# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound7 _database_code_depnum_ccdc_archive 'CCDC 860421' #TrackingRef 'compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H60 N2 S Th' _chemical_formula_sum 'C49 H60 N2 S Th' _chemical_formula_weight 941.09 _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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.025(3) _cell_length_b 20.974(5) _cell_length_c 21.352(5) _cell_angle_alpha 115.257(4) _cell_angle_beta 90.452(5) _cell_angle_gamma 99.122(5) _cell_volume 4393.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 643 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 3.476 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7684 _exptl_absorpt_correction_T_max 0.9337 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21622 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.2572 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.05 _reflns_number_total 15324 _reflns_number_gt 7406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^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 15324 _refine_ls_number_parameters 979 _refine_ls_number_restraints 618 _refine_ls_R_factor_all 0.1829 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1781 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4491(14) 0.2973(8) 0.8820(8) 0.020(4) Uani 1 1 d U . . H1 H 0.4715 0.3196 0.8522 0.025 Uiso 1 1 calc R . . C2 C 0.3320(14) 0.2976(9) 0.9057(8) 0.025(4) Uani 1 1 d U . . H2 H 0.2752 0.3203 0.8927 0.030 Uiso 1 1 calc R . . C3 C 0.2996(16) 0.2650(9) 0.9477(9) 0.032(5) Uani 1 1 d U . . H3 H 0.2205 0.2662 0.9650 0.038 Uiso 1 1 calc R . . C4 C 0.3796(16) 0.2303(10) 0.9654(9) 0.035(5) Uani 1 1 d U . . H4 H 0.3557 0.2062 0.9935 0.042 Uiso 1 1 calc R . . C5 C 0.5005(15) 0.2312(9) 0.9405(8) 0.027(4) Uani 1 1 d U . . C6 C 0.5838(14) 0.1890(9) 0.9497(8) 0.023(4) Uani 1 1 d U . . C7 C 0.5452(14) 0.1361(9) 0.9692(8) 0.024(4) Uani 1 1 d U . . H7 H 0.4644 0.1305 0.9835 0.028 Uiso 1 1 calc R . . C8 C 0.6292(15) 0.0867(10) 0.9683(8) 0.032(5) Uani 1 1 d U . . H8 H 0.6015 0.0482 0.9800 0.038 Uiso 1 1 calc R . . C9 C 0.7427(15) 0.0972(8) 0.9510(8) 0.024(4) Uani 1 1 d U . . H9 H 0.7954 0.0650 0.9497 0.029 Uiso 1 1 calc R . . C10 C 0.7929(14) 0.1592(8) 0.9329(8) 0.021(4) Uani 1 1 d U . . H10 H 0.8138 0.1355 0.8837 0.025 Uiso 1 1 calc R . . C11 C 0.9184(15) 0.2084(9) 0.9749(8) 0.025(4) Uani 1 1 d U . . C12 C 0.9078(13) 0.2504(8) 1.0523(7) 0.013(3) Uani 1 1 d U . . C13 C 0.8043(15) 0.2446(9) 1.0885(8) 0.024(4) Uani 1 1 d U . . H13 H 0.7308 0.2129 1.0636 0.028 Uiso 1 1 calc R . . C14 C 0.8066(14) 0.2833(8) 1.1583(7) 0.020(4) Uani 1 1 d U . . H14 H 0.7349 0.2779 1.1813 0.024 Uiso 1 1 calc R . . C15 C 0.9110(15) 0.3304(9) 1.1966(9) 0.030(4) Uani 1 1 d U . . H15 H 0.9113 0.3555 1.2456 0.036 Uiso 1 1 calc R . . C16 C 1.0160(15) 0.3414(9) 1.1639(8) 0.023(4) Uani 1 1 d U . . H16 H 1.0870 0.3753 1.1896 0.027 Uiso 1 1 calc R . . C17 C 1.0129(14) 0.3010(8) 1.0927(8) 0.021(4) Uani 1 1 d U . . H17 H 1.0841 0.3075 1.0698 0.025 Uiso 1 1 calc R . . C18 C 1.0068(13) 0.1550(8) 0.9663(8) 0.018(4) Uani 1 1 d U . . C19 C 1.0490(14) 0.1417(9) 1.0190(8) 0.024(4) Uani 1 1 d U . . H19 H 1.0222 0.1650 1.0641 0.029 Uiso 1 1 calc R . . C20 C 1.1308(16) 0.0945(10) 1.0074(9) 0.034(5) Uani 1 1 d U . . H20 H 1.1588 0.0854 1.0445 0.041 Uiso 1 1 calc R . . C21 C 1.1711(15) 0.0612(10) 0.9426(9) 0.034(5) Uani 1 1 d U . . H21 H 1.2262 0.0285 0.9350 0.041 Uiso 1 1 calc R . . C22 C 1.1331(15) 0.0742(9) 0.8891(8) 0.028(4) Uani 1 1 d U . . H22 H 1.1627 0.0515 0.8447 0.034 Uiso 1 1 calc R . . C23 C 1.0502(13) 0.1214(8) 0.9000(8) 0.019(4) Uani 1 1 d U . . H23 H 1.0233 0.1308 0.8629 0.022 Uiso 1 1 calc R . . C24 C 0.7735(14) 0.4239(9) 0.9813(8) 0.019(4) Uani 1 1 d U . . C25 C 0.6993(14) 0.4242(8) 0.9302(8) 0.015(4) Uani 1 1 d U . . H25 H 0.6135 0.4248 0.9330 0.019 Uiso 1 1 calc R . . C26 C 0.7619(15) 0.4237(9) 0.8732(8) 0.022(4) Uani 1 1 d U . . C27 C 0.8836(14) 0.4184(8) 0.8890(8) 0.017(4) Uani 1 1 d U . . H27 H 0.9483 0.4126 0.8590 0.021 Uiso 1 1 calc R . . C28 C 0.8928(15) 0.4235(8) 0.9583(8) 0.023(4) Uani 1 1 d U . . H28 H 0.9659 0.4261 0.9838 0.027 Uiso 1 1 calc R . . C29 C 0.7404(13) 0.4456(9) 1.0558(8) 0.016(4) Uani 1 1 d U . . C30 C 0.7328(15) 0.5261(9) 1.0893(8) 0.031(5) Uani 1 1 d U . . H30A H 0.8115 0.5539 1.0871 0.046 Uiso 1 1 calc R . . H30B H 0.7151 0.5411 1.1380 0.046 Uiso 1 1 calc R . . H30C H 0.6669 0.5344 1.0642 0.046 Uiso 1 1 calc R . . C31 C 0.6198(16) 0.4029(10) 1.0617(9) 0.038(5) Uani 1 1 d U . . H31A H 0.5535 0.4068 1.0334 0.057 Uiso 1 1 calc R . . H31B H 0.6006 0.4219 1.1104 0.057 Uiso 1 1 calc R . . H31C H 0.6275 0.3525 1.0452 0.057 Uiso 1 1 calc R . . C32 C 0.8431(15) 0.4373(10) 1.0983(8) 0.031(5) Uani 1 1 d U . . H32A H 0.8476 0.3865 1.0815 0.046 Uiso 1 1 calc R . . H32B H 0.8261 0.4570 1.1473 0.046 Uiso 1 1 calc R . . H32C H 0.9219 0.4633 1.0934 0.046 Uiso 1 1 calc R . . C33 C 0.7213(16) 0.4460(9) 0.8171(9) 0.030(5) Uani 1 1 d U . . C34 C 0.7099(17) 0.5255(10) 0.8582(9) 0.044(5) Uani 1 1 d U . . H34A H 0.6332 0.5287 0.8813 0.066 Uiso 1 1 calc R . . H34B H 0.7092 0.5479 0.8262 0.066 Uiso 1 1 calc R . . H34C H 0.7802 0.5505 0.8932 0.066 Uiso 1 1 calc R . . C35 C 0.5995(17) 0.4008(11) 0.7778(9) 0.048(6) Uani 1 1 d U . . H35A H 0.6059 0.3499 0.7585 0.072 Uiso 1 1 calc R . . H35B H 0.5801 0.4132 0.7400 0.072 Uiso 1 1 calc R . . H35C H 0.5340 0.4099 0.8097 0.072 Uiso 1 1 calc R . . C36 C 0.8201(15) 0.4427(9) 0.7652(8) 0.027(4) Uani 1 1 d U . . H36A H 0.8980 0.4728 0.7908 0.040 Uiso 1 1 calc R . . H36B H 0.7927 0.4602 0.7326 0.040 Uiso 1 1 calc R . . H36C H 0.8322 0.3931 0.7394 0.040 Uiso 1 1 calc R . . C37 C 0.8629(15) 0.2140(9) 0.7465(8) 0.021(4) Uani 1 1 d U . . C38 C 0.7944(15) 0.1555(9) 0.7558(8) 0.023(4) Uani 1 1 d U . . H38 H 0.8313 0.1222 0.7651 0.027 Uiso 1 1 calc R . . C39 C 0.6679(15) 0.1525(9) 0.7498(7) 0.019(4) Uani 1 1 d U . . C40 C 0.6543(17) 0.2148(10) 0.7428(8) 0.035(5) Uani 1 1 d U . . H40 H 0.5783 0.2303 0.7415 0.043 Uiso 1 1 calc R . . C41 C 0.7675(14) 0.2494(9) 0.7382(7) 0.021(4) Uani 1 1 d U . . H41 H 0.7809 0.2913 0.7305 0.025 Uiso 1 1 calc R . . C42 C 0.9959(15) 0.2236(9) 0.7303(7) 0.024(4) Uani 1 1 d U . . C43 C 0.9915(17) 0.1968(11) 0.6512(8) 0.049(6) Uani 1 1 d U . . H43A H 0.9518 0.1463 0.6285 0.074 Uiso 1 1 calc R . . H43B H 1.0755 0.2018 0.6371 0.074 Uiso 1 1 calc R . . H43C H 0.9442 0.2252 0.6373 0.074 Uiso 1 1 calc R . . C44 C 1.0701(16) 0.1792(9) 0.7505(9) 0.034(5) Uani 1 1 d U . . H44A H 1.0648 0.1914 0.8000 0.052 Uiso 1 1 calc R . . H44B H 1.1564 0.1894 0.7417 0.052 Uiso 1 1 calc R . . H44C H 1.0369 0.1282 0.7229 0.052 Uiso 1 1 calc R . . C45 C 1.0622(15) 0.3018(9) 0.7660(8) 0.034(5) Uani 1 1 d U . . H45A H 1.0092 0.3328 0.7607 0.051 Uiso 1 1 calc R . . H45B H 1.1393 0.3070 0.7447 0.051 Uiso 1 1 calc R . . H45C H 1.0805 0.3156 0.8156 0.051 Uiso 1 1 calc R . . C46 C 0.5694(16) 0.0899(9) 0.7392(8) 0.031(5) Uani 1 1 d U . . C47 C 0.5621(17) 0.0385(10) 0.6600(8) 0.043(5) Uani 1 1 d U . . H47A H 0.5414 0.0635 0.6327 0.064 Uiso 1 1 calc R . . H47B H 0.4984 -0.0038 0.6494 0.064 Uiso 1 1 calc R . . H47C H 0.6419 0.0236 0.6481 0.064 Uiso 1 1 calc R . . C48 C 0.6065(15) 0.0470(9) 0.7771(8) 0.030(5) Uani 1 1 d U . . H48A H 0.6859 0.0327 0.7626 0.044 Uiso 1 1 calc R . . H48B H 0.5435 0.0042 0.7655 0.044 Uiso 1 1 calc R . . H48C H 0.6137 0.0768 0.8274 0.044 Uiso 1 1 calc R . . C49 C 0.4422(14) 0.1076(10) 0.7554(9) 0.034(5) Uani 1 1 d U . . H49A H 0.4365 0.1275 0.8058 0.051 Uiso 1 1 calc R . . H49B H 0.3803 0.0638 0.7324 0.051 Uiso 1 1 calc R . . H49C H 0.4275 0.1427 0.7387 0.051 Uiso 1 1 calc R . . C50 C -0.0488(15) 0.3000(9) 0.4350(9) 0.028(5) Uani 1 1 d U . . H50 H -0.0276 0.3235 0.4837 0.034 Uiso 1 1 calc R . . C51 C -0.1635(15) 0.3023(9) 0.4110(9) 0.033(5) Uani 1 1 d U . . H51 H -0.2210 0.3244 0.4425 0.039 Uiso 1 1 calc R . . C52 C -0.1928(14) 0.2717(9) 0.3404(9) 0.025(4) Uani 1 1 d U . . H52 H -0.2704 0.2741 0.3226 0.030 Uiso 1 1 calc R . . C53 C -0.1130(15) 0.2388(9) 0.2967(9) 0.027(4) Uani 1 1 d U . . H53 H -0.1320 0.2189 0.2479 0.033 Uiso 1 1 calc R . . C54 C -0.0019(15) 0.2339(9) 0.3236(8) 0.022(4) Uani 1 1 d U . . C55 C 0.0924(14) 0.1934(8) 0.2838(8) 0.022(4) Uani 1 1 d U . . C56 C 0.0520(14) 0.1392(9) 0.2179(8) 0.022(4) Uani 1 1 d U . . H56 H -0.0278 0.1344 0.1974 0.026 Uiso 1 1 calc R . . C57 C 0.1329(14) 0.0907(9) 0.1815(8) 0.021(4) Uani 1 1 d U . . H57 H 0.1057 0.0519 0.1374 0.025 Uiso 1 1 calc R . . C58 C 0.2488(14) 0.1004(9) 0.2104(8) 0.024(4) Uani 1 1 d U . . H58 H 0.3001 0.0666 0.1869 0.029 Uiso 1 1 calc R . . C59 C 0.2982(14) 0.1632(8) 0.2784(8) 0.020(4) Uani 1 1 d U . . H59 H 0.3217 0.1407 0.3086 0.024 Uiso 1 1 calc R . . C60 C 0.4210(14) 0.2111(8) 0.2764(8) 0.018(4) Uani 1 1 d U . . C61 C 0.4097(13) 0.2544(8) 0.2360(8) 0.016(4) Uani 1 1 d U . . C62 C 0.3087(14) 0.2452(8) 0.1909(7) 0.018(4) Uani 1 1 d U . . H62 H 0.2358 0.2137 0.1898 0.021 Uiso 1 1 calc R . . C63 C 0.3086(14) 0.2789(8) 0.1480(8) 0.021(4) Uani 1 1 d U . . H63 H 0.2386 0.2689 0.1168 0.025 Uiso 1 1 calc R . . C64 C 0.4130(14) 0.3283(9) 0.1508(8) 0.028(4) Uani 1 1 d U . . H64 H 0.4147 0.3535 0.1229 0.034 Uiso 1 1 calc R . . C65 C 0.5125(14) 0.3391(8) 0.1954(8) 0.020(4) Uani 1 1 d U . . H65 H 0.5845 0.3715 0.1968 0.024 Uiso 1 1 calc R . . C66 C 0.5127(14) 0.3053(8) 0.2378(8) 0.018(4) Uani 1 1 d U . . H66 H 0.5830 0.3161 0.2690 0.022 Uiso 1 1 calc R . . C67 C 0.5156(14) 0.1639(9) 0.2489(7) 0.021(4) Uani 1 1 d U . . C68 C 0.5533(15) 0.1432(9) 0.1820(8) 0.027(4) Uani 1 1 d U . . H68 H 0.5147 0.1588 0.1525 0.032 Uiso 1 1 calc R . . C69 C 0.6415(17) 0.1022(10) 0.1557(9) 0.038(5) Uani 1 1 d U . . H69 H 0.6657 0.0913 0.1101 0.045 Uiso 1 1 calc R . . C70 C 0.6940(14) 0.0771(8) 0.1972(8) 0.019(4) Uani 1 1 d U . . H70 H 0.7541 0.0474 0.1799 0.023 Uiso 1 1 calc R . . C71 C 0.6598(15) 0.0948(9) 0.2652(9) 0.032(5) Uani 1 1 d U . . H71 H 0.6953 0.0774 0.2941 0.038 Uiso 1 1 calc R . . C72 C 0.5760(14) 0.1368(8) 0.2873(8) 0.020(4) Uani 1 1 d U . . H72 H 0.5551 0.1496 0.3337 0.024 Uiso 1 1 calc R . . C73 C 0.2623(14) 0.4216(8) 0.5582(8) 0.016(4) Uani 1 1 d U . . C74 C 0.3793(14) 0.4181(9) 0.5402(8) 0.021(4) Uani 1 1 d U . . H74 H 0.4440 0.4127 0.5662 0.025 Uiso 1 1 calc R . . C75 C 0.3901(14) 0.4235(8) 0.4784(8) 0.020(4) Uani 1 1 d U . . H75 H 0.4640 0.4245 0.4560 0.024 Uiso 1 1 calc R . . C76 C 0.2732(13) 0.4272(8) 0.4537(8) 0.015(4) Uani 1 1 d U . . C77 C 0.1919(16) 0.4263(9) 0.5043(8) 0.028(5) Uani 1 1 d U . . H77 H 0.1065 0.4284 0.5027 0.034 Uiso 1 1 calc R . . C78 C 0.2168(15) 0.4435(9) 0.6330(8) 0.026(4) Uani 1 1 d U . . C79 C 0.3125(15) 0.4388(9) 0.6820(8) 0.031(5) Uani 1 1 d U . . H79A H 0.3919 0.4672 0.6817 0.047 Uiso 1 1 calc R . . H79B H 0.3213 0.3887 0.6666 0.047 Uiso 1 1 calc R . . H79C H 0.2858 0.4574 0.7292 0.047 Uiso 1 1 calc R . . C80 C 0.0906(16) 0.4019(10) 0.6329(9) 0.042(5) Uani 1 1 d U . . H80A H 0.0650 0.4197 0.6803 0.062 Uiso 1 1 calc R . . H80B H 0.0948 0.3509 0.6154 0.062 Uiso 1 1 calc R . . H80C H 0.0306 0.4082 0.6028 0.062 Uiso 1 1 calc R . . C81 C 0.2041(19) 0.5224(11) 0.6616(9) 0.056(6) Uani 1 1 d U . . H81A H 0.1778 0.5385 0.7088 0.084 Uiso 1 1 calc R . . H81B H 0.1425 0.5279 0.6317 0.084 Uiso 1 1 calc R . . H81C H 0.2837 0.5514 0.6624 0.084 Uiso 1 1 calc R . . C82 C 0.2466(14) 0.4502(9) 0.3966(8) 0.019(4) Uani 1 1 d U . . C83 C 0.3496(16) 0.4377(10) 0.3465(8) 0.035(5) Uani 1 1 d U . . H83A H 0.4286 0.4654 0.3725 0.053 Uiso 1 1 calc R . . H83B H 0.3313 0.4531 0.3107 0.053 Uiso 1 1 calc R . . H83C H 0.3545 0.3866 0.3245 0.053 Uiso 1 1 calc R . . C84 C 0.1227(15) 0.4103(10) 0.3556(9) 0.036(5) Uani 1 1 d U . . H84A H 0.1280 0.3600 0.3271 0.054 Uiso 1 1 calc R . . H84B H 0.1016 0.4321 0.3255 0.054 Uiso 1 1 calc R . . H84C H 0.0589 0.4131 0.3879 0.054 Uiso 1 1 calc R . . C85 C 0.2410(15) 0.5301(9) 0.4327(8) 0.029(4) Uani 1 1 d U . . H85A H 0.1701 0.5373 0.4607 0.044 Uiso 1 1 calc R . . H85B H 0.2324 0.5480 0.3977 0.044 Uiso 1 1 calc R . . H85C H 0.3169 0.5562 0.4629 0.044 Uiso 1 1 calc R . . C86 C 0.3452(15) 0.2100(9) 0.5079(8) 0.026(4) Uani 1 1 d U . . C87 C 0.2836(14) 0.1536(9) 0.4479(8) 0.021(4) Uani 1 1 d U . . H87 H 0.3227 0.1204 0.4121 0.026 Uiso 1 1 calc R . . C88 C 0.1583(15) 0.1524(9) 0.4475(9) 0.029(4) Uani 1 1 d U . . C89 C 0.1373(16) 0.2107(9) 0.5084(8) 0.029(4) Uani 1 1 d U . . H89 H 0.0597 0.2234 0.5225 0.035 Uiso 1 1 calc R . . C90 C 0.2561(15) 0.2475(10) 0.5455(9) 0.028(4) Uani 1 1 d U . . H90 H 0.2710 0.2898 0.5881 0.034 Uiso 1 1 calc R . . C91 C 0.4799(16) 0.2152(9) 0.5335(9) 0.029(4) Uani 1 1 d U . . C92 C 0.5595(17) 0.1775(10) 0.4782(9) 0.046(6) Uani 1 1 d U . . H92A H 0.5820 0.2051 0.4516 0.069 Uiso 1 1 calc R . . H92B H 0.5143 0.1298 0.4471 0.069 Uiso 1 1 calc R . . H92C H 0.6344 0.1728 0.4997 0.069 Uiso 1 1 calc R . . C93 C 0.5424(16) 0.2944(10) 0.5720(9) 0.045(5) Uani 1 1 d U . . H93A H 0.6280 0.2974 0.5871 0.067 Uiso 1 1 calc R . . H93B H 0.4980 0.3188 0.6126 0.067 Uiso 1 1 calc R . . H93C H 0.5407 0.3175 0.5406 0.067 Uiso 1 1 calc R . . C94 C 0.472(2) 0.1833(13) 0.5874(11) 0.075(7) Uani 1 1 d U . . H94A H 0.4267 0.1339 0.5654 0.112 Uiso 1 1 calc R . . H94B H 0.4284 0.2121 0.6266 0.112 Uiso 1 1 calc R . . H94C H 0.5551 0.1839 0.6043 0.112 Uiso 1 1 calc R . . C95 C 0.0539(19) 0.0897(11) 0.4051(10) 0.047(6) Uani 1 1 d U . . C96 C 0.0882(16) 0.0475(9) 0.3308(8) 0.032(5) Uani 1 1 d U . . H96A H 0.0897 0.0769 0.3054 0.048 Uiso 1 1 calc R . . H96B H 0.0269 0.0035 0.3071 0.048 Uiso 1 1 calc R . . H96C H 0.1697 0.0351 0.3326 0.048 Uiso 1 1 calc R . . C97 C -0.0715(15) 0.1134(9) 0.4057(9) 0.034(5) Uani 1 1 d U . . H97A H -0.0915 0.1386 0.4538 0.052 Uiso 1 1 calc R . . H97B H -0.1356 0.0711 0.3807 0.052 Uiso 1 1 calc R . . H97C H -0.0674 0.1454 0.3829 0.052 Uiso 1 1 calc R . . C98 C 0.0457(17) 0.0392(10) 0.4429(9) 0.041(5) Uani 1 1 d U . . H98A H 0.1252 0.0239 0.4431 0.062 Uiso 1 1 calc R . . H98B H -0.0186 -0.0029 0.4183 0.062 Uiso 1 1 calc R . . H98C H 0.0256 0.0653 0.4909 0.062 Uiso 1 1 calc R . . N1 N 0.5324(11) 0.2656(7) 0.9009(7) 0.023(3) Uani 1 1 d . . . N2 N 0.7021(10) 0.2050(6) 0.9319(6) 0.014(3) Uani 1 1 d . . . N3 N 0.0338(11) 0.2673(7) 0.3945(6) 0.018(3) Uani 1 1 d . . . N4 N 0.2055(10) 0.2049(7) 0.3155(6) 0.014(3) Uani 1 1 d U . . S1 S 0.9712(4) 0.2689(2) 0.9360(2) 0.0205(10) Uani 1 1 d . . . S2 S 0.4702(4) 0.2758(2) 0.3684(2) 0.0214(10) Uani 1 1 d . . . Th1 Th 0.75916(5) 0.28267(3) 0.87700(3) 0.01724(18) Uani 1 1 d . . . Th2 Th 0.25738(5) 0.28355(3) 0.43636(3) 0.01762(19) Uani 1 1 d . . . _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.015(7) 0.016(7) 0.024(7) 0.002(6) 0.000(6) 0.009(6) C2 0.019(7) 0.023(8) 0.024(7) 0.003(6) -0.010(6) 0.001(6) C3 0.026(8) 0.023(8) 0.042(8) 0.006(7) 0.011(7) 0.010(6) C4 0.040(8) 0.034(8) 0.037(8) 0.019(7) -0.006(7) 0.015(7) C5 0.022(7) 0.026(8) 0.026(8) 0.008(6) 0.001(6) -0.001(6) C6 0.014(7) 0.025(8) 0.023(7) 0.004(6) 0.000(6) 0.003(6) C7 0.018(7) 0.026(8) 0.031(8) 0.014(6) 0.001(6) 0.010(6) C8 0.033(8) 0.037(8) 0.032(8) 0.021(7) 0.002(6) 0.007(7) C9 0.027(7) 0.011(7) 0.031(8) 0.008(6) -0.001(6) -0.004(6) C10 0.024(7) 0.018(7) 0.023(7) 0.010(6) 0.010(6) 0.011(6) C11 0.025(7) 0.020(8) 0.020(7) 0.000(6) 0.006(6) 0.000(6) C12 0.012(5) 0.015(5) 0.015(5) 0.007(4) 0.000(4) 0.009(4) C13 0.023(7) 0.027(8) 0.022(7) 0.010(6) 0.004(6) 0.007(6) C14 0.023(7) 0.024(8) 0.009(7) 0.004(6) 0.005(6) 0.003(6) C15 0.036(8) 0.030(8) 0.026(8) 0.015(6) 0.005(6) 0.003(6) C16 0.029(7) 0.017(7) 0.022(7) 0.006(6) -0.006(6) 0.014(6) C17 0.017(7) 0.018(7) 0.018(7) 0.001(6) -0.004(6) -0.001(6) C18 0.013(7) 0.020(7) 0.019(7) 0.005(6) 0.000(6) 0.006(6) C19 0.027(7) 0.024(8) 0.025(7) 0.011(6) 0.005(6) 0.014(6) C20 0.042(8) 0.038(9) 0.028(8) 0.018(7) 0.003(7) 0.014(7) C21 0.032(8) 0.034(8) 0.038(8) 0.014(7) -0.004(7) 0.015(7) C22 0.047(8) 0.028(8) 0.024(7) 0.021(6) 0.008(6) 0.020(6) C23 0.016(7) 0.025(8) 0.016(7) 0.008(6) 0.000(6) 0.006(6) C24 0.019(7) 0.023(8) 0.018(7) 0.012(6) -0.006(6) 0.002(6) C25 0.011(7) 0.006(7) 0.023(7) 0.000(6) 0.006(6) 0.003(6) C26 0.030(8) 0.015(7) 0.019(7) 0.003(6) -0.003(6) 0.007(6) C27 0.017(7) 0.019(7) 0.018(7) 0.008(6) 0.002(6) 0.010(6) C28 0.024(7) 0.015(7) 0.031(8) 0.008(6) 0.008(6) 0.014(6) C29 0.009(7) 0.021(8) 0.015(7) 0.006(6) 0.000(6) 0.004(6) C30 0.037(8) 0.026(8) 0.033(8) 0.015(6) 0.009(6) 0.011(6) C31 0.042(9) 0.040(9) 0.033(8) 0.018(7) 0.005(7) 0.006(7) C32 0.040(8) 0.033(8) 0.025(8) 0.014(6) 0.005(6) 0.016(7) C33 0.036(8) 0.020(8) 0.039(8) 0.015(6) 0.009(7) 0.014(6) C34 0.050(9) 0.044(9) 0.047(9) 0.027(7) 0.017(7) 0.013(7) C35 0.048(9) 0.055(10) 0.044(9) 0.021(7) 0.003(7) 0.019(7) C36 0.038(8) 0.022(8) 0.026(7) 0.015(6) 0.003(6) 0.010(6) C37 0.026(7) 0.016(7) 0.023(7) 0.010(6) 0.002(6) 0.003(6) C38 0.028(8) 0.018(8) 0.019(7) 0.003(6) -0.009(6) 0.007(6) C39 0.026(7) 0.025(8) 0.010(7) 0.011(6) -0.002(6) 0.007(6) C40 0.034(8) 0.040(9) 0.034(8) 0.014(7) -0.004(7) 0.018(7) C41 0.025(7) 0.018(7) 0.019(7) 0.009(6) -0.003(6) 0.004(6) C42 0.028(8) 0.033(8) 0.007(7) 0.002(6) 0.000(6) 0.011(6) C43 0.052(9) 0.060(10) 0.034(8) 0.016(7) 0.012(7) 0.017(7) C44 0.040(8) 0.031(8) 0.039(8) 0.020(7) 0.017(7) 0.010(7) C45 0.027(8) 0.035(8) 0.033(8) 0.009(7) 0.011(6) 0.003(7) C46 0.037(8) 0.024(8) 0.025(8) 0.004(6) 0.004(7) 0.000(7) C47 0.043(9) 0.035(9) 0.041(8) 0.008(7) -0.001(7) 0.006(7) C48 0.029(8) 0.024(8) 0.037(8) 0.017(7) -0.006(6) -0.004(6) C49 0.030(8) 0.034(8) 0.036(8) 0.012(7) 0.002(7) 0.010(7) C50 0.026(8) 0.021(8) 0.031(8) 0.007(6) 0.011(7) -0.002(6) C51 0.026(8) 0.023(8) 0.046(8) 0.011(7) 0.009(7) 0.006(6) C52 0.014(7) 0.025(8) 0.037(8) 0.013(6) 0.008(6) 0.004(6) C53 0.027(8) 0.028(8) 0.032(8) 0.018(6) 0.001(6) 0.003(6) C54 0.024(7) 0.016(7) 0.027(8) 0.010(6) 0.004(6) 0.002(6) C55 0.020(7) 0.016(7) 0.030(8) 0.011(6) 0.005(6) 0.002(6) C56 0.018(7) 0.027(8) 0.020(7) 0.009(6) 0.001(6) 0.007(6) C57 0.023(7) 0.023(8) 0.019(7) 0.016(6) 0.000(6) -0.004(6) C58 0.023(7) 0.025(8) 0.020(7) 0.005(6) 0.001(6) 0.007(6) C59 0.023(7) 0.016(7) 0.017(7) 0.005(6) -0.014(6) -0.002(6) C60 0.020(7) 0.020(7) 0.016(7) 0.009(6) -0.004(6) 0.002(6) C61 0.011(7) 0.019(7) 0.018(7) 0.007(6) 0.003(6) 0.002(6) C62 0.021(7) 0.012(7) 0.021(7) 0.007(6) 0.005(6) 0.007(6) C63 0.014(7) 0.022(8) 0.032(7) 0.016(6) 0.012(6) 0.001(6) C64 0.025(7) 0.033(8) 0.025(7) 0.010(6) 0.001(6) 0.010(6) C65 0.019(7) 0.017(7) 0.026(7) 0.008(6) 0.007(6) 0.010(6) C66 0.023(7) 0.019(7) 0.021(7) 0.015(6) 0.006(6) 0.010(6) C67 0.024(7) 0.025(8) 0.012(7) 0.004(6) 0.011(6) 0.009(6) C68 0.024(7) 0.027(8) 0.024(8) 0.006(6) 0.001(6) 0.007(6) C69 0.047(9) 0.038(9) 0.032(8) 0.019(7) 0.005(7) 0.008(7) C70 0.023(7) 0.009(7) 0.023(7) 0.004(6) -0.002(6) 0.007(6) C71 0.030(8) 0.033(8) 0.034(8) 0.016(7) -0.001(6) 0.005(6) C72 0.028(7) 0.012(7) 0.021(7) 0.004(6) 0.000(6) 0.014(6) C73 0.018(7) 0.010(7) 0.019(7) 0.002(6) -0.006(6) 0.009(6) C74 0.015(7) 0.023(8) 0.021(7) 0.006(6) 0.000(6) 0.004(6) C75 0.024(7) 0.017(7) 0.015(7) 0.004(6) 0.000(6) -0.001(6) C76 0.012(5) 0.013(5) 0.014(5) 0.001(4) -0.003(4) 0.001(4) C77 0.031(8) 0.034(8) 0.025(8) 0.015(6) 0.001(6) 0.012(7) C78 0.032(8) 0.023(8) 0.023(7) 0.007(6) 0.009(6) 0.011(6) C79 0.040(8) 0.030(8) 0.029(8) 0.015(6) -0.005(6) 0.014(7) C80 0.046(9) 0.040(9) 0.039(8) 0.016(7) 0.015(7) 0.010(7) C81 0.072(10) 0.061(10) 0.038(9) 0.025(7) 0.018(7) 0.013(8) C82 0.021(7) 0.013(7) 0.026(7) 0.012(6) 0.003(6) 0.003(6) C83 0.044(8) 0.029(8) 0.026(8) 0.004(6) 0.004(7) 0.011(7) C84 0.039(8) 0.036(9) 0.036(8) 0.021(7) -0.009(7) 0.003(7) C85 0.032(8) 0.025(8) 0.030(8) 0.009(6) -0.004(6) 0.009(6) C86 0.033(8) 0.025(8) 0.024(7) 0.017(6) -0.004(6) -0.004(6) C87 0.027(5) 0.018(5) 0.022(5) 0.012(4) 0.000(4) 0.006(4) C88 0.027(8) 0.029(8) 0.030(8) 0.011(6) -0.001(6) 0.009(6) C89 0.030(8) 0.038(8) 0.026(7) 0.021(6) 0.015(6) 0.007(6) C90 0.032(8) 0.030(8) 0.026(8) 0.015(6) 0.010(6) 0.006(6) C91 0.032(8) 0.027(8) 0.029(8) 0.010(6) -0.001(6) 0.012(6) C92 0.054(9) 0.052(9) 0.036(8) 0.024(7) -0.021(7) 0.013(7) C93 0.038(8) 0.044(9) 0.047(9) 0.012(7) -0.006(7) 0.018(7) C94 0.075(7) 0.075(7) 0.075(7) 0.033(3) 0.0063(12) 0.0135(16) C95 0.055(9) 0.043(9) 0.047(9) 0.023(7) 0.004(7) 0.008(7) C96 0.037(8) 0.031(8) 0.030(8) 0.016(7) -0.001(7) 0.008(7) C97 0.030(8) 0.039(8) 0.040(8) 0.026(7) 0.003(7) -0.006(6) C98 0.052(9) 0.033(9) 0.042(8) 0.020(7) -0.003(7) 0.005(7) N1 0.013(7) 0.019(9) 0.023(8) -0.003(7) -0.010(6) 0.007(6) N2 0.012(7) 0.014(8) 0.012(7) -0.001(6) 0.007(6) 0.007(6) N3 0.019(8) 0.020(8) 0.012(7) 0.006(6) -0.005(6) 0.001(6) N4 0.011(6) 0.018(6) 0.016(6) 0.008(5) 0.011(5) 0.002(5) S1 0.020(2) 0.023(3) 0.022(2) 0.013(2) 0.0036(19) 0.007(2) S2 0.023(2) 0.018(3) 0.020(2) 0.004(2) 0.003(2) 0.0059(19) Th1 0.0152(4) 0.0185(4) 0.0183(4) 0.0076(3) 0.0017(3) 0.0049(3) Th2 0.0166(4) 0.0196(4) 0.0166(4) 0.0068(3) 0.0032(3) 0.0061(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.367(19) . ? C1 C2 1.39(2) . ? C1 H1 0.9500 . ? C2 C3 1.36(2) . ? C2 H2 0.9500 . ? C3 C4 1.37(2) . ? C3 H3 0.9500 . ? C4 C5 1.44(2) . ? C4 H4 0.9500 . ? C5 N1 1.34(2) . ? C5 C6 1.44(2) . ? C6 C7 1.35(2) . ? C6 N2 1.392(18) . ? C7 C8 1.49(2) . ? C7 H7 0.9500 . ? C8 C9 1.32(2) . ? C8 H8 0.9500 . ? C9 C10 1.53(2) . ? C9 H9 0.9500 . ? C10 N2 1.500(18) . ? C10 C11 1.59(2) . ? C10 H10 1.0000 . ? C11 C12 1.52(2) . ? C11 C18 1.55(2) . ? C11 S1 1.821(17) . ? C12 C13 1.401(19) . ? C12 C17 1.424(19) . ? C13 C14 1.357(19) . ? C13 H13 0.9500 . ? C14 C15 1.38(2) . ? C14 H14 0.9500 . ? C15 C16 1.39(2) . ? C15 H15 0.9500 . ? C16 C17 1.387(19) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.36(2) . ? C18 C23 1.412(19) . ? C19 C20 1.39(2) . ? C19 H19 0.9500 . ? C20 C21 1.37(2) . ? C20 H20 0.9500 . ? C21 C22 1.36(2) . ? C21 H21 0.9500 . ? C22 C23 1.40(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.36(2) . ? C24 C28 1.41(2) . ? C24 C29 1.52(2) . ? C24 Th1 2.824(16) . ? C25 C26 1.40(2) . ? C25 Th1 2.880(15) . ? C25 H25 0.9500 . ? C26 C27 1.41(2) . ? C26 C33 1.55(2) . ? C26 Th1 2.988(17) . ? C27 C28 1.44(2) . ? C27 Th1 2.861(16) . ? C27 H27 0.9500 . ? C28 Th1 2.848(16) . ? C28 H28 0.9500 . ? C29 C31 1.52(2) . ? C29 C32 1.52(2) . ? C29 C30 1.54(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.52(2) . ? C33 C34 1.54(2) . ? C33 C36 1.55(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.43(2) . ? C37 C41 1.43(2) . ? C37 C42 1.51(2) . ? C37 Th1 2.880(15) . ? C38 C39 1.39(2) . ? C38 Th1 2.901(15) . ? C38 H38 0.9500 . ? C39 C40 1.41(2) . ? C39 C46 1.50(2) . ? C39 Th1 2.933(15) . ? C40 C41 1.37(2) . ? C40 Th1 2.741(16) . ? C40 H40 0.9500 . ? C41 Th1 2.746(15) . ? C41 H41 0.9500 . ? C42 C44 1.52(2) . ? C42 C45 1.53(2) . ? C42 C43 1.53(2) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C49 1.51(2) . ? C46 C48 1.54(2) . ? C46 C47 1.56(2) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N3 1.324(19) . ? C50 C51 1.38(2) . ? C50 H50 0.9500 . ? C51 C52 1.38(2) . ? C51 H51 0.9500 . ? C52 C53 1.33(2) . ? C52 H52 0.9500 . ? C53 C54 1.39(2) . ? C53 H53 0.9500 . ? C54 N3 1.392(18) . ? C54 C55 1.48(2) . ? C55 N4 1.351(18) . ? C55 C56 1.39(2) . ? C56 C57 1.44(2) . ? C56 H56 0.9500 . ? C57 C58 1.36(2) . ? C57 H57 0.9500 . ? C58 C59 1.506(19) . ? C58 H58 0.9500 . ? C59 N4 1.464(18) . ? C59 C60 1.56(2) . ? C59 H59 1.0000 . ? C60 C67 1.50(2) . ? C60 C61 1.51(2) . ? C60 S2 1.863(15) . ? C61 C62 1.402(19) . ? C61 C66 1.42(2) . ? C62 C63 1.38(2) . ? C62 H62 0.9500 . ? C63 C64 1.40(2) . ? C63 H63 0.9500 . ? C64 C65 1.37(2) . ? C64 H64 0.9500 . ? C65 C66 1.37(2) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.39(2) . ? C67 C72 1.40(2) . ? C68 C69 1.37(2) . ? C68 H68 0.9500 . ? C69 C70 1.37(2) . ? C69 H69 0.9500 . ? C70 C71 1.41(2) . ? C70 H70 0.9500 . ? C71 C72 1.33(2) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.35(2) . ? C73 C77 1.43(2) . ? C73 C78 1.57(2) . ? C73 Th2 2.946(15) . ? C74 C75 1.38(2) . ? C74 Th2 2.846(15) . ? C74 H74 0.9500 . ? C75 C76 1.41(2) . ? C75 Th2 2.816(15) . ? C75 H75 0.9500 . ? C76 C77 1.41(2) . ? C76 C82 1.53(2) . ? C76 Th2 2.850(16) . ? C77 Th2 2.931(18) . ? C77 H77 0.9500 . ? C78 C80 1.52(2) . ? C78 C79 1.53(2) . ? C78 C81 1.53(2) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C84 1.53(2) . ? C82 C85 1.53(2) . ? C82 C83 1.54(2) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 C87 1.39(2) . ? C86 C90 1.40(2) . ? C86 C91 1.55(2) . ? C86 Th2 2.849(17) . ? C87 C88 1.38(2) . ? C87 Th2 2.898(16) . ? C87 H87 0.9500 . ? C88 C89 1.41(2) . ? C88 C95 1.54(2) . ? C88 Th2 2.904(18) . ? C89 C90 1.44(2) . ? C89 Th2 2.802(16) . ? C89 H89 0.9500 . ? C90 Th2 2.740(16) . ? C90 H90 0.9500 . ? C91 C92 1.49(2) . ? C91 C93 1.54(2) . ? C91 C94 1.55(3) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 C96 1.54(2) . ? C95 C97 1.54(2) . ? C95 C98 1.57(2) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? N1 Th1 2.556(13) . ? N2 Th1 2.395(12) . ? N3 Th2 2.535(12) . ? N4 Th2 2.398(11) . ? S1 Th1 2.759(4) . ? S2 Th2 2.759(4) . ? _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.0(16) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 119.4(17) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 120.9(17) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 118.6(17) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 119.7(16) . . ? N1 C5 C6 118.1(15) . . ? C4 C5 C6 121.7(16) . . ? C7 C6 N2 125.0(16) . . ? C7 C6 C5 121.7(15) . . ? N2 C6 C5 113.2(15) . . ? C6 C7 C8 120.1(15) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 119.0(17) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 122.7(16) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? N2 C10 C9 115.6(13) . . ? N2 C10 C11 109.9(12) . . ? C9 C10 C11 115.8(13) . . ? N2 C10 H10 104.7 . . ? C9 C10 H10 104.7 . . ? C11 C10 H10 104.7 . . ? C12 C11 C18 107.7(13) . . ? C12 C11 C10 113.8(12) . . ? C18 C11 C10 104.5(12) . . ? C12 C11 S1 110.6(11) . . ? C18 C11 S1 112.5(11) . . ? C10 C11 S1 107.7(11) . . ? C13 C12 C17 116.0(13) . . ? C13 C12 C11 126.6(13) . . ? C17 C12 C11 117.3(13) . . ? C14 C13 C12 121.5(15) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 121.2(15) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 120.6(15) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 117.5(15) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C12 122.9(15) . . ? C16 C17 H17 118.5 . . ? C12 C17 H17 118.5 . . ? C19 C18 C23 118.9(15) . . ? C19 C18 C11 124.2(14) . . ? C23 C18 C11 116.8(14) . . ? C18 C19 C20 120.7(16) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 120.1(17) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.8(17) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.6(16) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C18 119.8(15) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? C25 C24 C28 106.2(14) . . ? C25 C24 C29 124.0(15) . . ? C28 C24 C29 126.7(14) . . ? C25 C24 Th1 78.5(9) . . ? C28 C24 Th1 76.6(10) . . ? C29 C24 Th1 126.5(11) . . ? C24 C25 C26 113.4(15) . . ? C24 C25 Th1 73.9(10) . . ? C26 C25 Th1 80.5(9) . . ? C24 C25 H25 123.3 . . ? C26 C25 H25 123.3 . . ? Th1 C25 H25 113.7 . . ? C25 C26 C27 104.2(14) . . ? C25 C26 C33 127.9(15) . . ? C27 C26 C33 125.6(15) . . ? C25 C26 Th1 71.9(9) . . ? C27 C26 Th1 71.1(9) . . ? C33 C26 Th1 133.9(11) . . ? C26 C27 C28 108.4(14) . . ? C26 C27 Th1 81.1(10) . . ? C28 C27 Th1 74.9(9) . . ? C26 C27 H27 125.8 . . ? C28 C27 H27 125.8 . . ? Th1 C27 H27 110.8 . . ? C24 C28 C27 107.4(14) . . ? C24 C28 Th1 74.7(9) . . ? C27 C28 Th1 75.9(9) . . ? C24 C28 H28 126.3 . . ? C27 C28 H28 126.3 . . ? Th1 C28 H28 115.4 . . ? C31 C29 C24 113.5(13) . . ? C31 C29 C32 108.9(14) . . ? C24 C29 C32 109.9(13) . . ? C31 C29 C30 109.3(13) . . ? C24 C29 C30 108.9(13) . . ? C32 C29 C30 106.1(13) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C34 111.4(15) . . ? C35 C33 C26 111.4(15) . . ? C34 C33 C26 104.4(14) . . ? C35 C33 C36 109.8(14) . . ? C34 C33 C36 107.2(14) . . ? C26 C33 C36 112.5(14) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C41 101.9(14) . . ? C38 C37 C42 127.7(15) . . ? C41 C37 C42 128.5(15) . . ? C38 C37 Th1 76.5(9) . . ? C41 C37 Th1 70.1(9) . . ? C42 C37 Th1 128.5(10) . . ? C39 C38 C37 112.9(15) . . ? C39 C38 Th1 77.5(9) . . ? C37 C38 Th1 74.9(9) . . ? C39 C38 H38 123.6 . . ? C37 C38 H38 123.6 . . ? Th1 C38 H38 115.5 . . ? C38 C39 C40 104.8(15) . . ? C38 C39 C46 126.8(16) . . ? C40 C39 C46 127.4(16) . . ? C38 C39 Th1 75.0(9) . . ? C40 C39 Th1 68.2(9) . . ? C46 C39 Th1 129.7(10) . . ? C41 C40 C39 109.4(16) . . ? C41 C40 Th1 75.7(9) . . ? C39 C40 Th1 83.3(10) . . ? C41 C40 H40 125.3 . . ? C39 C40 H40 125.3 . . ? Th1 C40 H40 108.3 . . ? C40 C41 C37 110.8(16) . . ? C40 C41 Th1 75.4(10) . . ? C37 C41 Th1 80.5(9) . . ? C40 C41 H41 124.6 . . ? C37 C41 H41 124.6 . . ? Th1 C41 H41 111.5 . . ? C37 C42 C44 112.4(14) . . ? C37 C42 C45 113.0(14) . . ? C44 C42 C45 107.8(14) . . ? C37 C42 C43 105.3(13) . . ? C44 C42 C43 108.4(14) . . ? C45 C42 C43 109.7(15) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C39 C46 C49 115.2(16) . . ? C39 C46 C48 111.8(14) . . ? C49 C46 C48 111.0(14) . . ? C39 C46 C47 105.3(14) . . ? C49 C46 C47 107.2(14) . . ? C48 C46 C47 105.5(15) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N3 C50 C51 124.2(16) . . ? N3 C50 H50 117.9 . . ? C51 C50 H50 117.9 . . ? C52 C51 C50 118.4(17) . . ? C52 C51 H51 120.8 . . ? C50 C51 H51 120.8 . . ? C53 C52 C51 120.4(16) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 119.0(16) . . ? C52 C53 H53 120.5 . . ? C54 C53 H53 120.5 . . ? C53 C54 N3 122.3(15) . . ? C53 C54 C55 126.7(15) . . ? N3 C54 C55 111.1(14) . . ? N4 C55 C56 124.0(15) . . ? N4 C55 C54 119.3(14) . . ? C56 C55 C54 116.2(14) . . ? C55 C56 C57 118.8(14) . . ? C55 C56 H56 120.6 . . ? C57 C56 H56 120.6 . . ? C58 C57 C56 119.7(15) . . ? C58 C57 H57 120.1 . . ? C56 C57 H57 120.1 . . ? C57 C58 C59 122.0(15) . . ? C57 C58 H58 119.0 . . ? C59 C58 H58 119.0 . . ? N4 C59 C58 114.2(12) . . ? N4 C59 C60 113.0(12) . . ? C58 C59 C60 115.5(13) . . ? N4 C59 H59 104.1 . . ? C58 C59 H59 104.1 . . ? C60 C59 H59 104.1 . . ? C67 C60 C61 111.3(13) . . ? C67 C60 C59 108.1(13) . . ? C61 C60 C59 115.0(12) . . ? C67 C60 S2 109.1(10) . . ? C61 C60 S2 107.2(11) . . ? C59 C60 S2 105.9(10) . . ? C62 C61 C66 114.7(14) . . ? C62 C61 C60 126.1(14) . . ? C66 C61 C60 119.0(13) . . ? C63 C62 C61 124.2(15) . . ? C63 C62 H62 117.9 . . ? C61 C62 H62 117.9 . . ? C62 C63 C64 119.1(16) . . ? C62 C63 H63 120.4 . . ? C64 C63 H63 120.4 . . ? C65 C64 C63 117.9(17) . . ? C65 C64 H64 121.1 . . ? C63 C64 H64 121.1 . . ? C66 C65 C64 122.9(16) . . ? C66 C65 H65 118.6 . . ? C64 C65 H65 118.6 . . ? C65 C66 C61 121.1(15) . . ? C65 C66 H66 119.4 . . ? C61 C66 H66 119.4 . . ? C68 C67 C72 112.8(15) . . ? C68 C67 C60 123.1(15) . . ? C72 C67 C60 124.2(14) . . ? C69 C68 C67 125.0(17) . . ? C69 C68 H68 117.5 . . ? C67 C68 H68 117.5 . . ? C68 C69 C70 117.7(17) . . ? C68 C69 H69 121.2 . . ? C70 C69 H69 121.2 . . ? C69 C70 C71 120.8(16) . . ? C69 C70 H70 119.6 . . ? C71 C70 H70 119.6 . . ? C72 C71 C70 117.4(17) . . ? C72 C71 H71 121.3 . . ? C70 C71 H71 121.3 . . ? C71 C72 C67 126.3(16) . . ? C71 C72 H72 116.8 . . ? C67 C72 H72 116.8 . . ? C74 C73 C77 108.3(15) . . ? C74 C73 C78 127.2(14) . . ? C77 C73 C78 121.5(14) . . ? C74 C73 Th2 72.4(9) . . ? C77 C73 Th2 75.3(9) . . ? C78 C73 Th2 133.9(11) . . ? C73 C74 C75 109.5(15) . . ? C73 C74 Th2 80.7(9) . . ? C75 C74 Th2 74.7(9) . . ? C73 C74 H74 125.3 . . ? C75 C74 H74 125.3 . . ? Th2 C74 H74 111.6 . . ? C74 C75 C76 108.9(14) . . ? C74 C75 Th2 77.1(9) . . ? C76 C75 Th2 76.9(9) . . ? C74 C75 H75 125.6 . . ? C76 C75 H75 125.6 . . ? Th2 C75 H75 112.7 . . ? C77 C76 C75 106.2(14) . . ? C77 C76 C82 124.7(14) . . ? C75 C76 C82 126.8(14) . . ? C77 C76 Th2 79.0(10) . . ? C75 C76 Th2 74.2(9) . . ? C82 C76 Th2 126.1(10) . . ? C76 C77 C73 107.1(15) . . ? C76 C77 Th2 72.7(9) . . ? C73 C77 Th2 76.5(10) . . ? C76 C77 H77 126.5 . . ? C73 C77 H77 126.5 . . ? Th2 C77 H77 116.5 . . ? C80 C78 C79 111.7(15) . . ? C80 C78 C81 106.7(15) . . ? C79 C78 C81 106.7(14) . . ? C80 C78 C73 113.1(14) . . ? C79 C78 C73 111.2(14) . . ? C81 C78 C73 107.0(14) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C78 C81 H81A 109.5 . . ? C78 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C78 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C84 C82 C85 108.2(13) . . ? C84 C82 C76 111.6(13) . . ? C85 C82 C76 107.0(13) . . ? C84 C82 C83 109.5(13) . . ? C85 C82 C83 109.7(13) . . ? C76 C82 C83 110.7(13) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C82 C85 H85A 109.5 . . ? C82 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C82 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C87 C86 C90 106.8(15) . . ? C87 C86 C91 123.5(16) . . ? C90 C86 C91 128.0(15) . . ? C87 C86 Th2 77.9(9) . . ? C90 C86 Th2 71.3(10) . . ? C91 C86 Th2 128.0(11) . . ? C88 C87 C86 110.9(16) . . ? C88 C87 Th2 76.5(10) . . ? C86 C87 Th2 74.0(10) . . ? C88 C87 H87 124.5 . . ? C86 C87 H87 124.5 . . ? Th2 C87 H87 116.7 . . ? C87 C88 C89 107.3(15) . . ? C87 C88 C95 128.4(17) . . ? C89 C88 C95 121.6(16) . . ? C87 C88 Th2 76.0(10) . . ? C89 C88 Th2 71.8(10) . . ? C95 C88 Th2 132.2(12) . . ? C88 C89 C90 107.0(15) . . ? C88 C89 Th2 79.8(10) . . ? C90 C89 Th2 72.5(9) . . ? C88 C89 H89 126.5 . . ? C90 C89 H89 126.5 . . ? Th2 C89 H89 113.7 . . ? C86 C90 C89 107.9(15) . . ? C86 C90 Th2 79.9(9) . . ? C89 C90 Th2 77.3(9) . . ? C86 C90 H90 126.0 . . ? C89 C90 H90 126.0 . . ? Th2 C90 H90 109.6 . . ? C92 C91 C93 108.0(15) . . ? C92 C91 C86 115.4(14) . . ? C93 C91 C86 109.8(14) . . ? C92 C91 C94 109.8(16) . . ? C93 C91 C94 107.4(15) . . ? C86 C91 C94 106.1(15) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C91 C94 H94A 109.5 . . ? C91 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C91 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C88 C95 C96 110.8(15) . . ? C88 C95 C97 112.9(16) . . ? C96 C95 C97 111.8(16) . . ? C88 C95 C98 104.4(15) . . ? C96 C95 C98 107.8(16) . . ? C97 C95 C98 108.6(15) . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C95 C97 H97A 109.5 . . ? C95 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C95 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C95 C98 H98A 109.5 . . ? C95 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C95 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C5 N1 C1 120.3(14) . . ? C5 N1 Th1 117.2(10) . . ? C1 N1 Th1 122.0(11) . . ? C6 N2 C10 117.4(13) . . ? C6 N2 Th1 124.6(10) . . ? C10 N2 Th1 116.6(9) . . ? C50 N3 C54 115.5(14) . . ? C50 N3 Th2 123.6(10) . . ? C54 N3 Th2 119.7(10) . . ? C55 N4 C59 120.3(12) . . ? C55 N4 Th2 122.5(10) . . ? C59 N4 Th2 116.9(9) . . ? C11 S1 Th1 104.7(6) . . ? C60 S2 Th2 105.2(5) . . ? N2 Th1 N1 64.5(4) . . ? N2 Th1 C40 108.0(5) . . ? N1 Th1 C40 80.7(5) . . ? N2 Th1 C41 129.3(4) . . ? N1 Th1 C41 107.6(4) . . ? C40 Th1 C41 28.9(5) . . ? N2 Th1 S1 71.9(3) . . ? N1 Th1 S1 133.0(3) . . ? C40 Th1 S1 130.9(4) . . ? C41 Th1 S1 113.3(3) . . ? N2 Th1 C24 106.3(4) . . ? N1 Th1 C24 85.2(4) . . ? C40 Th1 C24 132.3(5) . . ? C41 Th1 C24 123.4(5) . . ? S1 Th1 C24 91.0(3) . . ? N2 Th1 C28 119.0(4) . . ? N1 Th1 C28 113.9(4) . . ? C40 Th1 C28 132.7(5) . . ? C41 Th1 C28 109.9(5) . . ? S1 Th1 C28 72.8(3) . . ? C24 Th1 C28 28.7(4) . . ? N2 Th1 C27 148.1(4) . . ? N1 Th1 C27 120.3(4) . . ? C40 Th1 C27 103.8(5) . . ? C41 Th1 C27 81.2(5) . . ? S1 Th1 C27 88.6(3) . . ? C24 Th1 C27 47.6(4) . . ? C28 Th1 C27 29.2(4) . . ? N2 Th1 C37 113.3(4) . . ? N1 Th1 C37 127.2(4) . . ? C40 Th1 C37 48.3(5) . . ? C41 Th1 C37 29.3(4) . . ? S1 Th1 C37 85.4(3) . . ? C24 Th1 C37 136.7(5) . . ? C28 Th1 C37 111.5(4) . . ? C27 Th1 C37 89.2(4) . . ? N2 Th1 C25 121.9(4) . . ? N1 Th1 C25 75.4(4) . . ? C40 Th1 C25 104.8(5) . . ? C41 Th1 C25 101.2(5) . . ? S1 Th1 C25 116.7(3) . . ? C24 Th1 C25 27.6(4) . . ? C28 Th1 C25 45.5(4) . . ? C27 Th1 C25 45.5(4) . . ? C37 Th1 C25 124.4(5) . . ? N2 Th1 C38 86.6(4) . . ? N1 Th1 C38 107.6(4) . . ? C40 Th1 C38 46.1(5) . . ? C41 Th1 C38 46.2(5) . . ? S1 Th1 C38 85.8(3) . . ? C24 Th1 C38 165.1(5) . . ? C28 Th1 C38 137.5(4) . . ? C27 Th1 C38 117.7(5) . . ? C37 Th1 C38 28.5(4) . . ? C25 Th1 C38 147.2(4) . . ? N2 Th1 C39 83.1(4) . . ? N1 Th1 C39 81.6(4) . . ? C40 Th1 C39 28.5(5) . . ? C41 Th1 C39 46.8(5) . . ? S1 Th1 C39 110.4(3) . . ? C24 Th1 C39 158.5(4) . . ? C28 Th1 C39 156.5(4) . . ? C27 Th1 C39 128.1(4) . . ? C37 Th1 C39 47.6(4) . . ? C25 Th1 C39 131.4(4) . . ? C38 Th1 C39 27.5(4) . . ? N4 Th2 N3 65.3(4) . . ? N4 Th2 C90 127.7(5) . . ? N3 Th2 C90 106.6(4) . . ? N4 Th2 S2 71.4(3) . . ? N3 Th2 S2 131.7(3) . . ? C90 Th2 S2 116.4(4) . . ? N4 Th2 C89 105.5(4) . . ? N3 Th2 C89 78.6(5) . . ? C90 Th2 C89 30.1(4) . . ? S2 Th2 C89 134.7(4) . . ? N4 Th2 C75 120.7(4) . . ? N3 Th2 C75 114.0(4) . . ? C90 Th2 C75 109.9(5) . . ? S2 Th2 C75 71.4(3) . . ? C89 Th2 C75 133.4(5) . . ? N4 Th2 C74 148.7(4) . . ? N3 Th2 C74 120.2(4) . . ? C90 Th2 C74 82.1(5) . . ? S2 Th2 C74 87.5(3) . . ? C89 Th2 C74 105.7(5) . . ? C75 Th2 C74 28.1(4) . . ? N4 Th2 C86 110.9(5) . . ? N3 Th2 C86 124.6(4) . . ? C90 Th2 C86 28.8(4) . . ? S2 Th2 C86 89.7(4) . . ? C89 Th2 C86 47.9(5) . . ? C75 Th2 C86 113.4(5) . . ? C74 Th2 C86 91.3(5) . . ? N4 Th2 C76 108.1(4) . . ? N3 Th2 C76 85.2(4) . . ? C90 Th2 C76 123.2(5) . . ? S2 Th2 C76 88.9(3) . . ? C89 Th2 C76 131.8(5) . . ? C75 Th2 C76 28.9(4) . . ? C74 Th2 C76 47.0(4) . . ? C86 Th2 C76 138.3(4) . . ? N4 Th2 C87 84.2(4) . . ? N3 Th2 C87 106.2(4) . . ? C90 Th2 C87 46.7(5) . . ? S2 Th2 C87 89.2(3) . . ? C89 Th2 C87 46.3(5) . . ? C75 Th2 C87 138.7(4) . . ? C74 Th2 C87 119.3(5) . . ? C86 Th2 C87 28.0(4) . . ? C76 Th2 C87 166.2(4) . . ? N4 Th2 C88 80.7(4) . . ? N3 Th2 C88 80.1(4) . . ? C90 Th2 C88 47.7(5) . . ? S2 Th2 C88 113.3(3) . . ? C89 Th2 C88 28.5(4) . . ? C75 Th2 C88 157.5(4) . . ? C74 Th2 C88 129.9(5) . . ? C86 Th2 C88 46.7(5) . . ? C76 Th2 C88 157.8(5) . . ? C87 Th2 C88 27.5(4) . . ? N4 Th2 C77 123.4(4) . . ? N3 Th2 C77 74.6(4) . . ? C90 Th2 C77 100.4(5) . . ? S2 Th2 C77 115.6(4) . . ? C89 Th2 C77 103.6(5) . . ? C75 Th2 C77 46.3(5) . . ? C74 Th2 C77 46.0(5) . . ? C86 Th2 C77 124.6(5) . . ? C76 Th2 C77 28.3(4) . . ? C87 Th2 C77 146.6(4) . . ? C88 Th2 C77 130.2(5) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.695 _refine_diff_density_min -2.004 _refine_diff_density_rms 0.256 data_compound8 _database_code_depnum_ccdc_archive 'CCDC 860422' #TrackingRef 'compound 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H88 N2 S Th' _chemical_formula_sum 'C69 H88 N2 S Th' _chemical_formula_weight 1209.51 _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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 43.489(3) _cell_length_b 11.0821(8) _cell_length_c 25.3586(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.7940(10) _cell_angle_gamma 90.00 _cell_volume 12078.0(15) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9911 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.58 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4976 _exptl_absorpt_coefficient_mu 2.545 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3105 _exptl_absorpt_correction_T_max 0.4695 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34309 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.69 _reflns_number_total 13896 _reflns_number_gt 11172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+11.4623P] 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 13896 _refine_ls_number_parameters 667 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.18178(8) -0.0698(3) 0.00978(13) 0.0148(7) Uani 1 1 d . . . C2 C 0.17479(8) 0.0553(3) -0.00326(13) 0.0158(7) Uani 1 1 d . . . C3 C 0.19546(7) 0.1244(3) 0.03385(13) 0.0137(7) Uani 1 1 d . . . H3 H 0.1958 0.2101 0.0351 0.016 Uiso 1 1 calc R . . C4 C 0.21541(8) 0.0490(3) 0.06859(13) 0.0147(7) Uani 1 1 d . . . C5 C 0.20514(8) -0.0692(3) 0.05525(13) 0.0140(7) Uani 1 1 d . . . H5 H 0.2129 -0.1394 0.0743 0.017 Uiso 1 1 calc R . . C6 C 0.17831(8) -0.1873(3) -0.02378(13) 0.0152(7) Uani 1 1 d . . . C7 C 0.18194(8) -0.2993(3) 0.01240(13) 0.0183(8) Uani 1 1 d . . . H7A H 0.1669 -0.2953 0.0375 0.027 Uiso 1 1 calc R . . H7B H 0.2031 -0.3018 0.0323 0.027 Uiso 1 1 calc R . . H7C H 0.1781 -0.3721 -0.0095 0.027 Uiso 1 1 calc R . . C8 C 0.14824(8) -0.2064(3) -0.06329(14) 0.0210(8) Uani 1 1 d . . . H8A H 0.1495 -0.2830 -0.0821 0.032 Uiso 1 1 calc R . . H8B H 0.1456 -0.1401 -0.0892 0.032 Uiso 1 1 calc R . . H8C H 0.1304 -0.2082 -0.0438 0.032 Uiso 1 1 calc R . . C9 C 0.20639(8) -0.1876(3) -0.05521(14) 0.0220(8) Uani 1 1 d . . . H9A H 0.2057 -0.2607 -0.0771 0.033 Uiso 1 1 calc R . . H9B H 0.2259 -0.1859 -0.0300 0.033 Uiso 1 1 calc R . . H9C H 0.2053 -0.1163 -0.0783 0.033 Uiso 1 1 calc R . . C10 C 0.15452(8) 0.1161(3) -0.05134(13) 0.0168(7) Uani 1 1 d . . . C11 C 0.12007(8) 0.0805(4) -0.05611(14) 0.0218(8) Uani 1 1 d . . . H11A H 0.1182 -0.0076 -0.0572 0.033 Uiso 1 1 calc R . . H11B H 0.1085 0.1149 -0.0889 0.033 Uiso 1 1 calc R . . H11C H 0.1115 0.1116 -0.0252 0.033 Uiso 1 1 calc R . . C12 C 0.16741(9) 0.0869(4) -0.10312(13) 0.0227(8) Uani 1 1 d . . . H12A H 0.1897 0.1058 -0.0984 0.034 Uiso 1 1 calc R . . H12B H 0.1564 0.1353 -0.1325 0.034 Uiso 1 1 calc R . . H12C H 0.1644 0.0010 -0.1115 0.034 Uiso 1 1 calc R . . C13 C 0.15577(9) 0.2541(3) -0.04635(15) 0.0223(8) Uani 1 1 d . . . H13A H 0.1478 0.2786 -0.0139 0.034 Uiso 1 1 calc R . . H13B H 0.1430 0.2903 -0.0775 0.034 Uiso 1 1 calc R . . H13C H 0.1773 0.2814 -0.0445 0.034 Uiso 1 1 calc R . . C14 C 0.24951(8) 0.0779(3) 0.09057(13) 0.0175(7) Uani 1 1 d . . . C15 C 0.26811(9) 0.0368(4) 0.04601(15) 0.0247(8) Uani 1 1 d . . . H15A H 0.2609 0.0820 0.0132 0.037 Uiso 1 1 calc R . . H15B H 0.2648 -0.0497 0.0393 0.037 Uiso 1 1 calc R . . H15C H 0.2903 0.0521 0.0574 0.037 Uiso 1 1 calc R . . C16 C 0.25584(8) 0.2116(3) 0.09965(15) 0.0223(8) Uani 1 1 d . . . H16A H 0.2505 0.2550 0.0658 0.034 Uiso 1 1 calc R . . H16B H 0.2779 0.2237 0.1134 0.034 Uiso 1 1 calc R . . H16C H 0.2432 0.2423 0.1256 0.034 Uiso 1 1 calc R . . C17 C 0.26212(9) 0.0046(3) 0.14079(15) 0.0244(9) Uani 1 1 d . . . H17A H 0.2846 0.0179 0.1500 0.037 Uiso 1 1 calc R . . H17B H 0.2581 -0.0814 0.1338 0.037 Uiso 1 1 calc R . . H17C H 0.2517 0.0306 0.1705 0.037 Uiso 1 1 calc R . . C18 C 0.13808(8) 0.0598(3) 0.21239(13) 0.0187(8) Uani 1 1 d . . . C19 C 0.16991(8) 0.0980(3) 0.21356(13) 0.0173(8) Uani 1 1 d . . . C20 C 0.18656(8) -0.0069(3) 0.20087(13) 0.0161(7) Uani 1 1 d . . . H20 H 0.2081 -0.0080 0.1978 0.019 Uiso 1 1 calc R . . C21 C 0.16683(8) -0.1080(3) 0.19350(12) 0.0155(7) Uani 1 1 d . . . C22 C 0.13691(8) -0.0648(3) 0.19878(13) 0.0174(7) Uani 1 1 d . . . H22 H 0.1185 -0.1124 0.1939 0.021 Uiso 1 1 calc R . . C23 C 0.11042(9) 0.1221(4) 0.23292(14) 0.0245(9) Uani 1 1 d . . . C24 C 0.11939(9) 0.1482(4) 0.29326(13) 0.0261(9) Uani 1 1 d . . . H24A H 0.1356 0.2106 0.2985 0.039 Uiso 1 1 calc R . . H24B H 0.1273 0.0743 0.3118 0.039 Uiso 1 1 calc R . . H24C H 0.1010 0.1765 0.3077 0.039 Uiso 1 1 calc R . . C25 C 0.09952(10) 0.2392(4) 0.20234(15) 0.0391(12) Uani 1 1 d . . . H25A H 0.0841 0.2192 0.1712 0.059 Uiso 1 1 calc R . . H25B H 0.1174 0.2789 0.1905 0.059 Uiso 1 1 calc R . . H25C H 0.0902 0.2935 0.2259 0.059 Uiso 1 1 calc R . . C26 C 0.08223(9) 0.0395(5) 0.22957(16) 0.0382(12) Uani 1 1 d . . . H26A H 0.0653 0.0818 0.2433 0.057 Uiso 1 1 calc R . . H26B H 0.0878 -0.0331 0.2510 0.057 Uiso 1 1 calc R . . H26C H 0.0754 0.0165 0.1923 0.057 Uiso 1 1 calc R . . C27 C 0.18863(9) 0.2066(3) 0.24026(14) 0.0215(8) Uani 1 1 d . . . C28 C 0.19981(10) 0.1731(4) 0.29915(14) 0.0289(9) Uani 1 1 d . . . H28A H 0.2125 0.2390 0.3168 0.043 Uiso 1 1 calc R . . H28B H 0.2123 0.0993 0.3008 0.043 Uiso 1 1 calc R . . H28C H 0.1817 0.1598 0.3173 0.043 Uiso 1 1 calc R . . C29 C 0.21800(9) 0.2255(4) 0.21457(15) 0.0280(9) Uani 1 1 d . . . H29A H 0.2122 0.2311 0.1757 0.042 Uiso 1 1 calc R . . H29B H 0.2322 0.1572 0.2234 0.042 Uiso 1 1 calc R . . H29C H 0.2284 0.3002 0.2282 0.042 Uiso 1 1 calc R . . C30 C 0.17228(10) 0.3302(4) 0.23735(16) 0.0321(10) Uani 1 1 d . . . H30A H 0.1866 0.3911 0.2552 0.048 Uiso 1 1 calc R . . H30B H 0.1538 0.3254 0.2551 0.048 Uiso 1 1 calc R . . H30C H 0.1660 0.3530 0.1999 0.048 Uiso 1 1 calc R . . C31 C 0.17724(8) -0.2395(3) 0.20018(13) 0.0175(8) Uani 1 1 d . . . C32 C 0.18830(10) -0.2584(4) 0.26076(14) 0.0277(9) Uani 1 1 d . . . H32A H 0.2056 -0.2034 0.2729 0.041 Uiso 1 1 calc R . . H32B H 0.1952 -0.3420 0.2672 0.041 Uiso 1 1 calc R . . H32C H 0.1711 -0.2416 0.2805 0.041 Uiso 1 1 calc R . . C33 C 0.20442(10) -0.2683(4) 0.17021(15) 0.0289(9) Uani 1 1 d . . . H33A H 0.1978 -0.2572 0.1318 0.043 Uiso 1 1 calc R . . H33B H 0.2110 -0.3520 0.1772 0.043 Uiso 1 1 calc R . . H33C H 0.2218 -0.2140 0.1824 0.043 Uiso 1 1 calc R . . C34 C 0.15049(9) -0.3272(3) 0.18257(15) 0.0263(9) Uani 1 1 d . . . H34A H 0.1339 -0.3140 0.2041 0.039 Uiso 1 1 calc R . . H34B H 0.1581 -0.4103 0.1875 0.039 Uiso 1 1 calc R . . H34C H 0.1423 -0.3136 0.1448 0.039 Uiso 1 1 calc R . . C35 C 0.16155(9) 0.3351(3) 0.09238(13) 0.0196(8) Uani 1 1 d . . . H35 H 0.1822 0.3112 0.1062 0.024 Uiso 1 1 calc R . . C36 C 0.15620(9) 0.4536(3) 0.07852(15) 0.0223(8) Uani 1 1 d . . . H36 H 0.1726 0.5109 0.0830 0.027 Uiso 1 1 calc R . . C37 C 0.12587(10) 0.4877(3) 0.05767(16) 0.0276(9) Uani 1 1 d . . . H37 H 0.1214 0.5684 0.0463 0.033 Uiso 1 1 calc R . . C38 C 0.10272(9) 0.4038(3) 0.05379(14) 0.0227(8) Uani 1 1 d . . . H38 H 0.0820 0.4267 0.0401 0.027 Uiso 1 1 calc R . . C39 C 0.10911(8) 0.2842(3) 0.06969(13) 0.0160(7) Uani 1 1 d . . . C40 C 0.08533(8) 0.1912(3) 0.07126(13) 0.0161(7) Uani 1 1 d . . . C41 C 0.05465(9) 0.2257(3) 0.06789(14) 0.0213(8) Uani 1 1 d . . . H41 H 0.0484 0.3055 0.0577 0.026 Uiso 1 1 calc R . . C42 C 0.03245(8) 0.1385(4) 0.08008(14) 0.0221(8) Uani 1 1 d . . . H42 H 0.0116 0.1626 0.0813 0.027 Uiso 1 1 calc R . . C43 C 0.04075(8) 0.0242(4) 0.08964(14) 0.0196(7) Uani 1 1 d . . . H43 H 0.0256 -0.0313 0.0981 0.024 Uiso 1 1 calc R . . C44 C 0.07349(8) -0.0212(3) 0.08751(13) 0.0146(7) Uani 1 1 d . . . H44 H 0.0806 -0.0574 0.1234 0.018 Uiso 1 1 calc R . . C45 C 0.07489(8) -0.1273(3) 0.04680(13) 0.0154(7) Uani 1 1 d . . . C46 C 0.05573(8) -0.2337(3) 0.06436(13) 0.0196(8) Uani 1 1 d . . . C47 C 0.06787(9) -0.3130(4) 0.10465(15) 0.0245(8) Uani 1 1 d . . . H47 H 0.0886 -0.3021 0.1222 0.029 Uiso 1 1 calc R . . C48 C 0.05035(10) -0.4074(4) 0.11962(18) 0.0356(11) Uani 1 1 d . . . H48 H 0.0592 -0.4613 0.1469 0.043 Uiso 1 1 calc R . . C49 C 0.01982(11) -0.4242(4) 0.09503(18) 0.0412(12) Uani 1 1 d . . . H49 H 0.0078 -0.4891 0.1053 0.049 Uiso 1 1 calc R . . C50 C 0.00739(11) -0.3452(5) 0.05565(18) 0.0447(13) Uani 1 1 d . . . H50 H -0.0135 -0.3556 0.0386 0.054 Uiso 1 1 calc R . . C51 C 0.02506(9) -0.2499(4) 0.04045(15) 0.0318(10) Uani 1 1 d . . . H51 H 0.0160 -0.1956 0.0135 0.038 Uiso 1 1 calc R . . C52 C 0.06433(8) -0.1015(3) -0.01219(13) 0.0170(7) Uani 1 1 d . . . C53 C 0.06724(8) -0.1947(4) -0.04848(14) 0.0223(8) Uani 1 1 d . . . H53 H 0.0751 -0.2707 -0.0354 0.027 Uiso 1 1 calc R . . C54 C 0.05890(9) -0.1783(4) -0.10296(15) 0.0285(9) Uani 1 1 d . . . H54 H 0.0615 -0.2425 -0.1267 0.034 Uiso 1 1 calc R . . C55 C 0.04695(9) -0.0699(4) -0.12283(15) 0.0292(9) Uani 1 1 d . . . H55 H 0.0413 -0.0585 -0.1602 0.035 Uiso 1 1 calc R . . C56 C 0.04322(8) 0.0221(4) -0.08785(14) 0.0247(8) Uani 1 1 d . . . H56 H 0.0346 0.0967 -0.1012 0.030 Uiso 1 1 calc R . . C57 C 0.05205(8) 0.0069(3) -0.03265(14) 0.0196(8) Uani 1 1 d . . . H57 H 0.0496 0.0717 -0.0091 0.024 Uiso 1 1 calc R . . C58 C 0.09246(13) 0.3387(4) 0.79909(19) 0.104(3) Uani 1 1 d G . . H58 H 0.0924 0.2888 0.7686 0.124 Uiso 1 1 calc R . . C59 C 0.07311(10) 0.3116(5) 0.8363(3) 0.102(3) Uani 1 1 d G . . H59 H 0.0598 0.2431 0.8313 0.123 Uiso 1 1 calc R . . C60 C 0.07317(12) 0.3846(7) 0.8809(2) 0.127(4) Uani 1 1 d G . . H60 H 0.0599 0.3661 0.9063 0.152 Uiso 1 1 calc R . . C61 C 0.09258(16) 0.4848(5) 0.88824(16) 0.129(5) Uani 1 1 d G . . H61 H 0.0926 0.5347 0.9187 0.155 Uiso 1 1 calc R . . C62 C 0.11193(14) 0.5120(4) 0.8510(2) 0.091(3) Uani 1 1 d G . . H62 H 0.1252 0.5804 0.8561 0.109 Uiso 1 1 calc R . . C63 C 0.11187(11) 0.4389(4) 0.80645(19) 0.096(2) Uani 1 1 d G . . H63 H 0.1251 0.4575 0.7810 0.116 Uiso 1 1 calc R . . C64 C 0.00719(10) 0.9187(5) 0.2274(2) 0.0505(14) Uani 1 1 d . . . H64 H 0.0121 0.9931 0.2120 0.061 Uiso 1 1 calc R . . C65 C 0.01438(12) 0.8118(5) 0.20475(19) 0.0489(13) Uani 1 1 d . . . H65 H 0.0242 0.8117 0.1738 0.059 Uiso 1 1 calc R . . C66 C 0.00711(13) 0.7053(5) 0.22737(19) 0.0545(14) Uani 1 1 d . . . H66 H 0.0119 0.6309 0.2119 0.065 Uiso 1 1 calc R . . C67 C -0.01045(4) 0.3508(2) 0.19376(17) 0.104(4) Uani 0.50 1 d PGU A -1 H67 H -0.0170 0.3494 0.1563 0.125 Uiso 0.50 1 calc PR A -1 C68 C 0.02107(4) 0.3467(2) 0.21412(15) 0.088(3) Uani 0.50 1 d PGU A -1 H68 H 0.0360 0.3425 0.1906 0.106 Uiso 0.50 1 calc PR A -1 C69 C 0.03069(5) 0.3486(2) 0.26897(14) 0.110(3) Uani 0.50 1 d PGU A -1 H69 H 0.0522 0.3458 0.2829 0.132 Uiso 0.50 1 calc PR A -1 C70 C 0.00877(6) 0.3547(3) 0.30346(16) 0.096(3) Uani 0.50 1 d PGU A -1 H70 H 0.0153 0.3560 0.3409 0.116 Uiso 0.50 1 calc PR A -1 C71 C -0.02275(6) 0.3588(3) 0.28309(19) 0.095(3) Uani 0.50 1 d PGU A -1 H71 H -0.0377 0.3629 0.3067 0.114 Uiso 0.50 1 calc PR A -1 C72 C -0.03237(5) 0.3568(3) 0.22824(19) 0.117(4) Uani 0.50 1 d PGU A -1 H72 H -0.0539 0.3596 0.2143 0.140 Uiso 0.50 1 calc PR A -1 N1 N 0.138813(19) 0.250381(18) 0.08737(4) 0.0161(6) Uani 1 1 d G . . N2 N 0.096329(5) 0.07673(6) 0.08213(5) 0.0142(6) Uani 1 1 d G . . S1 S 0.116963(15) -0.16910(4) 0.05477(3) 0.01526(18) Uani 1 1 d G . . Th1 Th 0.151383(3) 0.024931(11) 0.098522(4) 0.01119(4) Uani 1 1 d G . . _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0130(17) 0.0207(18) 0.0116(15) 0.0018(14) 0.0048(13) 0.0004(15) C2 0.0153(17) 0.020(2) 0.0137(16) 0.0023(14) 0.0056(13) -0.0031(14) C3 0.0137(17) 0.0138(17) 0.0140(16) 0.0012(13) 0.0037(13) -0.0014(14) C4 0.0126(17) 0.020(2) 0.0121(16) -0.0002(13) 0.0040(13) 0.0011(13) C5 0.0134(16) 0.0155(17) 0.0141(16) 0.0008(14) 0.0047(13) 0.0011(15) C6 0.0143(17) 0.0203(19) 0.0120(16) -0.0022(14) 0.0052(13) -0.0022(14) C7 0.0224(19) 0.0157(18) 0.0178(17) -0.0032(14) 0.0063(15) -0.0013(15) C8 0.024(2) 0.021(2) 0.0184(18) -0.0032(15) 0.0029(15) -0.0028(16) C9 0.023(2) 0.024(2) 0.0204(18) -0.0024(15) 0.0078(16) 0.0017(16) C10 0.0143(17) 0.0204(19) 0.0151(17) 0.0030(14) 0.0010(14) -0.0016(15) C11 0.0194(19) 0.027(2) 0.0182(18) 0.0062(16) -0.0001(15) -0.0025(17) C12 0.024(2) 0.031(2) 0.0129(17) 0.0058(16) 0.0043(15) -0.0030(17) C13 0.023(2) 0.021(2) 0.0229(19) 0.0068(16) 0.0036(16) -0.0004(16) C14 0.0129(17) 0.0202(18) 0.0188(17) -0.0001(15) 0.0005(14) -0.0025(15) C15 0.0158(18) 0.031(2) 0.028(2) -0.0021(17) 0.0057(15) -0.0006(17) C16 0.0155(19) 0.025(2) 0.026(2) -0.0031(16) 0.0035(15) -0.0059(16) C17 0.0159(18) 0.033(2) 0.0230(19) 0.0008(16) -0.0021(15) 0.0007(16) C18 0.0204(19) 0.028(2) 0.0077(15) 0.0000(14) 0.0012(14) 0.0042(16) C19 0.0202(18) 0.022(2) 0.0097(15) -0.0006(14) 0.0018(14) 0.0044(15) C20 0.0161(17) 0.021(2) 0.0107(15) 0.0024(13) 0.0012(13) 0.0010(14) C21 0.0181(18) 0.0189(19) 0.0089(15) 0.0004(13) 0.0000(13) 0.0015(15) C22 0.0138(17) 0.0259(19) 0.0119(16) 0.0028(15) 0.0004(13) -0.0008(15) C23 0.0200(19) 0.042(2) 0.0118(17) -0.0046(16) 0.0028(15) 0.0104(18) C24 0.025(2) 0.041(3) 0.0130(17) -0.0023(16) 0.0053(15) 0.0068(18) C25 0.040(3) 0.059(3) 0.017(2) -0.002(2) 0.0022(18) 0.031(2) C26 0.019(2) 0.072(4) 0.025(2) -0.017(2) 0.0070(17) 0.004(2) C27 0.028(2) 0.021(2) 0.0149(17) -0.0051(15) 0.0025(15) -0.0025(16) C28 0.035(2) 0.035(2) 0.0153(18) -0.0068(17) -0.0020(17) -0.0046(19) C29 0.029(2) 0.027(2) 0.027(2) -0.0043(17) 0.0041(17) -0.0075(18) C30 0.047(3) 0.022(2) 0.029(2) -0.0038(17) 0.010(2) 0.001(2) C31 0.0208(19) 0.0169(19) 0.0139(16) 0.0051(14) -0.0004(14) 0.0012(15) C32 0.035(2) 0.029(2) 0.0185(19) 0.0057(16) -0.0005(17) 0.0053(18) C33 0.037(2) 0.024(2) 0.027(2) 0.0050(17) 0.0108(18) 0.0087(18) C34 0.031(2) 0.018(2) 0.028(2) 0.0031(16) -0.0017(17) -0.0007(17) C35 0.0229(19) 0.0178(19) 0.0183(18) -0.0034(15) 0.0036(15) 0.0007(15) C36 0.029(2) 0.015(2) 0.0230(18) -0.0023(14) 0.0045(16) -0.0026(15) C37 0.040(2) 0.0140(19) 0.028(2) 0.0042(16) 0.0034(18) 0.0018(17) C38 0.024(2) 0.017(2) 0.0254(19) 0.0016(15) 0.0005(16) 0.0041(16) C39 0.0160(18) 0.0211(19) 0.0104(16) 0.0004(14) 0.0001(13) 0.0025(15) C40 0.0205(19) 0.0151(18) 0.0119(16) 0.0013(13) 0.0001(14) 0.0024(15) C41 0.022(2) 0.020(2) 0.0216(19) 0.0041(15) -0.0003(15) 0.0058(16) C42 0.0143(18) 0.033(2) 0.0188(18) 0.0019(16) 0.0023(15) 0.0045(16) C43 0.0141(17) 0.029(2) 0.0165(17) -0.0009(16) 0.0032(14) -0.0023(17) C44 0.0100(16) 0.0184(17) 0.0155(16) 0.0020(14) 0.0016(13) 0.0011(15) C45 0.0111(17) 0.0197(18) 0.0152(16) 0.0002(14) 0.0019(13) -0.0028(14) C46 0.0207(19) 0.024(2) 0.0146(17) -0.0046(15) 0.0054(15) -0.0056(16) C47 0.020(2) 0.028(2) 0.027(2) 0.0026(17) 0.0068(16) -0.0015(17) C48 0.038(3) 0.029(3) 0.044(3) 0.012(2) 0.022(2) 0.003(2) C49 0.043(3) 0.042(3) 0.043(3) -0.002(2) 0.021(2) -0.026(2) C50 0.037(3) 0.062(3) 0.035(3) 0.003(2) 0.005(2) -0.031(2) C51 0.023(2) 0.049(3) 0.023(2) 0.0067(19) 0.0015(17) -0.016(2) C52 0.0099(16) 0.026(2) 0.0156(17) 0.0013(14) 0.0027(13) -0.0077(14) C53 0.0171(19) 0.032(2) 0.0179(18) -0.0009(16) 0.0025(15) -0.0038(16) C54 0.023(2) 0.046(3) 0.0171(19) -0.0046(18) 0.0045(16) -0.0057(19) C55 0.020(2) 0.053(3) 0.0151(18) 0.0044(19) 0.0029(15) -0.005(2) C56 0.0140(18) 0.040(2) 0.0194(18) 0.0124(18) 0.0000(14) -0.0044(18) C57 0.0093(16) 0.033(2) 0.0169(17) 0.0009(15) 0.0024(13) -0.0037(15) C58 0.135(7) 0.076(5) 0.104(6) -0.011(4) 0.029(5) -0.042(5) C59 0.051(4) 0.128(7) 0.121(7) 0.069(6) -0.006(4) -0.022(4) C60 0.119(8) 0.177(11) 0.099(7) 0.078(7) 0.064(6) 0.086(8) C61 0.238(14) 0.092(7) 0.055(5) 0.015(4) 0.013(6) 0.094(7) C62 0.142(8) 0.049(4) 0.076(5) -0.002(4) 0.000(5) -0.013(4) C63 0.118(7) 0.080(5) 0.099(6) -0.029(5) 0.043(5) -0.022(5) C64 0.021(2) 0.055(3) 0.073(4) 0.019(3) -0.001(2) 0.001(2) C65 0.046(3) 0.063(4) 0.039(3) 0.006(3) 0.010(2) -0.001(3) C66 0.070(4) 0.056(4) 0.041(3) -0.004(2) 0.017(3) 0.004(3) C67 0.101(6) 0.144(7) 0.071(5) -0.009(6) 0.023(5) -0.035(6) C68 0.094(5) 0.120(6) 0.055(5) 0.009(6) 0.024(5) 0.051(6) C69 0.094(5) 0.164(7) 0.074(5) 0.008(6) 0.023(4) 0.061(6) C70 0.093(5) 0.139(6) 0.062(5) -0.001(6) 0.027(4) 0.069(6) C71 0.089(5) 0.131(7) 0.069(5) -0.030(6) 0.026(5) -0.015(6) C72 0.099(5) 0.166(7) 0.088(6) -0.014(6) 0.020(5) -0.029(6) N1 0.0194(16) 0.0150(15) 0.0138(14) 0.0000(12) 0.0018(12) -0.0005(12) N2 0.0126(14) 0.0175(15) 0.0121(13) 0.0020(12) 0.0006(11) 0.0017(12) S1 0.0126(4) 0.0166(4) 0.0164(4) -0.0012(3) 0.0019(3) -0.0019(3) Th1 0.01049(6) 0.01262(6) 0.01043(6) 0.00067(5) 0.00148(4) -0.00023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.415(4) . ? C1 C2 1.446(5) . ? C1 C6 1.550(5) . ? C1 Th1 2.970(3) . ? C2 C3 1.422(5) . ? C2 C10 1.546(5) . ? C2 Th1 2.935(3) . ? C3 C4 1.412(5) . ? C3 Th1 2.923(3) . ? C3 H3 0.9500 . ? C4 C5 1.408(5) . ? C4 C14 1.536(5) . ? C4 Th1 3.008(3) . ? C5 Th1 2.923(3) . ? C5 H5 0.9500 . ? C6 C8 1.536(5) . ? C6 C7 1.537(5) . ? C6 C9 1.557(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C13 1.535(5) . ? C10 C11 1.536(5) . ? C10 C12 1.539(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.517(5) . ? C14 C17 1.540(5) . ? C14 C15 1.555(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C22 1.422(5) . ? C18 C19 1.444(5) . ? C18 C23 1.545(5) . ? C18 Th1 3.055(3) . ? C19 C20 1.432(5) . ? C19 C27 1.550(5) . ? C19 Th1 3.016(3) . ? C20 C21 1.406(5) . ? C20 Th1 2.826(3) . ? C20 H20 0.9500 . ? C21 C22 1.412(5) . ? C21 C31 1.528(5) . ? C21 Th1 2.815(3) . ? C22 Th1 2.887(3) . ? C22 H22 0.9500 . ? C23 C26 1.522(6) . ? C23 C24 1.548(5) . ? C23 C25 1.548(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.534(5) . ? C27 C30 1.540(5) . ? C27 C28 1.544(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C34 1.529(5) . ? C31 C33 1.534(5) . ? C31 C32 1.552(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N1 1.356(4) . ? C35 C36 1.370(5) . ? C35 H35 0.9500 . ? C36 C37 1.396(6) . ? C36 H36 0.9500 . ? C37 C38 1.363(5) . ? C37 H37 0.9500 . ? C38 C39 1.400(5) . ? C38 H38 0.9500 . ? C39 N1 1.354(3) . ? C39 C40 1.465(5) . ? C40 N2 1.369(3) . ? C40 C41 1.378(5) . ? C41 C42 1.432(5) . ? C41 H41 0.9500 . ? C42 C43 1.329(5) . ? C42 H42 0.9500 . ? C43 C44 1.519(5) . ? C43 H43 0.9500 . ? C44 N2 1.491(4) . ? C44 C45 1.572(5) . ? C44 H44 1.0000 . ? C45 C52 1.523(4) . ? C45 C46 1.548(5) . ? C45 S1 1.868(3) . ? C46 C47 1.389(5) . ? C46 C51 1.390(5) . ? C47 C48 1.381(5) . ? C47 H47 0.9500 . ? C48 C49 1.390(6) . ? C48 H48 0.9500 . ? C49 C50 1.375(7) . ? C49 H49 0.9500 . ? C50 C51 1.395(6) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.384(5) . ? C52 C53 1.401(5) . ? C53 C54 1.386(5) . ? C53 H53 0.9500 . ? C54 C55 1.374(6) . ? C54 H54 0.9500 . ? C55 C56 1.377(6) . ? C55 H55 0.9500 . ? C56 C57 1.404(5) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C59 1.3900 . ? C58 C63 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 C61 1.3900 . ? C60 H60 0.9500 . ? C61 C62 1.3900 . ? C61 H61 0.9500 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C65 1.374(7) . ? C64 C64 1.386(10) 2 ? C64 H64 0.9500 . ? C65 C66 1.370(7) . ? C65 H65 0.9500 . ? C66 C66 1.385(9) 2 ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C67 H67 0.9500 . ? C68 C69 1.3900 . ? C68 H68 0.9500 . ? C69 C70 1.3900 . ? C69 H69 0.9500 . ? C70 C71 1.3900 . ? C70 H70 0.9500 . ? C71 C72 1.3900 . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? N1 Th1 2.5639 . ? N2 Th1 2.4353 . ? S1 Th1 2.7545 . ? _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 106.4(3) . . ? C5 C1 C6 116.7(3) . . ? C2 C1 C6 132.8(3) . . ? C5 C1 Th1 74.24(19) . . ? C2 C1 Th1 74.47(18) . . ? C6 C1 Th1 134.1(2) . . ? C3 C2 C1 106.0(3) . . ? C3 C2 C10 120.9(3) . . ? C1 C2 C10 132.3(3) . . ? C3 C2 Th1 75.47(18) . . ? C1 C2 Th1 77.19(18) . . ? C10 C2 Th1 120.7(2) . . ? C4 C3 C2 111.1(3) . . ? C4 C3 Th1 79.61(19) . . ? C2 C3 Th1 76.43(19) . . ? C4 C3 H3 124.5 . . ? C2 C3 H3 124.5 . . ? Th1 C3 H3 111.5 . . ? C5 C4 C3 105.0(3) . . ? C5 C4 C14 122.3(3) . . ? C3 C4 C14 124.7(3) . . ? C5 C4 Th1 72.92(18) . . ? C3 C4 Th1 72.89(19) . . ? C14 C4 Th1 143.8(2) . . ? C4 C5 C1 111.2(3) . . ? C4 C5 Th1 79.65(19) . . ? C1 C5 Th1 77.98(19) . . ? C4 C5 H5 124.4 . . ? C1 C5 H5 124.4 . . ? Th1 C5 H5 110.1 . . ? C8 C6 C7 106.1(3) . . ? C8 C6 C1 118.4(3) . . ? C7 C6 C1 111.0(3) . . ? C8 C6 C9 108.8(3) . . ? C7 C6 C9 106.7(3) . . ? C1 C6 C9 105.4(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 C10 C11 106.5(3) . . ? C13 C10 C12 105.5(3) . . ? C11 C10 C12 110.9(3) . . ? C13 C10 C2 111.1(3) . . ? C11 C10 C2 112.5(3) . . ? C12 C10 C2 110.1(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C4 113.7(3) . . ? C16 C14 C17 110.9(3) . . ? C4 C14 C17 113.1(3) . . ? C16 C14 C15 107.1(3) . . ? C4 C14 C15 104.8(3) . . ? C17 C14 C15 106.7(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C18 C19 106.7(3) . . ? C22 C18 C23 121.0(3) . . ? C19 C18 C23 131.0(3) . . ? C22 C18 Th1 69.67(18) . . ? C19 C18 Th1 74.75(18) . . ? C23 C18 Th1 130.2(2) . . ? C20 C19 C18 105.9(3) . . ? C20 C19 C27 118.6(3) . . ? C18 C19 C27 132.4(3) . . ? C20 C19 Th1 68.54(18) . . ? C18 C19 Th1 77.75(18) . . ? C27 C19 Th1 132.5(2) . . ? C21 C20 C19 110.9(3) . . ? C21 C20 Th1 75.14(18) . . ? C19 C20 Th1 83.32(19) . . ? C21 C20 H20 124.5 . . ? C19 C20 H20 124.5 . . ? Th1 C20 H20 109.2 . . ? C20 C21 C22 105.6(3) . . ? C20 C21 C31 125.5(3) . . ? C22 C21 C31 125.1(3) . . ? C20 C21 Th1 75.99(18) . . ? C22 C21 Th1 78.51(19) . . ? C31 C21 Th1 128.4(2) . . ? C21 C22 C18 110.7(3) . . ? C21 C22 Th1 72.86(19) . . ? C18 C22 Th1 82.8(2) . . ? C21 C22 H22 124.7 . . ? C18 C22 H22 124.7 . . ? Th1 C22 H22 111.7 . . ? C26 C23 C18 112.0(3) . . ? C26 C23 C24 104.3(3) . . ? C18 C23 C24 109.0(3) . . ? C26 C23 C25 107.1(3) . . ? C18 C23 C25 113.6(3) . . ? C24 C23 C25 110.5(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 105.5(3) . . ? C29 C27 C28 106.5(3) . . ? C30 C27 C28 109.6(3) . . ? C29 C27 C19 109.6(3) . . ? C30 C27 C19 117.5(3) . . ? C28 C27 C19 107.6(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C21 C31 C34 112.0(3) . . ? C21 C31 C33 112.4(3) . . ? C34 C31 C33 109.4(3) . . ? C21 C31 C32 106.3(3) . . ? C34 C31 C32 108.1(3) . . ? C33 C31 C32 108.5(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1 C35 C36 123.2(3) . . ? N1 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C35 C36 C37 118.0(4) . . ? C35 C36 H36 121.0 . . ? C37 C36 H36 121.0 . . ? C38 C37 C36 119.2(4) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 120.9(4) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? N1 C39 C38 119.7(3) . . ? N1 C39 C40 116.0(3) . . ? C38 C39 C40 124.3(3) . . ? N2 C40 C41 125.1(3) . . ? N2 C40 C39 115.5(3) . . ? C41 C40 C39 119.0(3) . . ? C40 C41 C42 118.6(3) . . ? C40 C41 H41 120.7 . . ? C42 C41 H41 120.7 . . ? C43 C42 C41 120.6(3) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 122.6(3) . . ? C42 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? N2 C44 C43 113.8(3) . . ? N2 C44 C45 113.0(2) . . ? C43 C44 C45 113.7(3) . . ? N2 C44 H44 105.1 . . ? C43 C44 H44 105.1 . . ? C45 C44 H44 105.1 . . ? C52 C45 C46 109.3(3) . . ? C52 C45 C44 117.9(3) . . ? C46 C45 C44 107.7(3) . . ? C52 C45 S1 107.2(2) . . ? C46 C45 S1 110.0(2) . . ? C44 C45 S1 104.5(2) . . ? C47 C46 C51 118.0(4) . . ? C47 C46 C45 122.2(3) . . ? C51 C46 C45 119.7(3) . . ? C48 C47 C46 121.2(4) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C47 C48 C49 120.5(4) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 118.9(4) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C49 C50 C51 120.7(4) . . ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 . . ? C46 C51 C50 120.7(4) . . ? C46 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C57 C52 C53 117.5(3) . . ? C57 C52 C45 124.9(3) . . ? C53 C52 C45 117.6(3) . . ? C54 C53 C52 121.5(4) . . ? C54 C53 H53 119.2 . . ? C52 C53 H53 119.2 . . ? C55 C54 C53 120.4(4) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 119.1(4) . . ? C54 C55 H55 120.5 . . ? C56 C55 H55 120.5 . . ? C55 C56 C57 120.9(4) . . ? C55 C56 H56 119.6 . . ? C57 C56 H56 119.6 . . ? C52 C57 C56 120.6(3) . . ? C52 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C59 C58 C63 120.0 . . ? C59 C58 H58 120.0 . . ? C63 C58 H58 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C61 120.0 . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C63 C58 120.0 . . ? C62 C63 H63 120.0 . . ? C58 C63 H63 120.0 . . ? C65 C64 C64 120.4(3) . 2 ? C65 C64 H64 119.8 . . ? C64 C64 H64 119.8 2 . ? C66 C65 C64 119.1(5) . . ? C66 C65 H65 120.5 . . ? C64 C65 H65 120.5 . . ? C65 C66 C66 120.5(3) . 2 ? C65 C66 H66 119.7 . . ? C66 C66 H66 119.7 2 . ? C68 C67 C72 120.0 . . ? C68 C67 H67 120.0 . . ? C72 C67 H67 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C69 C70 C71 120.0 . . ? C69 C70 H70 120.0 . . ? C71 C70 H70 120.0 . . ? C70 C71 C72 120.0 . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72 120.0 . . ? C67 C72 H72 120.0 . . ? C39 N1 C35 119.0(2) . . ? C39 N1 Th1 118.88(16) . . ? C35 N1 Th1 121.64(16) . . ? C40 N2 C44 118.4(2) . . ? C40 N2 Th1 123.85(15) . . ? C44 N2 Th1 117.66(13) . . ? C45 S1 Th1 108.23(11) . . ? N2 Th1 N1 64.2 . . ? N2 Th1 S1 69.9 . . ? N1 Th1 S1 128.5 . . ? N2 Th1 C21 111.66(8) . . ? N1 Th1 C21 128.54(7) . . ? S1 Th1 C21 88.86(7) . . ? N2 Th1 C20 124.49(8) . . ? N1 Th1 C20 107.41(7) . . ? S1 Th1 C20 117.20(7) . . ? C21 Th1 C20 28.86(9) . . ? N2 Th1 C22 83.71(7) . . ? N1 Th1 C22 111.16(8) . . ? S1 Th1 C22 84.71(8) . . ? C21 Th1 C22 28.63(9) . . ? C20 Th1 C22 46.27(10) . . ? N2 Th1 C3 121.83(7) . . ? N1 Th1 C3 73.60(7) . . ? S1 Th1 C3 115.54(7) . . ? C21 Th1 C3 125.89(10) . . ? C20 Th1 C3 104.65(10) . . ? C22 Th1 C3 150.92(9) . . ? N2 Th1 C5 147.36(7) . . ? N1 Th1 C5 118.41(7) . . ? S1 Th1 C5 89.24(7) . . ? C21 Th1 C5 91.98(10) . . ? C20 Th1 C5 87.05(10) . . ? C22 Th1 C5 120.15(10) . . ? C3 Th1 C5 45.01(10) . . ? N2 Th1 C2 106.68(7) . . ? N1 Th1 C2 83.58(7) . . ? S1 Th1 C2 88.59(7) . . ? C21 Th1 C2 137.97(10) . . ? C20 Th1 C2 127.59(10) . . ? C22 Th1 C2 164.87(10) . . ? C3 Th1 C2 28.10(9) . . ? C5 Th1 C2 46.04(9) . . ? N2 Th1 C1 119.59(7) . . ? N1 Th1 C1 111.90(7) . . ? S1 Th1 C1 72.33(7) . . ? C21 Th1 C1 112.80(10) . . ? C20 Th1 C1 114.23(10) . . ? C22 Th1 C1 136.68(10) . . ? C3 Th1 C1 45.74(10) . . ? C5 Th1 C1 27.78(9) . . ? C2 Th1 C1 28.35(10) . . ? N2 Th1 C4 149.31(7) . . ? N1 Th1 C4 94.35(7) . . ? S1 Th1 C4 115.76(7) . . ? C21 Th1 C4 98.81(9) . . ? C20 Th1 C4 81.42(10) . . ? C22 Th1 C4 125.98(9) . . ? C3 Th1 C4 27.50(9) . . ? C5 Th1 C4 27.43(9) . . ? C2 Th1 C4 46.29(9) . . ? C1 Th1 C4 45.87(9) . . ? N2 Th1 C19 102.24(7) . . ? N1 Th1 C19 82.29(7) . . ? S1 Th1 C19 130.36(7) . . ? C21 Th1 C19 47.12(10) . . ? C20 Th1 C19 28.14(9) . . ? C22 Th1 C19 45.79(10) . . ? C3 Th1 C19 109.90(9) . . ? C5 Th1 C19 110.38(9) . . ? C2 Th1 C19 137.95(10) . . ? C1 Th1 C19 138.04(9) . . ? C4 Th1 C19 95.71(9) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.365 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.110