 0.098(6) 0.194(9) -0.028(5) -0.044(6) -0.022(5) O6 0.133(7) 0.112(6) 0.135(7) -0.005(5) -0.060(6) -0.025(5) C71 0.100(10) 0.117(10) 0.189(14) -0.078(10) -0.010(10) -0.023(9) C72 0.185(15) 0.154(13) 0.235(17) 0.012(13) -0.114(13) -0.046(12) S4 0.112(3) 0.099(3) 0.143(4) -0.010(3) -0.046(3) -0.019(2) O7 0.095(6) 0.113(6) 0.155(8) -0.013(6) -0.039(5) -0.008(5) O8 0.103(6) 0.123(6) 0.138(8) -0.028(6) -0.024(6) -0.009(5) C73 0.128(10) 0.107(9) 0.115(10) 0.003(8) -0.068(8) -0.029(8) C74 0.138(11) 0.123(10) 0.137(12) -0.008(8) -0.033(10) -0.031(9) C75A 0.082(13) 0.114(14) 0.171(13) 0.008(11) -0.050(10) -0.057(11) C76A 0.094(12) 0.111(11) 0.175(16) -0.003(12) -0.022(13) -0.043(10) C77A 0.105(12) 0.105(13) 0.182(15) -0.024(13) -0.007(12) -0.032(11) C78A 0.113(13) 0.083(13) 0.173(13) -0.013(11) -0.030(11) -0.026(11) C79A 0.105(11) 0.090(10) 0.161(15) -0.010(11) -0.035(12) -0.029(9) C80A 0.092(12) 0.099(12) 0.167(14) -0.001(12) -0.043(12) -0.044(10) C81 0.167(13) 0.105(10) 0.241(17) -0.009(14) -0.094(14) -0.013(11) C82 0.161(12) 0.134(12) 0.254(17) -0.004(13) -0.092(12) -0.041(12) C83 0.157(12) 0.138(12) 0.217(17) -0.013(14) -0.073(14) -0.047(11) C84 0.140(12) 0.126(11) 0.225(16) -0.006(14) -0.060(13) -0.045(11) C85 0.126(10) 0.131(12) 0.214(15) -0.007(12) -0.059(10) -0.030(11) C86 0.121(10) 0.131(12) 0.248(19) -0.016(14) -0.076(13) -0.053(10) C75B 0.105(17) 0.102(16) 0.168(17) 0.005(16) -0.025(16) -0.040(16) C76B 0.104(15) 0.108(15) 0.177(19) -0.007(16) -0.015(16) -0.026(15) C77B 0.105(16) 0.094(18) 0.169(16) -0.014(15) -0.030(15) -0.021(16) C78B 0.108(16) 0.098(16) 0.172(16) 0.000(16) -0.041(15) -0.024(15) C79B 0.107(16) 0.096(14) 0.171(18) 0.002(15) -0.033(16) -0.030(14) C80B 0.104(17) 0.098(17) 0.175(17) 0.007(15) -0.041(15) -0.029(16) C87 0.143(13) 0.126(12) 0.216(15) -0.045(10) -0.006(12) -0.047(10) C88 0.163(15) 0.154(12) 0.214(14) -0.061(10) 0.025(13) -0.055(12) C89 0.158(14) 0.166(13) 0.225(16) -0.056(11) 0.002(12) -0.092(12) C90 0.123(12) 0.107(10) 0.196(13) -0.040(9) -0.023(10) -0.025(10) C91 0.124(13) 0.133(11) 0.187(13) -0.034(9) -0.046(12) -0.011(11) C92 0.110(12) 0.166(13) 0.180(15) -0.032(10) -0.050(11) -0.028(12) C93 0.145(14) 0.141(12) 0.237(16) -0.012(11) -0.018(13) -0.017(13) C94 0.167(14) 0.161(14) 0.240(15) 0.025(14) 0.000(13) -0.045(14) C95 0.177(15) 0.143(14) 0.300(17) 0.013(15) 0.014(13) -0.018(14) C96 0.141(14) 0.155(13) 0.263(16) -0.006(12) -0.025(14) -0.034(13) C97 0.146(13) 0.139(12) 0.232(14) 0.021(12) -0.029(12) -0.038(13) C98 0.158(14) 0.140(13) 0.254(15) -0.029(13) -0.014(12) -0.010(13) C99 0.158(13) 0.199(13) 0.214(17) 0.003(14) -0.038(12) -0.063(11) C100 0.165(13) 0.169(12) 0.285(17) -0.017(13) -0.039(13) -0.079(12) C101 0.185(15) 0.183(12) 0.246(16) -0.021(12) -0.032(14) -0.082(14) C102 0.157(13) 0.166(12) 0.241(18) -0.067(14) -0.016(13) -0.066(11) C103 0.178(14) 0.195(13) 0.245(16) -0.081(13) -0.056(13) -0.020(13) C104 0.116(12) 0.222(13) 0.269(16) -0.070(13) -0.028(13) -0.028(13) C105 0.089(10) 0.33(2) 0.233(18) 0.134(16) -0.018(11) -0.039(13) C106 0.105(11) 0.222(15) 0.233(18) -0.094(13) -0.027(11) -0.062(11) C107 0.175(12) 0.196(13) 0.214(16) 0.023(12) -0.041(11) -0.076(12) C108 0.213(16) 0.228(15) 0.223(18) -0.043(13) -0.003(13) -0.099(14) _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 1.392(13) . ? C1 C30 1.408(16) . ? C1 C2 1.469(16) . ? C2 C3 1.366(13) . ? C2 S1 1.812(13) . ? C3 C4 1.413(15) . ? C3 S2 1.816(12) . ? C4 N1 1.354(14) . ? C4 C5 1.447(15) . ? C5 C6 1.361(15) . ? C5 C31 1.520(15) . ? C6 N2 1.404(14) . ? C6 C7 1.424(14) . ? C7 C8 1.370(13) . ? C7 H1 0.9500 . ? C8 C9 1.440(15) . ? C8 H2 0.9500 . ? C9 N2 1.368(14) . ? C9 C10 1.421(16) . ? C10 C11 1.364(15) . ? C10 C37 1.510(16) . ? C11 N3 1.346(14) . ? C11 C12 1.399(16) . ? C12 C13 1.339(13) . ? C12 H3 0.9500 . ? C13 C14 1.466(16) . ? C13 H4 0.9500 . ? C14 N3 1.337(14) . ? C14 C15 1.408(16) . ? C15 C43 1.467(17) . ? C15 C16 1.512(18) . ? C16 N4 1.327(14) . ? C16 C17 1.420(15) . ? C17 C18 1.396(14) . ? C17 S3 1.772(12) . ? C18 C19 1.368(15) . ? C18 S4 1.786(11) . ? C19 N4 1.341(14) . ? C19 C20 1.482(16) . ? C20 C21 1.348(15) . ? C20 C49 1.473(16) . ? C21 N5 1.393(13) . ? C21 C22 1.470(14) . ? C22 C23 1.359(13) . ? C22 H5 0.9500 . ? C23 C24 1.438(15) . ? C23 H6 0.9500 . ? C24 N5 1.392(13) . ? C24 C25 1.395(16) . ? C25 C26 1.378(16) . ? C25 C55 1.498(16) . ? C26 N6 1.374(14) . ? C26 C27 1.441(15) . ? C27 C28 1.346(13) . ? C27 H7 0.9500 . ? C28 C29 1.440(16) . ? C28 H8 0.9500 . ? C29 C30 1.366(17) . ? C29 N6 1.381(14) . ? C30 C61 1.431(17) . ? C31 C36 1.372(15) . ? C31 C32 1.389(15) . ? C32 F1 1.373(12) . ? C32 C33 1.402(16) . ? C33 C34 1.311(17) . ? C33 F2 1.382(14) . ? C34 F3 1.303(15) . ? C34 C35 1.368(18) . ? C35 F4 1.319(14) . ? C35 C36 1.338(17) . ? C36 F5 1.382(13) . ? C37 C38 1.324(15) . ? C37 C42 1.376(15) . ? C38 F6 1.342(13) . ? C38 C39 1.409(17) . ? C39 F7 1.355(13) . ? C39 C40 1.370(16) . ? C40 C41 1.349(15) . ? C40 F8 1.372(13) . ? C41 F9 1.339(12) . ? C41 C42 1.402(15) . ? C42 F10 1.343(12) . ? C43 C44 1.353(19) . ? C43 C48 1.384(19) . ? C44 C45 1.362(18) . ? C44 F11 1.382(16) . ? C45 F12 1.308(16) . ? C45 C46 1.41(2) . ? C46 C47 1.31(2) . ? C46 F13 1.362(16) . ? C47 F14 1.340(17) . ? C47 C48 1.383(19) . ? C48 F15 1.322(17) . ? C49 C50 1.391(15) . ? C49 C54 1.411(15) . ? C50 F16 1.347(13) . ? C50 C51 1.406(17) . ? C51 C52 1.324(16) . ? C51 F17 1.384(14) . ? C52 F18 1.333(14) . ? C52 C53 1.339(15) . ? C53 C54 1.352(15) . ? C53 F19 1.400(13) . ? C54 F20 1.347(12) . ? C55 C60 1.318(14) . ? C55 C56 1.362(16) . ? C56 F21 1.334(13) . ? C56 C57 1.421(17) . ? C57 F22 1.332(14) . ? C57 C58 1.341(17) . ? C58 C59 1.275(17) . ? C58 F23 1.369(15) . ? C59 F24 1.328(15) . ? C59 C60 1.435(17) . ? C60 F25 1.367(12) . ? C61 C66 1.357(18) . ? C61 C62 1.396(18) . ? C62 C63 1.330(17) . ? C62 F26 1.380(13) . ? C63 F27 1.336(16) . ? C63 C64 1.352(19) . ? C64 C65 1.36(2) . ? C64 F28 1.409(15) . ? C65 F29 1.339(16) . ? C65 C66 1.358(18) . ? C66 F30 1.388(15) . ? N2 H83 0.8800 . ? N3 H81 0.8800 . ? N5 H84 0.8800 . ? N6 H82 0.8800 . ? S1 O1 1.452(7) . ? S1 O2 1.471(7) . ? S1 C67 1.736(10) . ? C67 C68 1.550(12) . ? C67 H46 0.9900 . ? C67 H47 0.9900 . ? C68 H48 0.9800 . ? C68 H49 0.9800 . ? C68 H50 0.9800 . ? S2 O3 1.438(7) . ? S2 O4 1.464(7) . ? S2 C69 1.797(10) . ? C69 C70 1.538(12) . ? C69 H51 0.9900 . ? C69 H52 0.9900 . ? C70 H53 0.9800 . ? C70 H54 0.9800 . ? C70 H55 0.9800 . ? S3 O5 1.458(8) . ? S3 O6 1.487(7) . ? S3 C71 1.776(11) . ? C71 C72 1.503(14) . ? C71 H56 0.9900 . ? C71 H57 0.9900 . ? C72 H58 0.9800 . ? C72 H59 0.9800 . ? C72 H60 0.9800 . ? S4 O8 1.447(7) . ? S4 O7 1.453(8) . ? S4 C73 1.781(10) . ? C73 C74 1.532(12) . ? C73 H61 0.9900 . ? C73 H62 0.9900 . ? C74 H63 0.9800 . ? C74 H64 0.9800 . ? C74 H65 0.9800 . ? C75A C76A 1.3900 . ? C75A C80A 1.3900 . ? C75A H21 0.9500 . ? C76A C77A 1.3900 . ? C76A H22 0.9500 . ? C77A C78A 1.3900 . ? C77A H23 0.9500 . ? C78A C79A 1.3900 . ? C78A H24 0.9500 . ? C79A C80A 1.3900 . ? C79A H25 0.9500 . ? C80A H26 0.9500 . ? C81 C82 1.389(18) . ? C81 C86 1.392(18) . ? C81 H27 0.9500 . ? C82 C83 1.376(18) . ? C82 H28 0.9500 . ? C83 C84 1.439(18) . ? C83 H29 0.9500 . ? C84 C85 1.369(17) . ? C84 H30 0.9500 . ? C85 C86 1.376(18) . ? C85 H31 0.9500 . ? C86 H32 0.9500 . ? C75B C76B 1.3900 . ? C75B C80B 1.3900 . ? C75B H33 0.9500 . ? C76B C77B 1.3900 . ? C76B H34 0.9500 . ? C77B C78B 1.3900 . ? C77B H35 0.9500 . ? C78B C79B 1.3900 . ? C78B H36 0.9500 . ? C79B C80B 1.3900 . ? C79B H37 0.9500 . ? C80B H38 0.9500 . ? C87 C88 1.327(18) . ? C87 C92 1.346(17) . ? C87 H9 0.9500 . ? C88 C89 1.374(17) . ? C88 H10 0.9500 . ? C89 C90 1.367(17) . ? C89 H11 0.9500 . ? C90 C91 1.352(16) . ? C90 H12 0.9500 . ? C91 C92 1.361(16) . ? C91 H13 0.9500 . ? C92 H14 0.9500 . ? C93 C94 1.378(18) . ? C93 C98 1.437(18) . ? C93 H39 0.9500 . ? C94 C95 1.32(2) . ? C94 H40 0.9500 . ? C95 C96 1.43(2) . ? C95 H41 0.9500 . ? C96 C97 1.360(18) . ? C96 H42 0.9500 . ? C97 C98 1.320(18) . ? C97 H43 0.9500 . ? C98 H44 0.9500 . ? C99 C100 1.3900 . ? C99 C104 1.3900 . ? C99 H75 0.9500 . ? C100 C101 1.3900 . ? C100 H76 0.9500 . ? C101 C102 1.3900 . ? C101 H77 0.9500 . ? C102 C103 1.3900 . ? C102 H78 0.9500 . ? C103 C104 1.3900 . ? C103 H79 0.9500 . ? C104 H80 0.9500 . ? C105 C106 1.532(17) . ? C105 H85 0.9800 . ? C105 H86 0.9800 . ? C105 H87 0.9800 . ? C106 C107 1.531(18) . ? C106 H69 0.9900 . ? C106 H70 0.9900 . ? C107 C108 1.440(19) . ? C107 H71 0.9900 . ? C107 H72 0.9900 . ? C108 C108 1.70(3) 2_566 ? C108 H73 0.9900 . ? C108 H74 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 N1 C1 C30 119.0(16) . . ? N1 C1 C2 101.9(13) . . ? C30 C1 C2 139.1(16) . . ? C3 C2 C1 110.2(13) . . ? C3 C2 S1 124.9(13) . . ? C1 C2 S1 123.8(12) . . ? C2 C3 C4 107.2(13) . . ? C2 C3 S2 128.0(13) . . ? C4 C3 S2 124.2(13) . . ? N1 C4 C3 107.4(14) . . ? N1 C4 C5 118.6(15) . . ? C3 C4 C5 133.5(15) . . ? C6 C5 C4 122.9(15) . . ? C6 C5 C31 114.7(14) . . ? C4 C5 C31 121.1(13) . . ? C5 C6 N2 121.6(16) . . ? C5 C6 C7 132.3(17) . . ? N2 C6 C7 106.1(13) . . ? C8 C7 C6 111.1(13) . . ? C8 C7 H1 124.5 . . ? C6 C7 H1 124.5 . . ? C7 C8 C9 104.4(15) . . ? C7 C8 H2 127.8 . . ? C9 C8 H2 127.8 . . ? N2 C9 C10 122.3(16) . . ? N2 C9 C8 110.5(16) . . ? C10 C9 C8 126.8(17) . . ? C11 C10 C9 126.4(16) . . ? C11 C10 C37 119.6(14) . . ? C9 C10 C37 113.8(15) . . ? N3 C11 C10 124.2(17) . . ? N3 C11 C12 103.5(15) . . ? C10 C11 C12 132.3(17) . . ? C13 C12 C11 113.1(15) . . ? C13 C12 H3 123.4 . . ? C11 C12 H3 123.4 . . ? C12 C13 C14 103.8(15) . . ? C12 C13 H4 128.1 . . ? C14 C13 H4 128.1 . . ? N3 C14 C15 129.1(17) . . ? N3 C14 C13 106.1(15) . . ? C15 C14 C13 124.7(17) . . ? C14 C15 C43 122.1(16) . . ? C14 C15 C16 115.7(16) . . ? C43 C15 C16 121.7(15) . . ? N4 C16 C17 110.8(15) . . ? N4 C16 C15 117.4(16) . . ? C17 C16 C15 131.8(16) . . ? C18 C17 C16 104.2(12) . . ? C18 C17 S3 127.9(13) . . ? C16 C17 S3 127.4(12) . . ? C19 C18 C17 106.8(12) . . ? C19 C18 S4 126.1(14) . . ? C17 C18 S4 126.5(14) . . ? N4 C19 C18 111.4(14) . . ? N4 C19 C20 114.0(15) . . ? C18 C19 C20 134.6(16) . . ? C21 C20 C49 118.3(15) . . ? C21 C20 C19 121.1(15) . . ? C49 C20 C19 120.7(13) . . ? C20 C21 N5 124.7(15) . . ? C20 C21 C22 129.1(16) . . ? N5 C21 C22 106.1(12) . . ? C23 C22 C21 107.4(13) . . ? C23 C22 H5 126.3 . . ? C21 C22 H5 126.3 . . ? C22 C23 C24 109.9(14) . . ? C22 C23 H6 125.1 . . ? C24 C23 H6 125.1 . . ? N5 C24 C25 126.4(15) . . ? N5 C24 C23 106.1(13) . . ? C25 C24 C23 126.8(16) . . ? C26 C25 C24 121.3(16) . . ? C26 C25 C55 121.1(14) . . ? C24 C25 C55 117.4(14) . . ? N6 C26 C25 123.6(16) . . ? N6 C26 C27 101.7(14) . . ? C25 C26 C27 134.3(16) . . ? C28 C27 C26 113.0(14) . . ? C28 C27 H7 123.5 . . ? C26 C27 H7 123.5 . . ? C27 C28 C29 105.9(14) . . ? C27 C28 H8 127.0 . . ? C29 C28 H8 127.0 . . ? C30 C29 N6 125.7(17) . . ? C30 C29 C28 128.5(17) . . ? N6 C29 C28 105.7(14) . . ? C29 C30 C1 120.7(17) . . ? C29 C30 C61 116.4(15) . . ? C1 C30 C61 122.6(16) . . ? C36 C31 C32 111.5(14) . . ? C36 C31 C5 127.1(14) . . ? C32 C31 C5 121.4(14) . . ? F1 C32 C31 119.5(15) . . ? F1 C32 C33 118.7(15) . . ? C31 C32 C33 121.7(14) . . ? C34 C33 F2 121.8(17) . . ? C34 C33 C32 122.3(17) . . ? F2 C33 C32 115.8(15) . . ? F3 C34 C33 121.6(19) . . ? F3 C34 C35 120.2(18) . . ? C33 C34 C35 118.1(18) . . ? F4 C35 C36 119.7(17) . . ? F4 C35 C34 121.2(19) . . ? C36 C35 C34 118.8(17) . . ? C35 C36 C31 127.5(16) . . ? C35 C36 F5 118.9(15) . . ? C31 C36 F5 113.6(15) . . ? C38 C37 C42 116.7(15) . . ? C38 C37 C10 122.5(14) . . ? C42 C37 C10 120.8(13) . . ? C37 C38 F6 122.6(16) . . ? C37 C38 C39 123.1(15) . . ? F6 C38 C39 114.2(14) . . ? F7 C39 C40 121.0(17) . . ? F7 C39 C38 121.2(15) . . ? C40 C39 C38 117.8(14) . . ? C41 C40 C39 121.7(16) . . ? C41 C40 F8 121.2(15) . . ? C39 C40 F8 117.1(15) . . ? F9 C41 C40 120.6(15) . . ? F9 C41 C42 122.1(13) . . ? C40 C41 C42 117.3(14) . . ? F10 C42 C37 121.0(15) . . ? F10 C42 C41 115.8(13) . . ? C37 C42 C41 123.2(13) . . ? C44 C43 C48 114.8(19) . . ? C44 C43 C15 126.6(19) . . ? C48 C43 C15 118.5(18) . . ? C43 C44 C45 127(2) . . ? C43 C44 F11 117(2) . . ? C45 C44 F11 117(2) . . ? F12 C45 C44 124(2) . . ? F12 C45 C46 122(2) . . ? C44 C45 C46 113.7(18) . . ? C47 C46 F13 122(3) . . ? C47 C46 C45 124(2) . . ? F13 C46 C45 114(2) . . ? C46 C47 F14 120(2) . . ? C46 C47 C48 118(2) . . ? F14 C47 C48 122(2) . . ? F15 C48 C47 116(2) . . ? F15 C48 C43 121(2) . . ? C47 C48 C43 123(2) . . ? C50 C49 C54 113.3(15) . . ? C50 C49 C20 122.3(14) . . ? C54 C49 C20 124.2(13) . . ? F16 C50 C49 118.2(15) . . ? F16 C50 C51 120.4(15) . . ? C49 C50 C51 121.3(15) . . ? C52 C51 F17 121.8(17) . . ? C52 C51 C50 123.2(16) . . ? F17 C51 C50 115.0(15) . . ? C51 C52 F18 120.5(16) . . ? C51 C52 C53 115.7(17) . . ? F18 C52 C53 123.5(16) . . ? C52 C53 C54 124.5(15) . . ? C52 C53 F19 117.3(15) . . ? C54 C53 F19 118.1(13) . . ? F20 C54 C53 119.2(14) . . ? F20 C54 C49 118.8(14) . . ? C53 C54 C49 121.7(14) . . ? C60 C55 C56 119.2(16) . . ? C60 C55 C25 120.8(15) . . ? C56 C55 C25 119.9(14) . . ? F21 C56 C55 121.9(16) . . ? F21 C56 C57 118.6(15) . . ? C55 C56 C57 119.3(15) . . ? F22 C57 C58 126.8(18) . . ? F22 C57 C56 117.3(16) . . ? C58 C57 C56 115.9(16) . . ? C59 C58 C57 128.5(19) . . ? C59 C58 F23 117.3(19) . . ? C57 C58 F23 114.2(17) . . ? C58 C59 F24 127.7(19) . . ? C58 C59 C60 113.8(18) . . ? F24 C59 C60 118.4(15) . . ? C55 C60 F25 121.1(16) . . ? C55 C60 C59 123.2(15) . . ? F25 C60 C59 115.6(14) . . ? C66 C61 C62 110.3(17) . . ? C66 C61 C30 122.0(17) . . ? C62 C61 C30 127.7(18) . . ? C63 C62 F26 118.5(18) . . ? C63 C62 C61 127.3(18) . . ? F26 C62 C61 114.2(17) . . ? C62 C63 F27 122.2(19) . . ? C62 C63 C64 115.3(19) . . ? F27 C63 C64 123(2) . . ? C63 C64 C65 125(2) . . ? C63 C64 F28 118(2) . . ? C65 C64 F28 117(2) . . ? F29 C65 C66 125(2) . . ? F29 C65 C64 121(2) . . ? C66 C65 C64 114(2) . . ? C61 C66 C65 128.2(19) . . ? C61 C66 F30 118.3(18) . . ? C65 C66 F30 114(2) . . ? C4 N1 C1 113.2(14) . . ? C9 N2 C6 107.8(14) . . ? C9 N2 H83 126.1 . . ? C6 N2 H83 126.1 . . ? C14 N3 C11 113.4(16) . . ? C14 N3 H81 123.3 . . ? C11 N3 H81 123.3 . . ? C16 N4 C19 106.7(14) . . ? C24 N5 C21 110.5(12) . . ? C24 N5 H84 124.8 . . ? C21 N5 H84 124.8 . . ? C26 N6 C29 113.6(14) . . ? C26 N6 H82 123.2 . . ? C29 N6 H82 123.2 . . ? O1 S1 O2 116.8(5) . . ? O1 S1 C67 109.9(5) . . ? O2 S1 C67 107.2(5) . . ? O1 S1 C2 105.9(6) . . ? O2 S1 C2 106.7(6) . . ? C67 S1 C2 110.2(5) . . ? C68 C67 S1 114.8(7) . . ? C68 C67 H46 108.6 . . ? S1 C67 H46 108.6 . . ? C68 C67 H47 108.6 . . ? S1 C67 H47 108.6 . . ? H46 C67 H47 107.5 . . ? C67 C68 H48 109.5 . . ? C67 C68 H49 109.5 . . ? H48 C68 H49 109.5 . . ? C67 C68 H50 109.5 . . ? H48 C68 H50 109.5 . . ? H49 C68 H50 109.5 . . ? O3 S2 O4 116.4(5) . . ? O3 S2 C69 107.8(5) . . ? O4 S2 C69 109.3(5) . . ? O3 S2 C3 106.6(6) . . ? O4 S2 C3 109.5(6) . . ? C69 S2 C3 106.7(6) . . ? C70 C69 S2 107.3(8) . . ? C70 C69 H51 110.3 . . ? S2 C69 H51 110.3 . . ? C70 C69 H52 110.3 . . ? S2 C69 H52 110.3 . . ? H51 C69 H52 108.5 . . ? C69 C70 H53 109.5 . . ? C69 C70 H54 109.5 . . ? H53 C70 H54 109.5 . . ? C69 C70 H55 109.5 . . ? H53 C70 H55 109.5 . . ? H54 C70 H55 109.5 . . ? O5 S3 O6 116.4(5) . . ? O5 S3 C17 108.1(6) . . ? O6 S3 C17 106.5(6) . . ? O5 S3 C71 106.9(6) . . ? O6 S3 C71 112.7(6) . . ? C17 S3 C71 105.6(5) . . ? C72 C71 S3 106.7(9) . . ? C72 C71 H56 110.4 . . ? S3 C71 H56 110.4 . . ? C72 C71 H57 110.4 . . ? S3 C71 H57 110.4 . . ? H56 C71 H57 108.6 . . ? C71 C72 H58 109.5 . . ? C71 C72 H59 109.5 . . ? H58 C72 H59 109.5 . . ? C71 C72 H60 109.5 . . ? H58 C72 H60 109.5 . . ? H59 C72 H60 109.5 . . ? O8 S4 O7 119.8(6) . . ? O8 S4 C73 108.1(5) . . ? O7 S4 C73 107.8(5) . . ? O8 S4 C18 110.0(7) . . ? O7 S4 C18 105.7(6) . . ? C73 S4 C18 104.3(6) . . ? C74 C73 S4 109.2(8) . . ? C74 C73 H61 109.8 . . ? S4 C73 H61 109.8 . . ? C74 C73 H62 109.8 . . ? S4 C73 H62 109.8 . . ? H61 C73 H62 108.3 . . ? C73 C74 H63 109.5 . . ? C73 C74 H64 109.5 . . ? H63 C74 H64 109.5 . . ? C73 C74 H65 109.5 . . ? H63 C74 H65 109.5 . . ? H64 C74 H65 109.5 . . ? C76A C75A C80A 120.0 . . ? C76A C75A H21 120.0 . . ? C80A C75A H21 120.0 . . ? C75A C76A C77A 120.0 . . ? C75A C76A H22 120.0 . . ? C77A C76A H22 120.0 . . ? C78A C77A C76A 120.0 . . ? C78A C77A H23 120.0 . . ? C76A C77A H23 120.0 . . ? C79A C78A C77A 120.0 . . ? C79A C78A H24 120.0 . . ? C77A C78A H24 120.0 . . ? C78A C79A C80A 120.0 . . ? C78A C79A H25 120.0 . . ? C80A C79A H25 120.0 . . ? C79A C80A C75A 120.0 . . ? C79A C80A H26 120.0 . . ? C75A C80A H26 120.0 . . ? C82 C81 C86 124(2) . . ? C82 C81 H27 117.9 . . ? C86 C81 H27 117.9 . . ? C83 C82 C81 116(2) . . ? C83 C82 H28 122.0 . . ? C81 C82 H28 122.0 . . ? C82 C83 C84 121(2) . . ? C82 C83 H29 119.4 . . ? C84 C83 H29 119.4 . . ? C85 C84 C83 120(2) . . ? C85 C84 H30 120.1 . . ? C83 C84 H30 120.1 . . ? C84 C85 C86 120.3(19) . . ? C84 C85 H31 119.9 . . ? C86 C85 H31 119.9 . . ? C85 C86 C81 118(2) . . ? C85 C86 H32 120.8 . . ? C81 C86 H32 120.8 . . ? C76B C75B C80B 120.0 . . ? C76B C75B H33 120.0 . . ? C80B C75B H33 120.0 . . ? C75B C76B C77B 120.0 . . ? C75B C76B H34 120.0 . . ? C77B C76B H34 120.0 . . ? C78B C77B C76B 120.0 . . ? C78B C77B H35 120.0 . . ? C76B C77B H35 120.0 . . ? C79B C78B C77B 120.0 . . ? C79B C78B H36 120.0 . . ? C77B C78B H36 120.0 . . ? C78B C79B C80B 120.0 . . ? C78B C79B H37 120.0 . . ? C80B C79B H37 120.0 . . ? C79B C80B C75B 120.0 . . ? C79B C80B H38 120.0 . . ? C75B C80B H38 120.0 . . ? C88 C87 C92 117.6(19) . . ? C88 C87 H9 121.2 . . ? C92 C87 H9 121.2 . . ? C87 C88 C89 120.4(19) . . ? C87 C88 H10 119.8 . . ? C89 C88 H10 119.8 . . ? C90 C89 C88 123.4(17) . . ? C90 C89 H11 118.3 . . ? C88 C89 H11 118.3 . . ? C91 C90 C89 113.9(16) . . ? C91 C90 H12 123.0 . . ? C89 C90 H12 123.0 . . ? C90 C91 C92 122.7(18) . . ? C90 C91 H13 118.6 . . ? C92 C91 H13 118.6 . . ? C87 C92 C91 121.7(18) . . ? C87 C92 H14 119.1 . . ? C91 C92 H14 119.1 . . ? C94 C93 C98 122.5(19) . . ? C94 C93 H39 118.8 . . ? C98 C93 H39 118.8 . . ? C95 C94 C93 118(2) . . ? C95 C94 H40 121.0 . . ? C93 C94 H40 121.0 . . ? C94 C95 C96 120(2) . . ? C94 C95 H41 119.9 . . ? C96 C95 H41 119.9 . . ? C97 C96 C95 120(2) . . ? C97 C96 H42 119.8 . . ? C95 C96 H42 119.8 . . ? C98 C97 C96 121(2) . . ? C98 C97 H43 119.6 . . ? C96 C97 H43 119.6 . . ? C97 C98 C93 117(2) . . ? C97 C98 H44 121.3 . . ? C93 C98 H44 121.3 . . ? C100 C99 C104 120.0 . . ? C100 C99 H75 120.0 . . ? C104 C99 H75 120.0 . . ? C101 C100 C99 120.0 . . ? C101 C100 H76 120.0 . . ? C99 C100 H76 120.0 . . ? C100 C101 C102 120.0 . . ? C100 C101 H77 120.0 . . ? C102 C101 H77 120.0 . . ? C101 C102 C103 120.0 . . ? C101 C102 H78 120.0 . . ? C103 C102 H78 120.0 . . ? C104 C103 C102 120.0 . . ? C104 C103 H79 120.0 . . ? C102 C103 H79 120.0 . . ? C103 C104 C99 120.0 . . ? C103 C104 H80 120.0 . . ? C99 C104 H80 120.0 . . ? C106 C105 H85 109.5 . . ? C106 C105 H86 109.5 . . ? H85 C105 H86 109.5 . . ? C106 C105 H87 109.5 . . ? H85 C105 H87 109.5 . . ? H86 C105 H87 109.5 . . ? C105 C106 C107 108.0(14) . . ? C105 C106 H69 110.1 . . ? C107 C106 H69 110.1 . . ? C105 C106 H70 110.1 . . ? C107 C106 H70 110.1 . . ? H69 C106 H70 108.4 . . ? C108 C107 C106 113.2(17) . . ? C108 C107 H71 108.9 . . ? C106 C107 H71 108.9 . . ? C108 C107 H72 108.9 . . ? C106 C107 H72 108.9 . . ? H71 C107 H72 107.7 . . ? C107 C108 C108 116(2) . 2_566 ? C107 C108 H73 108.3 . . ? C108 C108 H73 108.3 2_566 . ? C107 C108 H74 108.3 . . ? C108 C108 H74 108.3 2_566 . ? H73 C108 H74 107.4 . . ? 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 -0.3(14) . . . . ? C30 C1 C2 C3 178.1(16) . . . . ? N1 C1 C2 S1 -169.2(8) . . . . ? C30 C1 C2 S1 9(2) . . . . ? C1 C2 C3 C4 -0.5(15) . . . . ? S1 C2 C3 C4 168.2(8) . . . . ? C1 C2 C3 S2 171.1(8) . . . . ? S1 C2 C3 S2 -20.2(18) . . . . ? C2 C3 C4 N1 1.1(14) . . . . ? S2 C3 C4 N1 -170.9(8) . . . . ? C2 C3 C4 C5 173.5(13) . . . . ? S2 C3 C4 C5 2(2) . . . . ? N1 C4 C5 C6 22.5(18) . . . . ? C3 C4 C5 C6 -149.2(14) . . . . ? N1 C4 C5 C31 -144.1(12) . . . . ? C3 C4 C5 C31 44(2) . . . . ? C4 C5 C6 N2 8.9(18) . . . . ? C31 C5 C6 N2 176.3(10) . . . . ? C4 C5 C6 C7 -171.3(12) . . . . ? C31 C5 C6 C7 -3.9(19) . . . . ? C5 C6 C7 C8 177.7(12) . . . . ? N2 C6 C7 C8 -2.4(13) . . . . ? C6 C7 C8 C9 -0.2(14) . . . . ? C7 C8 C9 N2 2.9(14) . . . . ? C7 C8 C9 C10 -170.1(11) . . . . ? N2 C9 C10 C11 7(2) . . . . ? C8 C9 C10 C11 179.2(13) . . . . ? N2 C9 C10 C37 -168.2(11) . . . . ? C8 C9 C10 C37 4.1(18) . . . . ? C9 C10 C11 N3 -158.3(12) . . . . ? C37 C10 C11 N3 16.5(19) . . . . ? C9 C10 C11 C12 25(2) . . . . ? C37 C10 C11 C12 -160.5(13) . . . . ? N3 C11 C12 C13 -0.1(15) . . . . ? C10 C11 C12 C13 177.4(14) . . . . ? C11 C12 C13 C14 2.4(15) . . . . ? C12 C13 C14 N3 -3.8(14) . . . . ? C12 C13 C14 C15 171.9(12) . . . . ? N3 C14 C15 C43 -179.7(14) . . . . ? C13 C14 C15 C43 6(2) . . . . ? N3 C14 C15 C16 8(2) . . . . ? C13 C14 C15 C16 -166.2(11) . . . . ? C14 C15 C16 N4 29.1(17) . . . . ? C43 C15 C16 N4 -142.7(14) . . . . ? C14 C15 C16 C17 -153.2(13) . . . . ? C43 C15 C16 C17 35(2) . . . . ? N4 C16 C17 C18 3.1(14) . . . . ? C15 C16 C17 C18 -174.6(13) . . . . ? N4 C16 C17 S3 -168.7(9) . . . . ? C15 C16 C17 S3 14(2) . . . . ? C16 C17 C18 C19 -1.2(14) . . . . ? S3 C17 C18 C19 170.5(9) . . . . ? C16 C17 C18 S4 170.4(9) . . . . ? S3 C17 C18 S4 -17.8(18) . . . . ? C17 C18 C19 N4 -1.0(15) . . . . ? S4 C18 C19 N4 -172.7(9) . . . . ? C17 C18 C19 C20 178.9(13) . . . . ? S4 C18 C19 C20 7(2) . . . . ? N4 C19 C20 C21 33.1(17) . . . . ? C18 C19 C20 C21 -146.8(14) . . . . ? N4 C19 C20 C49 -146.0(12) . . . . ? C18 C19 C20 C49 34(2) . . . . ? C49 C20 C21 N5 179.4(10) . . . . ? C19 C20 C21 N5 0.3(19) . . . . ? C49 C20 C21 C22 5.0(19) . . . . ? C19 C20 C21 C22 -174.1(11) . . . . ? C20 C21 C22 C23 172.8(12) . . . . ? N5 C21 C22 C23 -2.4(12) . . . . ? C21 C22 C23 C24 0.7(12) . . . . ? C22 C23 C24 N5 1.3(13) . . . . ? C22 C23 C24 C25 -169.7(11) . . . . ? N5 C24 C25 C26 7.0(19) . . . . ? C23 C24 C25 C26 176.2(11) . . . . ? N5 C24 C25 C55 -168.6(12) . . . . ? C23 C24 C25 C55 0.7(18) . . . . ? C24 C25 C26 N6 -156.4(11) . . . . ? C55 C25 C26 N6 19.0(19) . . . . ? C24 C25 C26 C27 32(2) . . . . ? C55 C25 C26 C27 -152.6(14) . . . . ? N6 C26 C27 C28 0.1(13) . . . . ? C25 C26 C27 C28 172.9(13) . . . . ? C26 C27 C28 C29 -0.3(14) . . . . ? C27 C28 C29 C30 176.6(13) . . . . ? C27 C28 C29 N6 0.4(13) . . . . ? N6 C29 C30 C1 12(2) . . . . ? C28 C29 C30 C1 -163.9(12) . . . . ? N6 C29 C30 C61 -174.6(12) . . . . ? C28 C29 C30 C61 10(2) . . . . ? N1 C1 C30 C29 22.4(19) . . . . ? C2 C1 C30 C29 -155.8(15) . . . . ? N1 C1 C30 C61 -151.0(13) . . . . ? C2 C1 C30 C61 31(3) . . . . ? C6 C5 C31 C36 -118.6(14) . . . . ? C4 C5 C31 C36 49.1(19) . . . . ? C6 C5 C31 C32 63.5(15) . . . . ? C4 C5 C31 C32 -128.9(13) . . . . ? C36 C31 C32 F1 -175.4(10) . . . . ? C5 C31 C32 F1 2.8(18) . . . . ? C36 C31 C32 C33 1.1(18) . . . . ? C5 C31 C32 C33 179.3(12) . . . . ? F1 C32 C33 C34 177.5(12) . . . . ? C31 C32 C33 C34 1(2) . . . . ? F1 C32 C33 F2 -4.4(17) . . . . ? C31 C32 C33 F2 179.1(10) . . . . ? F2 C33 C34 F3 3(2) . . . . ? C32 C33 C34 F3 -178.6(13) . . . . ? F2 C33 C34 C35 179.0(12) . . . . ? C32 C33 C34 C35 -3(2) . . . . ? F3 C34 C35 F4 -7(2) . . . . ? C33 C34 C35 F4 177.8(13) . . . . ? F3 C34 C35 C36 178.5(13) . . . . ? C33 C34 C35 C36 3(2) . . . . ? F4 C35 C36 C31 -175.8(12) . . . . ? C34 C35 C36 C31 -1(2) . . . . ? F4 C35 C36 F5 2(2) . . . . ? C34 C35 C36 F5 176.9(12) . . . . ? C32 C31 C36 C35 -1(2) . . . . ? C5 C31 C36 C35 -179.3(14) . . . . ? C32 C31 C36 F5 -179.0(10) . . . . ? C5 C31 C36 F5 2.9(19) . . . . ? C11 C10 C37 C38 107.5(15) . . . . ? C9 C10 C37 C38 -77.1(16) . . . . ? C11 C10 C37 C42 -76.4(17) . . . . ? C9 C10 C37 C42 99.1(14) . . . . ? C42 C37 C38 F6 -179.0(11) . . . . ? C10 C37 C38 F6 -3(2) . . . . ? C42 C37 C38 C39 4(2) . . . . ? C10 C37 C38 C39 179.9(14) . . . . ? C37 C38 C39 F7 179.2(11) . . . . ? F6 C38 C39 F7 1.6(18) . . . . ? C37 C38 C39 C40 0(2) . . . . ? F6 C38 C39 C40 -178.1(10) . . . . ? F7 C39 C40 C41 177.0(11) . . . . ? C38 C39 C40 C41 -3(2) . . . . ? F7 C39 C40 F8 -0.3(18) . . . . ? C38 C39 C40 F8 179.4(11) . . . . ? C39 C40 C41 F9 -177.6(12) . . . . ? F8 C40 C41 F9 -0.4(18) . . . . ? C39 C40 C41 C42 3.5(19) . . . . ? F8 C40 C41 C42 -179.2(11) . . . . ? C38 C37 C42 F10 177.4(11) . . . . ? C10 C37 C42 F10 1.1(19) . . . . ? C38 C37 C42 C41 -3(2) . . . . ? C10 C37 C42 C41 -179.6(13) . . . . ? F9 C41 C42 F10 0.3(18) . . . . ? C40 C41 C42 F10 179.1(10) . . . . ? F9 C41 C42 C37 -179.0(11) . . . . ? C40 C41 C42 C37 0(2) . . . . ? C14 C15 C43 C44 69.9(19) . . . . ? C16 C15 C43 C44 -118.8(16) . . . . ? C14 C15 C43 C48 -114.1(15) . . . . ? C16 C15 C43 C48 57.2(18) . . . . ? C48 C43 C44 C45 4(2) . . . . ? C15 C43 C44 C45 179.8(14) . . . . ? C48 C43 C44 F11 -179.9(10) . . . . ? C15 C43 C44 F11 -4(2) . . . . ? C43 C44 C45 F12 -179.6(12) . . . . ? F11 C44 C45 F12 4(2) . . . . ? C43 C44 C45 C46 -5(2) . . . . ? F11 C44 C45 C46 178.2(10) . . . . ? F12 C45 C46 C47 -179.6(14) . . . . ? C44 C45 C46 C47 6(2) . . . . ? F12 C45 C46 F13 -3.4(19) . . . . ? C44 C45 C46 F13 -177.6(12) . . . . ? F13 C46 C47 F14 4(2) . . . . ? C45 C46 C47 F14 179.6(12) . . . . ? F13 C46 C47 C48 179.0(12) . . . . ? C45 C46 C47 C48 -5(2) . . . . ? C46 C47 C48 F15 -179.2(12) . . . . ? F14 C47 C48 F15 -4(2) . . . . ? C46 C47 C48 C43 3(2) . . . . ? F14 C47 C48 C43 178.1(11) . . . . ? C44 C43 C48 F15 -179.9(12) . . . . ? C15 C43 C48 F15 4(2) . . . . ? C44 C43 C48 C47 -2(2) . . . . ? C15 C43 C48 C47 -178.5(14) . . . . ? C21 C20 C49 C50 -119.6(14) . . . . ? C19 C20 C49 C50 59.5(17) . . . . ? C21 C20 C49 C54 56.1(18) . . . . ? C19 C20 C49 C54 -124.8(14) . . . . ? C54 C49 C50 F16 -179.6(10) . . . . ? C20 C49 C50 F16 -3.5(18) . . . . ? C54 C49 C50 C51 3.9(18) . . . . ? C20 C49 C50 C51 180.0(13) . . . . ? F16 C50 C51 C52 -176.9(12) . . . . ? C49 C50 C51 C52 0(2) . . . . ? F16 C50 C51 F17 2.3(18) . . . . ? C49 C50 C51 F17 178.8(10) . . . . ? F17 C51 C52 F18 3(2) . . . . ? C50 C51 C52 F18 -178.1(12) . . . . ? F17 C51 C52 C53 178.1(11) . . . . ? C50 C51 C52 C53 -3(2) . . . . ? C51 C52 C53 C54 2(2) . . . . ? F18 C52 C53 C54 177.5(12) . . . . ? C51 C52 C53 F19 180.0(11) . . . . ? F18 C52 C53 F19 -5(2) . . . . ? C52 C53 C54 F20 175.2(11) . . . . ? F19 C53 C54 F20 -2.4(18) . . . . ? C52 C53 C54 C49 1(2) . . . . ? F19 C53 C54 C49 -176.3(10) . . . . ? C50 C49 C54 F20 -178.2(10) . . . . ? C20 C49 C54 F20 5.8(19) . . . . ? C50 C49 C54 C53 -4.3(18) . . . . ? C20 C49 C54 C53 179.7(13) . . . . ? C26 C25 C55 C60 -77.4(17) . . . . ? C24 C25 C55 C60 98.2(15) . . . . ? C26 C25 C55 C56 103.1(15) . . . . ? C24 C25 C55 C56 -81.3(16) . . . . ? C60 C55 C56 F21 177.0(11) . . . . ? C25 C55 C56 F21 -3(2) . . . . ? C60 C55 C56 C57 3(2) . . . . ? C25 C55 C56 C57 -177.2(13) . . . . ? F21 C56 C57 F22 6.2(19) . . . . ? C55 C56 C57 F22 -179.8(11) . . . . ? F21 C56 C57 C58 -176.9(12) . . . . ? C55 C56 C57 C58 -3(2) . . . . ? F22 C57 C58 C59 176.7(14) . . . . ? C56 C57 C58 C59 0(3) . . . . ? F22 C57 C58 F23 -2(2) . . . . ? C56 C57 C58 F23 -178.9(11) . . . . ? C57 C58 C59 F24 179.3(14) . . . . ? F23 C58 C59 F24 -2(2) . . . . ? C57 C58 C59 C60 2(2) . . . . ? F23 C58 C59 C60 -178.9(11) . . . . ? C56 C55 C60 F25 179.4(11) . . . . ? C25 C55 C60 F25 -0.1(19) . . . . ? C56 C55 C60 C59 -1(2) . . . . ? C25 C55 C60 C59 179.6(13) . . . . ? C58 C59 C60 C55 -2(2) . . . . ? F24 C59 C60 C55 -179.2(12) . . . . ? C58 C59 C60 F25 178.0(12) . . . . ? F24 C59 C60 F25 0.5(18) . . . . ? C29 C30 C61 C66 70.5(18) . . . . ? C1 C30 C61 C66 -115.9(15) . . . . ? C29 C30 C61 C62 -107.6(17) . . . . ? C1 C30 C61 C62 66(2) . . . . ? C66 C61 C62 C63 3(2) . . . . ? C30 C61 C62 C63 -179.2(15) . . . . ? C66 C61 C62 F26 -179.1(10) . . . . ? C30 C61 C62 F26 -1(2) . . . . ? F26 C62 C63 F27 0(2) . . . . ? C61 C62 C63 F27 177.9(11) . . . . ? F26 C62 C63 C64 177.6(10) . . . . ? C61 C62 C63 C64 -4(2) . . . . ? C62 C63 C64 C65 5(2) . . . . ? F27 C63 C64 C65 -177.0(12) . . . . ? C62 C63 C64 F28 179.3(11) . . . . ? F27 C63 C64 F28 -3(2) . . . . ? C63 C64 C65 F29 178.1(12) . . . . ? F28 C64 C65 F29 3.8(19) . . . . ? C63 C64 C65 C66 -4(2) . . . . ? F28 C64 C65 C66 -178.7(11) . . . . ? C62 C61 C66 C65 -2(2) . . . . ? C30 C61 C66 C65 179.9(15) . . . . ? C62 C61 C66 F30 -179.6(10) . . . . ? C30 C61 C66 F30 2(2) . . . . ? F29 C65 C66 C61 -179.9(12) . . . . ? C64 C65 C66 C61 3(2) . . . . ? F29 C65 C66 F30 -2.0(19) . . . . ? C64 C65 C66 F30 -179.4(10) . . . . ? C3 C4 N1 C1 -1.4(14) . . . . ? C5 C4 N1 C1 -175.1(10) . . . . ? C30 C1 N1 C4 -177.7(11) . . . . ? C2 C1 N1 C4 1.0(13) . . . . ? C10 C9 N2 C6 168.9(11) . . . . ? C8 C9 N2 C6 -4.5(14) . . . . ? C5 C6 N2 C9 -175.9(10) . . . . ? C7 C6 N2 C9 4.2(13) . . . . ? C15 C14 N3 C11 -171.3(12) . . . . ? C13 C14 N3 C11 4.2(15) . . . . ? C10 C11 N3 C14 179.6(12) . . . . ? C12 C11 N3 C14 -2.7(14) . . . . ? C17 C16 N4 C19 -3.8(14) . . . . ? C15 C16 N4 C19 174.3(11) . . . . ? C18 C19 N4 C16 3.0(15) . . . . ? C20 C19 N4 C16 -176.9(11) . . . . ? C25 C24 N5 C21 168.2(11) . . . . ? C23 C24 N5 C21 -2.9(12) . . . . ? C20 C21 N5 C24 -172.2(11) . . . . ? C22 C21 N5 C24 3.3(12) . . . . ? C25 C26 N6 C29 -173.7(11) . . . . ? C27 C26 N6 C29 0.2(12) . . . . ? C30 C29 N6 C26 -176.8(12) . . . . ? C28 C29 N6 C26 -0.4(13) . . . . ? C3 C2 S1 O1 -161.1(11) . . . . ? C1 C2 S1 O1 6.1(12) . . . . ? C3 C2 S1 O2 -36.0(13) . . . . ? C1 C2 S1 O2 131.2(10) . . . . ? C3 C2 S1 C67 80.1(12) . . . . ? C1 C2 S1 C67 -112.7(11) . . . . ? O1 S1 C67 C68 -48.5(9) . . . . ? O2 S1 C67 C68 -176.4(8) . . . . ? C2 S1 C67 C68 67.9(10) . . . . ? C2 C3 S2 O3 -155.0(11) . . . . ? C4 C3 S2 O3 15.3(12) . . . . ? C2 C3 S2 O4 -28.2(13) . . . . ? C4 C3 S2 O4 142.0(10) . . . . ? C2 C3 S2 C69 89.9(13) . . . . ? C4 C3 S2 C69 -99.8(11) . . . . ? O3 S2 C69 C70 62.6(9) . . . . ? O4 S2 C69 C70 -64.8(9) . . . . ? C3 S2 C69 C70 176.9(9) . . . . ? C18 C17 S3 O5 -160.8(11) . . . . ? C16 C17 S3 O5 9.1(13) . . . . ? C18 C17 S3 O6 -35.0(13) . . . . ? C16 C17 S3 O6 135.0(11) . . . . ? C18 C17 S3 C71 85.0(12) . . . . ? C16 C17 S3 C71 -105.0(12) . . . . ? O5 S3 C71 C72 76.0(10) . . . . ? O6 S3 C71 C72 -53.1(10) . . . . ? C17 S3 C71 C72 -169.1(9) . . . . ? C19 C18 S4 O8 144.7(11) . . . . ? C17 C18 S4 O8 -25.4(13) . . . . ? C19 C18 S4 O7 14.0(13) . . . . ? C17 C18 S4 O7 -156.1(11) . . . . ? C19 C18 S4 C73 -99.6(12) . . . . ? C17 C18 S4 C73 90.3(12) . . . . ? O8 S4 C73 C74 -83.1(9) . . . . ? O7 S4 C73 C74 47.7(10) . . . . ? C18 S4 C73 C74 159.8(9) . . . . ? C80A C75A C76A C77A 0.0 . . . . ? C75A C76A C77A C78A 0.0 . . . . ? C76A C77A C78A C79A 0.0 . . . . ? C77A C78A C79A C80A 0.0 . . . . ? C78A C79A C80A C75A 0.0 . . . . ? C76A C75A C80A C79A 0.0 . . . . ? C86 C81 C82 C83 0(3) . . . . ? C81 C82 C83 C84 -2(2) . . . . ? C82 C83 C84 C85 3(3) . . . . ? C83 C84 C85 C86 0(2) . . . . ? C84 C85 C86 C81 -2(2) . . . . ? C82 C81 C86 C85 3(3) . . . . ? C80B C75B C76B C77B 0.0 . . . . ? C75B C76B C77B C78B 0.0 . . . . ? C76B C77B C78B C79B 0.0 . . . . ? C77B C78B C79B C80B 0.0 . . . . ? C78B C79B C80B C75B 0.0 . . . . ? C76B C75B C80B C79B 0.0 . . . . ? C92 C87 C88 C89 -2(3) . . . . ? C87 C88 C89 C90 5(3) . . . . ? C88 C89 C90 C91 -7(3) . . . . ? C89 C90 C91 C92 5(2) . . . . ? C88 C87 C92 C91 0(3) . . . . ? C90 C91 C92 C87 -2(3) . . . . ? C98 C93 C94 C95 -2(3) . . . . ? C93 C94 C95 C96 3(3) . . . . ? C94 C95 C96 C97 -6(3) . . . . ? C95 C96 C97 C98 8(3) . . . . ? C96 C97 C98 C93 -7(3) . . . . ? C94 C93 C98 C97 4(3) . . . . ? C104 C99 C100 C101 0.0 . . . . ? C99 C100 C101 C102 0.0 . . . . ? C100 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C104 0.0 . . . . ? C102 C103 C104 C99 0.0 . . . . ? C100 C99 C104 C103 0.0 . . . . ? C105 C106 C107 C108 165.7(15) . . . . ? C106 C107 C108 C108 -170.8(15) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 61.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.390 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.065 data_0225hi _database_code_depnum_ccdc_archive 'CCDC 906720' #TrackingRef 'S_28-ChemSci.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H32 F30 N6 S4, C Cl4' _chemical_formula_sum 'C75 H32 Cl4 F30 N6 S4' _chemical_formula_weight 1857.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2654(2) _cell_length_b 15.3627(3) _cell_length_c 24.8758(4) _cell_angle_alpha 101.4320(8) _cell_angle_beta 93.5605(8) _cell_angle_gamma 112.7488(8) _cell_volume 4186.73(13) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 31654 _cell_measurement_theta_min 3.215 _cell_measurement_theta_max 68.20 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 3.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5645 _exptl_absorpt_correction_T_max 0.7384 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43923 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 60.00 _reflns_number_total 12291 _reflns_number_gt 6996 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12291 _refine_ls_number_parameters 1277 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.1176 _refine_ls_wR_factor_ref 0.3743 _refine_ls_wR_factor_gt 0.3210 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.275 _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 0.3522(7) 0.5356(6) 0.2936(3) 0.085(2) Uani 1 1 d . . . C4 C 0.2321(7) 0.5071(5) 0.2192(3) 0.0683(19) Uani 1 1 d . . . C5 C 0.1624(6) 0.4511(5) 0.1630(3) 0.0615(17) Uani 1 1 d . B . C6 C 0.1477(6) 0.3588(5) 0.1457(3) 0.0581(17) Uani 1 1 d . . . C7 C 0.0964(6) 0.2910(5) 0.0916(3) 0.0631(17) Uani 1 1 d . B . H1 H 0.0615 0.3043 0.0607 0.076 Uiso 1 1 calc R . . C8 C 0.1062(6) 0.2050(5) 0.0919(3) 0.0574(16) Uani 1 1 d . . . H2 H 0.0805 0.1496 0.0615 0.069 Uiso 1 1 calc R B . C9 C 0.1627(5) 0.2138(5) 0.1468(2) 0.0539(16) Uani 1 1 d . B . C10 C 0.1971(5) 0.1490(5) 0.1645(2) 0.0523(15) Uani 1 1 d . . . C11 C 0.2478(5) 0.1608(5) 0.2203(3) 0.0579(16) Uani 1 1 d . B . C12 C 0.2360(6) 0.2089(5) 0.2728(3) 0.0670(18) Uani 1 1 d . . . H3 H 0.1924 0.2484 0.2792 0.080 Uiso 1 1 calc R B . C13 C 0.2983(6) 0.1890(6) 0.3130(3) 0.0677(19) Uani 1 1 d . B . H4 H 0.3034 0.2113 0.3519 0.081 Uiso 1 1 calc R . . C14 C 0.3520(6) 0.1315(5) 0.2880(3) 0.0605(17) Uani 1 1 d . . . C15 C 0.4298(7) 0.0934(6) 0.3105(3) 0.070(2) Uani 1 1 d . B . C16 C 0.4994(7) 0.0577(6) 0.2781(3) 0.072(2) Uani 1 1 d . . . C17 C 0.5685(8) 0.0009(7) 0.2865(3) 0.090(3) Uani 1 1 d . B . C18 C 0.6192(8) -0.0110(6) 0.2386(3) 0.081(2) Uani 1 1 d . . . C19 C 0.5832(7) 0.0404(6) 0.2043(3) 0.072(2) Uani 1 1 d . B . C20 C 0.6259(6) 0.0633(5) 0.1514(3) 0.0580(16) Uani 1 1 d . . . C21 C 0.6355(6) 0.1499(5) 0.1416(3) 0.0613(17) Uani 1 1 d . B . C22 C 0.6613(6) 0.1863(5) 0.0913(3) 0.0629(18) Uani 1 1 d . . . H5 H 0.6803 0.1541 0.0590 0.076 Uiso 1 1 calc R B . C23 C 0.6534(6) 0.2725(5) 0.0985(3) 0.0628(17) Uani 1 1 d . B . H6 H 0.6645 0.3102 0.0717 0.075 Uiso 1 1 calc R . . C24 C 0.6251(5) 0.2994(5) 0.1541(3) 0.0583(17) Uani 1 1 d . . . C25 C 0.5987(5) 0.3737(5) 0.1767(3) 0.0559(16) Uani 1 1 d . B . C26 C 0.5746(6) 0.3961(5) 0.2322(3) 0.0603(17) Uani 1 1 d . . . C27 C 0.6145(6) 0.3813(5) 0.2836(3) 0.0677(19) Uani 1 1 d . B . H7 H 0.6612 0.3455 0.2881 0.081 Uiso 1 1 calc R . . C28 C 0.5738(6) 0.4277(5) 0.3253(3) 0.0676(18) Uani 1 1 d . . . H8 H 0.5900 0.4318 0.3637 0.081 Uiso 1 1 calc R B . C29 C 0.5057(6) 0.4673(5) 0.3018(3) 0.0672(18) Uani 1 1 d . A . C30 C 0.4397(8) 0.5230(6) 0.3267(3) 0.084(2) Uani 1 1 d . A . C31 C 0.1167(6) 0.4973(5) 0.1273(3) 0.0633(18) Uani 1 1 d . . . C36 C 0.1896(7) 0.5837(6) 0.1145(4) 0.082(2) Uani 1 1 d . B . C35 C 0.1499(7) 0.6307(6) 0.0818(4) 0.087(2) Uani 1 1 d . . . C34 C 0.0318(6) 0.5908(5) 0.0593(3) 0.0690(19) Uani 1 1 d . B . C33 C -0.0434(6) 0.5067(5) 0.0705(3) 0.0646(18) Uani 1 1 d . . . C32 C -0.0022(6) 0.4618(5) 0.1037(3) 0.0597(17) Uani 1 1 d . B . C37 C 0.1845(5) 0.0586(5) 0.1231(2) 0.0523(15) Uani 1 1 d . B . C38 C 0.0803(6) -0.0254(5) 0.1080(3) 0.0533(16) Uani 1 1 d . . . C39 C 0.0686(6) -0.1044(5) 0.0692(3) 0.0565(16) Uani 1 1 d . B . C40 C 0.1649(6) -0.1055(5) 0.0428(3) 0.0525(15) Uani 1 1 d . . . C41 C 0.2716(5) -0.0248(5) 0.0575(2) 0.0506(15) Uani 1 1 d . B . C42 C 0.2803(6) 0.0553(5) 0.0960(3) 0.0554(16) Uani 1 1 d . . . C43 C 0.4406(6) 0.0986(5) 0.37076(17) 0.076(2) Uani 1 1 d G . . C44 C 0.3484(6) 0.0342(5) 0.3915(3) 0.110(3) Uani 1 1 d G B . C45 C 0.3599(8) 0.0358(6) 0.4477(3) 0.137(5) Uani 1 1 d G B . C46 C 0.4636(9) 0.1018(6) 0.48310(18) 0.130(5) Uani 1 1 d G B . C47 C 0.5558(7) 0.1662(6) 0.4624(2) 0.123(4) Uani 1 1 d G B . C48 C 0.5443(6) 0.1646(5) 0.4062(2) 0.095(3) Uani 1 1 d G B . C49 C 0.6446(6) -0.0096(5) 0.1099(3) 0.0598(17) Uani 1 1 d . B . C50 C 0.5540(6) -0.1019(5) 0.0874(3) 0.0572(16) Uani 1 1 d . . . C51 C 0.5650(6) -0.1695(5) 0.0477(3) 0.0640(18) Uani 1 1 d . B . C52 C 0.6716(7) -0.1500(6) 0.0272(3) 0.0634(18) Uani 1 1 d . . . C53 C 0.7623(6) -0.0610(5) 0.0477(3) 0.0567(16) Uani 1 1 d . B . C54 C 0.7520(6) 0.0089(5) 0.0882(3) 0.0583(17) Uani 1 1 d . . . C55 C 0.5985(7) 0.4434(6) 0.1423(3) 0.071(2) Uani 1 1 d . . . C56 C 0.4926(8) 0.4341(7) 0.1135(3) 0.085(2) Uani 1 1 d . B . C57 C 0.4876(12) 0.4963(11) 0.0814(4) 0.130(4) Uani 1 1 d . . . C58 C 0.6008(16) 0.5727(11) 0.0784(6) 0.150(6) Uani 1 1 d . B . C59 C 0.7038(11) 0.5819(8) 0.1051(5) 0.114(4) Uani 1 1 d . . . C60 C 0.7016(8) 0.5185(6) 0.1376(4) 0.086(2) Uani 1 1 d . B . C61A C 0.452(2) 0.5527(17) 0.3922(6) 0.085(7) Uani 0.52(3) 1 d PGU A 3 C62A C 0.3716(19) 0.5022(14) 0.4237(10) 0.112(11) Uani 0.52(3) 1 d PGU A 3 C63A C 0.392(2) 0.5344(17) 0.4812(9) 0.090(7) Uani 0.52(3) 1 d PGU A 3 C64A C 0.494(2) 0.6170(18) 0.5073(6) 0.090(6) Uani 0.52(3) 1 d PGU A 3 C65A C 0.5745(17) 0.6675(15) 0.4758(7) 0.091(7) Uani 0.52(3) 1 d PGU A 3 C66A C 0.554(2) 0.6353(16) 0.4183(6) 0.089(7) Uani 0.52(3) 1 d PGU A 3 F26A F 0.2802(19) 0.4174(18) 0.4038(9) 0.086(5) Uani 0.52(3) 1 d P A 3 F27A F 0.328(2) 0.4915(16) 0.5140(7) 0.102(6) Uani 0.52(3) 1 d P A 3 F28A F 0.666(2) 0.7534(13) 0.4991(8) 0.122(7) Uani 0.52(3) 1 d P A 3 F29A F 0.521(2) 0.6540(18) 0.5627(7) 0.127(7) Uani 0.52(3) 1 d P A 3 F30A F 0.625(2) 0.6811(15) 0.3892(9) 0.106(6) Uani 0.52(3) 1 d P A 3 C61B C 0.487(2) 0.5752(18) 0.3847(6) 0.088(9) Uani 0.48(3) 1 d PGU A 4 C62B C 0.416(2) 0.5374(17) 0.4228(7) 0.076(8) Uani 0.48(3) 1 d PGU A 4 C63B C 0.450(3) 0.582(2) 0.4790(6) 0.092(9) Uani 0.48(3) 1 d PGU A 4 C64B C 0.556(3) 0.665(2) 0.4972(7) 0.092(10) Uani 0.48(3) 1 d PGU A 4 C65B C 0.628(2) 0.7033(17) 0.4590(10) 0.111(10) Uani 0.48(3) 1 d PGU A 4 C66B C 0.593(2) 0.6581(19) 0.4028(9) 0.111(12) Uani 0.48(3) 1 d PGU A 4 F26B F 0.320(3) 0.460(2) 0.4034(10) 0.093(7) Uani 0.48(3) 1 d PU A 4 F27B F 0.391(3) 0.554(3) 0.5131(8) 0.144(11) Uani 0.48(3) 1 d P A 4 F28B F 0.584(4) 0.703(2) 0.5480(8) 0.165(14) Uani 0.48(3) 1 d P A 4 F29B F 0.732(3) 0.777(2) 0.4800(13) 0.231(16) Uani 0.48(3) 1 d P A 4 F30B F 0.660(2) 0.7051(19) 0.3671(10) 0.135(8) Uani 0.48(3) 1 d P A 4 N1 N 0.3146(5) 0.4843(4) 0.2393(2) 0.0662(15) Uani 1 1 d . B . N2 N 0.1815(5) 0.3042(4) 0.1777(2) 0.0629(15) Uani 1 1 d . B . H9 H 0.2110 0.3257 0.2132 0.076 Uiso 1 1 calc R . . N3 N 0.3183(5) 0.1141(4) 0.2312(2) 0.0589(14) Uani 1 1 d . B . H10 H 0.3395 0.0778 0.2057 0.071 Uiso 1 1 calc R . . N4 N 0.5105(5) 0.0765(4) 0.2255(2) 0.0627(15) Uani 1 1 d . B . N5 N 0.6198(5) 0.2229(4) 0.1780(2) 0.0634(14) Uani 1 1 d . B . H11 H 0.6078 0.2215 0.2124 0.076 Uiso 1 1 calc R . . N6 N 0.5099(5) 0.4502(4) 0.2451(2) 0.0602(14) Uani 1 1 d . A . H12 H 0.4760 0.4710 0.2213 0.072 Uiso 1 1 calc R . . F1 F -0.0802(3) 0.3788(3) 0.11398(16) 0.0703(11) Uani 1 1 d . . . F2 F -0.1607(3) 0.4667(3) 0.04737(16) 0.0733(11) Uani 1 1 d . B . F3 F -0.0100(4) 0.6346(3) 0.02643(17) 0.0787(12) Uani 1 1 d . . . F4 F 0.2252(4) 0.7119(4) 0.0702(3) 0.127(2) Uani 1 1 d . B . F5 F 0.3081(4) 0.6236(3) 0.1352(3) 0.120(2) Uani 1 1 d . . . F6 F -0.0159(3) -0.0263(3) 0.13278(15) 0.0668(10) Uani 1 1 d . B . F7 F -0.0374(3) -0.1843(3) 0.05418(15) 0.0684(10) Uani 1 1 d . . . F8 F 0.1534(3) -0.1829(2) 0.00333(14) 0.0610(9) Uani 1 1 d . B . F9 F 0.3657(3) -0.0252(3) 0.03297(14) 0.0607(9) Uani 1 1 d . . . F10 F 0.3841(3) 0.1345(3) 0.10780(15) 0.0664(10) Uani 1 1 d . B . F11 F 0.2528(7) -0.0315(5) 0.3591(3) 0.158(3) Uani 1 1 d . . . F12 F 0.2790(11) -0.0289(7) 0.4686(3) 0.231(5) Uani 1 1 d . . . F13 F 0.4806(8) 0.1042(5) 0.53727(19) 0.163(3) Uani 1 1 d . . . F14 F 0.6564(7) 0.2313(7) 0.4967(2) 0.165(3) Uani 1 1 d . . . F15 F 0.6293(5) 0.2265(5) 0.3874(2) 0.1240(19) Uani 1 1 d . . . F16 F 0.4471(3) -0.1234(3) 0.10728(16) 0.0684(10) Uani 1 1 d . B . F17 F 0.4716(4) -0.2576(3) 0.02690(16) 0.0737(11) Uani 1 1 d . . . F18 F 0.6826(4) -0.2170(3) -0.01350(15) 0.0736(11) Uani 1 1 d . B . F19 F 0.8667(3) -0.0418(3) 0.02680(16) 0.0713(11) Uani 1 1 d . . . F20 F 0.8429(3) 0.0942(3) 0.10642(16) 0.0697(10) Uani 1 1 d . B . F21 F 0.3897(4) 0.3616(4) 0.1167(2) 0.1055(16) Uani 1 1 d . . . F22 F 0.3825(7) 0.4832(7) 0.0535(3) 0.175(3) Uani 1 1 d . B . F23 F 0.5932(9) 0.6334(7) 0.0468(4) 0.213(5) Uani 1 1 d . . . F24 F 0.8029(7) 0.6527(5) 0.1007(4) 0.176(3) Uani 1 1 d . B . F25 F 0.8056(4) 0.5300(3) 0.1638(2) 0.0958(14) Uani 1 1 d . . . C2 C 0.3016(15) 0.6133(11) 0.3040(7) 0.058(4) Uani 0.541(6) 1 d P B 1 C3 C 0.2351(15) 0.5935(14) 0.2535(8) 0.069(5) Uani 0.541(6) 1 d P B 1 S4 S 0.1373(4) 0.6528(3) 0.23847(16) 0.0761(16) Uani 0.541(6) 1 d P B 1 C73 C 0.2431(19) 0.7741(12) 0.2354(10) 0.142(9) Uani 0.541(6) 1 d PD B 1 H13 H 0.3028 0.8025 0.2696 0.170 Uiso 0.541(6) 1 calc PR B 1 H14 H 0.2865 0.7671 0.2036 0.170 Uiso 0.541(6) 1 calc PR B 1 C74 C 0.1851(11) 0.8468(9) 0.2291(7) 0.095(6) Uani 0.541(6) 1 d PD B 1 H50 H 0.2478 0.9098 0.2285 0.142 Uiso 0.541(6) 1 calc PR B 1 H51 H 0.1426 0.8550 0.2605 0.142 Uiso 0.541(6) 1 calc PR B 1 H52 H 0.1286 0.8211 0.1944 0.142 Uiso 0.541(6) 1 calc PR B 1 S3 S 0.3386(5) 0.6977(4) 0.3648(2) 0.0839(15) Uani 0.541(6) 1 d PU B 1 C71 C 0.2275(18) 0.7333(19) 0.3725(10) 0.098(4) Uani 0.541(6) 1 d PDU B 1 H18 H 0.2499 0.7884 0.4054 0.118 Uiso 0.541(6) 1 calc PR B 1 H19 H 0.2075 0.7539 0.3393 0.118 Uiso 0.541(6) 1 calc PR B 1 C72 C 0.122(2) 0.6452(18) 0.3799(9) 0.149(7) Uani 0.541(6) 1 d PDU B 1 H53 H 0.0539 0.6627 0.3862 0.223 Uiso 0.541(6) 1 calc PR B 1 H54 H 0.1443 0.6241 0.4120 0.223 Uiso 0.541(6) 1 calc PR B 1 H55 H 0.0991 0.5922 0.3465 0.223 Uiso 0.541(6) 1 calc PR B 1 C2A C 0.259(2) 0.5706(13) 0.3122(10) 0.072(6) Uani 0.459(6) 1 d P B 2 C3A C 0.1849(14) 0.5599(14) 0.2648(8) 0.053(5) Uani 0.459(6) 1 d P B 2 S3A S 0.2769(7) 0.6482(5) 0.3808(2) 0.0884(19) Uani 0.459(6) 1 d P B 2 C71A C 0.231(6) 0.748(4) 0.362(2) 0.42(7) Uani 0.459(6) 1 d PD B 2 H23 H 0.3036 0.8073 0.3627 0.506 Uiso 0.459(6) 1 calc PR B 2 H24 H 0.1852 0.7244 0.3238 0.506 Uiso 0.459(6) 1 calc PR B 2 C72A C 0.153(3) 0.774(3) 0.4043(17) 0.27(3) Uani 0.459(6) 1 d PD B 2 H56 H 0.1335 0.8262 0.3961 0.411 Uiso 0.459(6) 1 calc PR B 2 H57 H 0.1974 0.7944 0.4420 0.411 Uiso 0.459(6) 1 calc PR B 2 H58 H 0.0788 0.7160 0.4016 0.411 Uiso 0.459(6) 1 calc PR B 2 S4A S 0.0622(4) 0.5875(4) 0.25586(17) 0.0682(16) Uani 0.459(6) 1 d P B 2 C73A C -0.024(2) 0.540(3) 0.3043(12) 0.150(12) Uani 0.459(6) 1 d PD B 2 H28 H -0.0710 0.4692 0.2901 0.181 Uiso 0.459(6) 1 calc PR B 2 H29 H 0.0277 0.5515 0.3394 0.181 Uiso 0.459(6) 1 calc PR B 2 C74A C -0.110(3) 0.595(2) 0.3139(14) 0.200(14) Uani 0.459(6) 1 d PDU B 2 H59 H -0.1557 0.5746 0.3434 0.299 Uiso 0.459(6) 1 calc PR B 2 H60 H -0.1647 0.5782 0.2795 0.299 Uiso 0.459(6) 1 calc PR B 2 H61 H -0.0619 0.6651 0.3247 0.299 Uiso 0.459(6) 1 calc PR B 2 Cl3B Cl 0.9199(5) 0.1433(5) 0.2495(3) 0.123(3) Uani 0.478(6) 1 d P C 5 Cl1B Cl 0.9084(5) 0.3145(6) 0.2256(3) 0.132(3) Uani 0.478(6) 1 d P C 5 Cl12 Cl 0.8138(10) 0.2602(9) 0.3164(3) 0.118(3) Uani 0.478(6) 1 d P C 5 Cl13 Cl 1.0473(7) 0.3305(6) 0.3260(3) 0.107(2) Uani 0.478(6) 1 d P C 5 C87B C 0.9169(17) 0.252(2) 0.2768(10) 0.098(7) Uani 0.478(6) 1 d P C 5 C87 C 0.9431(16) 0.3321(16) 0.2779(7) 0.088(5) Uani 0.522(6) 1 d P C 6 Cl1 Cl 0.834(2) 0.288(2) 0.3294(9) 0.339(15) Uani 0.522(6) 1 d P C 6 Cl3 Cl 0.9119(4) 0.4174(4) 0.2515(2) 0.101(2) Uani 0.522(6) 1 d P C 6 Cl9 Cl 0.9242(5) 0.2331(5) 0.2219(3) 0.121(2) Uani 0.522(6) 1 d P C 6 Cl11 Cl 1.0893(5) 0.3846(5) 0.3140(2) 0.0932(16) Uani 0.522(6) 1 d P C 6 S1 S 0.7188(3) -0.0654(3) 0.22405(10) 0.1413(14) Uani 1 1 d D B . C67 C 0.597(3) -0.2037(17) 0.2167(16) 0.257(16) Uiso 0.610(9) 1 d PD B 7 H74 H 0.5476 -0.1941 0.2453 0.308 Uiso 0.610(9) 1 calc PR B 7 H75 H 0.5466 -0.2165 0.1809 0.308 Uiso 0.610(9) 1 calc PR B 7 C68 C 0.591(3) -0.3044(19) 0.2172(13) 0.221(13) Uiso 0.610(9) 1 d PD B 7 H92 H 0.5077 -0.3521 0.2068 0.332 Uiso 0.610(9) 1 calc PR B 7 H93 H 0.6219 -0.3044 0.2545 0.332 Uiso 0.610(9) 1 calc PR B 7 H94 H 0.6393 -0.3216 0.1906 0.332 Uiso 0.610(9) 1 calc PR B 7 S2 S 0.5585(6) -0.0531(4) 0.3458(3) 0.0814(17) Uani 0.610(9) 1 d P B 7 C69 C 0.719(2) -0.014(2) 0.3701(9) 0.190(9) Uani 0.610(9) 1 d PDU B 7 H38 H 0.7239 -0.0689 0.3836 0.228 Uiso 0.610(9) 1 calc PR B 7 H39 H 0.7559 -0.0136 0.3358 0.228 Uiso 0.610(9) 1 calc PR B 7 C70 C 0.823(2) 0.0911(18) 0.4189(8) 0.180(8) Uani 0.610(9) 1 d PDU B 7 H98 H 0.8982 0.0840 0.4260 0.270 Uiso 0.610(9) 1 calc PR B 7 H99 H 0.7903 0.0987 0.4537 0.270 Uiso 0.610(9) 1 calc PR B 7 H100 H 0.8377 0.1485 0.4041 0.270 Uiso 0.610(9) 1 calc PR B 7 C67A C 0.846(2) 0.013(2) 0.2764(11) 0.118(9) Uiso 0.390(9) 1 d PDU B 8 H82 H 0.9174 -0.0009 0.2693 0.141 Uiso 0.390(9) 1 calc PR B 8 H83 H 0.8657 0.0820 0.2783 0.141 Uiso 0.390(9) 1 calc PR B 8 C68A C 0.803(5) -0.015(5) 0.3294(11) 0.37(4) Uiso 0.390(9) 1 d PDU B 8 H95 H 0.8659 0.0231 0.3611 0.551 Uiso 0.390(9) 1 calc PR B 8 H96 H 0.7822 -0.0846 0.3259 0.551 Uiso 0.390(9) 1 calc PR B 8 H97 H 0.7316 -0.0019 0.3351 0.551 Uiso 0.390(9) 1 calc PR B 8 S2A S 0.609(2) -0.0167(15) 0.3472(6) 0.217(10) Uani 0.390(9) 1 d PD B 8 C69A C 0.575(3) -0.1558(14) 0.3166(8) 0.116(9) Uani 0.390(9) 1 d PDU B 8 H87 H 0.6508 -0.1576 0.3063 0.139 Uiso 0.390(9) 1 calc PR B 8 H88 H 0.5576 -0.1878 0.3478 0.139 Uiso 0.390(9) 1 calc PR B 8 C70A C 0.477(2) -0.222(2) 0.2675(11) 0.130(10) Uiso 0.390(9) 1 d PD B 8 H89 H 0.4201 -0.2771 0.2791 0.196 Uiso 0.390(9) 1 calc PR B 8 H90 H 0.5138 -0.2457 0.2372 0.196 Uiso 0.390(9) 1 calc PR B 8 H91 H 0.4357 -0.1850 0.2546 0.196 Uiso 0.390(9) 1 calc PR B 8 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 0.080(5) 0.106(6) 0.079(6) -0.003(5) -0.009(4) 0.064(5) C4 0.078(5) 0.085(5) 0.046(4) -0.007(4) -0.006(4) 0.051(4) C5 0.065(4) 0.057(4) 0.065(4) -0.001(3) -0.001(3) 0.037(4) C6 0.050(4) 0.083(5) 0.044(4) 0.007(3) -0.004(3) 0.037(4) C7 0.058(4) 0.088(5) 0.050(4) 0.010(4) 0.001(3) 0.041(4) C8 0.052(4) 0.070(4) 0.049(4) 0.003(3) -0.007(3) 0.033(3) C9 0.044(3) 0.078(4) 0.042(4) 0.005(3) 0.003(3) 0.031(3) C10 0.052(4) 0.068(4) 0.044(4) 0.011(3) -0.001(3) 0.035(3) C11 0.051(4) 0.078(4) 0.048(4) 0.008(3) 0.009(3) 0.033(4) C12 0.068(4) 0.084(5) 0.061(4) 0.010(4) 0.008(4) 0.047(4) C13 0.076(5) 0.106(6) 0.033(3) 0.009(4) 0.000(3) 0.054(5) C14 0.067(4) 0.075(4) 0.047(4) 0.017(3) 0.002(3) 0.037(4) C15 0.094(5) 0.099(5) 0.041(4) 0.020(4) 0.014(4) 0.064(5) C16 0.093(5) 0.096(5) 0.057(4) 0.029(4) 0.006(4) 0.064(5) C17 0.132(7) 0.127(7) 0.055(5) 0.030(5) 0.019(5) 0.094(6) C18 0.109(6) 0.117(6) 0.053(4) 0.016(4) 0.012(4) 0.085(6) C19 0.088(5) 0.094(5) 0.047(4) 0.006(4) -0.002(4) 0.058(5) C20 0.060(4) 0.078(4) 0.047(4) 0.015(3) 0.003(3) 0.041(4) C21 0.062(4) 0.078(4) 0.052(4) 0.008(3) 0.005(3) 0.041(4) C22 0.053(4) 0.089(5) 0.053(4) 0.018(4) 0.010(3) 0.034(4) C23 0.058(4) 0.071(4) 0.064(4) 0.023(4) 0.007(3) 0.028(4) C24 0.047(4) 0.084(5) 0.049(4) 0.021(4) -0.004(3) 0.032(4) C25 0.045(3) 0.065(4) 0.060(4) 0.012(3) 0.001(3) 0.027(3) C26 0.056(4) 0.071(4) 0.055(4) 0.012(3) -0.002(3) 0.031(4) C27 0.072(5) 0.085(5) 0.058(4) 0.014(4) -0.003(4) 0.049(4) C28 0.074(5) 0.086(5) 0.050(4) 0.008(4) -0.003(3) 0.046(4) C29 0.067(4) 0.071(4) 0.059(5) -0.005(4) -0.007(3) 0.037(4) C30 0.097(6) 0.109(6) 0.056(5) -0.002(4) -0.011(4) 0.069(5) C31 0.057(4) 0.067(4) 0.074(5) 0.015(4) -0.001(3) 0.037(4) C36 0.058(5) 0.075(5) 0.114(7) 0.026(5) -0.002(4) 0.029(4) C35 0.062(5) 0.085(6) 0.116(7) 0.046(5) 0.004(5) 0.022(4) C34 0.061(5) 0.075(5) 0.084(5) 0.032(4) 0.011(4) 0.036(4) C33 0.045(4) 0.087(5) 0.071(5) 0.029(4) 0.008(3) 0.032(4) C32 0.053(4) 0.066(4) 0.059(4) 0.016(3) 0.008(3) 0.023(3) C37 0.050(4) 0.076(4) 0.037(3) 0.008(3) 0.005(3) 0.035(4) C38 0.054(4) 0.072(4) 0.048(4) 0.020(3) 0.019(3) 0.036(4) C39 0.052(4) 0.071(4) 0.046(4) 0.013(3) 0.001(3) 0.026(4) C40 0.055(4) 0.070(4) 0.043(4) 0.015(3) 0.009(3) 0.035(4) C41 0.045(4) 0.076(4) 0.038(3) 0.017(3) 0.004(3) 0.032(3) C42 0.055(4) 0.069(4) 0.044(4) 0.008(3) -0.004(3) 0.032(4) C43 0.112(6) 0.097(6) 0.043(4) 0.017(4) 0.008(4) 0.069(5) C44 0.168(11) 0.115(8) 0.066(6) 0.041(6) 0.033(7) 0.067(8) C45 0.241(15) 0.157(11) 0.074(7) 0.050(7) 0.067(9) 0.129(11) C46 0.243(15) 0.170(11) 0.063(7) 0.063(7) 0.067(8) 0.152(11) C47 0.207(13) 0.152(10) 0.054(6) 0.002(6) 0.005(7) 0.133(10) C48 0.147(9) 0.132(8) 0.033(4) 0.012(5) -0.001(5) 0.091(8) C49 0.061(4) 0.076(5) 0.055(4) 0.012(3) 0.010(3) 0.042(4) C50 0.053(4) 0.078(5) 0.053(4) 0.020(4) 0.012(3) 0.038(4) C51 0.065(4) 0.063(4) 0.063(5) 0.007(4) 0.000(4) 0.030(4) C52 0.068(5) 0.085(5) 0.057(4) 0.021(4) 0.017(4) 0.050(4) C53 0.048(4) 0.075(5) 0.055(4) 0.018(4) 0.012(3) 0.032(4) C54 0.063(4) 0.078(5) 0.051(4) 0.015(4) 0.008(3) 0.047(4) C55 0.076(5) 0.094(5) 0.075(5) 0.035(4) 0.021(4) 0.059(5) C56 0.081(6) 0.128(7) 0.078(5) 0.048(5) 0.013(4) 0.064(6) C57 0.157(10) 0.232(14) 0.098(7) 0.089(9) 0.050(7) 0.151(11) C58 0.224(15) 0.198(13) 0.160(11) 0.133(10) 0.127(12) 0.166(13) C59 0.130(9) 0.124(8) 0.149(10) 0.082(8) 0.082(8) 0.082(8) C60 0.072(6) 0.098(6) 0.119(7) 0.052(6) 0.038(5) 0.053(5) C61A 0.104(15) 0.103(13) 0.073(13) -0.001(11) 0.009(11) 0.078(11) C62A 0.113(19) 0.099(17) 0.083(16) -0.017(13) 0.011(14) 0.020(15) C63A 0.105(15) 0.088(14) 0.087(15) 0.019(13) 0.011(14) 0.053(12) C64A 0.124(16) 0.112(15) 0.061(13) 0.018(12) 0.015(12) 0.076(13) C65A 0.119(15) 0.125(15) 0.043(11) 0.016(11) 0.015(10) 0.068(13) C66A 0.105(15) 0.110(14) 0.064(12) 0.013(12) 0.006(11) 0.061(12) F26A 0.077(10) 0.110(14) 0.078(8) 0.028(9) 0.022(7) 0.042(9) F27A 0.146(14) 0.146(14) 0.071(7) 0.042(8) 0.035(8) 0.111(12) F28A 0.134(15) 0.115(11) 0.103(13) -0.029(9) -0.038(10) 0.071(11) F29A 0.214(17) 0.188(16) 0.032(7) 0.025(8) 0.009(8) 0.140(15) F30A 0.136(14) 0.103(11) 0.056(11) 0.010(8) -0.030(10) 0.037(10) C61B 0.094(16) 0.140(19) 0.047(11) -0.009(12) -0.032(10) 0.086(15) C62B 0.105(16) 0.130(17) 0.037(9) 0.008(10) 0.008(9) 0.102(15) C63B 0.137(19) 0.143(19) 0.041(10) -0.002(12) 0.007(12) 0.118(16) C64B 0.15(2) 0.115(18) 0.036(13) -0.029(12) -0.038(13) 0.106(16) C65B 0.14(2) 0.112(17) 0.067(14) -0.034(13) -0.023(14) 0.076(16) C66B 0.12(2) 0.13(2) 0.071(18) -0.039(17) -0.050(17) 0.081(18) F26B 0.116(17) 0.112(16) 0.075(9) 0.041(13) 0.043(12) 0.058(13) F27B 0.20(3) 0.24(3) 0.073(10) 0.056(17) 0.037(15) 0.15(3) F28B 0.32(4) 0.21(2) 0.039(10) -0.007(12) -0.028(15) 0.21(3) F29B 0.18(3) 0.26(3) 0.138(19) -0.122(18) -0.076(18) 0.07(2) F30B 0.141(16) 0.155(16) 0.080(13) 0.026(10) -0.042(11) 0.039(13) N1 0.060(3) 0.092(4) 0.047(3) -0.004(3) -0.011(3) 0.045(3) N2 0.067(4) 0.080(4) 0.046(3) 0.003(3) -0.007(3) 0.043(3) N3 0.062(3) 0.081(4) 0.048(3) 0.015(3) 0.002(3) 0.044(3) N4 0.072(4) 0.091(4) 0.043(3) 0.015(3) 0.008(3) 0.052(3) N5 0.069(4) 0.081(4) 0.054(3) 0.012(3) 0.005(3) 0.047(3) N6 0.056(3) 0.072(4) 0.061(4) 0.013(3) -0.004(3) 0.038(3) F1 0.056(2) 0.083(3) 0.077(3) 0.026(2) 0.0045(19) 0.032(2) F2 0.057(2) 0.086(3) 0.077(3) 0.029(2) -0.0077(19) 0.027(2) F3 0.082(3) 0.076(3) 0.084(3) 0.031(2) 0.004(2) 0.034(2) F4 0.070(3) 0.106(4) 0.203(6) 0.080(4) 0.001(3) 0.018(3) F5 0.062(3) 0.090(3) 0.186(6) 0.034(3) -0.035(3) 0.016(3) F6 0.058(2) 0.082(3) 0.064(2) 0.014(2) 0.0140(18) 0.033(2) F7 0.062(2) 0.076(2) 0.065(2) 0.012(2) 0.0108(19) 0.027(2) F8 0.069(2) 0.063(2) 0.054(2) 0.0049(18) 0.0067(18) 0.0348(19) F9 0.054(2) 0.076(2) 0.054(2) 0.0081(18) 0.0059(17) 0.0313(19) F10 0.048(2) 0.080(3) 0.061(2) 0.003(2) 0.0055(17) 0.023(2) F11 0.188(7) 0.164(6) 0.093(4) 0.052(4) 0.053(4) 0.028(5) F12 0.383(14) 0.231(8) 0.124(6) 0.111(6) 0.138(8) 0.125(9) F13 0.326(10) 0.185(6) 0.043(3) 0.036(3) 0.033(4) 0.170(7) F14 0.191(7) 0.244(8) 0.059(3) 0.004(4) -0.020(4) 0.106(6) F15 0.125(4) 0.161(5) 0.062(3) 0.003(3) -0.010(3) 0.047(4) F16 0.058(2) 0.084(3) 0.072(2) 0.022(2) 0.0155(19) 0.035(2) F17 0.076(3) 0.074(3) 0.073(3) 0.012(2) 0.008(2) 0.036(2) F18 0.091(3) 0.088(3) 0.060(2) 0.013(2) 0.014(2) 0.058(2) F19 0.072(3) 0.096(3) 0.068(2) 0.026(2) 0.018(2) 0.054(2) F20 0.052(2) 0.074(3) 0.078(3) 0.008(2) 0.0044(19) 0.026(2) F21 0.065(3) 0.166(5) 0.098(4) 0.040(3) 0.002(2) 0.057(3) F22 0.185(6) 0.338(10) 0.124(5) 0.124(6) 0.043(5) 0.199(7) F23 0.311(10) 0.299(10) 0.241(8) 0.230(8) 0.180(8) 0.249(9) F24 0.194(7) 0.136(5) 0.277(9) 0.136(6) 0.154(7) 0.090(5) F25 0.070(3) 0.084(3) 0.129(4) 0.025(3) 0.028(3) 0.025(2) C2 0.064(11) 0.036(9) 0.071(10) -0.004(8) -0.007(8) 0.028(8) C3 0.037(10) 0.081(12) 0.076(12) 0.007(9) -0.004(8) 0.019(9) S4 0.090(3) 0.083(3) 0.067(2) 0.005(2) -0.011(2) 0.056(3) C73 0.144(18) 0.085(12) 0.18(2) -0.006(13) -0.059(16) 0.063(13) C74 0.052(8) 0.068(8) 0.163(16) 0.065(10) -0.039(9) 0.012(7) S3 0.114(4) 0.092(3) 0.052(2) -0.009(2) -0.019(2) 0.066(3) C71 0.126(8) 0.116(9) 0.065(7) -0.015(7) -0.030(7) 0.086(7) C72 0.175(16) 0.181(16) 0.100(13) -0.017(13) -0.008(12) 0.111(13) C2A 0.097(17) 0.026(10) 0.077(14) -0.008(9) 0.001(12) 0.020(11) C3A 0.016(9) 0.076(13) 0.057(11) 0.003(9) -0.013(7) 0.019(9) S3A 0.132(5) 0.110(5) 0.052(3) 0.004(3) 0.002(3) 0.089(4) C71A 0.87(18) 0.27(6) 0.22(7) -0.08(5) -0.11(8) 0.43(10) C72A 0.25(4) 0.19(3) 0.30(5) -0.05(3) 0.22(4) 0.01(3) S4A 0.076(3) 0.085(3) 0.060(3) 0.013(2) 0.002(2) 0.054(3) C73A 0.119(19) 0.27(4) 0.15(2) 0.09(2) 0.056(17) 0.14(2) C74A 0.19(2) 0.21(2) 0.14(2) 0.049(19) 0.030(19) 0.020(19) Cl3B 0.096(4) 0.145(5) 0.120(5) -0.004(4) -0.004(3) 0.061(4) Cl1B 0.103(4) 0.191(9) 0.127(5) 0.078(6) 0.021(4) 0.069(5) Cl12 0.149(6) 0.246(8) 0.070(3) 0.079(4) 0.055(3) 0.172(6) Cl13 0.102(5) 0.118(5) 0.109(5) 0.015(4) 0.000(3) 0.063(4) C87B 0.074(12) 0.150(19) 0.123(19) 0.091(17) 0.028(11) 0.073(13) C87 0.104(13) 0.131(16) 0.059(10) 0.036(11) 0.016(9) 0.072(13) Cl1 0.31(2) 0.62(4) 0.34(2) 0.34(3) 0.198(19) 0.33(3) Cl3 0.084(3) 0.134(5) 0.099(3) 0.045(3) 0.012(2) 0.051(3) Cl9 0.105(4) 0.131(5) 0.116(5) -0.009(4) -0.005(3) 0.059(3) Cl11 0.087(4) 0.105(4) 0.092(3) 0.015(3) 0.010(3) 0.049(3) S1 0.216(3) 0.239(3) 0.0687(15) 0.0340(18) 0.0221(17) 0.199(3) S2 0.122(3) 0.093(3) 0.048(3) 0.024(2) 0.008(2) 0.060(3) C69 0.213(17) 0.31(2) 0.115(13) 0.116(13) 0.016(11) 0.145(15) C70 0.213(17) 0.266(19) 0.121(12) 0.101(12) 0.092(11) 0.124(14) S2A 0.44(3) 0.36(2) 0.114(10) 0.160(13) 0.162(14) 0.37(2) C69A 0.18(2) 0.117(16) 0.083(14) 0.063(13) 0.028(14) 0.081(16) _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 1.371(9) . ? C1 C30 1.408(10) . ? C1 C2A 1.50(2) . ? C1 C2 1.532(16) . ? C4 N1 1.295(8) . ? C4 C3 1.41(2) . ? C4 C5 1.493(9) . ? C4 C3A 1.535(19) . ? C5 C6 1.335(9) . ? C5 C31 1.449(9) . ? C6 N2 1.414(8) . ? C6 C7 1.458(9) . ? C7 C8 1.373(9) . ? C7 H1 0.9500 . ? C8 C9 1.448(9) . ? C8 H2 0.9500 . ? C9 C10 1.356(8) . ? C9 N2 1.371(8) . ? C10 C11 1.433(8) . ? C10 C37 1.504(8) . ? C11 N3 1.364(8) . ? C11 C12 1.414(9) . ? C12 C13 1.374(9) . ? C12 H3 0.9500 . ? C13 C14 1.373(9) . ? C13 H4 0.9500 . ? C14 N3 1.389(8) . ? C14 C15 1.436(9) . ? C15 C16 1.397(9) . ? C15 C43 1.481(7) . ? C16 N4 1.398(8) . ? C16 C17 1.464(10) . ? C17 C18 1.392(10) . ? C17 S2A 1.664(15) . ? C17 S2 1.819(10) . ? C18 C19 1.426(10) . ? C18 S1 1.745(7) . ? C19 N4 1.306(8) . ? C19 C20 1.503(9) . ? C20 C21 1.362(9) . ? C20 C49 1.463(9) . ? C21 N5 1.377(8) . ? C21 C22 1.473(9) . ? C22 C23 1.341(9) . ? C22 H5 0.9500 . ? C23 C24 1.466(9) . ? C23 H6 0.9500 . ? C24 C25 1.333(9) . ? C24 N5 1.400(8) . ? C25 C26 1.434(9) . ? C25 C55 1.498(9) . ? C26 N6 1.365(8) . ? C26 C27 1.431(9) . ? C27 C28 1.370(9) . ? C27 H7 0.9500 . ? C28 C29 1.372(9) . ? C28 H8 0.9500 . ? C29 N6 1.388(8) . ? C29 C30 1.470(10) . ? C30 C61B 1.462(14) . ? C30 C61A 1.584(16) . ? C31 C32 1.386(9) . ? C31 C36 1.397(10) . ? C36 F5 1.359(8) . ? C36 C35 1.369(11) . ? C35 F4 1.332(8) . ? C35 C34 1.365(10) . ? C34 F3 1.348(7) . ? C34 C33 1.361(9) . ? C33 F2 1.360(7) . ? C33 C32 1.361(9) . ? C32 F1 1.351(7) . ? C37 C38 1.383(9) . ? C37 C42 1.403(8) . ? C38 C39 1.345(9) . ? C38 F6 1.361(6) . ? C39 F7 1.364(7) . ? C39 C40 1.391(8) . ? C40 F8 1.337(7) . ? C40 C41 1.374(9) . ? C41 F9 1.341(6) . ? C41 C42 1.364(9) . ? C42 F10 1.342(7) . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 F11 1.300(9) . ? C44 C45 1.3900 . ? C45 F12 1.325(9) . ? C45 C46 1.3900 . ? C46 F13 1.342(6) . ? C46 C47 1.3900 . ? C47 F14 1.352(9) . ? C47 C48 1.3900 . ? C48 F15 1.297(8) . ? C49 C50 1.395(9) . ? C49 C54 1.404(9) . ? C50 C51 1.338(9) . ? C50 F16 1.372(7) . ? C51 F17 1.365(8) . ? C51 C52 1.378(9) . ? C52 F18 1.347(7) . ? C52 C53 1.358(9) . ? C53 F19 1.361(7) . ? C53 C54 1.367(9) . ? C54 F20 1.319(8) . ? C55 C56 1.385(10) . ? C55 C60 1.373(11) . ? C56 F21 1.341(10) . ? C56 C57 1.378(12) . ? C57 F22 1.349(12) . ? C57 C58 1.448(19) . ? C58 C59 1.333(17) . ? C58 F23 1.358(11) . ? C59 F24 1.309(11) . ? C59 C60 1.379(12) . ? C60 F25 1.325(9) . ? C61A C62A 1.3900 . ? C61A C66A 1.3900 . ? C62A F26A 1.32(2) . ? C62A C63A 1.3900 . ? C63A F27A 1.27(2) . ? C63A C64A 1.3900 . ? C64A F29A 1.35(2) . ? C64A C65A 1.3900 . ? C65A F28A 1.35(2) . ? C65A C66A 1.3900 . ? C66A F30A 1.26(3) . ? C61B C62B 1.3900 . ? C61B C66B 1.3900 . ? C62B F26B 1.28(3) . ? C62B C63B 1.3900 . ? C63B F27B 1.19(3) . ? C63B C64B 1.3900 . ? C64B F28B 1.25(2) . ? C64B C65B 1.3900 . ? C65B F29B 1.32(3) . ? C65B C66B 1.3900 . ? C66B F30B 1.37(3) . ? N2 H9 0.8800 . ? N3 H10 0.8800 . ? N5 H11 0.8800 . ? N6 H12 0.8800 . ? C2 C3 1.37(2) . ? C2 S3 1.690(17) . ? C3 S4 1.826(19) . ? S4 C73 1.83(2) . ? C73 C74 1.564(17) . ? C73 H13 0.9900 . ? C73 H14 0.9900 . ? C74 H50 0.9800 . ? C74 H51 0.9800 . ? C74 H52 0.9800 . ? S3 C71 1.66(2) . ? C71 C72 1.52(2) . ? C71 H18 0.9900 . ? C71 H19 0.9900 . ? C72 H53 0.9800 . ? C72 H54 0.9800 . ? C72 H55 0.9800 . ? C2A C3A 1.38(3) . ? C2A S3A 1.82(2) . ? C3A S4A 1.728(16) . ? S3A C71A 1.96(6) . ? C71A C72A 1.56(3) . ? C71A H23 0.9900 . ? C71A H24 0.9900 . ? C72A H56 0.9800 . ? C72A H57 0.9800 . ? C72A H58 0.9800 . ? S4A C73A 1.73(2) . ? C73A C74A 1.58(3) . ? C73A H28 0.9900 . ? C73A H29 0.9900 . ? C74A H59 0.9800 . ? C74A H60 0.9800 . ? C74A H61 0.9800 . ? Cl3B C87B 1.69(3) . ? Cl1B C87B 1.761(19) . ? Cl12 C87B 1.68(2) . ? Cl13 C87B 1.79(3) . ? C87 Cl3 1.73(2) . ? C87 Cl11 1.752(19) . ? C87 Cl9 1.78(2) . ? C87 Cl1 1.93(2) . ? S1 C67A 1.80(3) . ? S1 C67 2.03(2) . ? C67 C68 1.523(10) . ? C67 H74 0.9900 . ? C67 H75 0.9900 . ? C68 H92 0.9800 . ? C68 H93 0.9800 . ? C68 H94 0.9800 . ? S2 C69 1.84(3) . ? C69 C70 1.77(2) . ? C69 H38 0.9900 . ? C69 H39 0.9900 . ? C70 H98 0.9800 . ? C70 H99 0.9800 . ? C70 H100 0.9800 . ? C67A C68A 1.530(10) . ? C67A H82 0.9900 . ? C67A H83 0.9900 . ? C68A H95 0.9800 . ? C68A H96 0.9800 . ? C68A H97 0.9800 . ? S2A C69A 1.99(2) . ? C69A C70A 1.530(10) . ? C69A H87 0.9900 . ? C69A H88 0.9900 . ? C70A H89 0.9800 . ? C70A H90 0.9800 . ? C70A H91 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C30 120.3(7) . . ? N1 C1 C2A 108.0(11) . . ? C30 C1 C2A 128.1(11) . . ? N1 C1 C2 108.4(9) . . ? C30 C1 C2 130.4(9) . . ? C2A C1 C2 28.2(7) . . ? N1 C4 C3 110.5(9) . . ? N1 C4 C5 119.1(6) . . ? C3 C4 C5 129.8(9) . . ? N1 C4 C3A 112.3(8) . . ? C3 C4 C3A 29.0(7) . . ? C5 C4 C3A 124.0(8) . . ? C6 C5 C31 120.9(6) . . ? C6 C5 C4 118.2(6) . . ? C31 C5 C4 120.8(6) . . ? C5 C6 N2 126.1(6) . . ? C5 C6 C7 130.2(6) . . ? N2 C6 C7 103.7(6) . . ? C8 C7 C6 109.7(6) . . ? C8 C7 H1 125.1 . . ? C6 C7 H1 125.1 . . ? C7 C8 C9 107.9(6) . . ? C7 C8 H2 126.1 . . ? C9 C8 H2 126.1 . . ? C10 C9 N2 125.5(6) . . ? C10 C9 C8 127.9(6) . . ? N2 C9 C8 106.5(5) . . ? C9 C10 C11 124.9(6) . . ? C9 C10 C37 118.7(5) . . ? C11 C10 C37 116.4(5) . . ? N3 C11 C12 105.3(6) . . ? N3 C11 C10 120.8(5) . . ? C12 C11 C10 133.7(6) . . ? C13 C12 C11 108.4(6) . . ? C13 C12 H3 125.8 . . ? C11 C12 H3 125.8 . . ? C12 C13 C14 109.0(6) . . ? C12 C13 H4 125.5 . . ? C14 C13 H4 125.5 . . ? C13 C14 N3 106.3(5) . . ? C13 C14 C15 131.7(6) . . ? N3 C14 C15 122.1(6) . . ? C16 C15 C14 122.2(6) . . ? C16 C15 C43 119.9(6) . . ? C14 C15 C43 117.8(5) . . ? C15 C16 N4 118.2(6) . . ? C15 C16 C17 133.9(6) . . ? N4 C16 C17 107.9(6) . . ? C18 C17 C16 106.1(6) . . ? C18 C17 S2A 126.4(8) . . ? C16 C17 S2A 125.4(7) . . ? C18 C17 S2 132.2(6) . . ? C16 C17 S2 121.1(6) . . ? S2A C17 S2 20.7(9) . . ? C17 C18 C19 105.5(6) . . ? C17 C18 S1 128.9(6) . . ? C19 C18 S1 125.3(6) . . ? N4 C19 C18 113.0(6) . . ? N4 C19 C20 118.6(6) . . ? C18 C19 C20 128.2(6) . . ? C21 C20 C49 121.8(6) . . ? C21 C20 C19 117.6(6) . . ? C49 C20 C19 120.3(6) . . ? C20 C21 N5 126.0(6) . . ? C20 C21 C22 129.3(6) . . ? N5 C21 C22 104.7(6) . . ? C23 C22 C21 108.9(6) . . ? C23 C22 H5 125.5 . . ? C21 C22 H5 125.5 . . ? C22 C23 C24 109.5(6) . . ? C22 C23 H6 125.2 . . ? C24 C23 H6 125.2 . . ? C25 C24 N5 126.0(6) . . ? C25 C24 C23 129.6(6) . . ? N5 C24 C23 104.1(6) . . ? C24 C25 C26 126.0(6) . . ? C24 C25 C55 118.0(6) . . ? C26 C25 C55 115.9(6) . . ? N6 C26 C27 106.0(6) . . ? N6 C26 C25 120.4(6) . . ? C27 C26 C25 133.4(6) . . ? C28 C27 C26 108.2(6) . . ? C28 C27 H7 125.9 . . ? C26 C27 H7 125.9 . . ? C29 C28 C27 108.1(6) . . ? C29 C28 H8 125.9 . . ? C27 C28 H8 125.9 . . ? C28 C29 N6 108.1(6) . . ? C28 C29 C30 131.1(7) . . ? N6 C29 C30 120.7(6) . . ? C1 C30 C29 120.6(7) . . ? C1 C30 C61B 124.6(11) . . ? C29 C30 C61B 114.0(11) . . ? C1 C30 C61A 119.9(12) . . ? C29 C30 C61A 118.7(11) . . ? C61B C30 C61A 18.8(15) . . ? C32 C31 C36 113.7(6) . . ? C32 C31 C5 124.0(6) . . ? C36 C31 C5 122.3(6) . . ? F5 C36 C35 117.5(7) . . ? F5 C36 C31 118.1(7) . . ? C35 C36 C31 124.4(7) . . ? F4 C35 C36 121.1(7) . . ? F4 C35 C34 120.2(7) . . ? C36 C35 C34 118.7(7) . . ? F3 C34 C33 120.3(6) . . ? F3 C34 C35 120.3(6) . . ? C33 C34 C35 119.4(7) . . ? F2 C33 C34 119.1(6) . . ? F2 C33 C32 120.1(6) . . ? C34 C33 C32 120.8(7) . . ? F1 C32 C33 118.8(6) . . ? F1 C32 C31 118.2(6) . . ? C33 C32 C31 123.0(6) . . ? C38 C37 C42 115.1(6) . . ? C38 C37 C10 123.9(5) . . ? C42 C37 C10 121.0(6) . . ? C39 C38 F6 118.8(6) . . ? C39 C38 C37 123.4(5) . . ? F6 C38 C37 117.8(5) . . ? C38 C39 F7 121.3(6) . . ? C38 C39 C40 120.2(6) . . ? F7 C39 C40 118.5(6) . . ? F8 C40 C41 120.7(5) . . ? F8 C40 C39 120.6(6) . . ? C41 C40 C39 118.6(6) . . ? F9 C41 C42 120.7(6) . . ? F9 C41 C40 119.4(6) . . ? C42 C41 C40 120.0(6) . . ? F10 C42 C41 118.7(6) . . ? F10 C42 C37 118.7(6) . . ? C41 C42 C37 122.6(6) . . ? C44 C43 C48 120.0 . . ? C44 C43 C15 119.6(5) . . ? C48 C43 C15 120.3(5) . . ? F11 C44 C45 118.4(5) . . ? F11 C44 C43 121.6(5) . . ? C45 C44 C43 120.0 . . ? F12 C45 C44 122.3(7) . . ? F12 C45 C46 117.5(8) . . ? C44 C45 C46 120.0 . . ? F13 C46 C47 117.7(8) . . ? F13 C46 C45 122.3(7) . . ? C47 C46 C45 120.0 . . ? F14 C47 C46 120.4(6) . . ? F14 C47 C48 119.6(6) . . ? C46 C47 C48 120.0 . . ? F15 C48 C47 119.7(5) . . ? F15 C48 C43 120.3(5) . . ? C47 C48 C43 120.0 . . ? C50 C49 C54 115.1(6) . . ? C50 C49 C20 121.9(6) . . ? C54 C49 C20 123.0(7) . . ? C51 C50 F16 118.6(7) . . ? C51 C50 C49 124.1(6) . . ? F16 C50 C49 117.3(6) . . ? C50 C51 F17 120.8(6) . . ? C50 C51 C52 119.9(7) . . ? F17 C51 C52 119.3(6) . . ? F18 C52 C53 121.6(6) . . ? F18 C52 C51 120.2(7) . . ? C53 C52 C51 118.2(6) . . ? C52 C53 F19 117.9(6) . . ? C52 C53 C54 122.6(6) . . ? F19 C53 C54 119.6(6) . . ? F20 C54 C53 120.0(6) . . ? F20 C54 C49 119.8(6) . . ? C53 C54 C49 120.2(7) . . ? C56 C55 C60 117.2(7) . . ? C56 C55 C25 120.7(7) . . ? C60 C55 C25 122.2(7) . . ? F21 C56 C57 117.8(9) . . ? F21 C56 C55 119.3(7) . . ? C57 C56 C55 122.9(10) . . ? F22 C57 C56 120.6(12) . . ? F22 C57 C58 123.2(10) . . ? C56 C57 C58 116.2(10) . . ? C59 C58 F23 123.3(14) . . ? C59 C58 C57 121.8(9) . . ? F23 C58 C57 114.9(14) . . ? F24 C59 C58 118.7(10) . . ? F24 C59 C60 122.5(12) . . ? C58 C59 C60 118.8(10) . . ? F25 C60 C59 117.2(9) . . ? F25 C60 C55 119.6(7) . . ? C59 C60 C55 123.1(9) . . ? C62A C61A C66A 120.0 . . ? C62A C61A C30 125.0(15) . . ? C66A C61A C30 115.0(15) . . ? F26A C62A C63A 115(2) . . ? F26A C62A C61A 125(2) . . ? C63A C62A C61A 120.0 . . ? F27A C63A C64A 114.8(18) . . ? F27A C63A C62A 125.1(18) . . ? C64A C63A C62A 120.0 . . ? F29A C64A C63A 124.1(16) . . ? F29A C64A C65A 115.9(16) . . ? C63A C64A C65A 120.0 . . ? F28A C65A C64A 121.4(15) . . ? F28A C65A C66A 118.2(15) . . ? C64A C65A C66A 120.0 . . ? F30A C66A C65A 120.7(18) . . ? F30A C66A C61A 119.3(18) . . ? C65A C66A C61A 120.0 . . ? C62B C61B C66B 120.0 . . ? C62B C61B C30 114.8(13) . . ? C66B C61B C30 125.2(13) . . ? F26B C62B C63B 123.2(16) . . ? F26B C62B C61B 116.8(16) . . ? C63B C62B C61B 120.0 . . ? F27B C63B C62B 122.4(19) . . ? F27B C63B C64B 117.6(19) . . ? C62B C63B C64B 120.0 . . ? F28B C64B C65B 122(2) . . ? F28B C64B C63B 118(2) . . ? C65B C64B C63B 120.0 . . ? F29B C65B C66B 123.5(19) . . ? F29B C65B C64B 116(2) . . ? C66B C65B C64B 120.0 . . ? F30B C66B C65B 116.9(17) . . ? F30B C66B C61B 122.6(16) . . ? C65B C66B C61B 120.0 . . ? C4 N1 C1 107.6(6) . . ? C9 N2 C6 112.0(5) . . ? C9 N2 H9 124.0 . . ? C6 N2 H9 124.0 . . ? C11 N3 C14 111.0(5) . . ? C11 N3 H10 124.5 . . ? C14 N3 H10 124.5 . . ? C19 N4 C16 107.4(5) . . ? C21 N5 C24 112.5(5) . . ? C21 N5 H11 123.7 . . ? C24 N5 H11 123.7 . . ? C26 N6 C29 109.4(5) . . ? C26 N6 H12 125.3 . . ? C29 N6 H12 125.3 . . ? C3 C2 C1 101.1(13) . . ? C3 C2 S3 136.6(13) . . ? C1 C2 S3 122.2(11) . . ? C2 C3 C4 109.8(15) . . ? C2 C3 S4 124.4(14) . . ? C4 C3 S4 124.4(12) . . ? C73 S4 C3 103.0(8) . . ? C74 C73 S4 114.8(13) . . ? C74 C73 H13 108.6 . . ? S4 C73 H13 108.6 . . ? C74 C73 H14 108.6 . . ? S4 C73 H14 108.6 . . ? H13 C73 H14 107.5 . . ? C73 C74 H50 109.5 . . ? C73 C74 H51 109.5 . . ? H50 C74 H51 109.5 . . ? C73 C74 H52 109.5 . . ? H50 C74 H52 109.5 . . ? H51 C74 H52 109.5 . . ? C71 S3 C2 108.2(10) . . ? C72 C71 S3 105.7(19) . . ? C72 C71 H18 110.6 . . ? S3 C71 H18 110.6 . . ? C72 C71 H19 110.6 . . ? S3 C71 H19 110.6 . . ? H18 C71 H19 108.7 . . ? C71 C72 H53 109.5 . . ? C71 C72 H54 109.5 . . ? H53 C72 H54 109.5 . . ? C71 C72 H55 109.5 . . ? H53 C72 H55 109.5 . . ? H54 C72 H55 109.5 . . ? C3A C2A C1 106.9(16) . . ? C3A C2A S3A 127.3(16) . . ? C1 C2A S3A 122.7(16) . . ? C2A C3A C4 102.2(14) . . ? C2A C3A S4A 131.3(16) . . ? C4 C3A S4A 126.3(12) . . ? C2A S3A C71A 101.2(18) . . ? C72A C71A S3A 109(4) . . ? C72A C71A H23 109.8 . . ? S3A C71A H23 109.8 . . ? C72A C71A H24 109.8 . . ? S3A C71A H24 109.8 . . ? H23 C71A H24 108.2 . . ? C71A C72A H56 109.5 . . ? C71A C72A H57 109.5 . . ? H56 C72A H57 109.5 . . ? C71A C72A H58 109.5 . . ? H56 C72A H58 109.5 . . ? H57 C72A H58 109.5 . . ? C73A S4A C3A 104.0(10) . . ? C74A C73A S4A 106.1(19) . . ? C74A C73A H28 110.5 . . ? S4A C73A H28 110.5 . . ? C74A C73A H29 110.5 . . ? S4A C73A H29 110.5 . . ? H28 C73A H29 108.7 . . ? C73A C74A H59 109.5 . . ? C73A C74A H60 109.5 . . ? H59 C74A H60 109.5 . . ? C73A C74A H61 109.5 . . ? H59 C74A H61 109.5 . . ? H60 C74A H61 109.5 . . ? Cl12 C87B Cl3B 120.9(14) . . ? Cl12 C87B Cl1B 105.3(10) . . ? Cl3B C87B Cl1B 112.1(15) . . ? Cl12 C87B Cl13 98.1(14) . . ? Cl3B C87B Cl13 112.2(9) . . ? Cl1B C87B Cl13 106.8(13) . . ? Cl3 C87 Cl11 110.1(12) . . ? Cl3 C87 Cl9 108.4(10) . . ? Cl11 C87 Cl9 110.8(9) . . ? Cl3 C87 Cl1 109.0(10) . . ? Cl11 C87 Cl1 108.3(11) . . ? Cl9 C87 Cl1 110.3(14) . . ? C18 S1 C67A 101.3(9) . . ? C18 S1 C67 95.5(10) . . ? C67A S1 C67 131.1(14) . . ? C68 C67 S1 141(3) . . ? C68 C67 H74 101.9 . . ? S1 C67 H74 101.9 . . ? C68 C67 H75 101.9 . . ? S1 C67 H75 101.9 . . ? H74 C67 H75 104.7 . . ? C67 C68 H92 109.5 . . ? C67 C68 H93 109.5 . . ? H92 C68 H93 109.5 . . ? C67 C68 H94 109.5 . . ? H92 C68 H94 109.5 . . ? H93 C68 H94 109.5 . . ? C69 S2 C17 99.6(8) . . ? C70 C69 S2 131.3(19) . . ? C70 C69 H38 104.4 . . ? S2 C69 H38 104.4 . . ? C70 C69 H39 104.4 . . ? S2 C69 H39 104.4 . . ? H38 C69 H39 105.6 . . ? C69 C70 H98 109.5 . . ? C69 C70 H99 109.5 . . ? H98 C70 H99 109.5 . . ? C69 C70 H100 109.5 . . ? H98 C70 H100 109.5 . . ? H99 C70 H100 109.5 . . ? C68A C67A S1 102(2) . . ? C68A C67A H82 111.3 . . ? S1 C67A H82 111.3 . . ? C68A C67A H83 111.3 . . ? S1 C67A H83 111.3 . . ? H82 C67A H83 109.2 . . ? C67A C68A H95 109.5 . . ? C67A C68A H96 109.5 . . ? H95 C68A H96 109.5 . . ? C67A C68A H97 109.5 . . ? H95 C68A H97 109.5 . . ? H96 C68A H97 109.5 . . ? C17 S2A C69A 94.3(11) . . ? C70A C69A S2A 123.6(18) . . ? C70A C69A H87 106.4 . . ? S2A C69A H87 106.4 . . ? C70A C69A H88 106.4 . . ? S2A C69A H88 106.4 . . ? H87 C69A H88 106.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C4 C5 C6 28.4(10) . . . . ? C3 C4 C5 C6 -161.3(11) . . . . ? C3A C4 C5 C6 -125.5(12) . . . . ? N1 C4 C5 C31 -148.8(7) . . . . ? C3 C4 C5 C31 21.5(14) . . . . ? C3A C4 C5 C31 57.3(13) . . . . ? C31 C5 C6 N2 -175.8(6) . . . . ? C4 C5 C6 N2 7.0(10) . . . . ? C31 C5 C6 C7 4.8(11) . . . . ? C4 C5 C6 C7 -172.4(6) . . . . ? C5 C6 C7 C8 176.5(7) . . . . ? N2 C6 C7 C8 -3.0(7) . . . . ? C6 C7 C8 C9 0.9(7) . . . . ? C7 C8 C9 C10 -175.1(6) . . . . ? C7 C8 C9 N2 1.6(7) . . . . ? N2 C9 C10 C11 6.8(10) . . . . ? C8 C9 C10 C11 -177.1(6) . . . . ? N2 C9 C10 C37 -171.8(5) . . . . ? C8 C9 C10 C37 4.4(10) . . . . ? C9 C10 C11 N3 -156.0(6) . . . . ? C37 C10 C11 N3 22.6(9) . . . . ? C9 C10 C11 C12 29.2(12) . . . . ? C37 C10 C11 C12 -152.2(7) . . . . ? N3 C11 C12 C13 -0.5(8) . . . . ? C10 C11 C12 C13 174.8(7) . . . . ? C11 C12 C13 C14 1.4(9) . . . . ? C12 C13 C14 N3 -1.7(8) . . . . ? C12 C13 C14 C15 177.4(8) . . . . ? C13 C14 C15 C16 -163.0(8) . . . . ? N3 C14 C15 C16 16.1(11) . . . . ? C13 C14 C15 C43 13.3(12) . . . . ? N3 C14 C15 C43 -167.7(6) . . . . ? C14 C15 C16 N4 12.3(12) . . . . ? C43 C15 C16 N4 -163.8(7) . . . . ? C14 C15 C16 C17 -167.6(9) . . . . ? C43 C15 C16 C17 16.3(14) . . . . ? C15 C16 C17 C18 -179.5(9) . . . . ? N4 C16 C17 C18 0.6(10) . . . . ? C15 C16 C17 S2A -15.2(19) . . . . ? N4 C16 C17 S2A 164.8(13) . . . . ? C15 C16 C17 S2 9.1(14) . . . . ? N4 C16 C17 S2 -170.9(6) . . . . ? C16 C17 C18 C19 1.8(10) . . . . ? S2A C17 C18 C19 -162.3(12) . . . . ? S2 C17 C18 C19 171.9(8) . . . . ? C16 C17 C18 S1 175.7(7) . . . . ? S2A C17 C18 S1 11.6(18) . . . . ? S2 C17 C18 S1 -14.2(15) . . . . ? C17 C18 C19 N4 -3.9(10) . . . . ? S1 C18 C19 N4 -178.1(7) . . . . ? C17 C18 C19 C20 170.7(8) . . . . ? S1 C18 C19 C20 -3.5(13) . . . . ? N4 C19 C20 C21 29.6(10) . . . . ? C18 C19 C20 C21 -144.7(8) . . . . ? N4 C19 C20 C49 -144.4(7) . . . . ? C18 C19 C20 C49 41.3(11) . . . . ? C49 C20 C21 N5 -179.9(6) . . . . ? C19 C20 C21 N5 6.2(10) . . . . ? C49 C20 C21 C22 1.6(11) . . . . ? C19 C20 C21 C22 -172.3(6) . . . . ? C20 C21 C22 C23 175.4(7) . . . . ? N5 C21 C22 C23 -3.3(7) . . . . ? C21 C22 C23 C24 1.4(8) . . . . ? C22 C23 C24 C25 -173.2(7) . . . . ? C22 C23 C24 N5 1.1(7) . . . . ? N5 C24 C25 C26 8.4(11) . . . . ? C23 C24 C25 C26 -178.5(6) . . . . ? N5 C24 C25 C55 -174.2(6) . . . . ? C23 C24 C25 C55 -1.1(11) . . . . ? C24 C25 C26 N6 -157.1(6) . . . . ? C55 C25 C26 N6 25.5(9) . . . . ? C24 C25 C26 C27 30.1(12) . . . . ? C55 C25 C26 C27 -147.4(8) . . . . ? N6 C26 C27 C28 -0.7(8) . . . . ? C25 C26 C27 C28 172.9(7) . . . . ? C26 C27 C28 C29 2.6(9) . . . . ? C27 C28 C29 N6 -3.5(8) . . . . ? C27 C28 C29 C30 179.0(8) . . . . ? N1 C1 C30 C29 9.8(13) . . . . ? C2A C1 C30 C29 165.7(12) . . . . ? C2 C1 C30 C29 -157.7(11) . . . . ? N1 C1 C30 C61B 178.9(15) . . . . ? C2A C1 C30 C61B -25(2) . . . . ? C2 C1 C30 C61B 11(2) . . . . ? N1 C1 C30 C61A -159.5(13) . . . . ? C2A C1 C30 C61A -3.6(19) . . . . ? C2 C1 C30 C61A 33.0(19) . . . . ? C28 C29 C30 C1 -164.1(9) . . . . ? N6 C29 C30 C1 18.7(12) . . . . ? C28 C29 C30 C61B 25.8(17) . . . . ? N6 C29 C30 C61B -151.4(14) . . . . ? C28 C29 C30 C61A 5.4(17) . . . . ? N6 C29 C30 C61A -171.8(12) . . . . ? C6 C5 C31 C32 56.6(10) . . . . ? C4 C5 C31 C32 -126.2(8) . . . . ? C6 C5 C31 C36 -124.6(8) . . . . ? C4 C5 C31 C36 52.5(10) . . . . ? C32 C31 C36 F5 -179.2(7) . . . . ? C5 C31 C36 F5 1.9(12) . . . . ? C32 C31 C36 C35 0.1(12) . . . . ? C5 C31 C36 C35 -178.8(8) . . . . ? F5 C36 C35 F4 0.8(14) . . . . ? C31 C36 C35 F4 -178.5(8) . . . . ? F5 C36 C35 C34 178.4(8) . . . . ? C31 C36 C35 C34 -0.9(14) . . . . ? F4 C35 C34 F3 -1.7(13) . . . . ? C36 C35 C34 F3 -179.3(8) . . . . ? F4 C35 C34 C33 178.6(8) . . . . ? C36 C35 C34 C33 1.0(13) . . . . ? F3 C34 C33 F2 1.1(11) . . . . ? C35 C34 C33 F2 -179.2(7) . . . . ? F3 C34 C33 C32 -180.0(6) . . . . ? C35 C34 C33 C32 -0.3(12) . . . . ? F2 C33 C32 F1 -1.5(10) . . . . ? C34 C33 C32 F1 179.6(6) . . . . ? F2 C33 C32 C31 178.3(6) . . . . ? C34 C33 C32 C31 -0.6(11) . . . . ? C36 C31 C32 F1 -179.5(6) . . . . ? C5 C31 C32 F1 -0.6(10) . . . . ? C36 C31 C32 C33 0.7(11) . . . . ? C5 C31 C32 C33 179.6(7) . . . . ? C9 C10 C37 C38 -85.0(8) . . . . ? C11 C10 C37 C38 96.4(7) . . . . ? C9 C10 C37 C42 94.0(7) . . . . ? C11 C10 C37 C42 -84.7(7) . . . . ? C42 C37 C38 C39 -1.9(9) . . . . ? C10 C37 C38 C39 177.0(6) . . . . ? C42 C37 C38 F6 -179.8(5) . . . . ? C10 C37 C38 F6 -0.8(9) . . . . ? F6 C38 C39 F7 0.4(9) . . . . ? C37 C38 C39 F7 -177.4(6) . . . . ? F6 C38 C39 C40 179.5(5) . . . . ? C37 C38 C39 C40 1.7(10) . . . . ? C38 C39 C40 F8 -178.6(5) . . . . ? F7 C39 C40 F8 0.6(9) . . . . ? C38 C39 C40 C41 0.2(9) . . . . ? F7 C39 C40 C41 179.4(5) . . . . ? F8 C40 C41 F9 -2.1(8) . . . . ? C39 C40 C41 F9 179.1(5) . . . . ? F8 C40 C41 C42 177.0(5) . . . . ? C39 C40 C41 C42 -1.8(9) . . . . ? F9 C41 C42 F10 1.8(8) . . . . ? C40 C41 C42 F10 -177.3(5) . . . . ? F9 C41 C42 C37 -179.4(5) . . . . ? C40 C41 C42 C37 1.5(9) . . . . ? C38 C37 C42 F10 179.1(5) . . . . ? C10 C37 C42 F10 0.1(8) . . . . ? C38 C37 C42 C41 0.3(9) . . . . ? C10 C37 C42 C41 -178.7(5) . . . . ? C16 C15 C43 C44 -108.2(7) . . . . ? C14 C15 C43 C44 75.5(7) . . . . ? C16 C15 C43 C48 69.1(8) . . . . ? C14 C15 C43 C48 -107.2(7) . . . . ? C48 C43 C44 F11 -176.6(8) . . . . ? C15 C43 C44 F11 0.7(8) . . . . ? C48 C43 C44 C45 0.0 . . . . ? C15 C43 C44 C45 177.3(5) . . . . ? F11 C44 C45 F12 2.2(8) . . . . ? C43 C44 C45 F12 -174.5(8) . . . . ? F11 C44 C45 C46 176.7(8) . . . . ? C43 C44 C45 C46 0.0 . . . . ? F12 C45 C46 F13 -3.1(8) . . . . ? C44 C45 C46 F13 -177.9(6) . . . . ? F12 C45 C46 C47 174.8(8) . . . . ? C44 C45 C46 C47 0.0 . . . . ? F13 C46 C47 F14 -2.8(7) . . . . ? C45 C46 C47 F14 179.2(7) . . . . ? F13 C46 C47 C48 177.9(6) . . . . ? C45 C46 C47 C48 0.0 . . . . ? F14 C47 C48 F15 -1.0(7) . . . . ? C46 C47 C48 F15 178.2(6) . . . . ? F14 C47 C48 C43 -179.2(7) . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 F15 -178.2(6) . . . . ? C15 C43 C48 F15 4.5(7) . . . . ? C44 C43 C48 C47 0.0 . . . . ? C15 C43 C48 C47 -177.3(5) . . . . ? C21 C20 C49 C50 -118.2(8) . . . . ? C19 C20 C49 C50 55.6(9) . . . . ? C21 C20 C49 C54 59.0(9) . . . . ? C19 C20 C49 C54 -127.3(7) . . . . ? C54 C49 C50 C51 -0.4(10) . . . . ? C20 C49 C50 C51 177.0(6) . . . . ? C54 C49 C50 F16 -179.8(5) . . . . ? C20 C49 C50 F16 -2.5(9) . . . . ? F16 C50 C51 F17 0.7(9) . . . . ? C49 C50 C51 F17 -178.8(6) . . . . ? F16 C50 C51 C52 -179.6(6) . . . . ? C49 C50 C51 C52 0.9(10) . . . . ? C50 C51 C52 F18 -178.7(6) . . . . ? F17 C51 C52 F18 1.0(9) . . . . ? C50 C51 C52 C53 -1.1(10) . . . . ? F17 C51 C52 C53 178.6(6) . . . . ? F18 C52 C53 F19 -1.6(9) . . . . ? C51 C52 C53 F19 -179.1(6) . . . . ? F18 C52 C53 C54 178.4(6) . . . . ? C51 C52 C53 C54 0.9(10) . . . . ? C52 C53 C54 F20 -179.8(6) . . . . ? F19 C53 C54 F20 0.2(9) . . . . ? C52 C53 C54 C49 -0.4(10) . . . . ? F19 C53 C54 C49 179.6(5) . . . . ? C50 C49 C54 F20 179.5(5) . . . . ? C20 C49 C54 F20 2.2(9) . . . . ? C50 C49 C54 C53 0.1(9) . . . . ? C20 C49 C54 C53 -177.2(6) . . . . ? C24 C25 C55 C56 97.3(8) . . . . ? C26 C25 C55 C56 -85.1(9) . . . . ? C24 C25 C55 C60 -82.5(9) . . . . ? C26 C25 C55 C60 95.1(8) . . . . ? C60 C55 C56 F21 179.7(7) . . . . ? C25 C55 C56 F21 -0.1(12) . . . . ? C60 C55 C56 C57 -0.2(13) . . . . ? C25 C55 C56 C57 -180.0(8) . . . . ? F21 C56 C57 F22 -1.0(14) . . . . ? C55 C56 C57 F22 178.9(8) . . . . ? F21 C56 C57 C58 -179.0(9) . . . . ? C55 C56 C57 C58 0.9(15) . . . . ? F22 C57 C58 C59 -177.8(11) . . . . ? C56 C57 C58 C59 0.1(18) . . . . ? F22 C57 C58 F23 2.6(17) . . . . ? C56 C57 C58 F23 -179.5(9) . . . . ? F23 C58 C59 F24 -0.3(19) . . . . ? C57 C58 C59 F24 -179.9(10) . . . . ? F23 C58 C59 C60 177.8(10) . . . . ? C57 C58 C59 C60 -1.7(19) . . . . ? F24 C59 C60 F25 -1.7(15) . . . . ? C58 C59 C60 F25 -179.8(10) . . . . ? F24 C59 C60 C55 -179.4(9) . . . . ? C58 C59 C60 C55 2.5(16) . . . . ? C56 C55 C60 F25 -179.2(7) . . . . ? C25 C55 C60 F25 0.6(12) . . . . ? C56 C55 C60 C59 -1.5(13) . . . . ? C25 C55 C60 C59 178.2(8) . . . . ? C1 C30 C61A C62A 72.3(19) . . . . ? C29 C30 C61A C62A -97.2(16) . . . . ? C61B C30 C61A C62A -178(7) . . . . ? C1 C30 C61A C66A -108.5(14) . . . . ? C29 C30 C61A C66A 81.9(15) . . . . ? C61B C30 C61A C66A 2(5) . . . . ? C66A C61A C62A F26A -172(3) . . . . ? C30 C61A C62A F26A 7(2) . . . . ? C66A C61A C62A C63A 0.0 . . . . ? C30 C61A C62A C63A 179(2) . . . . ? F26A C62A C63A F27A -4(2) . . . . ? C61A C62A C63A F27A -177(2) . . . . ? F26A C62A C63A C64A 173(2) . . . . ? C61A C62A C63A C64A 0.0 . . . . ? F27A C63A C64A F29A -4(2) . . . . ? C62A C63A C64A F29A 179(2) . . . . ? F27A C63A C64A C65A 177(2) . . . . ? C62A C63A C64A C65A 0.0 . . . . ? F29A C64A C65A F28A -7(2) . . . . ? C63A C64A C65A F28A 172(2) . . . . ? F29A C64A C65A C66A -179.4(19) . . . . ? C63A C64A C65A C66A 0.0 . . . . ? F28A C65A C66A F30A 6(2) . . . . ? C64A C65A C66A F30A 179(3) . . . . ? F28A C65A C66A C61A -173(2) . . . . ? C64A C65A C66A C61A 0.0 . . . . ? C62A C61A C66A F30A -179(3) . . . . ? C30 C61A C66A F30A 2(2) . . . . ? C62A C61A C66A C65A 0.0 . . . . ? C30 C61A C66A C65A -179.2(19) . . . . ? C1 C30 C61B C62B 81.2(18) . . . . ? C29 C30 C61B C62B -109.0(14) . . . . ? C61A C30 C61B C62B 0(5) . . . . ? C1 C30 C61B C66B -96.9(14) . . . . ? C29 C30 C61B C66B 72.8(14) . . . . ? C61A C30 C61B C66B -178(6) . . . . ? C66B C61B C62B F26B -179.4(18) . . . . ? C30 C61B C62B F26B 2(2) . . . . ? C66B C61B C62B C63B 0.0 . . . . ? C30 C61B C62B C63B -178.2(18) . . . . ? F26B C62B C63B F27B -3(3) . . . . ? C61B C62B C63B F27B 178(2) . . . . ? F26B C62B C63B C64B 179(2) . . . . ? C61B C62B C63B C64B 0.0 . . . . ? F27B C63B C64B F28B 2(2) . . . . ? C62B C63B C64B F28B -179.4(19) . . . . ? F27B C63B C64B C65B -178(2) . . . . ? C62B C63B C64B C65B 0.0 . . . . ? F28B C64B C65B F29B 5(3) . . . . ? C63B C64B C65B F29B -174(2) . . . . ? F28B C64B C65B C66B 179(2) . . . . ? C63B C64B C65B C66B 0.0 . . . . ? F29B C65B C66B F30B -13(3) . . . . ? C64B C65B C66B F30B 173(3) . . . . ? F29B C65B C66B C61B 174(2) . . . . ? C64B C65B C66B C61B 0.0 . . . . ? C62B C61B C66B F30B -172(3) . . . . ? C30 C61B C66B F30B 6(2) . . . . ? C62B C61B C66B C65B 0.0 . . . . ? C30 C61B C66B C65B 178(2) . . . . ? C3 C4 N1 C1 16.7(11) . . . . ? C5 C4 N1 C1 -171.2(7) . . . . ? C3A C4 N1 C1 -14.4(12) . . . . ? C30 C1 N1 C4 178.0(8) . . . . ? C2A C1 N1 C4 17.8(12) . . . . ? C2 C1 N1 C4 -11.9(11) . . . . ? C10 C9 N2 C6 173.1(6) . . . . ? C8 C9 N2 C6 -3.7(7) . . . . ? C5 C6 N2 C9 -175.4(6) . . . . ? C7 C6 N2 C9 4.2(7) . . . . ? C12 C11 N3 C14 -0.6(7) . . . . ? C10 C11 N3 C14 -176.6(6) . . . . ? C13 C14 N3 C11 1.4(8) . . . . ? C15 C14 N3 C11 -177.8(6) . . . . ? C18 C19 N4 C16 4.3(9) . . . . ? C20 C19 N4 C16 -170.9(6) . . . . ? C15 C16 N4 C19 177.1(7) . . . . ? C17 C16 N4 C19 -2.9(9) . . . . ? C20 C21 N5 C24 -174.7(6) . . . . ? C22 C21 N5 C24 4.1(7) . . . . ? C25 C24 N5 C21 171.2(6) . . . . ? C23 C24 N5 C21 -3.3(7) . . . . ? C27 C26 N6 C29 -1.4(7) . . . . ? C25 C26 N6 C29 -176.1(6) . . . . ? C28 C29 N6 C26 3.1(8) . . . . ? C30 C29 N6 C26 -179.1(7) . . . . ? N1 C1 C2 C3 2.5(15) . . . . ? C30 C1 C2 C3 171.2(12) . . . . ? C2A C1 C2 C3 -92(3) . . . . ? N1 C1 C2 S3 -174.4(10) . . . . ? C30 C1 C2 S3 -6(2) . . . . ? C2A C1 C2 S3 91(3) . . . . ? C1 C2 C3 C4 7.1(17) . . . . ? S3 C2 C3 C4 -176.6(14) . . . . ? C1 C2 C3 S4 173.9(11) . . . . ? S3 C2 C3 S4 -10(3) . . . . ? N1 C4 C3 C2 -15.6(17) . . . . ? C5 C4 C3 C2 173.5(11) . . . . ? C3A C4 C3 C2 84(3) . . . . ? N1 C4 C3 S4 177.6(10) . . . . ? C5 C4 C3 S4 7(2) . . . . ? C3A C4 C3 S4 -83(2) . . . . ? C2 C3 S4 C73 74.2(18) . . . . ? C4 C3 S4 C73 -120.9(15) . . . . ? C3 S4 C73 C74 -173.8(15) . . . . ? C3 C2 S3 C71 30(2) . . . . ? C1 C2 S3 C71 -154.2(15) . . . . ? C2 S3 C71 C72 67.1(16) . . . . ? N1 C1 C2A C3A -14.8(17) . . . . ? C30 C1 C2A C3A -173.0(13) . . . . ? C2 C1 C2A C3A 81(3) . . . . ? N1 C1 C2A S3A -176.3(11) . . . . ? C30 C1 C2A S3A 26(2) . . . . ? C2 C1 C2A S3A -81(3) . . . . ? C1 C2A C3A C4 6.0(18) . . . . ? S3A C2A C3A C4 166.3(14) . . . . ? C1 C2A C3A S4A -178.8(14) . . . . ? S3A C2A C3A S4A -18(3) . . . . ? N1 C4 C3A C2A 4.8(17) . . . . ? C3 C4 C3A C2A -88(2) . . . . ? C5 C4 C3A C2A 160.3(12) . . . . ? N1 C4 C3A S4A -170.7(11) . . . . ? C3 C4 C3A S4A 97(3) . . . . ? C5 C4 C3A S4A -15(2) . . . . ? C3A C2A S3A C71A -25(3) . . . . ? C1 C2A S3A C71A 132(2) . . . . ? C2A S3A C71A C72A 139(4) . . . . ? C2A C3A S4A C73A -47(2) . . . . ? C4 C3A S4A C73A 127.2(18) . . . . ? C3A S4A C73A C74A 160(2) . . . . ? C17 C18 S1 C67A -62.3(13) . . . . ? C19 C18 S1 C67A 110.4(11) . . . . ? C17 C18 S1 C67 71.5(14) . . . . ? C19 C18 S1 C67 -115.7(13) . . . . ? C18 S1 C67 C68 -162(4) . . . . ? C67A S1 C67 C68 -52(5) . . . . ? C18 C17 S2 C69 59.1(14) . . . . ? C16 C17 S2 C69 -132.0(12) . . . . ? S2A C17 S2 C69 -23.4(18) . . . . ? C17 S2 C69 C70 91.2(18) . . . . ? C18 S1 C67A C68A 72(4) . . . . ? C67 S1 C67A C68A -35(4) . . . . ? C18 C17 S2A C69A -59.7(17) . . . . ? C16 C17 S2A C69A 139.1(12) . . . . ? S2 C17 S2A C69A 54.3(18) . . . . ? C17 S2A C69A C70A -31(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H9 N1 0.88 2.20 2.681(8) 113.8 . N3 H10 N4 0.88 2.13 2.642(7) 116.1 . N5 H11 N4 0.88 2.19 2.679(8) 114.9 . N6 H12 N1 0.88 2.13 2.644(7) 116.4 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.927 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.105 # 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 0.011 0.500 520 148 ' ' _platon_squeeze_details ; ; data_0318hi _database_code_depnum_ccdc_archive 'CCDC 906721' #TrackingRef 'S_30-ChemSci.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H34 F30 N6 S4, 0.89(C2 H4 Cl4)' _chemical_formula_sum 'C75.78 H37.56 Cl3.56 F30 N6 S4' _chemical_formula_weight 1856.48 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.1330(8) _cell_length_b 7.8286(5) _cell_length_c 29.8370(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.318(3) _cell_angle_gamma 90.00 _cell_volume 3681.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 2017 _cell_measurement_theta_min 4.81 _cell_measurement_theta_max 72.20 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1858 _exptl_absorpt_coefficient_mu 3.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4176 _exptl_absorpt_correction_T_max 0.8434 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38255 _diffrn_reflns_av_R_equivalents 0.1210 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 68.24 _reflns_number_total 6708 _reflns_number_gt 2933 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 6708 _refine_ls_number_parameters 819 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1485 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.1805 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.6830(5) 0.5570(7) 0.04687(19) 0.0880(17) Uani 1 1 d . . . C2 C 0.6010(4) 0.6285(6) 0.03460(17) 0.0764(14) Uani 1 1 d . B . C3 C 0.5532(4) 0.5659(6) 0.06516(18) 0.0794(15) Uani 1 1 d . . . C4 C 0.6061(4) 0.4521(7) 0.09697(19) 0.0887(17) Uani 1 1 d . B . C5 C 0.5982(5) 0.3613(7) 0.13691(19) 0.0851(16) Uani 1 1 d . . . C6 C 0.5237(5) 0.3088(7) 0.1499(2) 0.0931(18) Uani 1 1 d . B . C7 C 0.5126(5) 0.2670(7) 0.1945(2) 0.099(2) Uani 1 1 d . . . H1 H 0.5565 0.2590 0.2212 0.119 Uiso 1 1 calc R B . C8 C 0.4287(6) 0.2402(7) 0.1927(2) 0.102(2) Uani 1 1 d . B . H2 H 0.4045 0.2130 0.2181 0.123 Uiso 1 1 calc R . . C9 C 0.3835(5) 0.2590(7) 0.1472(2) 0.0961(19) Uani 1 1 d . . . C10 C 0.2974(5) 0.2485(8) 0.1292(2) 0.100(2) Uani 1 1 d . A . C11A C 0.2668(8) 0.3095(19) 0.0889(5) 0.084(4) Uani 0.555(2) 1 d P A 1 C12A C 0.1831(9) 0.288(2) 0.0691(5) 0.093(4) Uani 0.555(2) 1 d P A 1 H3 H 0.1423 0.2422 0.0846 0.111 Uiso 0.555(2) 1 calc PR A 1 C13A C 0.1646(9) 0.342(2) 0.0230(5) 0.100(5) Uani 0.555(2) 1 d P A 1 H4 H 0.1104 0.3439 0.0028 0.120 Uiso 0.555(2) 1 calc PR A 1 C14A C 0.2389(8) 0.3906(19) 0.0134(5) 0.071(3) Uani 0.555(2) 1 d P A 1 C15A C 0.2540(9) 0.4508(19) -0.0293(5) 0.081(4) Uani 0.555(2) 1 d P . 1 N3A N 0.2987(8) 0.3655(15) 0.0512(4) 0.070(3) Uani 0.555(2) 1 d P A 1 H26 H 0.3530 0.3825 0.0524 0.084 Uiso 0.555(2) 1 calc PR A 1 C11B C 0.2420(12) 0.2522(18) 0.0819(6) 0.057(4) Uiso 0.445(2) 1 d P A 2 C12B C 0.1524(8) 0.207(2) 0.0610(5) 0.065(4) Uani 0.445(2) 1 d P A 2 H5 H 0.1134 0.1561 0.0767 0.078 Uiso 0.445(2) 1 calc PR A 2 C13B C 0.1350(9) 0.2500(19) 0.0152(5) 0.072(4) Uani 0.445(2) 1 d P A 2 H6 H 0.0821 0.2344 -0.0056 0.086 Uiso 0.445(2) 1 calc PR A 2 C14B C 0.2103(10) 0.323(2) 0.0041(7) 0.060(4) Uani 0.445(2) 1 d P A 2 C15B C 0.2221(9) 0.380(2) -0.0375(6) 0.062(4) Uani 0.445(2) 1 d P . 2 N3B N 0.2696(9) 0.323(2) 0.0464(7) 0.073(6) Uiso 0.445(2) 1 d P A 2 H27 H 0.3209 0.3657 0.0494 0.087 Uiso 0.445(2) 1 calc PR A 2 C16 C 0.6792(4) 0.3180(7) 0.16889(18) 0.0886(17) Uani 1 1 d . B . C17 C 0.7051(4) 0.1506(8) 0.18046(19) 0.0856(16) Uani 1 1 d . . . C18 C 0.7827(5) 0.1108(8) 0.2072(2) 0.0883(16) Uani 1 1 d . B . C19 C 0.8388(5) 0.2341(9) 0.2246(2) 0.0960(18) Uani 1 1 d . . . C20 C 0.8167(5) 0.4004(10) 0.2144(2) 0.1008(19) Uani 1 1 d . B . C21 C 0.7396(5) 0.4431(8) 0.18730(19) 0.0953(19) Uani 1 1 d . . . C22A C 0.2593(9) 0.224(2) 0.1652(6) 0.072(4) Uani 0.529(11) 1 d P A 5 C23A C 0.2394(9) 0.0554(19) 0.1746(4) 0.069(3) Uani 0.529(11) 1 d P A 5 C24A C 0.1846(9) 0.0082(19) 0.2040(5) 0.075(4) Uani 0.529(11) 1 d P A 5 C25A C 0.1509(15) 0.141(3) 0.2262(7) 0.084(6) Uani 0.529(11) 1 d P A 5 C26A C 0.1756(16) 0.300(3) 0.2182(8) 0.094(8) Uani 0.529(11) 1 d P A 5 C27A C 0.2198(18) 0.331(4) 0.1883(8) 0.103(10) Uani 0.529(11) 1 d P A 5 F6A F 0.2717(6) -0.0738(7) 0.1541(2) 0.083(3) Uani 0.529(11) 1 d P A 5 F7A F 0.1683(7) -0.1510(10) 0.2108(3) 0.097(3) Uani 0.529(11) 1 d P A 5 F8A F 0.1007(17) 0.095(4) 0.2541(10) 0.107(7) Uani 0.529(11) 1 d P A 5 F9A F 0.1358(8) 0.4300(15) 0.2400(5) 0.097(3) Uani 0.529(11) 1 d P A 5 F10A F 0.2361(14) 0.508(3) 0.1800(6) 0.099(5) Uani 0.529(11) 1 d P A 5 C22B C 0.2279(8) 0.1776(18) 0.1603(5) 0.065(5) Uani 0.471(11) 1 d PG A 6 C23B C 0.1945(9) 0.0138(15) 0.1599(4) 0.068(4) Uani 0.471(11) 1 d PG A 6 C24B C 0.1442(9) -0.0295(17) 0.1906(5) 0.088(5) Uani 0.471(11) 1 d PG A 6 C25B C 0.1274(9) 0.091(3) 0.2218(5) 0.087(9) Uani 0.471(11) 1 d PG A 6 C26B C 0.1608(11) 0.255(2) 0.2221(5) 0.103(16) Uani 0.471(11) 1 d PG A 6 C27B C 0.2111(10) 0.2980(17) 0.1914(6) 0.103(14) Uani 0.471(11) 1 d PG A 6 F6B F 0.2078(6) -0.1066(9) 0.1303(3) 0.087(3) Uani 0.471(11) 1 d P A 6 F7B F 0.1119(7) -0.1925(13) 0.1906(4) 0.111(3) Uani 0.471(11) 1 d P A 6 F8B F 0.0833(18) 0.051(4) 0.2520(10) 0.126(9) Uani 0.471(11) 1 d P A 6 F9B F 0.1479(12) 0.360(2) 0.2532(6) 0.115(5) Uani 0.471(11) 1 d P A 6 F10B F 0.2387(15) 0.452(3) 0.1928(7) 0.091(7) Uani 0.471(11) 1 d P A 6 N1 N 0.6835(3) 0.4569(6) 0.08467(15) 0.0907(14) Uani 1 1 d . . . H28 H 0.7286 0.4015 0.0995 0.109 Uiso 1 1 calc R B . N2 N 0.4449(4) 0.2990(6) 0.12163(17) 0.0969(15) Uani 1 1 d . B . H29 H 0.4343 0.3153 0.0918 0.116 Uiso 1 1 calc R . . F1 F 0.6525(2) 0.0229(4) 0.16383(10) 0.0981(10) Uani 1 1 d . B . F2 F 0.8028(2) -0.0548(4) 0.21646(11) 0.1064(10) Uani 1 1 d . . . F3 F 0.9144(2) 0.1973(5) 0.25116(12) 0.1147(11) Uani 1 1 d . B . F4 F 0.8705(3) 0.5282(5) 0.23212(11) 0.1247(13) Uani 1 1 d . . . F5 F 0.7198(2) 0.6072(4) 0.17948(11) 0.1157(12) Uani 1 1 d . B . C28B C 0.1481(7) 0.3834(14) -0.0739(4) 0.062(3) Uani 0.445(2) 1 d P . 2 C29B C 0.1298(13) 0.262(3) -0.1089(8) 0.097(7) Uani 0.445(2) 1 d P . 2 C30B C 0.0680(7) 0.2784(14) -0.1484(4) 0.062(3) Uani 0.445(2) 1 d P . 2 C31B C 0.0105(8) 0.4033(19) -0.1513(5) 0.075(4) Uani 0.445(2) 1 d P . 2 C32B C 0.0193(8) 0.5226(15) -0.1155(4) 0.071(3) Uani 0.445(2) 1 d P . 2 C33B C 0.0856(8) 0.5121(14) -0.0792(4) 0.068(3) Uani 0.445(2) 1 d P . 2 F11B F 0.1904(4) 0.1446(8) -0.1088(2) 0.091(2) Uani 0.445(2) 1 d P . 2 F12B F 0.0587(4) 0.1603(9) -0.1806(2) 0.092(2) Uani 0.445(2) 1 d P . 2 F13B F -0.0531(4) 0.4194(8) -0.1877(2) 0.0843(19) Uani 0.445(2) 1 d P . 2 F14B F -0.0426(4) 0.6448(10) -0.1180(3) 0.099(2) Uani 0.445(2) 1 d P . 2 F15B F 0.0857(5) 0.6245(10) -0.0446(2) 0.089(2) Uani 0.445(2) 1 d P . 2 C54 C 0.6085(13) 0.467(2) 0.4309(6) 0.121(6) Uani 0.445(2) 1 d P . 2 H22 H 0.6146 0.5471 0.4571 0.145 Uiso 0.445(2) 1 calc PR A 2 H23 H 0.6548 0.3823 0.4382 0.145 Uiso 0.445(2) 1 calc PR A 2 Cl1 Cl 0.6184(2) 0.5812(5) 0.38202(13) 0.1132(13) Uani 0.445(2) 1 d P . 2 Cl2 Cl 0.5094(2) 0.3610(5) 0.42343(14) 0.1117(13) Uani 0.445(2) 1 d P . 2 C55 C 0.3319(7) 0.1926(14) 0.4304(4) 0.075(3) Uani 0.445(2) 1 d P . 2 H24 H 0.3554 0.0880 0.4470 0.090 Uiso 0.445(2) 1 calc PR A 2 H25 H 0.2987 0.1577 0.3999 0.090 Uiso 0.445(2) 1 calc PR A 2 Cl3 Cl 0.26454(19) 0.2934(4) 0.46079(12) 0.0878(10) Uani 0.445(2) 1 d P . 2 Cl4 Cl 0.41456(19) 0.3220(4) 0.42298(13) 0.0966(11) Uani 0.445(2) 1 d P . 2 C28A C 0.1779(4) 0.5462(9) -0.0581(2) 0.087(3) Uani 0.555(2) 1 d PG A 1 C29A C 0.1386(5) 0.4828(10) -0.1009(3) 0.091(4) Uani 0.555(2) 1 d PG A 1 C30A C 0.0709(5) 0.5705(14) -0.1277(2) 0.091(3) Uani 0.555(2) 1 d PG A 1 C31A C 0.0424(4) 0.7217(13) -0.1117(3) 0.123(5) Uani 0.555(2) 1 d PG A 1 C32A C 0.0817(6) 0.7852(10) -0.0690(4) 0.125(4) Uani 0.555(2) 1 d PG A 1 C33A C 0.1494(5) 0.6974(10) -0.0422(2) 0.100(4) Uani 0.555(2) 1 d PG A 1 F11A F 0.1615(5) 0.3359(13) -0.1172(3) 0.100(2) Uani 0.555(2) 1 d P A 1 F12A F 0.0316(4) 0.5160(13) -0.1674(2) 0.130(3) Uani 0.555(2) 1 d P A 1 F13A F -0.0215(4) 0.8086(11) -0.1366(2) 0.136(3) Uani 0.555(2) 1 d P A 1 F14A F 0.0577(6) 0.9383(13) -0.0524(3) 0.158(3) Uani 0.555(2) 1 d P A 1 F15A F 0.1877(4) 0.7632(8) -0.0016(2) 0.118(2) Uani 0.555(2) 1 d P A 1 S1 S 0.56144(8) 0.78388(17) -0.00649(4) 0.0771(4) Uani 1 1 d . . . C34 C 0.6376(3) 0.9555(7) 0.00796(19) 0.0853(16) Uani 1 1 d . B . H7 H 0.6929 0.9171 0.0023 0.102 Uiso 1 1 calc R . . H8 H 0.6184 1.0540 -0.0125 0.102 Uiso 1 1 calc R . . C35 C 0.6494(3) 1.0130(7) 0.05719(19) 0.0903(16) Uani 1 1 d . . . H9 H 0.5953 1.0556 0.0627 0.135 Uiso 1 1 calc R B . H10 H 0.6918 1.1044 0.0632 0.135 Uiso 1 1 calc R . . H11 H 0.6687 0.9164 0.0776 0.135 Uiso 1 1 calc R . . S2A S 0.4642(6) 0.6425(14) 0.0647(4) 0.0674(15) Uani 0.527(19) 1 d P B 3 C36A C 0.4764(11) 0.739(3) 0.1251(7) 0.092(6) Uani 0.527(19) 1 d P B 3 H12 H 0.5028 0.6553 0.1486 0.111 Uiso 0.527(19) 1 calc PR B 3 H13 H 0.5129 0.8421 0.1281 0.111 Uiso 0.527(19) 1 calc PR B 3 C37A C 0.3949(9) 0.783(2) 0.1309(4) 0.102(5) Uani 0.527(19) 1 d P B 3 H14 H 0.3695 0.8661 0.1075 0.153 Uiso 0.527(19) 1 calc PR B 3 H15 H 0.3989 0.8321 0.1614 0.153 Uiso 0.527(19) 1 calc PR B 3 H16 H 0.3595 0.6798 0.1278 0.153 Uiso 0.527(19) 1 calc PR B 3 S2B S 0.4350(7) 0.6275(16) 0.0643(4) 0.0667(16) Uani 0.473(19) 1 d P B 4 C36B C 0.4400(12) 0.689(2) 0.1202(7) 0.074(6) Uani 0.473(19) 1 d P B 4 H17 H 0.3816 0.7113 0.1242 0.089 Uiso 0.473(19) 1 calc PR B 4 H18 H 0.4629 0.5929 0.1406 0.089 Uiso 0.473(19) 1 calc PR B 4 C37B C 0.4940(10) 0.848(2) 0.1360(6) 0.109(6) Uani 0.473(19) 1 d P B 4 H19 H 0.5530 0.8254 0.1343 0.163 Uiso 0.473(19) 1 calc PR B 4 H20 H 0.4913 0.8750 0.1677 0.163 Uiso 0.473(19) 1 calc PR B 4 H21 H 0.4722 0.9446 0.1161 0.163 Uiso 0.473(19) 1 calc PR B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.120(5) 0.085(4) 0.060(4) 0.009(3) 0.022(4) 0.029(4) C2 0.109(4) 0.061(3) 0.055(3) 0.008(2) 0.009(3) 0.014(3) C3 0.110(4) 0.063(3) 0.059(3) 0.004(3) 0.004(3) 0.007(3) C4 0.129(5) 0.076(4) 0.059(4) -0.006(3) 0.016(4) 0.017(4) C5 0.132(5) 0.069(3) 0.053(3) 0.002(3) 0.018(4) 0.013(3) C6 0.147(6) 0.078(4) 0.053(4) 0.007(3) 0.018(4) 0.017(4) C7 0.157(6) 0.080(4) 0.059(4) 0.008(3) 0.019(4) 0.016(4) C8 0.165(7) 0.086(4) 0.062(4) 0.011(3) 0.038(4) 0.024(4) C9 0.150(6) 0.080(4) 0.058(4) 0.011(3) 0.021(4) 0.033(4) C10 0.137(6) 0.111(5) 0.057(4) 0.028(3) 0.032(4) 0.049(4) C11A 0.086(9) 0.088(9) 0.072(9) 0.005(7) 0.005(7) -0.010(7) C12A 0.063(9) 0.135(13) 0.082(10) 0.023(8) 0.018(7) -0.030(8) C13A 0.052(8) 0.169(16) 0.071(9) 0.039(10) -0.003(7) -0.023(9) C14A 0.056(8) 0.091(10) 0.060(8) 0.010(7) 0.001(6) -0.001(6) C15A 0.073(9) 0.096(11) 0.061(8) 0.017(7) -0.013(7) -0.002(7) N3A 0.078(7) 0.078(7) 0.056(6) 0.019(5) 0.018(6) 0.018(6) C12B 0.037(7) 0.100(11) 0.059(9) 0.014(7) 0.009(6) -0.011(6) C13B 0.054(9) 0.095(11) 0.065(10) 0.005(8) 0.010(7) -0.023(6) C14B 0.036(8) 0.065(10) 0.077(12) -0.001(8) 0.006(8) -0.011(6) C15B 0.049(8) 0.080(11) 0.060(10) 0.000(8) 0.021(8) 0.006(6) C16 0.133(5) 0.078(4) 0.053(3) 0.003(3) 0.017(3) 0.010(4) C17 0.118(5) 0.075(4) 0.066(4) 0.002(3) 0.025(4) -0.004(4) C18 0.114(5) 0.080(4) 0.073(4) 0.009(3) 0.025(4) 0.015(4) C19 0.120(5) 0.100(5) 0.071(4) 0.000(4) 0.027(4) 0.004(4) C20 0.134(6) 0.099(5) 0.067(4) -0.010(4) 0.016(4) -0.021(5) C21 0.160(6) 0.069(4) 0.054(4) -0.002(3) 0.016(4) 0.005(4) C22A 0.058(9) 0.074(9) 0.077(10) -0.004(7) -0.001(7) -0.008(7) C23A 0.074(8) 0.073(9) 0.055(7) -0.003(6) 0.005(6) -0.004(7) C24A 0.078(9) 0.076(9) 0.064(8) 0.004(7) 0.000(7) -0.002(7) C25A 0.073(10) 0.14(2) 0.041(10) 0.003(10) 0.025(8) -0.034(13) C26A 0.111(17) 0.098(11) 0.087(16) -0.027(11) 0.052(10) 0.002(10) C27A 0.117(19) 0.11(2) 0.089(17) -0.024(16) 0.043(14) 0.037(16) F6A 0.100(6) 0.074(4) 0.081(5) -0.006(3) 0.030(4) 0.004(3) F7A 0.116(7) 0.079(5) 0.102(6) 0.007(4) 0.039(5) -0.006(5) F8A 0.098(10) 0.117(9) 0.096(13) -0.007(9) 0.000(8) 0.001(6) F9A 0.106(7) 0.097(8) 0.093(8) -0.020(5) 0.035(6) 0.004(6) F10A 0.113(7) 0.100(10) 0.082(11) -0.006(7) 0.015(8) -0.018(6) C22B 0.054(10) 0.080(13) 0.059(9) 0.011(9) 0.008(8) -0.009(8) C23B 0.065(9) 0.069(9) 0.072(10) 0.008(7) 0.018(7) -0.002(7) C24B 0.070(10) 0.092(13) 0.096(13) 0.028(10) 0.002(9) 0.006(9) C25B 0.070(13) 0.103(16) 0.092(17) 0.027(13) 0.026(11) 0.022(13) C26B 0.035(8) 0.24(5) 0.043(11) 0.06(2) 0.019(7) -0.006(17) C27B 0.10(2) 0.10(2) 0.08(2) 0.014(17) -0.046(17) 0.005(16) F6B 0.084(6) 0.079(5) 0.098(6) 0.002(4) 0.018(5) -0.007(4) F7B 0.103(7) 0.100(7) 0.137(9) 0.037(5) 0.039(6) -0.001(5) F8B 0.108(14) 0.18(2) 0.106(17) 0.059(13) 0.067(13) 0.054(13) F9B 0.126(7) 0.134(12) 0.088(8) 0.034(7) 0.029(6) 0.046(8) F10B 0.096(7) 0.13(2) 0.049(8) 0.000(9) 0.018(6) 0.027(12) N1 0.124(4) 0.087(3) 0.057(3) 0.004(2) 0.009(3) 0.030(3) N2 0.135(4) 0.099(4) 0.056(3) 0.016(3) 0.019(3) 0.020(3) F1 0.133(3) 0.078(2) 0.083(2) 0.0106(17) 0.0204(19) 0.0015(19) F2 0.120(3) 0.098(2) 0.106(3) 0.025(2) 0.036(2) 0.019(2) F3 0.102(2) 0.145(3) 0.093(3) 0.011(2) 0.014(2) 0.009(2) F4 0.167(3) 0.118(3) 0.084(2) -0.020(2) 0.017(2) -0.026(3) F5 0.188(3) 0.071(2) 0.080(2) -0.0122(17) 0.011(2) 0.000(2) C28B 0.081(8) 0.060(7) 0.040(7) 0.006(5) 0.004(6) -0.009(6) C29B 0.089(13) 0.089(14) 0.125(16) -0.001(11) 0.046(11) -0.019(9) C30B 0.058(6) 0.071(7) 0.054(7) -0.018(6) 0.004(5) 0.000(6) C31B 0.071(8) 0.085(10) 0.060(9) 0.012(7) -0.005(7) -0.022(7) C32B 0.074(8) 0.060(7) 0.073(9) 0.006(6) 0.001(7) 0.018(6) C33B 0.077(8) 0.063(7) 0.052(7) -0.006(6) -0.016(6) -0.003(6) F11B 0.089(4) 0.085(5) 0.080(5) -0.022(3) -0.024(4) 0.030(4) F12B 0.086(4) 0.107(5) 0.071(5) -0.029(4) -0.013(3) 0.012(4) F13B 0.060(4) 0.117(5) 0.062(4) 0.001(3) -0.017(3) -0.011(3) F14B 0.082(5) 0.110(6) 0.095(6) -0.002(4) -0.003(4) 0.018(4) F15B 0.085(5) 0.094(5) 0.079(5) -0.010(4) 0.001(4) 0.016(4) C54 0.164(18) 0.111(14) 0.091(12) 0.010(10) 0.035(11) -0.028(12) Cl1 0.113(3) 0.123(3) 0.103(3) 0.011(2) 0.022(2) 0.018(2) Cl2 0.085(2) 0.115(3) 0.130(3) 0.004(2) 0.010(2) 0.014(2) C55 0.081(7) 0.068(7) 0.081(8) -0.004(6) 0.026(6) -0.011(6) Cl3 0.0725(19) 0.105(2) 0.085(2) -0.0007(18) 0.0144(17) 0.0057(16) Cl4 0.0728(19) 0.094(2) 0.127(3) 0.007(2) 0.0315(19) -0.0061(16) C28A 0.078(7) 0.100(9) 0.084(8) 0.012(6) 0.019(6) -0.016(6) C29A 0.066(7) 0.141(12) 0.071(8) -0.020(9) 0.022(7) -0.029(7) C30A 0.083(8) 0.106(9) 0.082(9) 0.012(7) 0.010(7) -0.011(7) C31A 0.080(8) 0.152(13) 0.125(12) 0.040(10) -0.005(8) 0.001(9) C32A 0.118(11) 0.113(11) 0.138(13) 0.007(10) 0.012(9) 0.007(9) C33A 0.067(7) 0.067(7) 0.162(13) 0.009(8) 0.016(8) 0.021(6) F11A 0.088(5) 0.129(8) 0.072(5) -0.023(5) -0.004(4) 0.014(4) F12A 0.099(5) 0.200(9) 0.080(5) -0.010(5) -0.006(4) -0.012(5) F13A 0.107(5) 0.168(7) 0.120(6) 0.044(5) -0.004(4) 0.031(5) F14A 0.145(7) 0.137(8) 0.172(9) -0.017(6) -0.012(6) 0.066(6) F15A 0.107(5) 0.124(5) 0.106(5) -0.026(4) -0.015(4) 0.005(4) S1 0.0920(9) 0.0709(8) 0.0623(9) 0.0054(6) 0.0028(7) 0.0050(7) C34 0.076(3) 0.086(4) 0.093(4) 0.012(3) 0.016(3) 0.005(3) C35 0.088(4) 0.085(4) 0.091(4) -0.010(3) 0.002(3) -0.009(3) S2A 0.066(4) 0.069(2) 0.071(2) 0.0047(16) 0.022(3) -0.002(3) C36A 0.092(12) 0.087(15) 0.104(12) -0.042(10) 0.032(10) -0.026(9) C37A 0.127(12) 0.089(10) 0.104(10) -0.011(7) 0.058(8) 0.003(8) S2B 0.062(4) 0.074(3) 0.068(2) 0.0009(19) 0.025(4) -0.003(3) C36B 0.091(14) 0.056(10) 0.070(9) -0.015(7) 0.005(10) -0.001(9) C37B 0.119(12) 0.077(11) 0.131(14) -0.032(9) 0.033(10) -0.020(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C15A 1.240(16) 3_665 ? C1 N1 1.372(7) . ? C1 C2 1.410(8) . ? C1 C15B 1.688(15) 3_665 ? C2 C3 1.403(7) . ? C2 S1 1.748(5) . ? C3 C4 1.442(7) . ? C3 S2A 1.553(12) . ? C3 S2B 1.961(12) . ? C4 N1 1.375(7) . ? C4 C5 1.416(8) . ? C5 C6 1.402(8) . ? C5 C16 1.483(8) . ? C6 N2 1.370(7) . ? C6 C7 1.417(8) . ? C7 C8 1.358(8) . ? C7 H1 0.9500 . ? C8 C9 1.405(8) . ? C8 H2 0.9500 . ? C9 C10 1.380(9) . ? C9 N2 1.409(8) . ? C10 C11A 1.290(14) . ? C10 C22A 1.361(19) . ? C10 C11B 1.500(19) . ? C10 C22B 1.693(12) . ? C11A C12A 1.364(18) . ? C11A N3A 1.403(18) . ? C12A C13A 1.410(18) . ? C12A H3 0.9500 . ? C13A C14A 1.346(17) . ? C13A H4 0.9500 . ? C14A N3A 1.333(19) . ? C14A C15A 1.43(2) . ? C15A C1 1.240(16) 3_665 ? C15A C28A 1.535(15) . ? N3A H26 0.8800 . ? C11B N3B 1.35(3) . ? C11B C12B 1.49(2) . ? C12B C13B 1.375(19) . ? C12B H5 0.9500 . ? C13B C14B 1.444(19) . ? C13B H6 0.9500 . ? C14B C15B 1.37(2) . ? C14B N3B 1.41(3) . ? C15B C28B 1.433(19) . ? C15B C1 1.688(15) 3_665 ? N3B H27 0.8800 . ? C16 C17 1.397(7) . ? C16 C21 1.408(8) . ? C17 F1 1.336(6) . ? C17 C18 1.370(8) . ? C18 C19 1.348(8) . ? C18 F2 1.351(6) . ? C19 F3 1.336(7) . ? C19 C20 1.367(9) . ? C20 F4 1.356(7) . ? C20 C21 1.373(8) . ? C21 F5 1.333(6) . ? C22A C27A 1.33(2) . ? C22A C23A 1.402(19) . ? C23A F6A 1.343(13) . ? C23A C24A 1.421(18) . ? C24A F7A 1.299(16) . ? C24A C25A 1.41(3) . ? C25A F8A 1.33(3) . ? C25A C26A 1.34(3) . ? C26A C27A 1.28(4) . ? C26A F9A 1.43(2) . ? C27A F10A 1.44(4) . ? C22B C23B 1.3900 . ? C22B C27B 1.3900 . ? C23B F6B 1.340(12) . ? C23B C24B 1.3900 . ? C24B F7B 1.378(14) . ? C24B C25B 1.3900 . ? C25B F8B 1.30(3) . ? C25B C26B 1.3900 . ? C26B F9B 1.29(2) . ? C26B C27B 1.3900 . ? C27B F10B 1.29(3) . ? N1 H28 0.8800 . ? N2 H29 0.8800 . ? C28B C29B 1.40(2) . ? C28B C33B 1.410(15) . ? C29B F11B 1.34(2) . ? C29B C30B 1.38(2) . ? C30B F12B 1.319(11) . ? C30B C31B 1.338(16) . ? C31B F13B 1.331(13) . ? C31B C32B 1.402(17) . ? C32B C33B 1.353(15) . ? C32B F14B 1.374(12) . ? C33B F15B 1.357(12) . ? F11B Cl1 2.100(8) 4_565 ? C54 Cl1 1.744(16) . ? C54 Cl2 1.775(18) . ? C54 H22 0.9900 . ? C54 H23 0.9900 . ? Cl1 F11B 2.100(8) 4_666 ? Cl2 Cl4 1.558(5) . ? C55 Cl4 1.725(11) . ? C55 Cl3 1.747(12) . ? C55 H24 0.9900 . ? C55 H25 0.9900 . ? C28A C29A 1.3900 . ? C28A C33A 1.3900 . ? C29A F11A 1.330(10) . ? C29A C30A 1.3900 . ? C30A F12A 1.291(9) . ? C30A C31A 1.3900 . ? C31A F13A 1.323(8) . ? C31A C32A 1.3900 . ? C32A F14A 1.384(10) . ? C32A C33A 1.3900 . ? C33A F15A 1.338(9) . ? S1 C34 1.809(5) . ? C34 C35 1.509(7) . ? C34 H7 0.9900 . ? C34 H8 0.9900 . ? C35 H9 0.9800 . ? C35 H10 0.9800 . ? C35 H11 0.9800 . ? S2A C36A 1.93(2) . ? C36A C37A 1.40(2) . ? C36A H12 0.9900 . ? C36A H13 0.9900 . ? C37A H14 0.9800 . ? C37A H15 0.9800 . ? C37A H16 0.9800 . ? S2B C36B 1.72(2) . ? C36B C37B 1.53(2) . ? C36B H17 0.9900 . ? C36B H18 0.9900 . ? C37B H19 0.9800 . ? C37B H20 0.9800 . ? C37B H21 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15A C1 N1 117.2(9) 3_665 . ? C15A C1 C2 135.8(8) 3_665 . ? N1 C1 C2 106.3(6) . . ? C15A C1 C15B 24.5(8) 3_665 3_665 ? N1 C1 C15B 117.2(8) . 3_665 ? C2 C1 C15B 132.4(7) . 3_665 ? C3 C2 C1 107.9(5) . . ? C3 C2 S1 122.0(4) . . ? C1 C2 S1 129.8(5) . . ? C2 C3 C4 108.2(5) . . ? C2 C3 S2A 119.7(6) . . ? C4 C3 S2A 131.4(6) . . ? C2 C3 S2B 125.0(5) . . ? C4 C3 S2B 126.8(6) . . ? S2A C3 S2B 8.5(7) . . ? N1 C4 C5 119.2(6) . . ? N1 C4 C3 104.6(5) . . ? C5 C4 C3 135.8(6) . . ? C6 C5 C4 128.1(6) . . ? C6 C5 C16 116.4(5) . . ? C4 C5 C16 115.6(6) . . ? N2 C6 C5 125.7(6) . . ? N2 C6 C7 106.2(7) . . ? C5 C6 C7 128.0(7) . . ? C8 C7 C6 108.8(7) . . ? C8 C7 H1 125.6 . . ? C6 C7 H1 125.6 . . ? C7 C8 C9 109.3(7) . . ? C7 C8 H2 125.4 . . ? C9 C8 H2 125.4 . . ? C10 C9 C8 129.9(7) . . ? C10 C9 N2 124.7(6) . . ? C8 C9 N2 105.4(7) . . ? C11A C10 C22A 129.8(11) . . ? C11A C10 C9 119.5(9) . . ? C22A C10 C9 106.8(8) . . ? C11A C10 C11B 23.7(8) . . ? C22A C10 C11B 117.8(11) . . ? C9 C10 C11B 135.4(9) . . ? C11A C10 C22B 117.8(9) . . ? C22A C10 C22B 19.7(7) . . ? C9 C10 C22B 122.4(7) . . ? C11B C10 C22B 100.9(9) . . ? C10 C11A C12A 120.2(13) . . ? C10 C11A N3A 137.0(12) . . ? C12A C11A N3A 101.0(12) . . ? C11A C12A C13A 111.6(12) . . ? C11A C12A H3 124.2 . . ? C13A C12A H3 124.2 . . ? C14A C13A C12A 106.3(12) . . ? C14A C13A H4 126.9 . . ? C12A C13A H4 126.9 . . ? N3A C14A C13A 107.2(13) . . ? N3A C14A C15A 125.0(13) . . ? C13A C14A C15A 127.8(13) . . ? C1 C15A C14A 132.2(12) 3_665 . ? C1 C15A C28A 114.7(12) 3_665 . ? C14A C15A C28A 113.1(13) . . ? C14A N3A C11A 113.7(12) . . ? C14A N3A H26 123.1 . . ? C11A N3A H26 123.1 . . ? N3B C11B C12B 102.7(16) . . ? N3B C11B C10 121.0(15) . . ? C12B C11B C10 136.1(13) . . ? C13B C12B C11B 109.5(13) . . ? C13B C12B H5 125.3 . . ? C11B C12B H5 125.3 . . ? C12B C13B C14B 108.8(13) . . ? C12B C13B H6 125.6 . . ? C14B C13B H6 125.6 . . ? C15B C14B N3B 127.7(16) . . ? C15B C14B C13B 128.6(15) . . ? N3B C14B C13B 103.7(16) . . ? C14B C15B C28B 116.0(13) . . ? C14B C15B C1 123.5(12) . 3_665 ? C28B C15B C1 120.5(12) . 3_665 ? C11B N3B C14B 115.3(14) . . ? C11B N3B H27 122.3 . . ? C14B N3B H27 122.3 . . ? C17 C16 C21 114.2(6) . . ? C17 C16 C5 123.4(6) . . ? C21 C16 C5 122.2(5) . . ? F1 C17 C18 118.4(5) . . ? F1 C17 C16 118.5(6) . . ? C18 C17 C16 123.1(6) . . ? C19 C18 F2 119.8(6) . . ? C19 C18 C17 121.1(6) . . ? F2 C18 C17 119.1(6) . . ? F3 C19 C18 121.8(6) . . ? F3 C19 C20 120.0(7) . . ? C18 C19 C20 118.3(7) . . ? F4 C20 C19 120.0(7) . . ? F4 C20 C21 118.3(7) . . ? C19 C20 C21 121.6(7) . . ? F5 C21 C20 119.4(6) . . ? F5 C21 C16 118.9(6) . . ? C20 C21 C16 121.7(6) . . ? C27A C22A C10 132(2) . . ? C27A C22A C23A 110(2) . . ? C10 C22A C23A 116.7(13) . . ? F6A C23A C22A 119.5(12) . . ? F6A C23A C24A 116.0(12) . . ? C22A C23A C24A 124.5(13) . . ? F7A C24A C25A 121.8(14) . . ? F7A C24A C23A 121.2(13) . . ? C25A C24A C23A 117.0(14) . . ? F8A C25A C26A 128(3) . . ? F8A C25A C24A 116(2) . . ? C26A C25A C24A 116.2(18) . . ? C27A C26A C25A 122(2) . . ? C27A C26A F9A 124(2) . . ? C25A C26A F9A 113(2) . . ? C26A C27A C22A 130(3) . . ? C26A C27A F10A 117.0(18) . . ? C22A C27A F10A 113(3) . . ? C23B C22B C27B 120.0 . . ? C23B C22B C10 126.8(10) . . ? C27B C22B C10 113.0(10) . . ? F6B C23B C22B 122.5(10) . . ? F6B C23B C24B 117.5(10) . . ? C22B C23B C24B 120.0 . . ? F7B C24B C23B 120.0(11) . . ? F7B C24B C25B 120.0(11) . . ? C23B C24B C25B 120.0 . . ? F8B C25B C26B 119.1(18) . . ? F8B C25B C24B 120.9(18) . . ? C26B C25B C24B 120.0 . . ? F9B C26B C27B 121.7(16) . . ? F9B C26B C25B 118.2(16) . . ? C27B C26B C25B 120.0 . . ? F10B C27B C26B 117.1(17) . . ? F10B C27B C22B 122.9(17) . . ? C26B C27B C22B 120.0 . . ? C1 N1 C4 112.9(5) . . ? C1 N1 H28 123.6 . . ? C4 N1 H28 123.6 . . ? C6 N2 C9 110.3(5) . . ? C6 N2 H29 124.9 . . ? C9 N2 H29 124.9 . . ? C29B C28B C33B 111.7(13) . . ? C29B C28B C15B 124.2(14) . . ? C33B C28B C15B 124.0(11) . . ? F11B C29B C30B 117.5(18) . . ? F11B C29B C28B 115.3(17) . . ? C30B C29B C28B 125.0(18) . . ? F12B C30B C31B 119.7(10) . . ? F12B C30B C29B 120.3(13) . . ? C31B C30B C29B 119.4(13) . . ? F13B C31B C30B 121.7(12) . . ? F13B C31B C32B 119.5(12) . . ? C30B C31B C32B 118.8(11) . . ? C33B C32B F14B 121.9(11) . . ? C33B C32B C31B 120.2(11) . . ? F14B C32B C31B 117.9(11) . . ? C32B C33B F15B 116.3(11) . . ? C32B C33B C28B 123.9(11) . . ? F15B C33B C28B 119.5(9) . . ? C29B F11B Cl1 101.1(9) . 4_565 ? Cl1 C54 Cl2 112.1(10) . . ? Cl1 C54 H22 109.2 . . ? Cl2 C54 H22 109.2 . . ? Cl1 C54 H23 109.2 . . ? Cl2 C54 H23 109.2 . . ? H22 C54 H23 107.9 . . ? C54 Cl1 F11B 66.9(8) . 4_666 ? Cl4 Cl2 C54 161.9(8) . . ? Cl4 C55 Cl3 112.6(6) . . ? Cl4 C55 H24 109.1 . . ? Cl3 C55 H24 109.1 . . ? Cl4 C55 H25 109.1 . . ? Cl3 C55 H25 109.1 . . ? H24 C55 H25 107.8 . . ? Cl2 Cl4 C55 154.0(5) . . ? C29A C28A C33A 120.0 . . ? C29A C28A C15A 119.6(8) . . ? C33A C28A C15A 120.4(8) . . ? F11A C29A C28A 122.4(7) . . ? F11A C29A C30A 117.6(7) . . ? C28A C29A C30A 120.0 . . ? F12A C30A C29A 122.4(8) . . ? F12A C30A C31A 117.6(8) . . ? C29A C30A C31A 120.0 . . ? F13A C31A C32A 118.6(9) . . ? F13A C31A C30A 121.4(9) . . ? C32A C31A C30A 120.0 . . ? F14A C32A C31A 122.0(8) . . ? F14A C32A C33A 117.9(8) . . ? C31A C32A C33A 120.0 . . ? F15A C33A C32A 119.0(6) . . ? F15A C33A C28A 121.0(6) . . ? C32A C33A C28A 120.0 . . ? C2 S1 C34 102.8(3) . . ? C35 C34 S1 113.1(4) . . ? C35 C34 H7 109.0 . . ? S1 C34 H7 109.0 . . ? C35 C34 H8 109.0 . . ? S1 C34 H8 109.0 . . ? H7 C34 H8 107.8 . . ? C34 C35 H9 109.5 . . ? C34 C35 H10 109.5 . . ? H9 C35 H10 109.5 . . ? C34 C35 H11 109.5 . . ? H9 C35 H11 109.5 . . ? H10 C35 H11 109.5 . . ? C3 S2A C36A 103.5(8) . . ? C37A C36A S2A 107.4(13) . . ? C37A C36A H12 110.2 . . ? S2A C36A H12 110.2 . . ? C37A C36A H13 110.2 . . ? S2A C36A H13 110.2 . . ? H12 C36A H13 108.5 . . ? C36B S2B C3 102.2(9) . . ? C37B C36B S2B 115.6(16) . . ? C37B C36B H17 108.4 . . ? S2B C36B H17 108.4 . . ? C37B C36B H18 108.4 . . ? S2B C36B H18 108.4 . . ? H17 C36B H18 107.4 . . ? 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 C15A C1 C2 C3 168.9(12) 3_665 . . . ? N1 C1 C2 C3 -1.2(6) . . . . ? C15B C1 C2 C3 -157.0(8) 3_665 . . . ? C15A C1 C2 S1 -17.2(14) 3_665 . . . ? N1 C1 C2 S1 172.7(4) . . . . ? C15B C1 C2 S1 16.9(11) 3_665 . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? S1 C2 C3 C4 -174.9(4) . . . . ? C1 C2 C3 S2A 171.1(6) . . . . ? S1 C2 C3 S2A -3.4(8) . . . . ? C1 C2 C3 S2B 178.9(6) . . . . ? S1 C2 C3 S2B 4.4(8) . . . . ? C2 C3 C4 N1 1.8(6) . . . . ? S2A C3 C4 N1 -168.3(7) . . . . ? S2B C3 C4 N1 -177.5(6) . . . . ? C2 C3 C4 C5 174.1(6) . . . . ? S2A C3 C4 C5 4.0(11) . . . . ? S2B C3 C4 C5 -5.2(10) . . . . ? N1 C4 C5 C6 -164.6(5) . . . . ? C3 C4 C5 C6 24.0(10) . . . . ? N1 C4 C5 C16 15.9(7) . . . . ? C3 C4 C5 C16 -155.6(6) . . . . ? C4 C5 C6 N2 16.7(9) . . . . ? C16 C5 C6 N2 -163.7(5) . . . . ? C4 C5 C6 C7 -158.6(6) . . . . ? C16 C5 C6 C7 21.0(9) . . . . ? N2 C6 C7 C8 -2.4(7) . . . . ? C5 C6 C7 C8 173.6(6) . . . . ? C6 C7 C8 C9 1.5(7) . . . . ? C7 C8 C9 C10 -178.0(6) . . . . ? C7 C8 C9 N2 -0.1(7) . . . . ? C8 C9 C10 C11A 163.4(9) . . . . ? N2 C9 C10 C11A -14.1(12) . . . . ? C8 C9 C10 C22A 3.4(12) . . . . ? N2 C9 C10 C22A -174.1(9) . . . . ? C8 C9 C10 C11B -174.3(9) . . . . ? N2 C9 C10 C11B 8.2(13) . . . . ? C8 C9 C10 C22B -9.8(12) . . . . ? N2 C9 C10 C22B 172.7(8) . . . . ? C22A C10 C11A C12A -31(2) . . . . ? C9 C10 C11A C12A 174.7(12) . . . . ? C11B C10 C11A C12A 36(2) . . . . ? C22B C10 C11A C12A -11.8(19) . . . . ? C22A C10 C11A N3A 168.4(16) . . . . ? C9 C10 C11A N3A 14(2) . . . . ? C11B C10 C11A N3A -125(4) . . . . ? C22B C10 C11A N3A -172.9(16) . . . . ? C10 C11A C12A C13A -171.7(13) . . . . ? N3A C11A C12A C13A -4.8(18) . . . . ? C11A C12A C13A C14A 3(2) . . . . ? C12A C13A C14A N3A 0.7(18) . . . . ? C12A C13A C14A C15A 178.1(15) . . . . ? N3A C14A C15A C1 26(3) . . . 3_665 ? C13A C14A C15A C1 -151.0(16) . . . 3_665 ? N3A C14A C15A C28A -152.6(12) . . . . ? C13A C14A C15A C28A 30(2) . . . . ? C13A C14A N3A C11A -3.9(17) . . . . ? C15A C14A N3A C11A 178.6(14) . . . . ? C10 C11A N3A C14A 168.8(16) . . . . ? C12A C11A N3A C14A 5.4(17) . . . . ? C11A C10 C11B N3B 34(2) . . . . ? C22A C10 C11B N3B 160.8(15) . . . . ? C9 C10 C11B N3B -22(2) . . . . ? C22B C10 C11B N3B 171.6(14) . . . . ? C11A C10 C11B C12B -140(4) . . . . ? C22A C10 C11B C12B -13(2) . . . . ? C9 C10 C11B C12B 164.7(13) . . . . ? C22B C10 C11B C12B -2.1(18) . . . . ? N3B C11B C12B C13B 1.3(17) . . . . ? C10 C11B C12B C13B 175.7(15) . . . . ? C11B C12B C13B C14B 0.3(17) . . . . ? C12B C13B C14B C15B 178.6(17) . . . . ? C12B C13B C14B N3B -1.8(17) . . . . ? N3B C14B C15B C28B -172.9(16) . . . . ? C13B C14B C15B C28B 7(2) . . . . ? N3B C14B C15B C1 7(3) . . . 3_665 ? C13B C14B C15B C1 -173.2(13) . . . 3_665 ? C12B C11B N3B C14B -2.6(19) . . . . ? C10 C11B N3B C14B -178.1(13) . . . . ? C15B C14B N3B C11B -177.5(16) . . . . ? C13B C14B N3B C11B 2.8(19) . . . . ? C6 C5 C16 C17 61.4(7) . . . . ? C4 C5 C16 C17 -119.0(6) . . . . ? C6 C5 C16 C21 -123.9(6) . . . . ? C4 C5 C16 C21 55.8(7) . . . . ? C21 C16 C17 F1 -178.8(5) . . . . ? C5 C16 C17 F1 -3.6(8) . . . . ? C21 C16 C17 C18 -0.3(8) . . . . ? C5 C16 C17 C18 174.9(6) . . . . ? F1 C17 C18 C19 179.3(5) . . . . ? C16 C17 C18 C19 0.8(9) . . . . ? F1 C17 C18 F2 -1.0(8) . . . . ? C16 C17 C18 F2 -179.5(5) . . . . ? F2 C18 C19 F3 -0.3(9) . . . . ? C17 C18 C19 F3 179.3(5) . . . . ? F2 C18 C19 C20 179.5(5) . . . . ? C17 C18 C19 C20 -0.8(9) . . . . ? F3 C19 C20 F4 -1.8(9) . . . . ? C18 C19 C20 F4 178.3(5) . . . . ? F3 C19 C20 C21 -179.8(5) . . . . ? C18 C19 C20 C21 0.3(9) . . . . ? F4 C20 C21 F5 -0.2(9) . . . . ? C19 C20 C21 F5 177.8(5) . . . . ? F4 C20 C21 C16 -177.8(5) . . . . ? C19 C20 C21 C16 0.2(10) . . . . ? C17 C16 C21 F5 -177.9(5) . . . . ? C5 C16 C21 F5 6.9(9) . . . . ? C17 C16 C21 C20 -0.2(8) . . . . ? C5 C16 C21 C20 -175.5(6) . . . . ? C11A C10 C22A C27A -57(3) . . . . ? C9 C10 C22A C27A 100(2) . . . . ? C11B C10 C22A C27A -82(2) . . . . ? C22B C10 C22A C27A -115(4) . . . . ? C11A C10 C22A C23A 105.9(15) . . . . ? C9 C10 C22A C23A -97.0(11) . . . . ? C11B C10 C22A C23A 81.2(14) . . . . ? C22B C10 C22A C23A 48(3) . . . . ? C27A C22A C23A F6A 179.0(15) . . . . ? C10 C22A C23A F6A 12.2(16) . . . . ? C27A C22A C23A C24A 0.6(19) . . . . ? C10 C22A C23A C24A -166.2(11) . . . . ? F6A C23A C24A F7A 0.9(16) . . . . ? C22A C23A C24A F7A 179.4(11) . . . . ? F6A C23A C24A C25A 179.2(14) . . . . ? C22A C23A C24A C25A -2.3(19) . . . . ? F7A C24A C25A F8A -1(3) . . . . ? C23A C24A C25A F8A -179.1(18) . . . . ? F7A C24A C25A C26A 176.9(17) . . . . ? C23A C24A C25A C26A -1(3) . . . . ? F8A C25A C26A C27A -175(3) . . . . ? C24A C25A C26A C27A 7(3) . . . . ? F8A C25A C26A F9A -6(4) . . . . ? C24A C25A C26A F9A 177.1(16) . . . . ? C25A C26A C27A C22A -10(4) . . . . ? F9A C26A C27A C22A -179(2) . . . . ? C25A C26A C27A F10A 175(2) . . . . ? F9A C26A C27A F10A 6(3) . . . . ? C10 C22A C27A C26A 170(2) . . . . ? C23A C22A C27A C26A 6(3) . . . . ? C10 C22A C27A F10A -15(3) . . . . ? C23A C22A C27A F10A -179.1(17) . . . . ? C11A C10 C22B C23B 88.8(13) . . . . ? C22A C10 C22B C23B -138(4) . . . . ? C9 C10 C22B C23B -98.0(10) . . . . ? C11B C10 C22B C23B 71.0(11) . . . . ? C11A C10 C22B C27B -97.0(11) . . . . ? C22A C10 C22B C27B 36(3) . . . . ? C9 C10 C22B C27B 76.2(9) . . . . ? C11B C10 C22B C27B -114.7(9) . . . . ? C27B C22B C23B F6B 179.1(12) . . . . ? C10 C22B C23B F6B -7.0(13) . . . . ? C27B C22B C23B C24B 0.0 . . . . ? C10 C22B C23B C24B 173.9(12) . . . . ? F6B C23B C24B F7B 1.5(13) . . . . ? C22B C23B C24B F7B -179.3(12) . . . . ? F6B C23B C24B C25B -179.2(11) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? F7B C24B C25B F8B 2(2) . . . . ? C23B C24B C25B F8B -177(2) . . . . ? F7B C24B C25B C26B 179.3(12) . . . . ? C23B C24B C25B C26B 0.0 . . . . ? F8B C25B C26B F9B 1(2) . . . . ? C24B C25B C26B F9B -176.0(16) . . . . ? F8B C25B C26B C27B 177(2) . . . . ? C24B C25B C26B C27B 0.0 . . . . ? F9B C26B C27B F10B -5.5(18) . . . . ? C25B C26B C27B F10B 178.6(17) . . . . ? F9B C26B C27B C22B 175.9(16) . . . . ? C25B C26B C27B C22B 0.0 . . . . ? C23B C22B C27B F10B -178.5(18) . . . . ? C10 C22B C27B F10B 6.8(16) . . . . ? C23B C22B C27B C26B 0.0 . . . . ? C10 C22B C27B C26B -174.7(10) . . . . ? C15A C1 N1 C4 -169.8(9) 3_665 . . . ? C2 C1 N1 C4 2.5(6) . . . . ? C15B C1 N1 C4 162.6(7) 3_665 . . . ? C5 C4 N1 C1 -176.5(5) . . . . ? C3 C4 N1 C1 -2.7(6) . . . . ? C5 C6 N2 C9 -173.7(5) . . . . ? C7 C6 N2 C9 2.4(6) . . . . ? C10 C9 N2 C6 176.5(6) . . . . ? C8 C9 N2 C6 -1.5(6) . . . . ? C14B C15B C28B C29B -102.5(18) . . . . ? C1 C15B C28B C29B 77.4(19) 3_665 . . . ? C14B C15B C28B C33B 78.9(19) . . . . ? C1 C15B C28B C33B -101.3(15) 3_665 . . . ? C33B C28B C29B F11B 173.6(12) . . . . ? C15B C28B C29B F11B -5(2) . . . . ? C33B C28B C29B C30B 11(2) . . . . ? C15B C28B C29B C30B -167.6(14) . . . . ? F11B C29B C30B F12B 14(2) . . . . ? C28B C29B C30B F12B 176.3(13) . . . . ? F11B C29B C30B C31B -174.4(12) . . . . ? C28B C29B C30B C31B -12(2) . . . . ? F12B C30B C31B F13B -5.0(19) . . . . ? C29B C30B C31B F13B -176.4(12) . . . . ? F12B C30B C31B C32B 176.9(12) . . . . ? C29B C30B C31B C32B 5(2) . . . . ? F13B C31B C32B C33B -177.2(12) . . . . ? C30B C31B C32B C33B 1(2) . . . . ? F13B C31B C32B F14B 5(2) . . . . ? C30B C31B C32B F14B -176.8(11) . . . . ? F14B C32B C33B F15B 2.6(19) . . . . ? C31B C32B C33B F15B -175.1(12) . . . . ? F14B C32B C33B C28B 176.3(12) . . . . ? C31B C32B C33B C28B -1(2) . . . . ? C29B C28B C33B C32B -4(2) . . . . ? C15B C28B C33B C32B 174.6(13) . . . . ? C29B C28B C33B F15B 169.2(12) . . . . ? C15B C28B C33B F15B -12(2) . . . . ? C30B C29B F11B Cl1 -62.7(14) . . . 4_565 ? C28B C29B F11B Cl1 133.5(13) . . . 4_565 ? Cl2 C54 Cl1 F11B -105.4(12) . . . 4_666 ? Cl1 C54 Cl2 Cl4 -90(2) . . . . ? C54 Cl2 Cl4 C55 -141(2) . . . . ? Cl3 C55 Cl4 Cl2 133.8(8) . . . . ? C1 C15A C28A C29A 63.1(12) 3_665 . . . ? C14A C15A C28A C29A -118.1(11) . . . . ? C1 C15A C28A C33A -115.4(11) 3_665 . . . ? C14A C15A C28A C33A 63.4(13) . . . . ? C33A C28A C29A F11A -177.7(9) . . . . ? C15A C28A C29A F11A 3.8(11) . . . . ? C33A C28A C29A C30A 0.0 . . . . ? C15A C28A C29A C30A -178.5(9) . . . . ? F11A C29A C30A F12A -1.3(9) . . . . ? C28A C29A C30A F12A -179.1(9) . . . . ? F11A C29A C30A C31A 177.8(8) . . . . ? C28A C29A C30A C31A 0.0 . . . . ? F12A C30A C31A F13A -1.2(9) . . . . ? C29A C30A C31A F13A 179.6(8) . . . . ? F12A C30A C31A C32A 179.2(9) . . . . ? C29A C30A C31A C32A 0.0 . . . . ? F13A C31A C32A F14A -2.1(10) . . . . ? C30A C31A C32A F14A 177.5(10) . . . . ? F13A C31A C32A C33A -179.6(8) . . . . ? C30A C31A C32A C33A 0.0 . . . . ? F14A C32A C33A F15A 0.6(9) . . . . ? C31A C32A C33A F15A 178.2(8) . . . . ? F14A C32A C33A C28A -177.6(10) . . . . ? C31A C32A C33A C28A 0.0 . . . . ? C29A C28A C33A F15A -178.2(8) . . . . ? C15A C28A C33A F15A 0.3(11) . . . . ? C29A C28A C33A C32A 0.0 . . . . ? C15A C28A C33A C32A 178.4(9) . . . . ? C3 C2 S1 C34 121.1(5) . . . . ? C1 C2 S1 C34 -52.1(6) . . . . ? C2 S1 C34 C35 -55.1(4) . . . . ? C2 C3 S2A C36A -117.8(9) . . . . ? C4 C3 S2A C36A 51.4(11) . . . . ? S2B C3 S2A C36A 111(5) . . . . ? C3 S2A C36A C37A -168.9(12) . . . . ? C2 C3 S2B C36B -127.9(8) . . . . ? C4 C3 S2B C36B 51.3(10) . . . . ? S2A C3 S2B C36B -75(5) . . . . ? C3 S2B C36B C37B 64.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.404 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.065