# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Masahiro Irie' _publ_contact_author_email IRIEM@RIKKYO.NE.JP _publ_section_title ; Invisible Photochromism of Diarylethene Derivatives ; loop_ _publ_author_name 'Masahiro Irie' 'Tuyoshi Fukaminato' 'Lumi Kuroki' 'Masaaki Tanaka' # Attachment 'B804137G-1a.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 662776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2-Bis(3-methyl-5phenylthien-1,1dioxa-2-yl)-perfluorocyclopentene ; _chemical_name_common ;1,2-Bis(3-methyl-5phenylthien-1,1dioxa-2-yl)- perfluorocyclopentene ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H18 F6 O4 S2' _chemical_formula_weight 584.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0067(11) _cell_length_b 13.4973(11) _cell_length_c 18.0024(15) _cell_angle_alpha 70.2730(10) _cell_angle_beta 89.5390(10) _cell_angle_gamma 61.6610(10) _cell_volume 2573.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 4002 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9351 _exptl_absorpt_correction_T_max 0.9668 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22619 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 23.42 _reflns_number_total 7520 _reflns_number_gt 4992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The CF2 groups in each cyclopentene ring were disordered. The geometries were restrained by using SADI instruction on the C-C bond lengths and the occupancies of the disordered models were refined. ; _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^+0.5000P] 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 7520 _refine_ls_number_parameters 696 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2319 _refine_ls_wR_factor_gt 0.2044 _refine_ls_goodness_of_fit_ref 1.382 _refine_ls_restrained_S_all 1.382 _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 C1A C 0.5934(6) 0.3835(5) 0.0952(3) 0.0745(17) Uani 1 1 d . . . H1A H 0.6361 0.3301 0.0688 0.089 Uiso 1 1 calc R . . C2A C 0.6406(5) 0.4484(5) 0.1204(3) 0.0694(16) Uani 1 1 d . . . C3A C 0.5674(5) 0.5221(5) 0.1561(3) 0.0699(16) Uani 1 1 d . . . C4A C 0.4874(6) 0.4037(6) 0.1115(3) 0.0771(18) Uani 1 1 d . . . C5A C 0.5861(5) 0.5930(5) 0.1944(4) 0.0708(16) Uani 1 1 d . A . C6A C 0.4871(6) 0.7198(7) 0.1828(5) 0.102(2) Uani 1 1 d . . . C8A C 0.6666(6) 0.6726(5) 0.2592(4) 0.0774(18) Uani 1 1 d D . . C9A C 0.6845(5) 0.5656(4) 0.2400(3) 0.0624(15) Uani 1 1 d . A . C10A C 0.9488(5) 0.2461(5) 0.3232(3) 0.0553(13) Uani 1 1 d . A . H10A H 0.9773 0.1613 0.3483 0.066 Uiso 1 1 calc R . . C11A C 0.8218(4) 0.3360(5) 0.3048(3) 0.0542(13) Uani 1 1 d . A . C12A C 0.7986(4) 0.4521(4) 0.2717(3) 0.0567(13) Uani 1 1 d . . . C13A C 1.0226(5) 0.2902(5) 0.3026(3) 0.0563(13) Uani 1 1 d . . . C14A C 0.7580(5) 0.4335(5) 0.1024(4) 0.0771(17) Uani 1 1 d . . . H14A H 0.7640 0.5025 0.1039 0.116 Uiso 1 1 calc R . . H14B H 0.7654 0.4304 0.0489 0.116 Uiso 1 1 calc R . . H14C H 0.8217 0.3578 0.1426 0.116 Uiso 1 1 calc R . . C15A C 0.7338(5) 0.2939(5) 0.3221(3) 0.0647(15) Uani 1 1 d . . . H15A H 0.6572 0.3616 0.3219 0.097 Uiso 1 1 calc R A . H15B H 0.7622 0.2275 0.3749 0.097 Uiso 1 1 calc R . . H15C H 0.7242 0.2650 0.2809 0.097 Uiso 1 1 calc R . . C16A C 0.4150(7) 0.3528(7) 0.0968(4) 0.091(2) Uani 1 1 d . . . C17A C 0.2948(7) 0.3991(8) 0.1091(4) 0.105(2) Uani 1 1 d . . . H17A H 0.2600 0.4640 0.1277 0.126 Uiso 1 1 calc R . . C18A C 0.2301(9) 0.3508(11) 0.0944(5) 0.127(3) Uani 1 1 d . . . H18A H 0.1507 0.3808 0.1034 0.153 Uiso 1 1 calc R . . C19A C 0.2787(14) 0.2613(14) 0.0672(6) 0.149(4) Uani 1 1 d . . . H19A H 0.2322 0.2291 0.0564 0.179 Uiso 1 1 calc R . . C20A C 0.3923(12) 0.2143(11) 0.0544(6) 0.156(4) Uani 1 1 d . . . H20A H 0.4242 0.1502 0.0351 0.188 Uiso 1 1 calc R . . C21A C 0.4621(9) 0.2605(9) 0.0696(5) 0.120(3) Uani 1 1 d . . . H21A H 0.5418 0.2277 0.0611 0.144 Uiso 1 1 calc R . . C22A C 1.1477(5) 0.2300(5) 0.2997(3) 0.0614(14) Uani 1 1 d . A . C23A C 1.2191(6) 0.2780(7) 0.3083(4) 0.0831(18) Uani 1 1 d . . . H23A H 1.1872 0.3504 0.3189 0.100 Uiso 1 1 calc R A . C24A C 1.3385(7) 0.2175(9) 0.3012(4) 0.102(2) Uani 1 1 d . A . H24A H 1.3886 0.2486 0.3072 0.122 Uiso 1 1 calc R . . C25A C 1.3826(7) 0.1140(9) 0.2858(5) 0.118(3) Uani 1 1 d . . . H25A H 1.4635 0.0735 0.2805 0.142 Uiso 1 1 calc R A . C26A C 1.3133(8) 0.0690(8) 0.2781(6) 0.127(3) Uani 1 1 d . A . H26A H 1.3459 -0.0037 0.2679 0.153 Uiso 1 1 calc R . . C27A C 1.1964(6) 0.1254(6) 0.2845(5) 0.091(2) Uani 1 1 d . . . H27A H 1.1486 0.0920 0.2785 0.109 Uiso 1 1 calc R A . C1B C 0.2594(5) 0.6117(6) 0.5024(3) 0.0688(16) Uani 1 1 d . . . H1B H 0.3167 0.5324 0.5383 0.083 Uiso 1 1 calc R . . C2B C 0.1405(5) 0.6405(5) 0.4694(3) 0.0624(14) Uani 1 1 d . . . C3B C 0.0730(4) 0.7558(5) 0.4191(3) 0.0563(13) Uani 1 1 d . . . C4B C 0.2814(5) 0.7032(5) 0.4788(3) 0.0617(14) Uani 1 1 d . . . C5B C -0.0530(4) 0.8248(5) 0.3826(3) 0.0553(13) Uani 1 1 d . B . C9B C -0.1034(4) 0.8926(4) 0.3052(3) 0.0502(12) Uani 1 1 d . B . C10B C 0.0909(4) 0.8674(5) 0.1483(3) 0.0530(13) Uani 1 1 d . . . H10B H 0.1531 0.8159 0.1281 0.064 Uiso 1 1 calc R . . C11B C 0.0445(4) 0.8181(4) 0.2172(3) 0.0498(12) Uani 1 1 d . . . C12B C -0.0439(4) 0.9041(4) 0.2366(3) 0.0481(12) Uani 1 1 d . . . C13B C 0.0413(4) 0.9880(4) 0.1157(3) 0.0502(12) Uani 1 1 d . . . C14B C 0.1081(6) 0.5426(6) 0.4896(4) 0.088(2) Uani 1 1 d . . . H14D H 0.0943 0.5221 0.5450 0.132 Uiso 1 1 calc R . . H14E H 0.1732 0.4701 0.4842 0.132 Uiso 1 1 calc R . . H14F H 0.0358 0.5717 0.4529 0.132 Uiso 1 1 calc R . . C15B C 0.0970(5) 0.6842(5) 0.2574(3) 0.0684(15) Uani 1 1 d . . . H15D H 0.1739 0.6493 0.2910 0.103 Uiso 1 1 calc R . . H15E H 0.1081 0.6485 0.2167 0.103 Uiso 1 1 calc R . . H15F H 0.0434 0.6666 0.2909 0.103 Uiso 1 1 calc R . . C16B C 0.3868(5) 0.7100(6) 0.4981(3) 0.0686(16) Uani 1 1 d . . . C17B C 0.4849(6) 0.6077(7) 0.5516(4) 0.090(2) Uani 1 1 d . . . H17B H 0.4840 0.5336 0.5750 0.107 Uiso 1 1 calc R . . C18B C 0.5866(6) 0.6132(10) 0.5715(5) 0.111(3) Uani 1 1 d . . . H18B H 0.6542 0.5436 0.6085 0.133 Uiso 1 1 calc R . . C19B C 0.5852(8) 0.7228(12) 0.5356(5) 0.115(3) Uani 1 1 d . . . H19B H 0.6534 0.7276 0.5472 0.138 Uiso 1 1 calc R . . C20B C 0.4879(8) 0.8225(9) 0.4844(5) 0.112(3) Uani 1 1 d . . . H20B H 0.4878 0.8971 0.4616 0.134 Uiso 1 1 calc R . . C21B C 0.3892(6) 0.8173(7) 0.4650(4) 0.090(2) Uani 1 1 d . . . H21B H 0.3219 0.8880 0.4285 0.107 Uiso 1 1 calc R . . C22B C 0.0663(4) 1.0668(5) 0.0499(3) 0.0550(13) Uani 1 1 d . . . C23B C -0.0042(6) 1.1928(5) 0.0190(4) 0.0778(17) Uani 1 1 d . . . H23B H -0.0717 1.2300 0.0416 0.093 Uiso 1 1 calc R . . C24B C 0.0215(7) 1.2639(6) -0.0430(4) 0.089(2) Uani 1 1 d . . . H24B H -0.0281 1.3498 -0.0627 0.107 Uiso 1 1 calc R . . C25B C 0.1170(6) 1.2139(6) -0.0770(4) 0.0809(18) Uani 1 1 d . . . H25B H 0.1346 1.2642 -0.1200 0.097 Uiso 1 1 calc R . . C26B C 0.1877(5) 1.0898(6) -0.0483(4) 0.0751(17) Uani 1 1 d . . . H26B H 0.2544 1.0540 -0.0719 0.090 Uiso 1 1 calc R . . C27B C 0.1633(5) 1.0163(5) 0.0144(3) 0.0659(15) Uani 1 1 d . . . H27B H 0.2131 0.9304 0.0335 0.079 Uiso 1 1 calc R . . O1A O 0.4172(4) 0.4672(5) 0.2354(3) 0.1028(15) Uani 1 1 d . . . O2A O 0.3361(3) 0.6255(4) 0.1003(3) 0.1029(15) Uani 1 1 d . . . O3A O 0.9603(4) 0.4972(4) 0.3191(3) 0.0901(13) Uani 1 1 d . . . O4A O 0.9434(4) 0.5018(4) 0.1825(3) 0.0868(13) Uani 1 1 d . . . O1B O 0.0988(4) 0.9278(4) 0.4392(3) 0.0957(14) Uani 1 1 d . . . O2B O 0.1850(4) 0.8609(4) 0.3320(2) 0.0820(12) Uani 1 1 d . . . O3B O -0.0532(3) 1.1131(3) 0.2094(2) 0.0671(10) Uani 1 1 d . . . O4B O -0.1885(3) 1.1137(3) 0.1159(2) 0.0689(10) Uani 1 1 d . . . S1A S 0.43324(14) 0.51499(16) 0.15544(10) 0.0809(5) Uani 1 1 d . . . S2A S 0.93595(13) 0.45135(12) 0.26485(10) 0.0654(4) Uani 1 1 d . A . S1B S 0.15524(12) 0.83259(13) 0.40944(9) 0.0616(4) Uani 1 1 d . . . S2B S -0.07542(11) 1.04997(11) 0.16803(8) 0.0531(4) Uani 1 1 d . . . F1A F 0.7329(5) 0.7170(4) 0.2255(4) 0.156(2) Uani 1 1 d . A . F2A F 0.6932(5) 0.6433(4) 0.3367(3) 0.1257(16) Uani 1 1 d . A . F5A F 0.4471(4) 0.7905(4) 0.1053(3) 0.147(2) Uani 1 1 d . A . F6A F 0.3917(4) 0.7202(5) 0.2091(4) 0.164(2) Uani 1 1 d . A . F3A F 0.4848(6) 0.7513(7) 0.3033(4) 0.131(3) Uiso 0.681(10) 1 d P A 1 F4A F 0.5037(7) 0.8783(7) 0.1976(5) 0.121(3) Uiso 0.681(10) 1 d P A 1 C7A C 0.5328(8) 0.7544(11) 0.2369(9) 0.092(3) Uiso 0.681(10) 1 d PD A 1 F3B F 0.4912(13) 0.8555(14) 0.2439(11) 0.111(5) Uiso 0.319(10) 1 d P A 2 F4B F 0.5882(14) 0.8427(15) 0.1360(10) 0.136(7) Uiso 0.319(10) 1 d P A 2 C7B C 0.560(2) 0.7806(17) 0.1967(15) 0.092(3) Uiso 0.319(10) 1 d PD A 2 F7A F -0.1479(5) 0.9174(5) 0.4747(3) 0.0830(15) Uiso 0.668(6) 1 d P B 1 F8A F -0.1276(5) 0.7440(5) 0.4958(4) 0.0851(18) Uiso 0.668(6) 1 d P B 1 F9A F -0.3537(5) 0.9891(6) 0.4004(3) 0.0883(19) Uiso 0.668(6) 1 d P B 1 F10A F -0.2922(5) 0.8236(5) 0.3799(3) 0.0918(19) Uiso 0.668(6) 1 d P B 1 F11A F -0.2784(6) 1.0807(6) 0.2805(4) 0.0830(15) Uiso 0.668(6) 1 d P B 1 F12A F -0.2926(5) 0.9558(6) 0.2357(4) 0.0717(19) Uiso 0.668(6) 1 d P B 1 C28A C -0.2590(7) 0.9058(10) 0.3774(5) 0.078(3) Uiso 0.668(6) 1 d PD B 1 F7B F -0.1171(10) 0.8208(13) 0.5026(8) 0.095(4) Uiso 0.332(6) 1 d P B 2 F8B F -0.1555(11) 0.7244(11) 0.4472(8) 0.102(4) Uiso 0.332(6) 1 d P B 2 F9B F -0.2741(14) 1.0293(14) 0.4001(9) 0.138(6) Uiso 0.332(6) 1 d P B 2 F10B F -0.3523(13) 0.9247(15) 0.3957(8) 0.116(5) Uiso 0.332(6) 1 d P B 2 F11B F -0.2872(9) 1.0877(9) 0.2504(6) 0.056(3) Uiso 0.332(6) 1 d P B 2 F12B F -0.2884(10) 0.9196(12) 0.2617(8) 0.073(4) Uiso 0.332(6) 1 d P B 2 C28B C -0.2599(10) 0.934(2) 0.3799(6) 0.078(3) Uiso 0.332(6) 1 d PD B 2 C6B C -0.1458(5) 0.8404(6) 0.4348(4) 0.0779(17) Uani 1 1 d D . . C8B C -0.2371(5) 0.9623(5) 0.2964(3) 0.0622(14) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.066(4) 0.064(4) 0.055(4) -0.021(3) -0.002(3) -0.005(3) C2A 0.055(3) 0.058(3) 0.056(3) -0.018(3) 0.005(3) -0.002(3) C3A 0.049(3) 0.061(4) 0.065(4) -0.022(3) 0.008(3) -0.003(3) C4A 0.065(4) 0.073(4) 0.059(4) -0.020(3) -0.005(3) -0.011(3) C5A 0.061(4) 0.054(3) 0.075(4) -0.030(3) 0.019(3) -0.009(3) C6A 0.064(5) 0.074(5) 0.116(6) -0.047(5) 0.002(4) 0.011(4) C8A 0.074(4) 0.053(4) 0.088(5) -0.029(3) 0.028(4) -0.018(3) C9A 0.067(4) 0.041(3) 0.068(4) -0.025(3) 0.024(3) -0.016(3) C10A 0.060(3) 0.041(3) 0.056(3) -0.019(2) 0.006(3) -0.019(3) C11A 0.055(3) 0.053(3) 0.057(3) -0.026(3) 0.015(3) -0.026(3) C12A 0.058(3) 0.044(3) 0.065(3) -0.027(3) 0.021(3) -0.019(3) C13A 0.057(3) 0.049(3) 0.063(3) -0.027(3) 0.012(3) -0.023(3) C14A 0.067(4) 0.068(4) 0.068(4) -0.027(3) 0.015(3) -0.012(3) C15A 0.070(4) 0.064(4) 0.064(4) -0.024(3) 0.018(3) -0.036(3) C16A 0.091(5) 0.094(5) 0.060(4) -0.025(4) -0.001(4) -0.030(4) C17A 0.085(5) 0.120(6) 0.085(5) -0.026(5) -0.001(4) -0.041(5) C18A 0.129(8) 0.164(10) 0.088(6) -0.036(6) 0.006(5) -0.081(8) C19A 0.180(12) 0.214(13) 0.101(7) -0.055(8) 0.016(7) -0.137(11) C20A 0.173(11) 0.206(12) 0.155(10) -0.115(9) 0.052(9) -0.112(10) C21A 0.121(7) 0.140(8) 0.119(7) -0.074(6) 0.021(5) -0.064(6) C22A 0.053(3) 0.060(3) 0.067(4) -0.024(3) 0.010(3) -0.025(3) C23A 0.069(4) 0.104(5) 0.086(5) -0.046(4) 0.010(3) -0.043(4) C24A 0.069(5) 0.149(8) 0.088(5) -0.043(5) 0.009(4) -0.056(5) C25A 0.058(5) 0.133(8) 0.116(7) -0.040(6) 0.019(4) -0.017(5) C26A 0.078(6) 0.096(6) 0.182(9) -0.062(6) 0.040(6) -0.019(5) C27A 0.067(4) 0.062(4) 0.133(6) -0.045(4) 0.026(4) -0.019(3) C1B 0.053(3) 0.072(4) 0.062(4) -0.008(3) 0.000(3) -0.028(3) C2B 0.062(3) 0.065(4) 0.061(3) -0.018(3) 0.017(3) -0.037(3) C3B 0.052(3) 0.062(3) 0.057(3) -0.016(3) 0.010(3) -0.034(3) C4B 0.053(3) 0.076(4) 0.055(3) -0.024(3) 0.014(3) -0.032(3) C5B 0.043(3) 0.059(3) 0.069(4) -0.025(3) 0.015(3) -0.029(3) C9B 0.040(3) 0.049(3) 0.071(4) -0.029(3) 0.012(3) -0.026(2) C10B 0.044(3) 0.056(3) 0.051(3) -0.025(3) 0.007(2) -0.016(3) C11B 0.044(3) 0.042(3) 0.055(3) -0.020(2) 0.000(2) -0.014(2) C12B 0.043(3) 0.047(3) 0.053(3) -0.017(2) 0.004(2) -0.023(2) C13B 0.046(3) 0.050(3) 0.047(3) -0.015(2) 0.004(2) -0.020(3) C14B 0.081(4) 0.069(4) 0.108(5) -0.016(4) 0.019(4) -0.045(4) C15B 0.071(4) 0.049(3) 0.071(4) -0.022(3) 0.008(3) -0.020(3) C16B 0.055(4) 0.100(5) 0.055(3) -0.032(3) 0.014(3) -0.041(4) C17B 0.064(4) 0.127(6) 0.069(4) -0.039(4) 0.014(3) -0.041(4) C18B 0.062(5) 0.181(9) 0.072(5) -0.046(6) 0.009(4) -0.049(5) C19B 0.076(6) 0.201(10) 0.095(6) -0.066(7) 0.020(5) -0.082(7) C20B 0.097(6) 0.162(8) 0.117(6) -0.062(6) 0.033(5) -0.089(6) C21B 0.071(4) 0.124(6) 0.093(5) -0.039(5) 0.016(4) -0.065(4) C22B 0.053(3) 0.061(3) 0.050(3) -0.026(3) 0.008(3) -0.024(3) C23B 0.080(4) 0.055(4) 0.078(4) -0.019(3) 0.022(3) -0.023(3) C24B 0.109(5) 0.060(4) 0.084(5) -0.014(4) 0.029(4) -0.041(4) C25B 0.095(5) 0.083(5) 0.069(4) -0.022(4) 0.019(4) -0.052(4) C26B 0.072(4) 0.084(5) 0.072(4) -0.028(4) 0.023(3) -0.043(4) C27B 0.060(3) 0.065(4) 0.061(4) -0.022(3) 0.009(3) -0.025(3) O1A 0.094(3) 0.141(4) 0.074(3) -0.048(3) 0.029(3) -0.054(3) O2A 0.055(2) 0.088(3) 0.107(3) -0.036(3) -0.002(2) 0.008(2) O3A 0.098(3) 0.086(3) 0.133(4) -0.072(3) 0.040(3) -0.061(3) O4A 0.082(3) 0.063(2) 0.089(3) -0.010(2) 0.032(2) -0.029(2) O1B 0.071(3) 0.088(3) 0.150(4) -0.067(3) 0.030(3) -0.042(2) O2B 0.086(3) 0.103(3) 0.061(2) -0.007(2) 0.007(2) -0.067(3) O3B 0.082(3) 0.058(2) 0.071(2) -0.0353(19) 0.015(2) -0.034(2) O4B 0.048(2) 0.054(2) 0.078(3) -0.022(2) -0.0038(19) -0.0069(18) S1A 0.0586(10) 0.0832(11) 0.0722(11) -0.0332(9) 0.0112(8) -0.0117(9) S2A 0.0646(9) 0.0465(8) 0.0855(11) -0.0266(8) 0.0232(8) -0.0273(7) S1B 0.0522(8) 0.0636(9) 0.0710(10) -0.0202(8) 0.0082(7) -0.0340(7) S2B 0.0505(8) 0.0444(7) 0.0582(8) -0.0218(6) 0.0091(6) -0.0175(6) F1A 0.163(4) 0.075(3) 0.276(7) -0.096(4) 0.137(5) -0.076(3) F2A 0.184(5) 0.093(3) 0.117(4) -0.062(3) 0.032(3) -0.067(3) F5A 0.130(4) 0.068(3) 0.131(4) -0.024(3) -0.011(3) 0.024(3) F6A 0.090(3) 0.146(4) 0.233(6) -0.121(5) 0.061(4) -0.009(3) C6B 0.069(4) 0.086(5) 0.072(4) -0.018(4) 0.013(3) -0.042(4) C8B 0.056(3) 0.064(4) 0.082(4) -0.037(3) 0.014(3) -0.035(3) _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 C1A C4A 1.324(8) . ? C1A C2A 1.461(9) . ? C1A H1A 0.9500 . ? C2A C3A 1.353(7) . ? C2A C14A 1.490(8) . ? C3A C5A 1.456(8) . ? C3A S1A 1.793(6) . ? C4A C16A 1.473(10) . ? C4A S1A 1.779(7) . ? C5A C9A 1.346(8) . ? C5A C6A 1.517(8) . ? C6A F6A 1.323(9) . ? C6A F5A 1.331(9) . ? C6A C7A 1.449(13) . ? C6A C7B 1.59(3) . ? C8A F1A 1.307(7) . ? C8A F2A 1.313(7) . ? C8A C9A 1.509(8) . ? C8A C7A 1.515(10) . ? C8A C7B 1.519(13) . ? C9A C12A 1.463(7) . ? C10A C13A 1.342(7) . ? C10A C11A 1.465(7) . ? C10A H10A 0.9500 . ? C11A C12A 1.350(7) . ? C11A C15A 1.491(7) . ? C12A S2A 1.785(5) . ? C13A C22A 1.444(7) . ? C13A S2A 1.775(5) . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A C21A 1.360(10) . ? C16A C17A 1.430(10) . ? C17A C18A 1.358(11) . ? C17A H17A 0.9500 . ? C18A C19A 1.330(14) . ? C18A H18A 0.9500 . ? C19A C20A 1.358(14) . ? C19A H19A 0.9500 . ? C20A C21A 1.394(13) . ? C20A H20A 0.9500 . ? C21A H21A 0.9500 . ? C22A C27A 1.370(8) . ? C22A C23A 1.394(8) . ? C23A C24A 1.399(9) . ? C23A H23A 0.9500 . ? C24A C25A 1.362(11) . ? C24A H24A 0.9500 . ? C25A C26A 1.334(12) . ? C25A H25A 0.9500 . ? C26A C27A 1.364(10) . ? C26A H26A 0.9500 . ? C27A H27A 0.9500 . ? C1B C4B 1.330(8) . ? C1B C2B 1.477(7) . ? C1B H1B 0.9500 . ? C2B C3B 1.332(7) . ? C2B C14B 1.503(8) . ? C3B C5B 1.463(7) . ? C3B S1B 1.782(5) . ? C4B C16B 1.468(8) . ? C4B S1B 1.772(6) . ? C5B C9B 1.339(7) . ? C5B C6B 1.503(8) . ? C9B C12B 1.455(7) . ? C9B C8B 1.512(7) . ? C10B C13B 1.332(7) . ? C10B C11B 1.468(7) . ? C10B H10B 0.9500 . ? C11B C12B 1.339(6) . ? C11B C15B 1.486(7) . ? C12B S2B 1.781(5) . ? C13B C22B 1.453(7) . ? C13B S2B 1.788(5) . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B C17B 1.383(9) . ? C16B C21B 1.383(9) . ? C17B C18B 1.415(10) . ? C17B H17B 0.9500 . ? C18B C19B 1.391(12) . ? C18B H18B 0.9500 . ? C19B C20B 1.351(11) . ? C19B H19B 0.9500 . ? C20B C21B 1.373(9) . ? C20B H20B 0.9500 . ? C21B H21B 0.9500 . ? C22B C27B 1.389(7) . ? C22B C23B 1.390(7) . ? C23B C24B 1.361(8) . ? C23B H23B 0.9500 . ? C24B C25B 1.358(9) . ? C24B H24B 0.9500 . ? C25B C26B 1.371(8) . ? C25B H25B 0.9500 . ? C26B C27B 1.377(8) . ? C26B H26B 0.9500 . ? C27B H27B 0.9500 . ? O1A S1A 1.424(5) . ? O2A S1A 1.428(4) . ? O3A S2A 1.428(4) . ? O4A S2A 1.431(4) . ? O1B S1B 1.427(4) . ? O2B S1B 1.419(4) . ? O3B S2B 1.424(4) . ? O4B S2B 1.435(4) . ? F3A C7A 1.341(14) . ? F4A C7A 1.430(16) . ? F3B C7B 1.50(4) . ? F4B C7B 1.30(3) . ? F7A C6B 1.441(8) . ? F8A C6B 1.305(8) . ? F9A C28A 1.394(11) . ? F10A C28A 1.356(12) . ? F11A C8B 1.342(8) . ? F12A C8B 1.365(8) . ? C28A C6B 1.480(9) . ? C28A C8B 1.495(9) . ? F7B C6B 1.181(13) . ? F8B C6B 1.571(14) . ? F9B C28B 1.38(3) . ? F10B C28B 1.29(2) . ? F11B C8B 1.411(11) . ? F12B C8B 1.335(12) . ? C28B C6B 1.475(11) . ? C28B C8B 1.486(11) . ? 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 C4A C1A C2A 115.9(6) . . ? C4A C1A H1A 122.0 . . ? C2A C1A H1A 122.0 . . ? C3A C2A C1A 114.3(6) . . ? C3A C2A C14A 126.3(6) . . ? C1A C2A C14A 119.4(5) . . ? C2A C3A C5A 130.5(6) . . ? C2A C3A S1A 107.9(5) . . ? C5A C3A S1A 121.6(4) . . ? C1A C4A C16A 130.6(6) . . ? C1A C4A S1A 108.5(5) . . ? C16A C4A S1A 120.8(5) . . ? C9A C5A C3A 129.6(5) . . ? C9A C5A C6A 109.9(6) . . ? C3A C5A C6A 120.4(6) . . ? F6A C6A F5A 103.5(6) . . ? F6A C6A C7A 104.4(8) . . ? F5A C6A C7A 120.8(9) . . ? F6A C6A C5A 112.5(7) . . ? F5A C6A C5A 111.2(6) . . ? C7A C6A C5A 104.4(7) . . ? F6A C6A C7B 131.9(13) . . ? F5A C6A C7B 94.1(10) . . ? C7A C6A C7B 32.0(9) . . ? C5A C6A C7B 101.5(9) . . ? F1A C8A F2A 106.2(7) . . ? F1A C8A C9A 112.6(5) . . ? F2A C8A C9A 112.0(5) . . ? F1A C8A C7A 118.3(7) . . ? F2A C8A C7A 105.7(7) . . ? C9A C8A C7A 102.0(7) . . ? F1A C8A C7B 88.8(13) . . ? F2A C8A C7B 131.0(12) . . ? C9A C8A C7B 103.8(11) . . ? C7A C8A C7B 32.5(10) . . ? C5A C9A C12A 129.9(5) . . ? C5A C9A C8A 111.0(5) . . ? C12A C9A C8A 119.1(5) . . ? C13A C10A C11A 116.3(5) . . ? C13A C10A H10A 121.9 . . ? C11A C10A H10A 121.9 . . ? C12A C11A C10A 113.3(5) . . ? C12A C11A C15A 127.2(5) . . ? C10A C11A C15A 119.5(4) . . ? C11A C12A C9A 129.7(5) . . ? C11A C12A S2A 108.8(4) . . ? C9A C12A S2A 121.4(4) . . ? C10A C13A C22A 131.1(5) . . ? C10A C13A S2A 107.8(4) . . ? C22A C13A S2A 120.8(4) . . ? C2A C14A H14A 109.5 . . ? C2A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C2A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C11A C15A H15A 109.5 . . ? C11A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C11A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C21A C16A C17A 118.5(8) . . ? C21A C16A C4A 119.7(7) . . ? C17A C16A C4A 121.7(7) . . ? C18A C17A C16A 120.3(9) . . ? C18A C17A H17A 119.9 . . ? C16A C17A H17A 119.9 . . ? C19A C18A C17A 119.5(11) . . ? C19A C18A H18A 120.2 . . ? C17A C18A H18A 120.2 . . ? C18A C19A C20A 122.4(11) . . ? C18A C19A H19A 118.8 . . ? C20A C19A H19A 118.8 . . ? C19A C20A C21A 119.8(11) . . ? C19A C20A H20A 120.1 . . ? C21A C20A H20A 120.1 . . ? C16A C21A C20A 119.4(9) . . ? C16A C21A H21A 120.3 . . ? C20A C21A H21A 120.3 . . ? C27A C22A C23A 119.2(6) . . ? C27A C22A C13A 118.8(5) . . ? C23A C22A C13A 121.9(5) . . ? C22A C23A C24A 118.8(7) . . ? C22A C23A H23A 120.6 . . ? C24A C23A H23A 120.6 . . ? C25A C24A C23A 119.8(8) . . ? C25A C24A H24A 120.1 . . ? C23A C24A H24A 120.1 . . ? C26A C25A C24A 120.7(8) . . ? C26A C25A H25A 119.7 . . ? C24A C25A H25A 119.7 . . ? C25A C26A C27A 121.3(9) . . ? C25A C26A H26A 119.4 . . ? C27A C26A H26A 119.4 . . ? C26A C27A C22A 120.3(7) . . ? C26A C27A H27A 119.9 . . ? C22A C27A H27A 119.9 . . ? C4B C1B C2B 116.1(5) . . ? C4B C1B H1B 122.0 . . ? C2B C1B H1B 122.0 . . ? C3B C2B C1B 113.4(5) . . ? C3B C2B C14B 126.1(5) . . ? C1B C2B C14B 120.4(5) . . ? C2B C3B C5B 130.7(5) . . ? C2B C3B S1B 109.0(4) . . ? C5B C3B S1B 119.7(4) . . ? C1B C4B C16B 131.8(6) . . ? C1B C4B S1B 107.9(4) . . ? C16B C4B S1B 120.2(5) . . ? C9B C5B C3B 128.6(5) . . ? C9B C5B C6B 110.8(5) . . ? C3B C5B C6B 120.1(5) . . ? C5B C9B C12B 127.5(4) . . ? C5B C9B C8B 110.3(5) . . ? C12B C9B C8B 122.2(5) . . ? C13B C10B C11B 116.5(4) . . ? C13B C10B H10B 121.7 . . ? C11B C10B H10B 121.7 . . ? C12B C11B C10B 113.4(4) . . ? C12B C11B C15B 127.1(5) . . ? C10B C11B C15B 119.5(4) . . ? C11B C12B C9B 130.0(4) . . ? C11B C12B S2B 109.2(4) . . ? C9B C12B S2B 120.6(4) . . ? C10B C13B C22B 131.6(5) . . ? C10B C13B S2B 107.4(4) . . ? C22B C13B S2B 121.0(4) . . ? C2B C14B H14D 109.5 . . ? C2B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C2B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C11B C15B H15D 109.5 . . ? C11B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C11B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C17B C16B C21B 119.2(6) . . ? C17B C16B C4B 119.4(6) . . ? C21B C16B C4B 121.4(6) . . ? C16B C17B C18B 120.0(8) . . ? C16B C17B H17B 120.0 . . ? C18B C17B H17B 120.0 . . ? C19B C18B C17B 118.5(8) . . ? C19B C18B H18B 120.8 . . ? C17B C18B H18B 120.8 . . ? C20B C19B C18B 120.8(8) . . ? C20B C19B H19B 119.6 . . ? C18B C19B H19B 119.6 . . ? C19B C20B C21B 120.8(9) . . ? C19B C20B H20B 119.6 . . ? C21B C20B H20B 119.6 . . ? C20B C21B C16B 120.7(7) . . ? C20B C21B H21B 119.7 . . ? C16B C21B H21B 119.7 . . ? C27B C22B C23B 117.3(5) . . ? C27B C22B C13B 119.8(5) . . ? C23B C22B C13B 122.9(5) . . ? C24B C23B C22B 121.4(6) . . ? C24B C23B H23B 119.3 . . ? C22B C23B H23B 119.3 . . ? C25B C24B C23B 121.0(6) . . ? C25B C24B H24B 119.5 . . ? C23B C24B H24B 119.5 . . ? C24B C25B C26B 119.0(6) . . ? C24B C25B H25B 120.5 . . ? C26B C25B H25B 120.5 . . ? C25B C26B C27B 120.9(6) . . ? C25B C26B H26B 119.5 . . ? C27B C26B H26B 119.5 . . ? C26B C27B C22B 120.4(6) . . ? C26B C27B H27B 119.8 . . ? C22B C27B H27B 119.8 . . ? O1A S1A O2A 118.2(3) . . ? O1A S1A C4A 111.6(3) . . ? O2A S1A C4A 109.2(3) . . ? O1A S1A C3A 110.4(3) . . ? O2A S1A C3A 111.5(3) . . ? C4A S1A C3A 93.2(3) . . ? O3A S2A O4A 117.8(3) . . ? O3A S2A C13A 110.4(3) . . ? O4A S2A C13A 110.4(2) . . ? O3A S2A C12A 111.8(2) . . ? O4A S2A C12A 110.1(3) . . ? C13A S2A C12A 93.6(2) . . ? O2B S1B O1B 118.4(3) . . ? O2B S1B C4B 109.2(3) . . ? O1B S1B C4B 111.9(3) . . ? O2B S1B C3B 111.2(2) . . ? O1B S1B C3B 109.8(3) . . ? C4B S1B C3B 93.6(3) . . ? O3B S2B O4B 117.1(2) . . ? O3B S2B C12B 110.3(2) . . ? O4B S2B C12B 111.8(2) . . ? O3B S2B C13B 111.9(2) . . ? O4B S2B C13B 109.9(2) . . ? C12B S2B C13B 93.3(2) . . ? F3A C7A F4A 104.6(9) . . ? F3A C7A C6A 114.3(10) . . ? F4A C7A C6A 109.3(10) . . ? F3A C7A C8A 110.2(9) . . ? F4A C7A C8A 109.7(9) . . ? C6A C7A C8A 108.6(8) . . ? F4B C7B F3B 111.3(19) . . ? F4B C7B C8A 114(2) . . ? F3B C7B C8A 102.8(16) . . ? F4B C7B C6A 120.2(18) . . ? F3B C7B C6A 105(2) . . ? C8A C7B C6A 101.5(14) . . ? F10A C28A F9A 102.8(7) . . ? F10A C28A C6B 107.6(7) . . ? F9A C28A C6B 113.2(7) . . ? F10A C28A C8B 112.6(7) . . ? F9A C28A C8B 113.2(7) . . ? C6B C28A C8B 107.4(6) . . ? F10B C28B F9B 104.9(14) . . ? F10B C28B C6B 117.5(14) . . ? F9B C28B C6B 97.1(14) . . ? F10B C28B C8B 119.8(14) . . ? F9B C28B C8B 106.1(16) . . ? C6B C28B C8B 108.2(8) . . ? F7B C6B F8A 55.0(7) . . ? F7B C6B F7A 47.7(7) . . ? F8A C6B F7A 101.2(5) . . ? F7B C6B C28B 128.8(10) . . ? F8A C6B C28B 126.2(9) . . ? F7A C6B C28B 94.0(11) . . ? F7B C6B C28A 136.4(9) . . ? F8A C6B C28A 116.4(6) . . ? F7A C6B C28A 108.6(7) . . ? C28B C6B C28A 15.4(14) . . ? F7B C6B C5B 117.6(8) . . ? F8A C6B C5B 117.3(6) . . ? F7A C6B C5B 108.9(5) . . ? C28B C6B C5B 105.3(6) . . ? C28A C6B C5B 104.2(5) . . ? F7B C6B F8B 98.9(9) . . ? F8A C6B F8B 43.9(5) . . ? F7A C6B F8B 143.0(7) . . ? C28B C6B F8B 99.3(12) . . ? C28A C6B F8B 84.4(7) . . ? C5B C6B F8B 100.6(6) . . ? F12B C8B F11A 124.7(8) . . ? F12B C8B F12A 22.6(6) . . ? F11A C8B F12A 107.1(6) . . ? F12B C8B F11B 107.6(8) . . ? F11A C8B F11B 21.6(5) . . ? F12A C8B F11B 87.5(6) . . ? F12B C8B C28B 105.8(12) . . ? F11A C8B C28B 94.7(11) . . ? F12A C8B C28B 125.1(10) . . ? F11B C8B C28B 114.1(10) . . ? F12B C8B C28A 92.6(8) . . ? F11A C8B C28A 108.9(6) . . ? F12A C8B C28A 113.6(6) . . ? F11B C8B C28A 126.9(7) . . ? C28B C8B C28A 15.3(13) . . ? F12B C8B C9B 111.4(6) . . ? F11A C8B C9B 111.8(5) . . ? F12A C8B C9B 111.9(5) . . ? F11B C8B C9B 112.8(6) . . ? C28B C8B C9B 104.9(6) . . ? C28A C8B C9B 103.6(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 C4A C1A C2A C3A -0.9(8) . . . . ? C4A C1A C2A C14A -178.3(5) . . . . ? C1A C2A C3A C5A 174.6(6) . . . . ? C14A C2A C3A C5A -8.2(10) . . . . ? C1A C2A C3A S1A -2.1(6) . . . . ? C14A C2A C3A S1A 175.1(5) . . . . ? C2A C1A C4A C16A -178.5(6) . . . . ? C2A C1A C4A S1A 3.4(6) . . . . ? C2A C3A C5A C9A -37.6(10) . . . . ? S1A C3A C5A C9A 138.7(6) . . . . ? C2A C3A C5A C6A 140.2(7) . . . . ? S1A C3A C5A C6A -43.5(8) . . . . ? C9A C5A C6A F6A -121.4(7) . . . . ? C3A C5A C6A F6A 60.4(9) . . . . ? C9A C5A C6A F5A 123.0(7) . . . . ? C3A C5A C6A F5A -55.2(9) . . . . ? C9A C5A C6A C7A -8.8(10) . . . . ? C3A C5A C6A C7A 173.0(8) . . . . ? C9A C5A C6A C7B 23.9(13) . . . . ? C3A C5A C6A C7B -154.3(12) . . . . ? C3A C5A C9A C12A -6.7(11) . . . . ? C6A C5A C9A C12A 175.4(6) . . . . ? C3A C5A C9A C8A 173.7(6) . . . . ? C6A C5A C9A C8A -4.2(8) . . . . ? F1A C8A C9A C5A -113.0(7) . . . . ? F2A C8A C9A C5A 127.4(6) . . . . ? C7A C8A C9A C5A 14.8(8) . . . . ? C7B C8A C9A C5A -18.5(14) . . . . ? F1A C8A C9A C12A 67.3(8) . . . . ? F2A C8A C9A C12A -52.2(7) . . . . ? C7A C8A C9A C12A -164.8(7) . . . . ? C7B C8A C9A C12A 161.9(14) . . . . ? C13A C10A C11A C12A -2.1(7) . . . . ? C13A C10A C11A C15A 177.0(5) . . . . ? C10A C11A C12A C9A 175.1(5) . . . . ? C15A C11A C12A C9A -3.9(9) . . . . ? C10A C11A C12A S2A -1.3(6) . . . . ? C15A C11A C12A S2A 179.7(4) . . . . ? C5A C9A C12A C11A -42.3(9) . . . . ? C8A C9A C12A C11A 137.3(6) . . . . ? C5A C9A C12A S2A 133.8(6) . . . . ? C8A C9A C12A S2A -46.7(7) . . . . ? C11A C10A C13A C22A -168.7(5) . . . . ? C11A C10A C13A S2A 4.3(6) . . . . ? C1A C4A C16A C21A 7.8(11) . . . . ? S1A C4A C16A C21A -174.3(6) . . . . ? C1A C4A C16A C17A -171.3(7) . . . . ? S1A C4A C16A C17A 6.6(9) . . . . ? C21A C16A C17A C18A 0.4(11) . . . . ? C4A C16A C17A C18A 179.5(7) . . . . ? C16A C17A C18A C19A -1.0(13) . . . . ? C17A C18A C19A C20A 0.9(17) . . . . ? C18A C19A C20A C21A -0.2(18) . . . . ? C17A C16A C21A C20A 0.3(12) . . . . ? C4A C16A C21A C20A -178.8(8) . . . . ? C19A C20A C21A C16A -0.4(16) . . . . ? C10A C13A C22A C27A 29.0(9) . . . . ? S2A C13A C22A C27A -143.3(5) . . . . ? C10A C13A C22A C23A -153.8(6) . . . . ? S2A C13A C22A C23A 34.0(7) . . . . ? C27A C22A C23A C24A 0.0(9) . . . . ? C13A C22A C23A C24A -177.2(6) . . . . ? C22A C23A C24A C25A 0.2(11) . . . . ? C23A C24A C25A C26A -0.6(13) . . . . ? C24A C25A C26A C27A 0.6(15) . . . . ? C25A C26A C27A C22A -0.3(14) . . . . ? C23A C22A C27A C26A 0.0(11) . . . . ? C13A C22A C27A C26A 177.3(7) . . . . ? C4B C1B C2B C3B 0.9(8) . . . . ? C4B C1B C2B C14B 177.7(6) . . . . ? C1B C2B C3B C5B -170.7(5) . . . . ? C14B C2B C3B C5B 12.8(10) . . . . ? C1B C2B C3B S1B 1.0(6) . . . . ? C14B C2B C3B S1B -175.5(5) . . . . ? C2B C1B C4B C16B -179.9(5) . . . . ? C2B C1B C4B S1B -2.3(6) . . . . ? C2B C3B C5B C9B -129.4(7) . . . . ? S1B C3B C5B C9B 59.7(7) . . . . ? C2B C3B C5B C6B 59.6(8) . . . . ? S1B C3B C5B C6B -111.4(5) . . . . ? C3B C5B C9B C12B 7.1(9) . . . . ? C6B C5B C9B C12B 178.8(5) . . . . ? C3B C5B C9B C8B -171.6(5) . . . . ? C6B C5B C9B C8B 0.1(6) . . . . ? C13B C10B C11B C12B 0.8(6) . . . . ? C13B C10B C11B C15B -179.1(5) . . . . ? C10B C11B C12B C9B -172.4(5) . . . . ? C15B C11B C12B C9B 7.4(9) . . . . ? C10B C11B C12B S2B 1.6(5) . . . . ? C15B C11B C12B S2B -178.5(4) . . . . ? C5B C9B C12B C11B 47.1(8) . . . . ? C8B C9B C12B C11B -134.3(5) . . . . ? C5B C9B C12B S2B -126.3(5) . . . . ? C8B C9B C12B S2B 52.2(6) . . . . ? C11B C10B C13B C22B 177.9(5) . . . . ? C11B C10B C13B S2B -2.7(5) . . . . ? C1B C4B C16B C17B -1.8(10) . . . . ? S1B C4B C16B C17B -179.2(4) . . . . ? C1B C4B C16B C21B 179.4(6) . . . . ? S1B C4B C16B C21B 2.0(8) . . . . ? C21B C16B C17B C18B -0.5(9) . . . . ? C4B C16B C17B C18B -179.3(6) . . . . ? C16B C17B C18B C19B -0.5(10) . . . . ? C17B C18B C19B C20B 1.6(12) . . . . ? C18B C19B C20B C21B -1.7(13) . . . . ? C19B C20B C21B C16B 0.7(11) . . . . ? C17B C16B C21B C20B 0.4(10) . . . . ? C4B C16B C21B C20B 179.2(6) . . . . ? C10B C13B C22B C27B -5.8(8) . . . . ? S2B C13B C22B C27B 174.9(4) . . . . ? C10B C13B C22B C23B 173.2(6) . . . . ? S2B C13B C22B C23B -6.1(7) . . . . ? C27B C22B C23B C24B -0.7(9) . . . . ? C13B C22B C23B C24B -179.7(6) . . . . ? C22B C23B C24B C25B 0.2(11) . . . . ? C23B C24B C25B C26B 0.4(11) . . . . ? C24B C25B C26B C27B -0.4(10) . . . . ? C25B C26B C27B C22B -0.1(9) . . . . ? C23B C22B C27B C26B 0.6(8) . . . . ? C13B C22B C27B C26B 179.7(5) . . . . ? C1A C4A S1A O1A -117.3(5) . . . . ? C16A C4A S1A O1A 64.5(5) . . . . ? C1A C4A S1A O2A 110.2(5) . . . . ? C16A C4A S1A O2A -68.1(6) . . . . ? C1A C4A S1A C3A -3.9(5) . . . . ? C16A C4A S1A C3A 177.8(5) . . . . ? C2A C3A S1A O1A 117.8(4) . . . . ? C5A C3A S1A O1A -59.2(5) . . . . ? C2A C3A S1A O2A -108.8(4) . . . . ? C5A C3A S1A O2A 74.2(5) . . . . ? C2A C3A S1A C4A 3.4(4) . . . . ? C5A C3A S1A C4A -173.7(5) . . . . ? C10A C13A S2A O3A 110.7(4) . . . . ? C22A C13A S2A O3A -75.4(5) . . . . ? C10A C13A S2A O4A -117.3(4) . . . . ? C22A C13A S2A O4A 56.6(5) . . . . ? C10A C13A S2A C12A -4.2(4) . . . . ? C22A C13A S2A C12A 169.7(4) . . . . ? C11A C12A S2A O3A -110.6(4) . . . . ? C9A C12A S2A O3A 72.7(5) . . . . ? C11A C12A S2A O4A 116.4(4) . . . . ? C9A C12A S2A O4A -60.4(5) . . . . ? C11A C12A S2A C13A 3.2(4) . . . . ? C9A C12A S2A C13A -173.6(4) . . . . ? C1B C4B S1B O2B -111.5(4) . . . . ? C16B C4B S1B O2B 66.4(5) . . . . ? C1B C4B S1B O1B 115.4(4) . . . . ? C16B C4B S1B O1B -66.6(5) . . . . ? C1B C4B S1B C3B 2.4(4) . . . . ? C16B C4B S1B C3B -179.6(4) . . . . ? C2B C3B S1B O2B 110.3(4) . . . . ? C5B C3B S1B O2B -77.0(5) . . . . ? C2B C3B S1B O1B -116.8(4) . . . . ? C5B C3B S1B O1B 56.0(5) . . . . ? C2B C3B S1B C4B -2.0(4) . . . . ? C5B C3B S1B C4B 170.8(4) . . . . ? C11B C12B S2B O3B -117.5(4) . . . . ? C9B C12B S2B O3B 57.2(4) . . . . ? C11B C12B S2B O4B 110.3(4) . . . . ? C9B C12B S2B O4B -75.0(4) . . . . ? C11B C12B S2B C13B -2.7(4) . . . . ? C9B C12B S2B C13B 172.0(4) . . . . ? C10B C13B S2B O3B 116.5(4) . . . . ? C22B C13B S2B O3B -64.1(4) . . . . ? C10B C13B S2B O4B -111.6(4) . . . . ? C22B C13B S2B O4B 67.8(4) . . . . ? C10B C13B S2B C12B 3.0(4) . . . . ? C22B C13B S2B C12B -177.5(4) . . . . ? F6A C6A C7A F3A 13.0(11) . . . . ? F5A C6A C7A F3A 128.6(10) . . . . ? C5A C6A C7A F3A -105.3(9) . . . . ? C7B C6A C7A F3A 165.9(18) . . . . ? F6A C6A C7A F4A -103.9(10) . . . . ? F5A C6A C7A F4A 11.8(12) . . . . ? C5A C6A C7A F4A 137.8(8) . . . . ? C7B C6A C7A F4A 49.1(16) . . . . ? F6A C6A C7A C8A 136.5(8) . . . . ? F5A C6A C7A C8A -107.8(9) . . . . ? C5A C6A C7A C8A 18.2(12) . . . . ? C7B C6A C7A C8A -70.5(11) . . . . ? F1A C8A C7A F3A -130.2(9) . . . . ? F2A C8A C7A F3A -11.5(11) . . . . ? C9A C8A C7A F3A 105.7(9) . . . . ? C7B C8A C7A F3A -157(3) . . . . ? F1A C8A C7A F4A -15.6(13) . . . . ? F2A C8A C7A F4A 103.1(10) . . . . ? C9A C8A C7A F4A -139.6(9) . . . . ? C7B C8A C7A F4A -43(2) . . . . ? F1A C8A C7A C6A 103.9(11) . . . . ? F2A C8A C7A C6A -137.4(9) . . . . ? C9A C8A C7A C6A -20.2(11) . . . . ? C7B C8A C7A C6A 77(2) . . . . ? F1A C8A C7B F4B 13.6(19) . . . . ? F2A C8A C7B F4B 124.2(19) . . . . ? C9A C8A C7B F4B -99.4(19) . . . . ? C7A C8A C7B F4B 170(4) . . . . ? F1A C8A C7B F3B -107.0(17) . . . . ? F2A C8A C7B F3B 4(3) . . . . ? C9A C8A C7B F3B 140.0(14) . . . . ? C7A C8A C7B F3B 49.4(18) . . . . ? F1A C8A C7B C6A 144.4(15) . . . . ? F2A C8A C7B C6A -105.0(15) . . . . ? C9A C8A C7B C6A 31.4(18) . . . . ? C7A C8A C7B C6A -59.2(19) . . . . ? F6A C6A C7B F4B -131(2) . . . . ? F5A C6A C7B F4B -19.2(19) . . . . ? C7A C6A C7B F4B -168(3) . . . . ? C5A C6A C7B F4B 93.4(17) . . . . ? F6A C6A C7B F3B -5.1(18) . . . . ? F5A C6A C7B F3B 107.2(12) . . . . ? C7A C6A C7B F3B -41.4(17) . . . . ? C5A C6A C7B F3B -140.2(11) . . . . ? F6A C6A C7B C8A 101.7(16) . . . . ? F5A C6A C7B C8A -146.0(15) . . . . ? C7A C6A C7B C8A 65.4(10) . . . . ? C5A C6A C7B C8A -33.4(18) . . . . ? F10B C28B C6B F7B -67(3) . . . . ? F9B C28B C6B F7B 44.0(18) . . . . ? C8B C28B C6B F7B 153.6(13) . . . . ? F10B C28B C6B F8A 4(3) . . . . ? F9B C28B C6B F8A 115.1(14) . . . . ? C8B C28B C6B F8A -135.3(11) . . . . ? F10B C28B C6B F7A -102.9(19) . . . . ? F9B C28B C6B F7A 8.0(10) . . . . ? C8B C28B C6B F7A 117.6(15) . . . . ? F10B C28B C6B C28A 58(3) . . . . ? F9B C28B C6B C28A 169(2) . . . . ? C8B C28B C6B C28A -81.0(19) . . . . ? F10B C28B C6B C5B 146.3(16) . . . . ? F9B C28B C6B C5B -102.8(9) . . . . ? C8B C28B C6B C5B 6.8(19) . . . . ? F10B C28B C6B F8B 42(2) . . . . ? F9B C28B C6B F8B 153.4(10) . . . . ? C8B C28B C6B F8B -97.0(16) . . . . ? F10A C28A C6B F7B -93.8(15) . . . . ? F9A C28A C6B F7B 19.1(17) . . . . ? C8B C28A C6B F7B 144.8(13) . . . . ? F10A C28A C6B F8A -27.8(9) . . . . ? F9A C28A C6B F8A 85.0(10) . . . . ? C8B C28A C6B F8A -149.3(7) . . . . ? F10A C28A C6B F7A -141.2(6) . . . . ? F9A C28A C6B F7A -28.3(9) . . . . ? C8B C28A C6B F7A 97.4(8) . . . . ? F10A C28A C6B C28B -161(2) . . . . ? F9A C28A C6B C28B -48.0(18) . . . . ? C8B C28A C6B C28B 77.7(18) . . . . ? F10A C28A C6B C5B 102.9(6) . . . . ? F9A C28A C6B C5B -144.2(7) . . . . ? C8B C28A C6B C5B -18.5(9) . . . . ? F10A C28A C6B F8B 3.3(8) . . . . ? F9A C28A C6B F8B 116.2(9) . . . . ? C8B C28A C6B F8B -118.1(9) . . . . ? C9B C5B C6B F7B -155.5(9) . . . . ? C3B C5B C6B F7B 17.0(11) . . . . ? C9B C5B C6B F8A 141.8(6) . . . . ? C3B C5B C6B F8A -45.7(8) . . . . ? C9B C5B C6B F7A -104.2(5) . . . . ? C3B C5B C6B F7A 68.4(7) . . . . ? C9B C5B C6B C28B -4.3(13) . . . . ? C3B C5B C6B C28B 168.2(12) . . . . ? C9B C5B C6B C28A 11.6(8) . . . . ? C3B C5B C6B C28A -175.9(6) . . . . ? C9B C5B C6B F8B 98.5(7) . . . . ? C3B C5B C6B F8B -89.0(7) . . . . ? F10B C28B C8B F12B -27(2) . . . . ? F9B C28B C8B F12B -145.5(11) . . . . ? C6B C28B C8B F12B 111.2(15) . . . . ? F10B C28B C8B F11A 101(2) . . . . ? F9B C28B C8B F11A -17.4(10) . . . . ? C6B C28B C8B F11A -120.7(15) . . . . ? F10B C28B C8B F12A -14(2) . . . . ? F9B C28B C8B F12A -132.2(12) . . . . ? C6B C28B C8B F12A 124.5(12) . . . . ? F10B C28B C8B F11B 91(2) . . . . ? F9B C28B C8B F11B -27.3(13) . . . . ? C6B C28B C8B F11B -130.6(13) . . . . ? F10B C28B C8B C28A -58(3) . . . . ? F9B C28B C8B C28A -176(2) . . . . ? C6B C28B C8B C28A 80.5(19) . . . . ? F10B C28B C8B C9B -145.1(17) . . . . ? F9B C28B C8B C9B 96.6(9) . . . . ? C6B C28B C8B C9B -6.7(18) . . . . ? F10A C28A C8B F12B 13.0(8) . . . . ? F9A C28A C8B F12B -103.0(9) . . . . ? C6B C28A C8B F12B 131.3(9) . . . . ? F10A C28A C8B F11A 141.2(7) . . . . ? F9A C28A C8B F11A 25.1(9) . . . . ? C6B C28A C8B F11A -100.5(8) . . . . ? F10A C28A C8B F12A 21.9(9) . . . . ? F9A C28A C8B F12A -94.2(9) . . . . ? C6B C28A C8B F12A 140.2(7) . . . . ? F10A C28A C8B F11B 127.4(8) . . . . ? F9A C28A C8B F11B 11.4(12) . . . . ? C6B C28A C8B F11B -114.3(9) . . . . ? F10A C28A C8B C28B 164(2) . . . . ? F9A C28A C8B C28B 47.5(18) . . . . ? C6B C28A C8B C28B -78.2(18) . . . . ? F10A C28A C8B C9B -99.7(6) . . . . ? F9A C28A C8B C9B 144.2(7) . . . . ? C6B C28A C8B C9B 18.6(9) . . . . ? C5B C9B C8B F12B -110.0(8) . . . . ? C12B C9B C8B F12B 71.3(9) . . . . ? C5B C9B C8B F11A 105.5(6) . . . . ? C12B C9B C8B F11A -73.2(7) . . . . ? C5B C9B C8B F12A -134.4(5) . . . . ? C12B C9B C8B F12A 46.9(7) . . . . ? C5B C9B C8B F11B 128.9(6) . . . . ? C12B C9B C8B F11B -49.9(7) . . . . ? C5B C9B C8B C28B 4.1(12) . . . . ? C12B C9B C8B C28B -174.7(12) . . . . ? C5B C9B C8B C28A -11.6(7) . . . . ? C12B C9B C8B C28A 169.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.42 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.737 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.065 # Attachment '1b.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 662777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H18 F6 O4 S2' _chemical_formula_weight 584.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.866(4) _cell_length_b 13.907(5) _cell_length_c 16.158(9) _cell_angle_alpha 95.720(6) _cell_angle_beta 91.807(6) _cell_angle_gamma 117.035(4) _cell_volume 2552.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4702 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.87 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9191 _exptl_absorpt_correction_T_max 0.9191 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23480 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.15 _reflns_number_total 8067 _reflns_number_gt 5357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^+0.5000P] 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 8067 _refine_ls_number_parameters 764 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3676(3) 0.7468(3) 0.1308(2) 0.0502(9) Uani 1 1 d . A 1 H1 H 0.3108 0.7245 0.1704 0.060 Uiso 1 1 calc R A 1 C2 C 0.4655(3) 0.8614(3) 0.1406(2) 0.0463(8) Uani 1 1 d . A 1 C3 C 0.5490(3) 0.8572(3) 0.0777(2) 0.0474(9) Uani 1 1 d . A 1 C4 C 0.3619(3) 0.6773(3) 0.0658(2) 0.0517(9) Uani 1 1 d . A 1 C5 C 0.6626(3) 0.9268(3) 0.0865(2) 0.0497(9) Uani 1 1 d . A 1 C6 C 0.7592(3) 0.9421(3) 0.0315(3) 0.0580(10) Uani 1 1 d . A 1 C8 C 0.8309(3) 1.0923(3) 0.1453(3) 0.0689(12) Uani 1 1 d . A 1 C9 C 0.7103(3) 1.0090(3) 0.1594(2) 0.0482(9) Uani 1 1 d . A 1 C10 C 0.4736(3) 0.9331(3) 0.2957(2) 0.0460(8) Uani 1 1 d . A 1 H10 H 0.3927 0.8904 0.3017 0.055 Uiso 1 1 calc R A 1 C11 C 0.5324(3) 0.8966(3) 0.2296(2) 0.0429(8) Uani 1 1 d . A 1 C12 C 0.6488(3) 0.9959(2) 0.2263(2) 0.0434(8) Uani 1 1 d . A 1 C13 C 0.5364(3) 1.0261(3) 0.3458(2) 0.0446(8) Uani 1 1 d . A 1 C14 C 0.4192(3) 0.9414(3) 0.1189(3) 0.0625(10) Uani 1 1 d . A 1 H14A H 0.3891 0.9242 0.0600 0.094 Uiso 1 1 calc R A 1 H14B H 0.4831 1.0160 0.1290 0.094 Uiso 1 1 calc R A 1 H14C H 0.3561 0.9348 0.1540 0.094 Uiso 1 1 calc R A 1 C15 C 0.5537(3) 0.8036(3) 0.2572(2) 0.0521(9) Uani 1 1 d . A 1 H15A H 0.5848 0.7751 0.2118 0.078 Uiso 1 1 calc R A 1 H15B H 0.4796 0.7452 0.2708 0.078 Uiso 1 1 calc R A 1 H15C H 0.6101 0.8313 0.3066 0.078 Uiso 1 1 calc R A 1 C16 C 0.2758(3) 0.5624(3) 0.0415(2) 0.0527(9) Uani 1 1 d . A 1 C17 C 0.3087(4) 0.4880(3) 0.0024(3) 0.0698(11) Uani 1 1 d . A 1 H17 H 0.3878 0.5111 -0.0093 0.084 Uiso 1 1 calc R A 1 C18 C 0.2267(4) 0.3806(3) -0.0194(3) 0.0787(13) Uani 1 1 d . A 1 H18 H 0.2501 0.3302 -0.0456 0.094 Uiso 1 1 calc R A 1 C19 C 0.1130(4) 0.3465(3) -0.0039(3) 0.0740(13) Uani 1 1 d . A 1 H19 H 0.0570 0.2726 -0.0196 0.089 Uiso 1 1 calc R A 1 C20 C 0.0799(4) 0.4185(4) 0.0341(3) 0.0824(14) Uani 1 1 d . A 1 H20 H 0.0004 0.3945 0.0452 0.099 Uiso 1 1 calc R A 1 C21 C 0.1602(4) 0.5257(3) 0.0566(3) 0.0743(12) Uani 1 1 d . A 1 H21 H 0.1355 0.5750 0.0830 0.089 Uiso 1 1 calc R A 1 C22 C 0.5013(3) 1.0819(3) 0.4127(2) 0.0461(8) Uani 1 1 d . A 1 C23 C 0.5811(3) 1.1799(3) 0.4582(3) 0.0671(11) Uani 1 1 d . A 1 H23 H 0.6623 1.2075 0.4512 0.081 Uiso 1 1 calc R A 1 C24 C 0.5439(4) 1.2370(3) 0.5130(3) 0.0746(12) Uani 1 1 d . A 1 H24 H 0.5996 1.3045 0.5428 0.089 Uiso 1 1 calc R A 1 C25 C 0.4282(4) 1.1985(3) 0.5255(2) 0.0626(11) Uani 1 1 d . A 1 H25 H 0.4027 1.2399 0.5619 0.075 Uiso 1 1 calc R A 1 C26 C 0.3494(4) 1.0990(4) 0.4846(3) 0.0657(11) Uani 1 1 d . A 1 H26 H 0.2690 1.0697 0.4948 0.079 Uiso 1 1 calc R A 1 C27 C 0.3856(3) 1.0412(3) 0.4290(2) 0.0578(10) Uani 1 1 d . A 1 H27 H 0.3299 0.9721 0.4015 0.069 Uiso 1 1 calc R A 1 C28 C 0.9330(3) 0.4289(3) 0.3144(2) 0.0532(9) Uani 1 1 d . B 1 H28 H 0.8789 0.3557 0.3196 0.064 Uiso 1 1 calc R B 1 C30 C 0.9892(3) 0.6183(3) 0.3169(3) 0.0741(13) Uani 1 1 d . B 1 C31 C 1.0453(3) 0.4681(3) 0.3407(2) 0.0487(9) Uani 1 1 d . B 1 C32 C 0.9752(3) 0.7051(3) 0.3149(2) 0.0527(9) Uani 1 1 d . B 1 C33 C 1.0605(3) 0.8235(3) 0.3293(3) 0.0674(12) Uani 1 1 d . B 1 C35 C 0.8650(4) 0.8035(3) 0.2925(4) 0.0726(13) Uani 1 1 d . B 1 C36 C 0.8577(3) 0.6931(3) 0.2936(2) 0.0519(9) Uani 1 1 d . B 1 C37 C 0.6694(3) 0.4014(3) 0.2678(3) 0.0616(11) Uani 1 1 d . B 1 H37 H 0.6670 0.3331 0.2506 0.074 Uiso 1 1 calc R B 1 C39 C 0.7685(3) 0.5955(3) 0.2843(3) 0.0724(13) Uani 1 1 d . B 1 C40 C 0.5772(3) 0.4175(3) 0.2525(2) 0.0492(9) Uani 1 1 d . B 1 C43 C 1.1084(3) 0.4098(3) 0.3679(2) 0.0471(8) Uani 1 1 d . B 1 C44 C 1.2292(3) 0.4541(3) 0.3687(2) 0.0599(10) Uani 1 1 d . B 1 H44 H 1.2727 0.5226 0.3495 0.072 Uiso 1 1 calc R B 1 C45 C 1.2863(4) 0.3990(4) 0.3973(3) 0.0741(13) Uani 1 1 d . B 1 H45 H 1.3692 0.4300 0.3986 0.089 Uiso 1 1 calc R B 1 C46 C 1.2235(5) 0.2998(5) 0.4238(3) 0.0826(14) Uani 1 1 d . B 1 H46 H 1.2631 0.2622 0.4437 0.099 Uiso 1 1 calc R B 1 C47 C 1.1040(4) 0.2540(4) 0.4217(3) 0.0798(13) Uani 1 1 d . B 1 H47 H 1.0610 0.1843 0.4392 0.096 Uiso 1 1 calc R B 1 C48 C 1.0459(4) 0.3088(3) 0.3944(2) 0.0620(10) Uani 1 1 d . B 1 H48 H 0.9630 0.2774 0.3938 0.074 Uiso 1 1 calc R B 1 C49 C 0.4534(3) 0.3375(3) 0.2369(2) 0.0436(8) Uani 1 1 d . B 1 C50 C 0.3721(3) 0.3598(3) 0.1960(2) 0.0553(9) Uani 1 1 d . B 1 H50 H 0.3964 0.4282 0.1762 0.066 Uiso 1 1 calc R B 1 C51 C 0.2558(3) 0.2827(4) 0.1839(2) 0.0662(11) Uani 1 1 d . B 1 H51 H 0.2005 0.2984 0.1558 0.079 Uiso 1 1 calc R B 1 C52 C 0.2196(3) 0.1840(3) 0.2121(3) 0.0669(11) Uani 1 1 d . B 1 H52 H 0.1395 0.1314 0.2037 0.080 Uiso 1 1 calc R B 1 C53 C 0.2993(3) 0.1614(3) 0.2524(3) 0.0690(11) Uani 1 1 d . B 1 H53 H 0.2743 0.0926 0.2717 0.083 Uiso 1 1 calc R B 1 C54 C 0.4152(3) 0.2374(3) 0.2653(3) 0.0588(10) Uani 1 1 d . B 1 H54 H 0.4696 0.2210 0.2941 0.071 Uiso 1 1 calc R B 1 O1 O 0.4273(3) 0.7729(2) -0.06845(17) 0.0858(9) Uani 1 1 d . A 1 O2 O 0.5449(2) 0.6901(2) -0.01551(19) 0.0795(9) Uani 1 1 d . A 1 O3 O 0.7133(2) 1.19444(18) 0.29468(18) 0.0668(7) Uani 1 1 d . A 1 O4 O 0.7605(2) 1.0774(2) 0.37561(17) 0.0679(8) Uani 1 1 d . A 1 O5 O 1.2005(3) 0.6475(3) 0.2853(3) 0.1390(19) Uani 1 1 d . B 1 O6 O 1.1589(3) 0.6598(3) 0.4318(3) 0.1274(17) Uani 1 1 d . B 1 O7 O 0.5999(2) 0.5898(2) 0.1816(2) 0.0910(11) Uani 1 1 d . B 1 O8 O 0.5739(2) 0.5921(2) 0.3317(2) 0.0934(11) Uani 1 1 d . B 1 S1 S 0.47467(9) 0.74397(8) 0.00007(6) 0.0606(3) Uani 1 1 d . A 1 S2 S 0.68227(7) 1.08808(7) 0.31751(6) 0.0499(3) Uani 1 1 d . A 1 S3 S 1.11848(9) 0.61087(8) 0.34725(10) 0.0852(4) Uani 1 1 d . B 1 S4 S 0.61827(8) 0.55807(8) 0.26050(9) 0.0729(4) Uani 1 1 d . B 1 F1A F 0.7247(4) 0.9220(4) -0.0489(3) 0.0813(13) Uani 0.717(5) 1 d P A 1 F2A F 0.8073(4) 0.8774(3) 0.0501(3) 0.0776(13) Uani 0.717(5) 1 d P A 1 F3A F 0.8257(3) 1.1246(3) 0.0112(3) 0.0938(15) Uani 0.717(5) 1 d P A 1 F4A F 0.9626(3) 1.0835(4) 0.0476(4) 0.0779(14) Uani 0.717(5) 1 d P A 1 F5A F 0.8545(4) 1.1940(3) 0.1637(4) 0.119(2) Uani 0.717(5) 1 d P A 1 F6A F 0.9124(3) 1.0821(5) 0.2026(3) 0.1121(19) Uani 0.717(5) 1 d P A 1 C7A C 0.8491(5) 1.0585(6) 0.0601(5) 0.0598(17) Uani 0.717(5) 1 d P A 1 F1B F 0.7448(10) 0.9740(9) -0.0447(7) 0.071(4) Uiso 0.283(5) 1 d P A 2 F2B F 0.7750(9) 0.8531(8) 0.0042(6) 0.066(3) Uiso 0.283(5) 1 d P A 2 F3B F 0.9311(19) 1.0911(16) 0.0225(12) 0.106(7) Uiso 0.283(5) 1 d P A 2 F4B F 0.9250(7) 0.9899(7) 0.1199(5) 0.071(3) Uiso 0.283(5) 1 d P A 2 F5B F 0.8085(8) 1.1701(8) 0.0964(6) 0.072(3) Uiso 0.283(5) 1 d P A 2 F6B F 0.8993(9) 1.1477(9) 0.1998(6) 0.063(3) Uiso 0.283(5) 1 d P A 2 C7B C 0.884(2) 1.0361(18) 0.0769(13) 0.070(7) Uiso 0.283(5) 1 d P A 2 C29A C 0.8926(5) 0.5019(4) 0.2763(4) 0.0385(17) Uiso 0.605(9) 1 d P B 1 C38A C 0.7803(5) 0.4962(4) 0.3140(3) 0.0379(18) Uiso 0.605(9) 1 d P B 1 C41A C 0.8715(9) 0.4786(7) 0.1794(6) 0.054(3) Uiso 0.605(9) 1 d P B 1 H41A H 0.8099 0.4039 0.1631 0.081 Uiso 0.605(9) 1 calc PR B 1 H41B H 0.9441 0.4874 0.1557 0.081 Uiso 0.605(9) 1 calc PR B 1 H41C H 0.8473 0.5297 0.1584 0.081 Uiso 0.605(9) 1 calc PR B 1 C42A C 0.7909(10) 0.4990(8) 0.4093(7) 0.055(3) Uiso 0.605(9) 1 d P B 1 H42A H 0.7882 0.4309 0.4230 0.082 Uiso 0.605(9) 1 calc PR B 1 H42B H 0.7260 0.5077 0.4329 0.082 Uiso 0.605(9) 1 calc PR B 1 H42C H 0.8654 0.5603 0.4330 0.082 Uiso 0.605(9) 1 calc PR B 1 C29B C 0.8784(7) 0.5115(6) 0.3316(6) 0.039(3) Uiso 0.395(9) 1 d P B 2 C38B C 0.7962(7) 0.4986(6) 0.2538(5) 0.038(3) Uiso 0.395(9) 1 d P B 2 C41B C 0.8119(14) 0.4958(12) 0.4112(11) 0.053(5) Uiso 0.395(9) 1 d P B 2 H41D H 0.7483 0.4212 0.4064 0.080 Uiso 0.395(9) 1 calc PR B 2 H41E H 0.7792 0.5472 0.4177 0.080 Uiso 0.395(9) 1 calc PR B 2 H41F H 0.8661 0.5091 0.4600 0.080 Uiso 0.395(9) 1 calc PR B 2 C42B C 0.8567(13) 0.4947(11) 0.1725(9) 0.055(4) Uiso 0.395(9) 1 d P B 2 H42D H 0.8643 0.4275 0.1647 0.082 Uiso 0.395(9) 1 calc PR B 2 H42E H 0.9345 0.5576 0.1769 0.082 Uiso 0.395(9) 1 calc PR B 2 H42F H 0.8092 0.4966 0.1246 0.082 Uiso 0.395(9) 1 calc PR B 2 F7A F 1.1621(3) 0.8480(2) 0.2959(3) 0.0829(11) Uani 0.876(5) 1 d P B 1 F8A F 1.0881(4) 0.8597(3) 0.4110(3) 0.0966(13) Uani 0.876(5) 1 d P B 1 F9A F 1.0181(3) 0.8824(3) 0.2075(3) 0.1107(15) Uani 0.876(5) 1 d P B 1 F10A F 1.0314(6) 0.9785(5) 0.3224(5) 0.133(3) Uani 0.876(5) 1 d P B 1 F11A F 0.8017(3) 0.8115(2) 0.2284(3) 0.0951(13) Uani 0.876(5) 1 d P B 1 F12A F 0.8278(4) 0.8335(2) 0.3629(4) 0.1000(15) Uani 0.876(5) 1 d P B 1 C34A C 0.9960(4) 0.8790(4) 0.2895(5) 0.0760(17) Uani 0.876(5) 1 d P B 1 F7B F 1.124(4) 0.844(4) 0.260(3) 0.142(17) Uiso 0.124(5) 1 d P B 2 F8B F 1.134(4) 0.852(4) 0.391(3) 0.131(17) Uiso 0.124(5) 1 d P B 2 F9B F 1.035(3) 0.992(3) 0.3191(16) 0.053(8) Uiso 0.124(5) 1 d P B 2 F10B F 0.970(2) 0.9069(18) 0.4239(14) 0.095(8) Uiso 0.124(5) 1 d P B 2 F11B F 0.877(3) 0.825(2) 0.2124(18) 0.112(10) Uiso 0.124(5) 1 d P B 2 F12B F 0.795(4) 0.824(3) 0.316(3) 0.133(17) Uiso 0.124(5) 1 d P B 2 C34B C 0.985(3) 0.888(3) 0.348(2) 0.051(9) Uiso 0.124(5) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0373(19) 0.047(2) 0.059(2) 0.0006(18) 0.0019(16) 0.0136(16) C2 0.0354(18) 0.0375(19) 0.060(2) 0.0031(16) 0.0002(16) 0.0127(15) C3 0.049(2) 0.0389(19) 0.052(2) 0.0067(16) 0.0065(17) 0.0171(17) C4 0.041(2) 0.047(2) 0.062(2) 0.0048(18) 0.0009(17) 0.0160(17) C5 0.042(2) 0.0399(19) 0.064(2) 0.0114(17) 0.0101(17) 0.0152(17) C6 0.058(2) 0.045(2) 0.074(3) 0.010(2) 0.016(2) 0.0247(19) C8 0.045(2) 0.053(3) 0.095(3) 0.005(2) 0.013(2) 0.011(2) C9 0.0351(18) 0.0346(19) 0.069(2) 0.0035(17) 0.0038(18) 0.0115(15) C10 0.0343(18) 0.0363(19) 0.061(2) 0.0039(17) 0.0039(16) 0.0115(15) C11 0.0329(17) 0.0330(17) 0.059(2) 0.0045(15) 0.0042(15) 0.0118(14) C12 0.0332(18) 0.0309(18) 0.064(2) 0.0036(16) -0.0011(17) 0.0135(14) C13 0.0364(18) 0.0352(18) 0.060(2) 0.0020(16) 0.0005(16) 0.0153(15) C14 0.055(2) 0.060(2) 0.080(3) 0.009(2) -0.001(2) 0.033(2) C15 0.053(2) 0.0388(19) 0.065(2) 0.0089(17) 0.0038(18) 0.0203(17) C16 0.043(2) 0.041(2) 0.062(2) 0.0042(17) -0.0016(17) 0.0106(17) C17 0.059(3) 0.049(2) 0.097(3) 0.003(2) 0.000(2) 0.022(2) C18 0.080(3) 0.042(2) 0.106(4) 0.004(2) -0.003(3) 0.023(2) C19 0.073(3) 0.041(2) 0.084(3) 0.008(2) -0.004(2) 0.007(2) C20 0.053(3) 0.062(3) 0.101(4) -0.003(3) 0.010(2) 0.002(2) C21 0.053(3) 0.057(3) 0.092(3) -0.010(2) 0.009(2) 0.011(2) C22 0.045(2) 0.0407(19) 0.052(2) 0.0001(16) -0.0042(16) 0.0213(16) C23 0.049(2) 0.057(2) 0.080(3) -0.015(2) -0.002(2) 0.017(2) C24 0.071(3) 0.060(3) 0.075(3) -0.022(2) -0.005(2) 0.021(2) C25 0.077(3) 0.066(3) 0.055(2) -0.005(2) -0.003(2) 0.045(2) C26 0.055(2) 0.077(3) 0.070(3) -0.001(2) 0.006(2) 0.037(2) C27 0.044(2) 0.054(2) 0.070(3) -0.0076(19) 0.0011(18) 0.0209(18) C28 0.0333(19) 0.040(2) 0.082(3) 0.0158(18) -0.0027(18) 0.0117(16) C30 0.035(2) 0.042(2) 0.137(4) 0.023(2) -0.012(2) 0.0097(17) C31 0.0361(19) 0.043(2) 0.063(2) 0.0069(17) 0.0023(16) 0.0151(16) C32 0.0345(19) 0.038(2) 0.076(3) 0.0084(18) 0.0029(17) 0.0088(16) C33 0.042(2) 0.043(2) 0.105(4) 0.006(2) 0.002(2) 0.0098(18) C35 0.042(2) 0.043(2) 0.129(4) 0.015(3) 0.005(3) 0.0167(19) C36 0.041(2) 0.0354(19) 0.077(3) 0.0067(17) 0.0048(18) 0.0163(16) C37 0.0345(19) 0.0309(19) 0.110(3) -0.0049(19) -0.014(2) 0.0112(15) C39 0.038(2) 0.038(2) 0.136(4) -0.003(2) -0.013(2) 0.0168(18) C40 0.0363(19) 0.0363(19) 0.072(2) 0.0000(17) -0.0042(17) 0.0156(15) C43 0.045(2) 0.051(2) 0.046(2) -0.0024(16) -0.0029(16) 0.0252(17) C44 0.051(2) 0.077(3) 0.060(2) 0.000(2) 0.0032(19) 0.038(2) C45 0.063(3) 0.105(4) 0.073(3) 0.000(3) 0.000(2) 0.057(3) C46 0.105(4) 0.101(4) 0.077(3) -0.002(3) -0.008(3) 0.081(4) C47 0.092(4) 0.068(3) 0.091(3) 0.006(2) -0.011(3) 0.049(3) C48 0.058(2) 0.053(2) 0.078(3) 0.005(2) -0.006(2) 0.029(2) C49 0.0322(18) 0.042(2) 0.051(2) -0.0027(16) -0.0004(15) 0.0143(15) C50 0.041(2) 0.056(2) 0.066(2) 0.0140(19) -0.0005(18) 0.0179(18) C51 0.039(2) 0.091(3) 0.062(3) 0.011(2) -0.0086(18) 0.024(2) C52 0.041(2) 0.063(3) 0.072(3) 0.007(2) -0.0013(19) 0.004(2) C53 0.049(2) 0.052(2) 0.090(3) 0.015(2) -0.002(2) 0.009(2) C54 0.041(2) 0.044(2) 0.085(3) 0.0093(19) -0.0079(19) 0.0151(17) O1 0.090(2) 0.078(2) 0.0623(18) 0.0108(15) -0.0128(16) 0.0166(17) O2 0.0690(19) 0.0619(18) 0.101(2) -0.0096(16) 0.0231(16) 0.0271(15) O3 0.0549(16) 0.0289(13) 0.105(2) 0.0044(13) 0.0152(14) 0.0098(12) O4 0.0429(15) 0.0795(19) 0.0751(18) -0.0036(15) -0.0135(13) 0.0267(14) O5 0.0391(17) 0.121(3) 0.269(5) 0.125(3) 0.040(2) 0.0257(19) O6 0.072(2) 0.064(2) 0.225(5) -0.050(3) -0.081(3) 0.0321(18) O7 0.0577(18) 0.0571(18) 0.165(3) 0.038(2) -0.0041(19) 0.0288(15) O8 0.0544(18) 0.0592(18) 0.162(3) -0.0362(19) -0.0072(19) 0.0329(15) S1 0.0548(6) 0.0506(6) 0.0614(6) -0.0001(5) 0.0055(5) 0.0127(5) S2 0.0350(5) 0.0356(5) 0.0714(6) -0.0010(4) -0.0011(4) 0.0114(4) S3 0.0325(6) 0.0443(6) 0.1692(13) 0.0243(7) -0.0153(7) 0.0088(5) S4 0.0362(5) 0.0343(5) 0.1439(11) 0.0004(6) -0.0100(6) 0.0157(4) F1A 0.082(3) 0.064(3) 0.070(3) -0.001(2) 0.0278(19) 0.009(2) F2A 0.069(2) 0.068(2) 0.112(4) 0.024(2) 0.037(3) 0.041(2) F3A 0.088(3) 0.060(2) 0.121(3) 0.036(2) 0.003(2) 0.019(2) F4A 0.029(2) 0.081(3) 0.110(4) 0.006(3) 0.025(2) 0.014(2) F5A 0.103(3) 0.038(2) 0.167(5) -0.003(3) 0.072(4) -0.009(2) F6A 0.042(2) 0.161(5) 0.105(3) 0.039(3) 0.0025(19) 0.018(2) C7A 0.031(3) 0.062(4) 0.082(5) 0.017(4) 0.026(3) 0.015(3) F7A 0.0364(16) 0.0514(17) 0.142(3) 0.0222(18) 0.0117(19) 0.0022(13) F8A 0.092(3) 0.0524(19) 0.114(3) -0.0196(18) -0.005(2) 0.0127(19) F9A 0.070(2) 0.102(3) 0.158(4) 0.070(3) 0.026(2) 0.0268(18) F10A 0.070(2) 0.031(2) 0.279(8) 0.017(2) -0.007(3) 0.0091(18) F11A 0.057(2) 0.0599(18) 0.168(4) 0.051(2) -0.003(2) 0.0203(15) F12A 0.090(3) 0.0464(18) 0.162(4) -0.007(2) 0.035(3) 0.0322(17) C34A 0.053(3) 0.038(3) 0.125(6) 0.018(3) 0.010(3) 0.009(2) _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 C4 1.331(5) . ? C1 C2 1.504(5) . ? C1 H1 0.9500 . ? C2 C3 1.519(5) . ? C2 C14 1.543(5) . ? C2 C11 1.564(5) . ? C3 C5 1.329(5) . ? C3 S1 1.768(4) . ? C4 C16 1.474(5) . ? C4 S1 1.778(4) . ? C5 C9 1.456(5) . ? C5 C6 1.499(5) . ? C6 F1A 1.320(5) . ? C6 F2A 1.353(5) . ? C6 C7A 1.512(7) . ? C8 F5A 1.305(6) . ? C8 F6A 1.440(6) . ? C8 C7A 1.471(8) . ? C8 C9 1.498(5) . ? C9 C12 1.338(5) . ? C10 C13 1.334(4) . ? C10 C11 1.504(5) . ? C10 H10 0.9500 . ? C11 C12 1.513(4) . ? C11 C15 1.542(5) . ? C12 S2 1.756(4) . ? C13 C22 1.469(5) . ? C13 S2 1.771(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.374(5) . ? C16 C17 1.390(5) . ? C17 C18 1.381(5) . ? C17 H17 0.9500 . ? C18 C19 1.358(6) . ? C18 H18 0.9500 . ? C19 C20 1.357(6) . ? C19 H19 0.9500 . ? C20 C21 1.376(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.376(5) . ? C22 C23 1.390(5) . ? C23 C24 1.370(6) . ? C23 H23 0.9500 . ? C24 C25 1.363(6) . ? C24 H24 0.9500 . ? C25 C26 1.371(5) . ? C25 H25 0.9500 . ? C26 C27 1.376(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C31 1.329(5) . ? C28 C29A 1.505(6) . ? C28 H28 0.9500 . ? C30 C32 1.303(5) . ? C30 C29A 1.582(6) . ? C30 S3 1.770(4) . ? C31 C43 1.470(5) . ? C31 S3 1.758(4) . ? C32 C36 1.469(5) . ? C32 C33 1.495(5) . ? C33 F7A 1.338(5) . ? C33 F8A 1.341(6) . ? C33 C34A 1.531(7) . ? C35 F11A 1.343(6) . ? C35 F12A 1.348(7) . ? C35 C36 1.497(5) . ? C35 C34A 1.534(6) . ? C36 C39 1.310(5) . ? C37 C40 1.323(5) . ? C37 C38A 1.537(6) . ? C37 H37 0.9500 . ? C39 C38A 1.574(6) . ? C39 S4 1.775(4) . ? C40 C49 1.465(4) . ? C40 S4 1.768(3) . ? C43 C48 1.385(5) . ? C43 C44 1.385(5) . ? C44 C45 1.379(6) . ? C44 H44 0.9500 . ? C45 C46 1.366(7) . ? C45 H45 0.9500 . ? C46 C47 1.369(7) . ? C46 H46 0.9500 . ? C47 C48 1.377(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.382(5) . ? C49 C50 1.385(5) . ? C50 C51 1.382(5) . ? C50 H50 0.9500 . ? C51 C52 1.365(6) . ? C51 H51 0.9500 . ? C52 C53 1.366(6) . ? C52 H52 0.9500 . ? C53 C54 1.374(5) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? O1 S1 1.424(3) . ? O2 S1 1.426(3) . ? O3 S2 1.437(3) . ? O4 S2 1.422(3) . ? O5 S3 1.433(4) . ? O6 S3 1.431(4) . ? O7 S4 1.436(4) . ? O8 S4 1.432(3) . ? F3A C7A 1.393(10) . ? F4A C7A 1.365(8) . ? F3B C7B 1.21(3) . ? F4B C7B 1.25(2) . ? C29A C41A 1.556(11) . ? C29A C38A 1.557(8) . ? C38A C42A 1.537(13) . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C29B C41B 1.546(19) . ? C29B C38B 1.559(13) . ? C38B C42B 1.556(17) . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? F9A C34A 1.366(8) . ? F10A C34A 1.292(8) . ? F9B C34B 1.42(5) . ? F10B C34B 1.26(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 C2 118.9(3) . . ? C4 C1 H1 120.5 . . ? C2 C1 H1 120.5 . . ? C1 C2 C3 104.0(3) . . ? C1 C2 C14 110.6(3) . . ? C3 C2 C14 110.1(3) . . ? C1 C2 C11 112.3(3) . . ? C3 C2 C11 108.3(3) . . ? C14 C2 C11 111.3(3) . . ? C5 C3 C2 122.2(3) . . ? C5 C3 S1 127.5(3) . . ? C2 C3 S1 110.2(2) . . ? C1 C4 C16 129.8(3) . . ? C1 C4 S1 110.3(3) . . ? C16 C4 S1 119.8(3) . . ? C3 C5 C9 119.6(3) . . ? C3 C5 C6 131.7(4) . . ? C9 C5 C6 108.7(3) . . ? F1A C6 F2A 109.5(4) . . ? F1A C6 C5 113.4(4) . . ? F2A C6 C5 109.6(3) . . ? F1A C6 C7A 114.2(5) . . ? F2A C6 C7A 107.3(5) . . ? C5 C6 C7A 102.6(4) . . ? F5A C8 F6A 102.6(5) . . ? F5A C8 C7A 117.0(5) . . ? F6A C8 C7A 108.2(5) . . ? F5A C8 C9 116.4(4) . . ? F6A C8 C9 107.6(4) . . ? C7A C8 C9 104.7(4) . . ? C12 C9 C5 119.1(3) . . ? C12 C9 C8 131.5(3) . . ? C5 C9 C8 109.1(3) . . ? C13 C10 C11 119.3(3) . . ? C13 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C12 104.1(3) . . ? C10 C11 C15 109.6(3) . . ? C12 C11 C15 109.5(3) . . ? C10 C11 C2 114.7(3) . . ? C12 C11 C2 108.6(3) . . ? C15 C11 C2 110.0(3) . . ? C9 C12 C11 122.1(3) . . ? C9 C12 S2 127.4(3) . . ? C11 C12 S2 110.5(2) . . ? C10 C13 C22 130.6(3) . . ? C10 C13 S2 109.7(3) . . ? C22 C13 S2 119.6(2) . . ? C21 C16 C17 118.0(3) . . ? C21 C16 C4 120.8(4) . . ? C17 C16 C4 121.2(3) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.6(4) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.7(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 120.8(4) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C27 C22 C23 117.7(3) . . ? C27 C22 C13 120.4(3) . . ? C23 C22 C13 121.9(3) . . ? C24 C23 C22 120.7(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 121.0(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 118.9(4) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C25 C26 C27 120.6(4) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C22 C27 C26 121.0(4) . . ? C22 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C31 C28 C29A 119.0(3) . . ? C31 C28 H28 120.5 . . ? C29A C28 H28 120.5 . . ? C32 C30 C29A 122.0(4) . . ? C32 C30 S3 127.9(3) . . ? C29A C30 S3 109.4(3) . . ? C28 C31 C43 129.0(3) . . ? C28 C31 S3 111.2(3) . . ? C43 C31 S3 119.7(2) . . ? C30 C32 C36 119.2(3) . . ? C30 C32 C33 131.7(3) . . ? C36 C32 C33 109.1(3) . . ? F7A C33 F8A 106.1(4) . . ? F7A C33 C32 113.9(4) . . ? F8A C33 C32 111.4(4) . . ? F7A C33 C34A 110.8(4) . . ? F8A C33 C34A 110.4(5) . . ? C32 C33 C34A 104.2(3) . . ? F11A C35 F12A 106.7(4) . . ? F11A C35 C36 114.7(4) . . ? F12A C35 C36 110.8(4) . . ? F11A C35 C34A 111.0(4) . . ? F12A C35 C34A 109.6(5) . . ? C36 C35 C34A 104.1(3) . . ? C39 C36 C32 118.8(3) . . ? C39 C36 C35 131.9(3) . . ? C32 C36 C35 109.2(3) . . ? C40 C37 C38A 118.3(3) . . ? C40 C37 H37 120.9 . . ? C38A C37 H37 120.9 . . ? C36 C39 C38A 121.0(4) . . ? C36 C39 S4 128.1(3) . . ? C38A C39 S4 109.5(3) . . ? C37 C40 C49 129.0(3) . . ? C37 C40 S4 110.9(3) . . ? C49 C40 S4 119.9(2) . . ? C48 C43 C44 119.3(3) . . ? C48 C43 C31 119.2(3) . . ? C44 C43 C31 121.5(3) . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C46 C45 C44 119.9(4) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 120.6(4) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C46 C47 C48 120.2(5) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 119.9(4) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C54 C49 C50 118.6(3) . . ? C54 C49 C40 119.4(3) . . ? C50 C49 C40 122.0(3) . . ? C51 C50 C49 120.1(4) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C52 C51 C50 120.6(4) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 119.6(4) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C52 C53 C54 120.5(4) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C49 120.6(4) . . ? C53 C54 H54 119.7 . . ? C49 C54 H54 119.7 . . ? O1 S1 O2 119.2(2) . . ? O1 S1 C3 110.84(17) . . ? O2 S1 C3 109.62(17) . . ? O1 S1 C4 109.15(18) . . ? O2 S1 C4 112.80(18) . . ? C3 S1 C4 91.84(17) . . ? O4 S2 O3 118.00(17) . . ? O4 S2 C12 111.41(16) . . ? O3 S2 C12 108.94(17) . . ? O4 S2 C13 111.83(17) . . ? O3 S2 C13 110.74(15) . . ? C12 S2 C13 93.14(16) . . ? O6 S3 O5 117.5(3) . . ? O6 S3 C31 111.1(2) . . ? O5 S3 C31 112.1(2) . . ? O6 S3 C30 110.2(2) . . ? O5 S3 C30 110.2(2) . . ? C31 S3 C30 92.92(17) . . ? O8 S4 O7 117.9(2) . . ? O8 S4 C40 111.3(2) . . ? O7 S4 C40 111.75(19) . . ? O8 S4 C39 109.3(2) . . ? O7 S4 C39 111.1(2) . . ? C40 S4 C39 92.72(16) . . ? F4A C7A F3A 103.4(7) . . ? F4A C7A C8 114.5(6) . . ? F3A C7A C8 104.2(5) . . ? F4A C7A C6 116.0(5) . . ? F3A C7A C6 107.4(5) . . ? C8 C7A C6 110.0(5) . . ? F3B C7B F4B 126(3) . . ? C28 C29A C41A 113.4(5) . . ? C28 C29A C38A 111.5(4) . . ? C41A C29A C38A 109.8(5) . . ? C28 C29A C30 101.4(4) . . ? C41A C29A C30 118.3(5) . . ? C38A C29A C30 101.8(4) . . ? C37 C38A C42A 115.4(5) . . ? C37 C38A C29A 111.1(4) . . ? C42A C38A C29A 110.7(6) . . ? C37 C38A C39 100.1(3) . . ? C42A C38A C39 114.2(5) . . ? C29A C38A C39 104.5(4) . . ? C41B C29B C38B 110.5(9) . . ? C42B C38B C29B 110.1(8) . . ? C29B C41B H41D 109.5 . . ? C29B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C29B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C38B C42B H42D 109.5 . . ? C38B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C38B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? F10A C34A F9A 106.6(6) . . ? F10A C34A C33 113.3(6) . . ? F9A C34A C33 108.0(5) . . ? F10A C34A C35 115.1(6) . . ? F9A C34A C35 107.5(5) . . ? C33 C34A C35 106.0(4) . . ? F10B C34B F9B 105(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 C1 C2 C3 -11.7(4) . . . . ? C4 C1 C2 C14 106.4(4) . . . . ? C4 C1 C2 C11 -128.5(3) . . . . ? C1 C2 C3 C5 -154.8(3) . . . . ? C14 C2 C3 C5 86.7(4) . . . . ? C11 C2 C3 C5 -35.2(4) . . . . ? C1 C2 C3 S1 21.1(3) . . . . ? C14 C2 C3 S1 -97.4(3) . . . . ? C11 C2 C3 S1 140.6(2) . . . . ? C2 C1 C4 C16 -179.5(3) . . . . ? C2 C1 C4 S1 -3.0(4) . . . . ? C2 C3 C5 C9 1.3(5) . . . . ? S1 C3 C5 C9 -173.8(3) . . . . ? C2 C3 C5 C6 -176.4(3) . . . . ? S1 C3 C5 C6 8.5(6) . . . . ? C3 C5 C6 F1A 34.1(6) . . . . ? C9 C5 C6 F1A -143.8(4) . . . . ? C3 C5 C6 F2A -88.5(5) . . . . ? C9 C5 C6 F2A 93.6(4) . . . . ? C3 C5 C6 C7A 157.7(5) . . . . ? C9 C5 C6 C7A -20.2(5) . . . . ? C3 C5 C9 C12 17.9(5) . . . . ? C6 C5 C9 C12 -163.9(3) . . . . ? C3 C5 C9 C8 -166.7(3) . . . . ? C6 C5 C9 C8 11.5(4) . . . . ? F5A C8 C9 C12 -51.9(7) . . . . ? F6A C8 C9 C12 62.4(6) . . . . ? C7A C8 C9 C12 177.3(5) . . . . ? F5A C8 C9 C5 133.5(5) . . . . ? F6A C8 C9 C5 -112.2(4) . . . . ? C7A C8 C9 C5 2.7(5) . . . . ? C13 C10 C11 C12 -13.0(4) . . . . ? C13 C10 C11 C15 104.1(4) . . . . ? C13 C10 C11 C2 -131.5(3) . . . . ? C1 C2 C11 C10 -81.1(4) . . . . ? C3 C2 C11 C10 164.7(3) . . . . ? C14 C2 C11 C10 43.5(4) . . . . ? C1 C2 C11 C12 162.9(3) . . . . ? C3 C2 C11 C12 48.6(3) . . . . ? C14 C2 C11 C12 -72.5(3) . . . . ? C1 C2 C11 C15 43.0(4) . . . . ? C3 C2 C11 C15 -71.2(3) . . . . ? C14 C2 C11 C15 167.6(3) . . . . ? C5 C9 C12 C11 1.8(5) . . . . ? C8 C9 C12 C11 -172.4(4) . . . . ? C5 C9 C12 S2 -174.6(3) . . . . ? C8 C9 C12 S2 11.2(6) . . . . ? C10 C11 C12 C9 -158.4(3) . . . . ? C15 C11 C12 C9 84.5(4) . . . . ? C2 C11 C12 C9 -35.7(4) . . . . ? C10 C11 C12 S2 18.5(3) . . . . ? C15 C11 C12 S2 -98.6(3) . . . . ? C2 C11 C12 S2 141.2(2) . . . . ? C11 C10 C13 C22 177.9(3) . . . . ? C11 C10 C13 S2 1.4(4) . . . . ? C1 C4 C16 C21 33.7(6) . . . . ? S1 C4 C16 C21 -142.4(3) . . . . ? C1 C4 C16 C17 -146.4(4) . . . . ? S1 C4 C16 C17 37.4(5) . . . . ? C21 C16 C17 C18 -0.5(6) . . . . ? C4 C16 C17 C18 179.7(4) . . . . ? C16 C17 C18 C19 0.7(7) . . . . ? C17 C18 C19 C20 -0.6(7) . . . . ? C18 C19 C20 C21 0.3(7) . . . . ? C17 C16 C21 C20 0.3(7) . . . . ? C4 C16 C21 C20 -179.9(4) . . . . ? C19 C20 C21 C16 -0.2(7) . . . . ? C10 C13 C22 C27 -3.7(6) . . . . ? S2 C13 C22 C27 172.5(3) . . . . ? C10 C13 C22 C23 -179.8(4) . . . . ? S2 C13 C22 C23 -3.6(5) . . . . ? C27 C22 C23 C24 -4.4(6) . . . . ? C13 C22 C23 C24 171.8(4) . . . . ? C22 C23 C24 C25 1.2(7) . . . . ? C23 C24 C25 C26 2.6(7) . . . . ? C24 C25 C26 C27 -3.0(6) . . . . ? C23 C22 C27 C26 4.0(6) . . . . ? C13 C22 C27 C26 -172.3(4) . . . . ? C25 C26 C27 C22 -0.4(6) . . . . ? C29A C28 C31 C43 -169.9(4) . . . . ? C29A C28 C31 S3 14.1(5) . . . . ? C29A C30 C32 C36 15.3(7) . . . . ? S3 C30 C32 C36 -175.4(3) . . . . ? C29A C30 C32 C33 -163.2(5) . . . . ? S3 C30 C32 C33 6.1(8) . . . . ? C30 C32 C33 F7A 40.7(8) . . . . ? C36 C32 C33 F7A -138.0(4) . . . . ? C30 C32 C33 F8A -79.3(7) . . . . ? C36 C32 C33 F8A 102.0(5) . . . . ? C30 C32 C33 C34A 161.6(6) . . . . ? C36 C32 C33 C34A -17.0(5) . . . . ? C30 C32 C36 C39 5.9(6) . . . . ? C33 C32 C36 C39 -175.3(4) . . . . ? C30 C32 C36 C35 -178.0(4) . . . . ? C33 C32 C36 C35 0.8(5) . . . . ? F11A C35 C36 C39 -47.4(7) . . . . ? F12A C35 C36 C39 73.4(7) . . . . ? C34A C35 C36 C39 -168.9(5) . . . . ? F11A C35 C36 C32 137.2(4) . . . . ? F12A C35 C36 C32 -102.0(4) . . . . ? C34A C35 C36 C32 15.7(6) . . . . ? C32 C36 C39 C38A 13.4(7) . . . . ? C35 C36 C39 C38A -161.7(5) . . . . ? C32 C36 C39 S4 178.8(3) . . . . ? C35 C36 C39 S4 3.8(8) . . . . ? C38A C37 C40 C49 -156.9(4) . . . . ? C38A C37 C40 S4 18.4(5) . . . . ? C28 C31 C43 C48 -21.4(6) . . . . ? S3 C31 C43 C48 154.4(3) . . . . ? C28 C31 C43 C44 159.5(4) . . . . ? S3 C31 C43 C44 -24.7(5) . . . . ? C48 C43 C44 C45 -1.4(6) . . . . ? C31 C43 C44 C45 177.7(3) . . . . ? C43 C44 C45 C46 1.0(6) . . . . ? C44 C45 C46 C47 0.4(7) . . . . ? C45 C46 C47 C48 -1.3(7) . . . . ? C46 C47 C48 C43 0.9(6) . . . . ? C44 C43 C48 C47 0.4(6) . . . . ? C31 C43 C48 C47 -178.7(4) . . . . ? C37 C40 C49 C54 23.0(6) . . . . ? S4 C40 C49 C54 -152.0(3) . . . . ? C37 C40 C49 C50 -158.6(4) . . . . ? S4 C40 C49 C50 26.4(5) . . . . ? C54 C49 C50 C51 -0.4(5) . . . . ? C40 C49 C50 C51 -178.8(3) . . . . ? C49 C50 C51 C52 0.1(6) . . . . ? C50 C51 C52 C53 -0.1(6) . . . . ? C51 C52 C53 C54 0.5(7) . . . . ? C52 C53 C54 C49 -0.8(6) . . . . ? C50 C49 C54 C53 0.7(6) . . . . ? C40 C49 C54 C53 179.2(4) . . . . ? C5 C3 S1 O1 -93.8(4) . . . . ? C2 C3 S1 O1 90.7(3) . . . . ? C5 C3 S1 O2 39.9(4) . . . . ? C2 C3 S1 O2 -135.7(2) . . . . ? C5 C3 S1 C4 154.9(3) . . . . ? C2 C3 S1 C4 -20.7(3) . . . . ? C1 C4 S1 O1 -99.0(3) . . . . ? C16 C4 S1 O1 77.8(3) . . . . ? C1 C4 S1 O2 126.0(3) . . . . ? C16 C4 S1 O2 -57.1(3) . . . . ? C1 C4 S1 C3 13.8(3) . . . . ? C16 C4 S1 C3 -169.3(3) . . . . ? C9 C12 S2 O4 -84.9(3) . . . . ? C11 C12 S2 O4 98.4(2) . . . . ? C9 C12 S2 O3 47.0(3) . . . . ? C11 C12 S2 O3 -129.7(2) . . . . ? C9 C12 S2 C13 160.2(3) . . . . ? C11 C12 S2 C13 -16.5(2) . . . . ? C10 C13 S2 O4 -105.6(3) . . . . ? C22 C13 S2 O4 77.5(3) . . . . ? C10 C13 S2 O3 120.5(3) . . . . ? C22 C13 S2 O3 -56.4(3) . . . . ? C10 C13 S2 C12 8.9(3) . . . . ? C22 C13 S2 C12 -168.0(3) . . . . ? C28 C31 S3 O6 115.4(3) . . . . ? C43 C31 S3 O6 -61.1(3) . . . . ? C28 C31 S3 O5 -110.9(3) . . . . ? C43 C31 S3 O5 72.6(3) . . . . ? C28 C31 S3 C30 2.3(3) . . . . ? C43 C31 S3 C30 -174.1(3) . . . . ? C32 C30 S3 O6 59.7(5) . . . . ? C29A C30 S3 O6 -130.0(4) . . . . ? C32 C30 S3 O5 -71.7(5) . . . . ? C29A C30 S3 O5 98.6(4) . . . . ? C32 C30 S3 C31 173.4(5) . . . . ? C29A C30 S3 C31 -16.2(4) . . . . ? C37 C40 S4 O8 -111.0(3) . . . . ? C49 C40 S4 O8 64.8(3) . . . . ? C37 C40 S4 O7 114.9(3) . . . . ? C49 C40 S4 O7 -69.3(3) . . . . ? C37 C40 S4 C39 0.9(4) . . . . ? C49 C40 S4 C39 176.7(3) . . . . ? C36 C39 S4 O8 -71.3(5) . . . . ? C38A C39 S4 O8 95.5(4) . . . . ? C36 C39 S4 O7 60.4(5) . . . . ? C38A C39 S4 O7 -132.8(3) . . . . ? C36 C39 S4 C40 175.0(5) . . . . ? C38A C39 S4 C40 -18.2(4) . . . . ? F5A C8 C7A F4A 80.9(9) . . . . ? F6A C8 C7A F4A -34.2(8) . . . . ? C9 C8 C7A F4A -148.7(7) . . . . ? F5A C8 C7A F3A -31.5(6) . . . . ? F6A C8 C7A F3A -146.5(4) . . . . ? C9 C8 C7A F3A 99.0(4) . . . . ? F5A C8 C7A C6 -146.4(6) . . . . ? F6A C8 C7A C6 98.6(6) . . . . ? C9 C8 C7A C6 -15.9(7) . . . . ? F1A C6 C7A F4A -82.6(9) . . . . ? F2A C6 C7A F4A 39.0(9) . . . . ? C5 C6 C7A F4A 154.4(7) . . . . ? F1A C6 C7A F3A 32.6(6) . . . . ? F2A C6 C7A F3A 154.1(4) . . . . ? C5 C6 C7A F3A -90.5(5) . . . . ? F1A C6 C7A C8 145.4(5) . . . . ? F2A C6 C7A C8 -93.0(6) . . . . ? C5 C6 C7A C8 22.4(7) . . . . ? C31 C28 C29A C41A 103.3(6) . . . . ? C31 C28 C29A C38A -132.2(4) . . . . ? C31 C28 C29A C30 -24.6(5) . . . . ? C32 C30 C29A C28 -165.2(4) . . . . ? S3 C30 C29A C28 23.8(5) . . . . ? C32 C30 C29A C41A 70.1(7) . . . . ? S3 C30 C29A C41A -100.9(6) . . . . ? C32 C30 C29A C38A -50.2(6) . . . . ? S3 C30 C29A C38A 138.8(3) . . . . ? C40 C37 C38A C42A 93.1(6) . . . . ? C40 C37 C38A C29A -139.8(4) . . . . ? C40 C37 C38A C39 -29.9(5) . . . . ? C28 C29A C38A C37 -86.0(5) . . . . ? C41A C29A C38A C37 40.5(6) . . . . ? C30 C29A C38A C37 166.6(4) . . . . ? C28 C29A C38A C42A 43.6(6) . . . . ? C41A C29A C38A C42A 170.1(6) . . . . ? C30 C29A C38A C42A -63.8(6) . . . . ? C28 C29A C38A C39 166.9(4) . . . . ? C41A C29A C38A C39 -66.6(6) . . . . ? C30 C29A C38A C39 59.5(5) . . . . ? C36 C39 C38A C37 -164.5(4) . . . . ? S4 C39 C38A C37 27.6(4) . . . . ? C36 C39 C38A C42A 71.6(7) . . . . ? S4 C39 C38A C42A -96.3(6) . . . . ? C36 C39 C38A C29A -49.5(6) . . . . ? S4 C39 C38A C29A 142.6(4) . . . . ? C41B C29B C38B C42B -170.3(9) . . . . ? F7A C33 C34A F10A -83.4(7) . . . . ? F8A C33 C34A F10A 33.9(7) . . . . ? C32 C33 C34A F10A 153.7(6) . . . . ? F7A C33 C34A F9A 34.5(5) . . . . ? F8A C33 C34A F9A 151.8(4) . . . . ? C32 C33 C34A F9A -88.5(4) . . . . ? F7A C33 C34A C35 149.5(5) . . . . ? F8A C33 C34A C35 -93.2(5) . . . . ? C32 C33 C34A C35 26.5(6) . . . . ? F11A C35 C34A F10A 84.1(8) . . . . ? F12A C35 C34A F10A -33.5(8) . . . . ? C36 C35 C34A F10A -152.1(6) . . . . ? F11A C35 C34A F9A -34.5(5) . . . . ? F12A C35 C34A F9A -152.1(4) . . . . ? C36 C35 C34A F9A 89.3(5) . . . . ? F11A C35 C34A C33 -149.9(5) . . . . ? F12A C35 C34A C33 92.5(6) . . . . ? C36 C35 C34A C33 -26.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.15 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.309 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.048 # Attachment '2a.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 662778' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2-Bis-(3,5-dimethylthien-1,1dioxide-2-yl)-perfluorocyclopentene ; _chemical_name_common ;1,2-Bis-(3,5-dimethylthien-1,1dioxide-2-yl)- perfluorocyclopentene ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 F6 O4 S2' _chemical_formula_weight 460.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.151(2) _cell_length_b 8.0157(11) _cell_length_c 12.9963(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.729(2) _cell_angle_gamma 90.00 _cell_volume 1877.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 2114 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.91 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.364 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8987 _exptl_absorpt_correction_T_max 0.9308 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5091 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.91 _reflns_number_total 2108 _reflns_number_gt 1757 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^+0.5000P] 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 2108 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _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 0.08768(9) 0.2722(2) 0.26836(13) 0.0289(4) Uani 1 1 d . . . C2 C 0.09762(8) 0.1609(2) 0.19439(12) 0.0318(4) Uani 1 1 d . . . C3 C 0.15446(10) 0.0326(2) 0.22751(15) 0.0385(4) Uani 1 1 d . . . H3 H 0.1661 -0.0549 0.1828 0.046 Uiso 1 1 calc R . . C4 C 0.18776(9) 0.0474(2) 0.32279(14) 0.0373(4) Uani 1 1 d . . . C5 C 0.03728(9) 0.41523(19) 0.26139(12) 0.0295(4) Uani 1 1 d . . . C8 C 0.06078(11) 0.1617(3) 0.08609(14) 0.0475(5) Uani 1 1 d . . . H8A H 0.0235 0.0728 0.0774 0.071 Uiso 1 1 calc R . . H8B H 0.0979 0.1431 0.0383 0.071 Uiso 1 1 calc R . . H8C H 0.0366 0.2698 0.0711 0.071 Uiso 1 1 calc R . . C9 C 0.24453(11) -0.0561(3) 0.38558(18) 0.0533(5) Uani 1 1 d . . . H9A H 0.2591 -0.1493 0.3435 0.080 Uiso 1 1 calc R . . H9B H 0.2237 -0.0998 0.4464 0.080 Uiso 1 1 calc R . . H9C H 0.2881 0.0125 0.4081 0.080 Uiso 1 1 calc R . . O1 O 0.11763(7) 0.1913(2) 0.46872(11) 0.0520(4) Uani 1 1 d . . . O2 O 0.21040(7) 0.35495(18) 0.38892(10) 0.0485(4) Uani 1 1 d . . . S1 S 0.15365(2) 0.22993(6) 0.37894(3) 0.03436(19) Uani 1 1 d . . . C6 C 0.0620(8) 0.6039(16) 0.2641(10) 0.038(2) Uani 0.50 1 d P . . C7 C -0.0087(11) 0.7025(4) 0.258(2) 0.042(2) Uani 0.50 1 d P . . F1B F 0.0858(4) 0.6098(9) 0.3865(5) 0.0612(13) Uani 0.50 1 d P . . F2B F 0.13249(17) 0.6143(4) 0.2422(3) 0.0560(8) Uani 0.50 1 d P . . F3 F -0.01936(18) 0.7526(5) 0.3532(3) 0.0747(9) Uani 0.50 1 d P . . F4 F -0.00334(18) 0.8402(3) 0.2010(3) 0.0759(10) Uani 0.50 1 d P . . F1 F 0.1007(2) 0.6307(4) 0.1849(4) 0.0836(13) Uani 0.50 1 d P . . F2 F 0.1074(4) 0.6292(9) 0.3544(6) 0.084(2) Uani 0.50 1 d P . . C6B C 0.0699(8) 0.5792(17) 0.2866(10) 0.0318(19) Uani 0.50 1 d P . . 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 0.0248(8) 0.0299(8) 0.0318(8) -0.0011(6) 0.0021(6) -0.0028(6) C2 0.0280(8) 0.0310(8) 0.0365(9) -0.0020(6) 0.0044(7) -0.0030(6) C3 0.0328(9) 0.0338(9) 0.0496(10) -0.0051(7) 0.0085(8) 0.0017(7) C4 0.0298(8) 0.0353(9) 0.0476(10) 0.0017(7) 0.0082(7) 0.0023(7) C5 0.0340(8) 0.0263(8) 0.0287(8) -0.0020(6) 0.0060(6) -0.0025(6) C8 0.0514(11) 0.0510(12) 0.0385(10) -0.0128(8) -0.0012(8) 0.0071(9) C9 0.0390(10) 0.0580(13) 0.0620(13) 0.0082(10) 0.0016(9) 0.0135(9) O1 0.0441(8) 0.0771(10) 0.0354(7) 0.0062(7) 0.0077(6) 0.0055(8) O2 0.0380(7) 0.0495(8) 0.0547(8) -0.0042(6) -0.0087(6) -0.0093(6) S1 0.0293(3) 0.0392(3) 0.0339(3) -0.00072(16) 0.00080(19) 0.00009(16) C6 0.043(5) 0.019(4) 0.049(6) 0.004(3) 0.001(4) -0.007(3) C7 0.039(8) 0.0255(14) 0.063(8) 0.001(3) 0.010(5) 0.005(2) F1B 0.073(4) 0.051(2) 0.055(2) -0.0239(17) -0.0147(18) -0.006(2) F2B 0.0435(16) 0.0355(14) 0.092(3) -0.0006(16) 0.0216(15) -0.0090(12) F3 0.067(2) 0.083(2) 0.075(2) -0.0413(18) 0.0113(16) 0.0065(17) F4 0.0651(17) 0.0316(13) 0.130(3) 0.0232(14) 0.008(2) -0.0088(14) F1 0.089(3) 0.0438(17) 0.133(4) 0.011(2) 0.076(3) -0.005(2) F2 0.055(3) 0.040(2) 0.146(7) -0.023(4) -0.039(3) -0.004(2) C6B 0.032(3) 0.023(4) 0.041(5) 0.009(3) 0.008(3) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.339(2) . ? C1 C5 1.463(2) . ? C1 S1 1.7919(17) . ? C2 C3 1.484(2) . ? C2 C8 1.486(2) . ? C3 C4 1.318(3) . ? C3 H3 0.9500 . ? C4 C9 1.490(3) . ? C4 S1 1.7783(18) . ? C5 C5 1.351(3) 2 ? C5 C6B 1.463(17) . ? C5 C6 1.577(14) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O1 S1 1.4364(14) . ? O2 S1 1.4321(13) . ? C6 F1 1.330(15) . ? C6 F2 1.368(16) . ? C6 C7 1.50(2) . ? C7 F3 1.33(2) . ? C7 F4 1.341(14) . ? C7 C6B 1.55(2) 2 ? F1B C6B 1.319(16) . ? F2B C6B 1.363(15) . ? C6B C7 1.55(2) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 127.86(15) . . ? C2 C1 S1 108.42(12) . . ? C5 C1 S1 123.52(12) . . ? C1 C2 C3 113.65(15) . . ? C1 C2 C8 126.39(16) . . ? C3 C2 C8 119.88(15) . . ? C4 C3 C2 115.88(15) . . ? C4 C3 H3 122.1 . . ? C2 C3 H3 122.1 . . ? C3 C4 C9 132.51(18) . . ? C3 C4 S1 108.45(13) . . ? C9 C4 S1 119.04(15) . . ? C5 C5 C1 128.08(8) 2 . ? C5 C5 C6B 114.7(5) 2 . ? C1 C5 C6B 117.2(5) . . ? C5 C5 C6 106.2(5) 2 . ? C1 C5 C6 125.2(5) . . ? C6B C5 C6 13.3(8) . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 S1 O1 117.92(9) . . ? O2 S1 C4 109.35(8) . . ? O1 S1 C4 111.69(9) . . ? O2 S1 C1 110.26(8) . . ? O1 S1 C1 111.55(8) . . ? C4 S1 C1 93.36(8) . . ? F1 C6 F2 108.7(11) . . ? F1 C6 C7 113.7(11) . . ? F2 C6 C7 112.9(15) . . ? F1 C6 C5 108.2(10) . . ? F2 C6 C5 107.6(7) . . ? C7 C6 C5 105.4(10) . . ? F3 C7 F4 107.1(7) . . ? F3 C7 C6 109(2) . . ? F4 C7 C6 110.1(9) . . ? F3 C7 C6B 111.5(9) . 2 ? F4 C7 C6B 114(2) . 2 ? C6 C7 C6B 104.7(5) . 2 ? F1B C6B F2B 106.3(12) . . ? F1B C6B C5 115.1(9) . . ? F2B C6B C5 115.2(10) . . ? F1B C6B C7 108.5(12) . 2 ? F2B C6B C7 107.7(9) . 2 ? C5 C6B C7 103.6(12) . 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C6 C7 C6B -19.9(18) . . . 2 ? C5 C6B C7 C6 23.1(17) . . 2 2 ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.262 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.054 # Attachment '2b.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 662779' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 F6 O4 S2' _chemical_formula_weight 460.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.6990(14) _cell_length_b 15.316(2) _cell_length_c 14.199(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.291(2) _cell_angle_gamma 90.00 _cell_volume 1876.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 1825 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 22.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.364 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8987 _exptl_absorpt_correction_T_max 0.9308 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10170 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.06 _reflns_number_total 4011 _reflns_number_gt 2395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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 4011 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.2072 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _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 0.0509(5) 0.3408(2) 0.6949(3) 0.0554(11) Uani 1 1 d . . . C3 C -0.1175(5) 0.2201(3) 0.7152(3) 0.0597(12) Uani 1 1 d . . . H3 H -0.1438 0.1600 0.7170 0.072 Uiso 1 1 calc R A 1 C4 C -0.1830(5) 0.2773(3) 0.7656(3) 0.0534(10) Uani 1 1 d . C . C5 C 0.1724(4) 0.3806(2) 0.6709(3) 0.0430(9) Uani 1 1 d . C . C6 C 0.2244(5) 0.4734(3) 0.6835(3) 0.0594(11) Uani 1 1 d . . . C7 C 0.3888(6) 0.4740(3) 0.6563(5) 0.0774(15) Uani 1 1 d . C . C8 C 0.3958(5) 0.3955(3) 0.5888(3) 0.0606(11) Uani 1 1 d . . . C9 C 0.2821(4) 0.3318(2) 0.6210(3) 0.0465(9) Uani 1 1 d . C . C10 C 0.2719(5) 0.2460(3) 0.6154(3) 0.0565(11) Uani 1 1 d . . . C12 C 0.1383(4) 0.1092(2) 0.6118(3) 0.0494(10) Uani 1 1 d . . . H12 H 0.0502 0.0728 0.6131 0.059 Uiso 1 1 calc R B 1 C13 C 0.2504(4) 0.0867(2) 0.5631(3) 0.0455(9) Uani 1 1 d . C . C16 C -0.3208(5) 0.2689(3) 0.8173(3) 0.0574(11) Uani 1 1 d . . . H16A H -0.3534 0.2076 0.8172 0.086 Uiso 1 1 calc R C . H16B H -0.4055 0.3047 0.7859 0.086 Uiso 1 1 calc R . . H16C H -0.2940 0.2888 0.8830 0.086 Uiso 1 1 calc R . . C17 C 0.2809(5) 0.0022(3) 0.5174(3) 0.0644(12) Uani 1 1 d . . . H17A H 0.3782 -0.0227 0.5484 0.097 Uiso 1 1 calc R C . H17B H 0.2889 0.0119 0.4500 0.097 Uiso 1 1 calc R . . H17C H 0.1956 -0.0384 0.5237 0.097 Uiso 1 1 calc R . . F1 F 0.2110(3) 0.50850(18) 0.7676(2) 0.0917(10) Uani 1 1 d . C . F2 F 0.1359(4) 0.52728(19) 0.6232(3) 0.1051(11) Uani 1 1 d . C . F3 F 0.4814(4) 0.4539(2) 0.7410(3) 0.1089(11) Uani 1 1 d . . . F4 F 0.4382(4) 0.54705(19) 0.6294(3) 0.1166(13) Uani 1 1 d . . . F5 F 0.5396(3) 0.36527(17) 0.5921(2) 0.0837(9) Uani 1 1 d . C . F6 F 0.3489(4) 0.4242(2) 0.5009(2) 0.1006(10) Uani 1 1 d . C . O1 O -0.0130(4) 0.3969(2) 0.8619(2) 0.0720(9) Uani 1 1 d . . . O2 O -0.1805(4) 0.44610(19) 0.7202(2) 0.0751(9) Uani 1 1 d . . . O3 O 0.5269(4) 0.1524(2) 0.6176(3) 0.0808(10) Uani 1 1 d . . . O4 O 0.3953(4) 0.1971(2) 0.4624(2) 0.0875(11) Uani 1 1 d . . . S1 S -0.08733(12) 0.37904(7) 0.76755(8) 0.0569(4) Uani 1 1 d . C . S2 S 0.38503(13) 0.17175(7) 0.55795(8) 0.0587(4) Uani 1 1 d . C . C2A C 0.0020(6) 0.2521(3) 0.6533(4) 0.0397(15) Uiso 0.754(10) 1 d P C 1 C11A C 0.1533(6) 0.1962(3) 0.6667(4) 0.0397(15) Uiso 0.754(10) 1 d P C 1 C14 C -0.0671(9) 0.2569(5) 0.5481(5) 0.056(2) Uiso 0.754(10) 1 d P C 1 H14A H 0.0140 0.2736 0.5096 0.085 Uiso 0.754(10) 1 calc PR C 1 H14B H -0.1504 0.3004 0.5403 0.085 Uiso 0.754(10) 1 calc PR C 1 H14C H -0.1090 0.1996 0.5273 0.085 Uiso 0.754(10) 1 calc PR C 1 C15 C 0.2101(9) 0.1806(5) 0.7732(6) 0.049(2) Uiso 0.754(10) 1 d P C 1 H15A H 0.2118 0.2363 0.8074 0.073 Uiso 0.754(10) 1 calc PR C 1 H15B H 0.3148 0.1558 0.7800 0.073 Uiso 0.754(10) 1 calc PR C 1 H15C H 0.1397 0.1400 0.7996 0.073 Uiso 0.754(10) 1 calc PR C 1 C2B C 0.0644(17) 0.2334(9) 0.7090(11) 0.039(5) Uiso 0.246(10) 1 d P C 2 C11B C 0.0971(18) 0.2059(9) 0.6110(12) 0.041(4) Uiso 0.246(10) 1 d P C 2 C14B C 0.190(3) 0.1899(16) 0.7898(19) 0.055(7) Uiso 0.246(10) 1 d P C 2 H14D H 0.1663 0.2077 0.8527 0.082 Uiso 0.246(10) 1 calc PR C 2 H14E H 0.2940 0.2096 0.7810 0.082 Uiso 0.246(10) 1 calc PR C 2 H14F H 0.1842 0.1261 0.7845 0.082 Uiso 0.246(10) 1 calc PR C 2 C15B C -0.039(3) 0.2376(15) 0.5377(17) 0.054(6) Uiso 0.246(10) 1 d P C 2 H15D H -0.0234 0.2991 0.5224 0.081 Uiso 0.246(10) 1 calc PR C 2 H15E H -0.1368 0.2314 0.5647 0.081 Uiso 0.246(10) 1 calc PR C 2 H15F H -0.0433 0.2024 0.4798 0.081 Uiso 0.246(10) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.057(2) 0.038(2) 0.077(3) -0.0151(19) 0.034(2) -0.0060(17) C3 0.058(3) 0.038(2) 0.090(3) -0.012(2) 0.034(2) -0.0162(18) C4 0.050(2) 0.048(2) 0.066(3) -0.0049(19) 0.021(2) -0.0072(18) C5 0.051(2) 0.0318(19) 0.049(2) -0.0024(15) 0.0167(18) -0.0043(15) C6 0.073(3) 0.038(2) 0.073(3) -0.001(2) 0.034(2) -0.010(2) C7 0.072(3) 0.042(3) 0.126(5) -0.008(3) 0.044(3) -0.019(2) C8 0.059(3) 0.053(3) 0.077(3) 0.003(2) 0.033(2) -0.009(2) C9 0.048(2) 0.042(2) 0.053(2) 0.0003(17) 0.0188(18) -0.0055(16) C10 0.054(2) 0.041(2) 0.081(3) -0.010(2) 0.033(2) -0.0067(18) C12 0.050(2) 0.033(2) 0.067(3) -0.0022(17) 0.012(2) -0.0023(16) C13 0.047(2) 0.040(2) 0.050(2) -0.0013(16) 0.0083(18) 0.0031(16) C16 0.049(2) 0.054(3) 0.073(3) -0.004(2) 0.023(2) -0.0063(18) C17 0.069(3) 0.049(2) 0.080(3) -0.018(2) 0.028(2) -0.002(2) F1 0.106(2) 0.0564(17) 0.123(3) -0.0342(16) 0.0562(19) -0.0269(15) F2 0.097(2) 0.0586(18) 0.163(3) 0.0382(19) 0.030(2) 0.0098(16) F3 0.082(2) 0.104(3) 0.139(3) -0.047(2) 0.007(2) -0.0102(18) F4 0.137(3) 0.0569(18) 0.177(3) -0.0203(18) 0.103(3) -0.0416(17) F5 0.0577(16) 0.0676(17) 0.135(2) -0.0211(16) 0.0490(16) -0.0128(13) F6 0.121(3) 0.099(2) 0.089(2) 0.0298(18) 0.0415(19) -0.021(2) O1 0.0604(19) 0.077(2) 0.082(2) -0.0303(17) 0.0242(17) -0.0166(16) O2 0.074(2) 0.0432(17) 0.113(3) -0.0001(16) 0.0300(19) 0.0043(15) O3 0.0442(18) 0.079(2) 0.119(3) -0.030(2) 0.0110(18) 0.0008(15) O4 0.106(3) 0.072(2) 0.098(3) 0.0159(18) 0.063(2) 0.0062(19) S1 0.0533(6) 0.0430(6) 0.0803(8) -0.0170(5) 0.0319(6) -0.0108(4) S2 0.0562(7) 0.0441(6) 0.0821(8) -0.0075(5) 0.0328(6) 0.0000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.302(5) . ? C1 C2A 1.521(6) . ? C1 C2B 1.660(15) . ? C1 S1 1.780(4) . ? C3 C4 1.307(5) . ? C3 C2A 1.524(6) . ? C3 C2B 1.609(15) . ? C3 H3 0.9500 . ? C4 C16 1.488(5) . ? C4 S1 1.765(4) . ? C5 C9 1.463(5) . ? C5 C6 1.496(5) . ? C6 F1 1.327(5) . ? C6 F2 1.356(5) . ? C6 C7 1.528(6) . ? C7 F4 1.274(5) . ? C7 F3 1.394(6) . ? C7 C8 1.544(7) . ? C8 F5 1.329(5) . ? C8 F6 1.337(5) . ? C8 C9 1.502(5) . ? C9 C10 1.318(5) . ? C10 C11A 1.538(6) . ? C10 C11B 1.634(15) . ? C10 S2 1.770(4) . ? C12 C13 1.310(5) . ? C12 C11B 1.523(15) . ? C12 C11A 1.541(6) . ? C12 H12 0.9500 . ? C13 C17 1.487(5) . ? C13 S2 1.759(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O1 S1 1.437(3) . ? O2 S1 1.423(3) . ? O3 S2 1.437(3) . ? O4 S2 1.425(3) . ? C2A C14 1.540(9) . ? C2A C11A 1.561(7) . ? C11A C15 1.549(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C2B C11B 1.51(2) . ? C2B C14B 1.62(3) . ? C11B C15B 1.55(3) . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 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 C5 C1 C2A 120.9(3) . . ? C5 C1 C2B 116.6(6) . . ? C2A C1 C2B 34.2(5) . . ? C5 C1 S1 128.9(3) . . ? C2A C1 S1 110.1(3) . . ? C2B C1 S1 107.4(5) . . ? C4 C3 C2A 118.6(4) . . ? C4 C3 C2B 116.5(6) . . ? C2A C3 C2B 35.0(5) . . ? C4 C3 H3 120.7 . . ? C2A C3 H3 120.7 . . ? C2B C3 H3 111.4 . . ? C3 C4 C16 130.3(4) . . ? C3 C4 S1 111.2(3) . . ? C16 C4 S1 118.5(3) . . ? C1 C5 C9 119.2(3) . . ? C1 C5 C6 131.0(4) . . ? C9 C5 C6 109.7(3) . . ? F1 C6 F2 102.4(4) . . ? F1 C6 C5 115.6(3) . . ? F2 C6 C5 111.4(4) . . ? F1 C6 C7 114.6(4) . . ? F2 C6 C7 108.1(4) . . ? C5 C6 C7 104.7(3) . . ? F4 C7 F3 105.8(4) . . ? F4 C7 C6 116.3(4) . . ? F3 C7 C6 103.7(4) . . ? F4 C7 C8 117.2(4) . . ? F3 C7 C8 107.4(4) . . ? C6 C7 C8 105.3(4) . . ? F5 C8 F6 108.8(4) . . ? F5 C8 C9 114.6(4) . . ? F6 C8 C9 111.3(4) . . ? F5 C8 C7 111.1(4) . . ? F6 C8 C7 106.9(4) . . ? C9 C8 C7 103.7(3) . . ? C10 C9 C5 119.7(3) . . ? C10 C9 C8 132.1(4) . . ? C5 C9 C8 108.1(3) . . ? C9 C10 C11A 120.6(4) . . ? C9 C10 C11B 115.6(6) . . ? C11A C10 C11B 32.3(5) . . ? C9 C10 S2 129.1(3) . . ? C11A C10 S2 110.2(3) . . ? C11B C10 S2 108.0(6) . . ? C13 C12 C11B 116.2(6) . . ? C13 C12 C11A 118.2(4) . . ? C11B C12 C11A 33.7(6) . . ? C13 C12 H12 120.9 . . ? C11B C12 H12 112.3 . . ? C11A C12 H12 120.9 . . ? C12 C13 C17 130.1(4) . . ? C12 C13 S2 111.8(3) . . ? C17 C13 S2 118.0(3) . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 S1 O1 117.7(2) . . ? O2 S1 C4 113.0(2) . . ? O1 S1 C4 109.7(2) . . ? O2 S1 C1 110.4(2) . . ? O1 S1 C1 110.2(2) . . ? C4 S1 C1 93.01(18) . . ? O4 S2 O3 117.7(2) . . ? O4 S2 C13 111.4(2) . . ? O3 S2 C13 110.44(19) . . ? O4 S2 C10 111.7(2) . . ? O3 S2 C10 110.3(2) . . ? C13 S2 C10 92.54(18) . . ? C1 C2A C3 103.9(3) . . ? C1 C2A C14 112.9(4) . . ? C3 C2A C14 111.3(4) . . ? C1 C2A C11A 104.6(4) . . ? C3 C2A C11A 112.3(4) . . ? C14 C2A C11A 111.3(5) . . ? C10 C11A C12 102.0(3) . . ? C10 C11A C15 112.8(4) . . ? C12 C11A C15 110.9(4) . . ? C10 C11A C2A 106.0(4) . . ? C12 C11A C2A 113.4(4) . . ? C15 C11A C2A 111.3(5) . . ? C11B C2B C3 108.4(11) . . ? C11B C2B C14B 110.4(15) . . ? C3 C2B C14B 119.1(13) . . ? C11B C2B C1 100.6(10) . . ? C3 C2B C1 94.4(8) . . ? C14B C2B C1 121.6(12) . . ? C2B C11B C12 109.6(12) . . ? C2B C11B C15B 108.2(14) . . ? C12 C11B C15B 117.9(13) . . ? C2B C11B C10 98.2(11) . . ? C12 C11B C10 98.5(9) . . ? C15B C11B C10 122.4(13) . . ? C2B C14B H14D 109.5 . . ? C2B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C2B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C11B C15B H15D 109.5 . . ? C11B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C11B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A C3 C4 C16 167.4(4) . . . . ? C2B C3 C4 C16 -153.1(7) . . . . ? C2A C3 C4 S1 -11.6(6) . . . . ? C2B C3 C4 S1 28.0(8) . . . . ? C2A C1 C5 C9 -13.8(6) . . . . ? C2B C1 C5 C9 25.1(8) . . . . ? S1 C1 C5 C9 171.6(3) . . . . ? C2A C1 C5 C6 164.6(4) . . . . ? C2B C1 C5 C6 -156.5(7) . . . . ? S1 C1 C5 C6 -10.0(8) . . . . ? C1 C5 C6 F1 43.2(7) . . . . ? C9 C5 C6 F1 -138.2(4) . . . . ? C1 C5 C6 F2 -73.1(6) . . . . ? C9 C5 C6 F2 105.5(4) . . . . ? C1 C5 C6 C7 170.3(5) . . . . ? C9 C5 C6 C7 -11.1(5) . . . . ? F1 C6 C7 F4 -75.8(6) . . . . ? F2 C6 C7 F4 37.6(6) . . . . ? C5 C6 C7 F4 156.4(5) . . . . ? F1 C6 C7 F3 39.9(5) . . . . ? F2 C6 C7 F3 153.3(4) . . . . ? C5 C6 C7 F3 -87.9(4) . . . . ? F1 C6 C7 C8 152.6(4) . . . . ? F2 C6 C7 C8 -94.0(5) . . . . ? C5 C6 C7 C8 24.9(5) . . . . ? F4 C7 C8 F5 76.0(6) . . . . ? F3 C7 C8 F5 -42.8(5) . . . . ? C6 C7 C8 F5 -152.9(4) . . . . ? F4 C7 C8 F6 -42.5(6) . . . . ? F3 C7 C8 F6 -161.4(3) . . . . ? C6 C7 C8 F6 88.5(4) . . . . ? F4 C7 C8 C9 -160.3(5) . . . . ? F3 C7 C8 C9 80.9(4) . . . . ? C6 C7 C8 C9 -29.2(5) . . . . ? C1 C5 C9 C10 -11.7(6) . . . . ? C6 C5 C9 C10 169.5(4) . . . . ? C1 C5 C9 C8 171.2(4) . . . . ? C6 C5 C9 C8 -7.5(5) . . . . ? F5 C8 C9 C10 -32.5(7) . . . . ? F6 C8 C9 C10 91.5(6) . . . . ? C7 C8 C9 C10 -153.8(5) . . . . ? F5 C8 C9 C5 144.0(4) . . . . ? F6 C8 C9 C5 -92.0(4) . . . . ? C7 C8 C9 C5 22.7(5) . . . . ? C5 C9 C10 C11A -4.2(6) . . . . ? C8 C9 C10 C11A 172.0(4) . . . . ? C5 C9 C10 C11B 32.1(8) . . . . ? C8 C9 C10 C11B -151.7(8) . . . . ? C5 C9 C10 S2 178.5(3) . . . . ? C8 C9 C10 S2 -5.3(8) . . . . ? C11B C12 C13 C17 -153.4(8) . . . . ? C11A C12 C13 C17 168.7(4) . . . . ? C11B C12 C13 S2 29.3(8) . . . . ? C11A C12 C13 S2 -8.7(5) . . . . ? C3 C4 S1 O2 113.6(4) . . . . ? C16 C4 S1 O2 -65.4(4) . . . . ? C3 C4 S1 O1 -112.8(4) . . . . ? C16 C4 S1 O1 68.1(4) . . . . ? C3 C4 S1 C1 -0.1(4) . . . . ? C16 C4 S1 C1 -179.2(4) . . . . ? C5 C1 S1 O2 70.1(5) . . . . ? C2A C1 S1 O2 -104.9(3) . . . . ? C2B C1 S1 O2 -141.0(6) . . . . ? C5 C1 S1 O1 -61.6(5) . . . . ? C2A C1 S1 O1 123.3(3) . . . . ? C2B C1 S1 O1 87.2(6) . . . . ? C5 C1 S1 C4 -173.9(5) . . . . ? C2A C1 S1 C4 11.0(4) . . . . ? C2B C1 S1 C4 -25.1(6) . . . . ? C12 C13 S2 O4 -120.2(3) . . . . ? C17 C13 S2 O4 62.0(4) . . . . ? C12 C13 S2 O3 107.0(3) . . . . ? C17 C13 S2 O3 -70.7(4) . . . . ? C12 C13 S2 C10 -5.8(3) . . . . ? C17 C13 S2 C10 176.5(3) . . . . ? C9 C10 S2 O4 -50.4(5) . . . . ? C11A C10 S2 O4 132.1(3) . . . . ? C11B C10 S2 O4 97.9(7) . . . . ? C9 C10 S2 O3 82.5(5) . . . . ? C11A C10 S2 O3 -95.0(4) . . . . ? C11B C10 S2 O3 -129.2(7) . . . . ? C9 C10 S2 C13 -164.6(4) . . . . ? C11A C10 S2 C13 17.9(4) . . . . ? C11B C10 S2 C13 -16.3(7) . . . . ? C5 C1 C2A C3 167.3(4) . . . . ? C2B C1 C2A C3 74.5(9) . . . . ? S1 C1 C2A C3 -17.2(4) . . . . ? C5 C1 C2A C14 -71.9(6) . . . . ? C2B C1 C2A C14 -164.7(11) . . . . ? S1 C1 C2A C14 103.6(5) . . . . ? C5 C1 C2A C11A 49.3(6) . . . . ? C2B C1 C2A C11A -43.4(9) . . . . ? S1 C1 C2A C11A -135.1(3) . . . . ? C4 C3 C2A C1 19.0(6) . . . . ? C2B C3 C2A C1 -77.2(10) . . . . ? C4 C3 C2A C14 -102.9(5) . . . . ? C2B C3 C2A C14 160.9(11) . . . . ? C4 C3 C2A C11A 131.5(5) . . . . ? C2B C3 C2A C11A 35.3(9) . . . . ? C9 C10 C11A C12 159.2(4) . . . . ? C11B C10 C11A C12 69.0(10) . . . . ? S2 C10 C11A C12 -23.1(4) . . . . ? C9 C10 C11A C15 -81.7(6) . . . . ? C11B C10 C11A C15 -171.9(11) . . . . ? S2 C10 C11A C15 96.0(5) . . . . ? C9 C10 C11A C2A 40.3(6) . . . . ? C11B C10 C11A C2A -49.9(10) . . . . ? S2 C10 C11A C2A -141.9(3) . . . . ? C13 C12 C11A C10 20.7(5) . . . . ? C11B C12 C11A C10 -74.9(11) . . . . ? C13 C12 C11A C15 -99.7(5) . . . . ? C11B C12 C11A C15 164.6(12) . . . . ? C13 C12 C11A C2A 134.2(4) . . . . ? C11B C12 C11A C2A 38.6(11) . . . . ? C1 C2A C11A C10 -57.5(5) . . . . ? C3 C2A C11A C10 -169.5(4) . . . . ? C14 C2A C11A C10 64.9(5) . . . . ? C1 C2A C11A C12 -168.5(4) . . . . ? C3 C2A C11A C12 79.4(5) . . . . ? C14 C2A C11A C12 -46.2(6) . . . . ? C1 C2A C11A C15 65.6(5) . . . . ? C3 C2A C11A C15 -46.5(6) . . . . ? C14 C2A C11A C15 -172.1(5) . . . . ? C4 C3 C2B C11B -144.9(9) . . . . ? C2A C3 C2B C11B -42.2(9) . . . . ? C4 C3 C2B C14B 87.8(14) . . . . ? C2A C3 C2B C14B -169.5(19) . . . . ? C4 C3 C2B C1 -42.2(9) . . . . ? C2A C3 C2B C1 60.4(8) . . . . ? C5 C1 C2B C11B -59.6(11) . . . . ? C2A C1 C2B C11B 46.9(9) . . . . ? S1 C1 C2B C11B 147.2(9) . . . . ? C5 C1 C2B C3 -169.2(5) . . . . ? C2A C1 C2B C3 -62.7(8) . . . . ? S1 C1 C2B C3 37.5(8) . . . . ? C5 C1 C2B C14B 62.5(15) . . . . ? C2A C1 C2B C14B 169(2) . . . . ? S1 C1 C2B C14B -90.8(14) . . . . ? C3 C2B C11B C12 -90.3(12) . . . . ? C14B C2B C11B C12 41.9(16) . . . . ? C1 C2B C11B C12 171.5(8) . . . . ? C3 C2B C11B C15B 39.5(15) . . . . ? C14B C2B C11B C15B 171.7(15) . . . . ? C1 C2B C11B C15B -58.7(14) . . . . ? C3 C2B C11B C10 167.6(8) . . . . ? C14B C2B C11B C10 -60.2(14) . . . . ? C1 C2B C11B C10 69.4(10) . . . . ? C13 C12 C11B C2B -140.0(9) . . . . ? C11A C12 C11B C2B -37.8(9) . . . . ? C13 C12 C11B C15B 95.7(13) . . . . ? C11A C12 C11B C15B -162(2) . . . . ? C13 C12 C11B C10 -38.2(10) . . . . ? C11A C12 C11B C10 64.1(9) . . . . ? C9 C10 C11B C2B -65.2(11) . . . . ? C11A C10 C11B C2B 42.2(9) . . . . ? S2 C10 C11B C2B 141.7(8) . . . . ? C9 C10 C11B C12 -176.5(6) . . . . ? C11A C10 C11B C12 -69.1(10) . . . . ? S2 C10 C11B C12 30.3(9) . . . . ? C9 C10 C11B C15B 52.5(15) . . . . ? C11A C10 C11B C15B 160(2) . . . . ? S2 C10 C11B C15B -100.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.767 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.067