# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2011 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Fourmigue, Marc' _publ_contact_author_name 'Fourmigue, Marc' _publ_contact_author_email marc.fourmigue@univ-rennes1.fr _publ_section_title ; A binaphtol-substituted tetrathiafulvalene with axial chirality and its enantiopure TCNQF4 charge-transfer salts ; # Attachment '-R--1-TCNQF4.cif' data_-R--1-TCNQF4 _database_code_depnum_ccdc_archive 'CCDC 809759' #TrackingRef '-R--1-TCNQF4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 O2 S6, C12 F4 N4, C H2 Cl2' _chemical_formula_sum 'C43 H22 Cl2 F4 N4 O2 S6' _chemical_formula_weight 965.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.5380(2) _cell_length_b 12.9927(3) _cell_length_c 18.7805(5) _cell_angle_alpha 106.5700(10) _cell_angle_beta 90.8370(10) _cell_angle_gamma 92.7430(10) _cell_volume 1993.68(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8962 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.81 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.973 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.916962 #-------------------------------------------------------------------# _diffrn_ambient_temperature 150(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 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26784 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13579 _reflns_number_gt 11819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1243P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(7) _refine_ls_number_reflns 13579 _refine_ls_number_parameters 1137 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 S1 S 0.73196(16) 0.21483(11) 0.59488(8) 0.0241(3) Uani 1 1 d . . . S2 S 0.9172(2) 0.12869(13) 0.46133(10) 0.0407(4) Uani 1 1 d . . . S4 S 0.74367(17) 0.43444(11) 0.58594(8) 0.0281(3) Uani 1 1 d . A . S5 S 0.57081(14) 0.50959(10) 0.74540(7) 0.0197(3) Uani 1 1 d . . . S6 S 0.55788(15) 0.28653(10) 0.74906(7) 0.0215(3) Uani 1 1 d . . . O1 O 0.6119(4) 0.6086(3) 0.93532(19) 0.0223(8) Uani 1 1 d . . . O2 O 0.5098(4) 0.4039(3) 0.96077(19) 0.0212(7) Uani 1 1 d . . . C1 C 0.6859(6) 0.3456(4) 0.6340(3) 0.0212(11) Uani 1 1 d . . . C2 C 0.8367(7) 0.2393(5) 0.5226(4) 0.0319(13) Uani 1 1 d . A . C3 C 0.8470(8) 0.3435(5) 0.5204(4) 0.0399(16) Uani 1 1 d . . . S3 S 0.9779(6) 0.3975(2) 0.4686(2) 0.0348(13) Uani 0.629(12) 1 d P A 1 C4 C 0.978(3) 0.2789(14) 0.3831(9) 0.068(5) Uani 0.629(12) 1 d P A 1 H4A H 0.8753 0.2685 0.3587 0.082 Uiso 0.629(12) 1 calc PR A 1 H4B H 1.0536 0.2943 0.3489 0.082 Uiso 0.629(12) 1 calc PR A 1 C5 C 1.013(2) 0.1903(12) 0.3979(9) 0.059(4) Uani 0.629(12) 1 d P A 1 H5A H 1.1222 0.2007 0.4138 0.071 Uiso 0.629(12) 1 calc PR A 1 H5B H 1.0079 0.1355 0.3503 0.071 Uiso 0.629(12) 1 calc PR A 1 S3A S 0.8934(11) 0.3900(4) 0.4388(4) 0.036(2) Uani 0.371(12) 1 d P A 2 C4A C 1.034(3) 0.290(2) 0.4048(16) 0.044(6) Uiso 0.371(12) 1 d P A 2 H4A1 H 1.0852 0.2994 0.3610 0.052 Uiso 0.371(12) 1 calc PR A 2 H4A2 H 1.1133 0.2908 0.4426 0.052 Uiso 0.371(12) 1 calc PR A 2 C5A C 0.917(2) 0.1792(13) 0.3848(8) 0.024(4) Uani 0.371(12) 1 d P A 2 H5A1 H 0.9544 0.1262 0.3417 0.028 Uiso 0.371(12) 1 calc PR A 2 H5A2 H 0.8116 0.1955 0.3736 0.028 Uiso 0.371(12) 1 calc PR A 2 C6 C 0.6086(6) 0.3779(4) 0.7008(3) 0.0192(10) Uani 1 1 d . . . C7 C 0.5036(6) 0.4844(4) 0.8263(3) 0.0190(10) Uani 1 1 d . . . C8 C 0.4981(6) 0.3797(4) 0.8274(3) 0.0191(10) Uani 1 1 d . . . C9 C 0.4684(6) 0.5796(4) 0.8905(3) 0.0212(11) Uani 1 1 d . . . H9A H 0.4376 0.6390 0.8727 0.025 Uiso 1 1 calc R . . H9B H 0.3841 0.5607 0.9193 0.025 Uiso 1 1 calc R . . C10 C 0.4431(6) 0.3392(4) 0.8910(3) 0.0222(11) Uani 1 1 d . . . H10A H 0.3297 0.3396 0.8927 0.027 Uiso 1 1 calc R . . H10B H 0.4723 0.2655 0.8827 0.027 Uiso 1 1 calc R . . C11 C 0.5823(6) 0.6441(4) 1.0120(3) 0.0228(11) Uani 1 1 d . . . C12 C 0.4961(7) 0.7351(5) 1.0403(4) 0.0306(13) Uani 1 1 d . . . H12 H 0.4598 0.7724 1.0084 0.037 Uiso 1 1 calc R . . C13 C 0.4651(7) 0.7695(4) 1.1134(3) 0.0283(12) Uani 1 1 d . . . H13 H 0.4068 0.8296 1.1316 0.034 Uiso 1 1 calc R . . C14 C 0.5223(7) 0.7129(5) 1.1621(3) 0.0286(13) Uani 1 1 d . . . C15 C 0.4850(7) 0.7433(5) 1.2379(3) 0.0330(13) Uani 1 1 d . . . H15 H 0.4258 0.8028 1.2565 0.040 Uiso 1 1 calc R . . C16 C 0.5345(7) 0.6865(6) 1.2846(3) 0.0378(15) Uani 1 1 d . . . H16 H 0.5063 0.7065 1.3341 0.045 Uiso 1 1 calc R . . C17 C 0.6265(7) 0.5993(5) 1.2582(3) 0.0303(13) Uani 1 1 d . . . H17 H 0.6619 0.5625 1.2907 0.036 Uiso 1 1 calc R . . C18 C 0.6664(6) 0.5662(4) 1.1847(3) 0.0233(11) Uani 1 1 d . . . H18 H 0.7272 0.5071 1.1675 0.028 Uiso 1 1 calc R . . C19 C 0.6134(6) 0.6234(4) 1.1345(3) 0.0214(11) Uani 1 1 d . . . C20 C 0.6454(6) 0.5883(4) 1.0569(3) 0.0183(10) Uani 1 1 d . . . C21 C 0.7398(6) 0.4936(4) 1.0246(3) 0.0198(10) Uani 1 1 d . . . C22 C 0.9026(6) 0.4938(5) 1.0430(3) 0.0262(12) Uani 1 1 d . . . C23 C 0.9832(6) 0.5858(5) 1.0910(3) 0.0303(13) Uani 1 1 d . . . H23 H 0.9297 0.6477 1.1111 0.036 Uiso 1 1 calc R . . C24 C 1.1406(7) 0.5845(7) 1.1082(4) 0.0428(17) Uani 1 1 d . . . H24 H 1.1927 0.6463 1.1385 0.051 Uiso 1 1 calc R . . C25 C 1.2240(7) 0.4902(7) 1.0802(4) 0.0436(17) Uani 1 1 d . . . H25 H 1.3295 0.4892 1.0930 0.052 Uiso 1 1 calc R . . C26 C 1.1473(7) 0.4015(6) 1.0347(4) 0.0382(15) Uani 1 1 d . . . H26 H 1.2023 0.3398 1.0165 0.046 Uiso 1 1 calc R . . C27 C 0.9876(6) 0.3991(5) 1.0137(3) 0.0282(12) Uani 1 1 d . . . C28 C 0.9082(7) 0.3078(5) 0.9624(3) 0.0291(12) Uani 1 1 d . . . H28 H 0.9622 0.2461 0.9424 0.035 Uiso 1 1 calc R . . C29 C 0.7537(7) 0.3102(4) 0.9426(3) 0.0232(11) Uani 1 1 d . . . H29 H 0.7046 0.2510 0.9080 0.028 Uiso 1 1 calc R . . C30 C 0.6684(6) 0.4019(4) 0.9743(3) 0.0188(10) Uani 1 1 d . . . S1B S 0.25227(16) 0.46440(10) 1.63266(7) 0.0231(3) Uani 1 1 d . . . S2B S 0.12882(17) 0.59417(11) 1.77044(8) 0.0292(3) Uani 1 1 d . . . S3B S 0.03426(18) 0.34389(12) 1.80334(8) 0.0326(3) Uani 1 1 d . . . S4B S 0.19795(15) 0.25617(10) 1.66004(7) 0.0218(3) Uani 1 1 d . . . S5B S 0.37345(14) 0.14629(10) 1.50172(7) 0.0198(3) Uani 1 1 d . B . S6B S 0.41284(16) 0.35989(10) 1.48175(7) 0.0238(3) Uani 1 1 d . B . O1B O 0.4349(4) 0.0444(3) 1.28770(19) 0.0198(7) Uani 1 1 d . . . O2B O 0.3665(4) 0.2727(3) 1.29733(19) 0.0226(8) Uani 1 1 d . B . C1B C 0.2734(6) 0.3282(4) 1.6038(3) 0.0196(10) Uani 1 1 d . B . C2B C 0.1623(6) 0.4651(4) 1.7154(3) 0.0213(11) Uani 1 1 d . B . C3B C -0.038(3) 0.5692(16) 1.8134(13) 0.034(6) Uani 0.35(3) 1 d P B 3 H3B1 H -0.0690 0.6353 1.8482 0.041 Uiso 0.35(3) 1 calc PR B 3 H3B2 H -0.1227 0.5429 1.7766 0.041 Uiso 0.35(3) 1 calc PR B 3 C4B C -0.011(3) 0.4864(17) 1.8543(12) 0.024(5) Uani 0.35(3) 1 d P B 3 H4B1 H -0.1032 0.4823 1.8829 0.029 Uiso 0.35(3) 1 calc PR B 3 H4B2 H 0.0753 0.5153 1.8898 0.029 Uiso 0.35(3) 1 calc PR B 3 C3C C 0.0313(14) 0.5654(8) 1.8506(7) 0.032(4) Uani 0.65(3) 1 d P B 4 H3C1 H 0.1112 0.5624 1.8871 0.039 Uiso 0.65(3) 1 calc PR B 4 H3C2 H -0.0336 0.6245 1.8734 0.039 Uiso 0.65(3) 1 calc PR B 4 C4C C -0.0705(16) 0.4609(10) 1.8314(8) 0.024(3) Uani 0.65(3) 1 d P B 4 H4C1 H -0.1448 0.4611 1.7919 0.029 Uiso 0.65(3) 1 calc PR B 4 H4C2 H -0.1302 0.4587 1.8746 0.029 Uiso 0.65(3) 1 calc PR B 4 C5B C 0.1333(6) 0.3676(5) 1.7276(3) 0.0247(11) Uani 1 1 d . B . C6B C 0.3475(6) 0.2812(4) 1.5364(3) 0.0197(10) Uani 1 1 d . . . C7B C 0.4493(6) 0.1541(4) 1.4186(3) 0.0201(10) Uani 1 1 d . . . C8B C 0.4666(6) 0.2531(4) 1.4092(3) 0.0206(11) Uani 1 1 d . B . C9B C 0.4909(6) 0.0482(4) 1.3614(3) 0.0206(10) Uani 1 1 d . B . H9B1 H 0.6037 0.0426 1.3614 0.025 Uiso 1 1 calc R . . H9B2 H 0.4439 -0.0124 1.3754 0.025 Uiso 1 1 calc R . . C10B C 0.5118(6) 0.2793(5) 1.3392(3) 0.0238(11) Uani 1 1 d . . . H10C H 0.5616 0.3510 1.3505 0.029 Uiso 1 1 calc R B . H10D H 0.5836 0.2281 1.3115 0.029 Uiso 1 1 calc R . . C11B C 0.2745(6) 0.0258(4) 1.2710(3) 0.0187(10) Uani 1 1 d . . . C12B C 0.1824(6) -0.0456(4) 1.2998(3) 0.0241(11) Uani 1 1 d . . . H12B H 0.2268 -0.0772 1.3333 0.029 Uiso 1 1 calc R . . C13B C 0.0285(7) -0.0682(5) 1.2782(3) 0.0290(13) Uani 1 1 d . . . H13B H -0.0305 -0.1174 1.2957 0.035 Uiso 1 1 calc R . . C14B C -0.0427(6) -0.0175(5) 1.2295(3) 0.0272(12) Uani 1 1 d . . . C15B C -0.2070(7) -0.0312(6) 1.2112(4) 0.0425(17) Uani 1 1 d . . . H15B H -0.2680 -0.0799 1.2283 0.051 Uiso 1 1 calc R . . C16B C -0.2754(8) 0.0235(7) 1.1705(4) 0.0464(18) Uani 1 1 d . . . H16B H -0.3830 0.0140 1.1606 0.056 Uiso 1 1 calc R . . C17B C -0.1838(7) 0.0966(6) 1.1420(4) 0.0419(16) Uani 1 1 d . . . H17B H -0.2315 0.1332 1.1124 0.050 Uiso 1 1 calc R . . C18B C -0.0257(7) 0.1134(5) 1.1581(3) 0.0314(13) Uani 1 1 d . . . H18B H 0.0326 0.1625 1.1401 0.038 Uiso 1 1 calc R . . C19B C 0.0497(6) 0.0566(5) 1.2018(3) 0.0237(11) Uani 1 1 d . . . C20B C 0.2141(6) 0.0725(4) 1.2196(3) 0.0201(11) Uani 1 1 d . . . C21B C 0.3140(6) 0.1377(4) 1.1827(3) 0.0173(10) Uani 1 1 d . B . C22B C 0.3391(6) 0.0979(4) 1.1043(3) 0.0203(10) Uani 1 1 d . . . C23B C 0.2757(6) -0.0035(4) 1.0610(3) 0.0228(11) Uani 1 1 d . . . H23B H 0.2135 -0.0458 1.0830 0.027 Uiso 1 1 calc R . . C24B C 0.3053(7) -0.0399(5) 0.9869(3) 0.0287(12) Uani 1 1 d . . . H24B H 0.2621 -0.1065 0.9589 0.034 Uiso 1 1 calc R . . C25B C 0.4011(7) 0.0227(5) 0.9521(3) 0.0321(13) Uani 1 1 d . . . H25B H 0.4216 -0.0033 0.9018 0.039 Uiso 1 1 calc R . . C26B C 0.4620(7) 0.1193(5) 0.9916(3) 0.0315(13) Uani 1 1 d . . . H26B H 0.5236 0.1599 0.9680 0.038 Uiso 1 1 calc R . . C27B C 0.4346(6) 0.1619(5) 1.0694(3) 0.0241(11) Uani 1 1 d . . . C28B C 0.4989(7) 0.2633(5) 1.1113(3) 0.0301(13) Uani 1 1 d . . . H28B H 0.5570 0.3057 1.0878 0.036 Uiso 1 1 calc R . . C29B C 0.4770(7) 0.3002(5) 1.1862(3) 0.0282(12) Uani 1 1 d . B . H29B H 0.5219 0.3665 1.2138 0.034 Uiso 1 1 calc R . . C30B C 0.3845(6) 0.2355(4) 1.2212(3) 0.0209(10) Uani 1 1 d . . . N1D N 0.2327(6) 0.1410(4) 0.7785(3) 0.0348(12) Uani 1 1 d . . . N2D N 0.1224(7) -0.1584(4) 0.8126(3) 0.0346(12) Uani 1 1 d . . . N3D N 0.8434(7) -0.1619(5) 0.4156(3) 0.0393(13) Uani 1 1 d . . . N4D N 0.6560(7) -0.4638(5) 0.4329(3) 0.0456(15) Uani 1 1 d . . . F1D F 0.6300(4) -0.0336(2) 0.54020(18) 0.0264(7) Uani 1 1 d . . . F2D F 0.4505(4) 0.0567(3) 0.64941(18) 0.0277(7) Uani 1 1 d . . . F3D F 0.3441(4) -0.2823(3) 0.69204(18) 0.0288(7) Uani 1 1 d . . . F4D F 0.5241(4) -0.3719(2) 0.58433(17) 0.0261(7) Uani 1 1 d . . . C1D C 0.5853(6) -0.2092(4) 0.5540(3) 0.0203(10) Uani 1 1 d . . . C2D C 0.5622(6) -0.0964(4) 0.5777(3) 0.0207(10) Uani 1 1 d . . . C3D C 0.4682(6) -0.0504(4) 0.6360(3) 0.0210(11) Uani 1 1 d . . . C4D C 0.3869(6) -0.1066(4) 0.6785(3) 0.0204(11) Uani 1 1 d . . . C5D C 0.4149(6) -0.2188(4) 0.6554(3) 0.0231(11) Uani 1 1 d . . . C6D C 0.5060(6) -0.2663(4) 0.5976(3) 0.0202(11) Uani 1 1 d . . . C7D C 0.2867(6) -0.0589(4) 0.7373(3) 0.0219(11) Uani 1 1 d . . . C8D C 0.2606(6) 0.0529(4) 0.7597(3) 0.0240(11) Uani 1 1 d . . . C9D C 0.1997(6) -0.1185(4) 0.7771(3) 0.0235(11) Uani 1 1 d . . . C10D C 0.6732(6) -0.2596(4) 0.4909(3) 0.0228(11) Uani 1 1 d . . . C11D C 0.7628(7) -0.2008(5) 0.4503(3) 0.0284(12) Uani 1 1 d . . . C12D C 0.6669(7) -0.3736(5) 0.4597(3) 0.0281(12) Uani 1 1 d . . . N1E N 0.6288(6) 0.0880(4) 0.8124(3) 0.0295(11) Uani 1 1 d . . . N2E N 0.5938(7) -0.2285(4) 0.8236(3) 0.0395(13) Uani 1 1 d . . . N3E N 1.3003(6) -0.1076(4) 0.4528(3) 0.0298(11) Uani 1 1 d . . . N4E N 1.2383(7) -0.4241(4) 0.4600(3) 0.0385(13) Uani 1 1 d . . . F1E F 1.0543(4) -0.0177(3) 0.57267(19) 0.0313(8) Uani 1 1 d . . . F2E F 0.8613(4) 0.0417(2) 0.68218(18) 0.0291(7) Uani 1 1 d . . . F3E F 0.8088(4) -0.3177(2) 0.69524(17) 0.0270(7) Uani 1 1 d . . . F4E F 1.0006(4) -0.3768(2) 0.58538(19) 0.0297(7) Uani 1 1 d . . . C1E C 1.0376(6) -0.2011(4) 0.5719(3) 0.0200(10) Uani 1 1 d . . . C2E C 0.9938(6) -0.0945(4) 0.6012(3) 0.0226(11) Uani 1 1 d . . . C3E C 0.8938(6) -0.0630(4) 0.6595(3) 0.0216(11) Uani 1 1 d . . . C5E C 0.8683(6) -0.2422(4) 0.6656(3) 0.0188(10) Uani 1 1 d . . . C6E C 0.9662(6) -0.2737(4) 0.6072(3) 0.0192(10) Uani 1 1 d . . . C7E C 0.7224(6) -0.1028(4) 0.7554(3) 0.0202(10) Uani 1 1 d . . . C9E C 0.6551(7) -0.1752(5) 0.7923(3) 0.0278(12) Uani 1 1 d . . . C8E C 0.6751(7) 0.0050(5) 0.7864(3) 0.0249(11) Uani 1 1 d . . . C4E C 0.8245(6) -0.1344(4) 0.6957(3) 0.0182(10) Uani 1 1 d . . . C10E C 1.1452(6) -0.2331(4) 0.5141(3) 0.0200(10) Uani 1 1 d . . . C11E C 1.2234(6) -0.1605(5) 0.4811(3) 0.0231(11) Uani 1 1 d . . . C12E C 1.1937(7) -0.3401(5) 0.4857(3) 0.0264(12) Uani 1 1 d . . . C1F C 0.1483(11) 0.5142(8) 0.2764(5) 0.062(2) Uani 1 1 d . . . H1F1 H 0.2240 0.5184 0.2392 0.075 Uiso 1 1 calc R . . H1F2 H 0.2039 0.4994 0.3175 0.075 Uiso 1 1 calc R . . Cl1F Cl 0.0092(4) 0.4108(2) 0.23846(16) 0.0894(8) Uani 1 1 d . . . Cl2F Cl 0.0582(3) 0.6391(2) 0.30846(14) 0.0758(7) Uani 1 1 d . . . C1G C 0.8053(17) 0.8790(12) 0.9808(9) 0.120(5) Uiso 1 1 d . C 5 H1G1 H 0.7336 0.9070 1.0204 0.144 Uiso 1 1 calc R C 5 H1G2 H 0.7444 0.8292 0.9405 0.144 Uiso 1 1 calc R C 5 Cl1G Cl 0.8726(4) 0.9835(3) 0.95000(18) 0.0990(9) Uani 1 1 d . C 5 Cl2G Cl 0.9343(4) 0.8089(3) 1.0121(2) 0.1055(11) Uani 1 1 d . C 5 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 S1 0.0297(7) 0.0181(6) 0.0251(7) 0.0068(5) 0.0030(5) 0.0038(5) S2 0.0510(10) 0.0291(8) 0.0401(9) 0.0039(7) 0.0175(7) 0.0158(7) S4 0.0397(8) 0.0155(6) 0.0286(7) 0.0055(5) 0.0151(6) -0.0008(5) S5 0.0239(6) 0.0174(6) 0.0185(6) 0.0065(5) 0.0024(5) -0.0004(5) S6 0.0270(7) 0.0190(6) 0.0194(6) 0.0075(5) 0.0006(5) -0.0016(5) O1 0.0249(19) 0.025(2) 0.0177(19) 0.0085(15) -0.0020(14) -0.0030(15) O2 0.0218(18) 0.0235(19) 0.0178(18) 0.0060(15) 0.0006(14) -0.0022(14) C1 0.023(3) 0.019(3) 0.022(3) 0.006(2) -0.001(2) 0.000(2) C2 0.027(3) 0.032(3) 0.036(3) 0.007(3) 0.012(2) 0.001(2) C3 0.053(4) 0.025(3) 0.041(4) 0.007(3) 0.029(3) 0.005(3) S3 0.042(3) 0.0301(14) 0.034(2) 0.0119(12) 0.0158(19) 0.0023(12) C4 0.082(13) 0.062(10) 0.045(9) -0.012(8) 0.020(9) 0.007(9) C5 0.059(10) 0.051(9) 0.063(10) 0.006(7) 0.026(8) 0.005(7) S3A 0.046(5) 0.031(2) 0.030(3) 0.0094(19) 0.021(3) 0.000(2) C5A 0.027(9) 0.026(8) 0.012(7) -0.003(6) -0.012(6) -0.001(7) C6 0.021(3) 0.016(2) 0.020(3) 0.004(2) 0.002(2) -0.0023(19) C7 0.022(3) 0.022(3) 0.012(2) 0.0028(19) -0.0017(18) -0.0033(19) C8 0.023(3) 0.020(3) 0.013(2) 0.004(2) -0.0004(19) -0.0053(19) C9 0.021(3) 0.024(3) 0.017(3) 0.003(2) -0.0008(19) -0.001(2) C10 0.026(3) 0.025(3) 0.015(2) 0.006(2) -0.004(2) -0.006(2) C11 0.027(3) 0.022(3) 0.017(3) 0.002(2) -0.001(2) -0.005(2) C12 0.036(3) 0.019(3) 0.037(3) 0.008(2) 0.000(2) 0.003(2) C13 0.036(3) 0.019(3) 0.024(3) -0.003(2) -0.005(2) 0.004(2) C14 0.027(3) 0.029(3) 0.021(3) -0.006(2) -0.004(2) -0.007(2) C15 0.031(3) 0.039(3) 0.021(3) -0.004(3) -0.001(2) 0.003(2) C16 0.037(3) 0.049(4) 0.019(3) -0.003(3) 0.005(2) 0.003(3) C17 0.030(3) 0.042(3) 0.018(3) 0.009(2) -0.004(2) -0.010(2) C18 0.022(3) 0.023(3) 0.022(3) 0.004(2) 0.000(2) -0.003(2) C19 0.018(2) 0.023(3) 0.021(3) 0.004(2) -0.0023(19) -0.0044(19) C20 0.022(2) 0.015(2) 0.015(2) 0.0017(19) -0.0009(18) -0.0071(19) C21 0.022(3) 0.025(3) 0.014(2) 0.009(2) 0.0037(19) -0.001(2) C22 0.019(3) 0.042(3) 0.019(3) 0.011(2) 0.003(2) -0.001(2) C23 0.023(3) 0.041(4) 0.025(3) 0.007(3) -0.002(2) -0.008(2) C24 0.020(3) 0.067(5) 0.040(4) 0.015(3) -0.004(3) -0.011(3) C25 0.023(3) 0.073(5) 0.034(4) 0.015(3) -0.005(3) -0.002(3) C26 0.021(3) 0.062(5) 0.034(3) 0.016(3) 0.011(2) 0.011(3) C27 0.022(3) 0.040(3) 0.025(3) 0.013(3) 0.005(2) 0.002(2) C28 0.032(3) 0.035(3) 0.022(3) 0.008(2) 0.010(2) 0.013(2) C29 0.034(3) 0.019(3) 0.017(3) 0.006(2) 0.002(2) -0.003(2) C30 0.023(3) 0.020(3) 0.014(2) 0.007(2) 0.0032(19) 0.0001(19) S1B 0.0325(7) 0.0168(6) 0.0207(7) 0.0059(5) 0.0034(5) 0.0049(5) S2B 0.0349(8) 0.0210(7) 0.0286(7) 0.0013(6) 0.0094(6) 0.0040(5) S3B 0.0374(8) 0.0285(8) 0.0302(8) 0.0049(6) 0.0186(6) -0.0008(6) S4B 0.0282(7) 0.0181(6) 0.0187(6) 0.0047(5) 0.0046(5) -0.0007(5) S5B 0.0267(7) 0.0170(6) 0.0157(6) 0.0048(5) 0.0023(5) 0.0005(5) S6B 0.0383(8) 0.0165(6) 0.0165(6) 0.0048(5) 0.0020(5) -0.0014(5) O1B 0.0209(18) 0.0241(19) 0.0138(17) 0.0047(14) 0.0004(13) -0.0005(14) O2B 0.029(2) 0.027(2) 0.0111(17) 0.0049(15) 0.0000(14) -0.0003(15) C1B 0.022(3) 0.015(2) 0.022(3) 0.004(2) -0.001(2) 0.0008(19) C2B 0.019(3) 0.022(3) 0.020(3) 0.001(2) 0.0038(19) 0.000(2) C3B 0.039(11) 0.035(10) 0.034(12) 0.017(8) 0.001(10) 0.006(8) C4B 0.039(13) 0.022(11) 0.009(9) 0.001(7) 0.004(8) -0.003(9) C3C 0.034(6) 0.030(6) 0.030(7) 0.004(4) 0.010(5) -0.003(4) C4C 0.027(6) 0.023(6) 0.020(6) 0.004(5) 0.007(4) 0.000(4) C5B 0.023(3) 0.026(3) 0.021(3) 0.000(2) -0.001(2) -0.004(2) C6B 0.025(3) 0.018(3) 0.017(3) 0.007(2) -0.003(2) 0.002(2) C7B 0.022(3) 0.019(3) 0.017(3) 0.001(2) 0.0028(19) 0.0002(19) C8B 0.023(3) 0.022(3) 0.014(2) 0.004(2) -0.0016(19) -0.003(2) C9B 0.028(3) 0.016(2) 0.015(2) -0.0006(19) 0.001(2) 0.003(2) C10B 0.029(3) 0.023(3) 0.019(3) 0.006(2) 0.000(2) -0.004(2) C11B 0.017(2) 0.023(3) 0.013(2) 0.000(2) 0.0031(18) 0.0012(19) C12B 0.030(3) 0.021(3) 0.021(3) 0.007(2) 0.008(2) -0.002(2) C13B 0.033(3) 0.029(3) 0.024(3) 0.007(2) 0.012(2) -0.010(2) C14B 0.022(3) 0.033(3) 0.024(3) 0.005(2) 0.011(2) -0.001(2) C15B 0.026(3) 0.061(5) 0.039(4) 0.014(3) 0.007(3) -0.008(3) C16B 0.023(3) 0.067(5) 0.042(4) 0.006(4) 0.000(3) 0.003(3) C17B 0.028(3) 0.056(5) 0.043(4) 0.015(3) -0.003(3) 0.014(3) C18B 0.024(3) 0.042(4) 0.029(3) 0.010(3) 0.009(2) 0.011(2) C19B 0.018(2) 0.034(3) 0.018(3) 0.004(2) 0.0040(19) 0.006(2) C20B 0.022(3) 0.021(3) 0.013(2) -0.0003(19) 0.0084(19) -0.0054(19) C21B 0.021(2) 0.016(2) 0.016(2) 0.0068(19) 0.0009(19) 0.0006(18) C22B 0.020(3) 0.025(3) 0.015(2) 0.005(2) 0.0020(19) 0.003(2) C23B 0.028(3) 0.024(3) 0.016(2) 0.005(2) -0.002(2) -0.002(2) C24B 0.036(3) 0.029(3) 0.017(3) 0.001(2) -0.003(2) 0.004(2) C25B 0.036(3) 0.040(4) 0.019(3) 0.006(2) 0.002(2) 0.001(3) C26B 0.034(3) 0.044(4) 0.021(3) 0.017(3) 0.001(2) -0.004(3) C27B 0.029(3) 0.025(3) 0.021(3) 0.011(2) -0.002(2) -0.001(2) C28B 0.038(3) 0.032(3) 0.023(3) 0.015(3) -0.001(2) -0.011(2) C29B 0.041(3) 0.023(3) 0.022(3) 0.011(2) -0.003(2) -0.005(2) C30B 0.025(3) 0.025(3) 0.014(2) 0.008(2) 0.0020(19) 0.006(2) N1D 0.046(3) 0.027(3) 0.033(3) 0.009(2) 0.011(2) 0.009(2) N2D 0.045(3) 0.030(3) 0.026(3) 0.004(2) 0.009(2) -0.005(2) N3D 0.055(3) 0.036(3) 0.025(3) 0.006(2) 0.006(2) -0.010(2) N4D 0.068(4) 0.028(3) 0.036(3) 0.002(2) 0.014(3) -0.005(3) F1D 0.0345(18) 0.0196(16) 0.0276(17) 0.0111(13) 0.0074(13) -0.0011(13) F2D 0.0378(18) 0.0174(16) 0.0298(18) 0.0091(13) 0.0064(14) 0.0046(13) F3D 0.0392(19) 0.0197(16) 0.0294(18) 0.0106(14) 0.0098(14) -0.0042(13) F4D 0.0384(18) 0.0147(15) 0.0256(17) 0.0062(13) 0.0087(13) 0.0007(12) C1D 0.024(3) 0.019(2) 0.020(3) 0.008(2) -0.003(2) -0.0003(19) C2D 0.028(3) 0.017(2) 0.017(2) 0.007(2) -0.002(2) -0.003(2) C3D 0.025(3) 0.015(2) 0.022(3) 0.006(2) -0.002(2) 0.0018(19) C4D 0.019(2) 0.018(2) 0.022(3) 0.003(2) -0.008(2) -0.0014(19) C5D 0.027(3) 0.016(3) 0.027(3) 0.008(2) -0.003(2) -0.004(2) C6D 0.026(3) 0.012(2) 0.022(3) 0.004(2) -0.004(2) -0.0062(19) C7D 0.026(3) 0.018(3) 0.022(3) 0.007(2) -0.004(2) 0.000(2) C8D 0.028(3) 0.021(3) 0.024(3) 0.009(2) 0.003(2) 0.002(2) C9D 0.031(3) 0.020(3) 0.015(2) -0.002(2) -0.002(2) 0.000(2) C10D 0.029(3) 0.020(3) 0.020(3) 0.009(2) 0.001(2) 0.000(2) C11D 0.035(3) 0.025(3) 0.020(3) 0.000(2) -0.002(2) -0.002(2) C12D 0.037(3) 0.027(3) 0.021(3) 0.008(2) 0.006(2) -0.004(2) N1E 0.044(3) 0.022(2) 0.022(2) 0.004(2) 0.006(2) 0.010(2) N2E 0.060(4) 0.028(3) 0.031(3) 0.010(2) 0.015(2) -0.005(2) N3E 0.025(2) 0.038(3) 0.027(3) 0.012(2) 0.0047(19) -0.006(2) N4E 0.048(3) 0.025(3) 0.040(3) 0.004(2) 0.009(2) 0.005(2) F1E 0.0425(19) 0.0211(17) 0.0342(19) 0.0142(14) 0.0114(15) -0.0016(14) F2E 0.0413(19) 0.0130(15) 0.0335(18) 0.0069(13) 0.0061(14) 0.0041(13) F3E 0.0399(18) 0.0177(16) 0.0265(17) 0.0105(13) 0.0061(14) 0.0046(13) F4E 0.0414(19) 0.0170(16) 0.0315(18) 0.0074(14) 0.0115(14) 0.0038(13) C1E 0.020(3) 0.020(3) 0.020(3) 0.007(2) -0.0032(19) 0.0032(19) C2E 0.026(3) 0.022(3) 0.023(3) 0.012(2) -0.004(2) -0.002(2) C3E 0.023(3) 0.017(2) 0.025(3) 0.005(2) -0.002(2) 0.0031(19) C5E 0.022(2) 0.018(2) 0.019(3) 0.008(2) -0.0029(19) -0.0009(19) C6E 0.024(3) 0.014(2) 0.019(3) 0.003(2) -0.001(2) 0.0038(19) C7E 0.025(3) 0.019(3) 0.016(2) 0.003(2) -0.0025(19) 0.002(2) C9E 0.038(3) 0.022(3) 0.022(3) 0.002(2) -0.002(2) 0.007(2) C8E 0.032(3) 0.024(3) 0.018(3) 0.007(2) -0.001(2) -0.002(2) C4E 0.022(2) 0.020(2) 0.011(2) 0.0021(19) -0.0069(18) 0.0024(19) C10E 0.022(3) 0.021(3) 0.020(3) 0.009(2) 0.002(2) 0.0028(19) C11E 0.024(3) 0.028(3) 0.017(3) 0.005(2) -0.001(2) 0.004(2) C12E 0.029(3) 0.028(3) 0.025(3) 0.012(2) 0.001(2) -0.001(2) C1F 0.078(6) 0.065(6) 0.047(5) 0.020(4) -0.001(4) 0.012(5) Cl1F 0.126(2) 0.0609(16) 0.0811(18) 0.0213(13) -0.0210(16) 0.0069(15) Cl2F 0.0951(18) 0.0631(15) 0.0643(14) 0.0081(11) -0.0110(12) 0.0238(13) Cl1G 0.103(2) 0.112(3) 0.085(2) 0.0329(19) 0.0055(16) 0.0006(18) Cl2G 0.109(2) 0.093(2) 0.117(3) 0.041(2) -0.0216(19) -0.0326(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.715(6) . ? S1 C2 1.731(6) . ? S2 C5A 1.741(16) . ? S2 C2 1.742(6) . ? S2 C5 1.799(14) . ? S4 C1 1.716(5) . ? S4 C3 1.730(6) . ? S5 C6 1.726(5) . ? S5 C7 1.743(5) . ? S6 C8 1.719(5) . ? S6 C6 1.731(5) . ? O1 C11 1.412(6) . ? O1 C9 1.448(6) . ? O2 C30 1.376(6) . ? O2 C10 1.432(6) . ? C1 C6 1.391(7) . ? C2 C3 1.365(9) . ? C3 S3 1.742(6) . ? C3 S3A 1.842(8) . ? S3 C4 1.882(16) . ? C4 C5 1.30(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? S3A C4A 1.80(3) . ? C4A C5A 1.66(3) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C7 C8 1.364(7) . ? C7 C9 1.507(7) . ? C8 C10 1.509(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C20 1.377(7) . ? C11 C12 1.400(8) . ? C12 C13 1.350(8) . ? C12 H12 0.9300 . ? C13 C14 1.423(9) . ? C13 H13 0.9300 . ? C14 C19 1.407(8) . ? C14 C15 1.410(8) . ? C15 C16 1.371(10) . ? C15 H15 0.9300 . ? C16 C17 1.387(9) . ? C16 H16 0.9300 . ? C17 C18 1.378(8) . ? C17 H17 0.9300 . ? C18 C19 1.437(8) . ? C18 H18 0.9300 . ? C19 C20 1.432(7) . ? C20 C21 1.489(7) . ? C21 C30 1.398(7) . ? C21 C22 1.427(7) . ? C22 C23 1.415(8) . ? C22 C27 1.434(9) . ? C23 C24 1.379(8) . ? C23 H23 0.9300 . ? C24 C25 1.418(11) . ? C24 H24 0.9300 . ? C25 C26 1.356(10) . ? C25 H25 0.9300 . ? C26 C27 1.410(8) . ? C26 H26 0.9300 . ? C27 C28 1.430(9) . ? C28 C29 1.370(8) . ? C28 H28 0.9300 . ? C29 C30 1.413(8) . ? C29 H29 0.9300 . ? S1B C1B 1.715(5) . ? S1B C2B 1.741(5) . ? S2B C3B 1.711(19) . ? S2B C2B 1.740(6) . ? S2B C3C 1.852(10) . ? S3B C4C 1.754(11) . ? S3B C5B 1.758(6) . ? S3B C4B 1.89(2) . ? S4B C1B 1.713(5) . ? S4B C5B 1.750(6) . ? S5B C6B 1.714(5) . ? S5B C7B 1.727(5) . ? S6B C6B 1.723(5) . ? S6B C8B 1.729(6) . ? O1B C11B 1.395(6) . ? O1B C9B 1.443(6) . ? O2B C30B 1.385(6) . ? O2B C10B 1.445(6) . ? C1B C6B 1.412(7) . ? C2B C5B 1.363(8) . ? C3B C4B 1.51(3) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C3C C4C 1.526(17) . ? C3C H3C1 0.9700 . ? C3C H3C2 0.9700 . ? C4C H4C1 0.9700 . ? C4C H4C2 0.9700 . ? C7B C8B 1.349(7) . ? C7B C9B 1.545(7) . ? C8B C10B 1.501(7) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B C20B 1.384(8) . ? C11B C12B 1.414(7) . ? C12B C13B 1.362(8) . ? C12B H12B 0.9300 . ? C13B C14B 1.416(9) . ? C13B H13B 0.9300 . ? C14B C15B 1.430(8) . ? C14B C19B 1.431(8) . ? C15B C16B 1.328(10) . ? C15B H15B 0.9300 . ? C16B C17B 1.425(10) . ? C16B H16B 0.9300 . ? C17B C18B 1.373(9) . ? C17B H17B 0.9300 . ? C18B C19B 1.416(8) . ? C18B H18B 0.9300 . ? C19B C20B 1.430(7) . ? C20B C21B 1.486(6) . ? C21B C30B 1.375(7) . ? C21B C22B 1.438(7) . ? C22B C23B 1.414(7) . ? C22B C27B 1.430(7) . ? C23B C24B 1.368(7) . ? C23B H23B 0.9300 . ? C24B C25B 1.419(8) . ? C24B H24B 0.9300 . ? C25B C26B 1.338(9) . ? C25B H25B 0.9300 . ? C26B C27B 1.435(8) . ? C26B H26B 0.9300 . ? C27B C28B 1.408(8) . ? C28B C29B 1.370(8) . ? C28B H28B 0.9300 . ? C29B C30B 1.425(7) . ? C29B H29B 0.9300 . ? N1D C8D 1.136(7) . ? N2D C9D 1.151(7) . ? N3D C11D 1.150(8) . ? N4D C12D 1.134(8) . ? F1D C2D 1.338(6) . ? F2D C3D 1.357(6) . ? F3D C5D 1.345(6) . ? F4D C6D 1.339(6) . ? C1D C6D 1.414(7) . ? C1D C10D 1.423(8) . ? C1D C2D 1.428(7) . ? C2D C3D 1.379(8) . ? C3D C4D 1.398(7) . ? C4D C7D 1.423(8) . ? C4D C5D 1.430(7) . ? C5D C6D 1.360(8) . ? C7D C9D 1.416(7) . ? C7D C8D 1.421(8) . ? C10D C12D 1.427(8) . ? C10D C11D 1.429(8) . ? N1E C8E 1.142(7) . ? N2E C9E 1.142(8) . ? N3E C11E 1.166(7) . ? N4E C12E 1.146(8) . ? F1E C2E 1.346(6) . ? F2E C3E 1.349(6) . ? F3E C5E 1.341(6) . ? F4E C6E 1.333(6) . ? C1E C2E 1.408(7) . ? C1E C10E 1.415(7) . ? C1E C6E 1.421(7) . ? C2E C3E 1.379(8) . ? C3E C4E 1.412(7) . ? C5E C6E 1.368(7) . ? C5E C4E 1.424(7) . ? C7E C4E 1.410(7) . ? C7E C9E 1.424(8) . ? C7E C8E 1.435(8) . ? C10E C11E 1.416(7) . ? C10E C12E 1.423(8) . ? C1F Cl1F 1.732(10) . ? C1F Cl2F 1.778(9) . ? C1F H1F1 0.9700 . ? C1F H1F2 0.9700 . ? C1G Cl2G 1.665(14) . ? C1G Cl1G 1.700(14) . ? C1G H1G1 0.9700 . ? C1G H1G2 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 95.8(3) . . ? C5A S2 C2 96.3(6) . . ? C2 S2 C5 101.2(5) . . ? C1 S4 C3 95.5(3) . . ? C6 S5 C7 95.5(2) . . ? C8 S6 C6 96.1(2) . . ? C11 O1 C9 112.0(4) . . ? C30 O2 C10 118.8(4) . . ? C6 C1 S1 122.3(4) . . ? C6 C1 S4 122.1(4) . . ? S1 C1 S4 115.6(3) . . ? C3 C2 S1 116.0(5) . . ? C3 C2 S2 127.4(5) . . ? S1 C2 S2 116.5(4) . . ? C2 C3 S4 116.7(5) . . ? C2 C3 S3 126.1(5) . . ? S4 C3 S3 116.4(4) . . ? C2 C3 S3A 126.4(5) . . ? S4 C3 S3A 112.9(4) . . ? C3 S3 C4 98.5(7) . . ? C5 C4 S3 112.9(15) . . ? C5 C4 H4A 109.0 . . ? S3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? S3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 S2 127.6(12) . . ? C4 C5 H5A 105.4 . . ? S2 C5 H5A 105.4 . . ? C4 C5 H5B 105.4 . . ? S2 C5 H5B 105.4 . . ? H5A C5 H5B 106.0 . . ? C5A C4A S3A 100.1(15) . . ? C5A C4A H4A1 111.8 . . ? S3A C4A H4A1 111.8 . . ? C5A C4A H4A2 111.8 . . ? S3A C4A H4A2 111.8 . . ? H4A1 C4A H4A2 109.5 . . ? C4A C5A S2 108.5(13) . . ? C4A C5A H5A1 110.0 . . ? S2 C5A H5A1 110.0 . . ? C4A C5A H5A2 110.0 . . ? S2 C5A H5A2 110.0 . . ? H5A1 C5A H5A2 108.4 . . ? C1 C6 S5 124.0(4) . . ? C1 C6 S6 120.7(4) . . ? S5 C6 S6 115.0(3) . . ? C8 C7 C9 125.7(5) . . ? C8 C7 S5 116.4(4) . . ? C9 C7 S5 117.7(4) . . ? C7 C8 C10 125.6(5) . . ? C7 C8 S6 116.8(4) . . ? C10 C8 S6 117.6(4) . . ? O1 C9 C7 106.0(4) . . ? O1 C9 H9A 110.5 . . ? C7 C9 H9A 110.5 . . ? O1 C9 H9B 110.5 . . ? C7 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O2 C10 C8 111.7(4) . . ? O2 C10 H10A 109.3 . . ? C8 C10 H10A 109.3 . . ? O2 C10 H10B 109.3 . . ? C8 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C20 C11 C12 122.3(5) . . ? C20 C11 O1 117.6(5) . . ? C12 C11 O1 120.0(5) . . ? C13 C12 C11 120.9(5) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.4(5) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C19 C14 C15 119.1(6) . . ? C19 C14 C13 120.0(5) . . ? C15 C14 C13 120.8(6) . . ? C16 C15 C14 121.1(6) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 120.3(6) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 121.0(6) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.7(5) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C14 C19 C20 119.7(5) . . ? C14 C19 C18 118.8(5) . . ? C20 C19 C18 121.4(5) . . ? C11 C20 C19 117.5(5) . . ? C11 C20 C21 120.5(5) . . ? C19 C20 C21 122.0(4) . . ? C30 C21 C22 118.7(5) . . ? C30 C21 C20 119.5(5) . . ? C22 C21 C20 121.8(5) . . ? C23 C22 C21 121.4(6) . . ? C23 C22 C27 118.5(5) . . ? C21 C22 C27 120.1(5) . . ? C24 C23 C22 120.5(6) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.9(7) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 118.8(6) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C27 122.7(7) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C26 C27 C28 122.9(6) . . ? C26 C27 C22 118.4(6) . . ? C28 C27 C22 118.6(5) . . ? C29 C28 C27 120.7(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.5(5) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? O2 C30 C21 116.5(4) . . ? O2 C30 C29 122.1(5) . . ? C21 C30 C29 121.3(5) . . ? C1B S1B C2B 95.5(3) . . ? C3B S2B C2B 100.5(7) . . ? C2B S2B C3C 101.4(4) . . ? C4C S3B C5B 100.1(4) . . ? C5B S3B C4B 99.3(6) . . ? C1B S4B C5B 95.4(3) . . ? C6B S5B C7B 95.5(3) . . ? C6B S6B C8B 95.0(3) . . ? C11B O1B C9B 118.5(4) . . ? C30B O2B C10B 112.9(4) . . ? C6B C1B S4B 123.6(4) . . ? C6B C1B S1B 120.1(4) . . ? S4B C1B S1B 116.3(3) . . ? C5B C2B S2B 130.6(4) . . ? C5B C2B S1B 116.5(4) . . ? S2B C2B S1B 112.8(3) . . ? C4B C3B S2B 110.2(18) . . ? C4B C3B H3B1 109.6 . . ? S2B C3B H3B1 109.6 . . ? C4B C3B H3B2 109.6 . . ? S2B C3B H3B2 109.6 . . ? H3B1 C3B H3B2 108.1 . . ? C3B C4B S3B 121.6(16) . . ? C3B C4B H4B1 106.9 . . ? S3B C4B H4B1 106.9 . . ? C3B C4B H4B2 106.9 . . ? S3B C4B H4B2 106.9 . . ? H4B1 C4B H4B2 106.7 . . ? C4C C3C S2B 114.7(9) . . ? C4C C3C H3C1 108.6 . . ? S2B C3C H3C1 108.6 . . ? C4C C3C H3C2 108.6 . . ? S2B C3C H3C2 108.6 . . ? H3C1 C3C H3C2 107.6 . . ? C3C C4C S3B 114.5(10) . . ? C3C C4C H4C1 108.6 . . ? S3B C4C H4C1 108.6 . . ? C3C C4C H4C2 108.6 . . ? S3B C4C H4C2 108.6 . . ? H4C1 C4C H4C2 107.6 . . ? C2B C5B S4B 116.2(4) . . ? C2B C5B S3B 126.2(4) . . ? S4B C5B S3B 117.6(3) . . ? C1B C6B S5B 124.1(4) . . ? C1B C6B S6B 120.2(4) . . ? S5B C6B S6B 115.7(3) . . ? C8B C7B C9B 125.6(5) . . ? C8B C7B S5B 116.5(4) . . ? C9B C7B S5B 117.8(4) . . ? C7B C8B C10B 126.4(5) . . ? C7B C8B S6B 117.1(4) . . ? C10B C8B S6B 116.1(4) . . ? O1B C9B C7B 110.9(4) . . ? O1B C9B H9B1 109.5 . . ? C7B C9B H9B1 109.5 . . ? O1B C9B H9B2 109.5 . . ? C7B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 108.0 . . ? O2B C10B C8B 105.3(4) . . ? O2B C10B H10C 110.7 . . ? C8B C10B H10C 110.7 . . ? O2B C10B H10D 110.7 . . ? C8B C10B H10D 110.7 . . ? H10C C10B H10D 108.8 . . ? C20B C11B O1B 116.6(4) . . ? C20B C11B C12B 121.9(5) . . ? O1B C11B C12B 121.2(5) . . ? C13B C12B C11B 119.9(5) . . ? C13B C12B H12B 120.0 . . ? C11B C12B H12B 120.0 . . ? C12B C13B C14B 120.8(5) . . ? C12B C13B H13B 119.6 . . ? C14B C13B H13B 119.6 . . ? C13B C14B C15B 122.5(5) . . ? C13B C14B C19B 119.2(5) . . ? C15B C14B C19B 118.1(6) . . ? C16B C15B C14B 122.2(6) . . ? C16B C15B H15B 118.9 . . ? C14B C15B H15B 118.9 . . ? C15B C16B C17B 120.0(6) . . ? C15B C16B H16B 120.0 . . ? C17B C16B H16B 120.0 . . ? C18B C17B C16B 120.4(6) . . ? C18B C17B H17B 119.8 . . ? C16B C17B H17B 119.8 . . ? C17B C18B C19B 120.6(6) . . ? C17B C18B H18B 119.7 . . ? C19B C18B H18B 119.7 . . ? C18B C19B C20B 121.9(5) . . ? C18B C19B C14B 118.7(5) . . ? C20B C19B C14B 119.4(5) . . ? C11B C20B C19B 118.2(4) . . ? C11B C20B C21B 122.3(5) . . ? C19B C20B C21B 119.5(5) . . ? C30B C21B C22B 118.4(4) . . ? C30B C21B C20B 122.1(4) . . ? C22B C21B C20B 119.5(4) . . ? C23B C22B C27B 119.0(5) . . ? C23B C22B C21B 122.1(5) . . ? C27B C22B C21B 118.9(5) . . ? C24B C23B C22B 120.5(5) . . ? C24B C23B H23B 119.8 . . ? C22B C23B H23B 119.8 . . ? C23B C24B C25B 120.8(5) . . ? C23B C24B H24B 119.6 . . ? C25B C24B H24B 119.6 . . ? C26B C25B C24B 120.0(5) . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C27B 121.7(5) . . ? C25B C26B H26B 119.1 . . ? C27B C26B H26B 119.1 . . ? C28B C27B C22B 120.1(5) . . ? C28B C27B C26B 121.9(5) . . ? C22B C27B C26B 118.0(5) . . ? C29B C28B C27B 120.9(5) . . ? C29B C28B H28B 119.6 . . ? C27B C28B H28B 119.6 . . ? C28B C29B C30B 118.9(5) . . ? C28B C29B H29B 120.5 . . ? C30B C29B H29B 120.5 . . ? C21B C30B O2B 119.0(4) . . ? C21B C30B C29B 122.7(5) . . ? O2B C30B C29B 118.3(5) . . ? C6D C1D C10D 123.4(5) . . ? C6D C1D C2D 113.0(5) . . ? C10D C1D C2D 123.6(5) . . ? F1D C2D C3D 118.6(5) . . ? F1D C2D C1D 118.8(5) . . ? C3D C2D C1D 122.6(5) . . ? F2D C3D C2D 115.8(4) . . ? F2D C3D C4D 119.4(5) . . ? C2D C3D C4D 124.8(5) . . ? C3D C4D C7D 124.3(5) . . ? C3D C4D C5D 111.9(5) . . ? C7D C4D C5D 123.7(5) . . ? F3D C5D C6D 117.5(5) . . ? F3D C5D C4D 118.0(5) . . ? C6D C5D C4D 124.5(5) . . ? F4D C6D C5D 117.1(4) . . ? F4D C6D C1D 119.5(5) . . ? C5D C6D C1D 123.3(5) . . ? C9D C7D C8D 113.8(5) . . ? C9D C7D C4D 123.2(5) . . ? C8D C7D C4D 123.0(5) . . ? N1D C8D C7D 176.8(6) . . ? N2D C9D C7D 173.7(6) . . ? C1D C10D C12D 121.9(5) . . ? C1D C10D C11D 123.1(5) . . ? C12D C10D C11D 114.9(5) . . ? N3D C11D C10D 173.5(7) . . ? N4D C12D C10D 176.8(7) . . ? C2E C1E C10E 123.7(5) . . ? C2E C1E C6E 113.4(5) . . ? C10E C1E C6E 122.8(5) . . ? F1E C2E C3E 117.3(5) . . ? F1E C2E C1E 119.2(5) . . ? C3E C2E C1E 123.4(5) . . ? F2E C3E C2E 117.4(5) . . ? F2E C3E C4E 119.1(5) . . ? C2E C3E C4E 123.4(5) . . ? F3E C5E C6E 118.0(5) . . ? F3E C5E C4E 118.5(5) . . ? C6E C5E C4E 123.6(5) . . ? F4E C6E C5E 117.7(4) . . ? F4E C6E C1E 119.2(4) . . ? C5E C6E C1E 123.1(5) . . ? C4E C7E C9E 123.3(5) . . ? C4E C7E C8E 124.4(5) . . ? C9E C7E C8E 112.3(5) . . ? N2E C9E C7E 175.5(6) . . ? N1E C8E C7E 175.5(6) . . ? C7E C4E C3E 123.8(5) . . ? C7E C4E C5E 123.2(5) . . ? C3E C4E C5E 113.0(5) . . ? C1E C10E C11E 123.4(5) . . ? C1E C10E C12E 124.0(5) . . ? C11E C10E C12E 112.5(5) . . ? N3E C11E C10E 173.1(6) . . ? N4E C12E C10E 175.9(6) . . ? Cl1F C1F Cl2F 110.7(5) . . ? Cl1F C1F H1F1 109.5 . . ? Cl2F C1F H1F1 109.5 . . ? Cl1F C1F H1F2 109.5 . . ? Cl2F C1F H1F2 109.5 . . ? H1F1 C1F H1F2 108.1 . . ? Cl2G C1G Cl1G 118.8(9) . . ? Cl2G C1G H1G1 107.6 . . ? Cl1G C1G H1G1 107.6 . . ? Cl2G C1G H1G2 107.6 . . ? Cl1G C1G H1G2 107.6 . . ? H1G1 C1G H1G2 107.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 S1 C1 C6 -174.7(5) . . . . ? C2 S1 C1 S4 4.5(4) . . . . ? C3 S4 C1 C6 173.0(5) . . . . ? C3 S4 C1 S1 -6.2(4) . . . . ? C1 S1 C2 C3 -0.2(6) . . . . ? C1 S1 C2 S2 179.7(4) . . . . ? C5A S2 C2 C3 -27.2(9) . . . . ? C5 S2 C2 C3 0.0(10) . . . . ? C5A S2 C2 S1 152.9(7) . . . . ? C5 S2 C2 S1 -179.8(7) . . . . ? S1 C2 C3 S4 -4.1(8) . . . . ? S2 C2 C3 S4 176.0(4) . . . . ? S1 C2 C3 S3 164.6(5) . . . . ? S2 C2 C3 S3 -15.3(11) . . . . ? S1 C2 C3 S3A -159.8(6) . . . . ? S2 C2 C3 S3A 20.4(11) . . . . ? C1 S4 C3 C2 6.2(6) . . . . ? C1 S4 C3 S3 -163.7(5) . . . . ? C1 S4 C3 S3A 165.0(5) . . . . ? C2 C3 S3 C4 37.4(11) . . . . ? S4 C3 S3 C4 -153.9(8) . . . . ? S3A C3 S3 C4 -63.9(8) . . . . ? C3 S3 C4 C5 -54.5(18) . . . . ? S3 C4 C5 S2 55(3) . . . . ? C5A S2 C5 C4 57(2) . . . . ? C2 S2 C5 C4 -25(2) . . . . ? C2 C3 S3A C4A -37.5(13) . . . . ? S4 C3 S3A C4A 166.2(9) . . . . ? S3 C3 S3A C4A 62.8(10) . . . . ? C3 S3A C4A C5A 65.2(14) . . . . ? S3A C4A C5A S2 -93.6(15) . . . . ? C2 S2 C5A C4A 62.6(14) . . . . ? C5 S2 C5A C4A -39.7(16) . . . . ? S1 C1 C6 S5 175.7(3) . . . . ? S4 C1 C6 S5 -3.5(7) . . . . ? S1 C1 C6 S6 1.2(6) . . . . ? S4 C1 C6 S6 -177.9(3) . . . . ? C7 S5 C6 C1 -171.6(4) . . . . ? C7 S5 C6 S6 3.1(3) . . . . ? C8 S6 C6 C1 171.7(4) . . . . ? C8 S6 C6 S5 -3.2(3) . . . . ? C6 S5 C7 C8 -1.9(4) . . . . ? C6 S5 C7 C9 173.7(4) . . . . ? C9 C7 C8 C10 5.3(8) . . . . ? S5 C7 C8 C10 -179.6(4) . . . . ? C9 C7 C8 S6 -175.2(4) . . . . ? S5 C7 C8 S6 0.0(5) . . . . ? C6 S6 C8 C7 1.9(4) . . . . ? C6 S6 C8 C10 -178.5(4) . . . . ? C11 O1 C9 C7 -143.7(4) . . . . ? C8 C7 C9 O1 83.7(6) . . . . ? S5 C7 C9 O1 -91.4(4) . . . . ? C30 O2 C10 C8 -68.2(6) . . . . ? C7 C8 C10 O2 -46.3(7) . . . . ? S6 C8 C10 O2 134.2(4) . . . . ? C9 O1 C11 C20 121.0(5) . . . . ? C9 O1 C11 C12 -61.2(6) . . . . ? C20 C11 C12 C13 -3.0(9) . . . . ? O1 C11 C12 C13 179.2(5) . . . . ? C11 C12 C13 C14 0.7(9) . . . . ? C12 C13 C14 C19 1.4(8) . . . . ? C12 C13 C14 C15 -176.6(6) . . . . ? C19 C14 C15 C16 -0.7(9) . . . . ? C13 C14 C15 C16 177.4(6) . . . . ? C14 C15 C16 C17 1.8(10) . . . . ? C15 C16 C17 C18 -1.8(9) . . . . ? C16 C17 C18 C19 0.7(8) . . . . ? C15 C14 C19 C20 176.8(5) . . . . ? C13 C14 C19 C20 -1.3(8) . . . . ? C15 C14 C19 C18 -0.4(8) . . . . ? C13 C14 C19 C18 -178.5(5) . . . . ? C17 C18 C19 C14 0.4(7) . . . . ? C17 C18 C19 C20 -176.7(5) . . . . ? C12 C11 C20 C19 3.1(7) . . . . ? O1 C11 C20 C19 -179.1(4) . . . . ? C12 C11 C20 C21 -178.4(5) . . . . ? O1 C11 C20 C21 -0.6(7) . . . . ? C14 C19 C20 C11 -0.9(7) . . . . ? C18 C19 C20 C11 176.2(5) . . . . ? C14 C19 C20 C21 -179.4(5) . . . . ? C18 C19 C20 C21 -2.3(7) . . . . ? C11 C20 C21 C30 -64.2(6) . . . . ? C19 C20 C21 C30 114.2(5) . . . . ? C11 C20 C21 C22 115.1(6) . . . . ? C19 C20 C21 C22 -66.5(6) . . . . ? C30 C21 C22 C23 177.2(5) . . . . ? C20 C21 C22 C23 -2.2(8) . . . . ? C30 C21 C22 C27 -3.9(7) . . . . ? C20 C21 C22 C27 176.8(5) . . . . ? C21 C22 C23 C24 179.9(5) . . . . ? C27 C22 C23 C24 1.0(8) . . . . ? C22 C23 C24 C25 -2.1(10) . . . . ? C23 C24 C25 C26 1.6(10) . . . . ? C24 C25 C26 C27 0.1(10) . . . . ? C25 C26 C27 C28 176.4(6) . . . . ? C25 C26 C27 C22 -1.1(9) . . . . ? C23 C22 C27 C26 0.6(8) . . . . ? C21 C22 C27 C26 -178.4(5) . . . . ? C23 C22 C27 C28 -177.0(5) . . . . ? C21 C22 C27 C28 4.0(8) . . . . ? C26 C27 C28 C29 -178.5(5) . . . . ? C22 C27 C28 C29 -1.0(8) . . . . ? C27 C28 C29 C30 -2.0(8) . . . . ? C10 O2 C30 C21 153.7(4) . . . . ? C10 O2 C30 C29 -29.8(7) . . . . ? C22 C21 C30 O2 177.4(4) . . . . ? C20 C21 C30 O2 -3.3(7) . . . . ? C22 C21 C30 C29 0.9(7) . . . . ? C20 C21 C30 C29 -179.8(5) . . . . ? C28 C29 C30 O2 -174.1(5) . . . . ? C28 C29 C30 C21 2.1(7) . . . . ? C5B S4B C1B C6B 179.6(4) . . . . ? C5B S4B C1B S1B -1.4(4) . . . . ? C2B S1B C1B C6B -178.5(4) . . . . ? C2B S1B C1B S4B 2.5(4) . . . . ? C3B S2B C2B C5B -33.2(11) . . . . ? C3C S2B C2B C5B -2.9(7) . . . . ? C3B S2B C2B S1B 148.7(9) . . . . ? C3C S2B C2B S1B 179.0(5) . . . . ? C1B S1B C2B C5B -2.9(5) . . . . ? C1B S1B C2B S2B 175.5(3) . . . . ? C2B S2B C3B C4B 57(2) . . . . ? C3C S2B C3B C4B -37.7(17) . . . . ? S2B C3B C4B S3B -65(3) . . . . ? C4C S3B C4B C3B -63(3) . . . . ? C5B S3B C4B C3B 31(3) . . . . ? C3B S2B C3C C4C 58.2(16) . . . . ? C2B S2B C3C C4C -33.0(11) . . . . ? S2B C3C C4C S3B 68.0(14) . . . . ? C5B S3B C4C C3C -57.2(12) . . . . ? C4B S3B C4C C3C 32.4(19) . . . . ? S2B C2B C5B S4B -175.6(4) . . . . ? S1B C2B C5B S4B 2.5(6) . . . . ? S2B C2B C5B S3B 5.8(8) . . . . ? S1B C2B C5B S3B -176.1(3) . . . . ? C1B S4B C5B C2B -0.6(5) . . . . ? C1B S4B C5B S3B 178.1(3) . . . . ? C4C S3B C5B C2B 21.2(8) . . . . ? C4B S3B C5B C2B 0.0(11) . . . . ? C4C S3B C5B S4B -157.3(6) . . . . ? C4B S3B C5B S4B -178.5(10) . . . . ? S4B C1B C6B S5B -0.4(6) . . . . ? S1B C1B C6B S5B -179.4(3) . . . . ? S4B C1B C6B S6B 177.4(3) . . . . ? S1B C1B C6B S6B -1.5(6) . . . . ? C7B S5B C6B C1B 174.4(4) . . . . ? C7B S5B C6B S6B -3.6(3) . . . . ? C8B S6B C6B C1B -174.2(4) . . . . ? C8B S6B C6B S5B 3.9(3) . . . . ? C6B S5B C7B C8B 1.7(5) . . . . ? C6B S5B C7B C9B -178.0(4) . . . . ? C9B C7B C8B C10B 7.3(9) . . . . ? S5B C7B C8B C10B -172.4(4) . . . . ? C9B C7B C8B S6B -179.6(4) . . . . ? S5B C7B C8B S6B 0.7(6) . . . . ? C6B S6B C8B C7B -2.7(5) . . . . ? C6B S6B C8B C10B 171.1(4) . . . . ? C11B O1B C9B C7B -74.0(5) . . . . ? C8B C7B C9B O1B -44.8(7) . . . . ? S5B C7B C9B O1B 134.9(4) . . . . ? C30B O2B C10B C8B -146.2(4) . . . . ? C7B C8B C10B O2B 86.2(6) . . . . ? S6B C8B C10B O2B -87.0(5) . . . . ? C9B O1B C11B C20B 149.1(4) . . . . ? C9B O1B C11B C12B -37.0(7) . . . . ? C20B C11B C12B C13B -1.6(8) . . . . ? O1B C11B C12B C13B -175.2(5) . . . . ? C11B C12B C13B C14B -2.5(8) . . . . ? C12B C13B C14B C15B -173.9(6) . . . . ? C12B C13B C14B C19B 1.1(8) . . . . ? C13B C14B C15B C16B 174.2(7) . . . . ? C19B C14B C15B C16B -0.9(10) . . . . ? C14B C15B C16B C17B 1.6(11) . . . . ? C15B C16B C17B C18B -1.9(11) . . . . ? C16B C17B C18B C19B 1.4(10) . . . . ? C17B C18B C19B C20B -179.9(6) . . . . ? C17B C18B C19B C14B -0.7(9) . . . . ? C13B C14B C19B C18B -174.8(5) . . . . ? C15B C14B C19B C18B 0.4(8) . . . . ? C13B C14B C19B C20B 4.3(8) . . . . ? C15B C14B C19B C20B 179.6(5) . . . . ? O1B C11B C20B C19B -179.2(4) . . . . ? C12B C11B C20B C19B 7.0(7) . . . . ? O1B C11B C20B C21B 0.9(7) . . . . ? C12B C11B C20B C21B -172.9(5) . . . . ? C18B C19B C20B C11B 170.9(5) . . . . ? C14B C19B C20B C11B -8.2(7) . . . . ? C18B C19B C20B C21B -9.2(8) . . . . ? C14B C19B C20B C21B 171.7(5) . . . . ? C11B C20B C21B C30B -67.2(7) . . . . ? C19B C20B C21B C30B 112.8(6) . . . . ? C11B C20B C21B C22B 112.5(6) . . . . ? C19B C20B C21B C22B -67.4(7) . . . . ? C30B C21B C22B C23B 177.7(5) . . . . ? C20B C21B C22B C23B -2.1(8) . . . . ? C30B C21B C22B C27B -0.7(7) . . . . ? C20B C21B C22B C27B 179.5(5) . . . . ? C27B C22B C23B C24B 0.0(8) . . . . ? C21B C22B C23B C24B -178.4(5) . . . . ? C22B C23B C24B C25B 0.6(9) . . . . ? C23B C24B C25B C26B -0.9(9) . . . . ? C24B C25B C26B C27B 0.7(10) . . . . ? C23B C22B C27B C28B 179.9(5) . . . . ? C21B C22B C27B C28B -1.7(8) . . . . ? C23B C22B C27B C26B -0.2(8) . . . . ? C21B C22B C27B C26B 178.2(5) . . . . ? C25B C26B C27B C28B 179.7(6) . . . . ? C25B C26B C27B C22B -0.1(9) . . . . ? C22B C27B C28B C29B 2.8(9) . . . . ? C26B C27B C28B C29B -177.0(6) . . . . ? C27B C28B C29B C30B -1.5(9) . . . . ? C22B C21B C30B O2B -177.4(4) . . . . ? C20B C21B C30B O2B 2.3(7) . . . . ? C22B C21B C30B C29B 2.0(8) . . . . ? C20B C21B C30B C29B -178.2(5) . . . . ? C10B O2B C30B C21B 113.9(5) . . . . ? C10B O2B C30B C29B -65.5(6) . . . . ? C28B C29B C30B C21B -1.0(9) . . . . ? C28B C29B C30B O2B 178.5(5) . . . . ? C6D C1D C2D F1D -179.3(4) . . . . ? C10D C1D C2D F1D -2.0(8) . . . . ? C6D C1D C2D C3D -1.7(7) . . . . ? C10D C1D C2D C3D 175.6(5) . . . . ? F1D C2D C3D F2D 1.2(7) . . . . ? C1D C2D C3D F2D -176.4(4) . . . . ? F1D C2D C3D C4D 178.2(5) . . . . ? C1D C2D C3D C4D 0.5(8) . . . . ? F2D C3D C4D C7D -1.3(8) . . . . ? C2D C3D C4D C7D -178.2(5) . . . . ? F2D C3D C4D C5D 178.0(4) . . . . ? C2D C3D C4D C5D 1.2(7) . . . . ? C3D C4D C5D F3D 179.7(4) . . . . ? C7D C4D C5D F3D -1.0(8) . . . . ? C3D C4D C5D C6D -1.7(7) . . . . ? C7D C4D C5D C6D 177.6(5) . . . . ? F3D C5D C6D F4D -3.3(7) . . . . ? C4D C5D C6D F4D 178.1(5) . . . . ? F3D C5D C6D C1D 179.2(5) . . . . ? C4D C5D C6D C1D 0.6(9) . . . . ? C10D C1D C6D F4D 6.3(8) . . . . ? C2D C1D C6D F4D -176.4(4) . . . . ? C10D C1D C6D C5D -176.2(5) . . . . ? C2D C1D C6D C5D 1.1(7) . . . . ? C3D C4D C7D C9D 176.8(5) . . . . ? C5D C4D C7D C9D -2.4(8) . . . . ? C3D C4D C7D C8D -0.9(8) . . . . ? C5D C4D C7D C8D 179.8(5) . . . . ? C6D C1D C10D C12D 10.4(8) . . . . ? C2D C1D C10D C12D -166.6(5) . . . . ? C6D C1D C10D C11D -175.1(5) . . . . ? C2D C1D C10D C11D 7.9(9) . . . . ? C10E C1E C2E F1E 1.1(8) . . . . ? C6E C1E C2E F1E 179.6(4) . . . . ? C10E C1E C2E C3E -177.3(5) . . . . ? C6E C1E C2E C3E 1.2(7) . . . . ? F1E C2E C3E F2E 1.6(7) . . . . ? C1E C2E C3E F2E -179.9(4) . . . . ? F1E C2E C3E C4E -178.7(4) . . . . ? C1E C2E C3E C4E -0.2(8) . . . . ? F3E C5E C6E F4E -2.4(7) . . . . ? C4E C5E C6E F4E 178.6(4) . . . . ? F3E C5E C6E C1E -179.3(4) . . . . ? C2E C1E C6E F4E -178.8(4) . . . . ? C10E C1E C6E F4E -0.2(7) . . . . ? C2E C1E C6E C5E -1.9(7) . . . . ? C10E C1E C6E C5E 176.6(5) . . . . ? C9E C7E C4E C3E -179.0(5) . . . . ? C8E C7E C4E C3E 0.6(8) . . . . ? C9E C7E C4E C5E 1.0(8) . . . . ? C8E C7E C4E C5E -179.4(5) . . . . ? F2E C3E C4E C7E -0.4(7) . . . . ? C2E C3E C4E C7E 179.8(5) . . . . ? F2E C3E C4E C5E 179.6(4) . . . . ? C2E C3E C4E C5E -0.2(7) . . . . ? F3E C5E C4E C7E 0.4(7) . . . . ? C6E C5E C4E C7E 179.4(5) . . . . ? F3E C5E C4E C3E -179.6(4) . . . . ? C6E C5E C4E C3E -0.6(7) . . . . ? C2E C1E C10E C11E 1.8(8) . . . . ? C6E C1E C10E C11E -176.6(5) . . . . ? C2E C1E C10E C12E 178.0(5) . . . . ? C6E C1E C10E C12E -0.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.868 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.157 # Attachment '-R--1.cif' data_-R--1 _database_code_depnum_ccdc_archive 'CCDC 809760' #TrackingRef '-R--1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H20 O2 S6), C2 H3 N' _chemical_formula_sum 'C62 H43 N O4 S12' _chemical_formula_weight 1250.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall C2y loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 46.597(4) _cell_length_b 8.8358(7) _cell_length_c 13.4499(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.600(3) _cell_angle_gamma 90.00 _cell_volume 5526.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1727 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 22.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 0.990 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.665059 #-------------------------------------------------------------------# _diffrn_ambient_temperature 150(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 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16538 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.1485 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 60 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9752 _reflns_number_gt 5150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1073P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(14) _refine_ls_number_reflns 9752 _refine_ls_number_parameters 707 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1586 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.1662 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 S1 S 0.44225(6) 1.1270(4) 0.78698(19) 0.0522(8) Uani 1 1 d . . . S2 S 0.38453(6) 0.9909(4) 0.7613(2) 0.0623(9) Uani 1 1 d . . . S3 S 0.39322(6) 1.0291(5) 0.5092(2) 0.0651(10) Uani 1 1 d . . . S4 S 0.45083(5) 1.1526(4) 0.57282(18) 0.0500(8) Uani 1 1 d . . . S5 S 0.50975(5) 1.3385(4) 0.62420(17) 0.0446(7) Uani 1 1 d . A . S6 S 0.49970(5) 1.3338(4) 0.83885(16) 0.0398(7) Uani 1 1 d . A . O1 O 0.58268(12) 1.3384(8) 0.6592(4) 0.0351(15) Uani 1 1 d . . . O2 O 0.58163(12) 1.4290(8) 0.8807(4) 0.0328(16) Uani 1 1 d . A . C1 C 0.46264(19) 1.1998(13) 0.6964(7) 0.041(3) Uani 1 1 d . A . C2 C 0.4136(2) 1.0702(12) 0.7055(8) 0.041(3) Uani 1 1 d . A . C3 C 0.3749(8) 0.856(4) 0.6892(19) 0.063(10) Uiso 0.43(4) 1 d PD A 1 H3A H 0.3901 0.7805 0.6910 0.076 Uiso 0.43(4) 1 calc PR A 1 H3B H 0.3579 0.8085 0.7133 0.076 Uiso 0.43(4) 1 calc PR A 1 C4 C 0.3684(8) 0.906(4) 0.581(2) 0.068(11) Uiso 0.43(4) 1 d PD A 1 H4A H 0.3501 0.9585 0.5795 0.081 Uiso 0.43(4) 1 calc PR A 1 H4B H 0.3652 0.8145 0.5423 0.081 Uiso 0.43(4) 1 calc PR A 1 C3A C 0.3650(5) 0.895(3) 0.653(2) 0.067(8) Uiso 0.57(4) 1 d PD A 2 H3A1 H 0.3580 0.7984 0.6760 0.080 Uiso 0.57(4) 1 calc PR A 2 H3A2 H 0.3483 0.9555 0.6331 0.080 Uiso 0.57(4) 1 calc PR A 2 C4A C 0.3809(5) 0.863(3) 0.5589(13) 0.055(7) Uiso 0.57(4) 1 d PD A 2 H4A1 H 0.3681 0.8130 0.5100 0.066 Uiso 0.57(4) 1 calc PR A 2 H4A2 H 0.3971 0.7966 0.5752 0.066 Uiso 0.57(4) 1 calc PR A 2 C5 C 0.4176(2) 1.0846(14) 0.6082(9) 0.051(3) Uani 1 1 d . A . C6 C 0.48619(18) 1.2840(12) 0.7169(6) 0.035(2) Uani 1 1 d . . . C7 C 0.53663(18) 1.4174(12) 0.7090(7) 0.037(2) Uani 1 1 d . . . C8 C 0.5321(2) 1.4137(13) 0.8056(7) 0.040(3) Uani 1 1 d . A . C9 C 0.56376(18) 1.4668(13) 0.6604(7) 0.040(3) Uani 1 1 d . A . H9A H 0.5590 1.5017 0.5930 0.048 Uiso 1 1 calc R . . H9B H 0.5730 1.5491 0.6980 0.048 Uiso 1 1 calc R . . C10 C 0.55236(16) 1.4764(13) 0.8871(7) 0.036(2) Uani 1 1 d . . . H10A H 0.5516 1.5861 0.8845 0.043 Uiso 1 1 calc R A . H10B H 0.5458 1.4451 0.9509 0.043 Uiso 1 1 calc R . . C11 C 0.61106(18) 1.3758(12) 0.6806(6) 0.034(2) Uani 1 1 d . . . C12 C 0.6253(2) 1.4672(12) 0.6144(7) 0.037(2) Uani 1 1 d . . . H12 H 0.6155 1.5071 0.5580 0.044 Uiso 1 1 calc R . . C13 C 0.65426(19) 1.4972(12) 0.6347(7) 0.039(2) Uani 1 1 d . . . H13 H 0.6641 1.5538 0.5895 0.046 Uiso 1 1 calc R . . C14 C 0.66890(18) 1.4447(11) 0.7210(7) 0.035(2) Uani 1 1 d . . . C15 C 0.6982(2) 1.4769(13) 0.7459(8) 0.047(3) Uani 1 1 d . . . H15 H 0.7083 1.5336 0.7014 0.056 Uiso 1 1 calc R . . C16 C 0.7121(2) 1.4300(14) 0.8300(9) 0.055(3) Uani 1 1 d . . . H16 H 0.7313 1.4556 0.8442 0.066 Uiso 1 1 calc R . . C17 C 0.69754(18) 1.3424(13) 0.8960(7) 0.042(3) Uani 1 1 d . . . H17 H 0.7072 1.3084 0.9544 0.051 Uiso 1 1 calc R . . C18 C 0.66969(18) 1.3058(12) 0.8770(7) 0.036(2) Uani 1 1 d . . . H18 H 0.6603 1.2480 0.9229 0.043 Uiso 1 1 calc R . . C19 C 0.65416(18) 1.3550(12) 0.7865(6) 0.033(2) Uani 1 1 d . . . C20 C 0.62432(17) 1.3164(11) 0.7664(6) 0.028(2) Uani 1 1 d . . . C21 C 0.60886(16) 1.2180(11) 0.8343(6) 0.025(2) Uani 1 1 d . A . C22 C 0.61532(16) 1.0604(11) 0.8419(6) 0.025(2) Uani 1 1 d . . . C23 C 0.63386(18) 0.9881(12) 0.7790(7) 0.034(2) Uani 1 1 d . . . H23 H 0.6436 1.0460 0.7342 0.040 Uiso 1 1 calc R . . C24 C 0.63798(19) 0.8376(14) 0.7815(7) 0.041(2) Uani 1 1 d . . . H24 H 0.6501 0.7933 0.7376 0.049 Uiso 1 1 calc R . . C25 C 0.6241(2) 0.7456(12) 0.8498(8) 0.040(2) Uani 1 1 d . . . H25 H 0.6269 0.6414 0.8508 0.048 Uiso 1 1 calc R . . C26 C 0.60664(18) 0.8128(12) 0.9142(7) 0.035(2) Uani 1 1 d . . . H26 H 0.5978 0.7534 0.9605 0.042 Uiso 1 1 calc R . . C27 C 0.60147(16) 0.9712(11) 0.9124(6) 0.026(2) Uani 1 1 d . . . C28 C 0.58235(18) 1.0381(12) 0.9735(6) 0.032(2) Uani 1 1 d . . . H28 H 0.5742 0.9802 1.0221 0.039 Uiso 1 1 calc R . . C29 C 0.57536(19) 1.1839(13) 0.9641(6) 0.036(3) Uani 1 1 d . A . H29 H 0.5620 1.2260 1.0047 0.043 Uiso 1 1 calc R . . C30 C 0.58832(17) 1.2754(10) 0.8919(6) 0.023(2) Uani 1 1 d . . . S1B S 0.53500(5) 1.6950(4) 0.35743(17) 0.0491(8) Uani 1 1 d . . . S2B S 0.47656(6) 1.8021(5) 0.3894(2) 0.0695(11) Uani 1 1 d . . . S3B S 0.47335(5) 1.8857(4) 0.1364(2) 0.0512(8) Uani 1 1 d . . . S4B S 0.53061(5) 1.7391(3) 0.13929(18) 0.0417(7) Uani 1 1 d . . . S5B S 0.58911(5) 1.5281(4) 0.12609(18) 0.0469(8) Uani 1 1 d . . . S6B S 0.59013(5) 1.4901(4) 0.34418(19) 0.0496(8) Uani 1 1 d . . . O2B O 0.66084(12) 1.4821(9) 0.3732(5) 0.0434(19) Uani 1 1 d . . . O1B O 0.67156(14) 1.4130(10) 0.1589(5) 0.052(2) Uani 1 1 d . . . C1B C 0.54870(17) 1.6553(13) 0.2401(6) 0.036(3) Uani 1 1 d . . . C2B C 0.50285(17) 1.7705(13) 0.3028(7) 0.042(3) Uani 1 1 d . . . C3B C 0.4494(2) 1.9151(14) 0.3183(9) 0.055(3) Uani 1 1 d . . . H3B1 H 0.4342 1.8482 0.2924 0.066 Uiso 1 1 calc R . . H3B2 H 0.4410 1.9859 0.3633 0.066 Uiso 1 1 calc R . . C4B C 0.4607(2) 2.0021(14) 0.2331(7) 0.045(3) Uani 1 1 d . . . H4B1 H 0.4763 2.0665 0.2587 0.053 Uiso 1 1 calc R . . H4B2 H 0.4455 2.0671 0.2048 0.053 Uiso 1 1 calc R . . C5B C 0.50113(19) 1.7919(12) 0.2047(7) 0.036(2) Uani 1 1 d . . . C6B C 0.57264(19) 1.5700(13) 0.2365(7) 0.039(3) Uani 1 1 d . . . C7B C 0.6188(2) 1.4259(13) 0.1907(8) 0.047(3) Uani 1 1 d . . . C8B C 0.61868(18) 1.4156(13) 0.2856(8) 0.044(3) Uani 1 1 d . . . C9B C 0.6430(2) 1.3695(15) 0.1263(8) 0.053(3) Uani 1 1 d . . . H9B1 H 0.6422 1.2598 0.1237 0.063 Uiso 1 1 calc R . . H9B2 H 0.6391 1.4064 0.0589 0.063 Uiso 1 1 calc R . . C10B C 0.64359(19) 1.3595(15) 0.3521(8) 0.052(3) Uani 1 1 d . . . H10C H 0.6368 1.3171 0.4129 0.062 Uiso 1 1 calc R . . H10D H 0.6541 1.2819 0.3185 0.062 Uiso 1 1 calc R . . C11B C 0.6764(2) 1.5654(15) 0.1593(8) 0.049(3) Uani 1 1 d . . . C12B C 0.6650(2) 1.6624(16) 0.0812(8) 0.060(4) Uani 1 1 d . . . H12B H 0.6531 1.6217 0.0298 0.072 Uiso 1 1 calc R . . C14B C 0.68912(19) 1.8773(14) 0.1565(8) 0.045(3) Uani 1 1 d . . . C13B C 0.6711(2) 1.8130(16) 0.0805(9) 0.060(4) Uani 1 1 d . . . H13B H 0.6633 1.8737 0.0292 0.072 Uiso 1 1 calc R . . C15B C 0.6947(2) 2.0338(17) 0.1570(9) 0.062(4) Uani 1 1 d . . . H15B H 0.6869 2.0935 0.1053 0.074 Uiso 1 1 calc R . . C16B C 0.7107(3) 2.0972(16) 0.2284(10) 0.070(4) Uani 1 1 d . . . H16B H 0.7144 2.2007 0.2271 0.083 Uiso 1 1 calc R . . C17B C 0.7224(3) 2.0087(15) 0.3067(10) 0.062(3) Uani 1 1 d . . . H17B H 0.7338 2.0548 0.3573 0.075 Uiso 1 1 calc R . . C18B C 0.7177(2) 1.8572(15) 0.3113(8) 0.050(3) Uani 1 1 d . . . H18B H 0.7255 1.8016 0.3651 0.060 Uiso 1 1 calc R . . C19B C 0.70038(19) 1.7820(13) 0.2326(7) 0.042(3) Uani 1 1 d . . . C20B C 0.69491(18) 1.6238(13) 0.2339(7) 0.037(3) Uani 1 1 d . . . C21B C 0.70745(19) 1.5229(12) 0.3164(6) 0.036(2) Uani 1 1 d . . . C22B C 0.73819(17) 1.4972(14) 0.3291(7) 0.039(3) Uani 1 1 d . . . C23B C 0.7580(2) 1.5691(14) 0.2686(8) 0.048(3) Uani 1 1 d . . . H23B H 0.7512 1.6335 0.2178 0.058 Uiso 1 1 calc R . . C24B C 0.7874(2) 1.5446(16) 0.2844(8) 0.062(4) Uani 1 1 d . . . H24B H 0.8002 1.5927 0.2444 0.074 Uiso 1 1 calc R . . C25B C 0.7976(2) 1.4487(15) 0.3594(9) 0.061(4) Uani 1 1 d . . . H25B H 0.8173 1.4359 0.3707 0.074 Uiso 1 1 calc R . . C26B C 0.7798(2) 1.3731(15) 0.4170(8) 0.051(3) Uani 1 1 d . . . H26B H 0.7873 1.3048 0.4644 0.061 Uiso 1 1 calc R . . C27B C 0.74889(19) 1.3976(13) 0.4054(7) 0.040(3) Uani 1 1 d . . . C28B C 0.72935(18) 1.3232(13) 0.4670(6) 0.037(2) Uani 1 1 d . . . H28B H 0.7363 1.2549 0.5154 0.045 Uiso 1 1 calc R . . C29B C 0.70000(18) 1.3523(13) 0.4549(6) 0.040(3) Uani 1 1 d . . . H29B H 0.6874 1.3063 0.4965 0.048 Uiso 1 1 calc R . . C30B C 0.68970(17) 1.4504(12) 0.3806(7) 0.034(2) Uani 1 1 d . . . N1C N 0.7431(4) 1.622(3) 0.0302(12) 0.161(8) Uani 1 1 d . . . C1C C 0.7334(4) 1.705(3) -0.0288(14) 0.114(6) Uani 1 1 d . . . C2C C 0.7188(4) 1.814(3) -0.0989(14) 0.152(8) Uiso 1 1 d . . . H2C1 H 0.7058 1.8760 -0.0636 0.228 Uiso 1 1 calc R . . H2C2 H 0.7082 1.7602 -0.1510 0.228 Uiso 1 1 calc R . . H2C3 H 0.7328 1.8778 -0.1273 0.228 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0420(14) 0.075(3) 0.0414(15) 0.0053(16) 0.0145(12) -0.0070(15) S2 0.0474(16) 0.058(2) 0.084(2) -0.0060(19) 0.0268(15) -0.0148(16) S3 0.0415(15) 0.079(3) 0.074(2) -0.016(2) -0.0010(14) -0.0145(16) S4 0.0341(13) 0.076(3) 0.0404(14) -0.0069(15) 0.0068(11) -0.0082(14) S5 0.0310(12) 0.066(2) 0.0363(13) 0.0065(15) -0.0005(10) -0.0042(14) S6 0.0302(11) 0.057(2) 0.0323(12) -0.0034(14) 0.0039(9) 0.0048(12) O1 0.033(3) 0.031(4) 0.041(3) 0.005(3) 0.001(3) -0.005(3) O2 0.028(3) 0.035(5) 0.036(4) -0.005(3) 0.007(3) 0.003(3) C1 0.035(5) 0.049(8) 0.038(5) -0.004(5) 0.003(4) 0.014(5) C2 0.037(5) 0.031(7) 0.058(7) -0.003(5) 0.024(5) 0.003(5) C5 0.029(5) 0.059(9) 0.067(7) -0.001(6) 0.006(5) -0.008(5) C6 0.032(5) 0.041(7) 0.031(5) -0.003(5) 0.004(4) 0.008(5) C7 0.031(5) 0.025(7) 0.052(6) 0.010(5) -0.007(4) -0.007(4) C8 0.041(5) 0.037(7) 0.044(6) 0.008(5) 0.009(4) 0.009(5) C9 0.031(5) 0.039(7) 0.049(6) 0.009(5) 0.003(4) 0.000(5) C10 0.025(4) 0.036(7) 0.046(5) -0.010(5) 0.001(4) 0.012(4) C11 0.034(5) 0.032(7) 0.038(5) -0.012(5) 0.008(4) -0.008(4) C12 0.046(5) 0.028(7) 0.038(5) 0.000(5) 0.009(4) 0.001(5) C13 0.044(5) 0.026(7) 0.049(6) 0.007(5) 0.026(5) -0.002(5) C14 0.031(5) 0.026(7) 0.048(6) -0.002(5) 0.012(4) -0.002(4) C15 0.036(5) 0.043(8) 0.063(7) -0.018(6) 0.021(5) -0.013(5) C16 0.035(6) 0.041(8) 0.088(9) 0.001(7) -0.003(6) -0.003(5) C17 0.028(5) 0.049(8) 0.049(6) -0.003(6) 0.000(4) 0.010(5) C18 0.039(5) 0.024(7) 0.046(6) -0.015(5) 0.008(4) 0.004(5) C19 0.038(5) 0.028(6) 0.033(5) -0.006(5) 0.015(4) -0.001(5) C20 0.029(4) 0.026(6) 0.030(5) -0.014(4) 0.005(4) 0.002(4) C21 0.023(4) 0.029(6) 0.022(4) -0.004(4) -0.003(3) -0.005(4) C22 0.019(4) 0.021(6) 0.036(5) -0.001(4) 0.003(4) -0.001(4) C23 0.036(5) 0.021(6) 0.045(6) -0.005(5) 0.011(4) 0.006(5) C24 0.034(5) 0.039(7) 0.050(6) -0.006(6) 0.010(4) 0.005(5) C25 0.042(5) 0.010(6) 0.067(7) -0.004(5) 0.000(5) -0.001(5) C26 0.030(4) 0.028(7) 0.045(6) 0.010(5) -0.007(4) -0.009(4) C27 0.022(4) 0.029(6) 0.025(4) -0.003(4) -0.005(3) -0.009(4) C28 0.037(5) 0.031(7) 0.029(5) 0.007(5) 0.001(4) -0.001(5) C29 0.035(5) 0.052(8) 0.022(5) -0.003(5) 0.007(4) -0.006(5) C30 0.025(4) 0.015(6) 0.028(5) -0.007(4) 0.000(3) 0.003(4) S1B 0.0350(13) 0.079(3) 0.0340(14) 0.0015(15) 0.0052(10) 0.0194(14) S2B 0.0418(15) 0.104(3) 0.0654(18) 0.0297(19) 0.0256(13) 0.0287(18) S3B 0.0441(14) 0.056(2) 0.0523(16) -0.0060(15) -0.0102(12) 0.0190(14) S4B 0.0413(13) 0.046(2) 0.0381(14) 0.0022(13) 0.0001(11) 0.0080(13) S5B 0.0423(13) 0.059(2) 0.0401(14) -0.0159(15) 0.0097(11) -0.0049(14) S6B 0.0388(13) 0.067(2) 0.0419(14) -0.0143(15) -0.0096(11) 0.0193(14) O2B 0.020(3) 0.056(6) 0.054(4) 0.012(4) -0.004(3) -0.001(3) O1B 0.043(4) 0.047(6) 0.065(5) 0.010(4) -0.018(3) -0.009(4) C1B 0.019(4) 0.058(8) 0.031(5) -0.007(5) 0.007(3) 0.002(4) C2B 0.015(4) 0.060(9) 0.051(6) 0.005(5) 0.013(4) 0.005(4) C3B 0.034(5) 0.052(9) 0.080(8) 0.001(7) 0.007(5) 0.011(5) C4B 0.040(5) 0.045(8) 0.049(6) -0.002(6) 0.002(5) 0.000(5) C5B 0.037(5) 0.028(7) 0.042(6) 0.000(5) -0.002(4) 0.003(4) C6B 0.033(5) 0.050(8) 0.035(5) -0.014(5) 0.003(4) 0.001(5) C7B 0.037(5) 0.041(8) 0.063(7) 0.005(6) 0.015(5) 0.014(5) C8B 0.023(5) 0.042(8) 0.067(7) -0.003(6) 0.005(5) -0.007(5) C9B 0.046(6) 0.053(9) 0.059(7) -0.013(6) 0.008(5) -0.006(6) C10B 0.028(5) 0.060(10) 0.068(7) -0.007(7) 0.006(5) 0.010(6) C11B 0.039(6) 0.049(9) 0.058(7) 0.008(6) -0.007(5) -0.013(5) C12B 0.054(7) 0.066(10) 0.057(7) 0.034(7) -0.021(5) -0.014(6) C14B 0.032(5) 0.042(9) 0.059(7) 0.016(6) -0.009(5) 0.005(5) C13B 0.041(6) 0.066(11) 0.070(8) 0.039(7) -0.010(5) -0.011(6) C15B 0.048(6) 0.061(11) 0.075(8) 0.017(8) -0.010(6) 0.004(6) C16B 0.081(9) 0.041(9) 0.084(10) 0.026(8) -0.013(8) 0.009(7) C17B 0.068(8) 0.033(9) 0.086(9) -0.016(7) -0.003(7) 0.006(7) C18B 0.036(5) 0.049(9) 0.065(7) 0.003(7) -0.006(5) 0.012(6) C19B 0.029(5) 0.046(8) 0.053(6) 0.012(6) 0.012(4) 0.007(5) C20B 0.028(5) 0.039(8) 0.045(6) 0.015(5) 0.007(4) 0.007(5) C21B 0.040(5) 0.034(7) 0.034(5) 0.007(5) 0.000(4) 0.001(5) C22B 0.027(4) 0.052(8) 0.038(5) 0.004(5) 0.003(4) 0.011(5) C23B 0.034(5) 0.061(9) 0.051(6) 0.012(6) 0.015(5) 0.019(5) C24B 0.034(5) 0.093(12) 0.059(7) 0.039(7) 0.010(5) 0.022(6) C25B 0.029(5) 0.083(11) 0.075(8) 0.015(7) 0.026(5) -0.001(6) C26B 0.037(5) 0.058(9) 0.057(7) 0.000(6) -0.007(5) 0.022(6) C27B 0.035(5) 0.040(7) 0.045(6) 0.002(5) 0.002(4) 0.015(5) C28B 0.043(5) 0.040(7) 0.028(5) 0.004(5) -0.001(4) 0.001(5) C29B 0.040(5) 0.047(8) 0.032(5) 0.007(5) 0.008(4) 0.010(5) C30B 0.026(4) 0.041(7) 0.035(5) 0.001(5) 0.000(4) 0.011(4) N1C 0.179(17) 0.20(2) 0.093(12) 0.034(13) -0.040(11) -0.010(15) C1C 0.122(14) 0.123(19) 0.094(12) 0.018(13) -0.014(11) -0.010(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.716(10) . ? S1 C2 1.746(11) . ? S2 C3 1.58(3) . ? S2 C2 1.738(10) . ? S2 C3A 1.88(3) . ? S3 C4A 1.72(2) . ? S3 C5 1.766(11) . ? S3 C4 1.90(4) . ? S4 C5 1.753(10) . ? S4 C1 1.768(10) . ? S5 C6 1.778(9) . ? S5 C7 1.782(9) . ? S6 C8 1.752(10) . ? S6 C6 1.775(9) . ? O1 C11 1.376(10) . ? O1 C9 1.438(12) . ? O2 C30 1.398(11) . ? O2 C10 1.435(9) . ? C1 C6 1.340(13) . ? C2 C5 1.339(14) . ? C3 C4 1.53(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3A C4A 1.53(2) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C7 C8 1.329(13) . ? C7 C9 1.524(13) . ? C8 C10 1.505(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C20 1.378(12) . ? C11 C12 1.399(13) . ? C12 C13 1.387(13) . ? C12 H12 0.9300 . ? C13 C14 1.389(13) . ? C13 H13 0.9300 . ? C14 C19 1.397(13) . ? C14 C15 1.416(13) . ? C15 C16 1.334(15) . ? C15 H15 0.9300 . ? C16 C17 1.387(15) . ? C16 H16 0.9300 . ? C17 C18 1.346(12) . ? C17 H17 0.9300 . ? C18 C19 1.444(13) . ? C18 H18 0.9300 . ? C19 C20 1.441(11) . ? C20 C21 1.480(12) . ? C21 C30 1.366(11) . ? C21 C22 1.427(13) . ? C22 C23 1.401(12) . ? C22 C27 1.419(12) . ? C23 C24 1.344(15) . ? C23 H23 0.9300 . ? C24 C25 1.412(14) . ? C24 H24 0.9300 . ? C25 C26 1.362(14) . ? C25 H25 0.9300 . ? C26 C27 1.420(14) . ? C26 H26 0.9300 . ? C27 C28 1.382(12) . ? C28 C29 1.333(14) . ? C28 H28 0.9300 . ? C29 C30 1.427(12) . ? C29 H29 0.9300 . ? S1B C2B 1.758(9) . ? S1B C1B 1.774(9) . ? S2B C2B 1.765(9) . ? S2B C3B 1.832(11) . ? S3B C5B 1.748(9) . ? S3B C4B 1.787(11) . ? S4B C1B 1.719(9) . ? S4B C5B 1.741(10) . ? S5B C6B 1.754(9) . ? S5B C7B 1.826(11) . ? S6B C8B 1.719(10) . ? S6B C6B 1.764(10) . ? O2B C10B 1.368(13) . ? O2B C30B 1.371(10) . ? O1B C11B 1.365(13) . ? O1B C9B 1.426(11) . ? C1B C6B 1.349(12) . ? C2B C5B 1.330(12) . ? C3B C4B 1.502(15) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C7B C8B 1.280(14) . ? C7B C9B 1.548(14) . ? C8B C10B 1.504(14) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B C20B 1.382(14) . ? C11B C12B 1.431(15) . ? C12B C13B 1.361(17) . ? C12B H12B 0.9300 . ? C14B C13B 1.400(15) . ? C14B C19B 1.402(14) . ? C14B C15B 1.408(17) . ? C13B H13B 0.9300 . ? C15B C16B 1.305(16) . ? C15B H15B 0.9300 . ? C16B C17B 1.394(16) . ? C16B H16B 0.9300 . ? C17B C18B 1.359(17) . ? C17B H17B 0.9300 . ? C18B C19B 1.451(15) . ? C18B H18B 0.9300 . ? C19B C20B 1.421(15) . ? C20B C21B 1.511(13) . ? C21B C30B 1.389(13) . ? C21B C22B 1.450(11) . ? C22B C27B 1.418(14) . ? C22B C23B 1.418(14) . ? C23B C24B 1.391(13) . ? C23B H23B 0.9300 . ? C24B C25B 1.379(15) . ? C24B H24B 0.9300 . ? C25B C26B 1.347(15) . ? C25B H25B 0.9300 . ? C26B C27B 1.453(12) . ? C26B H26B 0.9300 . ? C27B C28B 1.429(13) . ? C28B C29B 1.391(12) . ? C28B H28B 0.9300 . ? C29B C30B 1.386(13) . ? C29B H29B 0.9300 . ? N1C C1C 1.15(2) . ? C1C C2C 1.49(3) . ? C2C H2C1 0.9600 . ? C2C H2C2 0.9600 . ? C2C H2C3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 95.6(5) . . ? C3 S2 C2 103.7(11) . . ? C3 S2 C3A 22.6(13) . . ? C2 S2 C3A 101.4(8) . . ? C4A S3 C5 99.0(8) . . ? C4A S3 C4 24.0(12) . . ? C5 S3 C4 99.2(9) . . ? C5 S4 C1 93.0(5) . . ? C6 S5 C7 95.6(4) . . ? C8 S6 C6 97.2(5) . . ? C11 O1 C9 112.9(8) . . ? C30 O2 C10 118.9(7) . . ? C6 C1 S1 123.1(7) . . ? C6 C1 S4 121.7(7) . . ? S1 C1 S4 115.2(6) . . ? C5 C2 S2 128.4(8) . . ? C5 C2 S1 116.0(7) . . ? S2 C2 S1 115.5(6) . . ? C4 C3 S2 113(3) . . ? C4 C3 H3A 108.9 . . ? S2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? S2 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? C3 C4 S3 124(2) . . ? C3 C4 H4A 106.3 . . ? S3 C4 H4A 106.3 . . ? C3 C4 H4B 106.3 . . ? S3 C4 H4B 106.3 . . ? H4A C4 H4B 106.4 . . ? C4A C3A S2 119.3(17) . . ? C4A C3A H3A1 107.5 . . ? S2 C3A H3A1 107.5 . . ? C4A C3A H3A2 107.5 . . ? S2 C3A H3A2 107.5 . . ? H3A1 C3A H3A2 107.0 . . ? C3A C4A S3 111(2) . . ? C3A C4A H4A1 109.4 . . ? S3 C4A H4A1 109.4 . . ? C3A C4A H4A2 109.4 . . ? S3 C4A H4A2 109.4 . . ? H4A1 C4A H4A2 108.0 . . ? C2 C5 S4 118.6(8) . . ? C2 C5 S3 126.0(8) . . ? S4 C5 S3 115.3(6) . . ? C1 C6 S6 124.4(7) . . ? C1 C6 S5 122.7(7) . . ? S6 C6 S5 112.5(5) . . ? C8 C7 C9 127.7(9) . . ? C8 C7 S5 118.0(7) . . ? C9 C7 S5 114.0(7) . . ? C7 C8 C10 125.0(9) . . ? C7 C8 S6 116.8(8) . . ? C10 C8 S6 118.2(7) . . ? O1 C9 C7 107.7(8) . . ? O1 C9 H9A 110.2 . . ? C7 C9 H9A 110.2 . . ? O1 C9 H9B 110.2 . . ? C7 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O2 C10 C8 113.7(7) . . ? O2 C10 H10A 108.8 . . ? C8 C10 H10A 108.8 . . ? O2 C10 H10B 108.8 . . ? C8 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O1 C11 C20 117.3(8) . . ? O1 C11 C12 119.5(8) . . ? C20 C11 C12 123.2(8) . . ? C13 C12 C11 118.6(9) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 121.4(8) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C19 118.8(8) . . ? C13 C14 C15 123.1(9) . . ? C19 C14 C15 118.1(9) . . ? C16 C15 C14 123.2(10) . . ? C16 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C15 C16 C17 119.0(9) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 121.2(9) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.9(9) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C20 121.5(8) . . ? C14 C19 C18 117.5(8) . . ? C20 C19 C18 120.9(8) . . ? C11 C20 C19 116.3(8) . . ? C11 C20 C21 122.0(7) . . ? C19 C20 C21 121.6(8) . . ? C30 C21 C22 118.3(8) . . ? C30 C21 C20 121.2(9) . . ? C22 C21 C20 120.5(8) . . ? C23 C22 C27 118.3(9) . . ? C23 C22 C21 122.5(8) . . ? C27 C22 C21 119.1(8) . . ? C24 C23 C22 121.9(9) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 121.0(9) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 118.6(10) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 121.7(9) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C22 119.8(9) . . ? C28 C27 C26 121.7(9) . . ? C22 C27 C26 118.4(8) . . ? C29 C28 C27 121.4(9) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 120.0(9) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C21 C30 O2 117.3(8) . . ? C21 C30 C29 121.2(9) . . ? O2 C30 C29 121.5(8) . . ? C2B S1B C1B 92.7(4) . . ? C2B S2B C3B 103.1(5) . . ? C5B S3B C4B 99.1(5) . . ? C1B S4B C5B 94.6(4) . . ? C6B S5B C7B 93.5(5) . . ? C8B S6B C6B 96.2(5) . . ? C10B O2B C30B 114.5(8) . . ? C11B O1B C9B 114.6(9) . . ? C6B C1B S4B 125.3(7) . . ? C6B C1B S1B 119.1(7) . . ? S4B C1B S1B 115.5(5) . . ? C5B C2B S1B 117.8(7) . . ? C5B C2B S2B 129.1(7) . . ? S1B C2B S2B 113.1(5) . . ? C4B C3B S2B 114.4(7) . . ? C4B C3B H3B1 108.6 . . ? S2B C3B H3B1 108.6 . . ? C4B C3B H3B2 108.6 . . ? S2B C3B H3B2 108.6 . . ? H3B1 C3B H3B2 107.6 . . ? C3B C4B S3B 114.1(9) . . ? C3B C4B H4B1 108.7 . . ? S3B C4B H4B1 108.7 . . ? C3B C4B H4B2 108.7 . . ? S3B C4B H4B2 108.7 . . ? H4B1 C4B H4B2 107.6 . . ? C2B C5B S4B 117.6(7) . . ? C2B C5B S3B 125.8(7) . . ? S4B C5B S3B 116.3(5) . . ? C1B C6B S5B 123.7(7) . . ? C1B C6B S6B 122.3(7) . . ? S5B C6B S6B 114.0(5) . . ? C8B C7B C9B 125.8(10) . . ? C8B C7B S5B 117.3(8) . . ? C9B C7B S5B 116.8(8) . . ? C7B C8B C10B 124.4(9) . . ? C7B C8B S6B 118.8(8) . . ? C10B C8B S6B 116.3(8) . . ? O1B C9B C7B 116.0(9) . . ? O1B C9B H9B1 108.3 . . ? C7B C9B H9B1 108.3 . . ? O1B C9B H9B2 108.3 . . ? C7B C9B H9B2 108.3 . . ? H9B1 C9B H9B2 107.4 . . ? O2B C10B C8B 106.5(10) . . ? O2B C10B H10C 110.4 . . ? C8B C10B H10C 110.4 . . ? O2B C10B H10D 110.4 . . ? C8B C10B H10D 110.4 . . ? H10C C10B H10D 108.6 . . ? O1B C11B C20B 117.7(10) . . ? O1B C11B C12B 122.3(10) . . ? C20B C11B C12B 119.7(12) . . ? C13B C12B C11B 121.4(11) . . ? C13B C12B H12B 119.3 . . ? C11B C12B H12B 119.3 . . ? C13B C14B C19B 117.9(11) . . ? C13B C14B C15B 120.3(10) . . ? C19B C14B C15B 121.7(10) . . ? C12B C13B C14B 120.5(11) . . ? C12B C13B H13B 119.7 . . ? C14B C13B H13B 119.7 . . ? C16B C15B C14B 121.5(12) . . ? C16B C15B H15B 119.2 . . ? C14B C15B H15B 119.2 . . ? C15B C16B C17B 119.5(14) . . ? C15B C16B H16B 120.2 . . ? C17B C16B H16B 120.2 . . ? C18B C17B C16B 122.0(12) . . ? C18B C17B H17B 119.0 . . ? C16B C17B H17B 119.0 . . ? C17B C18B C19B 120.1(11) . . ? C17B C18B H18B 119.9 . . ? C19B C18B H18B 119.9 . . ? C14B C19B C20B 122.7(10) . . ? C14B C19B C18B 115.0(11) . . ? C20B C19B C18B 122.2(10) . . ? C11B C20B C19B 117.5(9) . . ? C11B C20B C21B 120.5(10) . . ? C19B C20B C21B 121.9(9) . . ? C30B C21B C22B 118.5(8) . . ? C30B C21B C20B 120.7(8) . . ? C22B C21B C20B 120.9(8) . . ? C27B C22B C23B 118.8(8) . . ? C27B C22B C21B 118.9(8) . . ? C23B C22B C21B 122.4(9) . . ? C24B C23B C22B 120.9(10) . . ? C24B C23B H23B 119.6 . . ? C22B C23B H23B 119.6 . . ? C25B C24B C23B 119.8(10) . . ? C25B C24B H24B 120.1 . . ? C23B C24B H24B 120.1 . . ? C26B C25B C24B 122.0(10) . . ? C26B C25B H25B 119.0 . . ? C24B C25B H25B 119.0 . . ? C25B C26B C27B 120.4(10) . . ? C25B C26B H26B 119.8 . . ? C27B C26B H26B 119.8 . . ? C22B C27B C28B 119.8(8) . . ? C22B C27B C26B 118.1(9) . . ? C28B C27B C26B 122.1(9) . . ? C29B C28B C27B 120.3(9) . . ? C29B C28B H28B 119.9 . . ? C27B C28B H28B 119.9 . . ? C30B C29B C28B 119.6(9) . . ? C30B C29B H29B 120.2 . . ? C28B C29B H29B 120.2 . . ? O2B C30B C29B 118.3(8) . . ? O2B C30B C21B 118.7(8) . . ? C29B C30B C21B 123.0(8) . . ? N1C C1C C2C 175(2) . . ? C1C C2C H2C1 109.5 . . ? C1C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? C1C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 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 C2 S1 C1 C6 168.9(9) . . . . ? C2 S1 C1 S4 -12.3(7) . . . . ? C5 S4 C1 C6 -168.5(9) . . . . ? C5 S4 C1 S1 12.8(7) . . . . ? C3 S2 C2 C5 35.1(18) . . . . ? C3A S2 C2 C5 12.0(15) . . . . ? C3 S2 C2 S1 -140.2(16) . . . . ? C3A S2 C2 S1 -163.3(11) . . . . ? C1 S1 C2 C5 6.5(10) . . . . ? C1 S1 C2 S2 -177.5(6) . . . . ? C2 S2 C3 C4 -55(3) . . . . ? C3A S2 C3 C4 31(3) . . . . ? S2 C3 C4 S3 49(5) . . . . ? C4A S3 C4 C3 81(4) . . . . ? C5 S3 C4 C3 -11(4) . . . . ? C3 S2 C3A C4A -80(4) . . . . ? C2 S2 C3A C4A 18(3) . . . . ? S2 C3A C4A S3 -59(3) . . . . ? C5 S3 C4A C3A 64(2) . . . . ? C4 S3 C4A C3A -28(2) . . . . ? S2 C2 C5 S4 -173.7(7) . . . . ? S1 C2 C5 S4 1.6(13) . . . . ? S2 C2 C5 S3 1.8(17) . . . . ? S1 C2 C5 S3 177.1(7) . . . . ? C1 S4 C5 C2 -8.6(10) . . . . ? C1 S4 C5 S3 175.4(7) . . . . ? C4A S3 C5 C2 -38.8(14) . . . . ? C4 S3 C5 C2 -14.5(17) . . . . ? C4A S3 C5 S4 136.8(11) . . . . ? C4 S3 C5 S4 161.1(15) . . . . ? S1 C1 C6 S6 -0.4(13) . . . . ? S4 C1 C6 S6 -179.1(6) . . . . ? S1 C1 C6 S5 171.7(6) . . . . ? S4 C1 C6 S5 -7.0(13) . . . . ? C8 S6 C6 C1 171.5(9) . . . . ? C8 S6 C6 S5 -1.3(7) . . . . ? C7 S5 C6 C1 -172.1(9) . . . . ? C7 S5 C6 S6 0.9(6) . . . . ? C6 S5 C7 C8 0.1(9) . . . . ? C6 S5 C7 C9 174.0(8) . . . . ? C9 C7 C8 C10 7.7(17) . . . . ? S5 C7 C8 C10 -179.3(8) . . . . ? C9 C7 C8 S6 -174.1(8) . . . . ? S5 C7 C8 S6 -1.1(12) . . . . ? C6 S6 C8 C7 1.5(9) . . . . ? C6 S6 C8 C10 179.8(8) . . . . ? C11 O1 C9 C7 -140.1(7) . . . . ? C8 C7 C9 O1 85.4(13) . . . . ? S5 C7 C9 O1 -87.8(8) . . . . ? C30 O2 C10 C8 -64.2(11) . . . . ? C7 C8 C10 O2 -49.2(15) . . . . ? S6 C8 C10 O2 132.6(8) . . . . ? C9 O1 C11 C20 115.7(9) . . . . ? C9 O1 C11 C12 -66.0(11) . . . . ? O1 C11 C12 C13 -176.7(9) . . . . ? C20 C11 C12 C13 1.4(15) . . . . ? C11 C12 C13 C14 -3.1(15) . . . . ? C12 C13 C14 C19 2.4(15) . . . . ? C12 C13 C14 C15 -177.9(10) . . . . ? C13 C14 C15 C16 178.1(11) . . . . ? C19 C14 C15 C16 -2.2(16) . . . . ? C14 C15 C16 C17 1.4(17) . . . . ? C15 C16 C17 C18 -0.7(17) . . . . ? C16 C17 C18 C19 0.8(16) . . . . ? C13 C14 C19 C20 0.0(14) . . . . ? C15 C14 C19 C20 -179.7(9) . . . . ? C13 C14 C19 C18 -178.2(9) . . . . ? C15 C14 C19 C18 2.2(14) . . . . ? C17 C18 C19 C14 -1.6(14) . . . . ? C17 C18 C19 C20 -179.7(9) . . . . ? O1 C11 C20 C19 179.0(8) . . . . ? C12 C11 C20 C19 0.8(14) . . . . ? O1 C11 C20 C21 -0.9(13) . . . . ? C12 C11 C20 C21 -179.1(9) . . . . ? C14 C19 C20 C11 -1.5(13) . . . . ? C18 C19 C20 C11 176.5(9) . . . . ? C14 C19 C20 C21 178.4(9) . . . . ? C18 C19 C20 C21 -3.6(14) . . . . ? C11 C20 C21 C30 -71.2(11) . . . . ? C19 C20 C21 C30 108.9(10) . . . . ? C11 C20 C21 C22 109.5(10) . . . . ? C19 C20 C21 C22 -70.4(11) . . . . ? C30 C21 C22 C23 173.4(8) . . . . ? C20 C21 C22 C23 -7.2(12) . . . . ? C30 C21 C22 C27 -3.5(11) . . . . ? C20 C21 C22 C27 175.9(7) . . . . ? C27 C22 C23 C24 2.3(13) . . . . ? C21 C22 C23 C24 -174.6(9) . . . . ? C22 C23 C24 C25 -1.4(15) . . . . ? C23 C24 C25 C26 -0.7(14) . . . . ? C24 C25 C26 C27 1.7(13) . . . . ? C23 C22 C27 C28 -178.0(8) . . . . ? C21 C22 C27 C28 -1.0(11) . . . . ? C23 C22 C27 C26 -1.3(11) . . . . ? C21 C22 C27 C26 175.7(8) . . . . ? C25 C26 C27 C28 175.9(8) . . . . ? C25 C26 C27 C22 -0.7(12) . . . . ? C22 C27 C28 C29 3.7(12) . . . . ? C26 C27 C28 C29 -172.9(8) . . . . ? C27 C28 C29 C30 -1.9(13) . . . . ? C22 C21 C30 O2 -177.8(7) . . . . ? C20 C21 C30 O2 2.8(11) . . . . ? C22 C21 C30 C29 5.4(12) . . . . ? C20 C21 C30 C29 -174.0(7) . . . . ? C10 O2 C30 C21 143.2(7) . . . . ? C10 O2 C30 C29 -39.9(11) . . . . ? C28 C29 C30 C21 -2.8(13) . . . . ? C28 C29 C30 O2 -179.5(8) . . . . ? C5B S4B C1B C6B 170.2(10) . . . . ? C5B S4B C1B S1B -13.0(7) . . . . ? C2B S1B C1B C6B -169.6(9) . . . . ? C2B S1B C1B S4B 13.5(7) . . . . ? C1B S1B C2B C5B -8.8(10) . . . . ? C1B S1B C2B S2B 169.4(7) . . . . ? C3B S2B C2B C5B -13.5(13) . . . . ? C3B S2B C2B S1B 168.5(6) . . . . ? C2B S2B C3B C4B -24.5(10) . . . . ? S2B C3B C4B S3B 65.0(10) . . . . ? C5B S3B C4B C3B -61.9(8) . . . . ? S1B C2B C5B S4B 1.4(12) . . . . ? S2B C2B C5B S4B -176.5(7) . . . . ? S1B C2B C5B S3B -171.8(6) . . . . ? S2B C2B C5B S3B 10.3(16) . . . . ? C1B S4B C5B C2B 7.1(10) . . . . ? C1B S4B C5B S3B -179.0(6) . . . . ? C4B S3B C5B C2B 24.3(11) . . . . ? C4B S3B C5B S4B -149.1(6) . . . . ? S4B C1B C6B S5B -1.0(14) . . . . ? S1B C1B C6B S5B -177.7(6) . . . . ? S4B C1B C6B S6B 179.2(6) . . . . ? S1B C1B C6B S6B 2.5(13) . . . . ? C7B S5B C6B C1B 176.7(10) . . . . ? C7B S5B C6B S6B -3.4(7) . . . . ? C8B S6B C6B C1B -175.5(9) . . . . ? C8B S6B C6B S5B 4.7(7) . . . . ? C6B S5B C7B C8B 0.5(10) . . . . ? C6B S5B C7B C9B -175.3(9) . . . . ? C9B C7B C8B C10B 6(2) . . . . ? S5B C7B C8B C10B -169.2(9) . . . . ? C9B C7B C8B S6B 178.2(9) . . . . ? S5B C7B C8B S6B 2.9(14) . . . . ? C6B S6B C8B C7B -4.6(11) . . . . ? C6B S6B C8B C10B 168.1(9) . . . . ? C11B O1B C9B C7B -62.5(13) . . . . ? C8B C7B C9B O1B -48.7(17) . . . . ? S5B C7B C9B O1B 126.7(9) . . . . ? C30B O2B C10B C8B -144.3(8) . . . . ? C7B C8B C10B O2B 86.4(14) . . . . ? S6B C8B C10B O2B -85.8(9) . . . . ? C9B O1B C11B C20B 144.9(9) . . . . ? C9B O1B C11B C12B -40.7(15) . . . . ? O1B C11B C12B C13B -176.8(11) . . . . ? C20B C11B C12B C13B -2.5(18) . . . . ? C11B C12B C13B C14B 0.5(18) . . . . ? C19B C14B C13B C12B -0.2(16) . . . . ? C15B C14B C13B C12B -178.1(12) . . . . ? C13B C14B C15B C16B 178.0(12) . . . . ? C19B C14B C15B C16B 0.1(18) . . . . ? C14B C15B C16B C17B -0.6(19) . . . . ? C15B C16B C17B C18B 0.1(19) . . . . ? C16B C17B C18B C19B 1.0(17) . . . . ? C13B C14B C19B C20B 1.8(15) . . . . ? C15B C14B C19B C20B 179.7(10) . . . . ? C13B C14B C19B C18B -177.1(9) . . . . ? C15B C14B C19B C18B 0.8(14) . . . . ? C17B C18B C19B C14B -1.3(14) . . . . ? C17B C18B C19B C20B 179.8(10) . . . . ? O1B C11B C20B C19B 178.5(9) . . . . ? C12B C11B C20B C19B 4.0(15) . . . . ? O1B C11B C20B C21B -4.7(14) . . . . ? C12B C11B C20B C21B -179.2(10) . . . . ? C14B C19B C20B C11B -3.7(14) . . . . ? C18B C19B C20B C11B 175.1(9) . . . . ? C14B C19B C20B C21B 179.5(8) . . . . ? C18B C19B C20B C21B -1.7(14) . . . . ? C11B C20B C21B C30B -61.9(14) . . . . ? C19B C20B C21B C30B 114.8(11) . . . . ? C11B C20B C21B C22B 117.0(11) . . . . ? C19B C20B C21B C22B -66.4(13) . . . . ? C30B C21B C22B C27B 1.0(15) . . . . ? C20B C21B C22B C27B -177.9(10) . . . . ? C30B C21B C22B C23B -178.5(10) . . . . ? C20B C21B C22B C23B 2.7(16) . . . . ? C27B C22B C23B C24B -0.9(17) . . . . ? C21B C22B C23B C24B 178.5(11) . . . . ? C22B C23B C24B C25B 0.3(19) . . . . ? C23B C24B C25B C26B 2(2) . . . . ? C24B C25B C26B C27B -3.8(19) . . . . ? C23B C22B C27B C28B -179.7(10) . . . . ? C21B C22B C27B C28B 0.9(16) . . . . ? C23B C22B C27B C26B -0.6(16) . . . . ? C21B C22B C27B C26B 179.9(10) . . . . ? C25B C26B C27B C22B 3.0(16) . . . . ? C25B C26B C27B C28B -178.0(11) . . . . ? C22B C27B C28B C29B -2.4(15) . . . . ? C26B C27B C28B C29B 178.6(10) . . . . ? C27B C28B C29B C30B 2.1(15) . . . . ? C10B O2B C30B C29B -62.6(12) . . . . ? C10B O2B C30B C21B 120.2(10) . . . . ? C28B C29B C30B O2B -177.2(9) . . . . ? C28B C29B C30B C21B -0.2(16) . . . . ? C22B C21B C30B O2B 175.7(9) . . . . ? C20B C21B C30B O2B -5.5(15) . . . . ? C22B C21B C30B C29B -1.4(16) . . . . ? C20B C21B C30B C29B 177.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.720 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.168 # Attachment '-S--1-TCNQF4.cif' data_-S--1-TCNQF4 _database_code_depnum_ccdc_archive 'CCDC 809761' #TrackingRef '-S--1-TCNQF4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 O2 S6, C12 F4 N4, C H2 Cl2' _chemical_formula_sum 'C43 H22 Cl2 F4 N4 O2 S6' _chemical_formula_weight 965.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.5594(3) _cell_length_b 13.0019(3) _cell_length_c 18.8153(5) _cell_angle_alpha 106.5560(10) _cell_angle_beta 90.8750(10) _cell_angle_gamma 92.7280(10) _cell_volume 2003.93(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9167 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.42 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.973 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.901982 #-------------------------------------------------------------------# _diffrn_ambient_temperature 150(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 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32054 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.45 _reflns_number_total 15364 _reflns_number_gt 14332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0888P)^2^+0.3214P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 15364 _refine_ls_number_parameters 1137 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 S1 S 0.26770(11) 0.78503(7) 0.40524(5) 0.02254(19) Uani 1 1 d . . . S2 S 0.08324(14) 0.87121(9) 0.53874(7) 0.0383(3) Uani 1 1 d . . . S4 S 0.25676(12) 0.56533(7) 0.41424(5) 0.0268(2) Uani 1 1 d . A . S5 S 0.42916(9) 0.49032(7) 0.25479(5) 0.01749(17) Uani 1 1 d . . . S6 S 0.44165(10) 0.71372(7) 0.25121(5) 0.01949(18) Uani 1 1 d . . . O1 O 0.3895(3) 0.3914(2) 0.06480(13) 0.0197(5) Uani 1 1 d . . . O2 O 0.4896(3) 0.59608(19) 0.03915(13) 0.0178(5) Uani 1 1 d . . . C1 C 0.3138(4) 0.6542(3) 0.36621(19) 0.0192(7) Uani 1 1 d . . . C2 C 0.1635(5) 0.7597(3) 0.4770(2) 0.0301(9) Uani 1 1 d . A . C3 C 0.1535(6) 0.6566(3) 0.4801(3) 0.0413(12) Uani 1 1 d . . . S3 S 0.0233(4) 0.60196(14) 0.53165(15) 0.0322(9) Uani 0.613(8) 1 d P A 1 C4 C 0.0242(18) 0.7221(9) 0.6167(6) 0.063(3) Uani 0.613(8) 1 d P A 1 H4A H -0.0461 0.7057 0.6524 0.076 Uiso 0.613(8) 1 calc PR A 1 H4B H 0.1287 0.7351 0.6392 0.076 Uiso 0.613(8) 1 calc PR A 1 C5 C -0.0178(14) 0.8085(8) 0.6021(6) 0.053(3) Uani 0.613(8) 1 d P A 1 H5A H -0.0193 0.8634 0.6494 0.064 Uiso 0.613(8) 1 calc PR A 1 H5B H -0.1256 0.7941 0.5839 0.064 Uiso 0.613(8) 1 calc PR A 1 S3A S 0.1075(6) 0.6098(2) 0.5619(2) 0.0344(14) Uani 0.387(8) 1 d P A 2 C4A C -0.0336(18) 0.7089(14) 0.5953(10) 0.042(4) Uiso 0.387(8) 1 d P A 2 H4A1 H -0.1123 0.7075 0.5573 0.050 Uiso 0.387(8) 1 calc PR A 2 H4A2 H -0.0844 0.6995 0.6389 0.050 Uiso 0.387(8) 1 calc PR A 2 C5A C 0.081(2) 0.8216(9) 0.6155(5) 0.033(3) Uani 0.387(8) 1 d P A 2 H5A1 H 0.1858 0.8069 0.6281 0.039 Uiso 0.387(8) 1 calc PR A 2 H5A2 H 0.0406 0.8744 0.6578 0.039 Uiso 0.387(8) 1 calc PR A 2 C6 C 0.3898(4) 0.6225(3) 0.29893(19) 0.0189(7) Uani 1 1 d . . . C7 C 0.4966(4) 0.5156(3) 0.17416(18) 0.0166(6) Uani 1 1 d . . . C8 C 0.5023(4) 0.6202(3) 0.17270(18) 0.0173(7) Uani 1 1 d . . . C9 C 0.5308(4) 0.4212(3) 0.10969(19) 0.0205(7) Uani 1 1 d . . . H9A H 0.6147 0.4405 0.0811 0.025 Uiso 1 1 calc R . . H9B H 0.5621 0.3617 0.1272 0.025 Uiso 1 1 calc R . . C10 C 0.5561(4) 0.6610(3) 0.10923(18) 0.0200(7) Uani 1 1 d . . . H10A H 0.5263 0.7344 0.1176 0.024 Uiso 1 1 calc R . . H10B H 0.6693 0.6610 0.1076 0.024 Uiso 1 1 calc R . . C11 C 0.4176(4) 0.3563(3) -0.01176(19) 0.0204(7) Uani 1 1 d . . . C12 C 0.5043(5) 0.2645(3) -0.0392(2) 0.0277(8) Uani 1 1 d . . . H12 H 0.5411 0.2276 -0.0073 0.033 Uiso 1 1 calc R . . C13 C 0.5336(5) 0.2305(3) -0.1128(2) 0.0281(8) Uani 1 1 d . . . H13 H 0.5907 0.1700 -0.1311 0.034 Uiso 1 1 calc R . . C14 C 0.4781(4) 0.2864(3) -0.1619(2) 0.0243(8) Uani 1 1 d . . . C15 C 0.5156(5) 0.2570(4) -0.2379(2) 0.0323(9) Uani 1 1 d . . . H15 H 0.5760 0.1981 -0.2565 0.039 Uiso 1 1 calc R . . C16 C 0.4658(5) 0.3124(4) -0.2843(2) 0.0340(9) Uani 1 1 d . . . H16 H 0.4937 0.2920 -0.3338 0.041 Uiso 1 1 calc R . . C17 C 0.3722(5) 0.4004(4) -0.2579(2) 0.0295(9) Uani 1 1 d . . . H17 H 0.3364 0.4371 -0.2902 0.035 Uiso 1 1 calc R . . C18 C 0.3332(4) 0.4326(3) -0.18438(19) 0.0218(7) Uani 1 1 d . . . H18 H 0.2723 0.4915 -0.1673 0.026 Uiso 1 1 calc R . . C19 C 0.3851(4) 0.3765(3) -0.13419(19) 0.0190(7) Uani 1 1 d . . . C20 C 0.3544(4) 0.4112(3) -0.05635(19) 0.0181(7) Uani 1 1 d . . . C21 C 0.2602(4) 0.5066(3) -0.02388(18) 0.0180(7) Uani 1 1 d . . . C22 C 0.0973(4) 0.5059(3) -0.04325(19) 0.0235(8) Uani 1 1 d . . . C23 C 0.0164(4) 0.4133(3) -0.0905(2) 0.0284(8) Uani 1 1 d . . . H23 H 0.0692 0.3511 -0.1103 0.034 Uiso 1 1 calc R . . C24 C -0.1424(5) 0.4157(4) -0.1072(3) 0.0407(11) Uani 1 1 d . . . H24 H -0.1954 0.3542 -0.1374 0.049 Uiso 1 1 calc R . . C25 C -0.2236(5) 0.5094(4) -0.0793(3) 0.0411(11) Uani 1 1 d . . . H25 H -0.3290 0.5103 -0.0918 0.049 Uiso 1 1 calc R . . C26 C -0.1477(5) 0.5991(4) -0.0339(2) 0.0355(10) Uani 1 1 d . . . H26 H -0.2024 0.6609 -0.0161 0.043 Uiso 1 1 calc R . . C27 C 0.0118(4) 0.6005(3) -0.0133(2) 0.0257(8) Uani 1 1 d . . . C28 C 0.0903(5) 0.6919(3) 0.0369(2) 0.0263(8) Uani 1 1 d . . . H28 H 0.0363 0.7537 0.0564 0.032 Uiso 1 1 calc R . . C29 C 0.2456(4) 0.6902(3) 0.05701(19) 0.0213(7) Uani 1 1 d . . . H29 H 0.2946 0.7495 0.0913 0.026 Uiso 1 1 calc R . . C30 C 0.3303(4) 0.5985(3) 0.02564(18) 0.0165(6) Uani 1 1 d . . . S1B S 0.74841(10) 0.53579(7) -0.63272(5) 0.02048(18) Uani 1 1 d . . . S2B S 0.87141(11) 0.40622(8) -0.77046(5) 0.0271(2) Uani 1 1 d . . . S3B S 0.96465(12) 0.65662(8) -0.80346(6) 0.0294(2) Uani 1 1 d . . . S4B S 0.80147(10) 0.74413(7) -0.66027(5) 0.01962(18) Uani 1 1 d . . . S5B S 0.62689(10) 0.85389(7) -0.50201(4) 0.01787(17) Uani 1 1 d . B . S6B S 0.58786(11) 0.64003(7) -0.48187(5) 0.02176(19) Uani 1 1 d . B . O1B O 0.5644(3) 0.9558(2) -0.28806(13) 0.0184(5) Uani 1 1 d . . . O2B O 0.6329(3) 0.7266(2) -0.29737(13) 0.0205(5) Uani 1 1 d . B . C1B C 0.7272(4) 0.6720(3) -0.60329(19) 0.0186(7) Uani 1 1 d . B . C2B C 0.8381(4) 0.5355(3) -0.7153(2) 0.0200(7) Uani 1 1 d . B . C3B C 1.0388(18) 0.4313(12) -0.8125(10) 0.032(5) Uani 0.307(17) 1 d P B 3 H3B1 H 1.1219 0.4587 -0.7753 0.038 Uiso 0.307(17) 1 calc PR B 3 H3B2 H 1.0710 0.3650 -0.8464 0.038 Uiso 0.307(17) 1 calc PR B 3 C4B C 1.012(3) 0.5138(14) -0.8553(10) 0.026(4) Uani 0.307(17) 1 d P B 3 H4B1 H 0.9271 0.4844 -0.8912 0.031 Uiso 0.307(17) 1 calc PR B 3 H4B2 H 1.1050 0.5183 -0.8832 0.031 Uiso 0.307(17) 1 calc PR B 3 C3C C 0.9688(9) 0.4341(5) -0.8504(4) 0.029(2) Uani 0.693(17) 1 d P B 4 H3C1 H 1.0346 0.3754 -0.8725 0.035 Uiso 0.693(17) 1 calc PR B 4 H3C2 H 0.8895 0.4361 -0.8873 0.035 Uiso 0.693(17) 1 calc PR B 4 C4C C 1.0691(10) 0.5396(7) -0.8308(5) 0.0252(17) Uani 0.693(17) 1 d P B 4 H4C1 H 1.1295 0.5418 -0.8736 0.030 Uiso 0.693(17) 1 calc PR B 4 H4C2 H 1.1426 0.5398 -0.7910 0.030 Uiso 0.693(17) 1 calc PR B 4 C5B C 0.8677(4) 0.6330(3) -0.7275(2) 0.0219(7) Uani 1 1 d . B . C6B C 0.6529(4) 0.7188(3) -0.53673(18) 0.0178(7) Uani 1 1 d . . . C7B C 0.5507(4) 0.8466(3) -0.41825(18) 0.0182(7) Uani 1 1 d . . . C8B C 0.5331(4) 0.7466(3) -0.40930(19) 0.0183(7) Uani 1 1 d . B . C9B C 0.5089(4) 0.9514(3) -0.36168(18) 0.0180(7) Uani 1 1 d . B . H9B1 H 0.5553 1.0120 -0.3757 0.022 Uiso 1 1 calc R . . H9B2 H 0.3963 0.9566 -0.3619 0.022 Uiso 1 1 calc R . . C10B C 0.4881(4) 0.7211(3) -0.33897(18) 0.0207(7) Uani 1 1 d . . . H10C H 0.4174 0.7729 -0.3112 0.025 Uiso 1 1 calc R B . H10D H 0.4372 0.6498 -0.3500 0.025 Uiso 1 1 calc R . . C11B C 0.7244(4) 0.9746(3) -0.27100(18) 0.0161(6) Uani 1 1 d . . . C12B C 0.8166(4) 1.0466(3) -0.3001(2) 0.0216(7) Uani 1 1 d . . . H12B H 0.7722 1.0784 -0.3334 0.026 Uiso 1 1 calc R . . C13B C 0.9709(4) 1.0684(3) -0.2787(2) 0.0258(8) Uani 1 1 d . . . H13B H 1.0297 1.1179 -0.2958 0.031 Uiso 1 1 calc R . . C14B C 1.0428(4) 1.0165(3) -0.2307(2) 0.0262(8) Uani 1 1 d . . . C15B C 1.2072(5) 1.0303(4) -0.2126(2) 0.0375(10) Uani 1 1 d . . . H15B H 1.2682 1.0789 -0.2297 0.045 Uiso 1 1 calc R . . C16B C 1.2756(5) 0.9745(4) -0.1714(3) 0.0423(11) Uani 1 1 d . . . H16B H 1.3829 0.9836 -0.1612 0.051 Uiso 1 1 calc R . . C17B C 1.1838(5) 0.9021(4) -0.1437(3) 0.0390(10) Uani 1 1 d . . . H17B H 1.2316 0.8644 -0.1149 0.047 Uiso 1 1 calc R . . C18B C 1.0246(4) 0.8863(3) -0.1584(2) 0.0286(8) Uani 1 1 d . . . H18B H 0.9663 0.8385 -0.1396 0.034 Uiso 1 1 calc R . . C19B C 0.9498(4) 0.9433(3) -0.20251(18) 0.0196(7) Uani 1 1 d . . . C20B C 0.7864(4) 0.9270(3) -0.22042(17) 0.0172(7) Uani 1 1 d . . . C21B C 0.6849(4) 0.8620(3) -0.18315(18) 0.0161(6) Uani 1 1 d . B . C22B C 0.6605(4) 0.9012(3) -0.10488(18) 0.0181(7) Uani 1 1 d . . . C23B C 0.7247(4) 1.0029(3) -0.0609(2) 0.0217(7) Uani 1 1 d . . . H23B H 0.7870 1.0452 -0.0829 0.026 Uiso 1 1 calc R . . C24B C 0.6960(4) 1.0393(3) 0.0132(2) 0.0257(8) Uani 1 1 d . . . H24B H 0.7402 1.1055 0.0411 0.031 Uiso 1 1 calc R . . C25B C 0.6000(5) 0.9775(4) 0.0479(2) 0.0299(9) Uani 1 1 d . . . H25B H 0.5794 1.0036 0.0981 0.036 Uiso 1 1 calc R . . C26B C 0.5381(5) 0.8800(4) 0.0077(2) 0.0301(9) Uani 1 1 d . . . H26B H 0.4760 0.8395 0.0310 0.036 Uiso 1 1 calc R . . C27B C 0.5659(4) 0.8382(3) -0.06940(19) 0.0209(7) Uani 1 1 d . . . C28B C 0.5012(5) 0.7367(3) -0.1116(2) 0.0263(8) Uani 1 1 d . . . H28B H 0.4423 0.6943 -0.0884 0.032 Uiso 1 1 calc R . . C29B C 0.5240(5) 0.7000(3) -0.1863(2) 0.0251(8) Uani 1 1 d . B . H29B H 0.4804 0.6334 -0.2137 0.030 Uiso 1 1 calc R . . C30B C 0.6148(4) 0.7645(3) -0.22143(18) 0.0191(7) Uani 1 1 d . . . N1D N 0.7662(4) 0.8584(3) 0.2204(2) 0.0325(8) Uani 1 1 d . . . N2D N 0.8780(4) 1.1600(3) 0.1876(2) 0.0327(8) Uani 1 1 d . . . N3D N 0.1573(5) 1.1613(3) 0.58409(19) 0.0353(8) Uani 1 1 d . . . N4D N 0.3444(5) 1.4638(3) 0.5675(2) 0.0449(10) Uani 1 1 d . . . F1D F 0.3701(3) 1.03332(17) 0.45998(12) 0.0258(5) Uani 1 1 d . . . F2D F 0.5493(3) 0.94347(16) 0.35041(12) 0.0254(5) Uani 1 1 d . . . F3D F 0.6567(3) 1.28278(16) 0.30841(12) 0.0255(5) Uani 1 1 d . . . F4D F 0.4761(3) 1.37213(16) 0.41589(12) 0.0250(5) Uani 1 1 d . . . C1D C 0.4143(4) 1.2091(3) 0.44607(19) 0.0177(7) Uani 1 1 d . . . C2D C 0.4373(4) 1.0964(3) 0.42260(19) 0.0195(7) Uani 1 1 d . . . C3D C 0.5315(4) 1.0508(3) 0.36504(19) 0.0193(7) Uani 1 1 d . . . C4D C 0.6132(4) 1.1070(3) 0.32179(19) 0.0184(7) Uani 1 1 d . . . C5D C 0.5858(4) 1.2190(3) 0.3443(2) 0.0190(7) Uani 1 1 d . . . C6D C 0.4936(4) 1.2658(3) 0.40209(19) 0.0187(7) Uani 1 1 d . . . C7D C 0.7137(4) 1.0595(3) 0.26319(19) 0.0189(7) Uani 1 1 d . . . C8D C 0.7397(4) 0.9477(3) 0.2410(2) 0.0241(8) Uani 1 1 d . . . C9D C 0.8005(4) 1.1187(3) 0.2225(2) 0.0236(8) Uani 1 1 d . . . C10D C 0.3270(4) 1.2590(3) 0.50912(19) 0.0208(7) Uani 1 1 d . . . C11D C 0.2354(5) 1.2011(3) 0.5497(2) 0.0257(8) Uani 1 1 d . . . C12D C 0.3347(5) 1.3722(3) 0.5403(2) 0.0273(8) Uani 1 1 d . . . N1E N 0.3715(4) 0.9118(3) 0.18765(17) 0.0272(7) Uani 1 1 d . . . N2E N 0.4085(5) 1.2282(3) 0.1761(2) 0.0369(8) Uani 1 1 d . . . N3E N -0.3000(4) 1.1077(3) 0.54647(19) 0.0285(7) Uani 1 1 d . . . N4E N -0.2387(5) 1.4243(3) 0.5402(2) 0.0364(8) Uani 1 1 d . . . F1E F -0.0549(3) 1.01765(17) 0.42718(13) 0.0290(5) Uani 1 1 d . . . F2E F 0.1386(3) 0.95797(17) 0.31776(12) 0.0266(5) Uani 1 1 d . . . F3E F 0.1921(3) 1.31777(16) 0.30460(12) 0.0252(5) Uani 1 1 d . . . F4E F 0.0006(3) 1.37697(17) 0.41428(13) 0.0280(5) Uani 1 1 d . . . C1E C -0.0382(4) 1.2013(3) 0.42786(19) 0.0182(7) Uani 1 1 d . . . C2E C 0.0066(4) 1.0938(3) 0.3981(2) 0.0200(7) Uani 1 1 d . . . C3E C 0.1058(4) 1.0628(3) 0.3407(2) 0.0195(7) Uani 1 1 d . . . C5E C 0.1320(4) 1.2424(3) 0.33438(19) 0.0179(7) Uani 1 1 d . . . C6E C 0.0346(4) 1.2732(3) 0.3921(2) 0.0196(7) Uani 1 1 d . . . C7E C 0.2784(4) 1.1023(3) 0.24458(19) 0.0196(7) Uani 1 1 d . . . C9E C 0.3464(5) 1.1749(3) 0.2074(2) 0.0254(8) Uani 1 1 d . . . C8E C 0.3240(4) 0.9954(3) 0.21429(19) 0.0222(7) Uani 1 1 d . . . C4E C 0.1760(4) 1.1343(3) 0.30466(19) 0.0179(7) Uani 1 1 d . . . C10E C -0.1443(4) 1.2330(3) 0.48549(19) 0.0200(7) Uani 1 1 d . . . C11E C -0.2239(4) 1.1605(3) 0.5187(2) 0.0223(7) Uani 1 1 d . . . C12E C -0.1917(4) 1.3405(3) 0.5141(2) 0.0249(8) Uani 1 1 d . . . C1F C 0.8493(7) 0.4833(5) 0.7237(3) 0.0563(14) Uani 1 1 d . . . H1F1 H 0.7933 0.4979 0.6828 0.068 Uiso 1 1 calc R . . H1F2 H 0.7742 0.4786 0.7609 0.068 Uiso 1 1 calc R . . Cl1F Cl 0.9888(3) 0.58882(15) 0.76213(11) 0.0836(5) Uani 1 1 d . . . Cl2F Cl 0.9396(2) 0.35960(13) 0.69171(9) 0.0694(4) Uani 1 1 d . . . C1G C 0.2054(9) 0.1177(7) 0.0164(5) 0.084(2) Uiso 1 1 d . C 5 H1G1 H 0.2720 0.1664 0.0548 0.101 Uiso 1 1 calc R C 5 H1G2 H 0.2705 0.0864 -0.0251 0.101 Uiso 1 1 calc R C 5 Cl1G Cl 0.1280(2) 0.01572(16) 0.05027(10) 0.0751(5) Uani 1 1 d . C 5 Cl2G Cl 0.0662(2) 0.19111(15) -0.01242(11) 0.0807(5) Uani 1 1 d . C 5 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 S1 0.0276(4) 0.0157(4) 0.0249(4) 0.0061(4) 0.0030(4) 0.0034(3) S2 0.0472(6) 0.0267(5) 0.0393(6) 0.0039(5) 0.0163(5) 0.0161(5) S4 0.0379(5) 0.0139(4) 0.0286(5) 0.0053(4) 0.0159(4) -0.0008(4) S5 0.0212(4) 0.0153(4) 0.0170(4) 0.0065(3) 0.0022(3) -0.0003(3) S6 0.0260(4) 0.0148(4) 0.0183(4) 0.0060(3) -0.0003(3) -0.0015(3) O1 0.0203(12) 0.0220(13) 0.0166(11) 0.0062(10) -0.0023(9) -0.0037(10) O2 0.0181(11) 0.0201(12) 0.0140(11) 0.0039(10) -0.0015(9) -0.0029(9) C1 0.0231(17) 0.0138(16) 0.0203(17) 0.0046(14) -0.0002(14) -0.0011(13) C2 0.034(2) 0.023(2) 0.033(2) 0.0071(17) 0.0158(17) 0.0042(16) C3 0.059(3) 0.019(2) 0.043(3) 0.0032(19) 0.035(2) 0.0039(19) S3 0.0416(17) 0.0250(9) 0.0315(13) 0.0092(8) 0.0188(12) 0.0024(8) C4 0.085(9) 0.061(7) 0.031(5) -0.004(5) 0.021(5) -0.013(6) C5 0.055(6) 0.044(5) 0.057(6) 0.003(5) 0.031(5) 0.011(5) S3A 0.044(3) 0.0313(16) 0.0287(19) 0.0086(12) 0.018(2) 0.0002(13) C5A 0.053(8) 0.029(6) 0.009(4) -0.004(4) -0.003(5) -0.006(6) C6 0.0173(16) 0.0186(17) 0.0203(17) 0.0051(14) 0.0010(13) -0.0021(13) C7 0.0167(16) 0.0201(17) 0.0126(14) 0.0045(13) -0.0012(12) -0.0026(13) C8 0.0187(16) 0.0190(17) 0.0135(15) 0.0042(13) -0.0028(12) -0.0037(13) C9 0.0223(17) 0.0218(18) 0.0175(16) 0.0058(14) 0.0007(13) 0.0012(14) C10 0.0257(18) 0.0202(18) 0.0138(15) 0.0052(14) -0.0017(13) -0.0058(14) C11 0.0223(17) 0.0184(17) 0.0181(16) 0.0024(14) -0.0005(13) -0.0063(13) C12 0.035(2) 0.0174(18) 0.032(2) 0.0083(16) -0.0008(16) 0.0002(15) C13 0.032(2) 0.0187(18) 0.028(2) -0.0025(16) -0.0023(16) 0.0028(15) C14 0.0227(18) 0.0222(19) 0.0218(17) -0.0029(15) -0.0034(14) -0.0041(14) C15 0.031(2) 0.032(2) 0.0244(19) -0.0070(17) 0.0005(16) 0.0005(16) C16 0.035(2) 0.044(3) 0.0172(17) -0.0009(17) 0.0018(16) -0.0016(18) C17 0.033(2) 0.036(2) 0.0179(17) 0.0073(16) -0.0023(15) -0.0058(17) C18 0.0202(17) 0.0246(18) 0.0187(16) 0.0037(14) 0.0000(13) -0.0030(14) C19 0.0193(16) 0.0153(16) 0.0183(16) -0.0008(13) -0.0005(13) -0.0062(13) C20 0.0163(16) 0.0170(16) 0.0183(16) 0.0020(13) 0.0016(12) -0.0078(13) C21 0.0183(16) 0.0221(18) 0.0137(15) 0.0054(13) 0.0025(12) 0.0006(13) C22 0.0174(16) 0.038(2) 0.0153(15) 0.0081(15) 0.0002(13) -0.0026(15) C23 0.0189(18) 0.036(2) 0.0290(19) 0.0091(17) -0.0023(15) -0.0060(16) C24 0.022(2) 0.060(3) 0.039(2) 0.015(2) -0.0047(18) -0.008(2) C25 0.0177(19) 0.068(3) 0.034(2) 0.010(2) -0.0005(16) 0.002(2) C26 0.0205(19) 0.054(3) 0.033(2) 0.012(2) 0.0075(16) 0.0099(18) C27 0.0206(18) 0.036(2) 0.0233(18) 0.0119(17) 0.0059(14) 0.0022(15) C28 0.032(2) 0.030(2) 0.0183(17) 0.0082(16) 0.0076(15) 0.0110(16) C29 0.0275(18) 0.0179(17) 0.0179(16) 0.0049(14) 0.0021(14) -0.0034(14) C30 0.0159(15) 0.0210(17) 0.0144(15) 0.0076(13) 0.0038(12) 0.0000(13) S1B 0.0288(5) 0.0147(4) 0.0185(4) 0.0049(3) 0.0034(3) 0.0050(3) S2B 0.0327(5) 0.0179(4) 0.0273(5) 0.0002(4) 0.0090(4) 0.0035(4) S3B 0.0344(5) 0.0251(5) 0.0274(5) 0.0051(4) 0.0163(4) -0.0011(4) S4B 0.0248(4) 0.0163(4) 0.0173(4) 0.0043(3) 0.0043(3) -0.0005(3) S5B 0.0247(4) 0.0144(4) 0.0145(4) 0.0041(3) 0.0031(3) 0.0009(3) S6B 0.0361(5) 0.0147(4) 0.0144(4) 0.0041(3) 0.0034(3) -0.0005(4) O1B 0.0179(11) 0.0213(12) 0.0144(11) 0.0029(10) 0.0008(9) -0.0021(9) O2B 0.0241(12) 0.0243(13) 0.0117(11) 0.0029(10) 0.0017(9) 0.0002(10) C1B 0.0221(17) 0.0154(17) 0.0170(16) 0.0028(14) -0.0032(13) 0.0019(13) C2B 0.0202(17) 0.0194(17) 0.0179(16) 0.0012(14) 0.0047(13) 0.0025(13) C3B 0.022(7) 0.041(8) 0.041(10) 0.023(7) 0.011(7) 0.006(6) C4B 0.044(11) 0.014(8) 0.018(8) 0.000(6) 0.008(7) 0.006(7) C3C 0.033(4) 0.024(3) 0.026(4) 0.001(3) 0.012(3) 0.001(2) C4C 0.026(4) 0.022(4) 0.026(4) 0.004(3) 0.005(3) 0.001(3) C5B 0.0216(17) 0.0224(18) 0.0202(17) 0.0037(15) 0.0034(14) -0.0012(14) C6B 0.0237(17) 0.0158(16) 0.0138(15) 0.0039(13) -0.0013(13) 0.0004(13) C7B 0.0214(17) 0.0197(17) 0.0124(15) 0.0034(13) -0.0004(13) -0.0006(13) C8B 0.0205(16) 0.0164(16) 0.0156(15) 0.0017(13) -0.0020(13) -0.0043(13) C9B 0.0218(17) 0.0151(16) 0.0153(15) 0.0010(13) 0.0018(13) 0.0022(13) C10B 0.0267(18) 0.0231(18) 0.0123(15) 0.0063(14) -0.0029(13) -0.0041(14) C11B 0.0159(15) 0.0167(16) 0.0138(14) 0.0013(13) 0.0028(12) -0.0010(12) C12B 0.0254(18) 0.0189(17) 0.0210(17) 0.0065(14) 0.0048(14) -0.0014(14) C13B 0.0271(19) 0.0259(19) 0.0224(17) 0.0045(15) 0.0107(15) -0.0071(15) C14B 0.0195(17) 0.030(2) 0.0256(18) 0.0036(16) 0.0069(14) -0.0037(15) C15B 0.024(2) 0.051(3) 0.034(2) 0.007(2) 0.0073(17) -0.0088(18) C16B 0.0192(19) 0.062(3) 0.042(3) 0.009(2) 0.0005(18) 0.006(2) C17B 0.027(2) 0.052(3) 0.036(2) 0.009(2) -0.0028(18) 0.0097(19) C18B 0.0227(18) 0.036(2) 0.0277(19) 0.0093(17) 0.0066(15) 0.0085(16) C19B 0.0182(16) 0.0243(18) 0.0140(15) 0.0013(14) 0.0034(13) 0.0026(13) C20B 0.0205(16) 0.0190(17) 0.0103(14) 0.0018(13) 0.0035(12) -0.0035(13) C21B 0.0184(16) 0.0165(16) 0.0150(15) 0.0074(13) 0.0003(12) -0.0007(12) C22B 0.0185(16) 0.0216(17) 0.0147(15) 0.0059(14) 0.0001(13) 0.0019(13) C23B 0.0252(18) 0.0204(18) 0.0197(16) 0.0066(14) -0.0011(14) -0.0023(14) C24B 0.0295(19) 0.028(2) 0.0162(16) 0.0009(15) -0.0035(14) 0.0006(15) C25B 0.033(2) 0.040(2) 0.0152(17) 0.0044(17) 0.0038(15) -0.0009(17) C26B 0.032(2) 0.040(2) 0.0197(18) 0.0122(17) 0.0067(15) -0.0045(17) C27B 0.0229(17) 0.0253(19) 0.0172(16) 0.0114(15) -0.0029(14) -0.0029(14) C28B 0.032(2) 0.029(2) 0.0228(18) 0.0162(16) 0.0015(15) -0.0078(16) C29B 0.035(2) 0.0197(18) 0.0209(17) 0.0084(15) -0.0013(15) -0.0066(15) C30B 0.0233(17) 0.0226(18) 0.0142(15) 0.0092(14) 0.0026(13) 0.0023(14) N1D 0.042(2) 0.0256(18) 0.0312(18) 0.0078(15) 0.0108(15) 0.0097(15) N2D 0.041(2) 0.0265(18) 0.0285(17) 0.0044(15) 0.0103(15) -0.0036(15) N3D 0.051(2) 0.0308(19) 0.0233(16) 0.0072(15) 0.0110(16) -0.0078(16) N4D 0.075(3) 0.024(2) 0.0294(19) -0.0021(16) 0.0191(19) -0.0077(18) F1D 0.0344(12) 0.0197(11) 0.0257(11) 0.0111(9) 0.0051(9) -0.0032(9) F2D 0.0372(12) 0.0119(10) 0.0281(11) 0.0068(9) 0.0041(9) 0.0044(9) F3D 0.0363(12) 0.0149(10) 0.0265(11) 0.0080(9) 0.0107(9) -0.0017(8) F4D 0.0367(12) 0.0122(10) 0.0263(11) 0.0056(9) 0.0083(9) 0.0010(8) C1D 0.0205(16) 0.0165(16) 0.0166(16) 0.0059(14) -0.0024(13) -0.0005(13) C2D 0.0248(17) 0.0158(17) 0.0187(16) 0.0076(14) -0.0028(14) -0.0053(13) C3D 0.0235(18) 0.0133(16) 0.0212(16) 0.0056(14) -0.0061(14) 0.0008(13) C4D 0.0204(17) 0.0152(16) 0.0175(16) 0.0021(13) -0.0060(13) -0.0002(13) C5D 0.0200(17) 0.0161(17) 0.0226(17) 0.0088(14) -0.0014(14) -0.0030(13) C6D 0.0252(17) 0.0108(16) 0.0184(16) 0.0019(13) -0.0010(14) -0.0018(13) C7D 0.0187(16) 0.0172(16) 0.0202(16) 0.0046(14) -0.0026(13) 0.0004(13) C8D 0.0245(18) 0.026(2) 0.0231(18) 0.0083(16) 0.0005(14) 0.0019(15) C9D 0.0284(19) 0.0201(18) 0.0173(16) -0.0029(15) -0.0010(14) 0.0038(15) C10D 0.0302(19) 0.0180(17) 0.0148(15) 0.0062(14) -0.0009(14) -0.0017(14) C11D 0.033(2) 0.0238(19) 0.0179(17) 0.0017(15) -0.0019(15) -0.0006(15) C12D 0.036(2) 0.026(2) 0.0184(16) 0.0058(16) 0.0052(15) -0.0023(16) N1E 0.0385(18) 0.0183(16) 0.0229(16) 0.0021(13) 0.0051(14) 0.0051(13) N2E 0.056(2) 0.0288(19) 0.0278(17) 0.0114(16) 0.0105(16) -0.0031(16) N3E 0.0267(16) 0.0357(19) 0.0251(16) 0.0125(15) 0.0022(13) -0.0024(14) N4E 0.043(2) 0.0240(19) 0.041(2) 0.0059(16) 0.0126(17) 0.0100(16) F1E 0.0383(12) 0.0186(11) 0.0342(12) 0.0143(10) 0.0128(10) -0.0020(9) F2E 0.0373(12) 0.0110(10) 0.0319(12) 0.0065(9) 0.0065(9) 0.0032(8) F3E 0.0364(12) 0.0156(10) 0.0270(11) 0.0110(9) 0.0085(9) 0.0045(9) F4E 0.0386(13) 0.0150(10) 0.0310(11) 0.0063(9) 0.0114(10) 0.0062(9) C1E 0.0185(16) 0.0170(17) 0.0187(16) 0.0049(14) -0.0029(13) 0.0001(13) C2E 0.0217(17) 0.0143(16) 0.0286(18) 0.0148(15) -0.0032(14) -0.0031(13) C3E 0.0254(18) 0.0116(16) 0.0208(16) 0.0038(14) -0.0048(14) 0.0007(13) C5E 0.0236(17) 0.0153(16) 0.0168(15) 0.0084(14) -0.0021(13) -0.0014(13) C6E 0.0230(17) 0.0101(15) 0.0265(18) 0.0062(14) 0.0006(14) 0.0042(13) C7E 0.0260(18) 0.0168(17) 0.0156(15) 0.0043(14) -0.0022(13) 0.0003(14) C9E 0.034(2) 0.0165(17) 0.0237(18) 0.0029(16) -0.0009(16) 0.0007(15) C8E 0.0288(19) 0.0224(19) 0.0155(16) 0.0062(15) -0.0016(14) -0.0024(15) C4E 0.0194(16) 0.0146(16) 0.0186(16) 0.0031(13) -0.0052(13) 0.0012(13) C10E 0.0203(17) 0.0211(18) 0.0198(16) 0.0082(14) 0.0008(13) -0.0022(13) C11E 0.0228(18) 0.0270(19) 0.0173(16) 0.0064(15) -0.0006(14) 0.0041(15) C12E 0.0236(18) 0.030(2) 0.0233(18) 0.0112(17) 0.0008(15) 0.0000(15) C1F 0.072(4) 0.053(3) 0.045(3) 0.013(3) -0.002(3) 0.015(3) Cl1F 0.1184(15) 0.0547(10) 0.0770(11) 0.0193(8) -0.0209(10) 0.0039(9) Cl2F 0.0891(11) 0.0564(9) 0.0588(9) 0.0079(7) -0.0118(8) 0.0214(8) Cl1G 0.0799(11) 0.0865(13) 0.0626(9) 0.0271(9) 0.0027(8) 0.0038(9) Cl2G 0.0840(12) 0.0735(11) 0.0878(12) 0.0336(10) -0.0160(9) -0.0232(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.718(4) . ? S1 C2 1.730(4) . ? S2 C5A 1.741(11) . ? S2 C2 1.756(4) . ? S2 C5 1.831(10) . ? S4 C1 1.716(4) . ? S4 C3 1.738(4) . ? S5 C6 1.734(4) . ? S5 C7 1.742(3) . ? S6 C6 1.726(4) . ? S6 C8 1.730(4) . ? O1 C11 1.410(4) . ? O1 C9 1.436(4) . ? O2 C30 1.387(4) . ? O2 C10 1.440(4) . ? C1 C6 1.396(5) . ? C2 C3 1.356(6) . ? C3 S3 1.744(4) . ? C3 S3A 1.852(6) . ? S3 C4 1.890(11) . ? C4 C5 1.296(17) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? S3A C4A 1.796(17) . ? C4A C5A 1.67(2) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C7 C8 1.366(5) . ? C7 C9 1.504(5) . ? C8 C10 1.508(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C20 1.367(5) . ? C11 C12 1.410(5) . ? C12 C13 1.359(6) . ? C12 H12 0.9300 . ? C13 C14 1.418(6) . ? C13 H13 0.9300 . ? C14 C15 1.417(5) . ? C14 C19 1.425(5) . ? C15 C16 1.356(6) . ? C15 H15 0.9300 . ? C16 C17 1.405(6) . ? C16 H16 0.9300 . ? C17 C18 1.377(5) . ? C17 H17 0.9300 . ? C18 C19 1.425(5) . ? C18 H18 0.9300 . ? C19 C20 1.437(5) . ? C20 C21 1.497(5) . ? C21 C30 1.392(5) . ? C21 C22 1.434(5) . ? C22 C23 1.418(6) . ? C22 C27 1.439(6) . ? C23 C24 1.395(6) . ? C23 H23 0.9300 . ? C24 C25 1.404(7) . ? C24 H24 0.9300 . ? C25 C26 1.362(7) . ? C25 H25 0.9300 . ? C26 C27 1.412(5) . ? C26 H26 0.9300 . ? C27 C28 1.422(6) . ? C28 C29 1.380(5) . ? C28 H28 0.9300 . ? C29 C30 1.410(5) . ? C29 H29 0.9300 . ? S1B C1B 1.718(4) . ? S1B C2B 1.742(4) . ? S2B C3B 1.709(13) . ? S2B C2B 1.745(4) . ? S2B C3C 1.846(6) . ? S3B C4C 1.754(7) . ? S3B C5B 1.756(4) . ? S3B C4B 1.901(16) . ? S4B C1B 1.723(4) . ? S4B C5B 1.752(4) . ? S5B C6B 1.718(4) . ? S5B C7B 1.740(3) . ? S6B C6B 1.729(4) . ? S6B C8B 1.734(4) . ? O1B C11B 1.396(4) . ? O1B C9B 1.442(4) . ? O2B C30B 1.386(4) . ? O2B C10B 1.443(4) . ? C1B C6B 1.404(5) . ? C2B C5B 1.365(5) . ? C3B C4B 1.54(2) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C3C C4C 1.532(11) . ? C3C H3C1 0.9700 . ? C3C H3C2 0.9700 . ? C4C H4C1 0.9700 . ? C4C H4C2 0.9700 . ? C7B C8B 1.359(5) . ? C7B C9B 1.532(5) . ? C8B C10B 1.505(5) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B C20B 1.387(5) . ? C11B C12B 1.425(5) . ? C12B C13B 1.367(5) . ? C12B H12B 0.9300 . ? C13B C14B 1.421(6) . ? C13B H13B 0.9300 . ? C14B C19B 1.431(5) . ? C14B C15B 1.434(5) . ? C15B C16B 1.348(7) . ? C15B H15B 0.9300 . ? C16B C17B 1.413(7) . ? C16B H16B 0.9300 . ? C17B C18B 1.380(6) . ? C17B H17B 0.9300 . ? C18B C19B 1.424(5) . ? C18B H18B 0.9300 . ? C19B C20B 1.425(5) . ? C20B C21B 1.499(4) . ? C21B C30B 1.371(5) . ? C21B C22B 1.437(4) . ? C22B C23B 1.425(5) . ? C22B C27B 1.427(5) . ? C23B C24B 1.370(5) . ? C23B H23B 0.9300 . ? C24B C25B 1.415(6) . ? C24B H24B 0.9300 . ? C25B C26B 1.355(6) . ? C25B H25B 0.9300 . ? C26B C27B 1.426(5) . ? C26B H26B 0.9300 . ? C27B C28B 1.414(5) . ? C28B C29B 1.369(5) . ? C28B H28B 0.9300 . ? C29B C30B 1.420(5) . ? C29B H29B 0.9300 . ? N1D C8D 1.149(5) . ? N2D C9D 1.157(5) . ? N3D C11D 1.142(5) . ? N4D C12D 1.153(5) . ? F1D C2D 1.340(4) . ? F2D C3D 1.359(4) . ? F3D C5D 1.340(4) . ? F4D C6D 1.348(4) . ? C1D C6D 1.417(5) . ? C1D C10D 1.421(5) . ? C1D C2D 1.429(5) . ? C2D C3D 1.372(5) . ? C3D C4D 1.412(5) . ? C4D C7D 1.424(5) . ? C4D C5D 1.428(5) . ? C5D C6D 1.367(5) . ? C7D C8D 1.424(5) . ? C7D C9D 1.424(5) . ? C10D C12D 1.419(5) . ? C10D C11D 1.433(5) . ? N1E C8E 1.156(5) . ? N2E C9E 1.148(5) . ? N3E C11E 1.158(5) . ? N4E C12E 1.155(5) . ? F1E C2E 1.351(4) . ? F2E C3E 1.352(4) . ? F3E C5E 1.347(4) . ? F4E C6E 1.341(4) . ? C1E C10E 1.407(5) . ? C1E C2E 1.423(5) . ? C1E C6E 1.425(5) . ? C2E C3E 1.364(5) . ? C3E C4E 1.416(5) . ? C5E C6E 1.359(5) . ? C5E C4E 1.427(5) . ? C7E C8E 1.419(5) . ? C7E C4E 1.420(5) . ? C7E C9E 1.434(5) . ? C10E C11E 1.425(5) . ? C10E C12E 1.429(5) . ? C1F Cl1F 1.755(6) . ? C1F Cl2F 1.768(6) . ? C1F H1F1 0.9700 . ? C1F H1F2 0.9700 . ? C1G Cl2G 1.734(8) . ? C1G Cl1G 1.736(8) . ? C1G H1G1 0.9700 . ? C1G H1G2 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 95.43(18) . . ? C5A S2 C2 96.9(4) . . ? C2 S2 C5 101.4(3) . . ? C1 S4 C3 95.4(2) . . ? C6 S5 C7 95.34(17) . . ? C6 S6 C8 96.06(17) . . ? C11 O1 C9 112.9(3) . . ? C30 O2 C10 118.5(3) . . ? C6 C1 S4 122.5(3) . . ? C6 C1 S1 121.8(3) . . ? S4 C1 S1 115.7(2) . . ? C3 C2 S1 116.9(3) . . ? C3 C2 S2 127.1(3) . . ? S1 C2 S2 116.1(2) . . ? C2 C3 S4 116.2(3) . . ? C2 C3 S3 126.7(3) . . ? S4 C3 S3 116.1(3) . . ? C2 C3 S3A 127.0(3) . . ? S4 C3 S3A 112.9(3) . . ? C3 S3 C4 97.6(4) . . ? C5 C4 S3 113.0(10) . . ? C5 C4 H4A 109.0 . . ? S3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? S3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 S2 124.5(8) . . ? C4 C5 H5A 106.2 . . ? S2 C5 H5A 106.2 . . ? C4 C5 H5B 106.2 . . ? S2 C5 H5B 106.2 . . ? H5A C5 H5B 106.4 . . ? C4A S3A C3 93.8(6) . . ? C5A C4A S3A 100.9(10) . . ? C5A C4A H4A1 111.6 . . ? S3A C4A H4A1 111.6 . . ? C5A C4A H4A2 111.6 . . ? S3A C4A H4A2 111.6 . . ? H4A1 C4A H4A2 109.4 . . ? C4A C5A S2 108.9(9) . . ? C4A C5A H5A1 109.9 . . ? S2 C5A H5A1 109.9 . . ? C4A C5A H5A2 109.9 . . ? S2 C5A H5A2 109.9 . . ? H5A1 C5A H5A2 108.3 . . ? C1 C6 S6 121.2(3) . . ? C1 C6 S5 123.5(3) . . ? S6 C6 S5 115.2(2) . . ? C8 C7 C9 124.9(3) . . ? C8 C7 S5 116.7(3) . . ? C9 C7 S5 118.1(3) . . ? C7 C8 C10 126.1(3) . . ? C7 C8 S6 116.5(3) . . ? C10 C8 S6 117.4(3) . . ? O1 C9 C7 107.0(3) . . ? O1 C9 H9A 110.3 . . ? C7 C9 H9A 110.3 . . ? O1 C9 H9B 110.3 . . ? C7 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? O2 C10 C8 111.9(3) . . ? O2 C10 H10A 109.2 . . ? C8 C10 H10A 109.2 . . ? O2 C10 H10B 109.2 . . ? C8 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C20 C11 C12 123.0(3) . . ? C20 C11 O1 118.1(3) . . ? C12 C11 O1 118.9(3) . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.7(4) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 121.9(4) . . ? C15 C14 C19 118.7(4) . . ? C13 C14 C19 119.5(3) . . ? C16 C15 C14 121.7(4) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 120.2(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.7(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C14 C19 C18 118.4(3) . . ? C14 C19 C20 119.2(3) . . ? C18 C19 C20 122.3(3) . . ? C11 C20 C19 118.1(3) . . ? C11 C20 C21 120.4(3) . . ? C19 C20 C21 121.5(3) . . ? C30 C21 C22 118.7(3) . . ? C30 C21 C20 120.2(3) . . ? C22 C21 C20 121.1(3) . . ? C23 C22 C21 121.8(4) . . ? C23 C22 C27 118.6(3) . . ? C21 C22 C27 119.7(3) . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 121.0(4) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 119.9(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 121.6(4) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C26 C27 C28 122.1(4) . . ? C26 C27 C22 119.0(4) . . ? C28 C27 C22 118.9(3) . . ? C29 C28 C27 120.8(3) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? O2 C30 C21 115.8(3) . . ? O2 C30 C29 122.3(3) . . ? C21 C30 C29 121.8(3) . . ? C1B S1B C2B 95.70(17) . . ? C3B S2B C2B 100.3(5) . . ? C2B S2B C3C 101.8(2) . . ? C4C S3B C5B 99.5(3) . . ? C5B S3B C4B 99.9(5) . . ? C1B S4B C5B 95.69(17) . . ? C6B S5B C7B 95.79(17) . . ? C6B S6B C8B 95.27(17) . . ? C11B O1B C9B 118.7(3) . . ? C30B O2B C10B 112.6(3) . . ? C6B C1B S1B 120.5(3) . . ? C6B C1B S4B 123.6(3) . . ? S1B C1B S4B 115.9(2) . . ? C5B C2B S1B 116.8(3) . . ? C5B C2B S2B 130.5(3) . . ? S1B C2B S2B 112.7(2) . . ? C4B C3B S2B 110.4(13) . . ? C4B C3B H3B1 109.6 . . ? S2B C3B H3B1 109.6 . . ? C4B C3B H3B2 109.6 . . ? S2B C3B H3B2 109.6 . . ? H3B1 C3B H3B2 108.1 . . ? C3B C4B S3B 120.2(13) . . ? C3B C4B H4B1 107.3 . . ? S3B C4B H4B1 107.3 . . ? C3B C4B H4B2 107.3 . . ? S3B C4B H4B2 107.3 . . ? H4B1 C4B H4B2 106.9 . . ? C4C C3C S2B 114.1(5) . . ? C4C C3C H3C1 108.7 . . ? S2B C3C H3C1 108.7 . . ? C4C C3C H3C2 108.7 . . ? S2B C3C H3C2 108.7 . . ? H3C1 C3C H3C2 107.6 . . ? C3C C4C S3B 115.2(6) . . ? C3C C4C H4C1 108.5 . . ? S3B C4C H4C1 108.5 . . ? C3C C4C H4C2 108.5 . . ? S3B C4C H4C2 108.5 . . ? H4C1 C4C H4C2 107.5 . . ? C2B C5B S4B 115.9(3) . . ? C2B C5B S3B 126.3(3) . . ? S4B C5B S3B 117.8(2) . . ? C1B C6B S5B 124.3(3) . . ? C1B C6B S6B 120.1(3) . . ? S5B C6B S6B 115.6(2) . . ? C8B C7B C9B 125.8(3) . . ? C8B C7B S5B 116.1(3) . . ? C9B C7B S5B 118.2(3) . . ? C7B C8B C10B 125.8(3) . . ? C7B C8B S6B 117.2(3) . . ? C10B C8B S6B 116.6(3) . . ? O1B C9B C7B 111.2(3) . . ? O1B C9B H9B1 109.4 . . ? C7B C9B H9B1 109.4 . . ? O1B C9B H9B2 109.4 . . ? C7B C9B H9B2 109.4 . . ? H9B1 C9B H9B2 108.0 . . ? O2B C10B C8B 105.5(3) . . ? O2B C10B H10C 110.6 . . ? C8B C10B H10C 110.6 . . ? O2B C10B H10D 110.6 . . ? C8B C10B H10D 110.6 . . ? H10C C10B H10D 108.8 . . ? C20B C11B O1B 117.1(3) . . ? C20B C11B C12B 121.7(3) . . ? O1B C11B C12B 121.0(3) . . ? C13B C12B C11B 119.5(3) . . ? C13B C12B H12B 120.3 . . ? C11B C12B H12B 120.3 . . ? C12B C13B C14B 121.1(3) . . ? C12B C13B H13B 119.5 . . ? C14B C13B H13B 119.5 . . ? C13B C14B C19B 119.0(3) . . ? C13B C14B C15B 122.3(4) . . ? C19B C14B C15B 118.6(4) . . ? C16B C15B C14B 121.6(4) . . ? C16B C15B H15B 119.2 . . ? C14B C15B H15B 119.2 . . ? C15B C16B C17B 119.8(4) . . ? C15B C16B H16B 120.1 . . ? C17B C16B H16B 120.1 . . ? C18B C17B C16B 121.4(4) . . ? C18B C17B H17B 119.3 . . ? C16B C17B H17B 119.3 . . ? C17B C18B C19B 120.0(4) . . ? C17B C18B H18B 120.0 . . ? C19B C18B H18B 120.0 . . ? C18B C19B C20B 121.5(3) . . ? C18B C19B C14B 118.7(3) . . ? C20B C19B C14B 119.8(3) . . ? C11B C20B C19B 118.6(3) . . ? C11B C20B C21B 121.5(3) . . ? C19B C20B C21B 119.9(3) . . ? C30B C21B C22B 118.2(3) . . ? C30B C21B C20B 122.0(3) . . ? C22B C21B C20B 119.9(3) . . ? C23B C22B C27B 118.1(3) . . ? C23B C22B C21B 122.2(3) . . ? C27B C22B C21B 119.7(3) . . ? C24B C23B C22B 120.9(3) . . ? C24B C23B H23B 119.6 . . ? C22B C23B H23B 119.6 . . ? C23B C24B C25B 120.8(4) . . ? C23B C24B H24B 119.6 . . ? C25B C24B H24B 119.6 . . ? C26B C25B C24B 119.7(3) . . ? C26B C25B H25B 120.2 . . ? C24B C25B H25B 120.2 . . ? C25B C26B C27B 121.6(4) . . ? C25B C26B H26B 119.2 . . ? C27B C26B H26B 119.2 . . ? C28B C27B C26B 121.8(3) . . ? C28B C27B C22B 119.3(3) . . ? C26B C27B C22B 118.9(3) . . ? C29B C28B C27B 120.8(3) . . ? C29B C28B H28B 119.6 . . ? C27B C28B H28B 119.6 . . ? C28B C29B C30B 119.4(3) . . ? C28B C29B H29B 120.3 . . ? C30B C29B H29B 120.3 . . ? C21B C30B O2B 119.2(3) . . ? C21B C30B C29B 122.5(3) . . ? O2B C30B C29B 118.3(3) . . ? C6D C1D C10D 123.9(3) . . ? C6D C1D C2D 112.9(3) . . ? C10D C1D C2D 123.2(3) . . ? F1D C2D C3D 118.5(3) . . ? F1D C2D C1D 119.1(3) . . ? C3D C2D C1D 122.4(3) . . ? F2D C3D C2D 116.7(3) . . ? F2D C3D C4D 118.3(3) . . ? C2D C3D C4D 125.0(3) . . ? C3D C4D C7D 124.8(3) . . ? C3D C4D C5D 112.1(3) . . ? C7D C4D C5D 123.2(3) . . ? F3D C5D C6D 117.7(3) . . ? F3D C5D C4D 118.7(3) . . ? C6D C5D C4D 123.5(3) . . ? F4D C6D C5D 116.8(3) . . ? F4D C6D C1D 119.2(3) . . ? C5D C6D C1D 124.1(3) . . ? C8D C7D C4D 122.7(3) . . ? C8D C7D C9D 113.5(3) . . ? C4D C7D C9D 123.8(3) . . ? N1D C8D C7D 176.4(4) . . ? N2D C9D C7D 174.7(4) . . ? C12D C10D C1D 121.4(3) . . ? C12D C10D C11D 114.4(3) . . ? C1D C10D C11D 124.0(3) . . ? N3D C11D C10D 175.3(4) . . ? N4D C12D C10D 177.6(5) . . ? C10E C1E C2E 123.9(3) . . ? C10E C1E C6E 123.7(3) . . ? C2E C1E C6E 112.5(3) . . ? F1E C2E C3E 118.0(3) . . ? F1E C2E C1E 118.2(3) . . ? C3E C2E C1E 123.7(3) . . ? F2E C3E C2E 117.7(3) . . ? F2E C3E C4E 118.8(3) . . ? C2E C3E C4E 123.6(3) . . ? F3E C5E C6E 118.4(3) . . ? F3E C5E C4E 118.4(3) . . ? C6E C5E C4E 123.2(3) . . ? F4E C6E C5E 117.5(3) . . ? F4E C6E C1E 118.5(3) . . ? C5E C6E C1E 124.0(3) . . ? C8E C7E C4E 124.1(3) . . ? C8E C7E C9E 112.5(3) . . ? C4E C7E C9E 123.3(3) . . ? N2E C9E C7E 175.4(4) . . ? N1E C8E C7E 174.6(4) . . ? C3E C4E C7E 123.8(3) . . ? C3E C4E C5E 113.1(3) . . ? C7E C4E C5E 123.2(3) . . ? C1E C10E C11E 123.9(3) . . ? C1E C10E C12E 123.7(3) . . ? C11E C10E C12E 112.3(3) . . ? N3E C11E C10E 173.7(4) . . ? N4E C12E C10E 174.7(4) . . ? Cl1F C1F Cl2F 111.0(3) . . ? Cl1F C1F H1F1 109.4 . . ? Cl2F C1F H1F1 109.4 . . ? Cl1F C1F H1F2 109.4 . . ? Cl2F C1F H1F2 109.4 . . ? H1F1 C1F H1F2 108.0 . . ? Cl2G C1G Cl1G 114.3(4) . . ? Cl2G C1G H1G1 108.7 . . ? Cl1G C1G H1G1 108.7 . . ? Cl2G C1G H1G2 108.7 . . ? Cl1G C1G H1G2 108.7 . . ? H1G1 C1G H1G2 107.6 . . ? 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 C3 S4 C1 C6 -172.5(3) . . . . ? C3 S4 C1 S1 6.2(3) . . . . ? C2 S1 C1 C6 174.0(3) . . . . ? C2 S1 C1 S4 -4.7(3) . . . . ? C1 S1 C2 C3 0.6(4) . . . . ? C1 S1 C2 S2 -179.9(3) . . . . ? C5A S2 C2 C3 26.1(7) . . . . ? C5 S2 C2 C3 -2.0(7) . . . . ? C5A S2 C2 S1 -153.3(6) . . . . ? C5 S2 C2 S1 178.6(5) . . . . ? S1 C2 C3 S4 3.6(6) . . . . ? S2 C2 C3 S4 -175.8(3) . . . . ? S1 C2 C3 S3 -164.5(4) . . . . ? S2 C2 C3 S3 16.1(8) . . . . ? S1 C2 C3 S3A 159.5(4) . . . . ? S2 C2 C3 S3A -19.9(8) . . . . ? C1 S4 C3 C2 -5.8(5) . . . . ? C1 S4 C3 S3 163.6(3) . . . . ? C1 S4 C3 S3A -165.1(3) . . . . ? C2 C3 S3 C4 -37.8(8) . . . . ? S4 C3 S3 C4 154.2(6) . . . . ? S3A C3 S3 C4 63.8(6) . . . . ? C3 S3 C4 C5 57.8(12) . . . . ? S3 C4 C5 S2 -59.8(17) . . . . ? C5A S2 C5 C4 -55.1(14) . . . . ? C2 S2 C5 C4 28.3(14) . . . . ? C2 C3 S3A C4A 37.6(8) . . . . ? S4 C3 S3A C4A -165.8(6) . . . . ? S3 C3 S3A C4A -62.9(6) . . . . ? C3 S3A C4A C5A -65.1(9) . . . . ? S3A C4A C5A S2 92.6(11) . . . . ? C2 S2 C5A C4A -60.9(10) . . . . ? C5 S2 C5A C4A 40.2(10) . . . . ? S4 C1 C6 S6 178.6(2) . . . . ? S1 C1 C6 S6 0.0(4) . . . . ? S4 C1 C6 S5 2.3(4) . . . . ? S1 C1 C6 S5 -176.3(2) . . . . ? C8 S6 C6 C1 -172.8(3) . . . . ? C8 S6 C6 S5 3.8(2) . . . . ? C7 S5 C6 C1 172.7(3) . . . . ? C7 S5 C6 S6 -3.8(2) . . . . ? C6 S5 C7 C8 2.3(3) . . . . ? C6 S5 C7 C9 -172.6(3) . . . . ? C9 C7 C8 C10 -5.4(5) . . . . ? S5 C7 C8 C10 -179.9(3) . . . . ? C9 C7 C8 S6 174.5(3) . . . . ? S5 C7 C8 S6 0.0(4) . . . . ? C6 S6 C8 C7 -2.2(3) . . . . ? C6 S6 C8 C10 177.6(3) . . . . ? C11 O1 C9 C7 143.8(3) . . . . ? C8 C7 C9 O1 -83.6(4) . . . . ? S5 C7 C9 O1 90.9(3) . . . . ? C30 O2 C10 C8 68.7(4) . . . . ? C7 C8 C10 O2 45.9(5) . . . . ? S6 C8 C10 O2 -134.0(3) . . . . ? C9 O1 C11 C20 -120.7(3) . . . . ? C9 O1 C11 C12 61.5(4) . . . . ? C20 C11 C12 C13 3.1(6) . . . . ? O1 C11 C12 C13 -179.3(3) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? C12 C13 C14 C15 175.8(4) . . . . ? C12 C13 C14 C19 -2.6(6) . . . . ? C13 C14 C15 C16 -178.2(4) . . . . ? C19 C14 C15 C16 0.2(6) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C15 C16 C17 C18 1.4(6) . . . . ? C16 C17 C18 C19 -0.9(6) . . . . ? C15 C14 C19 C18 0.4(5) . . . . ? C13 C14 C19 C18 178.8(3) . . . . ? C15 C14 C19 C20 -176.2(3) . . . . ? C13 C14 C19 C20 2.2(5) . . . . ? C17 C18 C19 C14 -0.1(5) . . . . ? C17 C18 C19 C20 176.4(3) . . . . ? C12 C11 C20 C19 -3.4(5) . . . . ? O1 C11 C20 C19 179.0(3) . . . . ? C12 C11 C20 C21 178.5(3) . . . . ? O1 C11 C20 C21 0.9(5) . . . . ? C14 C19 C20 C11 0.6(5) . . . . ? C18 C19 C20 C11 -175.8(3) . . . . ? C14 C19 C20 C21 178.8(3) . . . . ? C18 C19 C20 C21 2.3(5) . . . . ? C11 C20 C21 C30 64.3(4) . . . . ? C19 C20 C21 C30 -113.8(4) . . . . ? C11 C20 C21 C22 -116.2(4) . . . . ? C19 C20 C21 C22 65.7(4) . . . . ? C30 C21 C22 C23 -176.9(3) . . . . ? C20 C21 C22 C23 3.6(5) . . . . ? C30 C21 C22 C27 2.0(5) . . . . ? C20 C21 C22 C27 -177.5(3) . . . . ? C21 C22 C23 C24 179.3(4) . . . . ? C27 C22 C23 C24 0.3(6) . . . . ? C22 C23 C24 C25 1.4(7) . . . . ? C23 C24 C25 C26 -1.3(7) . . . . ? C24 C25 C26 C27 -0.5(7) . . . . ? C25 C26 C27 C28 -176.9(4) . . . . ? C25 C26 C27 C22 2.3(6) . . . . ? C23 C22 C27 C26 -2.1(5) . . . . ? C21 C22 C27 C26 178.9(4) . . . . ? C23 C22 C27 C28 177.0(3) . . . . ? C21 C22 C27 C28 -1.9(5) . . . . ? C26 C27 C28 C29 178.8(4) . . . . ? C22 C27 C28 C29 -0.3(5) . . . . ? C27 C28 C29 C30 2.4(5) . . . . ? C10 O2 C30 C21 -153.1(3) . . . . ? C10 O2 C30 C29 30.1(4) . . . . ? C22 C21 C30 O2 -176.8(3) . . . . ? C20 C21 C30 O2 2.7(5) . . . . ? C22 C21 C30 C29 0.1(5) . . . . ? C20 C21 C30 C29 179.6(3) . . . . ? C28 C29 C30 O2 174.4(3) . . . . ? C28 C29 C30 C21 -2.3(5) . . . . ? C2B S1B C1B C6B 178.0(3) . . . . ? C2B S1B C1B S4B -1.9(2) . . . . ? C5B S4B C1B C6B -179.3(3) . . . . ? C5B S4B C1B S1B 0.5(2) . . . . ? C1B S1B C2B C5B 3.0(3) . . . . ? C1B S1B C2B S2B -175.6(2) . . . . ? C3B S2B C2B C5B 33.5(8) . . . . ? C3C S2B C2B C5B 2.8(5) . . . . ? C3B S2B C2B S1B -148.2(7) . . . . ? C3C S2B C2B S1B -178.9(3) . . . . ? C2B S2B C3B C4B -58.2(15) . . . . ? C3C S2B C3B C4B 37.5(12) . . . . ? S2B C3B C4B S3B 65(2) . . . . ? C4C S3B C4B C3B 60.9(19) . . . . ? C5B S3B C4B C3B -29.8(19) . . . . ? C3B S2B C3C C4C -58.2(11) . . . . ? C2B S2B C3C C4C 32.1(7) . . . . ? S2B C3C C4C S3B -68.0(9) . . . . ? C5B S3B C4C C3C 58.1(7) . . . . ? C4B S3B C4C C3C -34.9(15) . . . . ? S1B C2B C5B S4B -3.2(4) . . . . ? S2B C2B C5B S4B 175.1(2) . . . . ? S1B C2B C5B S3B 176.8(2) . . . . ? S2B C2B C5B S3B -4.9(5) . . . . ? C1B S4B C5B C2B 1.6(3) . . . . ? C1B S4B C5B S3B -178.4(2) . . . . ? C4C S3B C5B C2B -22.1(5) . . . . ? C4B S3B C5B C2B -1.1(9) . . . . ? C4C S3B C5B S4B 157.9(4) . . . . ? C4B S3B C5B S4B 178.9(8) . . . . ? S1B C1B C6B S5B 179.5(2) . . . . ? S4B C1B C6B S5B -0.7(4) . . . . ? S1B C1B C6B S6B 2.3(4) . . . . ? S4B C1B C6B S6B -177.9(2) . . . . ? C7B S5B C6B C1B -173.9(3) . . . . ? C7B S5B C6B S6B 3.5(2) . . . . ? C8B S6B C6B C1B 173.9(3) . . . . ? C8B S6B C6B S5B -3.5(2) . . . . ? C6B S5B C7B C8B -2.0(3) . . . . ? C6B S5B C7B C9B 178.3(3) . . . . ? C9B C7B C8B C10B -8.0(6) . . . . ? S5B C7B C8B C10B 172.3(3) . . . . ? C9B C7B C8B S6B 179.6(3) . . . . ? S5B C7B C8B S6B -0.1(4) . . . . ? C6B S6B C8B C7B 2.2(3) . . . . ? C6B S6B C8B C10B -171.0(3) . . . . ? C11B O1B C9B C7B 73.7(4) . . . . ? C8B C7B C9B O1B 45.3(5) . . . . ? S5B C7B C9B O1B -135.0(3) . . . . ? C30B O2B C10B C8B 146.1(3) . . . . ? C7B C8B C10B O2B -86.5(4) . . . . ? S6B C8B C10B O2B 86.0(3) . . . . ? C9B O1B C11B C20B -147.7(3) . . . . ? C9B O1B C11B C12B 37.0(4) . . . . ? C20B C11B C12B C13B 0.9(5) . . . . ? O1B C11B C12B C13B 176.0(3) . . . . ? C11B C12B C13B C14B 3.1(5) . . . . ? C12B C13B C14B C19B -2.2(5) . . . . ? C12B C13B C14B C15B 174.2(4) . . . . ? C13B C14B C15B C16B -175.1(4) . . . . ? C19B C14B C15B C16B 1.4(6) . . . . ? C14B C15B C16B C17B -1.3(7) . . . . ? C15B C16B C17B C18B 0.5(7) . . . . ? C16B C17B C18B C19B 0.2(6) . . . . ? C17B C18B C19B C20B 178.4(4) . . . . ? C17B C18B C19B C14B -0.1(6) . . . . ? C13B C14B C19B C18B 175.9(3) . . . . ? C15B C14B C19B C18B -0.7(5) . . . . ? C13B C14B C19B C20B -2.6(5) . . . . ? C15B C14B C19B C20B -179.2(3) . . . . ? O1B C11B C20B C19B 179.1(3) . . . . ? C12B C11B C20B C19B -5.7(5) . . . . ? O1B C11B C20B C21B -2.6(5) . . . . ? C12B C11B C20B C21B 172.6(3) . . . . ? C18B C19B C20B C11B -172.1(3) . . . . ? C14B C19B C20B C11B 6.4(5) . . . . ? C18B C19B C20B C21B 9.7(5) . . . . ? C14B C19B C20B C21B -171.9(3) . . . . ? C11B C20B C21B C30B 68.8(5) . . . . ? C19B C20B C21B C30B -113.0(4) . . . . ? C11B C20B C21B C22B -112.0(4) . . . . ? C19B C20B C21B C22B 66.3(4) . . . . ? C30B C21B C22B C23B -178.1(3) . . . . ? C20B C21B C22B C23B 2.6(5) . . . . ? C30B C21B C22B C27B 0.4(5) . . . . ? C20B C21B C22B C27B -178.9(3) . . . . ? C27B C22B C23B C24B -0.2(5) . . . . ? C21B C22B C23B C24B 178.3(3) . . . . ? C22B C23B C24B C25B -0.9(6) . . . . ? C23B C24B C25B C26B 1.4(6) . . . . ? C24B C25B C26B C27B -0.7(6) . . . . ? C25B C26B C27B C28B -179.8(4) . . . . ? C25B C26B C27B C22B -0.4(6) . . . . ? C23B C22B C27B C28B -179.8(3) . . . . ? C21B C22B C27B C28B 1.7(5) . . . . ? C23B C22B C27B C26B 0.9(5) . . . . ? C21B C22B C27B C26B -177.7(3) . . . . ? C26B C27B C28B C29B 177.2(4) . . . . ? C22B C27B C28B C29B -2.1(6) . . . . ? C27B C28B C29B C30B 0.4(6) . . . . ? C22B C21B C30B O2B 178.1(3) . . . . ? C20B C21B C30B O2B -2.6(5) . . . . ? C22B C21B C30B C29B -2.1(5) . . . . ? C20B C21B C30B C29B 177.2(3) . . . . ? C10B O2B C30B C21B -113.4(4) . . . . ? C10B O2B C30B C29B 66.8(4) . . . . ? C28B C29B C30B C21B 1.8(6) . . . . ? C28B C29B C30B O2B -178.4(3) . . . . ? C6D C1D C2D F1D 179.3(3) . . . . ? C10D C1D C2D F1D 2.1(5) . . . . ? C6D C1D C2D C3D 2.2(5) . . . . ? C10D C1D C2D C3D -175.0(3) . . . . ? F1D C2D C3D F2D 0.0(5) . . . . ? C1D C2D C3D F2D 177.1(3) . . . . ? F1D C2D C3D C4D -178.4(3) . . . . ? C1D C2D C3D C4D -1.3(5) . . . . ? F2D C3D C4D C7D 0.2(5) . . . . ? C2D C3D C4D C7D 178.5(3) . . . . ? F2D C3D C4D C5D -178.8(3) . . . . ? C2D C3D C4D C5D -0.5(5) . . . . ? C3D C4D C5D F3D 179.6(3) . . . . ? C7D C4D C5D F3D 0.6(5) . . . . ? C3D C4D C5D C6D 1.2(5) . . . . ? C7D C4D C5D C6D -177.8(3) . . . . ? F3D C5D C6D F4D 2.9(5) . . . . ? C4D C5D C6D F4D -178.7(3) . . . . ? F3D C5D C6D C1D -178.6(3) . . . . ? C4D C5D C6D C1D -0.2(5) . . . . ? C10D C1D C6D F4D -6.0(5) . . . . ? C2D C1D C6D F4D 176.9(3) . . . . ? C10D C1D C6D C5D 175.6(3) . . . . ? C2D C1D C6D C5D -1.5(5) . . . . ? C3D C4D C7D C8D 1.3(5) . . . . ? C5D C4D C7D C8D -179.8(3) . . . . ? C3D C4D C7D C9D -177.0(3) . . . . ? C5D C4D C7D C9D 1.9(5) . . . . ? C6D C1D C10D C12D -10.8(5) . . . . ? C2D C1D C10D C12D 166.0(3) . . . . ? C6D C1D C10D C11D 174.2(3) . . . . ? C2D C1D C10D C11D -8.9(5) . . . . ? C10E C1E C2E F1E -0.6(5) . . . . ? C6E C1E C2E F1E -179.8(3) . . . . ? C10E C1E C2E C3E 178.0(3) . . . . ? C6E C1E C2E C3E -1.2(5) . . . . ? F1E C2E C3E F2E -1.4(5) . . . . ? C1E C2E C3E F2E -179.9(3) . . . . ? F1E C2E C3E C4E 179.0(3) . . . . ? C1E C2E C3E C4E 0.4(5) . . . . ? F3E C5E C6E F4E 2.0(5) . . . . ? C4E C5E C6E F4E -179.2(3) . . . . ? F3E C5E C6E C1E 179.2(3) . . . . ? C4E C5E C6E C1E -2.0(5) . . . . ? C10E C1E C6E F4E -0.1(5) . . . . ? C2E C1E C6E F4E 179.1(3) . . . . ? C10E C1E C6E C5E -177.2(3) . . . . ? C2E C1E C6E C5E 2.0(5) . . . . ? F2E C3E C4E C7E 0.8(5) . . . . ? C2E C3E C4E C7E -179.5(3) . . . . ? F2E C3E C4E C5E -179.8(3) . . . . ? C2E C3E C4E C5E -0.2(5) . . . . ? C8E C7E C4E C3E -0.9(5) . . . . ? C9E C7E C4E C3E 178.7(3) . . . . ? C8E C7E C4E C5E 179.8(3) . . . . ? C9E C7E C4E C5E -0.6(5) . . . . ? F3E C5E C4E C3E 179.7(3) . . . . ? C6E C5E C4E C3E 0.9(5) . . . . ? F3E C5E C4E C7E -0.9(5) . . . . ? C6E C5E C4E C7E -179.7(3) . . . . ? C2E C1E C10E C11E -2.7(5) . . . . ? C6E C1E C10E C11E 176.4(3) . . . . ? C2E C1E C10E C12E -178.5(3) . . . . ? C6E C1E C10E C12E 0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.746 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.140 # Attachment '-rac--1.cif' data_-rac--1 _database_code_depnum_ccdc_archive 'CCDC 809762' #TrackingRef '-rac--1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 O2 S6' _chemical_formula_sum 'C30 H20 O2 S6' _chemical_formula_weight 604.82 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' 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 16.0832(6) _cell_length_b 9.0468(3) _cell_length_c 18.4128(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.842(2) _cell_angle_gamma 90.00 _cell_volume 2639.66(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4139 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.23 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.936 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.772882 #-------------------------------------------------------------------# _diffrn_ambient_temperature 150(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 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14697 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5944 _reflns_number_gt 4398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0695P)^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 5944 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 S1 S 1.16817(5) 0.65024(7) 0.46896(4) 0.02677(18) Uani 1 1 d . . . S2 S 1.29628(6) 0.48207(10) 0.56980(5) 0.0483(3) Uani 1 1 d . . . S3 S 1.14348(5) 0.46817(9) 0.68428(4) 0.0360(2) Uani 1 1 d . . . S4 S 1.03767(4) 0.63517(7) 0.56479(4) 0.02399(17) Uani 1 1 d . . . S5 S 0.91404(4) 0.83713(7) 0.46070(4) 0.02656(18) Uani 1 1 d . . . S6 S 1.03298(4) 0.87067(7) 0.35569(3) 0.02260(17) Uani 1 1 d . . . O1 O 0.74441(12) 0.96667(18) 0.34018(10) 0.0248(4) Uani 1 1 d . . . O2 O 0.84801(11) 1.09033(17) 0.23786(9) 0.0209(4) Uani 1 1 d . . . C1 C 1.06719(17) 0.7049(3) 0.48362(13) 0.0222(6) Uani 1 1 d . . . C2 C 1.19358(19) 0.5541(3) 0.55308(15) 0.0285(6) Uani 1 1 d . . . C3 C 1.3069(2) 0.4152(3) 0.66364(17) 0.0402(8) Uani 1 1 d . . . H3A H 1.2906 0.3118 0.6623 0.048 Uiso 1 1 calc R . . H3B H 1.3659 0.4208 0.6862 0.048 Uiso 1 1 calc R . . C4 C 1.25522(19) 0.4977(3) 0.71194(16) 0.0343(7) Uani 1 1 d . . . H4A H 1.2671 0.6026 0.7098 0.041 Uiso 1 1 calc R . . H4B H 1.2720 0.4657 0.7626 0.041 Uiso 1 1 calc R . . C5 C 1.13395(18) 0.5471(3) 0.59616(14) 0.0269(6) Uani 1 1 d . . . C6 C 1.01364(17) 0.7920(3) 0.43885(14) 0.0220(6) Uani 1 1 d . . . C7 C 0.89027(17) 0.9709(3) 0.39174(14) 0.0227(6) Uani 1 1 d . . . C8 C 0.94363(16) 0.9865(3) 0.34382(13) 0.0204(5) Uani 1 1 d . . . C9 C 0.80818(17) 1.0503(3) 0.38790(14) 0.0256(6) Uani 1 1 d . . . H9A H 0.7936 1.0584 0.4367 0.031 Uiso 1 1 calc R . . H9B H 0.8123 1.1491 0.3684 0.031 Uiso 1 1 calc R . . C10 C 0.93182(16) 1.0950(3) 0.28034(13) 0.0217(5) Uani 1 1 d . . . H10A H 0.9433 1.1941 0.2996 0.026 Uiso 1 1 calc R . . H10B H 0.9723 1.0730 0.2484 0.026 Uiso 1 1 calc R . . C11 C 0.68575(16) 1.0510(3) 0.29416(15) 0.0234(6) Uani 1 1 d . . . C12 C 0.63483(18) 1.1527(3) 0.32567(16) 0.0315(7) Uani 1 1 d . . . H12 H 0.6430 1.1661 0.3765 0.038 Uiso 1 1 calc R . . C13 C 0.57422(18) 1.2303(3) 0.28111(17) 0.0352(7) Uani 1 1 d . . . H13 H 0.5413 1.2975 0.3018 0.042 Uiso 1 1 calc R . . C14 C 0.56025(17) 1.2107(3) 0.20349(17) 0.0298(7) Uani 1 1 d . . . C15 C 0.49465(18) 1.2861(3) 0.1560(2) 0.0398(8) Uani 1 1 d . . . H15 H 0.4603 1.3515 0.1763 0.048 Uiso 1 1 calc R . . C16 C 0.48105(18) 1.2650(3) 0.0819(2) 0.0399(8) Uani 1 1 d . . . H16 H 0.4368 1.3133 0.0521 0.048 Uiso 1 1 calc R . . C17 C 0.53416(19) 1.1697(3) 0.05014(17) 0.0364(7) Uani 1 1 d . . . H17 H 0.5253 1.1565 -0.0007 0.044 Uiso 1 1 calc R . . C18 C 0.59898(17) 1.0960(3) 0.09368(15) 0.0271(6) Uani 1 1 d . . . H18 H 0.6344 1.0356 0.0718 0.032 Uiso 1 1 calc R . . C19 C 0.61258(16) 1.1107(3) 0.17144(15) 0.0237(6) Uani 1 1 d . . . C20 C 0.67782(16) 1.0304(3) 0.21911(14) 0.0215(6) Uani 1 1 d . . . C21 C 0.73710(15) 0.9286(2) 0.18974(13) 0.0192(5) Uani 1 1 d . . . C22 C 0.70881(16) 0.7952(3) 0.15166(13) 0.0204(5) Uani 1 1 d . . . C23 C 0.62322(16) 0.7482(3) 0.14132(15) 0.0264(6) Uani 1 1 d . . . H23 H 0.5833 0.8078 0.1580 0.032 Uiso 1 1 calc R . . C24 C 0.59817(18) 0.6167(3) 0.10724(16) 0.0330(7) Uani 1 1 d . . . H24 H 0.5419 0.5880 0.1017 0.040 Uiso 1 1 calc R . . C25 C 0.65730(19) 0.5246(3) 0.08052(16) 0.0317(7) Uani 1 1 d . . . H25 H 0.6399 0.4358 0.0573 0.038 Uiso 1 1 calc R . . C26 C 0.73963(18) 0.5663(3) 0.08882(14) 0.0263(6) Uani 1 1 d . . . H26 H 0.7780 0.5059 0.0705 0.032 Uiso 1 1 calc R . . C27 C 0.76814(16) 0.7007(3) 0.12505(13) 0.0204(5) Uani 1 1 d . . . C28 C 0.85419(16) 0.7401(3) 0.13850(13) 0.0206(5) Uani 1 1 d . . . H28 H 0.8932 0.6796 0.1211 0.025 Uiso 1 1 calc R . . C29 C 0.88128(16) 0.8654(3) 0.17653(13) 0.0192(5) Uani 1 1 d . . . H29 H 0.9384 0.8886 0.1858 0.023 Uiso 1 1 calc R . . C30 C 0.82228(16) 0.9598(3) 0.20174(13) 0.0188(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0352(4) 0.0275(4) 0.0195(3) 0.0006(3) 0.0100(3) 0.0013(3) S2 0.0476(5) 0.0663(6) 0.0351(5) 0.0115(4) 0.0188(4) 0.0283(4) S3 0.0392(5) 0.0430(5) 0.0282(4) 0.0153(3) 0.0127(3) 0.0081(3) S4 0.0300(4) 0.0246(3) 0.0183(3) 0.0013(3) 0.0068(3) -0.0009(3) S5 0.0318(4) 0.0294(4) 0.0198(3) 0.0042(3) 0.0084(3) -0.0015(3) S6 0.0267(4) 0.0233(3) 0.0182(3) 0.0007(3) 0.0051(3) -0.0024(3) O1 0.0296(11) 0.0190(9) 0.0272(10) 0.0006(8) 0.0089(8) 0.0002(7) O2 0.0224(10) 0.0172(9) 0.0232(9) -0.0014(7) 0.0046(8) -0.0011(7) C1 0.0316(15) 0.0185(12) 0.0171(13) -0.0034(11) 0.0059(11) -0.0066(11) C2 0.0364(17) 0.0258(14) 0.0244(15) 0.0018(12) 0.0084(12) 0.0070(12) C3 0.0398(19) 0.0332(16) 0.0481(19) 0.0128(15) 0.0089(15) 0.0119(14) C4 0.0420(19) 0.0340(16) 0.0270(16) 0.0100(13) 0.0064(14) 0.0033(13) C5 0.0378(17) 0.0227(13) 0.0217(14) 0.0041(11) 0.0096(12) 0.0068(11) C6 0.0295(15) 0.0189(12) 0.0184(13) -0.0019(11) 0.0068(11) -0.0053(11) C7 0.0305(15) 0.0193(13) 0.0181(13) -0.0023(10) 0.0039(11) -0.0041(11) C8 0.0255(14) 0.0166(12) 0.0185(13) -0.0015(10) 0.0019(11) -0.0016(10) C9 0.0323(16) 0.0236(14) 0.0218(14) -0.0063(11) 0.0069(12) -0.0025(11) C10 0.0241(14) 0.0210(13) 0.0202(13) -0.0008(11) 0.0045(11) -0.0052(11) C11 0.0218(14) 0.0176(12) 0.0330(15) 0.0002(11) 0.0110(12) -0.0028(10) C12 0.0327(17) 0.0289(15) 0.0368(17) -0.0045(13) 0.0169(14) -0.0009(12) C13 0.0286(17) 0.0271(15) 0.056(2) -0.0047(14) 0.0243(15) 0.0043(12) C14 0.0197(14) 0.0188(13) 0.0529(19) 0.0002(13) 0.0123(13) -0.0003(10) C15 0.0195(15) 0.0243(15) 0.077(3) 0.0078(16) 0.0123(15) 0.0028(12) C16 0.0237(16) 0.0254(15) 0.067(2) 0.0094(15) -0.0030(15) 0.0010(12) C17 0.0331(17) 0.0241(14) 0.0484(19) 0.0047(14) -0.0031(15) -0.0060(12) C18 0.0246(15) 0.0184(13) 0.0368(16) 0.0020(12) 0.0014(12) -0.0013(11) C19 0.0198(14) 0.0151(12) 0.0372(16) 0.0007(11) 0.0080(12) -0.0034(10) C20 0.0202(14) 0.0159(12) 0.0299(15) -0.0004(11) 0.0085(11) -0.0018(10) C21 0.0216(13) 0.0161(12) 0.0208(13) 0.0025(10) 0.0062(10) 0.0012(10) C22 0.0237(14) 0.0173(12) 0.0205(13) 0.0052(10) 0.0045(11) 0.0009(10) C23 0.0218(14) 0.0192(13) 0.0385(16) 0.0002(12) 0.0065(12) 0.0000(11) C24 0.0249(15) 0.0252(14) 0.0473(18) 0.0023(13) 0.0019(13) -0.0039(12) C25 0.0384(18) 0.0188(13) 0.0354(16) -0.0025(12) -0.0010(14) -0.0042(12) C26 0.0355(16) 0.0202(13) 0.0233(14) 0.0003(11) 0.0055(12) 0.0054(11) C27 0.0269(14) 0.0183(12) 0.0165(13) 0.0041(10) 0.0056(11) 0.0013(10) C28 0.0243(14) 0.0227(13) 0.0161(13) 0.0008(10) 0.0072(11) 0.0047(10) C29 0.0177(13) 0.0239(13) 0.0162(12) 0.0031(10) 0.0037(10) 0.0007(10) C30 0.0246(14) 0.0171(12) 0.0147(12) 0.0008(10) 0.0033(10) -0.0001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.762(3) . ? S1 C2 1.763(3) . ? S2 C2 1.753(3) . ? S2 C3 1.811(3) . ? S3 C5 1.755(3) . ? S3 C4 1.802(3) . ? S4 C5 1.750(3) . ? S4 C1 1.761(2) . ? S5 C7 1.749(3) . ? S5 C6 1.765(3) . ? S6 C8 1.761(3) . ? S6 C6 1.764(2) . ? O1 C11 1.384(3) . ? O1 C9 1.445(3) . ? O2 C30 1.383(3) . ? O2 C10 1.439(3) . ? C1 C6 1.341(4) . ? C2 C5 1.346(4) . ? C3 C4 1.514(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C7 C8 1.339(4) . ? C7 C9 1.494(4) . ? C8 C10 1.513(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C20 1.378(4) . ? C11 C12 1.420(4) . ? C12 C13 1.357(4) . ? C12 H12 0.9300 . ? C13 C14 1.419(4) . ? C13 H13 0.9300 . ? C14 C15 1.424(4) . ? C14 C19 1.430(4) . ? C15 C16 1.359(5) . ? C15 H15 0.9300 . ? C16 C17 1.409(4) . ? C16 H16 0.9300 . ? C17 C18 1.374(4) . ? C17 H17 0.9300 . ? C18 C19 1.417(4) . ? C18 H18 0.9300 . ? C19 C20 1.444(4) . ? C20 C21 1.492(3) . ? C21 C30 1.379(3) . ? C21 C22 1.430(3) . ? C22 C23 1.422(3) . ? C22 C27 1.429(3) . ? C23 C24 1.372(4) . ? C23 H23 0.9300 . ? C24 C25 1.414(4) . ? C24 H24 0.9300 . ? C25 C26 1.360(4) . ? C25 H25 0.9300 . ? C26 C27 1.424(3) . ? C26 H26 0.9300 . ? C27 C28 1.410(3) . ? C28 C29 1.364(3) . ? C28 H28 0.9300 . ? C29 C30 1.413(3) . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 94.88(12) . . ? C2 S2 C3 102.95(14) . . ? C5 S3 C4 97.25(13) . . ? C5 S4 C1 95.25(13) . . ? C7 S5 C6 95.11(12) . . ? C8 S6 C6 94.97(12) . . ? C11 O1 C9 114.98(18) . . ? C30 O2 C10 117.51(19) . . ? C6 C1 S4 119.6(2) . . ? C6 C1 S1 125.6(2) . . ? S4 C1 S1 114.77(14) . . ? C5 C2 S2 128.6(2) . . ? C5 C2 S1 117.4(2) . . ? S2 C2 S1 114.06(15) . . ? C4 C3 S2 115.1(2) . . ? C4 C3 H3A 108.5 . . ? S2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? S2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 S3 112.4(2) . . ? C3 C4 H4A 109.1 . . ? S3 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? S3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C2 C5 S4 117.6(2) . . ? C2 C5 S3 127.3(2) . . ? S4 C5 S3 115.02(15) . . ? C1 C6 S6 125.5(2) . . ? C1 C6 S5 120.6(2) . . ? S6 C6 S5 113.95(14) . . ? C8 C7 C9 125.4(2) . . ? C8 C7 S5 117.8(2) . . ? C9 C7 S5 116.66(19) . . ? C7 C8 C10 124.5(2) . . ? C7 C8 S6 117.2(2) . . ? C10 C8 S6 118.27(18) . . ? O1 C9 C7 107.87(19) . . ? O1 C9 H9A 110.1 . . ? C7 C9 H9A 110.1 . . ? O1 C9 H9B 110.1 . . ? C7 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? O2 C10 C8 112.5(2) . . ? O2 C10 H10A 109.1 . . ? C8 C10 H10A 109.1 . . ? O2 C10 H10B 109.1 . . ? C8 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C20 C11 O1 118.4(2) . . ? C20 C11 C12 122.4(2) . . ? O1 C11 C12 119.2(2) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 121.2(3) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 122.1(3) . . ? C13 C14 C19 119.4(3) . . ? C15 C14 C19 118.5(3) . . ? C16 C15 C14 121.6(3) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 119.9(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 121.0(3) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C14 118.4(2) . . ? C18 C19 C20 122.5(2) . . ? C14 C19 C20 119.0(2) . . ? C11 C20 C19 118.3(2) . . ? C11 C20 C21 119.4(2) . . ? C19 C20 C21 122.2(2) . . ? C30 C21 C22 118.4(2) . . ? C30 C21 C20 119.6(2) . . ? C22 C21 C20 121.9(2) . . ? C23 C22 C27 117.6(2) . . ? C23 C22 C21 122.5(2) . . ? C27 C22 C21 119.9(2) . . ? C24 C23 C22 121.5(2) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.8(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 121.2(2) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 121.8(2) . . ? C28 C27 C22 118.8(2) . . ? C26 C27 C22 119.4(2) . . ? C29 C28 C27 121.2(2) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 119.8(2) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C21 C30 O2 117.4(2) . . ? C21 C30 C29 121.8(2) . . ? O2 C30 C29 120.8(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 S4 C1 C6 -176.7(2) . . . . ? C5 S4 C1 S1 3.48(16) . . . . ? C2 S1 C1 C6 176.5(2) . . . . ? C2 S1 C1 S4 -3.67(16) . . . . ? C3 S2 C2 C5 -6.5(3) . . . . ? C3 S2 C2 S1 172.30(16) . . . . ? C1 S1 C2 C5 2.5(2) . . . . ? C1 S1 C2 S2 -176.40(15) . . . . ? C2 S2 C3 C4 -29.2(3) . . . . ? S2 C3 C4 S3 68.4(3) . . . . ? C5 S3 C4 C3 -62.7(2) . . . . ? S2 C2 C5 S4 178.25(16) . . . . ? S1 C2 C5 S4 -0.5(3) . . . . ? S2 C2 C5 S3 2.5(4) . . . . ? S1 C2 C5 S3 -176.26(15) . . . . ? C1 S4 C5 C2 -1.8(2) . . . . ? C1 S4 C5 S3 174.46(15) . . . . ? C4 S3 C5 C2 28.6(3) . . . . ? C4 S3 C5 S4 -147.23(16) . . . . ? S4 C1 C6 S6 -179.90(13) . . . . ? S1 C1 C6 S6 -0.1(4) . . . . ? S4 C1 C6 S5 0.0(3) . . . . ? S1 C1 C6 S5 179.84(13) . . . . ? C8 S6 C6 C1 -170.4(2) . . . . ? C8 S6 C6 S5 9.67(15) . . . . ? C7 S5 C6 C1 170.2(2) . . . . ? C7 S5 C6 S6 -9.85(16) . . . . ? C6 S5 C7 C8 6.3(2) . . . . ? C6 S5 C7 C9 -178.39(19) . . . . ? C9 C7 C8 C10 4.1(4) . . . . ? S5 C7 C8 C10 179.02(18) . . . . ? C9 C7 C8 S6 -175.30(19) . . . . ? S5 C7 C8 S6 -0.4(3) . . . . ? C6 S6 C8 C7 -5.7(2) . . . . ? C6 S6 C8 C10 174.85(19) . . . . ? C11 O1 C9 C7 -140.8(2) . . . . ? C8 C7 C9 O1 85.9(3) . . . . ? S5 C7 C9 O1 -89.0(2) . . . . ? C30 O2 C10 C8 -63.0(3) . . . . ? C7 C8 C10 O2 -48.1(3) . . . . ? S6 C8 C10 O2 131.33(19) . . . . ? C9 O1 C11 C20 121.3(2) . . . . ? C9 O1 C11 C12 -60.1(3) . . . . ? C20 C11 C12 C13 1.9(4) . . . . ? O1 C11 C12 C13 -176.6(2) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C15 177.2(3) . . . . ? C12 C13 C14 C19 -1.8(4) . . . . ? C13 C14 C15 C16 -179.0(3) . . . . ? C19 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 -1.9(4) . . . . ? C15 C16 C17 C18 1.0(4) . . . . ? C16 C17 C18 C19 1.8(4) . . . . ? C17 C18 C19 C14 -3.5(4) . . . . ? C17 C18 C19 C20 177.4(2) . . . . ? C13 C14 C19 C18 -178.3(2) . . . . ? C15 C14 C19 C18 2.6(4) . . . . ? C13 C14 C19 C20 0.8(4) . . . . ? C15 C14 C19 C20 -178.3(2) . . . . ? O1 C11 C20 C19 175.7(2) . . . . ? C12 C11 C20 C19 -2.9(4) . . . . ? O1 C11 C20 C21 -5.2(3) . . . . ? C12 C11 C20 C21 176.2(2) . . . . ? C18 C19 C20 C11 -179.4(2) . . . . ? C14 C19 C20 C11 1.5(3) . . . . ? C18 C19 C20 C21 1.5(4) . . . . ? C14 C19 C20 C21 -177.6(2) . . . . ? C11 C20 C21 C30 -62.4(3) . . . . ? C19 C20 C21 C30 116.6(3) . . . . ? C11 C20 C21 C22 115.0(3) . . . . ? C19 C20 C21 C22 -65.9(3) . . . . ? C30 C21 C22 C23 175.4(2) . . . . ? C20 C21 C22 C23 -2.1(4) . . . . ? C30 C21 C22 C27 -2.0(3) . . . . ? C20 C21 C22 C27 -179.5(2) . . . . ? C27 C22 C23 C24 0.2(4) . . . . ? C21 C22 C23 C24 -177.3(2) . . . . ? C22 C23 C24 C25 -0.7(4) . . . . ? C23 C24 C25 C26 0.2(4) . . . . ? C24 C25 C26 C27 0.9(4) . . . . ? C25 C26 C27 C28 175.5(2) . . . . ? C25 C26 C27 C22 -1.5(4) . . . . ? C23 C22 C27 C28 -176.2(2) . . . . ? C21 C22 C27 C28 1.3(3) . . . . ? C23 C22 C27 C26 0.9(3) . . . . ? C21 C22 C27 C26 178.4(2) . . . . ? C26 C27 C28 C29 -176.6(2) . . . . ? C22 C27 C28 C29 0.4(3) . . . . ? C27 C28 C29 C30 -1.4(4) . . . . ? C22 C21 C30 O2 179.2(2) . . . . ? C20 C21 C30 O2 -3.2(3) . . . . ? C22 C21 C30 C29 1.0(4) . . . . ? C20 C21 C30 C29 178.6(2) . . . . ? C10 O2 C30 C21 151.7(2) . . . . ? C10 O2 C30 C29 -30.1(3) . . . . ? C28 C29 C30 C21 0.7(4) . . . . ? C28 C29 C30 O2 -177.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.596 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.202