# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Marc Walter' _publ_contact_author_email marc.walter@tu-bs.de _publ_section_title ; A bipyridyl thorium metallocene: synthesis, structure and reactivity ; loop_ _publ_author_name M.Walter 'Guo-Fu Zi' 'Wenshan Ren' 'Xuebin Deng' 'Haibin Song' # Attachment '- compound 2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 860416' #TrackingRef '- compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H50 N2 Th' _chemical_formula_sum 'C36 H50 N2 Th' _chemical_formula_weight 742.82 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' N N 0.0061 0.0033 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7014(15) _cell_length_b 17.020(2) _cell_length_c 16.704(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.876(2) _cell_angle_gamma 90.00 _cell_volume 3295.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4434 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 24.96 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 4.550 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3730 _exptl_absorpt_correction_T_max 0.5118 _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 19214 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.65 _reflns_number_total 7514 _reflns_number_gt 5281 _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^)+(0.0313P)^2^+29.8999P] 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 7514 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1833(8) 0.0905(5) 0.5491(6) 0.041(2) Uani 1 1 d . . . H1 H 0.1586 0.0525 0.5848 0.050 Uiso 1 1 calc R . . C2 C 0.1951(9) 0.0677(6) 0.4739(6) 0.057(3) Uani 1 1 d . . . H2 H 0.1758 0.0156 0.4564 0.068 Uiso 1 1 calc R . . C3 C 0.2367(11) 0.1222(7) 0.4210(6) 0.070(4) Uani 1 1 d . . . H3 H 0.2535 0.1059 0.3695 0.084 Uiso 1 1 calc R . . C4 C 0.2522(9) 0.1975(7) 0.4444(6) 0.060(3) Uani 1 1 d . . . H4 H 0.2835 0.2338 0.4101 0.072 Uiso 1 1 calc R . . C5 C 0.2223(8) 0.2241(5) 0.5202(5) 0.041(2) Uani 1 1 d . . . C6 C 0.2045(7) 0.3031(5) 0.5374(5) 0.039(2) Uani 1 1 d . . . C7 C 0.2068(8) 0.3665(6) 0.4799(6) 0.050(2) Uani 1 1 d . . . H7 H 0.2396 0.3579 0.4317 0.060 Uiso 1 1 calc R . . C8 C 0.1630(9) 0.4374(6) 0.4941(7) 0.058(3) Uani 1 1 d . . . H8 H 0.1617 0.4776 0.4545 0.070 Uiso 1 1 calc R . . C9 C 0.1191(9) 0.4524(6) 0.5668(7) 0.058(3) Uani 1 1 d . . . H9 H 0.0824 0.5009 0.5753 0.069 Uiso 1 1 calc R . . C10 C 0.1307(8) 0.3961(5) 0.6242(6) 0.045(2) Uani 1 1 d . . . H10 H 0.1031 0.4073 0.6739 0.054 Uiso 1 1 calc R . . C11 C 0.1504(7) 0.2649(5) 0.8015(5) 0.0344(17) Uani 1 1 d . . . H11 H 0.1128 0.3144 0.7955 0.041 Uiso 1 1 calc R . . C12 C 0.1054(6) 0.1948(5) 0.7650(4) 0.0300(17) Uani 1 1 d . . . C13 C 0.1904(7) 0.1369(5) 0.7865(5) 0.0362(19) Uani 1 1 d . . . H13 H 0.1861 0.0836 0.7694 0.043 Uiso 1 1 calc R . . C14 C 0.2832(8) 0.1713(5) 0.8375(5) 0.039(2) Uani 1 1 d . . . H14 H 0.3510 0.1447 0.8608 0.046 Uiso 1 1 calc R . . C15 C 0.2591(7) 0.2518(5) 0.8484(5) 0.038(2) Uani 1 1 d . . . C16 C 0.5218(7) 0.2923(5) 0.6546(6) 0.040(2) Uani 1 1 d . . . C17 C 0.5350(8) 0.2798(5) 0.7422(6) 0.047(2) Uani 1 1 d . . . H17 H 0.5433 0.3198 0.7822 0.057 Uiso 1 1 calc R . . C18 C 0.5335(7) 0.1990(6) 0.7568(6) 0.042(2) Uani 1 1 d . . . H18 H 0.5411 0.1747 0.8085 0.051 Uiso 1 1 calc R . . C19 C 0.5184(7) 0.1587(5) 0.6802(5) 0.0350(19) Uani 1 1 d . . . C20 C 0.5119(8) 0.2174(6) 0.6223(6) 0.048(2) Uani 1 1 d . . . H20 H 0.5017 0.2072 0.5658 0.057 Uiso 1 1 calc R . . C21 C 0.5400(8) 0.3725(5) 0.6196(6) 0.043(2) Uani 1 1 d . . . C22 C 0.4505(9) 0.4317(5) 0.6395(7) 0.055(3) Uani 1 1 d . . . H22A H 0.4554 0.4371 0.6983 0.082 Uiso 1 1 calc R . . H22B H 0.3732 0.4134 0.6173 0.082 Uiso 1 1 calc R . . H22C H 0.4653 0.4828 0.6157 0.082 Uiso 1 1 calc R . . C23 C 0.6592(10) 0.3997(7) 0.6446(10) 0.095(5) Uani 1 1 d . . . H23A H 0.6735 0.4040 0.7036 0.142 Uiso 1 1 calc R . . H23B H 0.6698 0.4512 0.6204 0.142 Uiso 1 1 calc R . . H23C H 0.7134 0.3620 0.6263 0.142 Uiso 1 1 calc R . . C24 C 0.5203(11) 0.3629(7) 0.5244(6) 0.068(3) Uani 1 1 d . . . H24A H 0.5284 0.4142 0.4990 0.102 Uiso 1 1 calc R . . H24B H 0.4426 0.3423 0.5072 0.102 Uiso 1 1 calc R . . H24C H 0.5776 0.3264 0.5080 0.102 Uiso 1 1 calc R . . C25 C 0.5254(8) 0.0710(5) 0.6761(6) 0.040(2) Uani 1 1 d . . . C26 C 0.5122(12) 0.0482(6) 0.5845(7) 0.076(4) Uani 1 1 d . . . H26A H 0.5797 0.0666 0.5611 0.114 Uiso 1 1 calc R . . H26B H 0.4424 0.0727 0.5560 0.114 Uiso 1 1 calc R . . H26C H 0.5061 -0.0091 0.5791 0.114 Uiso 1 1 calc R . . C27 C 0.6360(10) 0.0399(7) 0.7165(10) 0.096(5) Uani 1 1 d . . . H27A H 0.6989 0.0584 0.6882 0.143 Uiso 1 1 calc R . . H27B H 0.6339 -0.0176 0.7156 0.143 Uiso 1 1 calc R . . H27C H 0.6489 0.0583 0.7727 0.143 Uiso 1 1 calc R . . C28 C 0.4266(9) 0.0295(5) 0.7069(7) 0.055(3) Uani 1 1 d . . . H28A H 0.4333 -0.0272 0.6985 0.082 Uiso 1 1 calc R . . H28B H 0.3535 0.0484 0.6774 0.082 Uiso 1 1 calc R . . H28C H 0.4284 0.0403 0.7647 0.082 Uiso 1 1 calc R . . C29 C 0.3219(8) 0.3088(6) 0.9072(6) 0.048(2) Uani 1 1 d . . . C30 C 0.2478(10) 0.3274(7) 0.9723(6) 0.069(3) Uani 1 1 d . . . H30A H 0.1756 0.3519 0.9477 0.104 Uiso 1 1 calc R . . H30B H 0.2892 0.3636 1.0117 0.104 Uiso 1 1 calc R . . H30C H 0.2304 0.2787 0.9996 0.104 Uiso 1 1 calc R . . C31 C 0.4371(9) 0.2756(6) 0.9462(6) 0.060(3) Uani 1 1 d . . . H31A H 0.4236 0.2283 0.9772 0.089 Uiso 1 1 calc R . . H31B H 0.4774 0.3150 0.9825 0.089 Uiso 1 1 calc R . . H31C H 0.4844 0.2621 0.9042 0.089 Uiso 1 1 calc R . . C32 C 0.3447(10) 0.3854(6) 0.8631(7) 0.067(3) Uani 1 1 d . . . H32A H 0.3907 0.3738 0.8197 0.101 Uiso 1 1 calc R . . H32B H 0.3868 0.4222 0.9014 0.101 Uiso 1 1 calc R . . H32C H 0.2710 0.4088 0.8400 0.101 Uiso 1 1 calc R . . C33 C -0.0199(7) 0.1817(5) 0.7289(5) 0.037(2) Uani 1 1 d . . . C34 C -0.0855(8) 0.1690(7) 0.8011(6) 0.063(3) Uani 1 1 d . . . H34A H -0.0522 0.1241 0.8330 0.095 Uiso 1 1 calc R . . H34B H -0.1668 0.1583 0.7816 0.095 Uiso 1 1 calc R . . H34C H -0.0795 0.2162 0.8349 0.095 Uiso 1 1 calc R . . C35 C -0.0694(9) 0.2520(6) 0.6820(7) 0.064(3) Uani 1 1 d . . . H35A H -0.0662 0.2977 0.7180 0.097 Uiso 1 1 calc R . . H35B H -0.1498 0.2414 0.6597 0.097 Uiso 1 1 calc R . . H35C H -0.0245 0.2628 0.6378 0.097 Uiso 1 1 calc R . . C36 C -0.0352(8) 0.1092(6) 0.6761(5) 0.049(2) Uani 1 1 d . . . H36A H 0.0101 0.1148 0.6312 0.073 Uiso 1 1 calc R . . H36B H -0.1169 0.1030 0.6546 0.073 Uiso 1 1 calc R . . H36C H -0.0087 0.0629 0.7082 0.073 Uiso 1 1 calc R . . N1 N 0.2046(6) 0.1655(4) 0.5777(4) 0.0349(16) Uani 1 1 d . . . N2 N 0.1791(6) 0.3243(4) 0.6157(4) 0.0378(16) Uani 1 1 d . . . Th1 Th 0.30269(3) 0.233725(17) 0.686762(19) 0.03156(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.047(5) 0.028(4) 0.048(6) -0.005(4) 0.005(4) 0.001(4) C2 0.070(7) 0.048(6) 0.050(6) -0.021(5) -0.003(5) 0.016(5) C3 0.104(10) 0.077(8) 0.032(6) -0.012(5) 0.024(6) 0.042(7) C4 0.074(7) 0.069(7) 0.043(6) 0.006(5) 0.029(5) 0.026(6) C5 0.048(5) 0.039(5) 0.040(5) 0.002(4) 0.023(4) 0.006(4) C6 0.038(5) 0.041(5) 0.042(5) 0.007(4) 0.014(4) 0.004(4) C7 0.047(6) 0.052(6) 0.054(6) 0.015(5) 0.018(5) 0.003(5) C8 0.047(6) 0.051(6) 0.076(8) 0.027(6) 0.002(5) 0.001(5) C9 0.068(7) 0.035(5) 0.067(7) 0.004(5) -0.001(6) 0.015(5) C10 0.050(6) 0.029(4) 0.056(6) -0.006(4) 0.010(5) 0.000(4) C11 0.039(4) 0.033(4) 0.031(4) 0.001(4) 0.003(3) 0.008(4) C12 0.024(4) 0.043(5) 0.024(4) -0.002(3) 0.008(3) 0.002(3) C13 0.038(5) 0.028(4) 0.043(5) 0.000(4) 0.008(4) -0.001(4) C14 0.040(5) 0.034(5) 0.040(5) 0.006(4) 0.000(4) 0.005(4) C15 0.040(5) 0.037(5) 0.036(5) 0.001(4) 0.000(4) 0.002(4) C16 0.032(5) 0.029(4) 0.060(6) -0.001(4) 0.013(4) -0.005(4) C17 0.056(6) 0.040(6) 0.047(6) 0.000(4) 0.008(4) 0.000(4) C18 0.041(5) 0.043(5) 0.042(5) 0.002(4) 0.002(4) 0.003(4) C19 0.031(4) 0.026(4) 0.050(5) 0.005(4) 0.014(4) 0.007(3) C20 0.036(5) 0.062(7) 0.047(6) 0.007(5) 0.014(4) 0.005(4) C21 0.049(5) 0.030(5) 0.050(6) 0.010(4) 0.007(4) -0.014(4) C22 0.062(7) 0.033(5) 0.070(7) 0.008(5) 0.009(5) -0.002(5) C23 0.056(8) 0.054(7) 0.170(15) 0.023(8) 0.000(8) -0.026(6) C24 0.089(9) 0.059(7) 0.061(7) 0.017(6) 0.026(6) -0.001(6) C25 0.039(5) 0.029(4) 0.056(6) 0.003(4) 0.019(4) 0.007(4) C26 0.110(11) 0.045(6) 0.079(9) -0.006(6) 0.040(8) 0.003(6) C27 0.045(7) 0.049(7) 0.185(16) -0.011(8) -0.013(8) 0.016(6) C28 0.054(6) 0.034(5) 0.077(8) 0.011(5) 0.008(5) 0.000(4) C29 0.049(6) 0.046(6) 0.047(6) -0.011(4) -0.002(4) -0.002(4) C30 0.062(7) 0.090(9) 0.054(7) -0.037(6) 0.001(5) -0.003(6) C31 0.050(6) 0.064(7) 0.058(7) -0.008(5) -0.017(5) -0.001(5) C32 0.070(8) 0.038(6) 0.086(9) -0.012(5) -0.015(6) -0.006(5) C33 0.031(4) 0.053(5) 0.030(4) -0.007(4) 0.010(3) -0.002(4) C34 0.034(5) 0.109(10) 0.049(6) -0.017(6) 0.014(5) -0.014(6) C35 0.038(5) 0.072(8) 0.076(8) -0.004(6) -0.015(5) 0.002(5) C36 0.043(5) 0.067(7) 0.038(5) -0.006(5) 0.012(4) -0.015(5) N1 0.044(4) 0.029(4) 0.034(4) 0.001(3) 0.012(3) 0.004(3) N2 0.044(4) 0.028(4) 0.044(4) 0.001(3) 0.013(3) 0.003(3) Th1 0.02854(15) 0.02378(14) 0.04373(18) -0.00337(15) 0.00989(11) 0.00220(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.341(12) . ? C1 N1 1.374(10) . ? C1 H1 0.9500 . ? C2 C3 1.413(16) . ? C2 H2 0.9500 . ? C3 C4 1.346(15) . ? C3 H3 0.9500 . ? C4 C5 1.432(12) . ? C4 H4 0.9500 . ? C5 C6 1.396(12) . ? C5 N1 1.420(10) . ? C5 Th1 2.817(9) . ? C6 N2 1.426(11) . ? C6 C7 1.447(12) . ? C6 Th1 2.855(9) . ? C7 C8 1.344(14) . ? C7 H7 0.9500 . ? C8 C9 1.406(15) . ? C8 H8 0.9500 . ? C9 C10 1.349(13) . ? C9 H9 0.9500 . ? C10 N2 1.363(10) . ? C10 H10 0.9500 . ? C11 C12 1.409(11) . ? C11 C15 1.417(12) . ? C11 Th1 2.840(8) . ? C11 H11 0.9500 . ? C12 C13 1.411(11) . ? C12 C33 1.523(11) . ? C12 Th1 2.882(7) . ? C13 C14 1.412(12) . ? C13 Th1 2.796(8) . ? C13 H13 0.9500 . ? C14 C15 1.414(11) . ? C14 Th1 2.771(8) . ? C14 H14 0.9500 . ? C15 C29 1.500(12) . ? C15 Th1 2.831(9) . ? C16 C20 1.383(13) . ? C16 C17 1.465(13) . ? C16 C21 1.512(11) . ? C16 Th1 2.869(8) . ? C17 C18 1.398(12) . ? C17 Th1 2.859(10) . ? C17 H17 0.9500 . ? C18 C19 1.441(12) . ? C18 Th1 2.854(9) . ? C18 H18 0.9500 . ? C19 C20 1.385(12) . ? C19 C25 1.497(11) . ? C19 Th1 2.844(8) . ? C20 Th1 2.820(9) . ? C20 H20 0.9500 . ? C21 C23 1.474(14) . ? C21 C22 1.523(13) . ? C21 C24 1.583(14) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.473(13) . ? C25 C28 1.505(12) . ? C25 C26 1.566(14) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.515(14) . ? C29 C31 1.523(13) . ? C29 C32 1.538(14) . ? 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 1.501(13) . ? C33 C36 1.513(12) . ? C33 C34 1.531(12) . ? 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 . ? N1 Th1 2.326(7) . ? N2 Th1 2.325(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 123.9(9) . . ? C2 C1 H1 118.1 . . ? N1 C1 H1 118.1 . . ? C1 C2 C3 119.0(9) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.2(9) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 121.3(10) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 N1 119.9(7) . . ? C6 C5 C4 123.2(8) . . ? N1 C5 C4 116.9(8) . . ? C6 C5 Th1 77.3(5) . . ? N1 C5 Th1 55.4(4) . . ? C4 C5 Th1 143.4(7) . . ? C5 C6 N2 119.2(7) . . ? C5 C6 C7 124.4(8) . . ? N2 C6 C7 116.4(8) . . ? C5 C6 Th1 74.2(5) . . ? N2 C6 Th1 54.1(4) . . ? C7 C6 Th1 147.8(7) . . ? C8 C7 C6 120.7(9) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 120.6(9) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 118.1(9) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 N2 124.5(9) . . ? C9 C10 H10 117.8 . . ? N2 C10 H10 117.8 . . ? C12 C11 C15 111.1(7) . . ? C12 C11 Th1 77.4(4) . . ? C15 C11 Th1 75.2(5) . . ? C12 C11 H11 124.5 . . ? C15 C11 H11 124.5 . . ? Th1 C11 H11 114.8 . . ? C11 C12 C13 105.8(7) . . ? C11 C12 C33 125.2(7) . . ? C13 C12 C33 127.3(8) . . ? C11 C12 Th1 74.1(4) . . ? C13 C12 Th1 72.3(4) . . ? C33 C12 Th1 129.9(5) . . ? C12 C13 C14 108.6(7) . . ? C12 C13 Th1 79.0(5) . . ? C14 C13 Th1 74.3(5) . . ? C12 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? Th1 C13 H13 113.3 . . ? C13 C14 C15 109.3(7) . . ? C13 C14 Th1 76.3(5) . . ? C15 C14 Th1 77.8(5) . . ? C13 C14 H14 125.4 . . ? C15 C14 H14 125.4 . . ? Th1 C14 H14 112.8 . . ? C14 C15 C11 105.1(7) . . ? C14 C15 C29 128.5(8) . . ? C11 C15 C29 125.6(8) . . ? C14 C15 Th1 73.0(5) . . ? C11 C15 Th1 75.9(5) . . ? C29 C15 Th1 124.0(6) . . ? C20 C16 C17 104.4(8) . . ? C20 C16 C21 133.6(9) . . ? C17 C16 C21 121.1(8) . . ? C20 C16 Th1 74.0(5) . . ? C17 C16 Th1 74.8(5) . . ? C21 C16 Th1 124.3(6) . . ? C18 C17 C16 108.4(8) . . ? C18 C17 Th1 75.6(5) . . ? C16 C17 Th1 75.6(5) . . ? C18 C17 H17 125.8 . . ? C16 C17 H17 125.8 . . ? Th1 C17 H17 115.1 . . ? C17 C18 C19 108.4(8) . . ? C17 C18 Th1 76.0(5) . . ? C19 C18 Th1 75.0(5) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? Th1 C18 H18 115.3 . . ? C20 C19 C18 105.4(8) . . ? C20 C19 C25 133.3(9) . . ? C18 C19 C25 120.9(8) . . ? C20 C19 Th1 74.9(5) . . ? C18 C19 Th1 75.7(5) . . ? C25 C19 Th1 120.2(5) . . ? C16 C20 C19 113.5(9) . . ? C16 C20 Th1 77.9(5) . . ? C19 C20 Th1 76.8(5) . . ? C16 C20 H20 123.3 . . ? C19 C20 H20 123.3 . . ? Th1 C20 H20 113.5 . . ? C23 C21 C16 110.7(8) . . ? C23 C21 C22 112.4(9) . . ? C16 C21 C22 112.0(8) . . ? C23 C21 C24 108.6(10) . . ? C16 C21 C24 106.7(8) . . ? C22 C21 C24 106.1(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C19 112.8(8) . . ? C27 C25 C28 110.1(9) . . ? C19 C25 C28 113.8(7) . . ? C27 C25 C26 108.7(9) . . ? C19 C25 C26 107.0(8) . . ? C28 C25 C26 103.8(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C15 C29 C30 109.1(8) . . ? C15 C29 C31 111.4(8) . . ? C30 C29 C31 109.3(9) . . ? C15 C29 C32 109.6(8) . . ? C30 C29 C32 108.7(9) . . ? C31 C29 C32 108.6(9) . . ? 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 C36 109.8(8) . . ? C35 C33 C12 111.9(7) . . ? C36 C33 C12 112.4(7) . . ? C35 C33 C34 108.9(8) . . ? C36 C33 C34 108.1(8) . . ? C12 C33 C34 105.6(7) . . ? 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 . . ? C1 N1 C5 117.0(7) . . ? C1 N1 Th1 141.5(6) . . ? C5 N1 Th1 94.4(5) . . ? C10 N2 C6 117.7(7) . . ? C10 N2 Th1 141.2(6) . . ? C6 N2 Th1 96.2(5) . . ? N2 Th1 N1 74.1(2) . . ? N2 Th1 C14 126.5(3) . . ? N1 Th1 C14 115.3(2) . . ? N2 Th1 C13 112.6(2) . . ? N1 Th1 C13 87.2(2) . . ? C14 Th1 C13 29.4(2) . . ? N2 Th1 C5 55.5(2) . . ? N1 Th1 C5 30.2(2) . . ? C14 Th1 C5 144.8(3) . . ? C13 Th1 C5 115.7(3) . . ? N2 Th1 C20 112.5(3) . . ? N1 Th1 C20 90.7(3) . . ? C14 Th1 C20 119.6(3) . . ? C13 Th1 C20 132.3(3) . . ? C5 Th1 C20 78.9(3) . . ? N2 Th1 C15 103.6(2) . . ? N1 Th1 C15 131.8(2) . . ? C14 Th1 C15 29.2(2) . . ? C13 Th1 C15 48.3(2) . . ? C5 Th1 C15 150.3(2) . . ? C20 Th1 C15 130.8(3) . . ? N2 Th1 C11 79.5(2) . . ? N1 Th1 C11 109.5(2) . . ? C14 Th1 C11 47.2(2) . . ? C13 Th1 C11 47.0(2) . . ? C5 Th1 C11 121.5(2) . . ? C20 Th1 C11 159.0(3) . . ? C15 Th1 C11 28.9(2) . . ? N2 Th1 C19 140.4(2) . . ? N1 Th1 C19 95.2(2) . . ? C14 Th1 C19 92.7(3) . . ? C13 Th1 C19 104.5(2) . . ? C5 Th1 C19 96.5(3) . . ? C20 Th1 C19 28.3(2) . . ? C15 Th1 C19 111.2(2) . . ? C11 Th1 C19 138.8(2) . . ? N2 Th1 C18 146.5(3) . . ? N1 Th1 C18 123.7(2) . . ? C14 Th1 C18 74.9(3) . . ? C13 Th1 C18 97.4(3) . . ? C5 Th1 C18 124.2(3) . . ? C20 Th1 C18 46.7(3) . . ? C15 Th1 C18 85.2(3) . . ? C11 Th1 C18 114.1(2) . . ? C19 Th1 C18 29.3(2) . . ? N2 Th1 C6 29.8(2) . . ? N1 Th1 C6 55.0(2) . . ? C14 Th1 C6 151.5(2) . . ? C13 Th1 C6 126.8(2) . . ? C5 Th1 C6 28.5(2) . . ? C20 Th1 C6 88.5(3) . . ? C15 Th1 C6 133.2(2) . . ? C11 Th1 C6 107.3(2) . . ? C19 Th1 C6 113.9(2) . . ? C18 Th1 C6 133.5(3) . . ? N2 Th1 C17 118.7(3) . . ? N1 Th1 C17 137.4(3) . . ? C14 Th1 C17 90.2(3) . . ? C13 Th1 C17 118.2(3) . . ? C5 Th1 C17 120.7(3) . . ? C20 Th1 C17 46.7(3) . . ? C15 Th1 C17 87.1(3) . . ? C11 Th1 C17 112.8(3) . . ? C19 Th1 C17 47.6(3) . . ? C18 Th1 C17 28.3(2) . . ? C6 Th1 C17 114.8(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 4.873 _refine_diff_density_min -3.022 _refine_diff_density_rms 0.178 # Attachment '- compound 3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 860417' #TrackingRef '- compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H42 Br2 Th' _chemical_formula_sum 'C26 H42 Br2 Th' _chemical_formula_weight 746.46 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' Br Br -0.2901 2.4595 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.672(3) _cell_length_b 16.500(2) _cell_length_c 8.6722(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.197(3) _cell_angle_gamma 90.00 _cell_volume 2786.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1390 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 20.09 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 8.230 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1915 _exptl_absorpt_correction_T_max 0.5589 _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 14047 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5052 _reflns_number_gt 3568 _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^)+(0.0207P)^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 5052 _refine_ls_number_parameters 279 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.982 _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 Br1 Br 0.30500(5) 0.61826(6) 1.02719(11) 0.0457(3) Uani 1 1 d . . . Br2 Br 0.22480(5) 0.38327(6) 1.07228(10) 0.0373(3) Uani 1 1 d . . . C1 C 0.3766(5) 0.2730(5) 0.9342(10) 0.037(2) Uani 1 1 d . . . H1A H 0.4053 0.2378 1.0076 0.055 Uiso 1 1 calc R . . H1B H 0.3705 0.2483 0.8304 0.055 Uiso 1 1 calc R . . H1C H 0.3316 0.2801 0.9688 0.055 Uiso 1 1 calc R . . C2 C 0.4190(4) 0.3946(5) 1.0894(9) 0.035(2) Uani 1 1 d . . . H2A H 0.3734 0.4059 1.1175 0.053 Uiso 1 1 calc R . . H2B H 0.4447 0.4454 1.0879 0.053 Uiso 1 1 calc R . . H2C H 0.4438 0.3577 1.1661 0.053 Uiso 1 1 calc R . . C3 C 0.4827(4) 0.3438(6) 0.8792(10) 0.040(3) Uani 1 1 d . . . H3A H 0.5105 0.3090 0.9554 0.060 Uiso 1 1 calc R . . H3B H 0.5051 0.3966 0.8752 0.060 Uiso 1 1 calc R . . H3C H 0.4781 0.3182 0.7762 0.060 Uiso 1 1 calc R . . C4 C 0.4112(4) 0.3553(5) 0.9276(9) 0.026(2) Uani 1 1 d . . . C5 C 0.3705(4) 0.4115(5) 0.8067(9) 0.024(2) Uani 1 1 d . . . C6 C 0.3862(4) 0.4926(5) 0.7808(9) 0.0231(19) Uani 1 1 d . . . H6 H 0.4179 0.5244 0.8482 0.028 Uiso 1 1 calc R . . C7 C 0.3486(4) 0.5203(5) 0.6413(9) 0.027(2) Uani 1 1 d . A . C8 C 0.3593(5) 0.5996(6) 0.5592(9) 0.034(2) Uani 1 1 d D . . C9 C 0.3860(5) 0.6681(6) 0.6743(11) 0.053(3) Uani 1 1 d U A . H9A H 0.3517 0.6798 0.7427 0.080 Uiso 1 1 calc R . . H9B H 0.3944 0.7171 0.6157 0.080 Uiso 1 1 calc R . . H9C H 0.4290 0.6509 0.7373 0.080 Uiso 1 1 calc R . . C10 C 0.4228(19) 0.590(2) 0.477(6) 0.043(5) Uani 0.49(9) 1 d PDU A 1 H10A H 0.4134 0.5503 0.3928 0.065 Uiso 0.49(9) 1 calc PR A 1 H10B H 0.4618 0.5719 0.5518 0.065 Uiso 0.49(9) 1 calc PR A 1 H10C H 0.4339 0.6425 0.4328 0.065 Uiso 0.49(9) 1 calc PR A 1 C10A C 0.406(2) 0.579(2) 0.434(5) 0.043(5) Uani 0.51(9) 1 d PDU A 2 H10D H 0.3836 0.5372 0.3629 0.065 Uiso 0.51(9) 1 calc PR A 2 H10E H 0.4503 0.5580 0.4849 0.065 Uiso 0.51(9) 1 calc PR A 2 H10F H 0.4136 0.6275 0.3741 0.065 Uiso 0.51(9) 1 calc PR A 2 C11 C 0.2951(5) 0.6301(6) 0.4605(10) 0.040(3) Uani 1 1 d . A . H11A H 0.2773 0.5882 0.3854 0.060 Uiso 1 1 calc R . . H11B H 0.3059 0.6790 0.4045 0.060 Uiso 1 1 calc R . . H11C H 0.2604 0.6429 0.5275 0.060 Uiso 1 1 calc R . . C12 C 0.3080(4) 0.4548(5) 0.5785(9) 0.027(2) Uani 1 1 d . . . H12 H 0.2774 0.4555 0.4834 0.032 Uiso 1 1 calc R A . C13 C 0.3203(4) 0.3876(5) 0.6797(8) 0.024(2) Uani 1 1 d . A . H13 H 0.2989 0.3360 0.6658 0.029 Uiso 1 1 calc R . . C14 C 0.0196(4) 0.6287(5) 0.9333(9) 0.032(2) Uani 1 1 d . . . H14A H 0.0033 0.6569 1.0206 0.048 Uiso 1 1 calc R . . H14B H 0.0005 0.5738 0.9248 0.048 Uiso 1 1 calc R . . H14C H 0.0046 0.6584 0.8366 0.048 Uiso 1 1 calc R . . C15 C 0.1268(5) 0.7094(5) 0.9590(10) 0.036(2) Uani 1 1 d . . . H15A H 0.1125 0.7340 0.8567 0.055 Uiso 1 1 calc R . . H15B H 0.1771 0.7067 0.9792 0.055 Uiso 1 1 calc R . . H15C H 0.1100 0.7423 1.0397 0.055 Uiso 1 1 calc R . . C16 C 0.1208(5) 0.5853(5) 1.1232(9) 0.034(2) Uani 1 1 d . . . H16A H 0.1711 0.5826 1.1420 0.051 Uiso 1 1 calc R . . H16B H 0.1019 0.5304 1.1252 0.051 Uiso 1 1 calc R . . H16C H 0.1044 0.6182 1.2044 0.051 Uiso 1 1 calc R . . C17 C 0.0972(4) 0.6243(4) 0.9612(9) 0.0212(19) Uani 1 1 d . A . C18 C 0.1209(4) 0.5732(4) 0.8327(9) 0.0185(18) Uani 1 1 d . . . C19 C 0.1042(3) 0.4897(4) 0.8035(8) 0.0132(16) Uani 1 1 d . A . H19 H 0.0848 0.4550 0.8732 0.016 Uiso 1 1 calc R . . C20 C 0.1204(4) 0.4661(4) 0.6572(8) 0.0163(18) Uani 1 1 d . . . C21 C 0.1015(4) 0.3850(5) 0.5754(8) 0.0203(19) Uani 1 1 d . A . C22 C 0.1235(5) 0.3135(5) 0.6845(9) 0.034(2) Uani 1 1 d . . . H22A H 0.1092 0.2625 0.6314 0.052 Uiso 1 1 calc R A . H22B H 0.1017 0.3184 0.7789 0.052 Uiso 1 1 calc R . . H22C H 0.1735 0.3139 0.7128 0.052 Uiso 1 1 calc R . . C23 C 0.0222(4) 0.3829(5) 0.5356(9) 0.034(2) Uani 1 1 d . . . H23A H 0.0072 0.4248 0.4581 0.051 Uiso 1 1 calc R A . H23B H 0.0016 0.3930 0.6302 0.051 Uiso 1 1 calc R . . H23C H 0.0077 0.3296 0.4932 0.051 Uiso 1 1 calc R . . C24 C 0.1325(5) 0.3764(5) 0.4259(9) 0.036(2) Uani 1 1 d . . . H24A H 0.1824 0.3706 0.4508 0.055 Uiso 1 1 calc R A . H24B H 0.1217 0.4247 0.3612 0.055 Uiso 1 1 calc R . . H24C H 0.1133 0.3283 0.3691 0.055 Uiso 1 1 calc R . . C25 C 0.1502(4) 0.5346(4) 0.5946(9) 0.0192(19) Uani 1 1 d . A . H25 H 0.1671 0.5370 0.4973 0.023 Uiso 1 1 calc R . . C26 C 0.1505(4) 0.5993(4) 0.7031(8) 0.0169(18) Uani 1 1 d . A . H26 H 0.1680 0.6521 0.6899 0.020 Uiso 1 1 calc R . . Th1 Th 0.248558(15) 0.492610(17) 0.83731(3) 0.01862(10) Uani 1 1 d . A . 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 Br1 0.0339(6) 0.0516(6) 0.0504(6) -0.0243(5) 0.0017(5) -0.0082(5) Br2 0.0331(6) 0.0473(6) 0.0330(5) 0.0187(4) 0.0098(4) 0.0043(5) C1 0.039(6) 0.030(5) 0.043(6) 0.014(4) 0.016(5) 0.008(5) C2 0.020(5) 0.043(6) 0.041(6) 0.014(5) -0.002(4) 0.011(5) C3 0.024(6) 0.055(7) 0.044(6) 0.011(5) 0.013(4) 0.020(5) C4 0.024(5) 0.022(5) 0.032(5) 0.006(4) 0.002(4) 0.010(4) C5 0.012(5) 0.024(5) 0.035(5) 0.001(4) 0.002(4) -0.004(4) C6 0.019(5) 0.019(4) 0.031(5) 0.005(4) 0.003(4) 0.000(4) C7 0.009(4) 0.041(6) 0.031(5) 0.007(4) 0.004(4) -0.001(4) C8 0.028(6) 0.051(6) 0.026(5) 0.016(4) 0.009(4) 0.004(5) C9 0.054(3) 0.052(3) 0.054(3) 0.0042(19) 0.0066(19) -0.0020(19) C10 0.032(7) 0.049(7) 0.051(8) 0.009(6) 0.012(6) -0.007(6) C10A 0.032(7) 0.049(7) 0.051(8) 0.009(6) 0.012(6) -0.007(6) C11 0.034(6) 0.048(6) 0.038(6) 0.022(5) 0.007(5) 0.003(5) C12 0.019(5) 0.043(5) 0.019(5) 0.002(4) 0.005(4) 0.005(4) C13 0.019(5) 0.031(5) 0.022(5) 0.002(4) 0.002(4) 0.003(4) C14 0.032(6) 0.037(5) 0.028(5) -0.008(4) 0.012(4) 0.008(4) C15 0.042(6) 0.021(5) 0.047(6) -0.009(4) 0.010(5) 0.007(4) C16 0.040(6) 0.034(5) 0.031(5) -0.008(4) 0.014(4) 0.006(5) C17 0.025(5) 0.011(4) 0.027(5) -0.001(3) 0.001(4) 0.002(4) C18 0.012(5) 0.018(4) 0.024(5) 0.001(3) -0.003(4) 0.006(4) C19 0.009(4) 0.017(4) 0.015(4) -0.002(3) 0.006(3) 0.001(3) C20 0.015(5) 0.017(4) 0.015(4) 0.000(3) -0.001(3) 0.002(3) C21 0.023(5) 0.021(4) 0.016(4) -0.005(3) 0.000(4) -0.001(4) C22 0.048(7) 0.017(5) 0.036(6) 0.002(4) -0.002(5) 0.011(4) C23 0.028(6) 0.034(5) 0.041(6) -0.019(4) 0.008(4) -0.014(4) C24 0.044(6) 0.038(6) 0.029(5) -0.017(4) 0.012(4) -0.017(5) C25 0.024(5) 0.017(4) 0.016(4) 0.002(3) 0.002(4) 0.006(4) C26 0.020(5) 0.007(4) 0.023(4) -0.003(3) 0.001(4) -0.001(3) Th1 0.01511(16) 0.02304(17) 0.01768(16) 0.00081(14) 0.00224(11) -0.00004(15) _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 Br1 Th1 2.7787(10) . ? Br2 Th1 2.8102(9) . ? C1 C4 1.525(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.533(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.535(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.536(10) . ? C5 C6 1.399(10) . ? C5 C13 1.426(10) . ? C5 Th1 2.793(8) . ? C6 C7 1.402(10) . ? C6 Th1 2.820(8) . ? C6 H6 0.9500 . ? C7 C12 1.406(11) . ? C7 C8 1.519(11) . ? C7 Th1 2.815(8) . ? C8 C11 1.508(11) . ? C8 C10 1.533(16) . ? C8 C9 1.550(12) . ? C8 C10A 1.561(16) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.412(11) . ? C12 Th1 2.747(8) . ? C12 H12 0.9500 . ? C13 Th1 2.722(8) . ? C13 H13 0.9500 . ? C14 C17 1.514(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.521(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.555(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.522(10) . ? C18 C26 1.405(10) . ? C18 C19 1.431(10) . ? C18 Th1 2.838(8) . ? C19 C20 1.406(10) . ? C19 Th1 2.814(7) . ? C19 H19 0.9500 . ? C20 C25 1.418(10) . ? C20 C21 1.536(10) . ? C20 Th1 2.804(7) . ? C21 C24 1.515(10) . ? C21 C22 1.535(10) . ? C21 C23 1.549(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.422(10) . ? C25 Th1 2.737(7) . ? C25 H25 0.9500 . ? C26 Th1 2.746(7) . ? C26 H26 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 C2 109.2(7) . . ? C1 C4 C3 109.4(7) . . ? C2 C4 C3 109.1(7) . . ? C1 C4 C5 111.7(7) . . ? C2 C4 C5 110.1(7) . . ? C3 C4 C5 107.3(7) . . ? C6 C5 C13 106.5(7) . . ? C6 C5 C4 125.5(7) . . ? C13 C5 C4 126.7(7) . . ? C6 C5 Th1 76.6(5) . . ? C13 C5 Th1 72.3(4) . . ? C4 C5 Th1 126.6(5) . . ? C5 C6 C7 110.4(7) . . ? C5 C6 Th1 74.5(5) . . ? C7 C6 Th1 75.4(5) . . ? C5 C6 H6 124.8 . . ? C7 C6 H6 124.8 . . ? Th1 C6 H6 117.0 . . ? C6 C7 C12 106.5(7) . . ? C6 C7 C8 126.4(8) . . ? C12 C7 C8 126.2(7) . . ? C6 C7 Th1 75.8(5) . . ? C12 C7 Th1 72.7(5) . . ? C8 C7 Th1 125.3(6) . . ? C11 C8 C7 113.1(7) . . ? C11 C8 C10 116(2) . . ? C7 C8 C10 108.0(14) . . ? C11 C8 C9 107.6(8) . . ? C7 C8 C9 112.6(7) . . ? C10 C8 C9 99(2) . . ? C11 C8 C10A 102.0(19) . . ? C7 C8 C10A 105.7(13) . . ? C10 C8 C10A 18.6(16) . . ? C9 C8 C10A 116(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? C8 C10A H10D 109.5 . . ? C8 C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C8 C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 C13 109.0(7) . . ? C7 C12 Th1 78.1(5) . . ? C13 C12 Th1 74.0(5) . . ? C7 C12 H12 125.5 . . ? C13 C12 H12 125.5 . . ? Th1 C12 H12 114.5 . . ? C12 C13 C5 107.5(7) . . ? C12 C13 Th1 76.0(5) . . ? C5 C13 Th1 77.8(5) . . ? C12 C13 H13 126.2 . . ? C5 C13 H13 126.2 . . ? Th1 C13 H13 112.5 . . ? C17 C14 H14A 109.5 . . ? C17 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C17 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 H15A 109.5 . . ? C17 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C17 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 C15 109.4(7) . . ? C14 C17 C18 108.5(6) . . ? C15 C17 C18 110.1(7) . . ? C14 C17 C16 109.2(7) . . ? C15 C17 C16 109.1(6) . . ? C18 C17 C16 110.5(6) . . ? C26 C18 C19 105.3(6) . . ? C26 C18 C17 128.4(7) . . ? C19 C18 C17 125.2(7) . . ? C26 C18 Th1 71.8(4) . . ? C19 C18 Th1 74.4(4) . . ? C17 C18 Th1 127.7(5) . . ? C20 C19 C18 110.5(7) . . ? C20 C19 Th1 75.1(4) . . ? C18 C19 Th1 76.2(4) . . ? C20 C19 H19 124.8 . . ? C18 C19 H19 124.8 . . ? Th1 C19 H19 115.7 . . ? C19 C20 C25 106.6(6) . . ? C19 C20 C21 125.9(7) . . ? C25 C20 C21 127.2(7) . . ? C19 C20 Th1 75.9(4) . . ? C25 C20 Th1 72.6(4) . . ? C21 C20 Th1 122.2(5) . . ? C24 C21 C22 110.1(7) . . ? C24 C21 C20 112.1(7) . . ? C22 C21 C20 110.9(6) . . ? C24 C21 C23 108.8(6) . . ? C22 C21 C23 107.8(7) . . ? C20 C21 C23 107.0(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 C26 107.9(7) . . ? C20 C25 Th1 77.8(4) . . ? C26 C25 Th1 75.3(4) . . ? C20 C25 H25 126.1 . . ? C26 C25 H25 126.1 . . ? Th1 C25 H25 113.3 . . ? C18 C26 C25 109.7(7) . . ? C18 C26 Th1 79.1(4) . . ? C25 C26 Th1 74.6(4) . . ? C18 C26 H26 125.1 . . ? C25 C26 H26 125.1 . . ? Th1 C26 H26 113.2 . . ? C13 Th1 C25 97.8(2) . . ? C13 Th1 C26 125.3(2) . . ? C25 Th1 C26 30.1(2) . . ? C13 Th1 C12 29.9(2) . . ? C25 Th1 C12 76.5(2) . . ? C26 Th1 C12 98.9(2) . . ? C13 Th1 Br1 125.48(17) . . ? C25 Th1 Br1 116.46(15) . . ? C26 Th1 Br1 88.29(15) . . ? C12 Th1 Br1 118.23(18) . . ? C13 Th1 C5 29.9(2) . . ? C25 Th1 C5 124.8(2) . . ? C26 Th1 C5 145.9(2) . . ? C12 Th1 C5 48.8(2) . . ? Br1 Th1 C5 97.92(16) . . ? C13 Th1 C20 96.3(2) . . ? C25 Th1 C20 29.6(2) . . ? C26 Th1 C20 48.9(2) . . ? C12 Th1 C20 87.9(2) . . ? Br1 Th1 C20 134.26(15) . . ? C5 Th1 C20 126.1(2) . . ? C13 Th1 Br2 96.16(17) . . ? C25 Th1 Br2 123.23(17) . . ? C26 Th1 Br2 122.66(16) . . ? C12 Th1 Br2 125.51(18) . . ? Br1 Th1 Br2 98.22(3) . . ? C5 Th1 Br2 89.72(17) . . ? C20 Th1 Br2 94.27(15) . . ? C13 Th1 C19 121.6(2) . . ? C25 Th1 C19 48.1(2) . . ? C26 Th1 C19 47.8(2) . . ? C12 Th1 C19 116.9(2) . . ? Br1 Th1 C19 112.74(14) . . ? C5 Th1 C19 148.2(2) . . ? C20 Th1 C19 29.0(2) . . ? Br2 Th1 C19 78.16(15) . . ? C13 Th1 C7 48.9(2) . . ? C25 Th1 C7 88.4(2) . . ? C26 Th1 C7 98.6(2) . . ? C12 Th1 C7 29.2(2) . . ? Br1 Th1 C7 88.99(18) . . ? C5 Th1 C7 48.4(2) . . ? C20 Th1 C7 109.8(2) . . ? Br2 Th1 C7 138.14(17) . . ? C19 Th1 C7 136.2(2) . . ? C13 Th1 C6 48.2(2) . . ? C25 Th1 C6 117.2(2) . . ? C26 Th1 C6 124.1(2) . . ? C12 Th1 C6 47.7(2) . . ? Br1 Th1 C6 77.91(16) . . ? C5 Th1 C6 28.9(2) . . ? C20 Th1 C6 135.5(2) . . ? Br2 Th1 C6 112.90(15) . . ? C19 Th1 C6 164.1(2) . . ? C7 Th1 C6 28.8(2) . . ? C13 Th1 C18 144.3(2) . . ? C25 Th1 C18 49.0(2) . . ? C26 Th1 C18 29.1(2) . . ? C12 Th1 C18 125.1(2) . . ? Br1 Th1 C18 86.38(15) . . ? C5 Th1 C18 173.7(2) . . ? C20 Th1 C18 48.8(2) . . ? Br2 Th1 C18 94.18(16) . . ? C19 Th1 C18 29.3(2) . . ? C7 Th1 C18 127.5(2) . . ? C6 Th1 C18 150.2(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.089 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.199 # Attachment '- compound 4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 860418' #TrackingRef '- compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H42 I2 Th' _chemical_formula_sum 'C26 H42 I2 Th' _chemical_formula_weight 840.44 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' I I -0.4742 1.8119 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.495(2) _cell_length_b 16.7311(19) _cell_length_c 8.8954(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.321(2) _cell_angle_gamma 90.00 _cell_volume 2877.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2088 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 23.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 7.337 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3216 _exptl_absorpt_correction_T_max 0.4730 _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 17049 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6580 _reflns_number_gt 4692 _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^)+(0.0289P)^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 6580 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3513(4) 0.4725(4) 0.9137(8) 0.0193(17) Uani 1 1 d . . . H1A H 0.3458 0.4701 1.0215 0.023 Uiso 1 1 calc R . . C2 C 0.3803(3) 0.5379(4) 0.8397(8) 0.0145(15) Uani 1 1 d . . . C3 C 0.4048(4) 0.6171(4) 0.9099(8) 0.0216(17) Uani 1 1 d . . . C4 C 0.3732(5) 0.6349(5) 1.0538(9) 0.043(2) Uani 1 1 d . . . H4A H 0.3243 0.6424 1.0295 0.064 Uiso 1 1 calc R . . H4B H 0.3936 0.6825 1.1000 0.064 Uiso 1 1 calc R . . H4C H 0.3819 0.5909 1.1230 0.064 Uiso 1 1 calc R . . C5 C 0.4832(4) 0.6134(5) 0.9480(10) 0.037(2) Uani 1 1 d . . . H5A H 0.4955 0.5697 1.0159 0.055 Uiso 1 1 calc R . . H5B H 0.4997 0.6625 0.9954 0.055 Uiso 1 1 calc R . . H5C H 0.5038 0.6058 0.8566 0.055 Uiso 1 1 calc R . . C6 C 0.3868(5) 0.6857(5) 0.7986(9) 0.039(2) Uani 1 1 d . . . H6A H 0.4017 0.6726 0.7028 0.058 Uiso 1 1 calc R . . H6B H 0.4098 0.7335 0.8378 0.058 Uiso 1 1 calc R . . H6C H 0.3377 0.6942 0.7853 0.058 Uiso 1 1 calc R . . C7 C 0.3948(4) 0.5085(4) 0.6967(8) 0.0169(15) Uani 1 1 d . . . H7A H 0.4203 0.5383 0.6270 0.020 Uiso 1 1 calc R . . C8 C 0.3779(4) 0.4282(4) 0.6808(8) 0.0206(17) Uani 1 1 d . . . C9 C 0.3989(4) 0.3726(4) 0.5569(9) 0.0249(18) Uani 1 1 d . . . C10 C 0.4783(4) 0.3721(5) 0.5719(10) 0.035(2) Uani 1 1 d . . . H10A H 0.4949 0.4259 0.5670 0.053 Uiso 1 1 calc R . . H10B H 0.4931 0.3413 0.4909 0.053 Uiso 1 1 calc R . . H10C H 0.4965 0.3488 0.6673 0.053 Uiso 1 1 calc R . . C11 C 0.3709(5) 0.4025(5) 0.3966(9) 0.038(2) Uani 1 1 d . . . H11A H 0.3213 0.4005 0.3834 0.057 Uiso 1 1 calc R . . H11B H 0.3882 0.3690 0.3222 0.057 Uiso 1 1 calc R . . H11C H 0.3859 0.4565 0.3843 0.057 Uiso 1 1 calc R . . C12 C 0.3732(4) 0.2867(5) 0.5767(10) 0.035(2) Uani 1 1 d . . . H12A H 0.3919 0.2670 0.6747 0.053 Uiso 1 1 calc R . . H12B H 0.3880 0.2531 0.4996 0.053 Uiso 1 1 calc R . . H12C H 0.3236 0.2865 0.5682 0.053 Uiso 1 1 calc R . . C13 C 0.3493(4) 0.4060(4) 0.8137(8) 0.0185(16) Uani 1 1 d . . . H13A H 0.3407 0.3507 0.8428 0.022 Uiso 1 1 calc R . . C14 C 0.1861(4) 0.6272(4) 0.8266(8) 0.0214(17) Uani 1 1 d . . . H14A H 0.2033 0.6821 0.8410 0.026 Uiso 1 1 calc R . . C15 C 0.1310(4) 0.6028(4) 0.7156(8) 0.0166(16) Uani 1 1 d . . . C16 C 0.0888(4) 0.6560(5) 0.5991(8) 0.0215(17) Uani 1 1 d . . . C17 C 0.1240(4) 0.7355(5) 0.5809(9) 0.033(2) Uani 1 1 d . . . H17A H 0.1354 0.7599 0.6785 0.049 Uiso 1 1 calc R . . H17B H 0.0934 0.7699 0.5172 0.049 Uiso 1 1 calc R . . H17C H 0.1655 0.7270 0.5355 0.049 Uiso 1 1 calc R . . C18 C 0.0730(5) 0.6134(5) 0.4458(8) 0.034(2) Uani 1 1 d . . . H18A H 0.1152 0.6051 0.4031 0.051 Uiso 1 1 calc R . . H18B H 0.0422 0.6457 0.3782 0.051 Uiso 1 1 calc R . . H18C H 0.0517 0.5627 0.4601 0.051 Uiso 1 1 calc R . . C19 C 0.0198(4) 0.6718(5) 0.6603(9) 0.031(2) Uani 1 1 d . . . H19A H -0.0029 0.6219 0.6739 0.047 Uiso 1 1 calc R . . H19B H -0.0092 0.7043 0.5893 0.047 Uiso 1 1 calc R . . H19C H 0.0284 0.6991 0.7557 0.047 Uiso 1 1 calc R . . C20 C 0.1129(4) 0.5258(5) 0.7556(8) 0.0219(17) Uani 1 1 d . . . H20A H 0.0729 0.4963 0.7057 0.026 Uiso 1 1 calc R . . C21 C 0.1526(4) 0.5018(4) 0.8926(8) 0.0206(17) Uani 1 1 d . . . C22 C 0.1386(4) 0.4309(5) 0.9947(9) 0.0278(19) Uani 1 1 d . . . C23 C 0.0871(5) 0.3724(5) 0.9143(10) 0.047(3) Uani 1 1 d . . . H23A H 0.0786 0.3302 0.9828 0.070 Uiso 1 1 calc R . . H23B H 0.1056 0.3501 0.8284 0.070 Uiso 1 1 calc R . . H23C H 0.0446 0.3996 0.8808 0.070 Uiso 1 1 calc R . . C24 C 0.1075(5) 0.4667(6) 1.1287(10) 0.046(3) Uani 1 1 d . . . H24A H 0.0647 0.4929 1.0927 0.069 Uiso 1 1 calc R . . H24B H 0.1392 0.5048 1.1797 0.069 Uiso 1 1 calc R . . H24C H 0.0990 0.4249 1.1980 0.069 Uiso 1 1 calc R . . C25 C 0.2040(4) 0.3865(5) 1.0555(10) 0.039(2) Uani 1 1 d . . . H25A H 0.2383 0.4241 1.0983 0.059 Uiso 1 1 calc R . . H25B H 0.2211 0.3579 0.9744 0.059 Uiso 1 1 calc R . . H25C H 0.1941 0.3495 1.1323 0.059 Uiso 1 1 calc R . . C26 C 0.1987(4) 0.5647(4) 0.9344(8) 0.0194(17) Uani 1 1 d . . . H26A H 0.2259 0.5704 1.0344 0.023 Uiso 1 1 calc R . . I1 I 0.27313(3) 0.61284(3) 0.41337(6) 0.03107(15) Uani 1 1 d . . . I2 I 0.17991(3) 0.36317(4) 0.53245(7) 0.03843(17) Uani 1 1 d . . . Th1 Th 0.249282(14) 0.508456(15) 0.68368(3) 0.01575(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(4) 0.022(4) 0.020(4) 0.005(3) 0.001(3) 0.005(3) C2 0.008(4) 0.013(4) 0.022(4) -0.005(3) 0.000(3) -0.004(3) C3 0.017(4) 0.024(4) 0.022(4) 0.001(3) -0.004(3) 0.000(3) C4 0.054(7) 0.036(5) 0.038(5) -0.024(4) 0.008(5) -0.014(5) C5 0.017(5) 0.033(5) 0.058(6) -0.008(4) -0.004(4) -0.002(4) C6 0.047(6) 0.025(5) 0.040(5) -0.009(4) -0.009(5) -0.007(4) C7 0.014(4) 0.015(4) 0.023(4) -0.001(3) 0.006(3) -0.001(3) C8 0.023(5) 0.022(4) 0.015(4) -0.008(3) -0.001(3) -0.001(3) C9 0.033(5) 0.018(4) 0.024(4) -0.003(3) 0.006(4) 0.002(4) C10 0.030(5) 0.040(5) 0.037(5) -0.004(4) 0.010(4) 0.008(4) C11 0.035(6) 0.049(6) 0.032(5) -0.009(4) 0.005(4) 0.007(4) C12 0.033(5) 0.021(4) 0.053(6) -0.011(4) 0.009(4) 0.003(4) C13 0.015(4) 0.018(4) 0.023(4) 0.006(3) 0.004(3) -0.006(3) C14 0.025(5) 0.018(4) 0.021(4) -0.009(3) 0.005(3) 0.003(3) C15 0.009(4) 0.023(4) 0.017(4) -0.004(3) -0.002(3) 0.003(3) C16 0.009(4) 0.030(4) 0.024(4) 0.001(3) -0.004(3) 0.003(3) C17 0.036(5) 0.025(5) 0.036(5) 0.011(4) 0.001(4) 0.009(4) C18 0.038(6) 0.035(5) 0.026(5) 0.010(4) -0.008(4) 0.001(4) C19 0.018(5) 0.038(5) 0.040(5) 0.006(4) 0.010(4) 0.008(4) C20 0.018(4) 0.030(5) 0.017(4) 0.000(3) -0.002(3) -0.005(3) C21 0.011(4) 0.027(4) 0.025(4) -0.004(3) 0.006(3) 0.002(3) C22 0.015(4) 0.036(5) 0.033(5) 0.012(4) 0.007(4) 0.002(4) C23 0.063(7) 0.035(6) 0.038(5) 0.016(4) -0.007(5) -0.026(5) C24 0.044(6) 0.062(7) 0.037(5) 0.007(5) 0.027(5) 0.000(5) C25 0.028(5) 0.046(6) 0.046(6) 0.019(5) 0.015(4) -0.002(4) C26 0.015(4) 0.024(4) 0.018(4) -0.004(3) 0.000(3) 0.000(3) I1 0.0330(3) 0.0373(3) 0.0236(3) 0.0100(2) 0.0063(2) 0.0030(3) I2 0.0365(4) 0.0348(3) 0.0415(4) -0.0118(3) -0.0045(3) -0.0057(3) Th1 0.01439(14) 0.01748(15) 0.01481(14) -0.00006(11) -0.00035(10) 0.00013(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C13 1.423(10) . ? C1 C2 1.430(10) . ? C1 Th1 2.732(7) . ? C1 H1A 0.9800 . ? C2 C7 1.425(9) . ? C2 C3 1.515(10) . ? C2 Th1 2.792(7) . ? C3 C4 1.518(11) . ? C3 C5 1.525(10) . ? C3 C6 1.528(10) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.386(9) . ? C7 Th1 2.824(7) . ? C7 H7A 0.9800 . ? C8 C13 1.420(10) . ? C8 C9 1.537(10) . ? C8 Th1 2.848(8) . ? C9 C10 1.536(11) . ? C9 C12 1.540(10) . ? C9 C11 1.544(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 Th1 2.739(7) . ? C13 H13A 0.9800 . ? C14 C26 1.420(10) . ? C14 C15 1.423(9) . ? C14 Th1 2.735(7) . ? C14 H14A 0.9800 . ? C15 C20 1.395(10) . ? C15 C16 1.524(9) . ? C15 Th1 2.839(7) . ? C16 C17 1.515(11) . ? C16 C18 1.535(10) . ? C16 C19 1.538(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.416(10) . ? C20 Th1 2.827(8) . ? C20 H20A 0.9800 . ? C21 C26 1.403(10) . ? C21 C22 1.540(10) . ? C21 Th1 2.813(7) . ? C22 C23 1.515(11) . ? C22 C25 1.515(11) . ? C22 C24 1.527(11) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 Th1 2.719(7) . ? C26 H26A 0.9800 . ? I1 Th1 3.0550(6) . ? I2 Th1 3.0139(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 C1 C2 107.0(6) . . ? C13 C1 Th1 75.2(4) . . ? C2 C1 Th1 77.3(4) . . ? C13 C1 H1A 125.6 . . ? C2 C1 H1A 125.6 . . ? Th1 C1 H1A 125.6 . . ? C7 C2 C1 106.4(6) . . ? C7 C2 C3 125.6(6) . . ? C1 C2 C3 127.0(6) . . ? C7 C2 Th1 76.6(4) . . ? C1 C2 Th1 72.7(4) . . ? C3 C2 Th1 125.4(5) . . ? C2 C3 C4 112.3(6) . . ? C2 C3 C5 108.1(6) . . ? C4 C3 C5 108.8(6) . . ? C2 C3 C6 110.9(6) . . ? C4 C3 C6 108.4(7) . . ? C5 C3 C6 108.3(7) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C2 110.8(6) . . ? C8 C7 Th1 76.8(4) . . ? C2 C7 Th1 74.0(4) . . ? C8 C7 H7A 124.2 . . ? C2 C7 H7A 124.2 . . ? Th1 C7 H7A 124.2 . . ? C7 C8 C13 106.4(6) . . ? C7 C8 C9 125.3(7) . . ? C13 C8 C9 127.4(7) . . ? C7 C8 Th1 74.9(4) . . ? C13 C8 Th1 71.1(4) . . ? C9 C8 Th1 127.4(5) . . ? C10 C9 C8 107.3(6) . . ? C10 C9 C12 108.9(6) . . ? C8 C9 C12 111.2(7) . . ? C10 C9 C11 108.4(7) . . ? C8 C9 C11 111.8(6) . . ? C12 C9 C11 109.0(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 C1 109.5(6) . . ? C8 C13 Th1 79.6(4) . . ? C1 C13 Th1 74.7(4) . . ? C8 C13 H13A 124.4 . . ? C1 C13 H13A 124.4 . . ? Th1 C13 H13A 124.4 . . ? C26 C14 C15 108.0(7) . . ? C26 C14 Th1 74.3(4) . . ? C15 C14 Th1 79.3(4) . . ? C26 C14 H14A 125.1 . . ? C15 C14 H14A 125.1 . . ? Th1 C14 H14A 125.1 . . ? C20 C15 C14 106.3(6) . . ? C20 C15 C16 125.5(6) . . ? C14 C15 C16 126.8(7) . . ? C20 C15 Th1 75.3(4) . . ? C14 C15 Th1 71.2(4) . . ? C16 C15 Th1 129.2(5) . . ? C17 C16 C15 111.8(6) . . ? C17 C16 C18 110.8(7) . . ? C15 C16 C18 111.3(6) . . ? C17 C16 C19 108.4(7) . . ? C15 C16 C19 106.3(6) . . ? C18 C16 C19 108.0(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 C21 110.7(7) . . ? C15 C20 Th1 76.2(4) . . ? C21 C20 Th1 74.9(4) . . ? C15 C20 H20A 124.2 . . ? C21 C20 H20A 124.2 . . ? Th1 C20 H20A 124.2 . . ? C26 C21 C20 106.1(7) . . ? C26 C21 C22 125.3(7) . . ? C20 C21 C22 127.4(7) . . ? C26 C21 Th1 71.6(4) . . ? C20 C21 Th1 76.0(4) . . ? C22 C21 Th1 127.2(5) . . ? C23 C22 C25 109.2(8) . . ? C23 C22 C24 108.5(7) . . ? C25 C22 C24 108.3(7) . . ? C23 C22 C21 112.1(6) . . ? C25 C22 C21 112.6(6) . . ? C24 C22 C21 106.0(7) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 C14 108.9(6) . . ? C21 C26 Th1 79.1(4) . . ? C14 C26 Th1 75.5(4) . . ? C21 C26 H26A 124.6 . . ? C14 C26 H26A 124.6 . . ? Th1 C26 H26A 124.6 . . ? C26 Th1 C1 76.5(2) . . ? C26 Th1 C14 30.2(2) . . ? C1 Th1 C14 98.0(2) . . ? C26 Th1 C13 100.5(2) . . ? C1 Th1 C13 30.1(2) . . ? C14 Th1 C13 126.7(2) . . ? C26 Th1 C2 86.3(2) . . ? C1 Th1 C2 30.0(2) . . ? C14 Th1 C2 94.5(2) . . ? C13 Th1 C2 49.0(2) . . ? C26 Th1 C21 29.3(2) . . ? C1 Th1 C21 88.9(2) . . ? C14 Th1 C21 48.9(2) . . ? C13 Th1 C21 101.4(2) . . ? C2 Th1 C21 109.1(2) . . ? C26 Th1 C7 115.7(2) . . ? C1 Th1 C7 48.5(2) . . ? C14 Th1 C7 119.4(2) . . ? C13 Th1 C7 47.6(2) . . ? C2 Th1 C7 29.39(19) . . ? C21 Th1 C7 136.6(2) . . ? C26 Th1 C20 47.9(2) . . ? C1 Th1 C20 118.0(2) . . ? C14 Th1 C20 47.8(2) . . ? C13 Th1 C20 127.4(2) . . ? C2 Th1 C20 134.2(2) . . ? C21 Th1 C20 29.1(2) . . ? C7 Th1 C20 163.6(2) . . ? C26 Th1 C15 48.8(2) . . ? C1 Th1 C15 124.8(2) . . ? C14 Th1 C15 29.51(19) . . ? C13 Th1 C15 148.2(2) . . ? C2 Th1 C15 123.8(2) . . ? C21 Th1 C15 48.3(2) . . ? C7 Th1 C15 145.1(2) . . ? C20 Th1 C15 28.5(2) . . ? C26 Th1 C8 125.6(2) . . ? C1 Th1 C8 49.1(2) . . ? C14 Th1 C8 142.8(2) . . ? C13 Th1 C8 29.4(2) . . ? C2 Th1 C8 48.4(2) . . ? C21 Th1 C8 130.7(2) . . ? C7 Th1 C8 28.28(19) . . ? C20 Th1 C8 154.8(2) . . ? C15 Th1 C8 172.2(2) . . ? C26 Th1 I2 117.14(16) . . ? C1 Th1 I2 113.53(15) . . ? C14 Th1 I2 126.18(16) . . ? C13 Th1 I2 86.46(15) . . ? C2 Th1 I2 133.98(14) . . ? C21 Th1 I2 87.86(15) . . ? C7 Th1 I2 114.18(14) . . ? C20 Th1 I2 78.60(16) . . ? C15 Th1 I2 99.75(14) . . ? C8 Th1 I2 87.78(14) . . ? C26 Th1 I1 123.74(15) . . ? C1 Th1 I1 123.09(16) . . ? C14 Th1 I1 94.20(16) . . ? C13 Th1 I1 121.25(15) . . ? C2 Th1 I1 93.96(15) . . ? C21 Th1 I1 136.44(15) . . ? C7 Th1 I1 77.26(14) . . ? C20 Th1 I1 111.17(15) . . ? C15 Th1 I1 88.15(15) . . ? C8 Th1 I1 92.30(15) . . ? I2 Th1 I1 102.377(19) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.302 _refine_diff_density_min -1.690 _refine_diff_density_rms 0.235 # Attachment '- compound 5.cif' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 860419' #TrackingRef '- compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H71 F5 N2 Th2' _chemical_formula_sum 'C49 H71 F5 N2 Th2' _chemical_formula_weight 1247.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1450(12) _cell_length_b 13.7490(14) _cell_length_c 17.2830(19) _cell_angle_alpha 102.725(10) _cell_angle_beta 96.148(9) _cell_angle_gamma 91.443(7) _cell_volume 2795.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11132 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 28.10 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 5.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3595 _exptl_absorpt_correction_T_max 0.4455 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35795 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.93 _reflns_number_total 13245 _reflns_number_gt 9449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disordered solvents were removed by SQEEZE programm. ; _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^)+(0.0101P)^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 SHELXL _refine_ls_extinction_coef 0.00032(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13245 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _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 Th1 Th 0.167873(12) 0.416427(12) 0.213594(10) 0.01794(5) Uani 1 1 d . . . Th2 Th 0.374915(13) 0.259372(12) 0.297871(10) 0.02043(5) Uani 1 1 d . . . F1 F 0.19622(17) 0.24962(16) 0.22326(13) 0.0221(6) Uani 1 1 d . . . F2 F 0.27633(18) 0.39988(16) 0.33949(13) 0.0208(6) Uani 1 1 d . . . F3 F 0.35838(17) 0.35808(16) 0.20438(13) 0.0211(6) Uani 1 1 d . . . F4 F 0.26727(18) 0.55739(17) 0.24708(13) 0.0254(6) Uani 1 1 d . . . F5 F 0.27044(19) 0.19297(18) 0.36612(14) 0.0300(7) Uani 1 1 d . . . N1 N 0.5333(3) 0.4052(3) 0.3497(2) 0.0265(10) Uani 1 1 d . . . N2 N 0.4752(3) 0.2894(3) 0.4474(2) 0.0278(10) Uani 1 1 d . . . C1 C 0.2036(4) 0.4515(3) 0.0605(2) 0.0215(11) Uani 1 1 d . . . C2 C 0.2109(3) 0.3462(3) 0.0502(2) 0.0217(11) Uani 1 1 d . . . H2A H 0.2771 0.3116 0.0432 0.026 Uiso 1 1 calc R . . C3 C 0.1056(4) 0.3004(3) 0.0518(2) 0.0219(11) Uani 1 1 d . . . C4 C 0.0338(3) 0.3776(3) 0.0660(2) 0.0217(11) Uani 1 1 d . . . H4A H -0.0427 0.3696 0.0715 0.026 Uiso 1 1 calc R . . C5 C 0.0917(3) 0.4706(3) 0.0713(2) 0.0230(11) Uani 1 1 d . . . H5A H 0.0606 0.5343 0.0804 0.028 Uiso 1 1 calc R . . C6 C 0.2924(4) 0.5232(3) 0.0461(3) 0.0239(11) Uani 1 1 d . . . C7 C 0.2948(4) 0.5051(3) -0.0446(2) 0.0324(12) Uani 1 1 d . . . H7A H 0.3523 0.5494 -0.0562 0.049 Uiso 1 1 calc R . . H7B H 0.2225 0.5189 -0.0699 0.049 Uiso 1 1 calc R . . H7C H 0.3111 0.4354 -0.0658 0.049 Uiso 1 1 calc R . . C8 C 0.2650(4) 0.6312(3) 0.0764(3) 0.0324(13) Uani 1 1 d . . . H8A H 0.2628 0.6445 0.1343 0.049 Uiso 1 1 calc R . . H8B H 0.1926 0.6432 0.0503 0.049 Uiso 1 1 calc R . . H8C H 0.3219 0.6756 0.0643 0.049 Uiso 1 1 calc R . . C9 C 0.4078(3) 0.5068(3) 0.0849(3) 0.0311(12) Uani 1 1 d . . . H9A H 0.4087 0.5225 0.1431 0.047 Uiso 1 1 calc R . . H9B H 0.4629 0.5505 0.0699 0.047 Uiso 1 1 calc R . . H9C H 0.4256 0.4370 0.0666 0.047 Uiso 1 1 calc R . . C10 C 0.0727(4) 0.1891(3) 0.0291(3) 0.0234(11) Uani 1 1 d . . . C11 C 0.0215(4) 0.1643(3) -0.0591(3) 0.0368(14) Uani 1 1 d . . . H11A H -0.0439 0.2035 -0.0650 0.055 Uiso 1 1 calc R . . H11B H -0.0002 0.0930 -0.0758 0.055 Uiso 1 1 calc R . . H11C H 0.0762 0.1808 -0.0926 0.055 Uiso 1 1 calc R . . C12 C -0.0126(3) 0.1608(3) 0.0807(3) 0.0336(13) Uani 1 1 d . . . H12A H 0.0213 0.1713 0.1362 0.050 Uiso 1 1 calc R . . H12B H -0.0371 0.0904 0.0608 0.050 Uiso 1 1 calc R . . H12C H -0.0764 0.2026 0.0782 0.050 Uiso 1 1 calc R . . C13 C 0.1732(3) 0.1263(3) 0.0351(3) 0.0287(12) Uani 1 1 d . . . H13A H 0.2248 0.1399 -0.0016 0.043 Uiso 1 1 calc R . . H13B H 0.1494 0.0554 0.0209 0.043 Uiso 1 1 calc R . . H13C H 0.2103 0.1432 0.0899 0.043 Uiso 1 1 calc R . . C14 C 0.0193(3) 0.5575(3) 0.2937(3) 0.0187(10) Uani 1 1 d . . . C15 C 0.0458(3) 0.4985(3) 0.3484(3) 0.0209(11) Uani 1 1 d . . . H15A H 0.0893 0.5209 0.3986 0.025 Uiso 1 1 calc R . . C16 C -0.0010(3) 0.4004(3) 0.3187(3) 0.0206(11) Uani 1 1 d . . . C17 C -0.0549(3) 0.3992(3) 0.2426(3) 0.0234(11) Uani 1 1 d . . . H17A H -0.0934 0.3429 0.2073 0.028 Uiso 1 1 calc R . . C18 C -0.0428(3) 0.4948(3) 0.2273(3) 0.0231(11) Uani 1 1 d . . . H18A H -0.0718 0.5139 0.1798 0.028 Uiso 1 1 calc R . . C19 C 0.0327(4) 0.6691(3) 0.3070(3) 0.0235(11) Uani 1 1 d . . . C20 C 0.0456(4) 0.7032(3) 0.2301(3) 0.0323(12) Uani 1 1 d . . . H20A H -0.0158 0.6739 0.1895 0.048 Uiso 1 1 calc R . . H20B H 0.1160 0.6815 0.2110 0.048 Uiso 1 1 calc R . . H20C H 0.0449 0.7762 0.2404 0.048 Uiso 1 1 calc R . . C21 C 0.1312(3) 0.7123(3) 0.3699(3) 0.0334(13) Uani 1 1 d . . . H21A H 0.1344 0.7853 0.3794 0.050 Uiso 1 1 calc R . . H21B H 0.2002 0.6869 0.3506 0.050 Uiso 1 1 calc R . . H21C H 0.1216 0.6922 0.4199 0.050 Uiso 1 1 calc R . . C22 C -0.0738(4) 0.7134(3) 0.3390(3) 0.0348(13) Uani 1 1 d . . . H22A H -0.0833 0.6941 0.3893 0.052 Uiso 1 1 calc R . . H22B H -0.1380 0.6877 0.2998 0.052 Uiso 1 1 calc R . . H22C H -0.0675 0.7863 0.3483 0.052 Uiso 1 1 calc R . . C23 C -0.0165(4) 0.3219(3) 0.3666(3) 0.0245(11) Uani 1 1 d . . . C24 C -0.0192(4) 0.2154(3) 0.3154(3) 0.0322(12) Uani 1 1 d . . . H24A H -0.0771 0.2077 0.2701 0.048 Uiso 1 1 calc R . . H24B H -0.0351 0.1677 0.3479 0.048 Uiso 1 1 calc R . . H24C H 0.0529 0.2026 0.2956 0.048 Uiso 1 1 calc R . . C25 C -0.1297(3) 0.3383(3) 0.3993(3) 0.0311(12) Uani 1 1 d . . . H25A H -0.1886 0.3308 0.3547 0.047 Uiso 1 1 calc R . . H25B H -0.1291 0.4056 0.4333 0.047 Uiso 1 1 calc R . . H25C H -0.1431 0.2889 0.4308 0.047 Uiso 1 1 calc R . . C26 C 0.0706(3) 0.3331(3) 0.4383(2) 0.0311(12) Uani 1 1 d . . . H26A H 0.0540 0.2838 0.4691 0.047 Uiso 1 1 calc R . . H26B H 0.0701 0.4005 0.4720 0.047 Uiso 1 1 calc R . . H26C H 0.1438 0.3223 0.4200 0.047 Uiso 1 1 calc R . . C27 C 0.5251(4) 0.1504(3) 0.1924(3) 0.0301(12) Uani 1 1 d . . . C28 C 0.4260(4) 0.0893(3) 0.1814(3) 0.0320(13) Uani 1 1 d . . . H28A H 0.3750 0.0754 0.1342 0.038 Uiso 1 1 calc R . . C29 C 0.4139(4) 0.0530(3) 0.2485(3) 0.0372(14) Uani 1 1 d . . . C30 C 0.5038(4) 0.0943(3) 0.3071(3) 0.0333(13) Uani 1 1 d . . . H30A H 0.5168 0.0836 0.3597 0.040 Uiso 1 1 calc R . . C31 C 0.5705(4) 0.1547(3) 0.2718(3) 0.0294(12) Uani 1 1 d . . . H31A H 0.6359 0.1924 0.2977 0.035 Uiso 1 1 calc R . . C32 C 0.5812(4) 0.1827(4) 0.1268(3) 0.0299(12) Uani 1 1 d . . . C33 C 0.6699(4) 0.2649(4) 0.1602(3) 0.0582(18) Uani 1 1 d . . . H33A H 0.7088 0.2789 0.1166 0.087 Uiso 1 1 calc R . . H33B H 0.7229 0.2437 0.1993 0.087 Uiso 1 1 calc R . . H33C H 0.6355 0.3254 0.1861 0.087 Uiso 1 1 calc R . . C34 C 0.4986(4) 0.2176(4) 0.0668(3) 0.0436(15) Uani 1 1 d . . . H34A H 0.4416 0.1643 0.0439 0.065 Uiso 1 1 calc R . . H34B H 0.5376 0.2339 0.0242 0.065 Uiso 1 1 calc R . . H34C H 0.4635 0.2771 0.0940 0.065 Uiso 1 1 calc R . . C35 C 0.6391(4) 0.0910(4) 0.0826(3) 0.0627(18) Uani 1 1 d . . . H35A H 0.5845 0.0350 0.0627 0.094 Uiso 1 1 calc R . . H35B H 0.6974 0.0723 0.1196 0.094 Uiso 1 1 calc R . . H35C H 0.6721 0.1079 0.0376 0.094 Uiso 1 1 calc R . . C36 C 0.3282(5) -0.0286(4) 0.2553(4) 0.0545(18) Uani 1 1 d . . . C37 C 0.3292(4) -0.0415(4) 0.3410(4) 0.069(2) Uani 1 1 d . . . H37A H 0.4055 -0.0488 0.3631 0.103 Uiso 1 1 calc R . . H37B H 0.2836 -0.1013 0.3412 0.103 Uiso 1 1 calc R . . H37C H 0.2991 0.0172 0.3735 0.103 Uiso 1 1 calc R . . C38 C 0.2099(4) -0.0056(4) 0.2230(3) 0.0612(19) Uani 1 1 d . . . H38A H 0.1574 -0.0596 0.2260 0.092 Uiso 1 1 calc R . . H38B H 0.2090 -0.0002 0.1674 0.092 Uiso 1 1 calc R . . H38C H 0.1885 0.0575 0.2553 0.092 Uiso 1 1 calc R . . C39 C 0.3644(5) -0.1289(4) 0.2060(4) 0.124(3) Uani 1 1 d . . . H39A H 0.4449 -0.1328 0.2164 0.186 Uiso 1 1 calc R . . H39B H 0.3439 -0.1326 0.1489 0.186 Uiso 1 1 calc R . . H39C H 0.3272 -0.1847 0.2214 0.186 Uiso 1 1 calc R . . C40 C 0.5584(4) 0.4634(4) 0.3008(3) 0.0368(14) Uani 1 1 d . . . H40 H 0.5219 0.4491 0.2478 0.044 Uiso 1 1 calc R . . C41 C 0.6357(4) 0.5438(4) 0.3240(3) 0.0470(16) Uani 1 1 d . . . H41 H 0.6518 0.5832 0.2874 0.056 Uiso 1 1 calc R . . C42 C 0.6885(4) 0.5655(4) 0.4012(3) 0.0418(15) Uani 1 1 d . . . H42 H 0.7416 0.6200 0.4185 0.050 Uiso 1 1 calc R . . C43 C 0.6629(3) 0.5067(3) 0.4530(3) 0.0355(14) Uani 1 1 d . . . H43 H 0.6979 0.5209 0.5064 0.043 Uiso 1 1 calc R . . C44 C 0.5854(3) 0.4264(3) 0.4261(3) 0.0260(12) Uani 1 1 d . . . C45 C 0.5552(4) 0.3626(3) 0.4791(3) 0.0274(12) Uani 1 1 d . . . C46 C 0.6029(4) 0.3770(4) 0.5584(3) 0.0372(14) Uani 1 1 d . . . H46 H 0.6589 0.4283 0.5793 0.045 Uiso 1 1 calc R . . C47 C 0.5686(4) 0.3170(4) 0.6061(3) 0.0458(15) Uani 1 1 d . . . H47 H 0.5988 0.3273 0.6605 0.055 Uiso 1 1 calc R . . C48 C 0.4891(4) 0.2411(4) 0.5731(3) 0.0415(14) Uani 1 1 d . . . H48 H 0.4655 0.1969 0.6040 0.050 Uiso 1 1 calc R . . C49 C 0.4451(4) 0.2308(4) 0.4956(3) 0.0374(14) Uani 1 1 d . . . H49 H 0.3897 0.1790 0.4742 0.045 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 Th1 0.01720(9) 0.01534(9) 0.02067(10) 0.00573(7) -0.00322(7) -0.00302(7) Th2 0.01823(10) 0.01416(9) 0.02759(11) 0.00541(8) -0.00387(8) -0.00286(7) F1 0.0210(14) 0.0141(14) 0.0284(15) 0.0041(12) -0.0053(11) -0.0092(11) F2 0.0227(14) 0.0165(14) 0.0223(14) 0.0044(11) -0.0007(11) -0.0017(11) F3 0.0219(14) 0.0200(14) 0.0210(14) 0.0065(12) -0.0025(11) -0.0043(11) F4 0.0246(14) 0.0255(15) 0.0261(15) 0.0067(12) 0.0000(12) 0.0025(12) F5 0.0255(15) 0.0265(16) 0.0398(17) 0.0130(13) 0.0019(13) -0.0050(12) N1 0.022(2) 0.020(2) 0.037(3) 0.007(2) -0.0030(19) -0.0010(17) N2 0.027(2) 0.025(2) 0.032(3) 0.010(2) -0.0013(19) 0.0011(19) C1 0.024(3) 0.022(3) 0.018(3) 0.003(2) -0.002(2) -0.002(2) C2 0.023(3) 0.020(3) 0.018(3) 0.000(2) -0.002(2) 0.000(2) C3 0.025(3) 0.020(3) 0.020(3) 0.005(2) -0.005(2) -0.007(2) C4 0.020(3) 0.021(3) 0.023(3) 0.005(2) -0.004(2) -0.006(2) C5 0.027(3) 0.018(3) 0.022(3) 0.005(2) -0.006(2) -0.001(2) C6 0.028(3) 0.020(3) 0.025(3) 0.008(2) 0.003(2) 0.000(2) C7 0.040(3) 0.027(3) 0.031(3) 0.010(2) 0.002(2) 0.000(2) C8 0.038(3) 0.021(3) 0.039(3) 0.009(2) 0.006(2) -0.008(2) C9 0.024(3) 0.033(3) 0.038(3) 0.016(3) -0.003(2) -0.007(2) C10 0.024(3) 0.021(3) 0.022(3) 0.004(2) -0.010(2) -0.005(2) C11 0.046(3) 0.025(3) 0.032(3) 0.000(2) -0.015(3) -0.001(2) C12 0.032(3) 0.023(3) 0.042(3) 0.003(2) -0.003(2) -0.013(2) C13 0.035(3) 0.015(3) 0.033(3) 0.001(2) -0.005(2) -0.002(2) C14 0.017(2) 0.015(2) 0.025(3) 0.007(2) 0.001(2) 0.0030(19) C15 0.018(2) 0.025(3) 0.019(3) 0.006(2) 0.0005(19) -0.003(2) C16 0.017(2) 0.018(3) 0.028(3) 0.009(2) 0.000(2) 0.000(2) C17 0.017(2) 0.022(3) 0.029(3) 0.006(2) -0.001(2) -0.008(2) C18 0.019(3) 0.026(3) 0.023(3) 0.007(2) 0.001(2) -0.001(2) C19 0.027(3) 0.020(3) 0.027(3) 0.010(2) 0.007(2) 0.001(2) C20 0.039(3) 0.026(3) 0.036(3) 0.015(2) 0.007(2) 0.005(2) C21 0.039(3) 0.019(3) 0.041(3) 0.007(2) 0.000(3) 0.000(2) C22 0.044(3) 0.023(3) 0.043(3) 0.014(2) 0.014(3) 0.004(2) C23 0.021(3) 0.030(3) 0.024(3) 0.008(2) 0.002(2) -0.002(2) C24 0.032(3) 0.030(3) 0.040(3) 0.019(3) 0.006(2) -0.005(2) C25 0.028(3) 0.037(3) 0.031(3) 0.014(2) 0.005(2) -0.003(2) C26 0.033(3) 0.032(3) 0.033(3) 0.015(2) 0.008(2) 0.003(2) C27 0.024(3) 0.022(3) 0.039(3) -0.001(2) 0.000(2) -0.001(2) C28 0.023(3) 0.022(3) 0.045(3) 0.000(3) -0.006(2) -0.004(2) C29 0.035(3) 0.016(3) 0.059(4) 0.001(3) 0.013(3) -0.002(2) C30 0.040(3) 0.014(3) 0.050(4) 0.016(3) 0.006(3) 0.009(2) C31 0.024(3) 0.019(3) 0.040(3) 0.001(2) -0.004(2) -0.002(2) C32 0.025(3) 0.026(3) 0.037(3) 0.003(2) 0.000(2) 0.001(2) C33 0.059(4) 0.073(5) 0.044(4) 0.019(3) 0.005(3) -0.028(3) C34 0.033(3) 0.061(4) 0.039(3) 0.017(3) -0.002(3) 0.008(3) C35 0.064(4) 0.064(5) 0.072(5) 0.024(4) 0.034(4) 0.024(4) C36 0.057(4) 0.017(3) 0.086(5) 0.000(3) 0.018(4) -0.010(3) C37 0.051(4) 0.034(4) 0.131(6) 0.045(4) 0.003(4) -0.007(3) C38 0.055(4) 0.053(4) 0.074(5) 0.018(4) -0.003(3) -0.038(3) C39 0.137(7) 0.023(4) 0.198(9) -0.030(5) 0.086(6) -0.035(4) C40 0.032(3) 0.032(3) 0.046(4) 0.013(3) 0.000(3) -0.011(2) C41 0.038(3) 0.045(4) 0.064(4) 0.031(3) -0.004(3) -0.012(3) C42 0.022(3) 0.028(3) 0.073(4) 0.014(3) -0.003(3) -0.009(2) C43 0.017(3) 0.028(3) 0.056(4) 0.002(3) -0.004(3) -0.001(2) C44 0.015(2) 0.019(3) 0.039(3) -0.001(2) -0.002(2) 0.001(2) C45 0.018(3) 0.026(3) 0.037(3) 0.008(2) 0.000(2) 0.002(2) C46 0.021(3) 0.043(4) 0.039(3) -0.002(3) -0.010(2) 0.002(2) C47 0.037(3) 0.057(4) 0.044(4) 0.017(3) -0.008(3) -0.003(3) C48 0.040(3) 0.049(4) 0.039(3) 0.022(3) -0.002(3) 0.008(3) C49 0.035(3) 0.032(3) 0.045(4) 0.015(3) -0.007(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 F4 2.188(2) . ? Th1 F1 2.367(2) . ? Th1 F3 2.478(2) . ? Th1 F2 2.478(2) . ? Th1 C5 2.796(4) . ? Th1 C4 2.812(4) . ? Th1 C18 2.815(4) . ? Th1 C17 2.818(4) . ? Th1 C1 2.867(4) . ? Th1 C2 2.885(4) . ? Th1 C14 2.909(4) . ? Th1 C3 2.909(4) . ? Th2 F5 2.138(2) . ? Th2 F2 2.318(2) . ? Th2 F3 2.324(2) . ? Th2 F1 2.388(2) . ? Th2 N2 2.676(4) . ? Th2 N1 2.678(3) . ? Th2 C30 2.813(4) . ? Th2 C31 2.834(4) . ? Th2 C29 2.845(5) . ? Th2 C28 2.859(4) . ? Th2 C27 2.922(5) . ? N1 C40 1.336(5) . ? N1 C44 1.368(5) . ? N2 C49 1.351(5) . ? N2 C45 1.361(5) . ? C1 C5 1.416(5) . ? C1 C2 1.424(5) . ? C1 C6 1.519(5) . ? C2 C3 1.418(5) . ? C2 H2A 0.9500 . ? C3 C4 1.387(5) . ? C3 C10 1.526(5) . ? C4 C5 1.425(5) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C8 1.520(5) . ? C6 C9 1.531(5) . ? C6 C7 1.536(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 1.520(5) . ? C10 C12 1.533(5) . ? C10 C11 1.544(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 C15 1.393(5) . ? C14 C18 1.406(5) . ? C14 C19 1.503(5) . ? C15 C16 1.413(5) . ? C15 H15A 0.9500 . ? C16 C17 1.401(5) . ? C16 C23 1.518(6) . ? C17 C18 1.404(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.526(5) . ? C19 C21 1.538(5) . ? C19 C22 1.548(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C26 1.518(5) . ? C23 C24 1.533(5) . ? C23 C25 1.545(5) . ? 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 C31 1.410(6) . ? C27 C28 1.421(5) . ? C27 C32 1.523(6) . ? C28 C29 1.381(6) . ? C28 H28A 0.9500 . ? C29 C30 1.421(6) . ? C29 C36 1.542(6) . ? C30 C31 1.419(6) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.513(6) . ? C32 C34 1.527(6) . ? C32 C35 1.550(6) . ? 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 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.528(7) . ? C36 C38 1.551(7) . ? C36 C39 1.555(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.392(6) . ? C40 H40 0.9500 . ? C41 C42 1.384(6) . ? C41 H41 0.9500 . ? C42 C43 1.384(6) . ? C42 H42 0.9500 . ? C43 C44 1.397(6) . ? C43 H43 0.9500 . ? C44 C45 1.467(6) . ? C45 C46 1.399(6) . ? C46 C47 1.375(6) . ? C46 H46 0.9500 . ? C47 C48 1.384(6) . ? C47 H47 0.9500 . ? C48 C49 1.364(6) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? 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 F4 Th1 F1 135.63(8) . . ? F4 Th1 F3 78.24(8) . . ? F1 Th1 F3 62.98(7) . . ? F4 Th1 F2 78.42(8) . . ? F1 Th1 F2 65.63(7) . . ? F3 Th1 F2 63.04(7) . . ? F4 Th1 C5 87.60(10) . . ? F1 Th1 C5 123.59(10) . . ? F3 Th1 C5 108.73(10) . . ? F2 Th1 C5 164.88(10) . . ? F4 Th1 C4 117.01(10) . . ? F1 Th1 C4 98.61(10) . . ? F3 Th1 C4 113.71(10) . . ? F2 Th1 C4 163.95(10) . . ? C5 Th1 C4 29.43(11) . . ? F4 Th1 C18 98.24(10) . . ? F1 Th1 C18 120.22(10) . . ? F3 Th1 C18 176.47(10) . . ? F2 Th1 C18 116.34(10) . . ? C5 Th1 C18 71.04(13) . . ? C4 Th1 C18 67.92(13) . . ? F4 Th1 C17 123.21(11) . . ? F1 Th1 C17 91.44(10) . . ? F3 Th1 C17 154.13(10) . . ? F2 Th1 C17 104.33(10) . . ? C5 Th1 C17 88.07(12) . . ? C4 Th1 C17 71.74(13) . . ? C18 Th1 C17 28.87(11) . . ? F4 Th1 C1 78.28(10) . . ? F1 Th1 C1 112.90(10) . . ? F3 Th1 C1 80.00(10) . . ? F2 Th1 C1 139.47(10) . . ? C5 Th1 C1 28.92(11) . . ? C4 Th1 C1 47.71(12) . . ? C18 Th1 C1 99.50(12) . . ? C17 Th1 C1 116.17(12) . . ? F4 Th1 C2 101.03(10) . . ? F1 Th1 C2 84.43(10) . . ? F3 Th1 C2 68.01(10) . . ? F2 Th1 C2 130.10(10) . . ? C5 Th1 C2 46.90(12) . . ? C4 Th1 C2 46.26(12) . . ? C18 Th1 C2 113.12(12) . . ? C17 Th1 C2 115.92(12) . . ? C1 Th1 C2 28.67(11) . . ? F4 Th1 C14 76.32(10) . . ? F1 Th1 C14 129.17(10) . . ? F3 Th1 C14 148.76(9) . . ? F2 Th1 C14 94.10(10) . . ? C5 Th1 C14 88.07(12) . . ? C4 Th1 C14 94.00(12) . . ? C18 Th1 C14 28.38(10) . . ? C17 Th1 C14 46.95(12) . . ? C1 Th1 C14 111.85(12) . . ? C2 Th1 C14 134.83(12) . . ? F4 Th1 C3 125.91(11) . . ? F1 Th1 C3 76.02(10) . . ? F3 Th1 C3 88.56(10) . . ? F2 Th1 C3 139.44(10) . . ? C5 Th1 C3 47.57(12) . . ? C4 Th1 C3 28.00(11) . . ? C18 Th1 C3 93.68(12) . . ? C17 Th1 C3 88.81(12) . . ? C1 Th1 C3 47.70(12) . . ? C2 Th1 C3 28.33(10) . . ? C14 Th1 C3 121.19(12) . . ? F5 Th2 F2 83.86(9) . . ? F5 Th2 F3 138.51(8) . . ? F2 Th2 F3 67.85(8) . . ? F5 Th2 F1 76.69(8) . . ? F2 Th2 F1 67.86(7) . . ? F3 Th2 F1 65.00(7) . . ? F5 Th2 N2 71.90(10) . . ? F2 Th2 N2 87.94(10) . . ? F3 Th2 N2 133.21(10) . . ? F1 Th2 N2 142.09(10) . . ? F5 Th2 N1 128.58(10) . . ? F2 Th2 N1 76.49(9) . . ? F3 Th2 N1 74.80(10) . . ? F1 Th2 N1 133.64(9) . . ? N2 Th2 N1 60.50(12) . . ? F5 Th2 C30 83.49(12) . . ? F2 Th2 C30 159.27(12) . . ? F3 Th2 C30 131.09(12) . . ? F1 Th2 C30 124.50(11) . . ? N2 Th2 C30 72.54(13) . . ? N1 Th2 C30 98.96(12) . . ? F5 Th2 C31 112.32(12) . . ? F2 Th2 C31 154.49(10) . . ? F3 Th2 C31 105.55(11) . . ? F1 Th2 C31 133.41(10) . . ? N2 Th2 C31 79.25(12) . . ? N1 Th2 C31 78.01(12) . . ? C30 Th2 C31 29.10(12) . . ? F5 Th2 C29 77.71(13) . . ? F2 Th2 C29 157.80(11) . . ? F3 Th2 C29 119.84(13) . . ? F1 Th2 C29 95.62(11) . . ? N2 Th2 C29 97.88(14) . . ? N1 Th2 C29 124.95(12) . . ? C30 Th2 C29 29.08(12) . . ? C31 Th2 C29 47.30(13) . . ? F5 Th2 C28 101.68(12) . . ? F2 Th2 C28 152.70(11) . . ? F3 Th2 C28 92.10(12) . . ? F1 Th2 C28 87.22(10) . . ? N2 Th2 C28 119.28(12) . . ? N1 Th2 C28 117.29(12) . . ? C30 Th2 C28 46.96(14) . . ? C31 Th2 C28 46.46(12) . . ? C29 Th2 C28 28.02(12) . . ? F5 Th2 C27 124.71(12) . . ? F2 Th2 C27 150.32(11) . . ? F3 Th2 C27 83.55(11) . . ? F1 Th2 C27 107.81(10) . . ? N2 Th2 C27 107.32(12) . . ? N1 Th2 C27 88.87(12) . . ? C30 Th2 C27 47.58(14) . . ? C31 Th2 C27 28.31(12) . . ? C29 Th2 C27 47.13(14) . . ? C28 Th2 C27 28.43(11) . . ? F5 Th2 Th1 98.79(6) . . ? F2 Th2 Th1 40.33(5) . . ? F3 Th2 Th1 40.36(5) . . ? F1 Th2 Th1 37.95(5) . . ? N2 Th2 Th1 128.19(8) . . ? N1 Th2 Th1 95.89(8) . . ? C30 Th2 Th1 158.93(10) . . ? C31 Th2 Th1 144.63(10) . . ? C29 Th2 Th1 130.74(11) . . ? C28 Th2 Th1 112.53(10) . . ? C27 Th2 Th1 118.30(10) . . ? Th1 F1 Th2 103.71(8) . . ? Th2 F2 Th1 102.41(8) . . ? Th2 F3 Th1 102.23(8) . . ? C40 N1 C44 118.4(4) . . ? C40 N1 Th2 119.1(3) . . ? C44 N1 Th2 122.4(3) . . ? C49 N2 C45 116.9(4) . . ? C49 N2 Th2 119.5(3) . . ? C45 N2 Th2 123.5(3) . . ? C5 C1 C2 105.6(4) . . ? C5 C1 C6 127.5(4) . . ? C2 C1 C6 125.9(4) . . ? C5 C1 Th1 72.7(2) . . ? C2 C1 Th1 76.4(2) . . ? C6 C1 Th1 125.0(3) . . ? C3 C2 C1 110.5(4) . . ? C3 C2 Th1 76.8(2) . . ? C1 C2 Th1 75.0(2) . . ? C3 C2 H2A 124.7 . . ? C1 C2 H2A 124.7 . . ? Th1 C2 H2A 115.4 . . ? C4 C3 C2 105.9(4) . . ? C4 C3 C10 126.1(4) . . ? C2 C3 C10 127.3(4) . . ? C4 C3 Th1 72.1(2) . . ? C2 C3 Th1 74.9(2) . . ? C10 C3 Th1 125.3(3) . . ? C3 C4 C5 110.0(4) . . ? C3 C4 Th1 79.9(2) . . ? C5 C4 Th1 74.6(2) . . ? C3 C4 H4A 125.0 . . ? C5 C4 H4A 125.0 . . ? Th1 C4 H4A 112.6 . . ? C1 C5 C4 108.0(4) . . ? C1 C5 Th1 78.3(2) . . ? C4 C5 Th1 75.9(2) . . ? C1 C5 H5A 126.0 . . ? C4 C5 H5A 126.0 . . ? Th1 C5 H5A 112.2 . . ? C1 C6 C8 111.4(4) . . ? C1 C6 C9 112.6(4) . . ? C8 C6 C9 108.8(4) . . ? C1 C6 C7 107.2(3) . . ? C8 C6 C7 108.0(4) . . ? C9 C6 C7 108.7(4) . . ? 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 C3 111.4(4) . . ? C13 C10 C12 109.4(4) . . ? C3 C10 C12 112.0(4) . . ? C13 C10 C11 107.4(4) . . ? C3 C10 C11 107.4(4) . . ? C12 C10 C11 109.1(4) . . ? 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 . . ? C15 C14 C18 106.2(4) . . ? C15 C14 C19 127.9(4) . . ? C18 C14 C19 124.8(4) . . ? C15 C14 Th1 76.9(2) . . ? C18 C14 Th1 72.1(2) . . ? C19 C14 Th1 125.2(3) . . ? C14 C15 C16 110.5(4) . . ? C14 C15 Th1 75.5(2) . . ? C16 C15 Th1 75.6(2) . . ? C14 C15 H15A 124.8 . . ? C16 C15 H15A 124.8 . . ? Th1 C15 H15A 115.9 . . ? C17 C16 C15 105.8(4) . . ? C17 C16 C23 125.8(4) . . ? C15 C16 C23 126.6(4) . . ? C17 C16 Th1 72.0(2) . . ? C15 C16 Th1 76.4(2) . . ? C23 C16 Th1 128.6(3) . . ? C16 C17 C18 108.8(4) . . ? C16 C17 Th1 79.8(2) . . ? C18 C17 Th1 75.4(2) . . ? C16 C17 H17A 125.6 . . ? C18 C17 H17A 125.6 . . ? Th1 C17 H17A 111.6 . . ? C17 C18 C14 108.7(4) . . ? C17 C18 Th1 75.7(2) . . ? C14 C18 Th1 79.5(2) . . ? C17 C18 H18A 125.7 . . ? C14 C18 H18A 125.7 . . ? Th1 C18 H18A 111.6 . . ? C14 C19 C20 112.4(4) . . ? C14 C19 C21 111.9(4) . . ? C20 C19 C21 109.5(4) . . ? C14 C19 C22 107.6(4) . . ? C20 C19 C22 107.6(4) . . ? C21 C19 C22 107.6(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 C26 112.7(4) . . ? C16 C23 C24 112.5(4) . . ? C26 C23 C24 109.6(4) . . ? C16 C23 C25 106.7(4) . . ? C26 C23 C25 106.9(4) . . ? C24 C23 C25 108.2(4) . . ? 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 . . ? C31 C27 C28 105.0(4) . . ? C31 C27 C32 127.7(4) . . ? C28 C27 C32 126.0(4) . . ? C31 C27 Th2 72.4(3) . . ? C28 C27 Th2 73.3(3) . . ? C32 C27 Th2 129.1(3) . . ? C29 C28 C27 110.8(4) . . ? C29 C28 Th2 75.4(3) . . ? C27 C28 Th2 78.3(3) . . ? C29 C28 H28A 124.6 . . ? C27 C28 H28A 124.6 . . ? Th2 C28 H28A 113.6 . . ? C28 C29 C30 107.6(4) . . ? C28 C29 C36 126.4(5) . . ? C30 C29 C36 125.5(5) . . ? C28 C29 Th2 76.6(3) . . ? C30 C29 Th2 74.2(3) . . ? C36 C29 Th2 121.5(3) . . ? C31 C30 C29 106.7(5) . . ? C31 C30 Th2 76.3(3) . . ? C29 C30 Th2 76.7(3) . . ? C31 C30 H30A 126.7 . . ? C29 C30 H30A 126.7 . . ? Th2 C30 H30A 113.0 . . ? C27 C31 C30 109.9(4) . . ? C27 C31 Th2 79.3(3) . . ? C30 C31 Th2 74.6(3) . . ? C27 C31 H31A 125.1 . . ? C30 C31 H31A 125.1 . . ? Th2 C31 H31A 113.1 . . ? C33 C32 C27 112.1(4) . . ? C33 C32 C34 108.7(4) . . ? C27 C32 C34 112.3(4) . . ? C33 C32 C35 107.3(4) . . ? C27 C32 C35 107.2(4) . . ? C34 C32 C35 109.0(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C29 112.3(5) . . ? C37 C36 C38 109.8(5) . . ? C29 C36 C38 110.9(5) . . ? C37 C36 C39 106.2(5) . . ? C29 C36 C39 106.7(5) . . ? C38 C36 C39 110.9(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N1 C40 C41 123.0(5) . . ? N1 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C42 C41 C40 118.8(5) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C43 C42 C41 119.1(5) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C44 119.4(5) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? N1 C44 C43 121.2(5) . . ? N1 C44 C45 117.5(4) . . ? C43 C44 C45 121.3(4) . . ? N2 C45 C46 121.3(5) . . ? N2 C45 C44 116.0(4) . . ? C46 C45 C44 122.6(4) . . ? C47 C46 C45 120.0(5) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 118.5(5) . . ? C46 C47 H47 120.8 . . ? C48 C47 H47 120.8 . . ? C49 C48 C47 119.0(5) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? N2 C49 C48 124.2(5) . . ? N2 C49 H49 117.9 . . ? C48 C49 H49 117.9 . . ? 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 F4 Th1 Th2 F5 129.20(9) . . . . ? F1 Th1 Th2 F5 -54.75(11) . . . . ? F3 Th1 Th2 F5 -171.35(10) . . . . ? F2 Th1 Th2 F5 69.55(10) . . . . ? C5 Th1 Th2 F5 -135.23(15) . . . . ? C4 Th1 Th2 F5 -95.42(13) . . . . ? C18 Th1 Th2 F5 14.01(15) . . . . ? C17 Th1 Th2 F5 -5.44(12) . . . . ? C1 Th1 Th2 F5 -150.30(11) . . . . ? C2 Th1 Th2 F5 -128.93(10) . . . . ? C14 Th1 Th2 F5 50.87(12) . . . . ? C3 Th1 Th2 F5 -101.28(11) . . . . ? F4 Th1 Th2 F2 59.65(10) . . . . ? F1 Th1 Th2 F2 -124.30(13) . . . . ? F3 Th1 Th2 F2 119.10(12) . . . . ? C5 Th1 Th2 F2 155.21(16) . . . . ? C4 Th1 Th2 F2 -164.98(14) . . . . ? C18 Th1 Th2 F2 -55.54(16) . . . . ? C17 Th1 Th2 F2 -74.99(13) . . . . ? C1 Th1 Th2 F2 140.14(12) . . . . ? C2 Th1 Th2 F2 161.52(12) . . . . ? C14 Th1 Th2 F2 -18.68(13) . . . . ? C3 Th1 Th2 F2 -170.83(12) . . . . ? F4 Th1 Th2 F3 -59.45(10) . . . . ? F1 Th1 Th2 F3 116.60(12) . . . . ? F2 Th1 Th2 F3 -119.10(12) . . . . ? C5 Th1 Th2 F3 36.11(16) . . . . ? C4 Th1 Th2 F3 75.92(14) . . . . ? C18 Th1 Th2 F3 -174.64(16) . . . . ? C17 Th1 Th2 F3 165.91(13) . . . . ? C1 Th1 Th2 F3 21.04(12) . . . . ? C2 Th1 Th2 F3 42.42(12) . . . . ? C14 Th1 Th2 F3 -137.78(13) . . . . ? C3 Th1 Th2 F3 70.07(12) . . . . ? F4 Th1 Th2 F1 -176.05(11) . . . . ? F3 Th1 Th2 F1 -116.60(12) . . . . ? F2 Th1 Th2 F1 124.30(12) . . . . ? C5 Th1 Th2 F1 -80.49(16) . . . . ? C4 Th1 Th2 F1 -40.68(15) . . . . ? C18 Th1 Th2 F1 68.75(17) . . . . ? C17 Th1 Th2 F1 49.31(14) . . . . ? C1 Th1 Th2 F1 -95.56(13) . . . . ? C2 Th1 Th2 F1 -74.18(12) . . . . ? C14 Th1 Th2 F1 105.62(14) . . . . ? C3 Th1 Th2 F1 -46.53(13) . . . . ? F4 Th1 Th2 N2 55.36(12) . . . . ? F1 Th1 Th2 N2 -128.59(14) . . . . ? F3 Th1 Th2 N2 114.81(13) . . . . ? F2 Th1 Th2 N2 -4.29(13) . . . . ? C5 Th1 Th2 N2 150.92(17) . . . . ? C4 Th1 Th2 N2 -169.27(15) . . . . ? C18 Th1 Th2 N2 -59.84(17) . . . . ? C17 Th1 Th2 N2 -79.28(14) . . . . ? C1 Th1 Th2 N2 135.85(14) . . . . ? C2 Th1 Th2 N2 157.23(13) . . . . ? C14 Th1 Th2 N2 -22.98(15) . . . . ? C3 Th1 Th2 N2 -175.12(14) . . . . ? F4 Th1 Th2 N1 -1.36(10) . . . . ? F1 Th1 Th2 N1 174.68(12) . . . . ? F3 Th1 Th2 N1 58.08(12) . . . . ? F2 Th1 Th2 N1 -61.02(12) . . . . ? C5 Th1 Th2 N1 94.20(16) . . . . ? C4 Th1 Th2 N1 134.01(14) . . . . ? C18 Th1 Th2 N1 -116.56(16) . . . . ? C17 Th1 Th2 N1 -136.01(13) . . . . ? C1 Th1 Th2 N1 79.13(12) . . . . ? C2 Th1 Th2 N1 100.50(12) . . . . ? C14 Th1 Th2 N1 -79.70(13) . . . . ? C3 Th1 Th2 N1 128.16(12) . . . . ? F4 Th1 Th2 C30 -136.1(3) . . . . ? F1 Th1 Th2 C30 40.0(3) . . . . ? F3 Th1 Th2 C30 -76.6(3) . . . . ? F2 Th1 Th2 C30 164.3(3) . . . . ? C5 Th1 Th2 C30 -40.5(3) . . . . ? C4 Th1 Th2 C30 -0.7(3) . . . . ? C18 Th1 Th2 C30 108.7(3) . . . . ? C17 Th1 Th2 C30 89.3(3) . . . . ? C1 Th1 Th2 C30 -55.6(3) . . . . ? C2 Th1 Th2 C30 -34.2(3) . . . . ? C14 Th1 Th2 C30 145.6(3) . . . . ? C3 Th1 Th2 C30 -6.6(3) . . . . ? F4 Th1 Th2 C31 -78.92(16) . . . . ? F1 Th1 Th2 C31 97.13(17) . . . . ? F3 Th1 Th2 C31 -19.47(17) . . . . ? F2 Th1 Th2 C31 -138.57(17) . . . . ? C5 Th1 Th2 C31 16.6(2) . . . . ? C4 Th1 Th2 C31 56.45(19) . . . . ? C18 Th1 Th2 C31 165.9(2) . . . . ? C17 Th1 Th2 C31 146.44(18) . . . . ? C1 Th1 Th2 C31 1.57(18) . . . . ? C2 Th1 Th2 C31 22.95(17) . . . . ? C14 Th1 Th2 C31 -157.25(18) . . . . ? C3 Th1 Th2 C31 50.60(17) . . . . ? F4 Th1 Th2 C29 -149.48(15) . . . . ? F1 Th1 Th2 C29 26.57(17) . . . . ? F3 Th1 Th2 C29 -90.03(16) . . . . ? F2 Th1 Th2 C29 150.87(16) . . . . ? C5 Th1 Th2 C29 -53.92(19) . . . . ? C4 Th1 Th2 C29 -14.11(18) . . . . ? C18 Th1 Th2 C29 95.3(2) . . . . ? C17 Th1 Th2 C29 75.88(17) . . . . ? C1 Th1 Th2 C29 -68.99(17) . . . . ? C2 Th1 Th2 C29 -47.61(16) . . . . ? C14 Th1 Th2 C29 132.19(17) . . . . ? C3 Th1 Th2 C29 -19.96(16) . . . . ? F4 Th1 Th2 C28 -124.18(12) . . . . ? F1 Th1 Th2 C28 51.87(14) . . . . ? F3 Th1 Th2 C28 -64.73(13) . . . . ? F2 Th1 Th2 C28 176.17(13) . . . . ? C5 Th1 Th2 C28 -28.62(17) . . . . ? C4 Th1 Th2 C28 11.19(16) . . . . ? C18 Th1 Th2 C28 120.63(17) . . . . ? C17 Th1 Th2 C28 101.18(14) . . . . ? C1 Th1 Th2 C28 -43.69(14) . . . . ? C2 Th1 Th2 C28 -22.31(13) . . . . ? C14 Th1 Th2 C28 157.49(14) . . . . ? C3 Th1 Th2 C28 5.34(13) . . . . ? F4 Th1 Th2 C27 -93.26(12) . . . . ? F1 Th1 Th2 C27 82.79(13) . . . . ? F3 Th1 Th2 C27 -33.81(13) . . . . ? F2 Th1 Th2 C27 -152.91(13) . . . . ? C5 Th1 Th2 C27 2.30(17) . . . . ? C4 Th1 Th2 C27 42.11(15) . . . . ? C18 Th1 Th2 C27 151.54(17) . . . . ? C17 Th1 Th2 C27 132.10(14) . . . . ? C1 Th1 Th2 C27 -12.77(13) . . . . ? C2 Th1 Th2 C27 8.61(13) . . . . ? C14 Th1 Th2 C27 -171.59(14) . . . . ? C3 Th1 Th2 C27 36.26(13) . . . . ? F4 Th1 F1 Th2 5.61(16) . . . . ? F3 Th1 F1 Th2 37.57(8) . . . . ? F2 Th1 F1 Th2 -33.30(8) . . . . ? C5 Th1 F1 Th2 132.97(12) . . . . ? C4 Th1 F1 Th2 149.86(11) . . . . ? C18 Th1 F1 Th2 -140.74(11) . . . . ? C17 Th1 F1 Th2 -138.40(11) . . . . ? C1 Th1 F1 Th2 102.30(11) . . . . ? C2 Th1 F1 Th2 105.70(11) . . . . ? C14 Th1 F1 Th2 -107.76(12) . . . . ? C3 Th1 F1 Th2 133.19(12) . . . . ? F5 Th2 F1 Th1 123.97(10) . . . . ? F2 Th2 F1 Th1 35.25(8) . . . . ? F3 Th2 F1 Th1 -39.71(8) . . . . ? N2 Th2 F1 Th1 89.40(16) . . . . ? N1 Th2 F1 Th1 -7.31(17) . . . . ? C30 Th2 F1 Th1 -163.73(13) . . . . ? C31 Th2 F1 Th1 -127.76(14) . . . . ? C29 Th2 F1 Th1 -160.09(13) . . . . ? C28 Th2 F1 Th1 -133.33(13) . . . . ? C27 Th2 F1 Th1 -113.44(12) . . . . ? F5 Th2 F2 Th1 -111.36(9) . . . . ? F3 Th2 F2 Th1 37.65(7) . . . . ? F1 Th2 F2 Th1 -33.26(8) . . . . ? N2 Th2 F2 Th1 176.62(10) . . . . ? N1 Th2 F2 Th1 116.50(11) . . . . ? C30 Th2 F2 Th1 -164.0(3) . . . . ? C31 Th2 F2 Th1 117.2(2) . . . . ? C29 Th2 F2 Th1 -77.4(3) . . . . ? C28 Th2 F2 Th1 -7.7(3) . . . . ? C27 Th2 F2 Th1 54.1(2) . . . . ? F4 Th1 F2 Th2 -119.13(9) . . . . ? F1 Th1 F2 Th2 34.24(8) . . . . ? F3 Th1 F2 Th2 -36.55(8) . . . . ? C5 Th1 F2 Th2 -96.4(4) . . . . ? C4 Th1 F2 Th2 45.6(4) . . . . ? C18 Th1 F2 Th2 147.33(11) . . . . ? C17 Th1 F2 Th2 119.22(11) . . . . ? C1 Th1 F2 Th2 -63.09(17) . . . . ? C2 Th1 F2 Th2 -24.37(15) . . . . ? C14 Th1 F2 Th2 165.75(10) . . . . ? C3 Th1 F2 Th2 13.83(18) . . . . ? F5 Th2 F3 Th1 12.97(15) . . . . ? F2 Th2 F3 Th1 -37.63(7) . . . . ? F1 Th2 F3 Th1 37.35(7) . . . . ? N2 Th2 F3 Th1 -101.80(13) . . . . ? N1 Th2 F3 Th1 -118.96(11) . . . . ? C30 Th2 F3 Th1 152.35(13) . . . . ? C31 Th2 F3 Th1 168.45(10) . . . . ? C29 Th2 F3 Th1 119.13(13) . . . . ? C28 Th2 F3 Th1 123.30(11) . . . . ? C27 Th2 F3 Th1 150.46(11) . . . . ? F4 Th1 F3 Th2 119.27(9) . . . . ? F1 Th1 F3 Th2 -38.51(8) . . . . ? F2 Th1 F3 Th2 36.40(7) . . . . ? C5 Th1 F3 Th2 -157.38(10) . . . . ? C4 Th1 F3 Th2 -126.20(11) . . . . ? C18 Th1 F3 Th2 117.1(16) . . . . ? C17 Th1 F3 Th2 -29.2(3) . . . . ? C1 Th1 F3 Th2 -160.75(11) . . . . ? C2 Th1 F3 Th2 -133.58(12) . . . . ? C14 Th1 F3 Th2 83.3(2) . . . . ? C3 Th1 F3 Th2 -113.53(11) . . . . ? F5 Th2 N1 C40 -153.4(3) . . . . ? F2 Th2 N1 C40 -82.8(4) . . . . ? F3 Th2 N1 C40 -12.5(3) . . . . ? F1 Th2 N1 C40 -42.7(4) . . . . ? N2 Th2 N1 C40 -178.2(4) . . . . ? C30 Th2 N1 C40 117.8(4) . . . . ? C31 Th2 N1 C40 97.5(4) . . . . ? C29 Th2 N1 C40 103.6(4) . . . . ? C28 Th2 N1 C40 71.9(4) . . . . ? C27 Th2 N1 C40 71.1(4) . . . . ? Th1 Th2 N1 C40 -47.2(4) . . . . ? F5 Th2 N1 C44 22.7(4) . . . . ? F2 Th2 N1 C44 93.3(3) . . . . ? F3 Th2 N1 C44 163.7(3) . . . . ? F1 Th2 N1 C44 133.5(3) . . . . ? N2 Th2 N1 C44 -2.0(3) . . . . ? C30 Th2 N1 C44 -66.0(3) . . . . ? C31 Th2 N1 C44 -86.4(3) . . . . ? C29 Th2 N1 C44 -80.3(4) . . . . ? C28 Th2 N1 C44 -111.9(3) . . . . ? C27 Th2 N1 C44 -112.7(3) . . . . ? Th1 Th2 N1 C44 128.9(3) . . . . ? F5 Th2 N2 C49 20.1(3) . . . . ? F2 Th2 N2 C49 104.3(4) . . . . ? F3 Th2 N2 C49 160.9(3) . . . . ? F1 Th2 N2 C49 55.6(4) . . . . ? N1 Th2 N2 C49 179.9(4) . . . . ? C30 Th2 N2 C49 -68.6(4) . . . . ? C31 Th2 N2 C49 -97.8(4) . . . . ? C29 Th2 N2 C49 -54.2(4) . . . . ? C28 Th2 N2 C49 -73.4(4) . . . . ? C27 Th2 N2 C49 -101.6(4) . . . . ? Th1 Th2 N2 C49 107.1(3) . . . . ? F5 Th2 N2 C45 -158.8(4) . . . . ? F2 Th2 N2 C45 -74.5(3) . . . . ? F3 Th2 N2 C45 -18.0(4) . . . . ? F1 Th2 N2 C45 -123.2(3) . . . . ? N1 Th2 N2 C45 1.1(3) . . . . ? C30 Th2 N2 C45 112.5(4) . . . . ? C31 Th2 N2 C45 83.3(3) . . . . ? C29 Th2 N2 C45 127.0(3) . . . . ? C28 Th2 N2 C45 107.7(3) . . . . ? C27 Th2 N2 C45 79.5(3) . . . . ? Th1 Th2 N2 C45 -71.8(4) . . . . ? F4 Th1 C1 C5 -106.7(3) . . . . ? F1 Th1 C1 C5 118.5(2) . . . . ? F3 Th1 C1 C5 173.4(3) . . . . ? F2 Th1 C1 C5 -162.8(2) . . . . ? C4 Th1 C1 C5 38.0(2) . . . . ? C18 Th1 C1 C5 -10.2(3) . . . . ? C17 Th1 C1 C5 14.7(3) . . . . ? C2 Th1 C1 C5 111.4(4) . . . . ? C14 Th1 C1 C5 -36.8(3) . . . . ? C3 Th1 C1 C5 76.2(3) . . . . ? F4 Th1 C1 C2 141.9(3) . . . . ? F1 Th1 C1 C2 7.1(3) . . . . ? F3 Th1 C1 C2 62.0(2) . . . . ? F2 Th1 C1 C2 85.8(3) . . . . ? C5 Th1 C1 C2 -111.4(4) . . . . ? C4 Th1 C1 C2 -73.5(3) . . . . ? C18 Th1 C1 C2 -121.6(2) . . . . ? C17 Th1 C1 C2 -96.7(3) . . . . ? C14 Th1 C1 C2 -148.2(2) . . . . ? C3 Th1 C1 C2 -35.3(2) . . . . ? F4 Th1 C1 C6 17.4(3) . . . . ? F1 Th1 C1 C6 -117.4(3) . . . . ? F3 Th1 C1 C6 -62.5(3) . . . . ? F2 Th1 C1 C6 -38.6(4) . . . . ? C5 Th1 C1 C6 124.1(5) . . . . ? C4 Th1 C1 C6 162.1(4) . . . . ? C18 Th1 C1 C6 114.0(3) . . . . ? C17 Th1 C1 C6 138.9(3) . . . . ? C2 Th1 C1 C6 -124.5(5) . . . . ? C14 Th1 C1 C6 87.4(4) . . . . ? C3 Th1 C1 C6 -159.7(4) . . . . ? C5 C1 C2 C3 1.9(5) . . . . ? C6 C1 C2 C3 -167.2(4) . . . . ? Th1 C1 C2 C3 69.3(3) . . . . ? C5 C1 C2 Th1 -67.4(3) . . . . ? C6 C1 C2 Th1 123.5(4) . . . . ? F4 Th1 C2 C3 -153.8(2) . . . . ? F1 Th1 C2 C3 70.7(3) . . . . ? F3 Th1 C2 C3 133.8(3) . . . . ? F2 Th1 C2 C3 122.1(2) . . . . ? C5 Th1 C2 C3 -77.8(3) . . . . ? C4 Th1 C2 C3 -36.9(2) . . . . ? C18 Th1 C2 C3 -49.8(3) . . . . ? C17 Th1 C2 C3 -18.2(3) . . . . ? C1 Th1 C2 C3 -115.8(4) . . . . ? C14 Th1 C2 C3 -72.2(3) . . . . ? F4 Th1 C2 C1 -38.0(3) . . . . ? F1 Th1 C2 C1 -173.5(2) . . . . ? F3 Th1 C2 C1 -110.4(3) . . . . ? F2 Th1 C2 C1 -122.1(2) . . . . ? C5 Th1 C2 C1 38.1(2) . . . . ? C4 Th1 C2 C1 79.0(3) . . . . ? C18 Th1 C2 C1 66.0(3) . . . . ? C17 Th1 C2 C1 97.7(3) . . . . ? C14 Th1 C2 C1 43.6(3) . . . . ? C3 Th1 C2 C1 115.8(4) . . . . ? C1 C2 C3 C4 -2.2(5) . . . . ? Th1 C2 C3 C4 66.0(3) . . . . ? C1 C2 C3 C10 168.7(4) . . . . ? Th1 C2 C3 C10 -123.1(4) . . . . ? C1 C2 C3 Th1 -68.1(3) . . . . ? F4 Th1 C3 C4 -80.3(3) . . . . ? F1 Th1 C3 C4 142.8(3) . . . . ? F3 Th1 C3 C4 -154.7(3) . . . . ? F2 Th1 C3 C4 161.9(2) . . . . ? C5 Th1 C3 C4 -37.4(2) . . . . ? C18 Th1 C3 C4 22.6(3) . . . . ? C17 Th1 C3 C4 51.1(3) . . . . ? C1 Th1 C3 C4 -76.9(3) . . . . ? C2 Th1 C3 C4 -112.6(4) . . . . ? C14 Th1 C3 C4 15.2(3) . . . . ? F4 Th1 C3 C2 32.3(3) . . . . ? F1 Th1 C3 C2 -104.5(3) . . . . ? F3 Th1 C3 C2 -42.0(3) . . . . ? F2 Th1 C3 C2 -85.4(3) . . . . ? C5 Th1 C3 C2 75.2(3) . . . . ? C4 Th1 C3 C2 112.6(4) . . . . ? C18 Th1 C3 C2 135.2(3) . . . . ? C17 Th1 C3 C2 163.7(3) . . . . ? C1 Th1 C3 C2 35.7(2) . . . . ? C14 Th1 C3 C2 127.9(2) . . . . ? F4 Th1 C3 C10 157.6(3) . . . . ? F1 Th1 C3 C10 20.8(3) . . . . ? F3 Th1 C3 C10 83.3(4) . . . . ? F2 Th1 C3 C10 39.9(4) . . . . ? C5 Th1 C3 C10 -159.5(4) . . . . ? C4 Th1 C3 C10 -122.0(5) . . . . ? C18 Th1 C3 C10 -99.5(4) . . . . ? C17 Th1 C3 C10 -71.0(4) . . . . ? C1 Th1 C3 C10 161.0(4) . . . . ? C2 Th1 C3 C10 125.3(5) . . . . ? C14 Th1 C3 C10 -106.8(4) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C10 C3 C4 C5 -169.5(4) . . . . ? Th1 C3 C4 C5 69.4(3) . . . . ? C2 C3 C4 Th1 -67.9(3) . . . . ? C10 C3 C4 Th1 121.1(4) . . . . ? F4 Th1 C4 C3 116.3(3) . . . . ? F1 Th1 C4 C3 -36.4(3) . . . . ? F3 Th1 C4 C3 27.8(3) . . . . ? F2 Th1 C4 C3 -46.8(5) . . . . ? C5 Th1 C4 C3 114.1(4) . . . . ? C18 Th1 C4 C3 -155.6(3) . . . . ? C17 Th1 C4 C3 -125.0(3) . . . . ? C1 Th1 C4 C3 76.9(3) . . . . ? C2 Th1 C4 C3 37.3(2) . . . . ? C14 Th1 C4 C3 -167.0(3) . . . . ? F4 Th1 C4 C5 2.2(3) . . . . ? F1 Th1 C4 C5 -150.5(3) . . . . ? F3 Th1 C4 C5 -86.3(3) . . . . ? F2 Th1 C4 C5 -160.9(3) . . . . ? C18 Th1 C4 C5 90.3(3) . . . . ? C17 Th1 C4 C5 120.8(3) . . . . ? C1 Th1 C4 C5 -37.3(2) . . . . ? C2 Th1 C4 C5 -76.8(3) . . . . ? C14 Th1 C4 C5 78.9(3) . . . . ? C3 Th1 C4 C5 -114.1(4) . . . . ? C2 C1 C5 C4 -0.9(5) . . . . ? C6 C1 C5 C4 167.9(4) . . . . ? Th1 C1 C5 C4 -70.9(3) . . . . ? C2 C1 C5 Th1 69.9(3) . . . . ? C6 C1 C5 Th1 -121.2(4) . . . . ? C3 C4 C5 C1 -0.4(5) . . . . ? Th1 C4 C5 C1 72.5(3) . . . . ? C3 C4 C5 Th1 -72.9(3) . . . . ? F4 Th1 C5 C1 69.8(2) . . . . ? F1 Th1 C5 C1 -76.3(3) . . . . ? F3 Th1 C5 C1 -6.9(3) . . . . ? F2 Th1 C5 C1 47.6(5) . . . . ? C4 Th1 C5 C1 -112.1(4) . . . . ? C18 Th1 C5 C1 169.4(3) . . . . ? C17 Th1 C5 C1 -166.8(3) . . . . ? C2 Th1 C5 C1 -37.7(2) . . . . ? C14 Th1 C5 C1 146.2(3) . . . . ? C3 Th1 C5 C1 -76.6(3) . . . . ? F4 Th1 C5 C4 -178.0(3) . . . . ? F1 Th1 C5 C4 35.8(3) . . . . ? F3 Th1 C5 C4 105.2(3) . . . . ? F2 Th1 C5 C4 159.8(3) . . . . ? C18 Th1 C5 C4 -78.5(3) . . . . ? C17 Th1 C5 C4 -54.7(3) . . . . ? C1 Th1 C5 C4 112.1(4) . . . . ? C2 Th1 C5 C4 74.4(3) . . . . ? C14 Th1 C5 C4 -101.6(3) . . . . ? C3 Th1 C5 C4 35.5(2) . . . . ? C5 C1 C6 C8 23.0(6) . . . . ? C2 C1 C6 C8 -170.3(4) . . . . ? Th1 C1 C6 C8 -71.6(4) . . . . ? C5 C1 C6 C9 145.5(4) . . . . ? C2 C1 C6 C9 -47.7(6) . . . . ? Th1 C1 C6 C9 50.9(5) . . . . ? C5 C1 C6 C7 -94.9(5) . . . . ? C2 C1 C6 C7 71.8(5) . . . . ? Th1 C1 C6 C7 170.5(3) . . . . ? C4 C3 C10 C13 -168.1(4) . . . . ? C2 C3 C10 C13 22.8(6) . . . . ? Th1 C3 C10 C13 -75.2(5) . . . . ? C4 C3 C10 C12 -45.2(6) . . . . ? C2 C3 C10 C12 145.7(4) . . . . ? Th1 C3 C10 C12 47.7(5) . . . . ? C4 C3 C10 C11 74.5(6) . . . . ? C2 C3 C10 C11 -94.6(5) . . . . ? Th1 C3 C10 C11 167.4(3) . . . . ? F4 Th1 C14 C15 -108.3(2) . . . . ? F1 Th1 C14 C15 30.3(3) . . . . ? F3 Th1 C14 C15 -72.0(3) . . . . ? F2 Th1 C14 C15 -31.3(2) . . . . ? C5 Th1 C14 C15 163.7(3) . . . . ? C4 Th1 C14 C15 134.8(2) . . . . ? C18 Th1 C14 C15 112.1(4) . . . . ? C17 Th1 C14 C15 74.5(3) . . . . ? C1 Th1 C14 C15 -179.5(2) . . . . ? C2 Th1 C14 C15 159.6(2) . . . . ? C3 Th1 C14 C15 127.7(2) . . . . ? F4 Th1 C14 C18 139.5(3) . . . . ? F1 Th1 C14 C18 -81.8(3) . . . . ? F3 Th1 C14 C18 175.9(2) . . . . ? F2 Th1 C14 C18 -143.4(3) . . . . ? C5 Th1 C14 C18 51.6(3) . . . . ? C4 Th1 C14 C18 22.7(3) . . . . ? C17 Th1 C14 C18 -37.6(2) . . . . ? C1 Th1 C14 C18 68.4(3) . . . . ? C2 Th1 C14 C18 47.5(3) . . . . ? C3 Th1 C14 C18 15.6(3) . . . . ? F4 Th1 C14 C19 19.1(3) . . . . ? F1 Th1 C14 C19 157.7(3) . . . . ? F3 Th1 C14 C19 55.4(4) . . . . ? F2 Th1 C14 C19 96.1(3) . . . . ? C5 Th1 C14 C19 -68.9(3) . . . . ? C4 Th1 C14 C19 -97.7(3) . . . . ? C18 Th1 C14 C19 -120.5(5) . . . . ? C17 Th1 C14 C19 -158.1(4) . . . . ? C1 Th1 C14 C19 -52.1(4) . . . . ? C2 Th1 C14 C19 -73.0(4) . . . . ? C3 Th1 C14 C19 -104.8(3) . . . . ? C18 C14 C15 C16 -1.6(5) . . . . ? C19 C14 C15 C16 167.1(4) . . . . ? Th1 C14 C15 C16 -68.3(3) . . . . ? C18 C14 C15 Th1 66.6(3) . . . . ? C19 C14 C15 Th1 -124.6(4) . . . . ? F4 Th1 C15 C14 67.6(2) . . . . ? F1 Th1 C15 C14 -156.2(2) . . . . ? F3 Th1 C15 C14 137.5(2) . . . . ? F2 Th1 C15 C14 146.7(3) . . . . ? C5 Th1 C15 C14 -18.0(3) . . . . ? C4 Th1 C15 C14 -50.1(3) . . . . ? C18 Th1 C15 C14 -37.8(2) . . . . ? C17 Th1 C15 C14 -78.5(3) . . . . ? C1 Th1 C15 C14 0.7(3) . . . . ? C2 Th1 C15 C14 -43.3(5) . . . . ? C3 Th1 C15 C14 -71.7(3) . . . . ? F4 Th1 C15 C16 -176.3(3) . . . . ? F1 Th1 C15 C16 -40.1(3) . . . . ? F3 Th1 C15 C16 -106.4(2) . . . . ? F2 Th1 C15 C16 -97.3(3) . . . . ? C5 Th1 C15 C16 98.1(3) . . . . ? C4 Th1 C15 C16 65.9(3) . . . . ? C18 Th1 C15 C16 78.2(3) . . . . ? C17 Th1 C15 C16 37.6(2) . . . . ? C1 Th1 C15 C16 116.8(3) . . . . ? C2 Th1 C15 C16 72.8(4) . . . . ? C14 Th1 C15 C16 116.1(4) . . . . ? C3 Th1 C15 C16 44.4(3) . . . . ? C14 C15 C16 C17 1.7(5) . . . . ? Th1 C15 C16 C17 -66.5(3) . . . . ? C14 C15 C16 C23 -163.5(4) . . . . ? Th1 C15 C16 C23 128.3(4) . . . . ? C14 C15 C16 Th1 68.2(3) . . . . ? F4 Th1 C16 C17 115.9(2) . . . . ? F1 Th1 C16 C17 -107.0(3) . . . . ? F3 Th1 C16 C17 -146.9(2) . . . . ? F2 Th1 C16 C17 -173.7(3) . . . . ? C5 Th1 C16 C17 16.7(3) . . . . ? C4 Th1 C16 C17 -9.5(3) . . . . ? C18 Th1 C16 C17 37.6(2) . . . . ? C1 Th1 C16 C17 12.3(4) . . . . ? C2 Th1 C16 C17 -35.2(3) . . . . ? C14 Th1 C16 C17 77.0(3) . . . . ? C3 Th1 C16 C17 -35.5(3) . . . . ? F4 Th1 C16 C15 4.0(3) . . . . ? F1 Th1 C16 C15 141.0(3) . . . . ? F3 Th1 C16 C15 101.2(3) . . . . ? F2 Th1 C16 C15 74.4(2) . . . . ? C5 Th1 C16 C15 -95.2(3) . . . . ? C4 Th1 C16 C15 -121.4(3) . . . . ? C18 Th1 C16 C15 -74.3(3) . . . . ? C17 Th1 C16 C15 -111.9(4) . . . . ? C1 Th1 C16 C15 -99.6(3) . . . . ? C2 Th1 C16 C15 -147.1(2) . . . . ? C14 Th1 C16 C15 -35.0(2) . . . . ? C3 Th1 C16 C15 -147.4(2) . . . . ? F4 Th1 C16 C23 -122.3(3) . . . . ? F1 Th1 C16 C23 14.7(3) . . . . ? F3 Th1 C16 C23 -25.1(4) . . . . ? F2 Th1 C16 C23 -51.9(3) . . . . ? C5 Th1 C16 C23 138.5(3) . . . . ? C4 Th1 C16 C23 112.3(3) . . . . ? C18 Th1 C16 C23 159.4(4) . . . . ? C17 Th1 C16 C23 121.8(5) . . . . ? C1 Th1 C16 C23 134.1(3) . . . . ? C2 Th1 C16 C23 86.6(4) . . . . ? C14 Th1 C16 C23 -161.2(4) . . . . ? C3 Th1 C16 C23 86.3(4) . . . . ? C15 C16 C17 C18 -1.1(5) . . . . ? C23 C16 C17 C18 164.3(4) . . . . ? Th1 C16 C17 C18 -70.6(3) . . . . ? C15 C16 C17 Th1 69.6(3) . . . . ? C23 C16 C17 Th1 -125.1(4) . . . . ? F4 Th1 C17 C16 -79.0(3) . . . . ? F1 Th1 C17 C16 71.5(2) . . . . ? F3 Th1 C17 C16 63.3(4) . . . . ? F2 Th1 C17 C16 6.4(3) . . . . ? C5 Th1 C17 C16 -164.9(3) . . . . ? C4 Th1 C17 C16 170.1(3) . . . . ? C18 Th1 C17 C16 -112.7(4) . . . . ? C1 Th1 C17 C16 -172.0(2) . . . . ? C2 Th1 C17 C16 156.1(2) . . . . ? C14 Th1 C17 C16 -75.7(3) . . . . ? C3 Th1 C17 C16 147.5(3) . . . . ? F4 Th1 C17 C18 33.6(3) . . . . ? F1 Th1 C17 C18 -175.8(3) . . . . ? F3 Th1 C17 C18 175.9(2) . . . . ? F2 Th1 C17 C18 119.0(3) . . . . ? C5 Th1 C17 C18 -52.2(3) . . . . ? C4 Th1 C17 C18 -77.2(3) . . . . ? C1 Th1 C17 C18 -59.3(3) . . . . ? C2 Th1 C17 C18 -91.3(3) . . . . ? C14 Th1 C17 C18 36.9(2) . . . . ? C3 Th1 C17 C18 -99.8(3) . . . . ? C16 C17 C18 C14 0.1(5) . . . . ? Th1 C17 C18 C14 -73.5(3) . . . . ? C16 C17 C18 Th1 73.6(3) . . . . ? C15 C14 C18 C17 0.9(5) . . . . ? C19 C14 C18 C17 -168.3(4) . . . . ? Th1 C14 C18 C17 70.9(3) . . . . ? C15 C14 C18 Th1 -70.0(3) . . . . ? C19 C14 C18 Th1 120.8(4) . . . . ? F4 Th1 C18 C17 -152.1(3) . . . . ? F1 Th1 C18 C17 4.9(3) . . . . ? F3 Th1 C18 C17 -149.9(15) . . . . ? F2 Th1 C18 C17 -71.0(3) . . . . ? C5 Th1 C18 C17 123.3(3) . . . . ? C4 Th1 C18 C17 92.0(3) . . . . ? C1 Th1 C18 C17 128.5(3) . . . . ? C2 Th1 C18 C17 102.1(3) . . . . ? C14 Th1 C18 C17 -112.5(4) . . . . ? C3 Th1 C18 C17 80.8(3) . . . . ? F4 Th1 C18 C14 -39.6(3) . . . . ? F1 Th1 C18 C14 117.4(2) . . . . ? F3 Th1 C18 C14 -37.4(18) . . . . ? F2 Th1 C18 C14 41.5(3) . . . . ? C5 Th1 C18 C14 -124.1(3) . . . . ? C4 Th1 C18 C14 -155.4(3) . . . . ? C17 Th1 C18 C14 112.5(4) . . . . ? C1 Th1 C18 C14 -119.0(3) . . . . ? C2 Th1 C18 C14 -145.4(3) . . . . ? C3 Th1 C18 C14 -166.7(3) . . . . ? C15 C14 C19 C20 154.1(4) . . . . ? C18 C14 C19 C20 -39.1(6) . . . . ? Th1 C14 C19 C20 52.7(5) . . . . ? C15 C14 C19 C21 30.4(6) . . . . ? C18 C14 C19 C21 -162.8(4) . . . . ? Th1 C14 C19 C21 -71.0(4) . . . . ? C15 C14 C19 C22 -87.7(5) . . . . ? C18 C14 C19 C22 79.1(5) . . . . ? Th1 C14 C19 C22 171.0(3) . . . . ? C17 C16 C23 C26 167.9(4) . . . . ? C15 C16 C23 C26 -29.7(6) . . . . ? Th1 C16 C23 C26 72.9(5) . . . . ? C17 C16 C23 C24 43.4(6) . . . . ? C15 C16 C23 C24 -154.2(4) . . . . ? Th1 C16 C23 C24 -51.6(5) . . . . ? C17 C16 C23 C25 -75.1(5) . . . . ? C15 C16 C23 C25 87.3(5) . . . . ? Th1 C16 C23 C25 -170.1(3) . . . . ? F5 Th2 C27 C31 -71.8(3) . . . . ? F2 Th2 C27 C31 125.9(3) . . . . ? F3 Th2 C27 C31 141.1(3) . . . . ? F1 Th2 C27 C31 -157.7(2) . . . . ? N2 Th2 C27 C31 7.8(3) . . . . ? N1 Th2 C27 C31 66.3(3) . . . . ? C30 Th2 C27 C31 -36.9(2) . . . . ? C29 Th2 C27 C31 -76.8(3) . . . . ? C28 Th2 C27 C31 -112.2(4) . . . . ? Th1 Th2 C27 C31 162.4(2) . . . . ? F5 Th2 C27 C28 40.4(3) . . . . ? F2 Th2 C27 C28 -121.9(3) . . . . ? F3 Th2 C27 C28 -106.6(3) . . . . ? F1 Th2 C27 C28 -45.5(3) . . . . ? N2 Th2 C27 C28 120.0(3) . . . . ? N1 Th2 C27 C28 178.5(3) . . . . ? C30 Th2 C27 C28 75.3(3) . . . . ? C31 Th2 C27 C28 112.2(4) . . . . ? C29 Th2 C27 C28 35.4(3) . . . . ? Th1 Th2 C27 C28 -85.4(3) . . . . ? F5 Th2 C27 C32 163.5(3) . . . . ? F2 Th2 C27 C32 1.2(5) . . . . ? F3 Th2 C27 C32 16.5(4) . . . . ? F1 Th2 C27 C32 77.6(4) . . . . ? N2 Th2 C27 C32 -116.9(4) . . . . ? N1 Th2 C27 C32 -58.3(4) . . . . ? C30 Th2 C27 C32 -161.6(5) . . . . ? C31 Th2 C27 C32 -124.7(5) . . . . ? C29 Th2 C27 C32 158.5(5) . . . . ? C28 Th2 C27 C32 123.1(5) . . . . ? Th1 Th2 C27 C32 37.8(4) . . . . ? C31 C27 C28 C29 -3.3(5) . . . . ? C32 C27 C28 C29 164.1(5) . . . . ? Th2 C27 C28 C29 -69.3(4) . . . . ? C31 C27 C28 Th2 66.0(3) . . . . ? C32 C27 C28 Th2 -126.6(5) . . . . ? F5 Th2 C28 C29 -31.7(3) . . . . ? F2 Th2 C28 C29 -131.0(3) . . . . ? F3 Th2 C28 C29 -172.3(3) . . . . ? F1 Th2 C28 C29 -107.5(3) . . . . ? N2 Th2 C28 C29 44.0(3) . . . . ? N1 Th2 C28 C29 113.8(3) . . . . ? C30 Th2 C28 C29 37.8(3) . . . . ? C31 Th2 C28 C29 78.1(3) . . . . ? C27 Th2 C28 C29 115.4(4) . . . . ? Th1 Th2 C28 C29 -136.4(3) . . . . ? F5 Th2 C28 C27 -147.1(3) . . . . ? F2 Th2 C28 C27 113.6(3) . . . . ? F3 Th2 C28 C27 72.3(3) . . . . ? F1 Th2 C28 C27 137.1(3) . . . . ? N2 Th2 C28 C27 -71.4(3) . . . . ? N1 Th2 C28 C27 -1.7(3) . . . . ? C30 Th2 C28 C27 -77.6(3) . . . . ? C31 Th2 C28 C27 -37.3(3) . . . . ? C29 Th2 C28 C27 -115.4(4) . . . . ? Th1 Th2 C28 C27 108.2(3) . . . . ? C27 C28 C29 C30 2.8(6) . . . . ? Th2 C28 C29 C30 -68.3(3) . . . . ? C27 C28 C29 C36 -169.5(5) . . . . ? Th2 C28 C29 C36 119.4(5) . . . . ? C27 C28 C29 Th2 71.1(3) . . . . ? F5 Th2 C29 C28 148.3(3) . . . . ? F2 Th2 C29 C28 113.7(4) . . . . ? F3 Th2 C29 C28 8.9(3) . . . . ? F1 Th2 C29 C28 73.2(3) . . . . ? N2 Th2 C29 C28 -142.3(3) . . . . ? N1 Th2 C29 C28 -83.0(3) . . . . ? C30 Th2 C29 C28 -113.0(4) . . . . ? C31 Th2 C29 C28 -74.9(3) . . . . ? C27 Th2 C29 C28 -35.9(3) . . . . ? Th1 Th2 C29 C28 57.2(3) . . . . ? F5 Th2 C29 C30 -98.8(3) . . . . ? F2 Th2 C29 C30 -133.4(3) . . . . ? F3 Th2 C29 C30 121.8(3) . . . . ? F1 Th2 C29 C30 -173.8(3) . . . . ? N2 Th2 C29 C30 -29.3(3) . . . . ? N1 Th2 C29 C30 30.0(4) . . . . ? C31 Th2 C29 C30 38.1(3) . . . . ? C28 Th2 C29 C30 113.0(4) . . . . ? C27 Th2 C29 C30 77.0(3) . . . . ? Th1 Th2 C29 C30 170.1(2) . . . . ? F5 Th2 C29 C36 23.6(4) . . . . ? F2 Th2 C29 C36 -11.0(7) . . . . ? F3 Th2 C29 C36 -115.8(4) . . . . ? F1 Th2 C29 C36 -51.5(4) . . . . ? N2 Th2 C29 C36 93.0(4) . . . . ? N1 Th2 C29 C36 152.4(4) . . . . ? C30 Th2 C29 C36 122.4(6) . . . . ? C31 Th2 C29 C36 160.5(5) . . . . ? C28 Th2 C29 C36 -124.7(6) . . . . ? C27 Th2 C29 C36 -160.6(5) . . . . ? Th1 Th2 C29 C36 -67.5(5) . . . . ? C28 C29 C30 C31 -1.1(5) . . . . ? C36 C29 C30 C31 171.3(5) . . . . ? Th2 C29 C30 C31 -71.0(3) . . . . ? C28 C29 C30 Th2 69.9(4) . . . . ? C36 C29 C30 Th2 -117.7(5) . . . . ? F5 Th2 C30 C31 -172.4(3) . . . . ? F2 Th2 C30 C31 -119.7(3) . . . . ? F3 Th2 C30 C31 33.3(3) . . . . ? F1 Th2 C30 C31 118.7(3) . . . . ? N2 Th2 C30 C31 -99.4(3) . . . . ? N1 Th2 C30 C31 -44.3(3) . . . . ? C29 Th2 C30 C31 111.2(4) . . . . ? C28 Th2 C30 C31 74.9(3) . . . . ? C27 Th2 C30 C31 35.9(2) . . . . ? Th1 Th2 C30 C31 90.0(4) . . . . ? F5 Th2 C30 C29 76.4(3) . . . . ? F2 Th2 C30 C29 129.1(3) . . . . ? F3 Th2 C30 C29 -77.9(3) . . . . ? F1 Th2 C30 C29 7.5(4) . . . . ? N2 Th2 C30 C29 149.4(3) . . . . ? N1 Th2 C30 C29 -155.5(3) . . . . ? C31 Th2 C30 C29 -111.2(4) . . . . ? C28 Th2 C30 C29 -36.3(3) . . . . ? C27 Th2 C30 C29 -75.3(3) . . . . ? Th1 Th2 C30 C29 -21.2(5) . . . . ? C28 C27 C31 C30 2.6(5) . . . . ? C32 C27 C31 C30 -164.6(4) . . . . ? Th2 C27 C31 C30 69.2(3) . . . . ? C28 C27 C31 Th2 -66.6(3) . . . . ? C32 C27 C31 Th2 126.2(5) . . . . ? C29 C30 C31 C27 -1.0(5) . . . . ? Th2 C30 C31 C27 -72.3(3) . . . . ? C29 C30 C31 Th2 71.3(3) . . . . ? F5 Th2 C31 C27 122.4(3) . . . . ? F2 Th2 C31 C27 -111.3(3) . . . . ? F3 Th2 C31 C27 -40.3(3) . . . . ? F1 Th2 C31 C27 29.8(3) . . . . ? N2 Th2 C31 C27 -172.4(3) . . . . ? N1 Th2 C31 C27 -110.6(3) . . . . ? C30 Th2 C31 C27 114.2(4) . . . . ? C29 Th2 C31 C27 76.2(3) . . . . ? C28 Th2 C31 C27 37.5(3) . . . . ? Th1 Th2 C31 C27 -27.4(3) . . . . ? F5 Th2 C31 C30 8.2(3) . . . . ? F2 Th2 C31 C30 134.5(3) . . . . ? F3 Th2 C31 C30 -154.6(3) . . . . ? F1 Th2 C31 C30 -84.5(3) . . . . ? N2 Th2 C31 C30 73.3(3) . . . . ? N1 Th2 C31 C30 135.2(3) . . . . ? C29 Th2 C31 C30 -38.1(3) . . . . ? C28 Th2 C31 C30 -76.8(3) . . . . ? C27 Th2 C31 C30 -114.2(4) . . . . ? Th1 Th2 C31 C30 -141.6(2) . . . . ? C31 C27 C32 C33 -27.9(7) . . . . ? C28 C27 C32 C33 167.5(4) . . . . ? Th2 C27 C32 C33 69.9(5) . . . . ? C31 C27 C32 C34 -150.7(5) . . . . ? C28 C27 C32 C34 44.7(6) . . . . ? Th2 C27 C32 C34 -52.9(5) . . . . ? C31 C27 C32 C35 89.6(6) . . . . ? C28 C27 C32 C35 -75.0(6) . . . . ? Th2 C27 C32 C35 -172.6(3) . . . . ? C28 C29 C36 C37 -173.1(5) . . . . ? C30 C29 C36 C37 15.9(7) . . . . ? Th2 C29 C36 C37 -76.7(6) . . . . ? C28 C29 C36 C38 -49.9(7) . . . . ? C30 C29 C36 C38 139.1(5) . . . . ? Th2 C29 C36 C38 46.5(6) . . . . ? C28 C29 C36 C39 70.9(7) . . . . ? C30 C29 C36 C39 -100.0(6) . . . . ? Th2 C29 C36 C39 167.4(4) . . . . ? C44 N1 C40 C41 0.5(7) . . . . ? Th2 N1 C40 C41 176.8(4) . . . . ? N1 C40 C41 C42 -0.5(8) . . . . ? C40 C41 C42 C43 0.0(8) . . . . ? C41 C42 C43 C44 0.6(7) . . . . ? C40 N1 C44 C43 0.1(7) . . . . ? Th2 N1 C44 C43 -176.1(3) . . . . ? C40 N1 C44 C45 179.0(4) . . . . ? Th2 N1 C44 C45 2.8(5) . . . . ? C42 C43 C44 N1 -0.6(7) . . . . ? C42 C43 C44 C45 -179.5(4) . . . . ? C49 N2 C45 C46 -0.7(7) . . . . ? Th2 N2 C45 C46 178.2(3) . . . . ? C49 N2 C45 C44 -179.1(4) . . . . ? Th2 N2 C45 C44 -0.2(5) . . . . ? N1 C44 C45 N2 -1.7(6) . . . . ? C43 C44 C45 N2 177.2(4) . . . . ? N1 C44 C45 C46 180.0(4) . . . . ? C43 C44 C45 C46 -1.1(7) . . . . ? N2 C45 C46 C47 -0.4(7) . . . . ? C44 C45 C46 C47 177.8(5) . . . . ? C45 C46 C47 C48 1.8(8) . . . . ? C46 C47 C48 C49 -2.1(8) . . . . ? C45 N2 C49 C48 0.4(7) . . . . ? Th2 N2 C49 C48 -178.5(4) . . . . ? C47 C48 C49 N2 1.0(8) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 0.000 0.500 567 124 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.321 _refine_diff_density_min -1.744 _refine_diff_density_rms 0.131 # Attachment '- compound 6.cif' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 860420' #TrackingRef '- compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H52 Se2 Th' _chemical_formula_sum 'C38 H52 Se2 Th' _chemical_formula_weight 898.76 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' Se Se -0.0929 2.2259 '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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 12.0333(16) _cell_length_b 16.165(2) _cell_length_c 19.461(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.175(2) _cell_angle_gamma 90.00 _cell_volume 3670.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4755 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 6.069 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2252 _exptl_absorpt_correction_T_max 0.3486 _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 17883 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.25 _reflns_number_total 9247 _reflns_number_gt 7973 _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^)+(0.0169P)^2^+18.0766P] 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 0.007(10) _refine_ls_number_reflns 9247 _refine_ls_number_parameters 762 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0086(10) 1.1064(8) 0.1100(7) 0.036(3) Uani 1 1 d . . . C2 C 1.0942(10) 1.0687(8) 0.0847(7) 0.035(3) Uani 1 1 d . . . H2 H 1.1265 1.0907 0.0487 0.043 Uiso 1 1 calc R . . C3 C 1.1265(10) 0.9933(8) 0.1200(6) 0.030(3) Uani 1 1 d U . . C4 C 1.0539(10) 0.9815(8) 0.1663(6) 0.035(3) Uani 1 1 d U . . H4 H 1.0534 0.9355 0.1966 0.042 Uiso 1 1 calc R . . C5 C 0.9820(12) 1.0520(10) 0.1586(7) 0.052(4) Uani 1 1 d . . . H5 H 0.9239 1.0608 0.1832 0.063 Uiso 1 1 calc R . . C6 C 0.9692(11) 1.1944(9) 0.0991(8) 0.048(4) Uani 1 1 d . . . C7 C 1.0308(12) 1.2443(10) 0.1659(10) 0.072(6) Uani 1 1 d . . . H7A H 1.0056 1.2242 0.2071 0.108 Uiso 1 1 calc R . . H7B H 1.0117 1.3031 0.1584 0.108 Uiso 1 1 calc R . . H7C H 1.1139 1.2370 0.1741 0.108 Uiso 1 1 calc R . . C8 C 0.8389(11) 1.2036(8) 0.0892(9) 0.053(4) Uani 1 1 d . . . H8A H 0.7988 1.1755 0.0455 0.080 Uiso 1 1 calc R . . H8B H 0.8184 1.2624 0.0862 0.080 Uiso 1 1 calc R . . H8C H 0.8164 1.1786 0.1296 0.080 Uiso 1 1 calc R . . C9 C 0.9995(13) 1.2371(8) 0.0353(9) 0.057(4) Uani 1 1 d . . . H9A H 1.0829 1.2367 0.0416 0.086 Uiso 1 1 calc R . . H9B H 0.9719 1.2943 0.0319 0.086 Uiso 1 1 calc R . . H9C H 0.9631 1.2073 -0.0083 0.086 Uiso 1 1 calc R . . C10 C 1.2400(11) 0.9450(8) 0.1260(7) 0.040(3) Uani 1 1 d . . . C11 C 1.3331(11) 0.9929(9) 0.1805(8) 0.047(4) Uani 1 1 d U . . H11A H 1.3164 0.9899 0.2273 0.070 Uiso 1 1 calc R . . H11B H 1.3334 1.0510 0.1659 0.070 Uiso 1 1 calc R . . H11C H 1.4083 0.9683 0.1829 0.070 Uiso 1 1 calc R . . C12 C 1.2349(13) 0.8577(9) 0.1534(8) 0.058(4) Uani 1 1 d . . . H12A H 1.1822 0.8245 0.1175 0.087 Uiso 1 1 calc R . . H12B H 1.2076 0.8591 0.1969 0.087 Uiso 1 1 calc R . . H12C H 1.3115 0.8329 0.1635 0.087 Uiso 1 1 calc R . . C13 C 1.2728(12) 0.9451(10) 0.0551(8) 0.052(4) Uani 1 1 d . . . H13A H 1.3502 0.9223 0.0614 0.078 Uiso 1 1 calc R . . H13B H 1.2712 1.0020 0.0373 0.078 Uiso 1 1 calc R . . H13C H 1.2182 0.9112 0.0209 0.078 Uiso 1 1 calc R . . C14 C 0.6591(11) 0.9534(9) -0.0315(7) 0.033(3) Uani 1 1 d . . . C15 C 0.6903(9) 0.8856(7) 0.0142(6) 0.025(2) Uani 1 1 d U . . H15 H 0.6911 0.8300 -0.0015 0.029 Uiso 1 1 calc R . . C16 C 0.7199(10) 0.9094(8) 0.0850(6) 0.035(3) Uani 1 1 d . . . C17 C 0.7122(10) 0.9984(8) 0.0854(6) 0.033(3) Uani 1 1 d . . . H17 H 0.7290 1.0329 0.1262 0.040 Uiso 1 1 calc R . . C18 C 0.6750(10) 1.0252(8) 0.0139(6) 0.033(3) Uani 1 1 d . . . H18 H 0.6626 1.0810 -0.0014 0.039 Uiso 1 1 calc R . . C19 C 0.5908(10) 0.9518(8) -0.1083(6) 0.033(3) Uani 1 1 d . . . C20 C 0.5655(11) 1.0385(7) -0.1392(7) 0.034(3) Uani 1 1 d . . . H20A H 0.5103 1.0659 -0.1172 0.051 Uiso 1 1 calc R . . H20B H 0.5334 1.0347 -0.1905 0.051 Uiso 1 1 calc R . . H20C H 0.6367 1.0707 -0.1297 0.051 Uiso 1 1 calc R . . C21 C 0.4772(11) 0.9097(9) -0.1087(8) 0.046(4) Uani 1 1 d . . . H21A H 0.4920 0.8575 -0.0825 0.069 Uiso 1 1 calc R . . H21B H 0.4352 0.8987 -0.1577 0.069 Uiso 1 1 calc R . . H21C H 0.4313 0.9460 -0.0861 0.069 Uiso 1 1 calc R . . C22 C 0.6513(11) 0.9025(8) -0.1564(6) 0.039(3) Uani 1 1 d U . . H22A H 0.7217 0.9312 -0.1593 0.059 Uiso 1 1 calc R . . H22B H 0.6003 0.8977 -0.2040 0.059 Uiso 1 1 calc R . . H22C H 0.6704 0.8471 -0.1365 0.059 Uiso 1 1 calc R . . C23 C 0.7367(12) 0.8567(9) 0.1511(7) 0.040(3) Uani 1 1 d . . . C24 C 0.6197(12) 0.8104(9) 0.1437(8) 0.053(4) Uani 1 1 d U . . H24A H 0.6232 0.7769 0.1861 0.080 Uiso 1 1 calc R . . H24B H 0.6051 0.7745 0.1019 0.080 Uiso 1 1 calc R . . H24C H 0.5577 0.8510 0.1385 0.080 Uiso 1 1 calc R . . C25 C 0.8294(13) 0.7930(9) 0.1531(8) 0.053(4) Uani 1 1 d . . . H25A H 0.9046 0.8197 0.1669 0.080 Uiso 1 1 calc R . . H25B H 0.8192 0.7682 0.1060 0.080 Uiso 1 1 calc R . . H25C H 0.8244 0.7498 0.1875 0.080 Uiso 1 1 calc R . . C26 C 0.7622(16) 0.9040(10) 0.2182(8) 0.067(5) Uani 1 1 d . . . H26A H 0.7682 0.8659 0.2581 0.100 Uiso 1 1 calc R . . H26B H 0.7005 0.9438 0.2174 0.100 Uiso 1 1 calc R . . H26C H 0.8348 0.9337 0.2235 0.100 Uiso 1 1 calc R . . C27 C 1.0186(11) 1.0798(9) -0.1112(7) 0.037(3) Uani 1 1 d . . . C28 C 1.0899(13) 1.0162(9) -0.1150(8) 0.051(4) Uani 1 1 d . . . H28 H 1.0672 0.9617 -0.1063 0.062 Uiso 1 1 calc R . . C29 C 1.1935(12) 1.0277(11) -0.1307(8) 0.055(4) Uani 1 1 d . . . H29 H 1.2417 0.9817 -0.1327 0.066 Uiso 1 1 calc R . . C30 C 1.2268(12) 1.1052(12) -0.1433(8) 0.062(5) Uani 1 1 d . . . H30 H 1.3003 1.1133 -0.1521 0.075 Uiso 1 1 calc R . . C31 C 1.1550(14) 1.1736(10) -0.1436(8) 0.058(4) Uani 1 1 d U . . H31 H 1.1765 1.2276 -0.1549 0.070 Uiso 1 1 calc R . . C32 C 1.0511(13) 1.1591(8) -0.1268(9) 0.057(4) Uani 1 1 d . . . H32 H 1.0009 1.2042 -0.1259 0.068 Uiso 1 1 calc R . . C33 C 0.8871(10) 0.7636(7) -0.0737(6) 0.030(3) Uani 1 1 d . . . C34 C 0.8045(10) 0.7092(8) -0.0597(8) 0.034(3) Uani 1 1 d . . . H34 H 0.8009 0.6996 -0.0121 0.041 Uiso 1 1 calc R . . C35 C 0.7278(11) 0.6691(8) -0.1150(7) 0.035(3) Uani 1 1 d . . . H35 H 0.6719 0.6326 -0.1049 0.042 Uiso 1 1 calc R . . C36 C 0.7327(11) 0.6819(8) -0.1829(7) 0.038(3) Uani 1 1 d . . . H36 H 0.6805 0.6548 -0.2208 0.046 Uiso 1 1 calc R . . C37 C 0.8159(10) 0.7356(8) -0.1964(7) 0.039(3) Uani 1 1 d . . . H37 H 0.8197 0.7458 -0.2438 0.046 Uiso 1 1 calc R . . C38 C 0.8907(10) 0.7731(7) -0.1425(7) 0.032(3) Uani 1 1 d . . . H38 H 0.9484 0.8075 -0.1531 0.038 Uiso 1 1 calc R . . C39 C 0.1547(9) 0.4874(7) -0.0349(6) 0.026(3) Uani 1 1 d . . . C40 C 0.1930(11) 0.5527(7) 0.0135(6) 0.032(3) Uani 1 1 d . . . H40 H 0.1969 0.6092 0.0009 0.038 Uiso 1 1 calc R . . C41 C 0.2251(10) 0.5211(7) 0.0845(6) 0.031(3) Uani 1 1 d . . . C42 C 0.2114(11) 0.4332(8) 0.0783(7) 0.039(3) Uani 1 1 d . . . H42 H 0.2265 0.3945 0.1162 0.047 Uiso 1 1 calc R . . C43 C 0.1708(9) 0.4144(7) 0.0048(6) 0.024(2) Uani 1 1 d U . . H43 H 0.1568 0.3603 -0.0143 0.029 Uiso 1 1 calc R . . C44 C 0.0842(9) 0.4995(8) -0.1108(6) 0.031(3) Uani 1 1 d . . . C45 C 0.0600(10) 0.4173(8) -0.1508(7) 0.038(3) Uani 1 1 d . . . H45A H 0.1322 0.3934 -0.1562 0.056 Uiso 1 1 calc R . . H45B H 0.0090 0.4270 -0.1977 0.056 Uiso 1 1 calc R . . H45C H 0.0233 0.3790 -0.1241 0.056 Uiso 1 1 calc R . . C46 C 0.1396(11) 0.5598(7) -0.1518(6) 0.035(3) Uani 1 1 d . . . H46A H 0.1547 0.6121 -0.1258 0.053 Uiso 1 1 calc R . . H46B H 0.0880 0.5697 -0.1985 0.053 Uiso 1 1 calc R . . H46C H 0.2119 0.5366 -0.1577 0.053 Uiso 1 1 calc R . . C47 C -0.0322(10) 0.5343(8) -0.1050(7) 0.038(3) Uani 1 1 d . . . H47A H -0.0643 0.4986 -0.0740 0.057 Uiso 1 1 calc R . . H47B H -0.0848 0.5362 -0.1522 0.057 Uiso 1 1 calc R . . H47C H -0.0215 0.5902 -0.0850 0.057 Uiso 1 1 calc R . . C48 C 0.2489(13) 0.5726(8) 0.1511(7) 0.041(4) Uani 1 1 d . . . C49 C 0.3398(13) 0.6394(8) 0.1526(7) 0.047(4) Uani 1 1 d . . . H49A H 0.3209 0.6704 0.1079 0.071 Uiso 1 1 calc R . . H49B H 0.4151 0.6133 0.1587 0.071 Uiso 1 1 calc R . . H49C H 0.3415 0.6773 0.1922 0.071 Uiso 1 1 calc R . . C50 C 0.1346(13) 0.6143(10) 0.1541(8) 0.058(4) Uani 1 1 d . . . H50A H 0.1448 0.6447 0.1988 0.088 Uiso 1 1 calc R . . H50B H 0.0755 0.5719 0.1511 0.088 Uiso 1 1 calc R . . H50C H 0.1112 0.6529 0.1143 0.088 Uiso 1 1 calc R . . C51 C 0.2894(15) 0.5173(9) 0.2167(8) 0.057(4) Uani 1 1 d . . . H51A H 0.3613 0.4900 0.2148 0.086 Uiso 1 1 calc R . . H51B H 0.2309 0.4754 0.2175 0.086 Uiso 1 1 calc R . . H51C H 0.3018 0.5513 0.2596 0.086 Uiso 1 1 calc R . . C52 C 0.5111(9) 0.3275(7) 0.1004(6) 0.025(2) Uani 1 1 d . . . C53 C 0.5951(10) 0.3667(8) 0.0749(7) 0.035(3) Uani 1 1 d . . . H53 H 0.6266 0.3438 0.0389 0.042 Uiso 1 1 calc R . . C54 C 0.6297(10) 0.4434(7) 0.1071(7) 0.025(3) Uani 1 1 d . . . C55 C 0.5567(11) 0.4549(8) 0.1553(6) 0.037(3) Uani 1 1 d . . . H55 H 0.5571 0.5017 0.1849 0.045 Uiso 1 1 calc R . . C56 C 0.4854(11) 0.3858(8) 0.1511(6) 0.035(3) Uani 1 1 d U . . H56 H 0.4291 0.3782 0.1773 0.042 Uiso 1 1 calc R . . C57 C 0.4690(11) 0.2392(8) 0.0955(8) 0.043(4) Uani 1 1 d . . . C58 C 0.3411(10) 0.2311(8) 0.0835(7) 0.043(3) Uani 1 1 d . . . H58A H 0.3204 0.1723 0.0823 0.065 Uiso 1 1 calc R . . H58B H 0.3034 0.2569 0.0383 0.065 Uiso 1 1 calc R . . H58C H 0.3162 0.2586 0.1221 0.065 Uiso 1 1 calc R . . C59 C 0.5334(12) 0.1926(9) 0.1589(9) 0.055(4) Uani 1 1 d . . . H59A H 0.5223 0.2193 0.2019 0.082 Uiso 1 1 calc R . . H59B H 0.6151 0.1923 0.1597 0.082 Uiso 1 1 calc R . . H59C H 0.5050 0.1356 0.1566 0.082 Uiso 1 1 calc R . . C60 C 0.4978(12) 0.1974(7) 0.0296(8) 0.045(3) Uani 1 1 d . . . H60A H 0.4908 0.1372 0.0331 0.068 Uiso 1 1 calc R . . H60B H 0.5764 0.2116 0.0281 0.068 Uiso 1 1 calc R . . H60C H 0.4443 0.2172 -0.0136 0.068 Uiso 1 1 calc R . . C61 C 0.7409(10) 0.4897(7) 0.1125(6) 0.032(3) Uani 1 1 d U . . C62 C 0.8344(11) 0.4417(9) 0.1647(8) 0.044(4) Uani 1 1 d . . . H62A H 0.8961 0.4796 0.1873 0.066 Uiso 1 1 calc R . . H62B H 0.8652 0.3985 0.1393 0.066 Uiso 1 1 calc R . . H62C H 0.8017 0.4162 0.2010 0.066 Uiso 1 1 calc R . . C63 C 0.7710(12) 0.4904(9) 0.0401(7) 0.050(4) Uani 1 1 d . . . H63A H 0.7174 0.5265 0.0074 0.075 Uiso 1 1 calc R . . H63B H 0.7655 0.4341 0.0208 0.075 Uiso 1 1 calc R . . H63C H 0.8494 0.5111 0.0458 0.075 Uiso 1 1 calc R . . C64 C 0.7413(13) 0.5763(8) 0.1412(8) 0.054(4) Uani 1 1 d . . . H64A H 0.6826 0.6094 0.1090 0.081 Uiso 1 1 calc R . . H64B H 0.8167 0.6014 0.1452 0.081 Uiso 1 1 calc R . . H64C H 0.7249 0.5744 0.1881 0.081 Uiso 1 1 calc R . . C65 C 0.3910(9) 0.6822(6) -0.0743(6) 0.026(3) Uani 1 1 d U . . C66 C 0.3168(11) 0.7353(7) -0.0510(7) 0.034(3) Uani 1 1 d U . . H66 H 0.3176 0.7373 -0.0021 0.041 Uiso 1 1 calc R . . C67 C 0.2405(11) 0.7860(8) -0.0997(8) 0.040(3) Uani 1 1 d . . . H67 H 0.1903 0.8227 -0.0839 0.048 Uiso 1 1 calc R . . C68 C 0.2396(11) 0.7818(8) -0.1699(8) 0.044(3) Uani 1 1 d . . . H68 H 0.1895 0.8166 -0.2029 0.053 Uiso 1 1 calc R . . C69 C 0.3110(11) 0.7272(8) -0.1939(6) 0.038(3) Uani 1 1 d . . . H69 H 0.3090 0.7246 -0.2430 0.045 Uiso 1 1 calc R . . C70 C 0.3856(10) 0.6760(7) -0.1461(6) 0.035(3) Uani 1 1 d . . . H70 H 0.4324 0.6372 -0.1626 0.041 Uiso 1 1 calc R . . C71 C 0.5137(10) 0.3639(8) -0.1242(7) 0.033(3) Uani 1 1 d . . . C72 C 0.5711(10) 0.4365(7) -0.1359(7) 0.035(3) Uani 1 1 d . . . H72 H 0.5377 0.4891 -0.1325 0.042 Uiso 1 1 calc R . . C73 C 0.6752(11) 0.4307(8) -0.1523(7) 0.042(3) Uani 1 1 d . . . H73 H 0.7140 0.4796 -0.1600 0.051 Uiso 1 1 calc R . . C74 C 0.7244(12) 0.3543(9) -0.1575(7) 0.046(3) Uani 1 1 d . . . H74 H 0.7962 0.3503 -0.1695 0.056 Uiso 1 1 calc R . . C75 C 0.6689(11) 0.2861(9) -0.1455(8) 0.048(4) Uani 1 1 d . . . H75 H 0.7043 0.2340 -0.1481 0.058 Uiso 1 1 calc R . . C76 C 0.5644(12) 0.2871(9) -0.1298(8) 0.049(4) Uani 1 1 d . . . H76 H 0.5272 0.2371 -0.1229 0.059 Uiso 1 1 calc R . . Se1 Se 0.86997(11) 1.06517(9) -0.09249(8) 0.0432(3) Uani 1 1 d . . . Se2 Se 0.99813(11) 0.81411(7) 0.00259(7) 0.0345(3) Uani 1 1 d . . . Se3 Se 0.49896(11) 0.61767(7) -0.00556(7) 0.0344(3) Uani 1 1 d . . . Se4 Se 0.36393(11) 0.36924(8) -0.10407(7) 0.0328(3) Uani 1 1 d . . . Th1 Th 0.89934(3) 0.96911(3) 0.03371(2) 0.02907(14) Uani 1 1 d . . . Th2 Th 0.39774(3) 0.46423(3) 0.02417(2) 0.02787(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(7) 0.043(8) 0.033(7) -0.006(6) 0.005(5) -0.004(6) C2 0.033(7) 0.042(8) 0.030(7) 0.004(6) 0.006(6) -0.001(6) C3 0.020(5) 0.036(6) 0.028(6) 0.002(5) -0.005(5) -0.008(5) C4 0.030(6) 0.046(6) 0.024(5) 0.006(5) -0.005(5) -0.002(5) C5 0.038(8) 0.074(11) 0.039(8) -0.022(7) -0.003(6) -0.015(8) C6 0.032(7) 0.037(8) 0.070(10) -0.020(7) 0.005(7) -0.005(6) C7 0.034(8) 0.056(11) 0.110(15) -0.038(10) -0.015(9) -0.001(7) C8 0.032(7) 0.036(8) 0.090(12) -0.015(7) 0.011(7) -0.002(6) C9 0.046(9) 0.027(7) 0.099(13) 0.016(8) 0.018(8) 0.004(6) C10 0.030(7) 0.034(7) 0.049(8) -0.013(6) -0.002(6) -0.003(5) C11 0.034(6) 0.049(7) 0.045(7) -0.009(6) -0.012(5) 0.001(6) C12 0.052(9) 0.045(9) 0.058(10) 0.001(7) -0.024(7) -0.008(7) C13 0.033(8) 0.064(10) 0.057(10) -0.015(7) 0.007(7) -0.001(7) C14 0.021(6) 0.040(8) 0.035(8) 0.001(6) 0.003(5) -0.001(5) C15 0.024(5) 0.020(5) 0.029(6) -0.006(4) 0.005(4) -0.012(4) C16 0.034(7) 0.041(8) 0.030(7) -0.001(5) 0.008(5) -0.016(6) C17 0.031(7) 0.037(7) 0.031(7) -0.020(5) 0.006(5) -0.007(5) C18 0.025(6) 0.035(7) 0.040(7) -0.007(5) 0.008(5) -0.003(5) C19 0.024(6) 0.038(7) 0.035(7) 0.003(5) 0.002(5) 0.000(5) C20 0.031(7) 0.028(7) 0.041(7) -0.007(5) 0.004(5) 0.001(5) C21 0.025(7) 0.045(9) 0.061(10) 0.004(7) -0.003(6) -0.013(6) C22 0.044(6) 0.037(6) 0.029(6) -0.012(5) -0.006(5) 0.006(5) C23 0.046(8) 0.048(8) 0.031(8) 0.009(6) 0.016(6) -0.011(7) C24 0.054(7) 0.051(7) 0.056(7) 0.006(6) 0.018(6) -0.017(6) C25 0.069(10) 0.044(9) 0.048(9) 0.025(7) 0.017(8) -0.005(7) C26 0.090(13) 0.052(10) 0.057(11) 0.021(8) 0.015(9) -0.009(9) C27 0.032(7) 0.045(8) 0.032(8) 0.008(6) 0.003(6) -0.001(6) C28 0.059(10) 0.037(8) 0.057(10) 0.013(7) 0.012(8) 0.003(7) C29 0.036(8) 0.074(12) 0.058(10) 0.023(8) 0.020(7) 0.014(7) C30 0.022(7) 0.101(14) 0.063(10) 0.000(9) 0.007(7) -0.008(8) C31 0.068(8) 0.043(7) 0.071(8) -0.004(6) 0.032(6) -0.025(6) C32 0.056(9) 0.028(8) 0.097(13) 0.008(8) 0.037(9) 0.007(7) C33 0.028(6) 0.028(6) 0.033(7) -0.005(5) 0.005(5) 0.007(5) C34 0.027(7) 0.036(7) 0.045(8) 0.004(6) 0.018(6) -0.005(6) C35 0.029(7) 0.028(7) 0.047(8) -0.010(6) 0.011(6) -0.002(5) C36 0.036(7) 0.036(7) 0.037(8) -0.015(6) 0.000(6) 0.001(6) C37 0.039(7) 0.044(8) 0.030(7) 0.004(6) 0.005(6) 0.010(6) C38 0.024(6) 0.021(6) 0.052(8) -0.002(5) 0.012(6) 0.003(5) C39 0.017(6) 0.034(7) 0.030(7) 0.006(5) 0.011(5) 0.006(5) C40 0.046(7) 0.028(7) 0.026(6) 0.003(5) 0.019(6) -0.004(5) C41 0.038(7) 0.034(7) 0.024(6) 0.001(5) 0.013(5) -0.015(5) C42 0.040(7) 0.042(8) 0.035(7) 0.009(6) 0.008(6) -0.015(6) C43 0.024(4) 0.022(4) 0.025(4) 0.003(3) 0.007(3) -0.007(3) C44 0.022(6) 0.039(7) 0.036(7) 0.004(5) 0.011(5) 0.006(5) C45 0.031(7) 0.038(7) 0.041(8) -0.009(6) 0.003(6) 0.002(6) C46 0.042(7) 0.029(7) 0.033(7) 0.002(5) 0.007(6) -0.007(6) C47 0.019(6) 0.045(8) 0.048(8) 0.000(6) 0.006(6) 0.001(5) C48 0.064(10) 0.034(8) 0.026(7) 0.009(6) 0.014(7) -0.003(7) C49 0.067(10) 0.040(8) 0.038(8) -0.011(6) 0.021(7) -0.012(7) C50 0.059(10) 0.076(11) 0.045(9) -0.013(8) 0.022(7) -0.001(8) C51 0.090(12) 0.041(9) 0.042(9) 0.000(6) 0.019(8) -0.014(8) C52 0.021(6) 0.031(6) 0.019(6) 0.004(5) -0.004(4) -0.003(5) C53 0.030(7) 0.027(7) 0.042(8) 0.004(6) -0.003(6) -0.008(5) C54 0.017(6) 0.020(6) 0.033(7) 0.006(5) -0.001(5) 0.000(5) C55 0.039(7) 0.040(8) 0.028(6) 0.004(5) -0.002(5) -0.004(6) C56 0.039(6) 0.039(6) 0.027(6) 0.013(5) 0.011(5) -0.007(5) C57 0.038(8) 0.033(8) 0.057(10) 0.000(7) 0.012(7) -0.013(6) C58 0.037(7) 0.036(7) 0.049(8) 0.010(6) -0.003(6) -0.006(6) C59 0.041(8) 0.041(9) 0.069(11) 0.025(8) -0.011(8) -0.010(7) C60 0.044(8) 0.020(6) 0.072(10) 0.012(6) 0.015(7) 0.003(6) C61 0.033(6) 0.024(5) 0.037(6) -0.001(4) 0.001(5) -0.014(5) C62 0.033(7) 0.038(8) 0.056(9) 0.007(7) 0.000(6) -0.022(6) C63 0.040(8) 0.057(9) 0.051(9) 0.013(7) 0.006(7) -0.011(7) C64 0.054(9) 0.039(8) 0.057(10) 0.000(7) -0.011(7) -0.009(7) C65 0.024(5) 0.009(5) 0.040(6) 0.002(4) 0.001(5) -0.004(4) C66 0.040(6) 0.022(6) 0.041(6) 0.007(5) 0.010(5) -0.008(5) C67 0.034(7) 0.033(7) 0.056(9) -0.001(6) 0.017(6) 0.003(6) C68 0.032(7) 0.041(8) 0.055(9) 0.012(7) 0.002(6) -0.007(6) C69 0.043(8) 0.041(8) 0.028(7) 0.003(5) 0.007(6) 0.001(6) C70 0.036(7) 0.029(7) 0.038(7) 0.004(5) 0.008(6) -0.001(5) C71 0.032(7) 0.032(7) 0.036(8) 0.004(6) 0.010(6) 0.007(6) C72 0.032(7) 0.015(6) 0.058(9) 0.006(6) 0.012(6) -0.010(5) C73 0.038(7) 0.040(8) 0.055(9) -0.006(6) 0.024(6) -0.011(6) C74 0.040(8) 0.059(10) 0.046(8) -0.010(7) 0.022(6) 0.010(7) C75 0.042(8) 0.042(8) 0.072(10) -0.002(7) 0.037(7) 0.012(7) C76 0.052(9) 0.038(8) 0.065(10) 0.005(7) 0.030(7) 0.007(7) Se1 0.0278(7) 0.0507(9) 0.0482(8) 0.0180(7) 0.0038(6) -0.0057(6) Se2 0.0281(6) 0.0330(7) 0.0400(7) -0.0072(5) 0.0040(5) -0.0048(5) Se3 0.0309(6) 0.0296(7) 0.0413(7) 0.0095(5) 0.0063(5) -0.0084(5) Se4 0.0262(6) 0.0323(7) 0.0411(7) 0.0008(5) 0.0105(5) -0.0042(5) Th1 0.0233(2) 0.0293(3) 0.0305(4) 0.0027(2) -0.0013(2) -0.0067(2) Th2 0.0245(2) 0.0284(2) 0.0283(3) 0.0106(2) 0.0019(2) -0.0078(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.39(2) . ? C1 C2 1.386(18) . ? C1 C6 1.498(19) . ? C1 Th1 2.811(12) . ? C2 C3 1.406(17) . ? C2 Th1 2.817(12) . ? C2 H2 0.9500 . ? C3 C4 1.414(18) . ? C3 C10 1.553(18) . ? C3 Th1 2.863(11) . ? C4 C5 1.416(19) . ? C4 Th1 2.795(11) . ? C4 H4 0.9500 . ? C5 Th1 2.740(13) . ? C5 H5 0.9500 . ? C6 C8 1.540(18) . ? C6 C9 1.54(2) . ? C6 C7 1.554(19) . ? 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 C12 1.516(19) . ? C10 C13 1.53(2) . ? C10 C11 1.549(16) . ? 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 C15 1.403(17) . ? C14 C18 1.442(17) . ? C14 C19 1.520(17) . ? C14 Th1 2.869(12) . ? C15 C16 1.391(16) . ? C15 Th1 2.797(10) . ? C15 H15 0.9500 . ? C16 C17 1.442(18) . ? C16 C23 1.515(17) . ? C16 Th1 2.765(12) . ? C17 C18 1.421(17) . ? C17 Th1 2.723(12) . ? C17 H17 0.9500 . ? C18 Th1 2.784(12) . ? C18 H18 0.9500 . ? C19 C20 1.525(16) . ? C19 C21 1.526(17) . ? C19 C22 1.542(17) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C26 1.48(2) . ? C23 C25 1.51(2) . ? C23 C24 1.570(18) . ? 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 C28 1.352(19) . ? C27 C32 1.395(19) . ? C27 Se1 1.926(14) . ? C28 C29 1.37(2) . ? C28 H28 0.9500 . ? C29 C30 1.36(2) . ? C29 H29 0.9500 . ? C30 C31 1.40(2) . ? C30 H30 0.9500 . ? C31 C32 1.39(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.360(17) . ? C33 C34 1.403(17) . ? C33 Se2 1.919(11) . ? C34 C35 1.394(17) . ? C34 H34 0.9500 . ? C35 C36 1.354(18) . ? C35 H35 0.9500 . ? C36 C37 1.398(18) . ? C36 H36 0.9500 . ? C37 C38 1.347(16) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C43 1.398(15) . ? C39 C40 1.415(17) . ? C39 C44 1.525(16) . ? C39 Th2 2.893(11) . ? C40 C41 1.434(16) . ? C40 Th2 2.812(12) . ? C40 H40 0.9500 . ? C41 C42 1.432(17) . ? C41 C48 1.508(18) . ? C41 Th2 2.781(12) . ? C42 C43 1.426(16) . ? C42 Th2 2.747(13) . ? C42 H42 0.9500 . ? C43 Th2 2.783(10) . ? C43 H43 0.9500 . ? C44 C46 1.514(17) . ? C44 C45 1.531(17) . ? C44 C47 1.539(16) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.532(19) . ? C48 C51 1.537(18) . ? C48 C50 1.55(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.383(17) . ? C52 C56 1.453(17) . ? C52 C57 1.509(16) . ? C52 Th2 2.821(11) . ? C53 C54 1.404(17) . ? C53 Th2 2.820(12) . ? C53 H53 0.9500 . ? C54 C55 1.446(18) . ? C54 C61 1.515(16) . ? C54 Th2 2.882(11) . ? C55 C56 1.399(17) . ? C55 Th2 2.793(11) . ? C55 H55 0.9500 . ? C56 Th2 2.748(11) . ? C56 H56 0.9500 . ? C57 C59 1.489(18) . ? C57 C58 1.505(17) . ? C57 C60 1.56(2) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C64 1.507(18) . ? C61 C62 1.530(18) . ? C61 C63 1.538(19) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C70 1.387(17) . ? C65 C66 1.392(17) . ? C65 Se3 1.927(11) . ? C66 C67 1.410(18) . ? C66 H66 0.9500 . ? C67 C68 1.366(19) . ? C67 H67 0.9500 . ? C68 C69 1.390(19) . ? C68 H68 0.9500 . ? C69 C70 1.395(16) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C76 1.398(17) . ? C71 C72 1.408(16) . ? C71 Se4 1.938(12) . ? C72 C73 1.369(17) . ? C72 H72 0.9500 . ? C73 C74 1.385(19) . ? C73 H73 0.9500 . ? C74 C75 1.34(2) . ? C74 H74 0.9500 . ? C75 C76 1.364(18) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? Se1 Th1 2.8536(15) . ? Se2 Th1 2.9000(14) . ? Se3 Th2 2.8837(12) . ? Se4 Th2 2.8729(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 106.2(13) . . ? C5 C1 C6 125.5(13) . . ? C2 C1 C6 127.2(13) . . ? C5 C1 Th1 72.7(7) . . ? C2 C1 Th1 76.0(7) . . ? C6 C1 Th1 125.7(8) . . ? C1 C2 C3 110.4(12) . . ? C1 C2 Th1 75.5(7) . . ? C3 C2 Th1 77.5(7) . . ? C1 C2 H2 124.8 . . ? C3 C2 H2 124.8 . . ? Th1 C2 H2 114.2 . . ? C2 C3 C4 106.8(11) . . ? C2 C3 C10 127.2(11) . . ? C4 C3 C10 123.6(11) . . ? C2 C3 Th1 73.9(7) . . ? C4 C3 Th1 72.9(6) . . ? C10 C3 Th1 132.1(8) . . ? C3 C4 C5 106.2(12) . . ? C3 C4 Th1 78.2(6) . . ? C5 C4 Th1 73.1(7) . . ? C3 C4 H4 126.9 . . ? C5 C4 H4 126.9 . . ? Th1 C4 H4 114.4 . . ? C1 C5 C4 110.3(13) . . ? C1 C5 Th1 78.4(8) . . ? C4 C5 Th1 77.3(7) . . ? C1 C5 H5 124.9 . . ? C4 C5 H5 124.9 . . ? Th1 C5 H5 111.6 . . ? C1 C6 C8 112.7(12) . . ? C1 C6 C9 114.2(12) . . ? C8 C6 C9 106.9(12) . . ? C1 C6 C7 107.7(12) . . ? C8 C6 C7 108.5(12) . . ? C9 C6 C7 106.5(13) . . ? 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 . . ? C12 C10 C13 111.2(12) . . ? C12 C10 C11 108.0(11) . . ? C13 C10 C11 108.4(12) . . ? C12 C10 C3 112.6(12) . . ? C13 C10 C3 110.5(11) . . ? C11 C10 C3 105.9(10) . . ? 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 . . ? C15 C14 C18 105.4(11) . . ? C15 C14 C19 127.3(11) . . ? C18 C14 C19 125.1(12) . . ? C15 C14 Th1 72.8(6) . . ? C18 C14 Th1 72.0(7) . . ? C19 C14 Th1 132.9(9) . . ? C16 C15 C14 112.0(11) . . ? C16 C15 Th1 74.2(6) . . ? C14 C15 Th1 78.5(7) . . ? C16 C15 H15 124.0 . . ? C14 C15 H15 124.0 . . ? Th1 C15 H15 114.9 . . ? C15 C16 C17 106.3(10) . . ? C15 C16 C23 129.4(11) . . ? C17 C16 C23 123.5(11) . . ? C15 C16 Th1 76.8(7) . . ? C17 C16 Th1 73.2(7) . . ? C23 C16 Th1 123.3(8) . . ? C18 C17 C16 107.7(10) . . ? C18 C17 Th1 77.4(7) . . ? C16 C17 Th1 76.4(7) . . ? C18 C17 H17 126.2 . . ? C16 C17 H17 126.2 . . ? Th1 C17 H17 112.6 . . ? C17 C18 C14 108.5(11) . . ? C17 C18 Th1 72.7(7) . . ? C14 C18 Th1 78.5(7) . . ? C17 C18 H18 125.7 . . ? C14 C18 H18 125.7 . . ? Th1 C18 H18 115.1 . . ? C14 C19 C20 112.3(10) . . ? C14 C19 C21 106.3(11) . . ? C20 C19 C21 108.4(10) . . ? C14 C19 C22 112.5(10) . . ? C20 C19 C22 108.4(10) . . ? C21 C19 C22 108.8(11) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C26 C23 C25 109.8(13) . . ? C26 C23 C16 114.5(12) . . ? C25 C23 C16 110.3(11) . . ? C26 C23 C24 108.4(12) . . ? C25 C23 C24 108.5(12) . . ? C16 C23 C24 105.1(11) . . ? 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 . . ? C28 C27 C32 118.1(14) . . ? C28 C27 Se1 123.2(11) . . ? C32 C27 Se1 118.5(11) . . ? C27 C28 C29 122.3(14) . . ? C27 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? C30 C29 C28 119.5(15) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 121.3(14) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 117.0(14) . . ? C32 C31 H31 121.5 . . ? C30 C31 H31 121.5 . . ? C31 C32 C27 121.6(14) . . ? C31 C32 H32 119.2 . . ? C27 C32 H32 119.2 . . ? C38 C33 C34 117.2(11) . . ? C38 C33 Se2 122.0(9) . . ? C34 C33 Se2 120.6(10) . . ? C35 C34 C33 120.5(12) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 120.3(12) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 118.8(11) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 120.5(12) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C33 122.6(12) . . ? C37 C38 H38 118.7 . . ? C33 C38 H38 118.7 . . ? C43 C39 C40 106.4(10) . . ? C43 C39 C44 127.8(11) . . ? C40 C39 C44 124.3(11) . . ? C43 C39 Th2 71.4(6) . . ? C40 C39 Th2 72.5(7) . . ? C44 C39 Th2 132.1(7) . . ? C39 C40 C41 110.1(10) . . ? C39 C40 Th2 78.8(7) . . ? C41 C40 Th2 74.0(7) . . ? C39 C40 H40 125.0 . . ? C41 C40 H40 125.0 . . ? Th2 C40 H40 114.2 . . ? C42 C41 C40 105.9(10) . . ? C42 C41 C48 127.9(11) . . ? C40 C41 C48 125.5(11) . . ? C42 C41 Th2 73.7(7) . . ? C40 C41 Th2 76.4(7) . . ? C48 C41 Th2 122.8(9) . . ? C43 C42 C41 107.5(10) . . ? C43 C42 Th2 76.4(7) . . ? C41 C42 Th2 76.3(7) . . ? C43 C42 H42 126.3 . . ? C41 C42 H42 126.3 . . ? Th2 C42 H42 113.5 . . ? C39 C43 C42 110.0(10) . . ? C39 C43 Th2 80.2(6) . . ? C42 C43 Th2 73.7(6) . . ? C39 C43 H43 125.0 . . ? C42 C43 H43 125.0 . . ? Th2 C43 H43 113.2 . . ? C46 C44 C39 112.4(10) . . ? C46 C44 C45 110.1(10) . . ? C39 C44 C45 111.9(10) . . ? C46 C44 C47 109.2(10) . . ? C39 C44 C47 106.0(10) . . ? C45 C44 C47 107.0(10) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C41 C48 C49 113.0(11) . . ? C41 C48 C51 110.3(11) . . ? C49 C48 C51 108.3(12) . . ? C41 C48 C50 106.9(11) . . ? C49 C48 C50 109.3(12) . . ? C51 C48 C50 109.0(12) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C56 104.0(10) . . ? C53 C52 C57 132.5(12) . . ? C56 C52 C57 122.1(11) . . ? C53 C52 Th2 75.8(7) . . ? C56 C52 Th2 72.1(6) . . ? C57 C52 Th2 126.6(7) . . ? C52 C53 C54 114.1(13) . . ? C52 C53 Th2 75.9(7) . . ? C54 C53 Th2 78.2(7) . . ? C52 C53 H53 122.9 . . ? C54 C53 H53 122.9 . . ? Th2 C53 H53 114.4 . . ? C53 C54 C55 104.0(11) . . ? C53 C54 C61 128.9(12) . . ? C55 C54 C61 124.0(11) . . ? C53 C54 Th2 73.3(7) . . ? C55 C54 Th2 71.9(6) . . ? C61 C54 Th2 134.3(8) . . ? C56 C55 C54 108.7(11) . . ? C56 C55 Th2 73.6(7) . . ? C54 C55 Th2 78.7(7) . . ? C56 C55 H55 125.6 . . ? C54 C55 H55 125.6 . . ? Th2 C55 H55 114.3 . . ? C55 C56 C52 109.1(11) . . ? C55 C56 Th2 77.2(7) . . ? C52 C56 Th2 77.7(6) . . ? C55 C56 H56 125.4 . . ? C52 C56 H56 125.4 . . ? Th2 C56 H56 112.0 . . ? C59 C57 C58 112.9(12) . . ? C59 C57 C52 109.1(11) . . ? C58 C57 C52 114.1(11) . . ? C59 C57 C60 106.6(12) . . ? C58 C57 C60 105.0(11) . . ? C52 C57 C60 108.7(11) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C64 C61 C54 114.0(11) . . ? C64 C61 C62 106.8(10) . . ? C54 C61 C62 106.7(9) . . ? C64 C61 C63 110.7(11) . . ? C54 C61 C63 110.0(10) . . ? C62 C61 C63 108.2(11) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C70 C65 C66 119.8(11) . . ? C70 C65 Se3 121.2(9) . . ? C66 C65 Se3 119.0(9) . . ? C65 C66 C67 120.3(12) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C68 C67 C66 119.2(13) . . ? C68 C67 H67 120.4 . . ? C66 C67 H67 120.4 . . ? C67 C68 C69 120.9(12) . . ? C67 C68 H68 119.5 . . ? C69 C68 H68 119.5 . . ? C68 C69 C70 120.1(12) . . ? C68 C69 H69 119.9 . . ? C70 C69 H69 119.9 . . ? C65 C70 C69 119.6(12) . . ? C65 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C76 C71 C72 119.1(12) . . ? C76 C71 Se4 120.1(10) . . ? C72 C71 Se4 120.8(9) . . ? C73 C72 C71 119.5(12) . . ? C73 C72 H72 120.2 . . ? C71 C72 H72 120.2 . . ? C72 C73 C74 120.7(12) . . ? C72 C73 H73 119.6 . . ? C74 C73 H73 119.6 . . ? C75 C74 C73 118.7(13) . . ? C75 C74 H74 120.6 . . ? C73 C74 H74 120.6 . . ? C74 C75 C76 123.7(13) . . ? C74 C75 H75 118.2 . . ? C76 C75 H75 118.2 . . ? C75 C76 C71 118.2(13) . . ? C75 C76 H76 120.9 . . ? C71 C76 H76 120.9 . . ? C27 Se1 Th1 107.8(4) . . ? C33 Se2 Th1 106.6(3) . . ? C65 Se3 Th2 111.0(3) . . ? C71 Se4 Th2 105.0(4) . . ? C17 Th1 C5 75.0(4) . . ? C17 Th1 C16 30.5(4) . . ? C5 Th1 C16 89.8(4) . . ? C17 Th1 C18 29.9(4) . . ? C5 Th1 C18 95.3(4) . . ? C16 Th1 C18 49.2(4) . . ? C17 Th1 C4 94.0(4) . . ? C5 Th1 C4 29.6(4) . . ? C16 Th1 C4 95.4(4) . . ? C18 Th1 C4 120.5(4) . . ? C17 Th1 C15 48.5(3) . . ? C5 Th1 C15 118.4(4) . . ? C16 Th1 C15 29.0(3) . . ? C18 Th1 C15 47.9(3) . . ? C4 Th1 C15 122.2(3) . . ? C17 Th1 C1 89.4(4) . . ? C5 Th1 C1 28.9(4) . . ? C16 Th1 C1 113.0(4) . . ? C18 Th1 C1 97.4(4) . . ? C4 Th1 C1 48.4(4) . . ? C15 Th1 C1 137.9(4) . . ? C17 Th1 C2 117.6(4) . . ? C5 Th1 C2 47.0(4) . . ? C16 Th1 C2 136.8(4) . . ? C18 Th1 C2 123.9(4) . . ? C4 Th1 C2 47.6(4) . . ? C15 Th1 C2 165.2(4) . . ? C1 Th1 C2 28.5(4) . . ? C17 Th1 Se1 106.5(3) . . ? C5 Th1 Se1 116.0(3) . . ? C16 Th1 Se1 123.9(3) . . ? C18 Th1 Se1 78.0(3) . . ? C4 Th1 Se1 132.1(3) . . ? C15 Th1 Se1 103.2(2) . . ? C1 Th1 Se1 88.2(3) . . ? C2 Th1 Se1 84.8(3) . . ? C17 Th1 C3 121.1(4) . . ? C5 Th1 C3 47.6(4) . . ? C16 Th1 C3 123.6(4) . . ? C18 Th1 C3 142.3(4) . . ? C4 Th1 C3 28.9(4) . . ? C15 Th1 C3 147.5(3) . . ? C1 Th1 C3 47.6(4) . . ? C2 Th1 C3 28.6(3) . . ? Se1 Th1 C3 109.2(2) . . ? C17 Th1 C14 49.0(4) . . ? C5 Th1 C14 122.9(4) . . ? C16 Th1 C14 48.5(4) . . ? C18 Th1 C14 29.5(3) . . ? C4 Th1 C14 141.7(4) . . ? C15 Th1 C14 28.6(4) . . ? C1 Th1 C14 126.4(4) . . ? C2 Th1 C14 150.2(4) . . ? Se1 Th1 C14 76.6(3) . . ? C3 Th1 C14 170.1(4) . . ? C17 Th1 Se2 130.2(3) . . ? C5 Th1 Se2 122.0(3) . . ? C16 Th1 Se2 99.8(3) . . ? C18 Th1 Se2 133.3(2) . . ? C4 Th1 Se2 92.3(3) . . ? C15 Th1 Se2 87.4(2) . . ? C1 Th1 Se2 129.0(3) . . ? C2 Th1 Se2 102.7(3) . . ? Se1 Th1 Se2 105.13(5) . . ? C3 Th1 Se2 81.9(3) . . ? C14 Th1 Se2 104.6(3) . . ? C42 Th2 C56 75.0(4) . . ? C42 Th2 C41 30.0(4) . . ? C56 Th2 C41 86.3(4) . . ? C42 Th2 C43 29.9(3) . . ? C56 Th2 C43 97.8(3) . . ? C41 Th2 C43 48.9(3) . . ? C42 Th2 C55 94.6(4) . . ? C56 Th2 C55 29.2(3) . . ? C41 Th2 C55 92.7(4) . . ? C43 Th2 C55 122.5(3) . . ? C42 Th2 C40 48.6(4) . . ? C56 Th2 C40 115.9(4) . . ? C41 Th2 C40 29.7(3) . . ? C43 Th2 C40 47.5(3) . . ? C55 Th2 C40 119.1(4) . . ? C42 Th2 C53 117.4(4) . . ? C56 Th2 C53 47.3(4) . . ? C41 Th2 C53 133.6(4) . . ? C43 Th2 C53 126.9(3) . . ? C55 Th2 C53 47.2(4) . . ? C40 Th2 C53 163.2(4) . . ? C42 Th2 C52 89.5(4) . . ? C56 Th2 C52 30.2(4) . . ? C41 Th2 C52 110.6(3) . . ? C43 Th2 C52 100.2(3) . . ? C55 Th2 C52 48.9(3) . . ? C40 Th2 C52 137.7(3) . . ? C53 Th2 C52 28.4(3) . . ? C42 Th2 Se4 106.3(3) . . ? C56 Th2 Se4 118.4(3) . . ? C41 Th2 Se4 125.6(2) . . ? C43 Th2 Se4 78.6(2) . . ? C55 Th2 Se4 133.2(3) . . ? C40 Th2 Se4 105.8(2) . . ? C53 Th2 Se4 86.2(3) . . ? C52 Th2 Se4 89.1(2) . . ? C42 Th2 C54 122.3(4) . . ? C56 Th2 C54 48.4(4) . . ? C41 Th2 C54 121.6(4) . . ? C43 Th2 C54 145.7(3) . . ? C55 Th2 C54 29.5(4) . . ? C40 Th2 C54 144.3(4) . . ? C53 Th2 C54 28.5(3) . . ? C52 Th2 C54 48.4(3) . . ? Se4 Th2 C54 109.6(3) . . ? C42 Th2 Se3 131.2(3) . . ? C56 Th2 Se3 119.3(3) . . ? C41 Th2 Se3 101.3(2) . . ? C43 Th2 Se3 132.1(2) . . ? C55 Th2 Se3 90.1(3) . . ? C40 Th2 Se3 87.3(2) . . ? C53 Th2 Se3 101.0(2) . . ? C52 Th2 Se3 127.3(2) . . ? Se4 Th2 Se3 105.21(4) . . ? C54 Th2 Se3 79.3(2) . . ? C42 Th2 C39 48.3(4) . . ? C56 Th2 C39 123.0(4) . . ? C41 Th2 C39 48.6(3) . . ? C43 Th2 C39 28.4(3) . . ? C55 Th2 C39 140.3(4) . . ? C40 Th2 C39 28.7(3) . . ? C53 Th2 C39 153.4(3) . . ? C52 Th2 C39 128.5(3) . . ? Se4 Th2 C39 79.0(3) . . ? C54 Th2 C39 169.8(3) . . ? Se3 Th2 C39 104.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.661 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.145 # Attachment '- compound 10.cif' data_compound10 _database_code_depnum_ccdc_archive 'CCDC 869908' #TrackingRef '- compound 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H93 S6 Th2' _chemical_formula_sum 'C54 H84 S6 Th2' _chemical_formula_weight 1389.65 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' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0783(8) _cell_length_b 14.4660(10) _cell_length_c 17.6890(15) _cell_angle_alpha 82.529(5) _cell_angle_beta 83.110(5) _cell_angle_gamma 70.635(4) _cell_volume 3119.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11081 _cell_measurement_theta_min 1.20 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 4.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3569 _exptl_absorpt_correction_T_max 0.4669 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 54435 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 33.75 _reflns_number_total 24512 _reflns_number_gt 20747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disordered solvents were removed by SQEEZE programm. ; _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^)+(0.0093P)^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 24512 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _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 Th1 Th 0.058180(6) 0.326050(6) 0.443790(4) 0.01265(2) Uani 1 1 d . . . Th2 Th 0.420577(6) 0.671019(6) 0.058827(4) 0.01283(2) Uani 1 1 d . . . S1 S -0.08430(5) 0.33903(4) 0.58059(3) 0.01740(11) Uani 1 1 d . . . S2 S -0.12171(5) 0.52259(4) 0.47659(3) 0.01564(11) Uani 1 1 d . . . S3 S -0.13899(5) 0.52872(5) 0.64504(3) 0.01984(12) Uani 1 1 d . . . S4 S 0.61628(5) 0.48390(4) 0.03076(3) 0.01570(11) Uani 1 1 d . . . S5 S 0.57758(5) 0.67124(4) -0.06843(3) 0.01928(12) Uani 1 1 d . . . S6 S 0.65385(5) 0.48388(5) -0.13843(3) 0.02135(13) Uani 1 1 d . . . C1 C 0.19277(18) 0.18616(16) 0.55243(13) 0.0162(4) Uani 1 1 d . . . C2 C 0.26157(18) 0.23689(17) 0.51209(13) 0.0176(5) Uani 1 1 d . . . H2 H 0.2887 0.2803 0.5333 0.021 Uiso 1 1 calc R . . C3 C 0.28397(19) 0.21306(17) 0.43503(14) 0.0192(5) Uani 1 1 d . . . C4 C 0.22515(18) 0.14952(17) 0.42681(14) 0.0184(5) Uani 1 1 d . . . H4 H 0.2240 0.1216 0.3813 0.022 Uiso 1 1 calc R . . C5 C 0.16796(18) 0.13454(16) 0.49846(13) 0.0168(4) Uani 1 1 d . . . H5 H 0.1206 0.0960 0.5084 0.020 Uiso 1 1 calc R . . C6 C 0.1795(2) 0.16774(18) 0.63865(13) 0.0203(5) Uani 1 1 d . . . C7 C 0.0913(2) 0.12050(19) 0.66641(14) 0.0249(5) Uani 1 1 d . . . H7A H 0.0198 0.1681 0.6564 0.037 Uiso 1 1 calc R . . H7B H 0.0938 0.1007 0.7215 0.037 Uiso 1 1 calc R . . H7C H 0.1037 0.0625 0.6391 0.037 Uiso 1 1 calc R . . C8 C 0.1578(2) 0.26207(19) 0.67689(14) 0.0242(5) Uani 1 1 d . . . H8A H 0.2177 0.2889 0.6615 0.036 Uiso 1 1 calc R . . H8B H 0.1523 0.2473 0.7326 0.036 Uiso 1 1 calc R . . H8C H 0.0895 0.3105 0.6611 0.036 Uiso 1 1 calc R . . C9 C 0.2892(2) 0.0931(2) 0.66209(15) 0.0316(6) Uani 1 1 d . . . H9A H 0.3057 0.0338 0.6355 0.047 Uiso 1 1 calc R . . H9B H 0.2843 0.0754 0.7175 0.047 Uiso 1 1 calc R . . H9C H 0.3470 0.1227 0.6481 0.047 Uiso 1 1 calc R . . C10 C 0.3769(2) 0.22882(19) 0.38002(15) 0.0244(5) Uani 1 1 d . . . C11 C 0.4150(2) 0.3100(2) 0.40169(18) 0.0337(7) Uani 1 1 d . . . H11A H 0.3551 0.3725 0.3991 0.050 Uiso 1 1 calc R . . H11B H 0.4763 0.3162 0.3661 0.050 Uiso 1 1 calc R . . H11C H 0.4379 0.2935 0.4539 0.050 Uiso 1 1 calc R . . C12 C 0.4720(2) 0.1308(2) 0.38660(18) 0.0372(7) Uani 1 1 d . . . H12A H 0.4861 0.1110 0.4405 0.056 Uiso 1 1 calc R . . H12B H 0.5373 0.1395 0.3575 0.056 Uiso 1 1 calc R . . H12C H 0.4528 0.0796 0.3659 0.056 Uiso 1 1 calc R . . C13 C 0.3478(2) 0.2517(2) 0.29664(15) 0.0315(6) Uani 1 1 d . . . H13A H 0.3197 0.2015 0.2834 0.047 Uiso 1 1 calc R . . H13B H 0.4130 0.2517 0.2629 0.047 Uiso 1 1 calc R . . H13C H 0.2923 0.3165 0.2904 0.047 Uiso 1 1 calc R . . C14 C -0.03259(19) 0.34621(18) 0.29835(13) 0.0186(5) Uani 1 1 d . . . C15 C -0.12220(19) 0.35247(17) 0.35442(13) 0.0174(5) Uani 1 1 d . . . H15 H -0.1829 0.4099 0.3616 0.021 Uiso 1 1 calc R . . C16 C -0.10693(19) 0.25975(17) 0.39782(13) 0.0175(5) Uani 1 1 d . . . C17 C -0.00435(19) 0.19748(17) 0.37143(13) 0.0187(5) Uani 1 1 d . . . H17 H 0.0286 0.1310 0.3908 0.022 Uiso 1 1 calc R . . C18 C 0.0415(2) 0.24987(18) 0.31157(13) 0.0202(5) Uani 1 1 d . . . H18 H 0.1107 0.2247 0.2846 0.024 Uiso 1 1 calc R . . C19 C -0.0349(2) 0.41490(19) 0.22577(13) 0.0216(5) Uani 1 1 d . . . C20 C -0.1017(2) 0.3862(2) 0.17185(15) 0.0333(7) Uani 1 1 d . . . H20A H -0.0667 0.3171 0.1621 0.050 Uiso 1 1 calc R . . H20B H -0.1053 0.4281 0.1234 0.050 Uiso 1 1 calc R . . H20C H -0.1754 0.3952 0.1959 0.050 Uiso 1 1 calc R . . C21 C -0.0910(2) 0.52301(19) 0.24042(15) 0.0289(6) Uani 1 1 d . . . H21A H -0.1630 0.5307 0.2671 0.043 Uiso 1 1 calc R . . H21B H -0.0987 0.5642 0.1915 0.043 Uiso 1 1 calc R . . H21C H -0.0471 0.5433 0.2720 0.043 Uiso 1 1 calc R . . C22 C 0.0800(2) 0.4013(2) 0.18475(14) 0.0270(6) Uani 1 1 d . . . H22A H 0.1218 0.4259 0.2150 0.041 Uiso 1 1 calc R . . H22B H 0.0734 0.4381 0.1340 0.041 Uiso 1 1 calc R . . H22C H 0.1174 0.3313 0.1793 0.041 Uiso 1 1 calc R . . C23 C -0.1953(2) 0.2252(2) 0.44551(14) 0.0241(5) Uani 1 1 d . . . C24 C -0.2416(2) 0.1778(2) 0.38965(16) 0.0373(7) Uani 1 1 d . . . H24A H -0.2776 0.2284 0.3503 0.056 Uiso 1 1 calc R . . H24B H -0.2942 0.1486 0.4180 0.056 Uiso 1 1 calc R . . H24C H -0.1821 0.1266 0.3653 0.056 Uiso 1 1 calc R . . C25 C -0.2889(2) 0.3107(2) 0.47760(15) 0.0313(6) Uani 1 1 d . . . H25A H -0.2600 0.3462 0.5087 0.047 Uiso 1 1 calc R . . H25B H -0.3418 0.2847 0.5094 0.047 Uiso 1 1 calc R . . H25C H -0.3246 0.3558 0.4352 0.047 Uiso 1 1 calc R . . C26 C -0.1490(2) 0.1464(2) 0.51048(15) 0.0318(6) Uani 1 1 d . . . H26A H -0.0909 0.0914 0.4892 0.048 Uiso 1 1 calc R . . H26B H -0.2069 0.1225 0.5371 0.048 Uiso 1 1 calc R . . H26C H -0.1196 0.1749 0.5466 0.048 Uiso 1 1 calc R . . C27 C -0.11823(18) 0.46389(17) 0.56737(13) 0.0157(4) Uani 1 1 d . . . C28 C 0.49242(19) 0.65039(17) 0.21170(13) 0.0176(5) Uani 1 1 d . . . C29 C 0.58467(19) 0.65205(17) 0.16130(13) 0.0173(4) Uani 1 1 d . . . H29 H 0.6496 0.5980 0.1554 0.021 Uiso 1 1 calc R . . C30 C 0.56521(19) 0.74668(17) 0.12102(13) 0.0172(5) Uani 1 1 d . . . C31 C 0.45700(19) 0.80277(17) 0.14309(13) 0.0197(5) Uani 1 1 d . . . H31 H 0.4209 0.8689 0.1244 0.024 Uiso 1 1 calc R . . C32 C 0.4116(2) 0.74338(17) 0.19799(13) 0.0199(5) Uani 1 1 d . . . H32 H 0.3395 0.7626 0.2215 0.024 Uiso 1 1 calc R . . C33 C 0.4935(2) 0.57972(19) 0.28311(14) 0.0227(5) Uani 1 1 d . . . C34 C 0.3792(2) 0.5838(2) 0.31809(14) 0.0283(6) Uani 1 1 d . . . H34A H 0.3368 0.6517 0.3276 0.043 Uiso 1 1 calc R . . H34B H 0.3846 0.5415 0.3664 0.043 Uiso 1 1 calc R . . H34C H 0.3430 0.5607 0.2826 0.043 Uiso 1 1 calc R . . C35 C 0.5597(2) 0.47365(19) 0.26824(16) 0.0296(6) Uani 1 1 d . . . H35A H 0.5231 0.4503 0.2332 0.044 Uiso 1 1 calc R . . H35B H 0.5659 0.4315 0.3167 0.044 Uiso 1 1 calc R . . H35C H 0.6325 0.4712 0.2453 0.044 Uiso 1 1 calc R . . C36 C 0.5496(2) 0.6137(2) 0.34130(15) 0.0339(7) Uani 1 1 d . . . H36A H 0.6250 0.6063 0.3218 0.051 Uiso 1 1 calc R . . H36B H 0.5487 0.5735 0.3903 0.051 Uiso 1 1 calc R . . H36C H 0.5106 0.6830 0.3487 0.051 Uiso 1 1 calc R . . C37 C 0.6509(2) 0.79070(19) 0.08232(14) 0.0222(5) Uani 1 1 d . . . C38 C 0.6065(2) 0.87281(18) 0.01979(15) 0.0261(6) Uani 1 1 d . . . H38A H 0.5889 0.8450 -0.0227 0.039 Uiso 1 1 calc R . . H38B H 0.6614 0.9048 0.0013 0.039 Uiso 1 1 calc R . . H38C H 0.5407 0.9214 0.0406 0.039 Uiso 1 1 calc R . . C39 C 0.6827(2) 0.8350(2) 0.14613(16) 0.0348(7) Uani 1 1 d . . . H39A H 0.6190 0.8866 0.1661 0.052 Uiso 1 1 calc R . . H39B H 0.7399 0.8636 0.1258 0.052 Uiso 1 1 calc R . . H39C H 0.7097 0.7834 0.1874 0.052 Uiso 1 1 calc R . . C40 C 0.7527(2) 0.7136(2) 0.05007(16) 0.0291(6) Uani 1 1 d . . . H40A H 0.7805 0.6607 0.0904 0.044 Uiso 1 1 calc R . . H40B H 0.8085 0.7444 0.0315 0.044 Uiso 1 1 calc R . . H40C H 0.7344 0.6861 0.0077 0.044 Uiso 1 1 calc R . . C41 C 0.19254(18) 0.77348(18) 0.05359(14) 0.0196(5) Uani 1 1 d . . . C42 C 0.22808(18) 0.75225(17) -0.02344(13) 0.0178(5) Uani 1 1 d . . . H42 H 0.2097 0.7070 -0.0492 0.021 Uiso 1 1 calc R . . C43 C 0.29490(18) 0.80891(16) -0.05547(13) 0.0157(4) Uani 1 1 d . . . C44 C 0.30612(19) 0.86204(17) 0.00358(13) 0.0182(5) Uani 1 1 d . . . H44 H 0.3490 0.9045 -0.0007 0.022 Uiso 1 1 calc R . . C45 C 0.24200(18) 0.84067(17) 0.07033(14) 0.0197(5) Uani 1 1 d . . . H45 H 0.2340 0.8672 0.1179 0.024 Uiso 1 1 calc R . . C46 C 0.0983(2) 0.7490(2) 0.10231(15) 0.0252(6) Uani 1 1 d . . . C47 C -0.0017(2) 0.8428(2) 0.09129(18) 0.0385(8) Uani 1 1 d . . . H47A H -0.0654 0.8326 0.1218 0.058 Uiso 1 1 calc R . . H47B H -0.0159 0.8563 0.0371 0.058 Uiso 1 1 calc R . . H47C H 0.0131 0.8989 0.1079 0.058 Uiso 1 1 calc R . . C48 C 0.1177(2) 0.7286(2) 0.18758(15) 0.0334(7) Uani 1 1 d . . . H48A H 0.1795 0.6684 0.1957 0.050 Uiso 1 1 calc R . . H48B H 0.0525 0.7201 0.2172 0.050 Uiso 1 1 calc R . . H48C H 0.1334 0.7841 0.2043 0.050 Uiso 1 1 calc R . . C49 C 0.0746(2) 0.6634(2) 0.07395(17) 0.0341(7) Uani 1 1 d . . . H49A H 0.1388 0.6044 0.0775 0.051 Uiso 1 1 calc R . . H49B H 0.0567 0.6803 0.0206 0.051 Uiso 1 1 calc R . . H49C H 0.0130 0.6505 0.1056 0.051 Uiso 1 1 calc R . . C50 C 0.3200(2) 0.83055(19) -0.14085(14) 0.0214(5) Uani 1 1 d . . . C51 C 0.3554(2) 0.7385(2) -0.18305(14) 0.0261(6) Uani 1 1 d . . . H51A H 0.4240 0.6932 -0.1649 0.039 Uiso 1 1 calc R . . H51B H 0.3657 0.7566 -0.2381 0.039 Uiso 1 1 calc R . . H51C H 0.2994 0.7062 -0.1733 0.039 Uiso 1 1 calc R . . C52 C 0.2116(2) 0.9004(2) -0.17112(17) 0.0378(7) Uani 1 1 d . . . H52A H 0.1564 0.8672 -0.1618 0.057 Uiso 1 1 calc R . . H52B H 0.2230 0.9179 -0.2262 0.057 Uiso 1 1 calc R . . H52C H 0.1870 0.9603 -0.1445 0.057 Uiso 1 1 calc R . . C53 C 0.4041(2) 0.88488(19) -0.15683(15) 0.0259(6) Uani 1 1 d . . . H53A H 0.3803 0.9431 -0.1283 0.039 Uiso 1 1 calc R . . H53B H 0.4113 0.9053 -0.2117 0.039 Uiso 1 1 calc R . . H53C H 0.4745 0.8410 -0.1407 0.039 Uiso 1 1 calc R . . C54 C 0.61920(18) 0.54618(17) -0.05867(13) 0.0165(4) 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 Th1 0.01278(4) 0.01127(4) 0.01362(4) -0.00198(3) -0.00144(3) -0.00306(3) Th2 0.01241(4) 0.01134(4) 0.01456(4) -0.00247(3) -0.00149(3) -0.00298(3) S1 0.0200(3) 0.0133(3) 0.0177(3) -0.0004(2) 0.0006(2) -0.0048(2) S2 0.0151(3) 0.0146(3) 0.0165(3) -0.0012(2) -0.0034(2) -0.0033(2) S3 0.0262(3) 0.0195(3) 0.0160(3) -0.0045(2) 0.0032(2) -0.0108(3) S4 0.0150(3) 0.0138(3) 0.0178(3) -0.0019(2) -0.0032(2) -0.0032(2) S5 0.0208(3) 0.0146(3) 0.0209(3) -0.0005(2) 0.0015(2) -0.0053(2) S6 0.0275(3) 0.0201(3) 0.0181(3) -0.0048(2) 0.0050(2) -0.0111(3) C1 0.0154(11) 0.0131(10) 0.0169(11) -0.0005(8) -0.0024(8) -0.0006(9) C2 0.0152(11) 0.0144(11) 0.0217(12) 0.0005(9) -0.0044(9) -0.0026(9) C3 0.0139(11) 0.0171(11) 0.0237(12) -0.0017(9) 0.0013(9) -0.0021(9) C4 0.0169(11) 0.0138(11) 0.0218(12) -0.0044(9) -0.0013(9) -0.0006(9) C5 0.0153(11) 0.0112(10) 0.0226(12) -0.0015(9) -0.0025(9) -0.0023(8) C6 0.0199(12) 0.0188(12) 0.0170(11) 0.0014(9) -0.0049(9) 0.0006(10) C7 0.0279(14) 0.0192(12) 0.0225(13) 0.0023(10) 0.0027(10) -0.0041(11) C8 0.0256(13) 0.0276(14) 0.0191(12) -0.0053(10) -0.0058(10) -0.0054(11) C9 0.0292(15) 0.0287(15) 0.0250(14) 0.0043(12) -0.0069(11) 0.0055(12) C10 0.0170(12) 0.0247(13) 0.0261(13) 0.0004(11) 0.0046(10) -0.0029(10) C11 0.0211(14) 0.0350(17) 0.0459(18) -0.0015(14) 0.0042(12) -0.0138(13) C12 0.0202(14) 0.0370(18) 0.0437(18) 0.0027(14) 0.0068(12) -0.0005(13) C13 0.0241(14) 0.0317(16) 0.0299(15) -0.0014(12) 0.0082(11) -0.0014(12) C14 0.0215(12) 0.0192(12) 0.0161(11) -0.0042(9) -0.0027(9) -0.0064(10) C15 0.0183(11) 0.0167(11) 0.0174(11) -0.0031(9) -0.0044(8) -0.0043(9) C16 0.0202(12) 0.0207(12) 0.0160(11) -0.0010(9) -0.0057(9) -0.0112(10) C17 0.0228(12) 0.0132(10) 0.0210(12) -0.0018(9) -0.0068(9) -0.0052(9) C18 0.0221(12) 0.0194(12) 0.0182(11) -0.0052(9) -0.0025(9) -0.0039(10) C19 0.0274(14) 0.0222(13) 0.0159(11) -0.0005(10) -0.0049(9) -0.0083(11) C20 0.0421(18) 0.0412(18) 0.0236(14) 0.0022(13) -0.0127(12) -0.0211(15) C21 0.0346(16) 0.0226(13) 0.0264(14) 0.0042(11) -0.0066(11) -0.0061(12) C22 0.0328(15) 0.0289(14) 0.0201(12) -0.0016(11) 0.0005(11) -0.0122(12) C23 0.0262(14) 0.0296(14) 0.0228(13) -0.0014(11) -0.0050(10) -0.0167(12) C24 0.0408(18) 0.049(2) 0.0360(17) -0.0072(15) -0.0101(13) -0.0299(16) C25 0.0226(14) 0.0475(19) 0.0265(14) -0.0007(13) 0.0001(11) -0.0165(13) C26 0.0406(17) 0.0319(16) 0.0307(15) 0.0047(12) -0.0066(12) -0.0237(14) C27 0.0122(10) 0.0170(11) 0.0182(11) -0.0039(9) -0.0009(8) -0.0046(9) C28 0.0194(12) 0.0169(11) 0.0172(11) -0.0042(9) -0.0024(9) -0.0053(9) C29 0.0163(11) 0.0147(11) 0.0199(11) -0.0025(9) -0.0043(9) -0.0024(9) C30 0.0189(12) 0.0161(11) 0.0188(11) -0.0015(9) -0.0052(9) -0.0073(9) C31 0.0254(13) 0.0148(11) 0.0197(11) -0.0018(9) -0.0073(9) -0.0057(10) C32 0.0191(12) 0.0195(12) 0.0203(12) -0.0080(9) -0.0032(9) -0.0025(10) C33 0.0259(14) 0.0237(13) 0.0180(12) 0.0008(10) -0.0030(10) -0.0080(11) C34 0.0324(15) 0.0342(16) 0.0185(12) -0.0031(11) 0.0035(10) -0.0126(13) C35 0.0314(15) 0.0217(13) 0.0318(15) 0.0057(11) -0.0020(12) -0.0067(12) C36 0.0458(18) 0.0410(18) 0.0214(13) 0.0006(12) -0.0126(12) -0.0205(15) C37 0.0222(13) 0.0217(12) 0.0267(13) 0.0013(10) -0.0094(10) -0.0111(10) C38 0.0275(14) 0.0208(13) 0.0317(15) 0.0048(11) -0.0076(11) -0.0110(11) C39 0.0365(17) 0.0373(17) 0.0408(17) -0.0032(14) -0.0158(13) -0.0217(14) C40 0.0187(13) 0.0314(15) 0.0377(16) 0.0048(13) -0.0055(11) -0.0105(12) C41 0.0128(11) 0.0194(12) 0.0224(12) -0.0003(10) -0.0010(9) -0.0005(9) C42 0.0131(11) 0.0161(11) 0.0227(12) -0.0031(9) -0.0050(9) -0.0013(9) C43 0.0137(11) 0.0137(10) 0.0175(11) -0.0007(8) -0.0019(8) -0.0016(8) C44 0.0184(12) 0.0131(10) 0.0221(12) -0.0018(9) -0.0044(9) -0.0028(9) C45 0.0150(11) 0.0194(12) 0.0225(12) -0.0057(10) -0.0025(9) -0.0007(9) C46 0.0124(11) 0.0292(14) 0.0304(14) -0.0017(11) 0.0041(10) -0.0044(10) C47 0.0150(13) 0.0420(19) 0.050(2) -0.0028(15) 0.0027(12) -0.0010(13) C48 0.0231(14) 0.0405(18) 0.0298(15) -0.0024(13) 0.0107(11) -0.0062(13) C49 0.0240(15) 0.0367(17) 0.0448(18) -0.0006(14) 0.0021(12) -0.0168(13) C50 0.0223(13) 0.0202(12) 0.0173(11) 0.0004(9) -0.0051(9) -0.0006(10) C51 0.0278(14) 0.0307(15) 0.0185(12) -0.0015(11) -0.0053(10) -0.0071(12) C52 0.0302(16) 0.0403(18) 0.0313(16) 0.0091(14) -0.0085(12) 0.0015(14) C53 0.0301(15) 0.0182(12) 0.0247(13) 0.0055(10) 0.0030(11) -0.0062(11) C54 0.0121(10) 0.0189(11) 0.0188(11) -0.0022(9) -0.0014(8) -0.0052(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 Th1 C17 2.765(2) . ? Th1 C5 2.770(2) . ? Th1 C18 2.772(2) . ? Th1 C4 2.779(2) . ? Th1 S1 2.8578(6) . ? Th1 C3 2.858(2) . ? Th1 S3 2.8664(6) 2_566 ? Th1 C16 2.871(2) . ? Th1 C2 2.879(2) . ? Th1 C1 2.885(2) . ? Th1 C15 2.890(2) . ? Th1 C14 2.902(2) . ? Th2 C31 2.755(2) . ? Th2 C32 2.773(2) . ? Th2 C45 2.781(2) . ? Th2 C44 2.782(2) . ? Th2 C30 2.859(2) . ? Th2 S5 2.8595(6) . ? Th2 C41 2.863(2) . ? Th2 S6 2.8720(6) 2_665 ? Th2 C42 2.883(2) . ? Th2 C43 2.888(2) . ? Th2 C29 2.895(2) . ? Th2 C28 2.915(2) . ? S1 C27 1.702(2) . ? S2 C27 1.714(2) . ? S2 Th1 3.1237(6) 2_566 ? S3 C27 1.708(2) . ? S3 Th1 2.8663(6) 2_566 ? S4 C54 1.719(2) . ? S4 Th2 3.0966(6) 2_665 ? S5 C54 1.699(2) . ? S6 C54 1.707(2) . ? S6 Th2 2.8720(6) 2_665 ? C1 C5 1.413(3) . ? C1 C2 1.416(3) . ? C1 C6 1.513(3) . ? C2 C3 1.422(3) . ? C2 H2 0.9500 . ? C3 C4 1.410(3) . ? C3 C10 1.522(3) . ? C4 C5 1.422(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C8 1.529(3) . ? C6 C7 1.529(3) . ? C6 C9 1.548(3) . ? 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 C11 1.525(4) . ? C10 C13 1.534(4) . ? C10 C12 1.548(4) . ? 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 C18 1.418(3) . ? C14 C15 1.428(3) . ? C14 C19 1.515(3) . ? C15 C16 1.421(3) . ? C15 H15 0.9500 . ? C16 C17 1.409(3) . ? C16 C23 1.529(3) . ? C17 C18 1.412(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C21 1.533(3) . ? C19 C20 1.545(3) . ? C19 C22 1.549(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C26 1.535(4) . ? C23 C25 1.537(4) . ? C23 C24 1.551(3) . ? 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 . ? C28 C29 1.417(3) . ? C28 C32 1.421(3) . ? C28 C33 1.516(3) . ? C29 C30 1.416(3) . ? C29 H29 0.9500 . ? C30 C31 1.415(3) . ? C30 C37 1.519(3) . ? C31 C32 1.420(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C35 1.530(3) . ? C33 C34 1.534(3) . ? C33 C36 1.547(3) . ? 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 1.525(3) . ? C37 C39 1.529(3) . ? C37 C40 1.530(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C45 1.410(3) . ? C41 C42 1.425(3) . ? C41 C46 1.531(3) . ? C42 C43 1.411(3) . ? C42 H42 0.9500 . ? C43 C44 1.422(3) . ? C43 C50 1.521(3) . ? C44 C45 1.426(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C49 1.528(4) . ? C46 C48 1.534(4) . ? C46 C47 1.551(4) . ? 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 C51 1.521(3) . ? C50 C53 1.533(3) . ? C50 C52 1.552(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Th1 C5 70.80(7) . . ? C17 Th1 C18 29.56(7) . . ? C5 Th1 C18 86.79(7) . . ? C17 Th1 C4 67.94(7) . . ? C5 Th1 C4 29.69(6) . . ? C18 Th1 C4 69.95(7) . . ? C17 Th1 S1 100.15(5) . . ? C5 Th1 S1 87.84(5) . . ? C18 Th1 S1 126.72(5) . . ? C4 Th1 S1 117.53(5) . . ? C17 Th1 C3 94.96(7) . . ? C5 Th1 C3 48.04(7) . . ? C18 Th1 C3 88.17(7) . . ? C4 Th1 C3 28.93(7) . . ? S1 Th1 C3 124.41(5) . . ? C17 Th1 S3 119.98(5) . 2_566 ? C5 Th1 S3 130.08(5) . 2_566 ? C18 Th1 S3 90.56(5) . 2_566 ? C4 Th1 S3 104.31(5) . 2_566 ? S1 Th1 S3 130.583(17) . 2_566 ? C3 Th1 S3 82.07(5) . 2_566 ? C17 Th1 C16 28.89(7) . . ? C5 Th1 C16 89.43(7) . . ? C18 Th1 C16 48.01(7) . . ? C4 Th1 C16 95.14(7) . . ? S1 Th1 C16 78.99(5) . . ? C3 Th1 C16 123.32(7) . . ? S3 Th1 C16 123.84(5) 2_566 . ? C17 Th1 C2 113.84(7) . . ? C5 Th1 C2 47.15(7) . . ? C18 Th1 C2 115.39(7) . . ? C4 Th1 C2 47.33(7) . . ? S1 Th1 C2 98.30(5) . . ? C3 Th1 C2 28.70(6) . . ? S3 Th1 C2 91.04(5) 2_566 . ? C16 Th1 C2 136.53(7) . . ? C17 Th1 C1 99.08(7) . . ? C5 Th1 C1 28.84(6) . . ? C18 Th1 C1 114.76(7) . . ? C4 Th1 C1 48.06(7) . . ? S1 Th1 C1 77.09(5) . . ? C3 Th1 C1 47.68(7) . . ? S3 Th1 C1 119.27(5) 2_566 . ? C16 Th1 C1 112.94(7) . . ? C2 Th1 C1 28.44(6) . . ? C17 Th1 C15 47.20(7) . . ? C5 Th1 C15 116.36(7) . . ? C18 Th1 C15 47.23(7) . . ? C4 Th1 C15 113.46(7) . . ? S1 Th1 C15 89.93(5) . . ? C3 Th1 C15 135.40(7) . . ? S3 Th1 C15 96.81(5) 2_566 . ? C16 Th1 C15 28.56(6) . . ? C2 Th1 C15 160.72(7) . . ? C1 Th1 C15 141.49(7) . . ? C17 Th1 C14 47.87(7) . . ? C5 Th1 C14 114.93(7) . . ? C18 Th1 C14 28.82(6) . . ? C4 Th1 C14 98.10(7) . . ? S1 Th1 C14 118.47(5) . . ? C3 Th1 C14 111.23(7) . . ? S3 Th1 C14 77.42(5) 2_566 . ? C16 Th1 C14 47.61(6) . . ? C2 Th1 C14 139.92(7) . . ? C1 Th1 C14 143.43(7) . . ? C15 Th1 C14 28.55(6) . . ? C31 Th2 C32 29.77(7) . . ? C31 Th2 C45 67.76(7) . . ? C32 Th2 C45 70.62(7) . . ? C31 Th2 C44 70.51(7) . . ? C32 Th2 C44 87.34(7) . . ? C45 Th2 C44 29.70(7) . . ? C31 Th2 C30 29.12(7) . . ? C32 Th2 C30 48.14(7) . . ? C45 Th2 C30 95.04(7) . . ? C44 Th2 C30 88.96(7) . . ? C31 Th2 S5 100.17(5) . . ? C32 Th2 S5 126.66(5) . . ? C45 Th2 S5 117.04(5) . . ? C44 Th2 S5 87.34(5) . . ? C30 Th2 S5 78.72(5) . . ? C31 Th2 C41 94.79(7) . . ? C32 Th2 C41 88.82(7) . . ? C45 Th2 C41 28.89(7) . . ? C44 Th2 C41 48.02(7) . . ? C30 Th2 C41 123.26(7) . . ? S5 Th2 C41 123.81(5) . . ? C31 Th2 S6 118.57(5) . 2_665 ? C32 Th2 S6 88.91(5) . 2_665 ? C45 Th2 S6 104.68(5) . 2_665 ? C44 Th2 S6 130.98(5) . 2_665 ? C30 Th2 S6 122.68(5) . 2_665 ? S5 Th2 S6 131.446(18) . 2_665 ? C41 Th2 S6 83.05(5) . 2_665 ? C31 Th2 C42 113.76(7) . . ? C32 Th2 C42 116.14(7) . . ? C45 Th2 C42 47.44(7) . . ? C44 Th2 C42 47.35(7) . . ? C30 Th2 C42 136.28(7) . . ? S5 Th2 C42 97.78(5) . . ? C41 Th2 C42 28.71(6) . . ? S6 Th2 C42 92.47(5) 2_665 . ? C31 Th2 C43 98.98(7) . . ? C32 Th2 C43 115.42(7) . . ? C45 Th2 C43 48.00(7) . . ? C44 Th2 C43 28.98(6) . . ? C30 Th2 C43 112.60(7) . . ? S5 Th2 C43 76.70(5) . . ? C41 Th2 C43 47.44(6) . . ? S6 Th2 C43 120.63(5) 2_665 . ? C42 Th2 C43 28.31(6) . . ? C31 Th2 C29 47.42(7) . . ? C32 Th2 C29 47.28(7) . . ? C45 Th2 C29 113.75(7) . . ? C44 Th2 C29 116.01(7) . . ? C30 Th2 C29 28.49(6) . . ? S5 Th2 C29 89.39(5) . . ? C41 Th2 C29 136.06(7) . . ? S6 Th2 C29 95.91(5) 2_665 . ? C42 Th2 C29 161.02(7) . . ? C43 Th2 C29 141.09(6) . . ? C31 Th2 C28 47.85(7) . . ? C32 Th2 C28 28.80(6) . . ? C45 Th2 C28 98.94(7) . . ? C44 Th2 C28 115.19(7) . . ? C30 Th2 C28 47.22(6) . . ? S5 Th2 C28 117.59(5) . . ? C41 Th2 C28 112.48(7) . . ? S6 Th2 C28 76.46(5) 2_665 . ? C42 Th2 C28 141.18(7) . . ? C43 Th2 C28 143.91(6) . . ? C29 Th2 C28 28.22(6) . . ? C27 S1 Th1 89.32(8) . . ? C27 S2 Th1 81.29(8) . . ? C27 S2 Th1 82.40(8) . 2_566 ? Th1 S2 Th1 117.735(18) . 2_566 ? C27 S3 Th1 90.85(8) . 2_566 ? C54 S4 Th2 81.19(8) . . ? C54 S4 Th2 82.92(8) . 2_665 ? Th2 S4 Th2 117.300(19) . 2_665 ? C54 S5 Th2 89.03(8) . . ? C54 S6 Th2 90.39(8) . 2_665 ? C5 C1 C2 106.2(2) . . ? C5 C1 C6 126.9(2) . . ? C2 C1 C6 124.5(2) . . ? C5 C1 Th1 71.03(13) . . ? C2 C1 Th1 75.54(13) . . ? C6 C1 Th1 132.33(15) . . ? C1 C2 C3 109.8(2) . . ? C1 C2 Th1 76.02(13) . . ? C3 C2 Th1 74.84(13) . . ? C1 C2 H2 125.1 . . ? C3 C2 H2 125.1 . . ? Th1 C2 H2 115.9 . . ? C4 C3 C2 106.8(2) . . ? C4 C3 C10 125.6(2) . . ? C2 C3 C10 125.5(2) . . ? C4 C3 Th1 72.42(13) . . ? C2 C3 Th1 76.46(13) . . ? C10 C3 Th1 129.46(16) . . ? C3 C4 C5 108.1(2) . . ? C3 C4 Th1 78.65(13) . . ? C5 C4 Th1 74.78(13) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Th1 C4 H4 113.0 . . ? C1 C5 C4 109.1(2) . . ? C1 C5 Th1 80.13(13) . . ? C4 C5 Th1 75.53(13) . . ? C1 C5 H5 125.5 . . ? C4 C5 H5 125.5 . . ? Th1 C5 H5 111.3 . . ? C1 C6 C8 111.4(2) . . ? C1 C6 C7 112.9(2) . . ? C8 C6 C7 110.4(2) . . ? C1 C6 C9 105.6(2) . . ? C8 C6 C9 109.0(2) . . ? C7 C6 C9 107.3(2) . . ? 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 . . ? C3 C10 C11 112.0(2) . . ? C3 C10 C13 112.6(2) . . ? C11 C10 C13 109.3(2) . . ? C3 C10 C12 106.1(2) . . ? C11 C10 C12 108.3(2) . . ? C13 C10 C12 108.3(2) . . ? 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 . . ? C18 C14 C15 105.9(2) . . ? C18 C14 C19 126.2(2) . . ? C15 C14 C19 125.2(2) . . ? C18 C14 Th1 70.50(13) . . ? C15 C14 Th1 75.25(13) . . ? C19 C14 Th1 133.85(16) . . ? C16 C15 C14 109.7(2) . . ? C16 C15 Th1 74.98(13) . . ? C14 C15 Th1 76.20(13) . . ? C16 C15 H15 125.1 . . ? C14 C15 H15 125.1 . . ? Th1 C15 H15 115.6 . . ? C17 C16 C15 106.4(2) . . ? C17 C16 C23 125.1(2) . . ? C15 C16 C23 126.3(2) . . ? C17 C16 Th1 71.38(13) . . ? C15 C16 Th1 76.45(13) . . ? C23 C16 Th1 130.60(15) . . ? C16 C17 C18 109.0(2) . . ? C16 C17 Th1 79.73(13) . . ? C18 C17 Th1 75.50(13) . . ? C16 C17 H17 125.5 . . ? C18 C17 H17 125.5 . . ? Th1 C17 H17 111.7 . . ? C17 C18 C14 108.9(2) . . ? C17 C18 Th1 74.94(13) . . ? C14 C18 Th1 80.68(13) . . ? C17 C18 H18 125.6 . . ? C14 C18 H18 125.6 . . ? Th1 C18 H18 111.3 . . ? C14 C19 C21 112.0(2) . . ? C14 C19 C20 105.8(2) . . ? C21 C19 C20 108.7(2) . . ? C14 C19 C22 112.5(2) . . ? C21 C19 C22 110.1(2) . . ? C20 C19 C22 107.5(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 C26 112.0(2) . . ? C16 C23 C25 112.5(2) . . ? C26 C23 C25 110.2(2) . . ? C16 C23 C24 105.6(2) . . ? C26 C23 C24 108.1(2) . . ? C25 C23 C24 108.2(2) . . ? 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 . . ? S1 C27 S3 119.26(13) . . ? S1 C27 S2 120.05(13) . . ? S3 C27 S2 120.53(14) . . ? C29 C28 C32 106.6(2) . . ? C29 C28 C33 125.2(2) . . ? C32 C28 C33 125.1(2) . . ? C29 C28 Th2 75.10(13) . . ? C32 C28 Th2 70.04(13) . . ? C33 C28 Th2 135.50(16) . . ? C30 C29 C28 109.5(2) . . ? C30 C29 Th2 74.33(13) . . ? C28 C29 Th2 76.68(13) . . ? C30 C29 H29 125.2 . . ? C28 C29 H29 125.2 . . ? Th2 C29 H29 115.7 . . ? C31 C30 C29 107.0(2) . . ? C31 C30 C37 124.1(2) . . ? C29 C30 C37 126.3(2) . . ? C31 C30 Th2 71.39(13) . . ? C29 C30 Th2 77.18(13) . . ? C37 C30 Th2 131.14(15) . . ? C30 C31 C32 108.3(2) . . ? C30 C31 Th2 79.49(13) . . ? C32 C31 Th2 75.80(13) . . ? C30 C31 H31 125.8 . . ? C32 C31 H31 125.8 . . ? Th2 C31 H31 111.4 . . ? C31 C32 C28 108.4(2) . . ? C31 C32 Th2 74.43(13) . . ? C28 C32 Th2 81.17(13) . . ? C31 C32 H32 125.8 . . ? C28 C32 H32 125.8 . . ? Th2 C32 H32 111.1 . . ? C28 C33 C35 111.8(2) . . ? C28 C33 C34 113.0(2) . . ? C35 C33 C34 109.5(2) . . ? C28 C33 C36 105.3(2) . . ? C35 C33 C36 108.8(2) . . ? C34 C33 C36 108.3(2) . . ? 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 . . ? C30 C37 C38 112.4(2) . . ? C30 C37 C39 104.5(2) . . ? C38 C37 C39 108.5(2) . . ? C30 C37 C40 112.9(2) . . ? C38 C37 C40 109.9(2) . . ? C39 C37 C40 108.3(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C45 C41 C42 107.1(2) . . ? C45 C41 C46 125.1(2) . . ? C42 C41 C46 126.3(2) . . ? C45 C41 Th2 72.31(13) . . ? C42 C41 Th2 76.40(13) . . ? C46 C41 Th2 127.89(16) . . ? C43 C42 C41 109.4(2) . . ? C43 C42 Th2 76.07(13) . . ? C41 C42 Th2 74.90(13) . . ? C43 C42 H42 125.3 . . ? C41 C42 H42 125.3 . . ? Th2 C42 H42 115.7 . . ? C42 C43 C44 106.9(2) . . ? C42 C43 C50 124.4(2) . . ? C44 C43 C50 126.4(2) . . ? C42 C43 Th2 75.62(13) . . ? C44 C43 Th2 71.34(13) . . ? C50 C43 Th2 131.83(15) . . ? C43 C44 C45 108.3(2) . . ? C43 C44 Th2 79.68(13) . . ? C45 C44 Th2 75.13(13) . . ? C43 C44 H44 125.9 . . ? C45 C44 H44 125.9 . . ? Th2 C44 H44 111.8 . . ? C41 C45 C44 108.3(2) . . ? C41 C45 Th2 78.80(14) . . ? C44 C45 Th2 75.17(13) . . ? C41 C45 H45 125.9 . . ? C44 C45 H45 125.9 . . ? Th2 C45 H45 112.6 . . ? C49 C46 C41 111.5(2) . . ? C49 C46 C48 110.9(2) . . ? C41 C46 C48 112.1(2) . . ? C49 C46 C47 108.5(2) . . ? C41 C46 C47 105.1(2) . . ? C48 C46 C47 108.5(2) . . ? 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 . . ? C51 C50 C43 112.5(2) . . ? C51 C50 C53 110.9(2) . . ? C43 C50 C53 111.6(2) . . ? C51 C50 C52 108.0(2) . . ? C43 C50 C52 105.7(2) . . ? C53 C50 C52 107.8(2) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? S5 C54 S6 119.49(14) . . ? S5 C54 S4 119.83(14) . . ? S6 C54 S4 120.49(14) . . ? 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 C17 Th1 S1 C27 -131.61(9) . . . . ? C5 Th1 S1 C27 158.34(9) . . . . ? C18 Th1 S1 C27 -117.28(10) . . . . ? C4 Th1 S1 C27 158.08(9) . . . . ? C3 Th1 S1 C27 125.15(10) . . . . ? S3 Th1 S1 C27 13.64(8) 2_566 . . . ? C16 Th1 S1 C27 -111.83(9) . . . . ? C2 Th1 S1 C27 112.22(9) . . . . ? C1 Th1 S1 C27 131.30(9) . . . . ? C15 Th1 S1 C27 -85.28(9) . . . . ? C14 Th1 S1 C27 -84.31(9) . . . . ? C17 Th1 S2 C27 104.21(9) . . . . ? C5 Th1 S2 C27 9.95(12) . . . . ? C18 Th1 S2 C27 136.99(9) . . . . ? C4 Th1 S2 C27 -34.8(6) . . . . ? S1 Th1 S2 C27 17.59(8) . . . . ? C3 Th1 S2 C27 -89.34(12) . . . . ? S3 Th1 S2 C27 -138.61(8) 2_566 . . . ? C16 Th1 S2 C27 95.93(9) . . . . ? C2 Th1 S2 C27 -57.83(10) . . . . ? C1 Th1 S2 C27 -21.71(10) . . . . ? C15 Th1 S2 C27 119.29(9) . . . . ? C14 Th1 S2 C27 143.57(9) . . . . ? C17 Th1 S2 Th1 -179.19(6) . . . 2_566 ? C5 Th1 S2 Th1 86.55(9) . . . 2_566 ? C18 Th1 S2 Th1 -146.41(6) . . . 2_566 ? C4 Th1 S2 Th1 41.8(6) . . . 2_566 ? S1 Th1 S2 Th1 94.19(2) . . . 2_566 ? C3 Th1 S2 Th1 -12.74(10) . . . 2_566 ? S3 Th1 S2 Th1 -62.02(2) 2_566 . . 2_566 ? C16 Th1 S2 Th1 172.52(5) . . . 2_566 ? C2 Th1 S2 Th1 18.77(6) . . . 2_566 ? C1 Th1 S2 Th1 54.89(6) . . . 2_566 ? C15 Th1 S2 Th1 -164.11(5) . . . 2_566 ? C14 Th1 S2 Th1 -139.83(5) . . . 2_566 ? C31 Th2 S4 C54 -104.74(10) . . . . ? C32 Th2 S4 C54 -137.65(10) . . . . ? C45 Th2 S4 C54 28.6(6) . . . . ? C44 Th2 S4 C54 -11.36(12) . . . . ? C30 Th2 S4 C54 -96.21(9) . . . . ? S5 Th2 S4 C54 -18.05(8) . . . . ? C41 Th2 S4 C54 87.71(12) . . . . ? S6 Th2 S4 C54 139.53(8) 2_665 . . . ? C42 Th2 S4 C54 56.64(10) . . . . ? C43 Th2 S4 C54 20.74(10) . . . . ? C29 Th2 S4 C54 -119.34(9) . . . . ? C28 Th2 S4 C54 -143.48(9) . . . . ? C31 Th2 S4 Th2 177.99(6) . . . 2_665 ? C32 Th2 S4 Th2 145.08(6) . . . 2_665 ? C45 Th2 S4 Th2 -48.7(6) . . . 2_665 ? C44 Th2 S4 Th2 -88.62(9) . . . 2_665 ? C30 Th2 S4 Th2 -173.48(5) . . . 2_665 ? S5 Th2 S4 Th2 -95.32(2) . . . 2_665 ? C41 Th2 S4 Th2 10.44(10) . . . 2_665 ? S6 Th2 S4 Th2 62.27(2) 2_665 . . 2_665 ? C42 Th2 S4 Th2 -20.62(6) . . . 2_665 ? C43 Th2 S4 Th2 -56.53(6) . . . 2_665 ? C29 Th2 S4 Th2 163.39(5) . . . 2_665 ? C28 Th2 S4 Th2 139.26(5) . . . 2_665 ? C31 Th2 S5 C54 132.08(9) . . . . ? C32 Th2 S5 C54 117.05(10) . . . . ? C45 Th2 S5 C54 -157.81(9) . . . . ? C44 Th2 S5 C54 -158.26(9) . . . . ? C30 Th2 S5 C54 112.27(9) . . . . ? C41 Th2 S5 C54 -125.08(10) . . . . ? S6 Th2 S5 C54 -11.68(8) 2_665 . . . ? C42 Th2 S5 C54 -111.96(9) . . . . ? C43 Th2 S5 C54 -131.00(9) . . . . ? C29 Th2 S5 C54 85.67(9) . . . . ? C28 Th2 S5 C54 84.58(9) . . . . ? C17 Th1 C1 C5 11.22(15) . . . . ? C18 Th1 C1 C5 -15.10(15) . . . . ? C4 Th1 C1 C5 -37.87(13) . . . . ? S1 Th1 C1 C5 109.64(13) . . . . ? C3 Th1 C1 C5 -77.23(15) . . . . ? S3 Th1 C1 C5 -120.82(13) 2_566 . . . ? C16 Th1 C1 C5 37.69(15) . . . . ? C2 Th1 C1 C5 -113.1(2) . . . . ? C15 Th1 C1 C5 36.49(18) . . . . ? C14 Th1 C1 C5 -11.15(19) . . . . ? C17 Th1 C1 C2 124.36(14) . . . . ? C5 Th1 C1 C2 113.1(2) . . . . ? C18 Th1 C1 C2 98.05(14) . . . . ? C4 Th1 C1 C2 75.28(14) . . . . ? S1 Th1 C1 C2 -137.22(14) . . . . ? C3 Th1 C1 C2 35.92(13) . . . . ? S3 Th1 C1 C2 -7.67(15) 2_566 . . . ? C16 Th1 C1 C2 150.83(13) . . . . ? C15 Th1 C1 C2 149.64(13) . . . . ? C14 Th1 C1 C2 101.99(16) . . . . ? C17 Th1 C1 C6 -111.9(2) . . . . ? C5 Th1 C1 C6 -123.1(3) . . . . ? C18 Th1 C1 C6 -138.2(2) . . . . ? C4 Th1 C1 C6 -161.0(2) . . . . ? S1 Th1 C1 C6 -13.4(2) . . . . ? C3 Th1 C1 C6 159.7(2) . . . . ? S3 Th1 C1 C6 116.1(2) 2_566 . . . ? C16 Th1 C1 C6 -85.4(2) . . . . ? C2 Th1 C1 C6 123.8(3) . . . . ? C15 Th1 C1 C6 -86.6(2) . . . . ? C14 Th1 C1 C6 -134.2(2) . . . . ? C5 C1 C2 C3 -3.0(3) . . . . ? C6 C1 C2 C3 160.3(2) . . . . ? Th1 C1 C2 C3 -67.92(17) . . . . ? C5 C1 C2 Th1 64.89(15) . . . . ? C6 C1 C2 Th1 -131.8(2) . . . . ? C17 Th1 C2 C1 -63.02(15) . . . . ? C5 Th1 C2 C1 -37.22(13) . . . . ? C18 Th1 C2 C1 -95.57(14) . . . . ? C4 Th1 C2 C1 -78.07(15) . . . . ? S1 Th1 C2 C1 41.99(13) . . . . ? C3 Th1 C2 C1 -115.4(2) . . . . ? S3 Th1 C2 C1 173.31(13) 2_566 . . . ? C16 Th1 C2 C1 -40.72(17) . . . . ? C15 Th1 C2 C1 -72.4(2) . . . . ? C14 Th1 C2 C1 -115.15(14) . . . . ? C17 Th1 C2 C3 52.37(15) . . . . ? C5 Th1 C2 C3 78.17(15) . . . . ? C18 Th1 C2 C3 19.83(16) . . . . ? C4 Th1 C2 C3 37.33(13) . . . . ? S1 Th1 C2 C3 157.39(13) . . . . ? S3 Th1 C2 C3 -71.30(13) 2_566 . . . ? C16 Th1 C2 C3 74.67(16) . . . . ? C1 Th1 C2 C3 115.4(2) . . . . ? C15 Th1 C2 C3 43.0(3) . . . . ? C14 Th1 C2 C3 0.25(19) . . . . ? C1 C2 C3 C4 2.1(3) . . . . ? Th1 C2 C3 C4 -66.61(16) . . . . ? C1 C2 C3 C10 -162.2(2) . . . . ? Th1 C2 C3 C10 129.1(2) . . . . ? C1 C2 C3 Th1 68.69(16) . . . . ? C17 Th1 C3 C4 -20.55(15) . . . . ? C5 Th1 C3 C4 37.98(13) . . . . ? C18 Th1 C3 C4 -49.34(14) . . . . ? S1 Th1 C3 C4 85.34(14) . . . . ? S3 Th1 C3 C4 -140.17(14) 2_566 . . . ? C16 Th1 C3 C4 -14.63(17) . . . . ? C2 Th1 C3 C4 112.8(2) . . . . ? C1 Th1 C3 C4 77.23(15) . . . . ? C15 Th1 C3 C4 -48.50(17) . . . . ? C14 Th1 C3 C4 -67.02(15) . . . . ? C17 Th1 C3 C2 -133.35(14) . . . . ? C5 Th1 C3 C2 -74.82(15) . . . . ? C18 Th1 C3 C2 -162.15(14) . . . . ? C4 Th1 C3 C2 -112.8(2) . . . . ? S1 Th1 C3 C2 -27.46(16) . . . . ? S3 Th1 C3 C2 107.03(14) 2_566 . . . ? C16 Th1 C3 C2 -127.44(14) . . . . ? C1 Th1 C3 C2 -35.58(13) . . . . ? C15 Th1 C3 C2 -161.30(13) . . . . ? C14 Th1 C3 C2 -179.83(13) . . . . ? C17 Th1 C3 C10 101.5(2) . . . . ? C5 Th1 C3 C10 160.0(3) . . . . ? C18 Th1 C3 C10 72.7(2) . . . . ? C4 Th1 C3 C10 122.0(3) . . . . ? S1 Th1 C3 C10 -152.61(19) . . . . ? S3 Th1 C3 C10 -18.1(2) 2_566 . . . ? C16 Th1 C3 C10 107.4(2) . . . . ? C2 Th1 C3 C10 -125.1(3) . . . . ? C1 Th1 C3 C10 -160.7(3) . . . . ? C15 Th1 C3 C10 73.5(2) . . . . ? C14 Th1 C3 C10 55.0(2) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C10 C3 C4 C5 163.9(2) . . . . ? Th1 C3 C4 C5 -69.68(16) . . . . ? C2 C3 C4 Th1 69.40(16) . . . . ? C10 C3 C4 Th1 -126.4(2) . . . . ? C17 Th1 C4 C3 157.83(16) . . . . ? C5 Th1 C4 C3 -112.5(2) . . . . ? C18 Th1 C4 C3 126.18(15) . . . . ? S1 Th1 C4 C3 -111.99(13) . . . . ? S3 Th1 C4 C3 40.90(14) 2_566 . . . ? C16 Th1 C4 C3 167.76(14) . . . . ? C2 Th1 C4 C3 -37.01(13) . . . . ? C1 Th1 C4 C3 -75.79(15) . . . . ? C15 Th1 C4 C3 145.02(14) . . . . ? C14 Th1 C4 C3 119.91(14) . . . . ? C17 Th1 C4 C5 -89.67(14) . . . . ? C18 Th1 C4 C5 -121.32(15) . . . . ? S1 Th1 C4 C5 0.51(15) . . . . ? C3 Th1 C4 C5 112.5(2) . . . . ? S3 Th1 C4 C5 153.39(12) 2_566 . . . ? C16 Th1 C4 C5 -79.74(14) . . . . ? C2 Th1 C4 C5 75.49(14) . . . . ? C1 Th1 C4 C5 36.71(13) . . . . ? C15 Th1 C4 C5 -102.48(14) . . . . ? C14 Th1 C4 C5 -127.60(14) . . . . ? C2 C1 C5 C4 2.8(3) . . . . ? C6 C1 C5 C4 -160.0(2) . . . . ? Th1 C1 C5 C4 70.82(16) . . . . ? C2 C1 C5 Th1 -68.00(16) . . . . ? C6 C1 C5 Th1 129.2(2) . . . . ? C3 C4 C5 C1 -1.6(3) . . . . ? Th1 C4 C5 C1 -73.94(16) . . . . ? C3 C4 C5 Th1 72.34(16) . . . . ? C17 Th1 C5 C1 -168.26(15) . . . . ? C18 Th1 C5 C1 166.30(14) . . . . ? C4 Th1 C5 C1 112.8(2) . . . . ? S1 Th1 C5 C1 -66.74(13) . . . . ? C3 Th1 C5 C1 75.87(15) . . . . ? S3 Th1 C5 C1 78.26(14) 2_566 . . . ? C16 Th1 C5 C1 -145.74(14) . . . . ? C2 Th1 C5 C1 36.67(13) . . . . ? C15 Th1 C5 C1 -155.59(13) . . . . ? C14 Th1 C5 C1 172.70(13) . . . . ? C17 Th1 C5 C4 78.93(14) . . . . ? C18 Th1 C5 C4 53.49(14) . . . . ? S1 Th1 C5 C4 -179.55(13) . . . . ? C3 Th1 C5 C4 -36.94(13) . . . . ? S3 Th1 C5 C4 -34.55(16) 2_566 . . . ? C16 Th1 C5 C4 101.45(14) . . . . ? C2 Th1 C5 C4 -76.14(14) . . . . ? C1 Th1 C5 C4 -112.8(2) . . . . ? C15 Th1 C5 C4 91.60(14) . . . . ? C14 Th1 C5 C4 59.89(15) . . . . ? C5 C1 C6 C8 -150.9(2) . . . . ? C2 C1 C6 C8 49.3(3) . . . . ? Th1 C1 C6 C8 -53.2(3) . . . . ? C5 C1 C6 C7 -26.1(3) . . . . ? C2 C1 C6 C7 174.1(2) . . . . ? Th1 C1 C6 C7 71.7(3) . . . . ? C5 C1 C6 C9 90.9(3) . . . . ? C2 C1 C6 C9 -68.9(3) . . . . ? Th1 C1 C6 C9 -171.39(17) . . . . ? C4 C3 C10 C11 174.3(2) . . . . ? C2 C3 C10 C11 -24.4(3) . . . . ? Th1 C3 C10 C11 78.0(3) . . . . ? C4 C3 C10 C13 50.6(3) . . . . ? C2 C3 C10 C13 -148.1(2) . . . . ? Th1 C3 C10 C13 -45.7(3) . . . . ? C4 C3 C10 C12 -67.8(3) . . . . ? C2 C3 C10 C12 93.6(3) . . . . ? Th1 C3 C10 C12 -164.00(18) . . . . ? C17 Th1 C14 C18 -37.90(14) . . . . ? C5 Th1 C14 C18 -13.35(16) . . . . ? C4 Th1 C14 C18 12.30(15) . . . . ? S1 Th1 C14 C18 -115.17(13) . . . . ? C3 Th1 C14 C18 39.03(16) . . . . ? S3 Th1 C14 C18 115.24(14) 2_566 . . . ? C16 Th1 C14 C18 -77.29(15) . . . . ? C2 Th1 C14 C18 38.90(19) . . . . ? C1 Th1 C14 C18 -7.4(2) . . . . ? C15 Th1 C14 C18 -113.1(2) . . . . ? C17 Th1 C14 C15 75.25(15) . . . . ? C5 Th1 C14 C15 99.80(14) . . . . ? C18 Th1 C14 C15 113.1(2) . . . . ? C4 Th1 C14 C15 125.44(14) . . . . ? S1 Th1 C14 C15 -2.02(15) . . . . ? C3 Th1 C14 C15 152.17(13) . . . . ? S3 Th1 C14 C15 -131.61(14) 2_566 . . . ? C16 Th1 C14 C15 35.86(13) . . . . ? C2 Th1 C14 C15 152.05(13) . . . . ? C1 Th1 C14 C15 105.70(15) . . . . ? C17 Th1 C14 C19 -159.8(3) . . . . ? C5 Th1 C14 C19 -135.3(2) . . . . ? C18 Th1 C14 C19 -121.9(3) . . . . ? C4 Th1 C14 C19 -109.6(2) . . . . ? S1 Th1 C14 C19 122.9(2) . . . . ? C3 Th1 C14 C19 -82.9(2) . . . . ? S3 Th1 C14 C19 -6.7(2) 2_566 . . . ? C16 Th1 C14 C19 160.8(3) . . . . ? C2 Th1 C14 C19 -83.0(2) . . . . ? C1 Th1 C14 C19 -129.3(2) . . . . ? C15 Th1 C14 C19 125.0(3) . . . . ? C18 C14 C15 C16 -3.9(3) . . . . ? C19 C14 C15 C16 158.1(2) . . . . ? Th1 C14 C15 C16 -68.19(16) . . . . ? C18 C14 C15 Th1 64.30(16) . . . . ? C19 C14 C15 Th1 -133.7(2) . . . . ? C17 Th1 C15 C16 37.37(13) . . . . ? C5 Th1 C15 C16 20.98(16) . . . . ? C18 Th1 C15 C16 78.05(15) . . . . ? C4 Th1 C15 C16 53.64(15) . . . . ? S1 Th1 C15 C16 -66.58(13) . . . . ? C3 Th1 C15 C16 76.90(16) . . . . ? S3 Th1 C15 C16 162.50(13) 2_566 . . . ? C2 Th1 C15 C16 49.1(3) . . . . ? C1 Th1 C15 C16 2.30(19) . . . . ? C14 Th1 C15 C16 115.2(2) . . . . ? C17 Th1 C15 C14 -77.82(15) . . . . ? C5 Th1 C15 C14 -94.22(14) . . . . ? C18 Th1 C15 C14 -37.14(13) . . . . ? C4 Th1 C15 C14 -61.55(15) . . . . ? S1 Th1 C15 C14 178.22(13) . . . . ? C3 Th1 C15 C14 -38.29(17) . . . . ? S3 Th1 C15 C14 47.30(13) 2_566 . . . ? C16 Th1 C15 C14 -115.2(2) . . . . ? C2 Th1 C15 C14 -66.1(2) . . . . ? C1 Th1 C15 C14 -112.89(15) . . . . ? C14 C15 C16 C17 3.4(3) . . . . ? Th1 C15 C16 C17 -65.60(15) . . . . ? C14 C15 C16 C23 -160.2(2) . . . . ? Th1 C15 C16 C23 130.8(2) . . . . ? C14 C15 C16 Th1 68.99(16) . . . . ? C5 Th1 C16 C17 -48.49(15) . . . . ? C18 Th1 C16 C17 37.71(13) . . . . ? C4 Th1 C16 C17 -19.32(15) . . . . ? S1 Th1 C16 C17 -136.41(14) . . . . ? C3 Th1 C16 C17 -12.28(17) . . . . ? S3 Th1 C16 C17 91.72(14) 2_566 . . . ? C2 Th1 C16 C17 -45.93(18) . . . . ? C1 Th1 C16 C17 -65.64(15) . . . . ? C15 Th1 C16 C17 112.8(2) . . . . ? C14 Th1 C16 C17 76.96(15) . . . . ? C17 Th1 C16 C15 -112.8(2) . . . . ? C5 Th1 C16 C15 -161.29(14) . . . . ? C18 Th1 C16 C15 -75.09(14) . . . . ? C4 Th1 C16 C15 -132.12(14) . . . . ? S1 Th1 C16 C15 110.80(14) . . . . ? C3 Th1 C16 C15 -125.07(14) . . . . ? S3 Th1 C16 C15 -21.07(15) 2_566 . . . ? C2 Th1 C16 C15 -158.73(13) . . . . ? C1 Th1 C16 C15 -178.44(13) . . . . ? C14 Th1 C16 C15 -35.84(13) . . . . ? C17 Th1 C16 C23 120.7(3) . . . . ? C5 Th1 C16 C23 72.2(2) . . . . ? C18 Th1 C16 C23 158.4(3) . . . . ? C4 Th1 C16 C23 101.4(2) . . . . ? S1 Th1 C16 C23 -15.7(2) . . . . ? C3 Th1 C16 C23 108.4(2) . . . . ? S3 Th1 C16 C23 -147.6(2) 2_566 . . . ? C2 Th1 C16 C23 74.8(2) . . . . ? C1 Th1 C16 C23 55.1(2) . . . . ? C15 Th1 C16 C23 -126.5(3) . . . . ? C14 Th1 C16 C23 -162.3(3) . . . . ? C15 C16 C17 C18 -1.5(3) . . . . ? C23 C16 C17 C18 162.3(2) . . . . ? Th1 C16 C17 C18 -70.65(16) . . . . ? C15 C16 C17 Th1 69.10(15) . . . . ? C23 C16 C17 Th1 -127.1(2) . . . . ? C5 Th1 C17 C16 127.54(15) . . . . ? C18 Th1 C17 C16 -112.9(2) . . . . ? C4 Th1 C17 C16 159.17(16) . . . . ? S1 Th1 C17 C16 43.44(14) . . . . ? C3 Th1 C17 C16 169.73(14) . . . . ? S3 Th1 C17 C16 -106.58(13) 2_566 . . . ? C2 Th1 C17 C16 147.29(13) . . . . ? C1 Th1 C17 C16 121.83(14) . . . . ? C15 Th1 C17 C16 -36.93(13) . . . . ? C14 Th1 C17 C16 -75.97(15) . . . . ? C5 Th1 C17 C18 -119.61(15) . . . . ? C4 Th1 C17 C18 -87.97(15) . . . . ? S1 Th1 C17 C18 156.30(13) . . . . ? C3 Th1 C17 C18 -77.42(14) . . . . ? S3 Th1 C17 C18 6.28(16) 2_566 . . . ? C16 Th1 C17 C18 112.9(2) . . . . ? C2 Th1 C17 C18 -99.86(14) . . . . ? C1 Th1 C17 C18 -125.31(14) . . . . ? C15 Th1 C17 C18 75.93(15) . . . . ? C14 Th1 C17 C18 36.89(13) . . . . ? C16 C17 C18 C14 -0.9(3) . . . . ? Th1 C17 C18 C14 -74.37(17) . . . . ? C16 C17 C18 Th1 73.51(16) . . . . ? C15 C14 C18 C17 2.9(3) . . . . ? C19 C14 C18 C17 -158.9(2) . . . . ? Th1 C14 C18 C17 70.46(16) . . . . ? C15 C14 C18 Th1 -67.58(16) . . . . ? C19 C14 C18 Th1 130.7(2) . . . . ? C5 Th1 C18 C17 55.32(14) . . . . ? C4 Th1 C18 C17 80.40(14) . . . . ? S1 Th1 C18 C17 -29.58(16) . . . . ? C3 Th1 C18 C17 103.39(14) . . . . ? S3 Th1 C18 C17 -174.56(13) 2_566 . . . ? C16 Th1 C18 C17 -36.80(13) . . . . ? C2 Th1 C18 C17 94.01(14) . . . . ? C1 Th1 C18 C17 62.55(15) . . . . ? C15 Th1 C18 C17 -75.80(15) . . . . ? C14 Th1 C18 C17 -112.6(2) . . . . ? C17 Th1 C18 C14 112.6(2) . . . . ? C5 Th1 C18 C14 167.90(15) . . . . ? C4 Th1 C18 C14 -167.03(16) . . . . ? S1 Th1 C18 C14 82.99(15) . . . . ? C3 Th1 C18 C14 -144.04(15) . . . . ? S3 Th1 C18 C14 -61.99(14) 2_566 . . . ? C16 Th1 C18 C14 75.78(15) . . . . ? C2 Th1 C18 C14 -153.41(13) . . . . ? C1 Th1 C18 C14 175.12(13) . . . . ? C15 Th1 C18 C14 36.77(13) . . . . ? C18 C14 C19 C21 -157.0(2) . . . . ? C15 C14 C19 C21 44.6(3) . . . . ? Th1 C14 C19 C21 -59.6(3) . . . . ? C18 C14 C19 C20 84.7(3) . . . . ? C15 C14 C19 C20 -73.7(3) . . . . ? Th1 C14 C19 C20 -177.86(18) . . . . ? C18 C14 C19 C22 -32.4(3) . . . . ? C15 C14 C19 C22 169.2(2) . . . . ? Th1 C14 C19 C22 65.0(3) . . . . ? C17 C16 C23 C26 44.7(3) . . . . ? C15 C16 C23 C26 -154.6(2) . . . . ? Th1 C16 C23 C26 -50.4(3) . . . . ? C17 C16 C23 C25 169.5(2) . . . . ? C15 C16 C23 C25 -29.8(3) . . . . ? Th1 C16 C23 C25 74.4(3) . . . . ? C17 C16 C23 C24 -72.7(3) . . . . ? C15 C16 C23 C24 87.9(3) . . . . ? Th1 C16 C23 C24 -167.81(18) . . . . ? Th1 S1 C27 S3 -142.56(13) . . . . ? Th1 S1 C27 S2 32.76(13) . . . . ? Th1 S3 C27 S1 147.83(13) 2_566 . . . ? Th1 S3 C27 S2 -27.47(13) 2_566 . . . ? Th1 S2 C27 S1 -30.29(12) . . . . ? Th1 S2 C27 S1 -149.99(14) 2_566 . . . ? Th1 S2 C27 S3 144.98(14) . . . . ? Th1 S2 C27 S3 25.28(12) 2_566 . . . ? C31 Th2 C28 C29 -75.91(14) . . . . ? C32 Th2 C28 C29 -114.3(2) . . . . ? C45 Th2 C28 C29 -124.67(14) . . . . ? C44 Th2 C28 C29 -98.53(14) . . . . ? C30 Th2 C28 C29 -36.08(13) . . . . ? S5 Th2 C28 C29 2.30(15) . . . . ? C41 Th2 C28 C29 -151.28(13) . . . . ? S6 Th2 C28 C29 132.27(13) 2_665 . . . ? C42 Th2 C28 C29 -150.95(13) . . . . ? C43 Th2 C28 C29 -103.73(15) . . . . ? C31 Th2 C28 C32 38.40(14) . . . . ? C45 Th2 C28 C32 -10.36(15) . . . . ? C44 Th2 C28 C32 15.78(16) . . . . ? C30 Th2 C28 C32 78.23(15) . . . . ? S5 Th2 C28 C32 116.61(13) . . . . ? C41 Th2 C28 C32 -36.97(16) . . . . ? S6 Th2 C28 C32 -113.42(14) 2_665 . . . ? C42 Th2 C28 C32 -36.64(19) . . . . ? C43 Th2 C28 C32 10.6(2) . . . . ? C29 Th2 C28 C32 114.3(2) . . . . ? C31 Th2 C28 C33 158.6(3) . . . . ? C32 Th2 C28 C33 120.2(3) . . . . ? C45 Th2 C28 C33 109.9(2) . . . . ? C44 Th2 C28 C33 136.0(2) . . . . ? C30 Th2 C28 C33 -161.5(3) . . . . ? S5 Th2 C28 C33 -123.2(2) . . . . ? C41 Th2 C28 C33 83.3(2) . . . . ? S6 Th2 C28 C33 6.8(2) 2_665 . . . ? C42 Th2 C28 C33 83.6(3) . . . . ? C43 Th2 C28 C33 130.8(2) . . . . ? C29 Th2 C28 C33 -125.5(3) . . . . ? C32 C28 C29 C30 4.4(3) . . . . ? C33 C28 C29 C30 -156.5(2) . . . . ? Th2 C28 C29 C30 67.77(16) . . . . ? C32 C28 C29 Th2 -63.37(16) . . . . ? C33 C28 C29 Th2 135.7(2) . . . . ? C31 Th2 C29 C30 -37.43(13) . . . . ? C32 Th2 C29 C30 -78.32(15) . . . . ? C45 Th2 C29 C30 -52.43(15) . . . . ? C44 Th2 C29 C30 -19.71(16) . . . . ? S5 Th2 C29 C30 67.03(13) . . . . ? C41 Th2 C29 C30 -75.22(16) . . . . ? S6 Th2 C29 C30 -161.33(13) 2_665 . . . ? C42 Th2 C29 C30 -45.6(3) . . . . ? C43 Th2 C29 C30 -0.66(19) . . . . ? C28 Th2 C29 C30 -115.0(2) . . . . ? C31 Th2 C29 C28 77.58(15) . . . . ? C32 Th2 C29 C28 36.69(13) . . . . ? C45 Th2 C29 C28 62.57(15) . . . . ? C44 Th2 C29 C28 95.30(14) . . . . ? C30 Th2 C29 C28 115.0(2) . . . . ? S5 Th2 C29 C28 -177.96(13) . . . . ? C41 Th2 C29 C28 39.78(17) . . . . ? S6 Th2 C29 C28 -46.33(13) 2_665 . . . ? C42 Th2 C29 C28 69.4(2) . . . . ? C43 Th2 C29 C28 114.35(14) . . . . ? C28 C29 C30 C31 -3.6(3) . . . . ? Th2 C29 C30 C31 65.69(15) . . . . ? C28 C29 C30 C37 158.6(2) . . . . ? Th2 C29 C30 C37 -132.1(2) . . . . ? C28 C29 C30 Th2 -69.32(16) . . . . ? C32 Th2 C30 C31 -38.13(13) . . . . ? C45 Th2 C30 C31 20.12(15) . . . . ? C44 Th2 C30 C31 49.22(15) . . . . ? S5 Th2 C30 C31 136.72(14) . . . . ? C41 Th2 C30 C31 13.50(17) . . . . ? S6 Th2 C30 C31 -90.91(14) 2_665 . . . ? C42 Th2 C30 C31 47.22(18) . . . . ? C43 Th2 C30 C31 66.42(15) . . . . ? C29 Th2 C30 C31 -113.1(2) . . . . ? C28 Th2 C30 C31 -77.41(15) . . . . ? C31 Th2 C30 C29 113.1(2) . . . . ? C32 Th2 C30 C29 75.00(14) . . . . ? C45 Th2 C30 C29 133.25(14) . . . . ? C44 Th2 C30 C29 162.36(14) . . . . ? S5 Th2 C30 C29 -110.15(13) . . . . ? C41 Th2 C30 C29 126.64(13) . . . . ? S6 Th2 C30 C29 22.22(15) 2_665 . . . ? C42 Th2 C30 C29 160.35(13) . . . . ? C43 Th2 C30 C29 179.55(13) . . . . ? C28 Th2 C30 C29 35.72(13) . . . . ? C31 Th2 C30 C37 -119.5(3) . . . . ? C32 Th2 C30 C37 -157.6(3) . . . . ? C45 Th2 C30 C37 -99.3(2) . . . . ? C44 Th2 C30 C37 -70.2(2) . . . . ? S5 Th2 C30 C37 17.3(2) . . . . ? C41 Th2 C30 C37 -106.0(2) . . . . ? S6 Th2 C30 C37 149.64(19) 2_665 . . . ? C42 Th2 C30 C37 -72.2(2) . . . . ? C43 Th2 C30 C37 -53.0(2) . . . . ? C29 Th2 C30 C37 127.4(3) . . . . ? C28 Th2 C30 C37 163.1(3) . . . . ? C29 C30 C31 C32 1.4(3) . . . . ? C37 C30 C31 C32 -161.3(2) . . . . ? Th2 C30 C31 C32 71.07(16) . . . . ? C29 C30 C31 Th2 -69.66(16) . . . . ? C37 C30 C31 Th2 127.6(2) . . . . ? C32 Th2 C31 C30 112.1(2) . . . . ? C45 Th2 C31 C30 -158.27(16) . . . . ? C44 Th2 C31 C30 -126.57(15) . . . . ? S5 Th2 C31 C30 -43.09(14) . . . . ? C41 Th2 C31 C30 -168.70(14) . . . . ? S6 Th2 C31 C30 106.61(13) 2_665 . . . ? C42 Th2 C31 C30 -146.34(13) . . . . ? C43 Th2 C31 C30 -121.06(14) . . . . ? C29 Th2 C31 C30 36.56(13) . . . . ? C28 Th2 C31 C30 75.09(15) . . . . ? C45 Th2 C31 C32 89.59(15) . . . . ? C44 Th2 C31 C32 121.29(15) . . . . ? C30 Th2 C31 C32 -112.1(2) . . . . ? S5 Th2 C31 C32 -155.23(13) . . . . ? C41 Th2 C31 C32 79.16(14) . . . . ? S6 Th2 C31 C32 -5.53(15) 2_665 . . . ? C42 Th2 C31 C32 101.52(14) . . . . ? C43 Th2 C31 C32 126.79(14) . . . . ? C29 Th2 C31 C32 -75.58(15) . . . . ? C28 Th2 C31 C32 -37.05(13) . . . . ? C30 C31 C32 C28 1.3(3) . . . . ? Th2 C31 C32 C28 74.90(16) . . . . ? C30 C31 C32 Th2 -73.62(16) . . . . ? C29 C28 C32 C31 -3.5(3) . . . . ? C33 C28 C32 C31 157.5(2) . . . . ? Th2 C28 C32 C31 -70.26(16) . . . . ? C29 C28 C32 Th2 66.79(16) . . . . ? C33 C28 C32 Th2 -132.2(2) . . . . ? C45 Th2 C32 C31 -78.87(14) . . . . ? C44 Th2 C32 C31 -53.75(14) . . . . ? C30 Th2 C32 C31 37.24(13) . . . . ? S5 Th2 C32 C31 30.94(16) . . . . ? C41 Th2 C32 C31 -101.78(14) . . . . ? S6 Th2 C32 C31 175.14(14) 2_665 . . . ? C42 Th2 C32 C31 -92.64(14) . . . . ? C43 Th2 C32 C31 -61.13(15) . . . . ? C29 Th2 C32 C31 76.07(15) . . . . ? C28 Th2 C32 C31 112.0(2) . . . . ? C31 Th2 C32 C28 -112.0(2) . . . . ? C45 Th2 C32 C28 169.15(16) . . . . ? C44 Th2 C32 C28 -165.74(15) . . . . ? C30 Th2 C32 C28 -74.75(15) . . . . ? S5 Th2 C32 C28 -81.04(15) . . . . ? C41 Th2 C32 C28 146.23(15) . . . . ? S6 Th2 C32 C28 63.16(14) 2_665 . . . ? C42 Th2 C32 C28 155.37(13) . . . . ? C43 Th2 C32 C28 -173.12(13) . . . . ? C29 Th2 C32 C28 -35.91(13) . . . . ? C29 C28 C33 C35 -45.9(3) . . . . ? C32 C28 C33 C35 156.6(2) . . . . ? Th2 C28 C33 C35 59.7(3) . . . . ? C29 C28 C33 C34 -169.9(2) . . . . ? C32 C28 C33 C34 32.5(3) . . . . ? Th2 C28 C33 C34 -64.4(3) . . . . ? C29 C28 C33 C36 72.1(3) . . . . ? C32 C28 C33 C36 -85.4(3) . . . . ? Th2 C28 C33 C36 177.66(18) . . . . ? C31 C30 C37 C38 -43.1(3) . . . . ? C29 C30 C37 C38 157.5(2) . . . . ? Th2 C30 C37 C38 51.5(3) . . . . ? C31 C30 C37 C39 74.4(3) . . . . ? C29 C30 C37 C39 -85.0(3) . . . . ? Th2 C30 C37 C39 168.96(17) . . . . ? C31 C30 C37 C40 -168.1(2) . . . . ? C29 C30 C37 C40 32.6(3) . . . . ? Th2 C30 C37 C40 -73.5(3) . . . . ? C31 Th2 C41 C45 20.29(15) . . . . ? C32 Th2 C41 C45 49.48(15) . . . . ? C44 Th2 C41 C45 -38.00(13) . . . . ? C30 Th2 C41 C45 13.74(17) . . . . ? S5 Th2 C41 C45 -85.34(15) . . . . ? S6 Th2 C41 C45 138.53(14) 2_665 . . . ? C42 Th2 C41 C45 -113.3(2) . . . . ? C43 Th2 C41 C45 -77.51(15) . . . . ? C29 Th2 C41 C45 47.21(18) . . . . ? C28 Th2 C41 C45 66.32(15) . . . . ? C31 Th2 C41 C42 133.54(14) . . . . ? C32 Th2 C41 C42 162.73(14) . . . . ? C45 Th2 C41 C42 113.3(2) . . . . ? C44 Th2 C41 C42 75.25(14) . . . . ? C30 Th2 C41 C42 126.99(14) . . . . ? S5 Th2 C41 C42 27.91(16) . . . . ? S6 Th2 C41 C42 -108.22(14) 2_665 . . . ? C43 Th2 C41 C42 35.74(13) . . . . ? C29 Th2 C41 C42 160.46(13) . . . . ? C28 Th2 C41 C42 179.58(13) . . . . ? C31 Th2 C41 C46 -100.8(2) . . . . ? C32 Th2 C41 C46 -71.6(2) . . . . ? C45 Th2 C41 C46 -121.1(3) . . . . ? C44 Th2 C41 C46 -159.1(2) . . . . ? C30 Th2 C41 C46 -107.4(2) . . . . ? S5 Th2 C41 C46 153.54(19) . . . . ? S6 Th2 C41 C46 17.4(2) 2_665 . . . ? C42 Th2 C41 C46 125.6(3) . . . . ? C43 Th2 C41 C46 161.4(3) . . . . ? C29 Th2 C41 C46 -73.9(2) . . . . ? C28 Th2 C41 C46 -54.8(2) . . . . ? C45 C41 C42 C43 -2.6(3) . . . . ? C46 C41 C42 C43 163.7(2) . . . . ? Th2 C41 C42 C43 -68.95(16) . . . . ? C45 C41 C42 Th2 66.33(16) . . . . ? C46 C41 C42 Th2 -127.3(2) . . . . ? C31 Th2 C42 C43 62.76(15) . . . . ? C32 Th2 C42 C43 95.58(14) . . . . ? C45 Th2 C42 C43 77.83(15) . . . . ? C44 Th2 C42 C43 37.07(13) . . . . ? C30 Th2 C42 C43 39.79(17) . . . . ? S5 Th2 C42 C43 -42.00(13) . . . . ? C41 Th2 C42 C43 114.9(2) . . . . ? S6 Th2 C42 C43 -174.42(13) 2_665 . . . ? C29 Th2 C42 C43 69.3(2) . . . . ? C28 Th2 C42 C43 114.26(15) . . . . ? C31 Th2 C42 C41 -52.12(15) . . . . ? C32 Th2 C42 C41 -19.30(16) . . . . ? C45 Th2 C42 C41 -37.06(13) . . . . ? C44 Th2 C42 C41 -77.81(15) . . . . ? C30 Th2 C42 C41 -75.09(16) . . . . ? S5 Th2 C42 C41 -156.89(13) . . . . ? S6 Th2 C42 C41 70.69(14) 2_665 . . . ? C43 Th2 C42 C41 -114.9(2) . . . . ? C29 Th2 C42 C41 -45.5(3) . . . . ? C28 Th2 C42 C41 -0.62(19) . . . . ? C41 C42 C43 C44 3.2(3) . . . . ? Th2 C42 C43 C44 -64.98(16) . . . . ? C41 C42 C43 C50 -160.6(2) . . . . ? Th2 C42 C43 C50 131.2(2) . . . . ? C41 C42 C43 Th2 68.18(16) . . . . ? C31 Th2 C43 C42 -124.53(14) . . . . ? C32 Th2 C43 C42 -98.41(14) . . . . ? C45 Th2 C43 C42 -75.66(14) . . . . ? C44 Th2 C43 C42 -113.8(2) . . . . ? C30 Th2 C43 C42 -151.37(13) . . . . ? S5 Th2 C43 C42 137.05(14) . . . . ? C41 Th2 C43 C42 -36.27(13) . . . . ? S6 Th2 C43 C42 6.48(15) 2_665 . . . ? C29 Th2 C43 C42 -151.03(13) . . . . ? C28 Th2 C43 C42 -104.03(16) . . . . ? C31 Th2 C43 C44 -10.75(15) . . . . ? C32 Th2 C43 C44 15.37(16) . . . . ? C45 Th2 C43 C44 38.11(13) . . . . ? C30 Th2 C43 C44 -37.59(15) . . . . ? S5 Th2 C43 C44 -109.17(14) . . . . ? C41 Th2 C43 C44 77.51(15) . . . . ? S6 Th2 C43 C44 120.25(13) 2_665 . . . ? C42 Th2 C43 C44 113.8(2) . . . . ? C29 Th2 C43 C44 -37.25(18) . . . . ? C28 Th2 C43 C44 9.74(19) . . . . ? C31 Th2 C43 C50 111.8(2) . . . . ? C32 Th2 C43 C50 138.0(2) . . . . ? C45 Th2 C43 C50 160.7(2) . . . . ? C44 Th2 C43 C50 122.6(3) . . . . ? C30 Th2 C43 C50 85.0(2) . . . . ? S5 Th2 C43 C50 13.4(2) . . . . ? C41 Th2 C43 C50 -159.9(2) . . . . ? S6 Th2 C43 C50 -117.2(2) 2_665 . . . ? C42 Th2 C43 C50 -123.6(3) . . . . ? C29 Th2 C43 C50 85.3(2) . . . . ? C28 Th2 C43 C50 132.3(2) . . . . ? C42 C43 C44 C45 -2.5(3) . . . . ? C50 C43 C44 C45 160.8(2) . . . . ? Th2 C43 C44 C45 -70.43(16) . . . . ? C42 C43 C44 Th2 67.88(16) . . . . ? C50 C43 C44 Th2 -128.7(2) . . . . ? C31 Th2 C44 C43 168.73(15) . . . . ? C32 Th2 C44 C43 -166.14(14) . . . . ? C45 Th2 C44 C43 -112.2(2) . . . . ? C30 Th2 C44 C43 145.72(14) . . . . ? S5 Th2 C44 C43 66.96(13) . . . . ? C41 Th2 C44 C43 -75.33(15) . . . . ? S6 Th2 C44 C43 -79.90(14) 2_665 . . . ? C42 Th2 C44 C43 -36.17(13) . . . . ? C29 Th2 C44 C43 154.97(13) . . . . ? C28 Th2 C44 C43 -173.68(13) . . . . ? C31 Th2 C44 C45 -79.06(14) . . . . ? C32 Th2 C44 C45 -53.92(14) . . . . ? C30 Th2 C44 C45 -102.07(14) . . . . ? S5 Th2 C44 C45 179.17(13) . . . . ? C41 Th2 C44 C45 36.89(13) . . . . ? S6 Th2 C44 C45 32.32(16) 2_665 . . . ? C42 Th2 C44 C45 76.05(15) . . . . ? C43 Th2 C44 C45 112.2(2) . . . . ? C29 Th2 C44 C45 -92.81(14) . . . . ? C28 Th2 C44 C45 -61.46(15) . . . . ? C42 C41 C45 C44 1.0(3) . . . . ? C46 C41 C45 C44 -165.6(2) . . . . ? Th2 C41 C45 C44 70.12(16) . . . . ? C42 C41 C45 Th2 -69.12(16) . . . . ? C46 C41 C45 Th2 124.3(2) . . . . ? C43 C44 C45 C41 1.0(3) . . . . ? Th2 C44 C45 C41 -72.60(17) . . . . ? C43 C44 C45 Th2 73.56(16) . . . . ? C31 Th2 C45 C41 -158.08(16) . . . . ? C32 Th2 C45 C41 -126.32(16) . . . . ? C44 Th2 C45 C41 112.5(2) . . . . ? C30 Th2 C45 C41 -168.50(14) . . . . ? S5 Th2 C45 C41 111.60(13) . . . . ? S6 Th2 C45 C41 -42.81(15) 2_665 . . . ? C42 Th2 C45 C41 36.81(13) . . . . ? C43 Th2 C45 C41 75.41(15) . . . . ? C29 Th2 C45 C41 -146.20(14) . . . . ? C28 Th2 C45 C41 -121.05(14) . . . . ? C31 Th2 C45 C44 89.39(14) . . . . ? C32 Th2 C45 C44 121.15(15) . . . . ? C30 Th2 C45 C44 78.97(14) . . . . ? S5 Th2 C45 C44 -0.93(15) . . . . ? C41 Th2 C45 C44 -112.5(2) . . . . ? S6 Th2 C45 C44 -155.34(12) 2_665 . . . ? C42 Th2 C45 C44 -75.72(15) . . . . ? C43 Th2 C45 C44 -37.12(13) . . . . ? C29 Th2 C45 C44 101.28(14) . . . . ? C28 Th2 C45 C44 126.42(14) . . . . ? C45 C41 C46 C49 -172.2(2) . . . . ? C42 C41 C46 C49 23.8(4) . . . . ? Th2 C41 C46 C49 -77.8(3) . . . . ? C45 C41 C46 C48 -47.1(3) . . . . ? C42 C41 C46 C48 148.8(2) . . . . ? Th2 C41 C46 C48 47.2(3) . . . . ? C45 C41 C46 C47 70.4(3) . . . . ? C42 C41 C46 C47 -93.6(3) . . . . ? Th2 C41 C46 C47 164.83(18) . . . . ? C42 C43 C50 C51 -48.7(3) . . . . ? C44 C43 C50 C51 150.6(2) . . . . ? Th2 C43 C50 C51 53.4(3) . . . . ? C42 C43 C50 C53 -174.1(2) . . . . ? C44 C43 C50 C53 25.3(3) . . . . ? Th2 C43 C50 C53 -72.0(3) . . . . ? C42 C43 C50 C52 68.9(3) . . . . ? C44 C43 C50 C52 -91.7(3) . . . . ? Th2 C43 C50 C52 171.02(18) . . . . ? Th2 S5 C54 S6 141.49(13) . . . . ? Th2 S5 C54 S4 -33.61(13) . . . . ? Th2 S6 C54 S5 -148.46(13) 2_665 . . . ? Th2 S6 C54 S4 26.60(13) 2_665 . . . ? Th2 S4 C54 S5 31.17(12) . . . . ? Th2 S4 C54 S5 150.31(14) 2_665 . . . ? Th2 S4 C54 S6 -143.88(14) . . . . ? Th2 S4 C54 S6 -24.74(12) 2_665 . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.248 0.005 0.244 210 53 ' ' 2 0.000 0.500 0.000 23 3 ' ' 3 -0.248 0.995 0.756 210 53 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 33.75 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.196 _refine_diff_density_min -2.244 _refine_diff_density_rms 0.139