# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1419 data_devan13 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C30 H54 O6 S6 Tl7, F6 P' _chemical_formula_structural '[(Tl7 {SCH2(C4H7O)}6)n] (PF6)n' _chemical_formula_analytical ? _chemical_formula_sum 'C30 H54 F6 O6 P S6 Tl7' _chemical_formula_weight 2278.65 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1, (equiv. to no. 14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 14.401(2) _cell_length_b 23.660(2) _cell_length_c 15.2958(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.404(9) _cell_angle_gamma 90.00 _cell_volume 5168.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 9 _exptl_crystal_description needles _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.928 _exptl_crystal_density_method ? _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 22.071 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.974 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 10000 _diffrn_standards_decay_% 32.0 _diffrn_reflns_number 5054 _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_av_sigmaI/netI 0.1274 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 20.0 _reflns_number_total 4819 _reflns_number_observed 1683 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS, Enraf-Nonius (1992)' _computing_cell_refinement 'CAD4/EXPRESS, Enraf-Nonius (1992)' _computing_data_reduction 'CAD4 processing, (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP, Unitek, Windows Draw' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0279P)^2^] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4819 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1613 _refine_ls_R_factor_obs 0.0521 _refine_ls_wR_factor_all 0.1328 _refine_ls_wR_factor_obs 0.0873 _refine_ls_goodness_of_fit_all 0.955 _refine_ls_goodness_of_fit_obs 1.141 _refine_ls_restrained_S_all 0.955 _refine_ls_restrained_S_obs 1.141 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tl1 Tl 0.68429(14) 0.08914(7) 0.09567(12) 0.0795(6) Uani 1 d . . Tl2 Tl 0.27695(15) 0.04379(8) 0.05898(13) 0.0863(7) Uani 1 d . . Tl3 Tl 0.54646(14) -0.13983(7) 0.07144(12) 0.0807(7) Uani 1 d . . Tl4 Tl 0.47348(14) 0.14333(8) 0.42158(12) 0.0864(7) Uani 1 d . . Tl5 Tl 0.71318(15) -0.05883(8) 0.45105(13) 0.0865(7) Uani 1 d . . Tl6 Tl 0.31392(14) -0.08245(8) 0.39998(12) 0.0829(7) Uani 1 d . . Tl7 Tl 0.50830(15) -0.00326(8) 0.24772(14) 0.0718(5) Uani 1 d . . S1 S 0.3810(8) -0.0649(5) 0.0865(7) 0.070(4) Uani 1 d . . C1 C 0.3156(45) -0.1247(27) 0.1413(39) 0.146(23) Uiso 1 d . . C11 C 0.2223(81) -0.1246(47) 0.1350(71) 0.139(36) Uiso 0.60 d P . C12 C 0.1560(49) -0.1503(30) 0.1811(47) 0.069(23) Uiso 0.60 d P . C13 C 0.0883(59) -0.1765(32) 0.0987(54) 0.103(27) Uiso 0.60 d P . C14 C 0.0900(38) -0.1297(22) 0.0327(35) 0.127(19) Uiso 1 d . . O15 O 0.1760(32) -0.1003(19) 0.0501(31) 0.075(14) Uiso 0.60 d P . C11A C 0.2817(76) -0.0850(43) 0.1483(63) 0.061(30) Uiso 0.40 d P . C12A C 0.1869(55) -0.0737(31) 0.1205(50) 0.029(21) Uiso 0.40 d P . C13A C 0.1622(61) -0.1746(34) 0.1434(58) 0.029(24) Uiso 0.40 d P . O15A O 0.2127(61) -0.1459(36) 0.0412(58) 0.127(29) Uiso 0.40 d P . S2 S 0.6588(8) -0.0350(4) 0.1120(8) 0.075(4) Uani 1 d . . C2 C 0.7587(44) -0.0566(22) 0.1954(38) 0.134(21) Uiso 1 d . . C21 C 0.8474(48) -0.0489(27) 0.1699(44) 0.158(24) Uiso 1 d . . C22 C 0.9221(44) -0.0415(26) 0.2587(39) 0.053(18) Uiso 0.60 d P . C23 C 1.0003(44) -0.0232(24) 0.2312(40) 0.150(22) Uiso 1 d . . C24 C 0.9675(40) 0.0103(21) 0.1455(36) 0.129(19) Uiso 1 d . . O25 O 0.8681(37) -0.0028(21) 0.1135(35) 0.096(17) Uiso 0.60 d P . C22A C 0.9335(55) -0.0773(33) 0.2329(52) 0.033(22) Uiso 0.40 d P . O25A O 0.8618(59) 0.0104(35) 0.1822(61) 0.121(30) Uiso 0.40 d P . S3 S 0.4711(8) 0.0906(4) 0.1025(7) 0.065(3) Uani 1 d . . C3 C 0.4511(24) 0.1563(13) 0.1670(22) 0.046(10) Uiso 1 d . . C31 C 0.5277(32) 0.1942(19) 0.1704(32) 0.101(16) Uiso 1 d . . C32 C 0.4946(31) 0.2491(19) 0.2228(29) 0.098(15) Uiso 1 d . . C33 C 0.4553(45) 0.2895(24) 0.1466(40) 0.058(18) Uiso 0.60 d P . C34 C 0.5105(36) 0.2731(21) 0.0706(34) 0.122(18) Uiso 1 d . . O35 O 0.5498(21) 0.2133(13) 0.0906(21) 0.109(11) Uiso 1 d . . C33A C 0.5419(66) 0.2912(36) 0.1680(60) 0.057(27) Uiso 0.40 d P . S4 S 0.5178(9) -0.0987(5) 0.4020(7) 0.076(4) Uani 1 d . . C4 C 0.5159(31) -0.1625(17) 0.3287(27) 0.081(14) Uiso 1 d . . C41 C 0.6011(47) -0.1947(26) 0.3552(43) 0.145(22) Uiso 1 d . . C42 C 0.6056(40) -0.2473(23) 0.2955(35) 0.127(19) Uiso 1 d . . C43 C 0.6998(52) -0.2554(29) 0.2864(46) 0.183(27) Uiso 1 d . . C44 C 0.7585(70) -0.2001(42) 0.2795(67) 0.152(38) Uiso 0.60 d P . O45 O 0.6785(46) -0.1680(25) 0.3293(42) 0.143(22) Uiso 0.60 d P . C44A C 0.7536(91) -0.2271(53) 0.3661(90) 0.116(46) Uiso 0.40 d P . O45A O 0.6675(59) -0.1969(31) 0.4157(54) 0.110(27) Uiso 0.40 d P . S5 S 0.3534(8) 0.0389(5) 0.3752(7) 0.072(4) Uani 1 d . . C5 C 0.2484(32) 0.0613(18) 0.3120(28) 0.082(14) Uiso 1 d . . C51 C 0.2326(57) 0.1209(33) 0.2977(52) 0.082(28) Uiso 0.60 d P . C52 C 0.1133(50) 0.1414(33) 0.2785(50) 0.079(23) Uiso 0.60 d P . C53 C 0.1353(41) 0.1961(26) 0.2803(41) 0.156(23) Uiso 1 d . . C54 C 0.1975(42) 0.2064(25) 0.3729(40) 0.154(23) Uiso 1 d . . O55 O 0.2412(31) 0.1516(20) 0.3932(29) 0.193(18) Uiso 1 d . . C51A C 0.1945(98) 0.1068(58) 0.3243(90) 0.101(49) Uiso 0.40 d P . C52A C 0.1413(59) 0.1247(33) 0.2329(56) 0.038(25) Uiso 0.40 d P . S6 S 0.6273(10) 0.0587(4) 0.4153(8) 0.089(5) Uani 1 d . . C6 C 0.7171(41) 0.1013(21) 0.3685(35) 0.118(19) Uiso 1 d . . C61 C 0.8065(59) 0.0909(30) 0.3965(53) 0.190(30) Uiso 1 d . . C62 C 0.8977(41) 0.1193(21) 0.3720(35) 0.121(18) Uiso 1 d . . C63 C 0.9679(44) 0.0987(26) 0.4319(45) 0.154(23) Uiso 1 d . . C64 C 0.9399(60) 0.0631(31) 0.5019(54) 0.220(33) Uiso 1 d . . O65 O 0.8413(27) 0.0594(14) 0.4774(24) 0.127(12) Uiso 1 d . . P8 P 0.1871(14) 0.2258(8) -0.0010(17) 0.146(7) Uani 1 d . . F81 F 0.2824(33) 0.2476(18) -0.0320(29) 0.143(15) Uiso 0.70 d P . F82 F 0.1502(39) 0.2533(25) -0.0914(39) 0.196(22) Uiso 0.70 d P . F83 F 0.0968(37) 0.2372(24) 0.0312(31) 0.160(18) Uiso 0.70 d P . F84 F 0.1441(57) 0.2916(31) 0.0067(50) 0.177(28) Uiso 0.50 d P . F85 F 0.2470(78) 0.1834(50) 0.0880(79) 0.221(47) Uiso 0.40 d P . F86 F 0.2340(52) 0.2307(36) 0.0980(53) 0.158(27) Uiso 0.50 d P . F87 F 0.2553(37) 0.1795(22) -0.0124(37) 0.181(19) Uiso 0.70 d P . F88 F 0.1416(42) 0.1911(26) -0.0879(42) 0.175(23) Uiso 0.60 d P . F89 F 0.2307(66) 0.2758(38) 0.0350(62) 0.245(36) Uiso 0.60 d P . F90 F 0.1122(51) 0.1851(30) 0.0293(45) 0.203(27) Uiso 0.60 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.090(2) 0.0817(14) 0.0652(14) -0.0146(11) 0.0049(12) -0.0101(12) Tl2 0.091(2) 0.0980(15) 0.0733(15) -0.0046(12) 0.0239(13) 0.0084(13) Tl3 0.104(2) 0.0740(13) 0.0636(14) 0.0099(10) 0.0090(12) 0.0066(12) Tl4 0.113(2) 0.0797(13) 0.0655(14) 0.0103(11) 0.0067(13) -0.0169(13) Tl5 0.096(2) 0.0950(14) 0.0721(14) -0.0076(12) 0.0227(13) -0.0085(13) Tl6 0.096(2) 0.0914(15) 0.0623(14) -0.0112(11) 0.0124(13) -0.0192(12) Tl7 0.0875(13) 0.0763(11) 0.0512(9) 0.0015(8) 0.0083(9) -0.0079(10) S1 0.053(8) 0.083(8) 0.074(9) -0.007(7) 0.005(7) -0.002(7) S2 0.085(9) 0.061(7) 0.081(9) -0.006(7) 0.012(8) -0.004(7) S3 0.064(8) 0.063(7) 0.066(8) 0.009(6) -0.001(7) -0.003(6) S4 0.104(10) 0.080(8) 0.046(8) -0.006(6) 0.020(7) -0.016(8) S5 0.069(9) 0.084(8) 0.059(8) -0.005(7) -0.009(7) -0.016(7) S6 0.141(13) 0.060(8) 0.074(9) 0.002(7) 0.044(9) -0.002(8) P8 0.109(15) 0.111(15) 0.222(25) 0.025(16) 0.040(17) 0.033(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl1 S1 2.880(11) 3_655 ? Tl1 S2 2.974(10) . ? Tl1 S3 3.086(11) . ? Tl2 S2 2.891(12) 3_655 ? Tl2 S1 2.980(11) . ? Tl2 S3 3.002(11) . ? Tl3 S3 2.885(11) 3_655 ? Tl3 S2 2.983(11) . ? Tl3 S1 3.002(11) . ? Tl4 S4 2.886(11) 3_656 ? Tl4 S6 2.997(13) . ? Tl4 S5 3.046(11) . ? Tl5 S4 2.971(12) . ? Tl5 S5 2.976(11) 3_656 ? Tl5 S6 3.064(11) . ? Tl6 S6 2.898(13) 3_656 ? Tl6 S4 2.957(12) . ? Tl6 S5 2.962(11) . ? Tl7 S3 3.138(10) . ? S1 C11A 1.87(10) . ? S1 C1 1.95(6) . ? S1 Tl1 2.880(11) 3_655 ? C1 C11A 1.07(10) . ? C1 C11 1.34(11) . ? C11 C11A 1.27(12) . ? C11 C12A 1.32(11) . ? C11 C12 1.40(11) . ? C11 C13A 1.48(12) . ? C11 O15 1.50(11) . ? C11 O15A 1.51(12) . ? C12 C13 1.61(10) . ? C13 C13A 1.19(9) . ? C13 C14 1.50(8) . ? C14 O15 1.41(6) . ? O15 O15A 1.22(8) . ? O15 C12A 1.24(8) . ? C11A C12A 1.40(12) . ? S2 C2 1.87(6) . ? S2 Tl2 2.892(12) 3_655 ? C2 C21 1.39(7) . ? C21 O25A 1.43(9) . ? C21 O25 1.45(7) . ? C21 C22A 1.61(9) . ? C21 C22 1.63(8) . ? C22 C23 1.32(7) . ? C23 C24 1.55(7) . ? C23 C22A 1.60(9) . ? C24 O25 1.49(6) . ? C24 O25A 1.69(9) . ? O25 O25A 1.11(8) . ? S3 C3 1.88(3) . ? S3 Tl3 2.885(11) 3_655 ? C3 C31 1.42(5) . ? C31 O35 1.38(5) . ? C31 C32 1.63(5) . ? C32 C33A 1.52(9) . ? C32 C33 1.56(7) . ? C33 C33A 1.25(9) . ? C33 C34 1.54(7) . ? C34 O35 1.54(5) . ? C34 C33A 1.56(9) . ? S4 C4 1.88(4) . ? S4 Tl4 2.886(11) 3_656 ? C4 C41 1.46(6) . ? C41 O45A 1.24(9) . ? C41 O45 1.38(7) . ? C41 C42 1.55(7) . ? C42 C43 1.40(7) . ? C43 C44A 1.51(13) . ? C43 C44 1.57(10) . ? C44 C44A 1.48(14) . ? C44 O45 1.65(10) . ? O45 O45A 1.51(9) . ? O45 C44A 1.81(13) . ? C44A O45A 1.69(13) . ? S5 C5 1.77(5) . ? S5 Tl5 2.976(11) 3_656 ? C5 C51A 1.35(13) . ? C5 C51 1.44(8) . ? C51 C52A 1.54(10) . ? C51 O55 1.62(8) . ? C51 C52 1.77(11) . ? C52 C53 1.33(7) . ? C52 C51A 1.52(14) . ? C53 C54 1.59(7) . ? C54 O55 1.46(6) . ? O55 C51A 1.58(13) . ? C51A C52A 1.56(16) . ? S6 C6 1.85(5) . ? S6 Tl6 2.898(13) 3_656 ? C6 C61 1.33(8) . ? C61 O65 1.48(7) . ? C61 C62 1.56(7) . ? C62 C63 1.36(7) . ? C63 C64 1.46(8) . ? C64 O65 1.42(8) . ? P8 F89 1.42(8) . ? P8 F83 1.47(5) . ? P8 F87 1.50(5) . ? P8 F82 1.56(6) . ? P8 F90 1.56(7) . ? P8 F86 1.58(8) . ? P8 F81 1.59(5) . ? P8 F88 1.63(6) . ? P8 F84 1.68(7) . ? P8 F85 1.82(12) . ? 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 S1 Tl1 S2 81.7(3) 3_655 . ? S1 Tl1 S3 80.4(3) 3_655 . ? S2 Tl1 S3 82.8(3) . . ? S2 Tl2 S1 81.5(3) 3_655 . ? S2 Tl2 S3 80.2(3) 3_655 . ? S1 Tl2 S3 81.4(3) . . ? S3 Tl3 S2 80.6(3) 3_655 . ? S3 Tl3 S1 81.7(3) 3_655 . ? S2 Tl3 S1 84.7(3) . . ? S4 Tl4 S6 80.9(3) 3_656 . ? S4 Tl4 S5 82.9(3) 3_656 . ? S6 Tl4 S5 81.4(3) . . ? S4 Tl5 S5 82.7(3) . 3_656 ? S4 Tl5 S6 84.0(3) . . ? S5 Tl5 S6 81.2(3) 3_656 . ? S6 Tl6 S4 81.4(3) 3_656 . ? S6 Tl6 S5 84.2(3) 3_656 . ? S4 Tl6 S5 85.5(3) . . ? C11A S1 C1 32.4(31) . . ? C11A S1 Tl1 105.2(31) . 3_655 ? C1 S1 Tl1 99.0(19) . 3_655 ? C11A S1 Tl2 83.5(32) . . ? C1 S1 Tl2 115.2(19) . . ? Tl1 S1 Tl2 86.5(3) 3_655 . ? C11A S1 Tl3 123.6(32) . . ? C1 S1 Tl3 92.1(19) . . ? Tl1 S1 Tl3 88.4(3) 3_655 . ? Tl2 S1 Tl3 152.7(4) . . ? C11 C1 S1 120.4(68) . . ? C12A C11 C1 112.2(98) . . ? C11A C11 C12 137.0(100) . . ? C12A C11 C12 102.0(91) . . ? C1 C11 C12 135.2(100) . . ? C12A C11 C13A 121.9(98) . . ? C1 C11 C13A 126.0(99) . . ? C11A C11 O15 94.1(88) . . ? C1 C11 O15 113.3(86) . . ? C12 C11 O15 110.4(84) . . ? C13A C11 O15 100.5(79) . . ? C11A C11 O15A 112.1(98) . . ? C12A C11 O15A 99.2(85) . . ? C1 C11 O15A 92.1(81) . . ? C12 C11 O15A 110.5(90) . . ? C11 C12 C13 98.9(69) . . ? C13A C13 C14 105.5(72) . . ? C14 C13 C12 100.4(54) . . ? O15 C14 C13 109.0(53) . . ? O15A O15 C12A 122.6(70) . . ? C12A O15 C14 115.0(54) . . ? C14 O15 C11 104.8(57) . . ? C1 C11A C12A 125.3(100) . . ? C11 C11A S1 130.5(88) . . ? C12A C11A S1 125.1(70) . . ? O15 C12A C11A 100.1(70) . . ? C12 C13A C13 104.9(100) . . ? C13 C13A C11 118.0(85) . . ? C12 C13A O15A 114.0(94) . . ? O15 O15A C13A 90.4(59) . . ? C2 S2 Tl2 106.8(18) . 3_655 ? C2 S2 Tl1 103.6(17) . . ? Tl2 S2 Tl1 86.4(3) 3_655 . ? C2 S2 Tl3 105.3(17) . . ? Tl2 S2 Tl3 88.9(3) 3_655 . ? Tl1 S2 Tl3 150.8(5) . . ? C21 C2 S2 115.3(47) . . ? C2 C21 O25A 102.3(63) . . ? C2 C21 O25 122.0(61) . . ? C2 C21 C22A 116.1(60) . . ? O25A C21 C22A 104.1(63) . . ? O25 C21 C22A 117.9(59) . . ? C2 C21 C22 108.1(56) . . ? O25 C21 C22 104.6(52) . . ? C23 C22 C21 105.5(53) . . ? C22A C22 O25A 114.9(76) . . ? C22 C23 C24 105.0(54) . . ? C24 C23 C22A 107.7(51) . . ? O25 C24 C23 110.2(47) . . ? C21 O25 C24 103.0(49) . . ? C23 C22A C21 94.2(51) . . ? C21 O25A C24 94.4(59) . . ? O25 O25A C22 108.9(68) . . ? C3 S3 Tl3 98.6(10) . 3_655 ? C3 S3 Tl2 102.7(11) . . ? Tl3 S3 Tl2 88.6(3) 3_655 . ? C3 S3 Tl1 104.3(11) . . ? Tl3 S3 Tl1 86.7(3) 3_655 . ? Tl2 S3 Tl1 153.0(4) . . ? C3 S3 Tl7 103.7(11) . . ? Tl3 S3 Tl7 157.6(4) 3_655 . ? Tl2 S3 Tl7 88.0(3) . . ? Tl1 S3 Tl7 86.3(3) . . ? C31 C3 S3 111.7(27) . . ? O35 C31 C3 116.3(40) . . ? O35 C31 C32 106.9(36) . . ? C3 C31 C32 104.3(35) . . ? C33A C32 C31 94.1(43) . . ? C33 C32 C31 102.8(37) . . ? C34 C33 C32 103.7(44) . . ? O35 C34 C33 107.1(40) . . ? O35 C34 C33A 90.6(45) . . ? C31 O35 C34 110.9(35) . . ? C32 C33A C34 104.6(60) . . ? C4 S4 Tl4 105.1(13) . 3_656 ? C4 S4 Tl6 99.2(14) . . ? Tl4 S4 Tl6 88.9(3) 3_656 . ? C4 S4 Tl5 110.3(14) . . ? Tl4 S4 Tl5 87.4(3) 3_656 . ? Tl6 S4 Tl5 150.2(4) . . ? C41 C4 S4 107.9(37) . . ? O45 C41 C4 111.2(56) . . ? O45A C41 C42 108.5(65) . . ? O45 C41 C42 95.8(51) . . ? C4 C41 C42 110.7(55) . . ? C43 C42 C41 106.5(55) . . ? C42 C43 C44A 105.2(73) . . ? C42 C43 C44 115.6(66) . . ? C41 O45 C44 124.1(62) . . ? O45A O45 C44 110.7(61) . . ? C41 O45 C44A 91.7(60) . . ? C44 C44A O45A 109.9(92) . . ? C43 C44A O45A 102.7(85) . . ? C41 O45A C44A 102.9(77) . . ? C5 S5 Tl6 101.3(15) . . ? C5 S5 Tl5 95.2(15) . 3_656 ? Tl6 S5 Tl5 87.1(3) . 3_656 ? C5 S5 Tl4 107.7(15) . . ? Tl6 S5 Tl4 150.4(4) . . ? Tl5 S5 Tl4 84.4(3) 3_656 . ? C51A C5 S5 128.8(67) . . ? C51 C5 S5 118.9(44) . . ? C5 C51 C52A 105.1(61) . . ? C5 C51 O55 108.0(55) . . ? C52A C51 O55 120.8(62) . . ? C5 C51 C52 115.1(61) . . ? O55 C51 C52 89.2(48) . . ? C52A C52 C53 107.4(89) . . ? C53 C52 C51A 110.3(78) . . ? C53 C52 C51 92.2(55) . . ? C52 C53 C54 105.8(58) . . ? C54 C53 C52A 116.1(49) . . ? O55 C54 C53 103.4(47) . . ? C54 O55 C51A 108.7(64) . . ? C54 O55 C51 103.1(47) . . ? C51 C51A C52 94.4(100) . . ? C5 C51A C52A 108.4(98) . . ? C5 C51A O55 115.1(99) . . ? C52 C51A O55 100.4(88) . . ? C52A C51A O55 122.0(96) . . ? C6 S6 Tl6 98.1(18) . 3_656 ? C6 S6 Tl4 101.8(17) . . ? Tl6 S6 Tl4 87.9(3) 3_656 . ? C6 S6 Tl5 106.1(18) . . ? Tl6 S6 Tl5 86.6(3) 3_656 . ? Tl4 S6 Tl5 152.1(4) . . ? C61 C6 S6 118.1(54) . . ? C6 C61 O65 125.1(72) . . ? C6 C61 C62 130.9(75) . . ? O65 C61 C62 102.3(59) . . ? C63 C62 C61 105.1(55) . . ? C62 C63 C64 116.6(63) . . ? O65 C64 C63 101.7(62) . . ? C64 O65 C61 114.1(54) . . ? F89 P8 F83 94.7(45) . . ? F89 P8 F87 113.1(46) . . ? F89 P8 F82 94.6(45) . . ? F83 P8 F82 90.3(29) . . ? F87 P8 F82 110.8(34) . . ? F89 P8 F90 133.5(50) . . ? F87 P8 F90 94.2(34) . . ? F82 P8 F90 110.5(37) . . ? F83 P8 F88 94.9(32) . . ? F81 P8 F88 101.1(30) . . ? F90 P8 F84 105.9(35) . . ? F81 P8 F84 93.4(34) . . ? F88 P8 F84 114.2(37) . . ? F89 P8 F85 91.5(53) . . ? F83 P8 F85 101.8(44) . . ? F81 P8 F85 93.3(39) . . ? F88 P8 F85 115.9(47) . . ? F84 P8 F85 126.9(52) . . ? _refine_diff_density_max 0.981 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.224