# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1357747294.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H40 N Na O6 Th' _chemical_formula_weight 753.65 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' 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' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 16.9230(6) _cell_length_b 12.8262(4) _cell_length_c 13.4858(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2927.20(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68974 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 5.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.445 _exptl_absorpt_correction_T_max 0.662 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps (310 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 68974 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8618 _reflns_number_gt 7235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0327P)^2^+0.8161P] 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' _chemical_absolute_configuration unk _refine_ls_abs_structure_Flack 0.487(7) _refine_ls_number_reflns 8618 _refine_ls_number_parameters 344 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.950 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.091 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 Th Th 0.046797(6) 0.921293(7) 0.10419(3) 0.02462(4) Uani 1 1 d . . . Na Na 0.04210(8) 0.44311(12) 0.1125(4) 0.0318(5) Uani 1 1 d . . . O1 O -0.0676(2) 0.4151(2) 0.2369(3) 0.0361(7) Uani 1 1 d . . . O2 O -0.09434(19) 0.4580(2) 0.0378(2) 0.0353(6) Uani 1 1 d . . . O3 O 0.01148(19) 0.3360(2) -0.0516(2) 0.0362(6) Uani 1 1 d . . . O4 O 0.14178(19) 0.4583(2) -0.0319(2) 0.0399(7) Uani 1 1 d . . . O5 O 0.1856(2) 0.4173(2) 0.1617(3) 0.0422(7) Uani 1 1 d . . . O6 O 0.0761(2) 0.3349(3) 0.2893(3) 0.0393(8) Uani 1 1 d . . . N1 N 0.0384(2) 0.6263(3) 0.1316(3) 0.0394(10) Uani 1 1 d . . . C1 C 0.0383(2) 0.7163(3) 0.1249(3) 0.0326(13) Uani 1 1 d . . . C2 C 0.1918(2) 0.8138(3) 0.1014(7) 0.0399(8) Uani 1 1 d . . . H2 H 0.2080 0.7445 0.1003 0.048 Uiso 1 1 calc R . . C3 C 0.1825(4) 0.8515(5) 0.1979(5) 0.0414(19) Uani 1 1 d . . . H3 H 0.1902 0.7997 0.2451 0.050 Uiso 1 1 calc R . . C4 C 0.1646(4) 0.9473(8) 0.2410(5) 0.045(2) Uani 1 1 d . . . H4 H 0.1595 0.9437 0.3095 0.054 Uiso 1 1 calc R . . C5 C 0.1526(4) 1.0484(7) 0.2033(5) 0.0380(16) Uani 1 1 d . . . H5 H 0.1440 1.0972 0.2532 0.046 Uiso 1 1 calc R . . C6 C 0.1506(2) 1.0922(3) 0.1097(9) 0.0366(10) Uani 1 1 d . . . H6 H 0.1447 1.1643 0.1119 0.044 Uiso 1 1 calc R . . C7 C 0.1554(4) 1.0543(5) 0.0117(5) 0.0366(17) Uani 1 1 d . . . H7 H 0.1502 1.1070 -0.0352 0.044 Uiso 1 1 calc R . . C8 C 0.1663(4) 0.9551(6) -0.0321(5) 0.0345(16) Uani 1 1 d . . . H8 H 0.1616 0.9562 -0.1008 0.041 Uiso 1 1 calc R . . C9 C 0.1826(4) 0.8554(6) 0.0056(5) 0.0391(18) Uani 1 1 d . . . H9 H 0.1886 0.8056 -0.0439 0.047 Uiso 1 1 calc R . . C10 C -0.1051(4) 0.8574(5) 0.1572(5) 0.0333(15) Uani 1 1 d . . . H10 H -0.1252 0.7987 0.1888 0.040 Uiso 1 1 calc R . . C11 C -0.0835(5) 0.9360(5) 0.2260(6) 0.0328(15) Uani 1 1 d . . . H11 H -0.0872 0.9151 0.2919 0.039 Uiso 1 1 calc R . . C12 C -0.0577(3) 1.0390(5) 0.2142(4) 0.0342(13) Uani 1 1 d . . . H12 H -0.0491 1.0720 0.2746 0.041 Uiso 1 1 calc R . . C13 C -0.0418(3) 1.1038(4) 0.1343(4) 0.0303(13) Uani 1 1 d . . . H13 H -0.0294 1.1714 0.1538 0.036 Uiso 1 1 calc R . . C14 C -0.0399(3) 1.0915(4) 0.0316(5) 0.0342(13) Uani 1 1 d . . . H14 H -0.0276 1.1535 -0.0006 0.041 Uiso 1 1 calc R . . C15 C -0.0518(3) 1.0103(5) -0.0346(4) 0.0312(12) Uani 1 1 d . . . H15 H -0.0391 1.0283 -0.0995 0.037 Uiso 1 1 calc R . . C16 C -0.0789(5) 0.9058(5) -0.0257(6) 0.0321(14) Uani 1 1 d . . . H16 H -0.0800 0.8705 -0.0860 0.039 Uiso 1 1 calc R . . C17 C -0.1040(4) 0.8451(6) 0.0535(5) 0.0304(14) Uani 1 1 d . . . H17 H -0.1251 0.7816 0.0333 0.036 Uiso 1 1 calc R . . C18 C -0.1463(3) 0.4294(4) 0.2040(4) 0.0419(11) Uani 1 1 d . . . H18A H -0.1775 0.4617 0.2559 0.050 Uiso 1 1 calc R . . H18B H -0.1698 0.3625 0.1879 0.050 Uiso 1 1 calc R . . C19 C -0.1450(2) 0.4975(3) 0.1145(6) 0.0384(11) Uani 1 1 d . . . H19A H -0.1983 0.5038 0.0887 0.046 Uiso 1 1 calc R . . H19B H -0.1272 0.5666 0.1334 0.046 Uiso 1 1 calc R . . C20 C -0.1211(3) 0.3622(4) -0.0051(4) 0.0392(10) Uani 1 1 d . . . H20A H -0.1749 0.3693 -0.0289 0.047 Uiso 1 1 calc R . . H20B H -0.1194 0.3065 0.0435 0.047 Uiso 1 1 calc R . . C21 C -0.0662(5) 0.3396(7) -0.0891(5) 0.0371(15) Uani 1 1 d . . . H21A H -0.0797 0.2733 -0.1194 0.044 Uiso 1 1 calc R . . H21B H -0.0705 0.3936 -0.1392 0.044 Uiso 1 1 calc R . . C22 C 0.0692(3) 0.3391(4) -0.1277(4) 0.0401(12) Uani 1 1 d . . . H22A H 0.0567 0.3941 -0.1746 0.048 Uiso 1 1 calc R . . H22B H 0.0700 0.2733 -0.1632 0.048 Uiso 1 1 calc R . . C23 C 0.1475(4) 0.3590(5) -0.0817(5) 0.0435(14) Uani 1 1 d . . . H23A H 0.1603 0.3043 -0.0347 0.052 Uiso 1 1 calc R . . H23B H 0.1884 0.3611 -0.1321 0.052 Uiso 1 1 calc R . . C24 C 0.2145(3) 0.4957(4) 0.0068(4) 0.0508(12) Uani 1 1 d . . . H24A H 0.2070 0.5664 0.0305 0.061 Uiso 1 1 calc R . . H24B H 0.2532 0.4978 -0.0462 0.061 Uiso 1 1 calc R . . C25 C 0.2459(3) 0.4301(4) 0.0897(8) 0.052(2) Uani 1 1 d . . . H25A H 0.2622 0.3626 0.0645 0.062 Uiso 1 1 calc R . . H25B H 0.2915 0.4637 0.1194 0.062 Uiso 1 1 calc R . . C26 C 0.2104(3) 0.3503(4) 0.2400(3) 0.0410(10) Uani 1 1 d . . . H26A H 0.2631 0.3693 0.2617 0.049 Uiso 1 1 calc R . . H26B H 0.2115 0.2786 0.2172 0.049 Uiso 1 1 calc R . . C27 C 0.1536(4) 0.3614(6) 0.3230(4) 0.0454(16) Uani 1 1 d . . . H27A H 0.1688 0.3157 0.3771 0.054 Uiso 1 1 calc R . . H27B H 0.1542 0.4326 0.3472 0.054 Uiso 1 1 calc R . . C28 C 0.0175(3) 0.3572(4) 0.3640(3) 0.0387(10) Uani 1 1 d . . . H28A H 0.0243 0.4278 0.3884 0.046 Uiso 1 1 calc R . . H28B H 0.0235 0.3095 0.4193 0.046 Uiso 1 1 calc R . . C29 C -0.0628(5) 0.3454(7) 0.3197(4) 0.0367(16) Uani 1 1 d . . . H29A H -0.0709 0.2741 0.2980 0.044 Uiso 1 1 calc R . . H29B H -0.1030 0.3625 0.3683 0.044 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 Th 0.02375(6) 0.02560(6) 0.02450(6) -0.00038(14) -0.00055(13) 0.00048(4) Na 0.0311(7) 0.0287(6) 0.0357(15) 0.0007(13) 0.0027(10) 0.0001(5) O1 0.0298(15) 0.0427(18) 0.0358(17) 0.0036(13) -0.0005(13) -0.0010(12) O2 0.0379(18) 0.0353(15) 0.0328(15) 0.0003(12) -0.0025(13) -0.0017(13) O3 0.0388(18) 0.0382(15) 0.0317(14) -0.0004(12) -0.0008(13) -0.0028(13) O4 0.0404(17) 0.0370(15) 0.0421(17) -0.0013(13) 0.0043(14) -0.0026(14) O5 0.0319(18) 0.0479(19) 0.0468(19) 0.0023(14) -0.0022(14) 0.0013(13) O6 0.0396(19) 0.0438(19) 0.0344(17) -0.0063(16) -0.0038(18) 0.0022(15) N1 0.0343(19) 0.039(2) 0.045(3) -0.0024(15) 0.0023(14) -0.0020(14) C1 0.0254(18) 0.0308(18) 0.042(4) -0.0006(16) -0.0014(15) -0.0023(13) C2 0.0288(17) 0.0326(16) 0.058(2) -0.006(4) 0.005(4) 0.0034(13) C3 0.039(4) 0.026(3) 0.059(5) 0.020(3) -0.004(3) 0.006(3) C4 0.018(3) 0.093(5) 0.025(3) 0.015(4) -0.005(3) -0.001(3) C5 0.020(3) 0.065(4) 0.030(3) -0.006(3) -0.002(2) -0.005(3) C6 0.0301(17) 0.0364(17) 0.043(3) -0.019(3) -0.004(4) -0.0020(13) C7 0.046(4) 0.023(3) 0.041(4) 0.012(3) -0.006(3) -0.005(3) C8 0.042(4) 0.034(3) 0.027(3) 0.008(3) -0.001(3) -0.008(3) C9 0.023(4) 0.060(5) 0.034(3) -0.007(3) 0.006(3) -0.008(3) C10 0.029(4) 0.034(3) 0.037(3) 0.008(3) 0.001(3) -0.001(2) C11 0.028(3) 0.045(3) 0.025(2) 0.007(2) 0.003(2) 0.003(3) C12 0.033(3) 0.045(3) 0.024(3) -0.001(2) -0.002(2) 0.009(2) C13 0.031(2) 0.0255(18) 0.035(3) 0.0004(19) 0.0015(18) 0.0037(15) C14 0.035(3) 0.041(3) 0.026(3) 0.006(2) 0.000(2) 0.003(2) C15 0.027(2) 0.046(3) 0.021(2) 0.006(2) 0.0011(17) 0.004(2) C16 0.035(3) 0.036(3) 0.025(3) -0.005(2) -0.003(2) 0.001(3) C17 0.025(3) 0.034(3) 0.033(3) 0.000(2) 0.001(2) -0.002(2) C18 0.026(2) 0.055(3) 0.045(3) 0.000(2) 0.003(2) 0.000(2) C19 0.0326(17) 0.0415(18) 0.041(3) -0.010(3) -0.004(2) 0.0043(14) C20 0.035(2) 0.036(2) 0.047(2) -0.0014(19) -0.0066(19) -0.0014(19) C21 0.042(3) 0.032(3) 0.038(3) -0.004(3) -0.013(3) -0.002(2) C22 0.053(3) 0.035(2) 0.032(2) -0.003(2) 0.007(3) -0.004(2) C23 0.043(3) 0.043(3) 0.045(3) 0.003(3) 0.013(3) 0.003(2) C24 0.043(3) 0.057(3) 0.052(3) 0.002(2) 0.005(2) -0.014(2) C25 0.031(2) 0.065(3) 0.060(6) 0.001(3) 0.008(3) -0.0028(17) C26 0.035(3) 0.040(2) 0.048(2) -0.005(2) -0.011(2) 0.0066(18) C27 0.038(3) 0.054(3) 0.044(3) -0.003(3) -0.011(3) 0.001(2) C28 0.051(3) 0.039(2) 0.026(2) 0.0030(17) 0.006(2) 0.007(2) C29 0.047(4) 0.035(3) 0.028(3) 0.004(2) 0.007(2) 0.002(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 Th C1 2.648(4) . ? Th C4 2.737(7) . ? Th C15 2.754(5) . ? Th C12 2.758(6) . ? Th C11 2.756(8) . ? Th C16 2.763(9) . ? Th C5 2.766(7) . ? Th C8 2.767(7) . ? Th C3 2.770(7) . ? Th C9 2.786(7) . ? Th C10 2.791(7) . ? Th C7 2.801(7) . ? Th C13 2.809(5) . ? Th C14 2.807(5) . ? Th C6 2.811(4) . ? Th C2 2.815(3) . ? Th C17 2.817(7) . ? Na N1 2.365(4) . ? Na O2 2.527(4) . ? Na O1 2.527(5) . ? Na O5 2.539(4) . ? Na O4 2.584(5) . ? Na O3 2.656(5) . ? Na O6 2.818(6) . ? O1 C18 1.416(6) . ? O1 C29 1.433(8) . ? O2 C20 1.431(5) . ? O2 C19 1.436(7) . ? O3 C21 1.409(8) . ? O3 C22 1.417(6) . ? O4 C24 1.419(6) . ? O4 C23 1.443(7) . ? O5 C25 1.418(9) . ? O5 C26 1.424(6) . ? O6 C27 1.430(7) . ? O6 C28 1.442(6) . ? N1 C1 1.157(6) . ? C2 C3 1.396(10) . ? C2 C9 1.407(10) . ? C2 H2 0.9300 . ? C3 C4 1.393(11) . ? C3 H3 0.9300 . ? C4 C5 1.407(11) . ? C4 H4 0.9300 . ? C5 C6 1.382(13) . ? C5 H5 0.9300 . ? C6 C7 1.410(13) . ? C6 H6 0.9300 . ? C7 C8 1.415(9) . ? C7 H7 0.9300 . ? C8 C9 1.404(10) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C17 1.408(5) . ? C10 C11 1.418(10) . ? C10 H10 0.9300 . ? C11 C12 1.401(9) . ? C11 H11 0.9300 . ? C12 C13 1.387(8) . ? C12 H12 0.9300 . ? C13 C14 1.393(10) . ? C13 H13 0.9300 . ? C14 C15 1.386(8) . ? C14 H14 0.9300 . ? C15 C16 1.422(8) . ? C15 H15 0.9300 . ? C16 C17 1.389(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.490(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.494(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.486(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.497(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.482(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.491(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Th C4 95.1(2) . . ? C1 Th C15 116.78(16) . . ? C4 Th C15 148.1(3) . . ? C1 Th C12 116.88(18) . . ? C4 Th C12 92.2(2) . . ? C15 Th C12 75.5(2) . . ? C1 Th C11 87.81(15) . . ? C4 Th C11 99.9(3) . . ? C15 Th C11 83.81(19) . . ? C12 Th C11 29.43(19) . . ? C1 Th C16 87.36(15) . . ? C4 Th C16 175.6(3) . . ? C15 Th C16 29.86(17) . . ? C12 Th C16 83.51(19) . . ? C11 Th C16 76.53(13) . . ? C1 Th C5 124.7(2) . . ? C4 Th C5 29.6(2) . . ? C15 Th C5 118.4(2) . . ? C12 Th C5 80.3(2) . . ? C11 Th C5 100.9(2) . . ? C16 Th C5 147.9(2) . . ? C1 Th C8 105.39(17) . . ? C4 Th C8 84.03(11) . . ? C15 Th C8 85.79(17) . . ? C12 Th C8 137.7(2) . . ? C11 Th C8 165.92(18) . . ? C16 Th C8 98.8(3) . . ? C5 Th C8 75.8(2) . . ? C1 Th C3 71.08(16) . . ? C4 Th C3 29.3(2) . . ? C15 Th C3 161.07(17) . . ? C12 Th C3 117.59(19) . . ? C11 Th C3 114.4(2) . . ? C16 Th C3 154.7(2) . . ? C5 Th C3 55.5(2) . . ? C8 Th C3 75.4(2) . . ? C1 Th C9 78.10(18) . . ? C4 Th C9 76.0(2) . . ? C15 Th C9 107.52(17) . . ? C12 Th C9 162.1(2) . . ? C11 Th C9 164.8(2) . . ? C16 Th C9 108.1(2) . . ? C5 Th C9 82.9(2) . . ? C8 Th C9 29.3(2) . . ? C3 Th C9 55.65(12) . . ? C1 Th C10 68.38(17) . . ? C4 Th C10 122.3(2) . . ? C15 Th C10 74.80(17) . . ? C12 Th C10 55.4(2) . . ? C11 Th C10 29.6(2) . . ? C16 Th C10 55.4(2) . . ? C5 Th C10 130.2(2) . . ? C8 Th C10 152.8(2) . . ? C3 Th C10 123.50(19) . . ? C9 Th C10 142.4(2) . . ? C1 Th C7 133.42(17) . . ? C4 Th C7 75.4(2) . . ? C15 Th C7 80.94(19) . . ? C12 Th C7 109.1(2) . . ? C11 Th C7 138.5(2) . . ? C16 Th C7 105.5(2) . . ? C5 Th C7 55.34(13) . . ? C8 Th C7 29.4(2) . . ? C3 Th C7 81.7(2) . . ? C9 Th C7 55.3(2) . . ? C10 Th C7 153.8(2) . . ? C1 Th C13 141.57(14) . . ? C4 Th C13 100.9(2) . . ? C15 Th C13 55.22(17) . . ? C12 Th C13 28.85(16) . . ? C11 Th C13 55.26(16) . . ? C16 Th C13 74.97(16) . . ? C5 Th C13 77.6(2) . . ? C8 Th C13 110.81(19) . . ? C3 Th C13 130.23(19) . . ? C9 Th C13 139.62(19) . . ? C10 Th C13 73.52(18) . . ? C7 Th C13 84.65(19) . . ? C1 Th C14 141.34(14) . . ? C4 Th C14 121.4(2) . . ? C15 Th C14 28.85(17) . . ? C12 Th C14 55.0(2) . . ? C11 Th C14 74.71(18) . . ? C16 Th C14 55.41(18) . . ? C5 Th C14 92.8(2) . . ? C8 Th C14 91.64(19) . . ? C3 Th C14 147.56(19) . . ? C9 Th C14 120.06(19) . . ? C10 Th C14 80.57(18) . . ? C7 Th C14 73.39(19) . . ? C13 Th C14 28.7(2) . . ? C1 Th C6 143.66(13) . . ? C4 Th C6 55.3(3) . . ? C15 Th C6 94.2(2) . . ? C12 Th C6 87.68(19) . . ? C11 Th C6 115.5(2) . . ? C16 Th C6 123.7(2) . . ? C5 Th C6 28.7(3) . . ? C8 Th C6 55.8(2) . . ? C3 Th C6 73.8(2) . . ? C9 Th C6 74.6(2) . . ? C10 Th C6 142.94(19) . . ? C7 Th C6 29.1(3) . . ? C13 Th C6 71.32(14) . . ? C14 Th C6 74.30(17) . . ? C1 Th C2 64.04(11) . . ? C4 Th C2 55.5(2) . . ? C15 Th C2 136.2(2) . . ? C12 Th C2 146.5(2) . . ? C11 Th C2 137.6(2) . . ? C16 Th C2 128.9(2) . . ? C5 Th C2 74.4(2) . . ? C8 Th C2 55.3(2) . . ? C3 Th C2 28.9(2) . . ? C9 Th C2 29.1(2) . . ? C10 Th C2 131.49(18) . . ? C7 Th C2 73.76(19) . . ? C13 Th C2 151.06(14) . . ? C14 Th C2 146.32(18) . . ? C6 Th C2 80.64(10) . . ? C1 Th C17 68.42(17) . . ? C4 Th C17 150.0(2) . . ? C15 Th C17 55.26(19) . . ? C12 Th C17 74.91(19) . . ? C11 Th C17 56.2(2) . . ? C16 Th C17 28.8(2) . . ? C5 Th C17 155.3(2) . . ? C8 Th C17 123.7(2) . . ? C3 Th C17 138.58(18) . . ? C9 Th C17 121.7(2) . . ? C10 Th C17 29.07(11) . . ? C7 Th C17 134.3(2) . . ? C13 Th C17 80.83(18) . . ? C14 Th C17 73.23(18) . . ? C6 Th C17 147.5(2) . . ? C2 Th C17 128.08(18) . . ? N1 Na O2 86.81(13) . . ? N1 Na O1 92.85(15) . . ? O2 Na O1 66.71(11) . . ? N1 Na O5 97.25(13) . . ? O2 Na O5 171.2(2) . . ? O1 Na O5 120.7(2) . . ? N1 Na O4 91.40(15) . . ? O2 Na O4 106.9(2) . . ? O1 Na O4 172.06(19) . . ? O5 Na O4 65.31(12) . . ? N1 Na O3 126.8(2) . . ? O2 Na O3 61.86(13) . . ? O1 Na O3 109.66(12) . . ? O5 Na O3 109.69(14) . . ? O4 Na O3 62.50(15) . . ? N1 Na O6 113.7(2) . . ? O2 Na O6 124.14(15) . . ? O1 Na O6 61.19(15) . . ? O5 Na O6 61.29(14) . . ? O4 Na O6 122.79(12) . . ? O3 Na O6 119.36(11) . . ? C18 O1 C29 112.2(4) . . ? C18 O1 Na 117.7(3) . . ? C29 O1 Na 124.4(4) . . ? C20 O2 C19 113.9(3) . . ? C20 O2 Na 112.7(3) . . ? C19 O2 Na 106.6(3) . . ? C21 O3 C22 112.4(4) . . ? C21 O3 Na 117.7(4) . . ? C22 O3 Na 117.0(3) . . ? C24 O4 C23 114.3(4) . . ? C24 O4 Na 108.3(3) . . ? C23 O4 Na 109.2(3) . . ? C25 O5 C26 111.4(4) . . ? C25 O5 Na 119.6(4) . . ? C26 O5 Na 123.6(3) . . ? C27 O6 C28 111.3(4) . . ? C27 O6 Na 109.8(3) . . ? C28 O6 Na 110.7(3) . . ? C1 N1 Na 169.2(4) . . ? N1 C1 Th 176.4(3) . . ? C3 C2 C9 135.4(3) . . ? C3 C2 Th 73.7(3) . . ? C9 C2 Th 74.3(3) . . ? C3 C2 H2 112.3 . . ? C9 C2 H2 112.3 . . ? Th C2 H2 136.5 . . ? C4 C3 C2 135.9(6) . . ? C4 C3 Th 74.0(4) . . ? C2 C3 Th 77.3(3) . . ? C4 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? Th C3 H3 131.3 . . ? C3 C4 C5 133.9(7) . . ? C3 C4 Th 76.7(4) . . ? C5 C4 Th 76.3(4) . . ? C3 C4 H4 113.0 . . ? C5 C4 H4 113.0 . . ? Th C4 H4 126.6 . . ? C6 C5 C4 135.0(7) . . ? C6 C5 Th 77.4(3) . . ? C4 C5 Th 74.0(4) . . ? C6 C5 H5 112.5 . . ? C4 C5 H5 112.5 . . ? Th C5 H5 130.1 . . ? C5 C6 C7 135.6(4) . . ? C5 C6 Th 73.9(4) . . ? C7 C6 Th 75.1(3) . . ? C5 C6 H6 112.2 . . ? C7 C6 H6 112.2 . . ? Th C6 H6 135.1 . . ? C6 C7 C8 135.1(6) . . ? C6 C7 Th 75.8(4) . . ? C8 C7 Th 73.9(4) . . ? C6 C7 H7 112.4 . . ? C8 C7 H7 112.4 . . ? Th C7 H7 133.1 . . ? C9 C8 C7 134.0(6) . . ? C9 C8 Th 76.1(4) . . ? C7 C8 Th 76.6(4) . . ? C9 C8 H8 113.0 . . ? C7 C8 H8 113.0 . . ? Th C8 H8 127.0 . . ? C8 C9 C2 134.4(6) . . ? C8 C9 Th 74.6(4) . . ? C2 C9 Th 76.6(3) . . ? C8 C9 H9 112.8 . . ? C2 C9 H9 112.8 . . ? Th C9 H9 129.9 . . ? C17 C10 C11 136.6(8) . . ? C17 C10 Th 76.5(5) . . ? C11 C10 Th 73.8(4) . . ? C17 C10 H10 111.7 . . ? C11 C10 H10 111.7 . . ? Th C10 H10 133.8 . . ? C12 C11 C10 132.5(7) . . ? C12 C11 Th 75.4(4) . . ? C10 C11 Th 76.5(4) . . ? C12 C11 H11 113.7 . . ? C10 C11 H11 113.7 . . ? Th C11 H11 127.1 . . ? C13 C12 C11 135.6(6) . . ? C13 C12 Th 77.6(3) . . ? C11 C12 Th 75.2(4) . . ? C13 C12 H12 112.2 . . ? C11 C12 H12 112.2 . . ? Th C12 H12 128.4 . . ? C12 C13 C14 135.1(6) . . ? C12 C13 Th 73.5(3) . . ? C14 C13 Th 75.5(4) . . ? C12 C13 H13 112.5 . . ? C14 C13 H13 112.5 . . ? Th C13 H13 134.3 . . ? C15 C14 C13 136.2(6) . . ? C15 C14 Th 73.5(3) . . ? C13 C14 Th 75.7(4) . . ? C15 C14 H14 111.9 . . ? C13 C14 H14 111.9 . . ? Th C14 H14 135.3 . . ? C14 C15 C16 134.5(6) . . ? C14 C15 Th 77.7(3) . . ? C16 C15 Th 75.4(4) . . ? C14 C15 H15 112.7 . . ? C16 C15 H15 112.7 . . ? Th C15 H15 127.0 . . ? C17 C16 C15 133.8(7) . . ? C17 C16 Th 77.8(4) . . ? C15 C16 Th 74.7(4) . . ? C17 C16 H16 113.1 . . ? C15 C16 H16 113.1 . . ? Th C16 H16 127.2 . . ? C16 C17 C10 134.9(8) . . ? C16 C17 Th 73.4(5) . . ? C10 C17 Th 74.4(5) . . ? C16 C17 H17 112.6 . . ? C10 C17 H17 112.6 . . ? Th C17 H17 136.2 . . ? O1 C18 C19 108.4(4) . . ? O1 C18 H18A 110.0 . . ? C19 C18 H18A 110.0 . . ? O1 C18 H18B 110.0 . . ? C19 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? O2 C19 C18 112.7(3) . . ? O2 C19 H19A 109.1 . . ? C18 C19 H19A 109.1 . . ? O2 C19 H19B 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? O2 C20 C21 106.0(4) . . ? O2 C20 H20A 110.5 . . ? C21 C20 H20A 110.5 . . ? O2 C20 H20B 110.5 . . ? C21 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? O3 C21 C20 108.3(5) . . ? O3 C21 H21A 110.0 . . ? C20 C21 H21A 110.0 . . ? O3 C21 H21B 110.0 . . ? C20 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? O3 C22 C23 108.5(5) . . ? O3 C22 H22A 110.0 . . ? C23 C22 H22A 110.0 . . ? O3 C22 H22B 110.0 . . ? C23 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? O4 C23 C22 106.6(5) . . ? O4 C23 H23A 110.4 . . ? C22 C23 H23A 110.4 . . ? O4 C23 H23B 110.4 . . ? C22 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? O4 C24 C25 113.1(4) . . ? O4 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? O4 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O5 C25 C24 108.7(4) . . ? O5 C25 H25A 109.9 . . ? C24 C25 H25A 109.9 . . ? O5 C25 H25B 109.9 . . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? O5 C26 C27 108.2(4) . . ? O5 C26 H26A 110.1 . . ? C27 C26 H26A 110.1 . . ? O5 C26 H26B 110.1 . . ? C27 C26 H26B 110.1 . . ? H26A C26 H26B 108.4 . . ? O6 C27 C26 109.4(4) . . ? O6 C27 H27A 109.8 . . ? C26 C27 H27A 109.8 . . ? O6 C27 H27B 109.8 . . ? C26 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? O6 C28 C29 109.1(4) . . ? O6 C28 H28A 109.9 . . ? C29 C28 H28A 109.9 . . ? O6 C28 H28B 109.9 . . ? C29 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? O1 C29 C28 107.5(5) . . ? O1 C29 H29A 110.2 . . ? C28 C29 H29A 110.2 . . ? O1 C29 H29B 110.2 . . ? C28 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 918802' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1357747294.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 N3 Na O6 Th' _chemical_formula_weight 769.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 'P 21/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 12.7844(4) _cell_length_b 19.3693(6) _cell_length_c 13.0254(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.214(2) _cell_angle_gamma 90.00 _cell_volume 2918.11(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 123806 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 30.51 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 5.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.459 _exptl_absorpt_correction_T_max 0.733 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (520 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 123806 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8909 _reflns_number_gt 7211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for the C atoms of the crown ether moiety. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0421P)^2^+4.2611P] 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 8909 _refine_ls_number_parameters 352 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.697 _refine_diff_density_min -1.433 _refine_diff_density_rms 0.165 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 Th Th 0.311536(12) 0.120893(7) 0.550053(11) 0.02118(5) Uani 1 1 d . . . Na Na -0.12797(15) 0.14174(9) 0.00547(14) 0.0281(3) Uani 1 1 d . . . O1 O -0.0974(5) 0.2570(2) -0.0567(4) 0.0720(15) Uani 1 1 d . . . O2 O -0.0524(5) 0.1382(2) -0.1407(4) 0.0649(13) Uani 1 1 d . . . O3 O -0.2268(4) 0.0534(2) -0.1516(4) 0.0721(15) Uani 1 1 d . . . O4 O -0.1169(3) 0.01678(18) 0.0773(4) 0.0533(10) Uani 1 1 d . . . O5 O -0.2362(5) 0.12412(18) 0.1216(4) 0.0615(14) Uani 1 1 d . . . O6 O -0.2927(3) 0.2222(2) -0.0376(3) 0.0469(10) Uani 1 1 d . . . N1 N 0.1496(3) 0.1145(2) 0.3535(3) 0.0330(8) Uani 1 1 d . . . N2 N 0.1080(3) 0.1362(2) 0.2600(3) 0.0304(7) Uani 1 1 d . . . N3 N 0.0648(4) 0.1563(2) 0.1674(3) 0.0443(10) Uani 1 1 d . . . C1 C 0.1087(4) 0.0599(2) 0.5405(4) 0.0320(9) Uani 1 1 d . . . H1 H 0.0319 0.0577 0.4875 0.038 Uiso 1 1 calc R . . C2 C 0.1299(4) 0.1170(2) 0.6126(4) 0.0319(9) Uani 1 1 d . . . H2 H 0.0666 0.1464 0.5912 0.038 Uiso 1 1 calc R . . C3 C 0.2247(4) 0.1396(2) 0.7093(4) 0.0319(9) Uani 1 1 d . . . H3 H 0.2117 0.1815 0.7367 0.038 Uiso 1 1 calc R . . C4 C 0.3353(4) 0.1128(2) 0.7741(4) 0.0331(10) Uani 1 1 d . . . H4 H 0.3755 0.1385 0.8395 0.040 Uiso 1 1 calc R . . C5 C 0.4003(4) 0.0569(2) 0.7649(4) 0.0328(9) Uani 1 1 d . . . H5 H 0.4720 0.0540 0.8269 0.039 Uiso 1 1 calc R . . C6 C 0.3842(4) 0.0041(2) 0.6854(4) 0.0339(10) Uani 1 1 d . . . H6 H 0.4501 -0.0226 0.7029 0.041 Uiso 1 1 calc R . . C7 C 0.2904(4) -0.0172(2) 0.5855(4) 0.0347(10) Uani 1 1 d . . . H7 H 0.3086 -0.0536 0.5495 0.042 Uiso 1 1 calc R . . C8 C 0.1743(4) 0.0049(2) 0.5279(4) 0.0320(9) Uani 1 1 d . . . H8 H 0.1309 -0.0238 0.4673 0.038 Uiso 1 1 calc R . . C9 C 0.3445(4) 0.2063(2) 0.3926(4) 0.0359(10) Uani 1 1 d . . . H9 H 0.3000 0.2207 0.3185 0.043 Uiso 1 1 calc R . . C10 C 0.3338(4) 0.2503(2) 0.4714(4) 0.0361(10) Uani 1 1 d . . . H10 H 0.2783 0.2843 0.4374 0.043 Uiso 1 1 calc R . . C11 C 0.3868(4) 0.2561(2) 0.5915(4) 0.0362(10) Uani 1 1 d . . . H11 H 0.3558 0.2908 0.6194 0.043 Uiso 1 1 calc R . . C12 C 0.4770(4) 0.2194(3) 0.6762(4) 0.0385(11) Uani 1 1 d . . . H12 H 0.4974 0.2381 0.7480 0.046 Uiso 1 1 calc R . . C13 C 0.5440(4) 0.1614(3) 0.6788(4) 0.0402(11) Uani 1 1 d . . . H13 H 0.6018 0.1532 0.7511 0.048 Uiso 1 1 calc R . . C14 C 0.5455(4) 0.1132(2) 0.6007(5) 0.0377(11) Uani 1 1 d . . . H14 H 0.5985 0.0780 0.6347 0.045 Uiso 1 1 calc R . . C15 C 0.4864(4) 0.1048(3) 0.4828(5) 0.0357(10) Uani 1 1 d . . . H15 H 0.5044 0.0638 0.4567 0.043 Uiso 1 1 calc R . . C16 C 0.4059(4) 0.1455(3) 0.3965(4) 0.0348(10) Uani 1 1 d . . . H16 H 0.3891 0.1281 0.3246 0.042 Uiso 1 1 calc R . . C17 C -0.0014(10) 0.2499(5) -0.0935(9) 0.119(4) Uani 1 1 d DU . . H17A H 0.0070 0.2931 -0.1271 0.143 Uiso 1 1 calc R . . H17B H 0.0705 0.2411 -0.0274 0.143 Uiso 1 1 calc R . . C18 C -0.0226(9) 0.1933(5) -0.1768(9) 0.112(3) Uani 1 1 d DU . . H18A H -0.0834 0.2066 -0.2495 0.134 Uiso 1 1 calc R . . H18B H 0.0470 0.1846 -0.1871 0.134 Uiso 1 1 calc R . . C19 C -0.1240(7) 0.0986(6) -0.2418(6) 0.094(3) Uani 1 1 d DU . . H19A H -0.0806 0.0882 -0.2854 0.112 Uiso 1 1 calc R . . H19B H -0.1917 0.1252 -0.2893 0.112 Uiso 1 1 calc R . . C20 C -0.1598(7) 0.0339(5) -0.2057(8) 0.107(3) Uani 1 1 d DU . . H20A H -0.2038 0.0052 -0.2709 0.129 Uiso 1 1 calc R . . H20B H -0.0927 0.0082 -0.1545 0.129 Uiso 1 1 calc R . . C21 C -0.2632(8) -0.0060(4) -0.1066(8) 0.103(3) Uani 1 1 d U . . H21A H -0.2904 -0.0418 -0.1641 0.124 Uiso 1 1 calc R . . H21B H -0.3276 0.0075 -0.0901 0.124 Uiso 1 1 calc R . . C22 C -0.1688(8) -0.0352(3) -0.0007(9) 0.111(3) Uani 1 1 d U . . H22A H -0.2010 -0.0694 0.0320 0.133 Uiso 1 1 calc R . . H22B H -0.1115 -0.0577 -0.0196 0.133 Uiso 1 1 calc R . . C23 C -0.1425(8) 0.0229(5) 0.1779(8) 0.112(3) Uani 1 1 d DU . . H23A H -0.0769 0.0449 0.2381 0.134 Uiso 1 1 calc R . . H23B H -0.1485 -0.0234 0.2035 0.134 Uiso 1 1 calc R . . C24 C -0.2483(8) 0.0615(4) 0.1634(7) 0.098(3) Uani 1 1 d DU . . H24A H -0.3173 0.0380 0.1105 0.118 Uiso 1 1 calc R . . H24B H -0.2529 0.0667 0.2354 0.118 Uiso 1 1 calc R . . C25 C -0.3542(7) 0.1478(5) 0.0651(7) 0.084(2) Uani 1 1 d U . . H25A H -0.3915 0.1445 0.1160 0.101 Uiso 1 1 calc R . . H25B H -0.3968 0.1193 -0.0010 0.101 Uiso 1 1 calc R . . C26 C -0.3536(5) 0.2188(5) 0.0309(5) 0.071(2) Uani 1 1 d U . . H26A H -0.4322 0.2350 -0.0114 0.085 Uiso 1 1 calc R . . H26B H -0.3163 0.2479 0.0973 0.085 Uiso 1 1 calc R . . C27 C -0.2721(7) 0.2915(3) -0.0586(6) 0.077(2) Uani 1 1 d U . . H27A H -0.2317 0.3158 0.0126 0.093 Uiso 1 1 calc R . . H27B H -0.3450 0.3149 -0.1016 0.093 Uiso 1 1 calc R . . C28 C -0.2016(9) 0.2913(4) -0.1233(6) 0.092(3) Uani 1 1 d U . . H28A H -0.2421 0.2674 -0.1950 0.110 Uiso 1 1 calc R . . H28B H -0.1861 0.3382 -0.1389 0.110 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 Th 0.02002(8) 0.02288(8) 0.02092(8) 0.00013(5) 0.00898(6) -0.00214(5) Na 0.0266(8) 0.0303(8) 0.0262(8) 0.0015(7) 0.0101(7) 0.0026(7) O1 0.132(5) 0.039(2) 0.085(3) -0.010(2) 0.086(4) -0.023(3) O2 0.103(4) 0.061(2) 0.055(3) 0.019(2) 0.057(3) 0.034(3) O3 0.055(3) 0.059(3) 0.063(3) -0.028(2) -0.013(2) 0.030(2) O4 0.043(2) 0.0337(19) 0.083(3) 0.0129(19) 0.026(2) 0.0038(16) O5 0.105(4) 0.039(2) 0.076(3) -0.0066(18) 0.072(3) -0.016(2) O6 0.042(2) 0.054(2) 0.0338(18) -0.0114(16) 0.0060(16) 0.0206(17) N1 0.0246(19) 0.045(2) 0.0243(18) 0.0031(15) 0.0051(15) -0.0036(15) N2 0.0230(17) 0.0350(18) 0.0293(18) -0.0021(15) 0.0074(15) -0.0040(15) N3 0.037(2) 0.055(3) 0.027(2) 0.0075(18) 0.0005(17) -0.005(2) C1 0.025(2) 0.043(2) 0.028(2) -0.0008(18) 0.0119(18) -0.0095(18) C2 0.026(2) 0.038(2) 0.037(2) 0.0010(18) 0.0186(19) 0.0007(17) C3 0.036(2) 0.032(2) 0.033(2) -0.0049(18) 0.020(2) -0.0028(19) C4 0.037(3) 0.039(2) 0.025(2) -0.0032(17) 0.0141(19) -0.0111(19) C5 0.032(2) 0.042(2) 0.022(2) 0.0068(17) 0.0092(18) -0.0032(19) C6 0.037(3) 0.032(2) 0.038(2) 0.0095(19) 0.020(2) 0.0041(19) C7 0.050(3) 0.024(2) 0.043(3) -0.0011(18) 0.032(2) -0.0013(19) C8 0.041(3) 0.032(2) 0.028(2) -0.0057(17) 0.019(2) -0.0133(19) C9 0.037(3) 0.041(2) 0.026(2) 0.0095(18) 0.0098(19) -0.009(2) C10 0.031(2) 0.029(2) 0.045(3) 0.0080(19) 0.013(2) -0.0015(18) C11 0.044(3) 0.025(2) 0.047(3) -0.0037(19) 0.027(2) -0.0083(19) C12 0.042(3) 0.043(3) 0.031(2) -0.0094(19) 0.017(2) -0.022(2) C13 0.030(2) 0.050(3) 0.034(2) 0.005(2) 0.007(2) -0.014(2) C14 0.020(2) 0.042(3) 0.050(3) 0.014(2) 0.014(2) 0.0020(18) C15 0.031(2) 0.035(2) 0.052(3) -0.002(2) 0.028(2) -0.0002(19) C16 0.038(3) 0.042(2) 0.030(2) -0.0073(19) 0.020(2) -0.012(2) C17 0.144(7) 0.142(7) 0.110(6) -0.024(5) 0.090(6) -0.090(6) C18 0.115(7) 0.129(7) 0.134(7) 0.035(6) 0.095(6) 0.025(5) C19 0.070(5) 0.177(7) 0.035(3) -0.011(4) 0.024(3) 0.048(5) C20 0.069(5) 0.120(6) 0.094(5) -0.070(5) -0.003(4) 0.037(5) C21 0.079(5) 0.037(3) 0.124(6) -0.007(4) -0.024(4) -0.006(3) C22 0.081(5) 0.034(3) 0.141(7) 0.000(4) -0.027(5) 0.002(3) C23 0.099(6) 0.138(7) 0.124(6) 0.097(5) 0.071(5) 0.022(5) C24 0.164(8) 0.076(5) 0.083(5) -0.004(4) 0.079(5) -0.023(5) C25 0.061(4) 0.139(6) 0.073(4) -0.046(5) 0.050(4) -0.045(4) C26 0.034(3) 0.125(6) 0.049(3) -0.030(4) 0.013(3) 0.022(3) C27 0.080(5) 0.039(3) 0.064(4) -0.012(3) -0.017(3) 0.027(3) C28 0.160(7) 0.038(3) 0.045(3) 0.008(3) 0.013(4) -0.023(4) _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 Th N1 2.518(4) . ? Th C15 2.744(4) . ? Th C7 2.747(4) . ? Th C3 2.762(4) . ? Th C11 2.762(4) . ? Th C10 2.768(4) . ? Th C2 2.770(4) . ? Th C6 2.774(4) . ? Th C14 2.779(5) . ? Th C16 2.782(4) . ? Th C8 2.790(4) . ? Th C12 2.803(4) . ? Th C1 2.804(4) . ? Th C9 2.804(4) . ? Th C4 2.807(4) . ? Th C5 2.820(4) . ? Th C13 2.830(5) . ? Na O1 2.463(4) . ? Na O5 2.470(4) . ? Na O2 2.477(4) . ? Na O6 2.484(4) . ? Na N3 2.484(4) . ? Na O3 2.551(4) . ? Na O4 2.577(4) . ? N1 N2 1.179(5) . ? N2 N3 1.159(5) . ? C1 C2 1.401(6) . ? C1 C8 1.407(7) . ? C1 H1 0.9300 . ? C2 C3 1.395(7) . ? C2 H2 0.9300 . ? C3 C4 1.401(7) . ? C3 H3 0.9300 . ? C4 C5 1.400(7) . ? C4 H4 0.9300 . ? C5 C6 1.407(6) . ? C5 H5 0.9300 . ? C6 C7 1.404(7) . ? C6 H6 0.9300 . ? C7 C8 1.415(7) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.386(7) . ? C9 C16 1.405(7) . ? C9 H9 0.9300 . ? C10 C11 1.420(7) . ? C10 H10 0.9300 . ? C11 C12 1.402(7) . ? C11 H11 0.9300 . ? C12 C13 1.406(8) . ? C12 H12 0.9300 . ? C13 C14 1.386(8) . ? C13 H13 0.9300 . ? C14 C15 1.403(8) . ? C14 H14 0.9300 . ? C15 C16 1.399(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.485(5) . ? C17 O1 1.502(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O2 1.287(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O2 1.461(10) . ? C19 C20 1.477(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O3 1.374(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O3 1.455(10) . ? C21 C22 1.503(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O4 1.383(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O4 1.485(10) . ? C23 C24 1.485(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O5 1.366(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O5 1.443(10) . ? C25 C26 1.447(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O6 1.414(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O6 1.417(8) . ? C27 C28 1.473(12) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O1 1.408(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Th C15 95.66(15) . . ? N1 Th C7 91.50(14) . . ? C15 Th C7 95.44(14) . . ? N1 Th C3 110.53(14) . . ? C15 Th C3 153.81(15) . . ? C7 Th C3 84.34(14) . . ? N1 Th C11 108.19(14) . . ? C15 Th C11 84.64(15) . . ? C7 Th C11 160.22(16) . . ? C3 Th C11 86.98(14) . . ? N1 Th C10 80.65(14) . . ? C15 Th C10 76.04(15) . . ? C7 Th C10 167.66(15) . . ? C3 Th C10 107.27(15) . . ? C11 Th C10 29.75(14) . . ? N1 Th C2 82.44(14) . . ? C15 Th C2 171.77(14) . . ? C7 Th C2 76.65(13) . . ? C3 Th C2 29.22(14) . . ? C11 Th C2 103.56(14) . . ? C10 Th C2 111.39(14) . . ? N1 Th C6 120.93(14) . . ? C15 Th C6 90.72(14) . . ? C7 Th C6 29.45(15) . . ? C3 Th C6 76.24(14) . . ? C11 Th C6 130.88(15) . . ? C10 Th C6 156.14(15) . . ? C2 Th C6 83.47(13) . . ? N1 Th C14 125.07(15) . . ? C15 Th C14 29.42(16) . . ? C7 Th C14 94.63(14) . . ? C3 Th C14 124.39(15) . . ? C11 Th C14 75.77(15) . . ? C10 Th C14 82.34(14) . . ? C2 Th C14 151.76(15) . . ? C6 Th C14 76.72(14) . . ? N1 Th C16 72.42(13) . . ? C15 Th C16 29.32(15) . . ? C7 Th C16 113.04(14) . . ? C3 Th C16 162.51(15) . . ? C11 Th C16 75.90(14) . . ? C10 Th C16 55.56(15) . . ? C2 Th C16 152.98(15) . . ? C6 Th C16 117.80(14) . . ? C14 Th C16 55.06(15) . . ? N1 Th C8 69.31(13) . . ? C15 Th C8 115.94(14) . . ? C7 Th C8 29.60(15) . . ? C3 Th C8 75.34(13) . . ? C11 Th C8 159.28(14) . . ? C10 Th C8 148.26(14) . . ? C2 Th C8 55.89(13) . . ? C6 Th C8 55.54(14) . . ? C14 Th C8 123.19(14) . . ? C16 Th C8 120.66(13) . . ? N1 Th C12 135.86(14) . . ? C15 Th C12 75.56(15) . . ? C7 Th C12 131.92(16) . . ? C3 Th C12 85.11(14) . . ? C11 Th C12 29.17(15) . . ? C10 Th C12 55.21(15) . . ? C2 Th C12 111.35(14) . . ? C6 Th C12 102.60(15) . . ? C14 Th C12 55.26(16) . . ? C16 Th C12 81.65(14) . . ? C8 Th C12 153.34(13) . . ? N1 Th C1 65.79(13) . . ? C15 Th C1 143.28(14) . . ? C7 Th C1 56.06(15) . . ? C3 Th C1 55.16(13) . . ? C11 Th C1 130.33(14) . . ? C10 Th C1 127.17(14) . . ? C2 Th C1 29.12(13) . . ? C6 Th C1 74.76(14) . . ? C14 Th C1 150.39(14) . . ? C16 Th C1 135.75(13) . . ? C8 Th C1 29.14(14) . . ? C12 Th C1 139.99(13) . . ? N1 Th C9 66.41(13) . . ? C15 Th C9 55.71(15) . . ? C7 Th C9 138.92(14) . . ? C3 Th C9 134.92(15) . . ? C11 Th C9 55.61(14) . . ? C10 Th C9 28.79(14) . . ? C2 Th C9 129.61(14) . . ? C6 Th C9 146.35(14) . . ? C14 Th C9 73.93(14) . . ? C16 Th C9 29.12(15) . . ? C8 Th C9 133.13(13) . . ? C12 Th C9 73.49(14) . . ? C1 Th C9 129.85(14) . . ? N1 Th C4 137.08(14) . . ? C15 Th C4 125.69(15) . . ? C7 Th C4 75.25(13) . . ? C3 Th C4 29.14(14) . . ? C11 Th C4 88.61(13) . . ? C10 Th C4 116.93(14) . . ? C2 Th C4 54.95(15) . . ? C6 Th C4 55.58(14) . . ? C14 Th C4 96.96(15) . . ? C16 Th C4 150.35(14) . . ? C8 Th C4 81.21(13) . . ? C12 Th C4 73.04(13) . . ? C1 Th C4 73.21(13) . . ? C9 Th C4 144.14(14) . . ? N1 Th C5 142.81(13) . . ? C15 Th C5 103.23(15) . . ? C7 Th C5 55.39(14) . . ? C3 Th C5 55.42(14) . . ? C11 Th C5 105.26(14) . . ? C10 Th C5 134.75(14) . . ? C2 Th C5 74.29(14) . . ? C6 Th C5 29.13(13) . . ? C14 Th C5 78.67(14) . . ? C16 Th C5 132.42(14) . . ? C8 Th C5 73.63(13) . . ? C12 Th C5 80.41(14) . . ? C1 Th C5 80.34(13) . . ? C9 Th C5 149.69(14) . . ? C4 Th C5 28.80(14) . . ? N1 Th C13 144.78(13) . . ? C15 Th C13 55.12(16) . . ? C7 Th C13 108.88(15) . . ? C3 Th C13 100.09(14) . . ? C11 Th C13 55.33(16) . . ? C10 Th C13 73.80(15) . . ? C2 Th C13 129.30(15) . . ? C6 Th C13 82.34(15) . . ? C14 Th C13 28.59(16) . . ? C16 Th C13 73.20(14) . . ? C8 Th C13 137.72(15) . . ? C12 Th C13 28.89(15) . . ? C1 Th C13 149.41(13) . . ? C9 Th C13 79.79(14) . . ? C4 Th C13 77.19(14) . . ? C5 Th C13 69.93(14) . . ? O1 Na O5 122.37(15) . . ? O1 Na O2 66.63(15) . . ? O5 Na O2 166.15(19) . . ? O1 Na O6 66.09(17) . . ? O5 Na O6 65.36(16) . . ? O2 Na O6 114.47(15) . . ? O1 Na N3 86.40(19) . . ? O5 Na N3 96.18(19) . . ? O2 Na N3 94.89(18) . . ? O6 Na N3 124.00(16) . . ? O1 Na O3 116.00(18) . . ? O5 Na O3 100.55(18) . . ? O2 Na O3 65.62(19) . . ? O6 Na O3 99.04(14) . . ? N3 Na O3 136.91(16) . . ? O1 Na O4 168.29(18) . . ? O5 Na O4 66.83(14) . . ? O2 Na O4 105.92(15) . . ? O6 Na O4 125.57(15) . . ? N3 Na O4 85.26(15) . . ? O3 Na O4 65.97(16) . . ? C28 O1 C17 122.3(7) . . ? C28 O1 Na 112.9(4) . . ? C17 O1 Na 106.7(5) . . ? C18 O2 C19 106.0(7) . . ? C18 O2 Na 122.1(4) . . ? C19 O2 Na 114.0(4) . . ? C20 O3 C21 111.5(7) . . ? C20 O3 Na 113.0(4) . . ? C21 O3 Na 110.0(4) . . ? C22 O4 C23 119.3(7) . . ? C22 O4 Na 118.8(5) . . ? C23 O4 Na 104.3(4) . . ? C24 O5 C25 102.4(6) . . ? C24 O5 Na 123.7(4) . . ? C25 O5 Na 112.4(4) . . ? C26 O6 C27 111.3(6) . . ? C26 O6 Na 118.0(4) . . ? C27 O6 Na 115.4(4) . . ? N2 N1 Th 147.8(3) . . ? N3 N2 N1 178.3(5) . . ? N2 N3 Na 134.9(4) . . ? C2 C1 C8 136.2(4) . . ? C2 C1 Th 74.1(2) . . ? C8 C1 Th 74.9(2) . . ? C2 C1 H1 111.9 . . ? C8 C1 H1 111.9 . . ? Th C1 H1 135.7 . . ? C3 C2 C1 134.3(4) . . ? C3 C2 Th 75.1(3) . . ? C1 C2 Th 76.8(3) . . ? C3 C2 H2 112.9 . . ? C1 C2 H2 112.9 . . ? Th C2 H2 128.8 . . ? C2 C3 C4 133.9(4) . . ? C2 C3 Th 75.7(3) . . ? C4 C3 Th 77.2(3) . . ? C2 C3 H3 113.1 . . ? C4 C3 H3 113.1 . . ? Th C3 H3 126.7 . . ? C5 C4 C3 135.9(4) . . ? C5 C4 Th 76.1(3) . . ? C3 C4 Th 73.6(3) . . ? C5 C4 H4 112.1 . . ? C3 C4 H4 112.1 . . ? Th C4 H4 134.0 . . ? C4 C5 C6 136.0(4) . . ? C4 C5 Th 75.1(3) . . ? C6 C5 Th 73.6(2) . . ? C4 C5 H5 112.0 . . ? C6 C5 H5 112.0 . . ? Th C5 H5 135.9 . . ? C7 C6 C5 134.0(4) . . ? C7 C6 Th 74.2(3) . . ? C5 C6 Th 77.2(3) . . ? C7 C6 H6 113.0 . . ? C5 C6 H6 113.0 . . ? Th C6 H6 129.2 . . ? C6 C7 C8 133.8(4) . . ? C6 C7 Th 76.3(3) . . ? C8 C7 Th 76.9(2) . . ? C6 C7 H7 113.1 . . ? C8 C7 H7 113.1 . . ? Th C7 H7 126.2 . . ? C1 C8 C7 135.2(4) . . ? C1 C8 Th 76.0(2) . . ? C7 C8 Th 73.5(2) . . ? C1 C8 H8 112.4 . . ? C7 C8 H8 112.4 . . ? Th C8 H8 133.6 . . ? C10 C9 C16 136.0(4) . . ? C10 C9 Th 74.2(3) . . ? C16 C9 Th 74.6(2) . . ? C10 C9 H9 112.0 . . ? C16 C9 H9 112.0 . . ? Th C9 H9 136.0 . . ? C9 C10 C11 135.5(5) . . ? C9 C10 Th 77.0(3) . . ? C11 C10 Th 74.9(3) . . ? C9 C10 H10 112.3 . . ? C11 C10 H10 112.3 . . ? Th C10 H10 129.8 . . ? C12 C11 C10 132.4(5) . . ? C12 C11 Th 77.0(3) . . ? C10 C11 Th 75.3(3) . . ? C12 C11 H11 113.8 . . ? C10 C11 H11 113.8 . . ? Th C11 H11 126.3 . . ? C11 C12 C13 135.4(5) . . ? C11 C12 Th 73.8(3) . . ? C13 C12 Th 76.6(3) . . ? C11 C12 H12 112.3 . . ? C13 C12 H12 112.3 . . ? Th C12 H12 132.2 . . ? C14 C13 C12 136.1(5) . . ? C14 C13 Th 73.6(3) . . ? C12 C13 Th 74.5(3) . . ? C14 C13 H13 112.0 . . ? C12 C13 H13 112.0 . . ? Th C13 H13 137.2 . . ? C13 C14 C15 135.4(5) . . ? C13 C14 Th 77.8(3) . . ? C15 C14 Th 73.9(3) . . ? C13 C14 H14 112.3 . . ? C15 C14 H14 112.3 . . ? Th C14 H14 130.1 . . ? C16 C15 C14 133.1(5) . . ? C16 C15 Th 76.8(3) . . ? C14 C15 Th 76.7(3) . . ? C16 C15 H15 113.5 . . ? C14 C15 H15 113.5 . . ? Th C15 H15 125.1 . . ? C15 C16 C9 135.2(4) . . ? C15 C16 Th 73.8(3) . . ? C9 C16 Th 76.3(3) . . ? C15 C16 H16 112.4 . . ? C9 C16 H16 112.4 . . ? Th C16 H16 132.6 . . ? C18 C17 O1 112.5(6) . . ? C18 C17 H17A 109.1 . . ? O1 C17 H17A 109.1 . . ? C18 C17 H17B 109.1 . . ? O1 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? O2 C18 C17 109.6(7) . . ? O2 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? O2 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? O2 C19 C20 108.6(6) . . ? O2 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? O2 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.3 . . ? O3 C20 C19 106.0(6) . . ? O3 C20 H20A 110.5 . . ? C19 C20 H20A 110.5 . . ? O3 C20 H20B 110.5 . . ? C19 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? O3 C21 C22 113.4(7) . . ? O3 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? O3 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? O4 C22 C21 110.3(6) . . ? O4 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? O4 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? O4 C23 C24 117.3(6) . . ? O4 C23 H23A 108.0 . . ? C24 C23 H23A 108.0 . . ? O4 C23 H23B 108.0 . . ? C24 C23 H23B 108.0 . . ? H23A C23 H23B 107.2 . . ? O5 C24 C23 104.2(7) . . ? O5 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? O5 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? O5 C25 C26 108.5(5) . . ? O5 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? O5 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O6 C26 C25 108.4(5) . . ? O6 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O6 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? O6 C27 C28 108.4(5) . . ? O6 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O6 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? O1 C28 C27 107.4(5) . . ? O1 C28 H28A 110.2 . . ? C27 C28 H28A 110.2 . . ? O1 C28 H28B 110.2 . . ? C27 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 918803' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6.Na(18c6)(THF)2 #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1357747294.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H73 Na O8 Th2' _chemical_formula_weight 1313.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 15.2646(3) _cell_length_b 15.2646(3) _cell_length_c 22.1864(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5169.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 123984 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.51 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 5.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.396 _exptl_absorpt_correction_T_max 0.666 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps (317 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 123984 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 30.51 _reflns_number_total 7863 _reflns_number_gt 6326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The atom H1 was found on a Fourier-difference map and all the other H atoms were introduced at calculated positions; the positional parameters of H1 were refined, but not its displacement parameter, fixed at 1.2 times that of Th; all the other H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0284P)^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 mixed _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 0.491(7) _chemical_absolute_configuration unk _refine_ls_number_reflns 7863 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.500 _refine_diff_density_min -1.618 _refine_diff_density_rms 0.142 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 Th Th 0.614815(8) 0.099207(8) 0.018453(8) 0.03420(5) Uani 1 1 d . . . H1 H 0.5000 0.0000 0.027(4) 0.041 Uiso 1 2 d S . . Na Na 0.5000 0.5000 0.76706(13) 0.0449(7) Uani 1 2 d S . . O1 O 0.5324(2) 0.58470(18) 0.86446(14) 0.0476(8) Uani 1 1 d . . . O2 O 0.5492(2) 0.6638(2) 0.75505(17) 0.0500(9) Uani 1 1 d . . . O3 O 0.5801(2) 0.5512(2) 0.65953(16) 0.0554(8) Uani 1 1 d . . . O4 O 0.3573(3) 0.5632(2) 0.77764(19) 0.0608(10) Uani 1 1 d . . . C1 C 0.5018(5) 0.1215(4) -0.0765(3) 0.079(2) Uani 1 1 d . . . H1A H 0.4610 0.0850 -0.0950 0.095 Uiso 1 1 calc R . . C2 C 0.4647(3) 0.1705(5) -0.0293(4) 0.085(3) Uani 1 1 d . . . H2 H 0.4052 0.1596 -0.0244 0.102 Uiso 1 1 calc R . . C3 C 0.4961(5) 0.2306(5) 0.0111(3) 0.081(2) Uani 1 1 d . . . H3 H 0.4551 0.2456 0.0404 0.097 Uiso 1 1 calc R . . C4 C 0.5745(5) 0.2740(3) 0.0182(4) 0.082(2) Uani 1 1 d . . . H4 H 0.5740 0.3118 0.0511 0.099 Uiso 1 1 calc R . . C5 C 0.6522(4) 0.2746(3) -0.0112(4) 0.078(2) Uani 1 1 d . . . H5 H 0.6899 0.3172 0.0039 0.094 Uiso 1 1 calc R . . C6 C 0.6885(4) 0.2291(5) -0.0567(4) 0.075(2) Uani 1 1 d . . . H6 H 0.7449 0.2484 -0.0654 0.090 Uiso 1 1 calc R . . C7 C 0.6633(5) 0.1612(5) -0.0937(3) 0.077(2) Uani 1 1 d . . . H7 H 0.7086 0.1423 -0.1186 0.092 Uiso 1 1 calc R . . C8 C 0.5865(5) 0.1140(4) -0.1030(3) 0.079(2) Uani 1 1 d . . . H8 H 0.5913 0.0697 -0.1315 0.094 Uiso 1 1 calc R . . C9 C 0.6526(3) -0.0533(3) 0.0823(3) 0.0522(13) Uani 1 1 d . . . H9 H 0.6258 -0.1078 0.0858 0.063 Uiso 1 1 calc R . . C10 C 0.6230(3) 0.0057(3) 0.1257(2) 0.0556(13) Uani 1 1 d . . . H10 H 0.5791 -0.0177 0.1498 0.067 Uiso 1 1 calc R . . C11 C 0.6444(3) 0.0932(4) 0.1415(2) 0.0572(13) Uani 1 1 d . . . H11 H 0.6098 0.1155 0.1724 0.069 Uiso 1 1 calc R . . C12 C 0.7072(4) 0.1533(3) 0.1201(3) 0.0580(14) Uani 1 1 d . . . H12 H 0.7047 0.2069 0.1400 0.070 Uiso 1 1 calc R . . C13 C 0.7725(3) 0.1512(3) 0.0759(3) 0.0526(13) Uani 1 1 d . . . H13 H 0.8076 0.2010 0.0767 0.063 Uiso 1 1 calc R . . C14 C 0.7972(3) 0.0939(3) 0.0318(2) 0.0514(13) Uani 1 1 d . . . H14 H 0.8426 0.1162 0.0085 0.062 Uiso 1 1 calc R . . C15 C 0.7722(3) 0.0111(3) 0.0127(3) 0.0554(12) Uani 1 1 d . . . H15 H 0.8008 -0.0073 -0.0221 0.066 Uiso 1 1 calc R . . C16 C 0.7122(3) -0.0505(3) 0.0353(2) 0.0538(15) Uani 1 1 d . . . H16 H 0.7127 -0.1023 0.0132 0.065 Uiso 1 1 calc R . . C17 C 0.4903(3) 0.5480(3) 0.9161(2) 0.0489(11) Uani 1 1 d . . . H17A H 0.4276 0.5579 0.9141 0.059 Uiso 1 1 calc R . . H17B H 0.5126 0.5750 0.9526 0.059 Uiso 1 1 calc R . . C18 C 0.5099(4) 0.6745(3) 0.8571(2) 0.0614(14) Uani 1 1 d . . . H18A H 0.5194 0.7062 0.8944 0.074 Uiso 1 1 calc R . . H18B H 0.4487 0.6801 0.8459 0.074 Uiso 1 1 calc R . . C19 C 0.5673(4) 0.7102(3) 0.8084(3) 0.0657(16) Uani 1 1 d . . . H19A H 0.5556 0.7721 0.8026 0.079 Uiso 1 1 calc R . . H19B H 0.6284 0.7032 0.8193 0.079 Uiso 1 1 calc R . . C20 C 0.6052(3) 0.6879(3) 0.7075(2) 0.0541(13) Uani 1 1 d . . . H20A H 0.6648 0.6699 0.7164 0.065 Uiso 1 1 calc R . . H20B H 0.6046 0.7510 0.7023 0.065 Uiso 1 1 calc R . . C21 C 0.5741(3) 0.6442(3) 0.6514(2) 0.0522(13) Uani 1 1 d . . . H21A H 0.5139 0.6607 0.6432 0.063 Uiso 1 1 calc R . . H21B H 0.6099 0.6622 0.6175 0.063 Uiso 1 1 calc R . . C22 C 0.5477(4) 0.5040(4) 0.6096(2) 0.0674(15) Uani 1 1 d . . . H22A H 0.5732 0.4458 0.6096 0.081 Uiso 1 1 calc R . . H22B H 0.5659 0.5331 0.5728 0.081 Uiso 1 1 calc R . . C23 C 0.3254(5) 0.6291(5) 0.7375(4) 0.091(3) Uani 1 1 d . . . H23A H 0.3699 0.6445 0.7081 0.109 Uiso 1 1 calc R . . H23B H 0.3091 0.6814 0.7596 0.109 Uiso 1 1 calc R . . C24 C 0.2479(4) 0.5905(5) 0.7072(4) 0.096(2) Uani 1 1 d . . . H24A H 0.2650 0.5592 0.6711 0.115 Uiso 1 1 calc R . . H24B H 0.2060 0.6356 0.6965 0.115 Uiso 1 1 calc R . . C25 C 0.2101(5) 0.5293(5) 0.7529(4) 0.095(2) Uani 1 1 d . . . H25A H 0.1962 0.4731 0.7348 0.115 Uiso 1 1 calc R . . H25B H 0.1574 0.5535 0.7707 0.115 Uiso 1 1 calc R . . C26 C 0.2816(4) 0.5201(5) 0.7993(3) 0.0808(19) Uani 1 1 d . . . H26A H 0.2631 0.5460 0.8371 0.097 Uiso 1 1 calc R . . H26B H 0.2943 0.4586 0.8062 0.097 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 Th 0.02866(7) 0.03047(7) 0.04347(8) 0.00151(7) -0.00098(7) 0.00019(4) Na 0.0541(15) 0.0381(13) 0.0426(17) 0.000 0.000 -0.0029(12) O1 0.070(2) 0.0353(15) 0.0378(19) -0.0019(13) 0.0048(16) -0.0004(14) O2 0.067(2) 0.0358(16) 0.047(2) -0.0005(14) 0.0038(17) -0.0109(16) O3 0.065(2) 0.0450(17) 0.056(2) 0.0039(16) 0.0007(17) 0.0046(15) O4 0.065(2) 0.054(2) 0.063(3) 0.0107(18) 0.0094(19) 0.0054(18) C1 0.094(5) 0.052(3) 0.091(5) 0.037(3) -0.067(4) -0.034(3) C2 0.030(2) 0.114(5) 0.111(7) 0.087(5) -0.008(3) -0.009(3) C3 0.083(4) 0.096(5) 0.063(5) 0.045(4) 0.027(4) 0.060(4) C4 0.138(6) 0.039(3) 0.070(4) -0.003(3) -0.020(5) 0.027(3) C5 0.087(4) 0.041(3) 0.107(6) 0.022(3) -0.038(4) -0.026(3) C6 0.044(3) 0.096(5) 0.086(5) 0.049(4) 0.011(3) -0.011(3) C7 0.078(4) 0.100(5) 0.052(4) 0.017(4) 0.022(4) 0.038(4) C8 0.148(7) 0.044(3) 0.043(3) -0.011(3) -0.037(4) 0.029(4) C9 0.047(3) 0.043(2) 0.066(4) 0.013(2) -0.020(3) -0.008(2) C10 0.040(2) 0.069(3) 0.058(3) 0.025(3) -0.005(2) -0.004(2) C11 0.053(3) 0.074(3) 0.044(3) -0.005(3) -0.006(2) 0.022(3) C12 0.071(3) 0.042(3) 0.061(4) -0.011(2) -0.025(3) 0.009(2) C13 0.043(2) 0.050(3) 0.065(4) 0.003(2) -0.012(2) -0.014(2) C14 0.0301(19) 0.063(3) 0.061(4) 0.004(3) -0.002(2) -0.0034(19) C15 0.043(2) 0.061(3) 0.061(3) -0.005(3) -0.004(3) 0.019(2) C16 0.050(3) 0.044(2) 0.067(4) -0.014(2) -0.021(3) 0.013(2) C17 0.063(3) 0.049(2) 0.035(3) -0.002(2) 0.006(2) -0.002(2) C18 0.104(4) 0.038(2) 0.043(3) -0.007(2) 0.007(3) -0.006(3) C19 0.105(5) 0.038(2) 0.054(4) -0.001(2) -0.009(3) -0.018(3) C20 0.063(3) 0.045(2) 0.055(4) 0.014(2) -0.004(3) -0.009(2) C21 0.059(3) 0.046(2) 0.052(3) 0.014(2) 0.008(2) -0.001(2) C22 0.092(4) 0.057(3) 0.054(4) -0.002(3) 0.015(3) 0.001(3) C23 0.077(4) 0.077(4) 0.117(7) 0.053(4) 0.011(4) 0.011(4) C24 0.059(3) 0.106(5) 0.122(7) 0.057(5) 0.010(4) 0.010(3) C25 0.075(4) 0.109(6) 0.102(6) 0.039(5) 0.006(4) -0.010(4) C26 0.075(4) 0.104(5) 0.063(4) 0.035(4) 0.005(3) -0.005(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 Th C3 2.708(5) . ? Th C4 2.738(5) . ? Th C8 2.738(6) . ? Th C1 2.745(5) . ? Th C2 2.749(5) . ? Th C16 2.752(4) . ? Th C15 2.755(4) . ? Th C7 2.764(7) . ? Th C11 2.769(5) . ? Th C10 2.777(5) . ? Th C12 2.784(5) . ? Th C9 2.786(4) . ? Th C14 2.800(4) . ? Th C5 2.815(4) . ? Th C6 2.825(5) . ? Th C13 2.836(4) . ? Th H1 2.323(7) . ? Na O4 2.394(4) 2_665 ? Na O4 2.394(4) . ? Na O1 2.566(4) 2_665 ? Na O1 2.566(4) . ? Na O2 2.624(3) 2_665 ? Na O2 2.624(3) . ? Na O3 2.793(4) 2_665 ? Na O3 2.793(4) . ? O1 C18 1.422(5) . ? O1 C17 1.427(5) . ? O2 C20 1.406(6) . ? O2 C19 1.406(6) . ? O3 C22 1.413(6) . ? O3 C21 1.433(5) . ? O4 C26 1.413(7) . ? O4 C23 1.429(7) . ? C1 C2 1.407(10) . ? C1 C8 1.424(10) . ? C1 H1A 0.9300 . ? C2 C3 1.369(10) . ? C2 H2 0.9300 . ? C3 C4 1.377(10) . ? C3 H3 0.9300 . ? C4 C5 1.353(9) . ? C4 H4 0.9300 . ? C5 C6 1.347(10) . ? C5 H5 0.9300 . ? C6 C7 1.377(11) . ? C6 H6 0.9300 . ? C7 C8 1.391(10) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C16 1.387(7) . ? C9 C10 1.392(7) . ? C9 H9 0.9300 . ? C10 C11 1.420(7) . ? C10 H10 0.9300 . ? C11 C12 1.410(8) . ? C11 H11 0.9300 . ? C12 C13 1.398(7) . ? C12 H12 0.9300 . ? C13 C14 1.365(7) . ? C13 H13 0.9300 . ? C14 C15 1.387(6) . ? C14 H14 0.9300 . ? C15 C16 1.405(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C17 1.496(8) 2_665 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.494(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.490(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C22 1.460(11) 2_665 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.482(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.495(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.507(9) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Th C4 29.3(2) . . ? C3 Th C8 76.9(2) . . ? C4 Th C8 83.24(19) . . ? C3 Th C1 56.1(2) . . ? C4 Th C1 74.7(2) . . ? C8 Th C1 30.1(2) . . ? C3 Th C2 29.1(2) . . ? C4 Th C2 55.0(2) . . ? C8 Th C2 57.1(2) . . ? C1 Th C2 29.7(2) . . ? C3 Th C16 170.00(19) . . ? C4 Th C16 158.58(19) . . ? C8 Th C16 106.70(16) . . ? C1 Th C16 123.12(19) . . ? C2 Th C16 146.2(2) . . ? C3 Th C15 160.4(2) . . ? C4 Th C15 132.2(2) . . ? C8 Th C15 97.6(2) . . ? C1 Th C15 124.9(2) . . ? C2 Th C15 154.4(2) . . ? C16 Th C15 29.56(15) . . ? C3 Th C7 82.61(17) . . ? C4 Th C7 74.0(2) . . ? C8 Th C7 29.3(2) . . ? C1 Th C7 55.6(2) . . ? C2 Th C7 74.95(19) . . ? C16 Th C7 105.18(17) . . ? C15 Th C7 83.79(17) . . ? C3 Th C11 101.1(2) . . ? C4 Th C11 94.0(2) . . ? C8 Th C11 177.13(17) . . ? C1 Th C11 149.7(2) . . ? C2 Th C11 121.9(2) . . ? C16 Th C11 75.58(16) . . ? C15 Th C11 83.56(17) . . ? C7 Th C11 148.8(2) . . ? C3 Th C10 117.53(18) . . ? C4 Th C10 120.8(2) . . ? C8 Th C10 153.19(18) . . ? C1 Th C10 138.56(16) . . ? C2 Th C10 124.84(16) . . ? C16 Th C10 55.43(16) . . ? C15 Th C10 75.51(16) . . ? C7 Th C10 159.30(16) . . ? C11 Th C10 29.66(15) . . ? C3 Th C12 99.7(2) . . ? C4 Th C12 79.99(18) . . ? C8 Th C12 148.4(2) . . ? C1 Th C12 154.61(18) . . ? C2 Th C12 128.1(2) . . ? C16 Th C12 82.12(14) . . ? C15 Th C12 74.98(16) . . ? C7 Th C12 119.5(2) . . ? C11 Th C12 29.41(16) . . ? C10 Th C12 55.67(15) . . ? C3 Th C9 141.99(17) . . ? C4 Th C9 149.5(2) . . ? C8 Th C9 127.04(16) . . ? C1 Th C9 128.61(14) . . ? C2 Th C9 134.38(15) . . ? C16 Th C9 28.99(15) . . ? C15 Th C9 55.65(16) . . ? C7 Th C9 133.56(17) . . ? C11 Th C9 55.74(16) . . ? C10 Th C9 28.99(15) . . ? C12 Th C9 74.40(15) . . ? C3 Th C14 133.9(2) . . ? C4 Th C14 104.6(2) . . ? C8 Th C14 105.3(2) . . ? C1 Th C14 135.2(2) . . ? C2 Th C14 151.72(15) . . ? C16 Th C14 54.88(14) . . ? C15 Th C14 28.89(13) . . ? C7 Th C14 80.74(18) . . ? C11 Th C14 74.50(16) . . ? C10 Th C14 81.36(14) . . ? C12 Th C14 54.51(16) . . ? C9 Th C14 73.53(14) . . ? C3 Th C5 54.3(2) . . ? C4 Th C5 28.16(19) . . ? C8 Th C5 74.0(2) . . ? C1 Th C5 80.24(16) . . ? C2 Th C5 72.67(17) . . ? C16 Th C5 135.41(17) . . ? C15 Th C5 106.06(18) . . ? C7 Th C5 53.8(2) . . ? C11 Th C5 103.2(2) . . ? C10 Th C5 132.8(2) . . ? C12 Th C5 78.72(19) . . ? C9 Th C5 150.66(15) . . ? C14 Th C5 81.42(16) . . ? C3 Th C6 73.21(18) . . ? C4 Th C6 53.5(2) . . ? C8 Th C6 54.8(2) . . ? C1 Th C6 73.14(19) . . ? C2 Th C6 80.00(16) . . ? C16 Th C6 116.60(18) . . ? C15 Th C6 88.15(17) . . ? C7 Th C6 28.5(2) . . ? C11 Th C6 122.7(2) . . ? C10 Th C6 148.07(18) . . ? C12 Th C6 93.9(2) . . ? C9 Th C6 143.58(16) . . ? C14 Th C6 71.75(16) . . ? C5 Th C6 27.6(2) . . ? C3 Th C13 112.8(2) . . ? C4 Th C13 85.33(18) . . ? C8 Th C13 123.6(2) . . ? C1 Th C13 147.53(16) . . ? C2 Th C13 140.3(2) . . ? C16 Th C13 73.34(14) . . ? C15 Th C13 54.41(15) . . ? C7 Th C13 94.7(2) . . ? C11 Th C13 55.11(16) . . ? C10 Th C13 73.78(14) . . ? C12 Th C13 28.77(15) . . ? C9 Th C13 80.21(13) . . ? C14 Th C13 28.02(14) . . ? C5 Th C13 70.54(15) . . ? C6 Th C13 74.40(17) . . ? C3 Th H1 89.0(2) . . ? C4 Th H1 117.8(2) . . ? C8 Th H1 91(2) . . ? C1 Th H1 70.5(18) . . ? C2 Th H1 70.1(9) . . ? C16 Th H1 81.7(3) . . ? C15 Th H1 110.07(11) . . ? C7 Th H1 120(2) . . ? C11 Th H1 91(2) . . ? C10 Th H1 68.4(19) . . ? C12 Th H1 121(2) . . ? C9 Th H1 64.7(11) . . ? C14 Th H1 136.3(5) . . ? C5 Th H1 142.3(6) . . ? C6 Th H1 143.5(19) . . ? C13 Th H1 142.0(18) . . ? Th H1 Th 171.1 . 2_655 ? O4 Na O4 168.7(2) 2_665 . ? O4 Na O1 83.65(14) 2_665 2_665 ? O4 Na O1 86.87(14) . 2_665 ? O4 Na O1 86.87(14) 2_665 . ? O4 Na O1 83.66(14) . . ? O1 Na O1 65.28(15) 2_665 . ? O4 Na O2 83.49(11) 2_665 2_665 ? O4 Na O2 97.66(12) . 2_665 ? O1 Na O2 63.28(11) 2_665 2_665 ? O1 Na O2 128.37(15) . 2_665 ? O4 Na O2 97.66(12) 2_665 . ? O4 Na O2 83.49(11) . . ? O1 Na O2 128.37(15) 2_665 . ? O1 Na O2 63.28(11) . . ? O2 Na O2 168.3(2) 2_665 . ? O4 Na O3 111.69(14) 2_665 2_665 ? O4 Na O3 78.34(13) . 2_665 ? O1 Na O3 119.60(10) 2_665 2_665 ? O1 Na O3 160.86(10) . 2_665 ? O2 Na O3 61.38(11) 2_665 2_665 ? O2 Na O3 107.79(14) . 2_665 ? O4 Na O3 78.35(13) 2_665 . ? O4 Na O3 111.68(14) . . ? O1 Na O3 160.86(10) 2_665 . ? O1 Na O3 119.60(10) . . ? O2 Na O3 107.78(14) 2_665 . ? O2 Na O3 61.38(11) . . ? O3 Na O3 62.65(16) 2_665 . ? C18 O1 C17 111.2(3) . . ? C18 O1 Na 110.0(3) . . ? C17 O1 Na 113.1(2) . . ? C20 O2 C19 112.3(4) . . ? C20 O2 Na 120.0(3) . . ? C19 O2 Na 116.8(3) . . ? C22 O3 C21 112.6(4) . . ? C22 O3 Na 111.9(3) . . ? C21 O3 Na 110.9(3) . . ? C26 O4 C23 105.2(5) . . ? C26 O4 Na 126.1(4) . . ? C23 O4 Na 122.2(4) . . ? C2 C1 C8 135.5(5) . . ? C2 C1 Th 75.3(3) . . ? C8 C1 Th 74.7(3) . . ? C2 C1 H1A 112.2 . . ? C8 C1 H1A 112.2 . . ? Th C1 H1A 133.2 . . ? C3 C2 C1 134.8(5) . . ? C3 C2 Th 73.8(3) . . ? C1 C2 Th 75.0(3) . . ? C3 C2 H2 112.6 . . ? C1 C2 H2 112.6 . . ? Th C2 H2 134.3 . . ? C2 C3 C4 134.5(6) . . ? C2 C3 Th 77.1(3) . . ? C4 C3 Th 76.5(3) . . ? C2 C3 H3 112.8 . . ? C4 C3 H3 112.8 . . ? Th C3 H3 126.1 . . ? C5 C4 C3 135.2(7) . . ? C5 C4 Th 79.1(3) . . ? C3 C4 Th 74.2(3) . . ? C5 C4 H4 112.4 . . ? C3 C4 H4 112.4 . . ? Th C4 H4 127.3 . . ? C6 C5 C4 136.0(6) . . ? C6 C5 Th 76.6(3) . . ? C4 C5 Th 72.7(3) . . ? C6 C5 H5 112.0 . . ? C4 C5 H5 112.0 . . ? Th C5 H5 134.9 . . ? C5 C6 C7 136.1(5) . . ? C5 C6 Th 75.8(3) . . ? C7 C6 Th 73.3(4) . . ? C5 C6 H6 111.9 . . ? C7 C6 H6 111.9 . . ? Th C6 H6 135.5 . . ? C6 C7 C8 135.5(6) . . ? C6 C7 Th 78.2(4) . . ? C8 C7 Th 74.3(4) . . ? C6 C7 H7 112.2 . . ? C8 C7 H7 112.2 . . ? Th C7 H7 128.8 . . ? C7 C8 C1 131.5(5) . . ? C7 C8 Th 76.4(4) . . ? C1 C8 Th 75.2(3) . . ? C7 C8 H8 114.2 . . ? C1 C8 H8 114.2 . . ? Th C8 H8 126.7 . . ? C16 C9 C10 135.5(5) . . ? C16 C9 Th 74.2(3) . . ? C10 C9 Th 75.1(3) . . ? C16 C9 H9 112.3 . . ? C10 C9 H9 112.3 . . ? Th C9 H9 134.3 . . ? C9 C10 C11 134.9(5) . . ? C9 C10 Th 75.9(3) . . ? C11 C10 Th 74.9(3) . . ? C9 C10 H10 112.6 . . ? C11 C10 H10 112.6 . . ? Th C10 H10 131.2 . . ? C12 C11 C10 133.2(5) . . ? C12 C11 Th 75.9(3) . . ? C10 C11 Th 75.5(3) . . ? C12 C11 H11 113.4 . . ? C10 C11 H11 113.4 . . ? Th C11 H11 128.5 . . ? C13 C12 C11 135.0(5) . . ? C13 C12 Th 77.7(3) . . ? C11 C12 Th 74.7(3) . . ? C13 C12 H12 112.5 . . ? C11 C12 H12 112.5 . . ? Th C12 H12 128.6 . . ? C14 C13 C12 135.5(5) . . ? C14 C13 Th 74.5(3) . . ? C12 C13 Th 73.6(3) . . ? C14 C13 H13 112.2 . . ? C12 C13 H13 112.2 . . ? Th C13 H13 136.6 . . ? C13 C14 C15 136.7(5) . . ? C13 C14 Th 77.5(3) . . ? C15 C14 Th 73.8(2) . . ? C13 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? Th C14 H14 132.3 . . ? C14 C15 C16 132.9(5) . . ? C14 C15 Th 77.3(2) . . ? C16 C15 Th 75.1(3) . . ? C14 C15 H15 113.6 . . ? C16 C15 H15 113.6 . . ? Th C15 H15 126.6 . . ? C9 C16 C15 135.8(5) . . ? C9 C16 Th 76.9(3) . . ? C15 C16 Th 75.3(3) . . ? C9 C16 H16 112.1 . . ? C15 C16 H16 112.1 . . ? Th C16 H16 129.7 . . ? O1 C17 C17 107.2(3) . 2_665 ? O1 C17 H17A 110.3 . . ? C17 C17 H17A 110.3 2_665 . ? O1 C17 H17B 110.3 . . ? C17 C17 H17B 110.3 2_665 . ? H17A C17 H17B 108.5 . . ? O1 C18 C19 107.0(4) . . ? O1 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? O1 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? O2 C19 C18 108.1(4) . . ? O2 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? O2 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? O2 C20 C21 108.4(4) . . ? O2 C20 H20A 110.0 . . ? C21 C20 H20A 110.0 . . ? O2 C20 H20B 110.0 . . ? C21 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? O3 C21 C20 108.5(4) . . ? O3 C21 H21A 110.0 . . ? C20 C21 H21A 110.0 . . ? O3 C21 H21B 110.0 . . ? C20 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? O3 C22 C22 113.1(4) . 2_665 ? O3 C22 H22A 109.0 . . ? C22 C22 H22A 109.0 2_665 . ? O3 C22 H22B 109.0 . . ? C22 C22 H22B 109.0 2_665 . ? H22A C22 H22B 107.8 . . ? O4 C23 C24 105.9(6) . . ? O4 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? O4 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? C23 C24 C25 104.5(6) . . ? C23 C24 H24A 110.9 . . ? C25 C24 H24A 110.9 . . ? C23 C24 H24B 110.9 . . ? C25 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C24 C25 C26 103.9(6) . . ? C24 C25 H25A 111.0 . . ? C26 C25 H25A 111.0 . . ? C24 C25 H25B 111.0 . . ? C26 C25 H25B 111.0 . . ? H25A C25 H25B 109.0 . . ? O4 C26 C25 108.5(5) . . ? O4 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O4 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? _database_code_depnum_ccdc_archive 'CCDC 918804' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6.K(18c6) #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1357747294.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H57 K O6 Th2' _chemical_formula_weight 1185.08 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' Th Th -7.2400 8.8979 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.0796(18) _cell_length_b 9.8234(3) _cell_length_c 25.6897(13) _cell_angle_alpha 90.00 _cell_angle_beta 118.992(2) _cell_angle_gamma 90.00 _cell_volume 8184.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 148463 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 30.51 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 7.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.311 _exptl_absorpt_correction_T_max 0.553 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps (554 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 148463 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 30.51 _reflns_number_total 12469 _reflns_number_gt 7918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydride proton H1 was found on a Fourier-difference map, but it could not be refined, and all the other H atoms were introduced at calculated positions; all H atoms were treated as riding atoms (H1 is riding on Th2) with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0107P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12469 _refine_ls_number_parameters 478 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0527 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.927 _refine_diff_density_min -1.410 _refine_diff_density_rms 0.213 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 0.092278(5) 0.664502(15) 0.241255(6) 0.02362(4) Uani 1 1 d . . . Th2 Th 0.171192(5) 0.970142(15) 0.387480(6) 0.02210(4) Uani 1 1 d . . . H1 H 0.1345 0.8169 0.3098 0.027 Uiso 1 1 d R . . K K 0.12115(3) 0.89487(9) 0.04247(4) 0.0286(2) Uani 1 1 d . . . O1 O 0.05253(8) 1.0647(3) 0.00128(11) 0.0280(7) Uani 1 1 d . . . O2 O 0.04808(8) 0.8034(3) -0.04717(11) 0.0281(7) Uani 1 1 d . . . O3 O 0.10749(9) 0.6030(3) 0.02251(11) 0.0316(7) Uani 1 1 d . . . O4 O 0.18207(8) 0.7019(3) 0.11239(11) 0.0301(7) Uani 1 1 d . . . O5 O 0.18805(8) 0.9641(3) 0.15718(10) 0.0288(7) Uani 1 1 d . . . O6 O 0.13058(8) 1.1650(3) 0.08579(11) 0.0300(7) Uani 1 1 d . . . C1 C 0.06653(15) 0.9351(4) 0.20883(17) 0.0362(12) Uani 1 1 d . . . H1A H 0.0719 1.0184 0.2284 0.043 Uiso 1 1 calc R . . C2 C 0.09350(14) 0.9090(5) 0.18647(18) 0.0414(12) Uani 1 1 d . . . H2 H 0.1135 0.9763 0.1966 0.050 Uiso 1 1 calc R . . C3 C 0.09742(14) 0.8038(6) 0.15193(19) 0.0469(14) Uani 1 1 d . . . H3 H 0.1207 0.8134 0.1473 0.056 Uiso 1 1 calc R . . C4 C 0.07391(16) 0.6877(5) 0.12294(17) 0.0457(14) Uani 1 1 d . . . H4 H 0.0847 0.6385 0.1027 0.055 Uiso 1 1 calc R . . C5 C 0.03845(15) 0.6317(5) 0.11823(17) 0.0398(12) Uani 1 1 d . . . H5 H 0.0291 0.5596 0.0914 0.048 Uiso 1 1 calc R . . C6 C 0.01277(13) 0.6541(4) 0.14287(17) 0.0372(12) Uani 1 1 d . . . H6 H -0.0085 0.5909 0.1301 0.045 Uiso 1 1 calc R . . C7 C 0.01157(13) 0.7500(5) 0.18243(17) 0.0365(11) Uani 1 1 d . . . H7 H -0.0084 0.7305 0.1933 0.044 Uiso 1 1 calc R . . C8 C 0.03370(14) 0.8677(5) 0.20908(17) 0.0351(11) Uani 1 1 d . . . H8 H 0.0244 0.9113 0.2324 0.042 Uiso 1 1 calc R . . C9 C 0.14032(18) 0.5516(4) 0.35375(18) 0.0453(14) Uani 1 1 d . . . H9 H 0.1563 0.5869 0.3918 0.054 Uiso 1 1 calc R . . C10 C 0.16392(14) 0.5323(4) 0.3244(2) 0.0446(13) Uani 1 1 d . . . H10 H 0.1912 0.5601 0.3473 0.054 Uiso 1 1 calc R . . C11 C 0.15569(15) 0.4814(4) 0.2690(2) 0.0428(12) Uani 1 1 d . . . H11 H 0.1776 0.4913 0.2612 0.051 Uiso 1 1 calc R . . C12 C 0.12129(16) 0.4185(4) 0.2231(2) 0.0428(12) Uani 1 1 d . . . H12 H 0.1251 0.3972 0.1908 0.051 Uiso 1 1 calc R . . C13 C 0.08242(16) 0.3801(4) 0.2141(2) 0.0432(13) Uani 1 1 d . . . H13 H 0.0688 0.3244 0.1809 0.052 Uiso 1 1 calc R . . C14 C 0.05882(15) 0.4033(4) 0.2419(2) 0.0420(12) Uani 1 1 d . . . H14 H 0.0326 0.3654 0.2214 0.050 Uiso 1 1 calc R . . C15 C 0.06590(16) 0.4714(4) 0.2939(2) 0.0443(13) Uani 1 1 d . . . H15 H 0.0423 0.4775 0.2978 0.053 Uiso 1 1 calc R . . C16 C 0.09985(18) 0.5317(4) 0.3409(2) 0.0416(13) Uani 1 1 d . . . H16 H 0.0943 0.5662 0.3699 0.050 Uiso 1 1 calc R . . C17 C 0.09853(14) 0.8895(5) 0.3856(2) 0.0423(12) Uani 1 1 d . . . H17 H 0.0780 0.8266 0.3635 0.051 Uiso 1 1 calc R . . C18 C 0.09006(13) 1.0171(5) 0.35918(18) 0.0394(12) Uani 1 1 d U . . H18 H 0.0658 1.0181 0.3229 0.047 Uiso 1 1 calc R . . C19 C 0.10937(15) 1.1454(5) 0.37416(19) 0.0413(13) Uani 1 1 d . . . H19 H 0.0962 1.2103 0.3445 0.050 Uiso 1 1 calc R . . C20 C 0.14419(15) 1.1957(4) 0.4243(2) 0.0381(12) Uani 1 1 d . . . H20 H 0.1488 1.2876 0.4210 0.046 Uiso 1 1 calc R . . C21 C 0.17362(14) 1.1397(5) 0.47828(19) 0.0376(12) Uani 1 1 d . . . H21 H 0.1914 1.2052 0.5042 0.045 Uiso 1 1 calc R . . C22 C 0.18276(14) 1.0099(5) 0.50254(16) 0.0389(12) Uani 1 1 d . . . H22 H 0.2062 1.0090 0.5398 0.047 Uiso 1 1 calc R . . C23 C 0.16563(16) 0.8807(5) 0.48511(19) 0.0427(13) Uani 1 1 d . . . H23 H 0.1814 0.8125 0.5114 0.051 Uiso 1 1 calc R . . C24 C 0.13013(16) 0.8328(5) 0.4370(2) 0.0413(12) Uani 1 1 d . . . H24 H 0.1265 0.7398 0.4396 0.050 Uiso 1 1 calc R . . C25 C 0.21681(13) 0.8466(5) 0.33907(18) 0.0346(11) Uani 1 1 d . . . H25 H 0.2142 0.7682 0.3173 0.042 Uiso 1 1 calc R . . C26 C 0.19765(13) 0.9582(5) 0.30218(17) 0.0330(11) Uani 1 1 d . . . H26 H 0.1852 0.9351 0.2621 0.040 Uiso 1 1 calc R . . C27 C 0.19262(13) 1.0958(5) 0.31060(18) 0.0342(11) Uani 1 1 d . . . H27 H 0.1752 1.1408 0.2754 0.041 Uiso 1 1 calc R . . C28 C 0.20809(13) 1.1809(4) 0.36067(19) 0.0344(11) Uani 1 1 d . . . H28 H 0.1983 1.2697 0.3518 0.041 Uiso 1 1 calc R . . C29 C 0.23526(13) 1.1600(4) 0.42130(18) 0.0337(11) Uani 1 1 d . . . H29 H 0.2427 1.2417 0.4422 0.040 Uiso 1 1 calc R . . C30 C 0.25420(12) 1.0487(4) 0.45869(17) 0.0323(11) Uani 1 1 d . . . H30 H 0.2704 1.0743 0.4982 0.039 Uiso 1 1 calc R . . C31 C 0.25451(12) 0.9081(4) 0.45066(17) 0.0307(10) Uani 1 1 d . . . H31 H 0.2680 0.8606 0.4864 0.037 Uiso 1 1 calc R . . C32 C 0.23898(12) 0.8223(4) 0.40068(17) 0.0287(10) Uani 1 1 d . . . H32 H 0.2445 0.7307 0.4103 0.034 Uiso 1 1 calc R . . C33 C 0.02265(12) 1.0293(4) -0.05895(16) 0.0310(10) Uani 1 1 d . . . H33A H 0.0339 1.0472 -0.0854 0.037 Uiso 1 1 calc R . . H33B H -0.0020 1.0840 -0.0719 0.037 Uiso 1 1 calc R . . C34 C 0.01220(13) 0.8827(4) -0.06130(17) 0.0330(11) Uani 1 1 d . . . H34A H 0.0026 0.8637 -0.0330 0.040 Uiso 1 1 calc R . . H34B H -0.0096 0.8595 -0.1008 0.040 Uiso 1 1 calc R . . C35 C 0.03955(13) 0.6622(4) -0.05183(18) 0.0358(11) Uani 1 1 d . . . H35A H 0.0179 0.6407 -0.0917 0.043 Uiso 1 1 calc R . . H35B H 0.0302 0.6363 -0.0239 0.043 Uiso 1 1 calc R . . C36 C 0.07785(13) 0.5846(4) -0.03861(17) 0.0356(11) Uani 1 1 d . . . H36A H 0.0715 0.4887 -0.0469 0.043 Uiso 1 1 calc R . . H36B H 0.0889 0.6174 -0.0636 0.043 Uiso 1 1 calc R . . C37 C 0.14533(13) 0.5350(4) 0.03817(17) 0.0313(10) Uani 1 1 d . . . H37A H 0.1573 0.5697 0.0146 0.038 Uiso 1 1 calc R . . H37B H 0.1406 0.4381 0.0307 0.038 Uiso 1 1 calc R . . C38 C 0.17385(13) 0.5601(4) 0.10273(17) 0.0333(11) Uani 1 1 d . . . H38A H 0.1614 0.5279 0.1260 0.040 Uiso 1 1 calc R . . H38B H 0.1994 0.5109 0.1153 0.040 Uiso 1 1 calc R . . C39 C 0.21064(13) 0.7328(4) 0.17288(16) 0.0338(11) Uani 1 1 d . . . H39A H 0.2345 0.6738 0.1870 0.041 Uiso 1 1 calc R . . H39B H 0.1979 0.7181 0.1976 0.041 Uiso 1 1 calc R . . C40 C 0.22367(13) 0.8790(4) 0.17682(17) 0.0355(11) Uani 1 1 d . . . H40A H 0.2437 0.9013 0.2176 0.043 Uiso 1 1 calc R . . H40B H 0.2364 0.8937 0.1520 0.043 Uiso 1 1 calc R . . C41 C 0.19875(13) 1.1042(4) 0.16065(17) 0.0338(11) Uani 1 1 d . . . H41A H 0.2084 1.1245 0.1325 0.041 Uiso 1 1 calc R . . H41B H 0.2206 1.1259 0.2003 0.041 Uiso 1 1 calc R . . C42 C 0.16106(13) 1.1867(4) 0.14631(16) 0.0340(11) Uani 1 1 d . . . H42A H 0.1502 1.1603 0.1724 0.041 Uiso 1 1 calc R . . H42B H 0.1682 1.2825 0.1527 0.041 Uiso 1 1 calc R . . C43 C 0.09297(13) 1.2326(4) 0.07094(17) 0.0331(11) Uani 1 1 d . . . H43A H 0.0977 1.3297 0.0773 0.040 Uiso 1 1 calc R . . H43B H 0.0820 1.1998 0.0961 0.040 Uiso 1 1 calc R . . C44 C 0.06281(13) 1.2051(4) 0.00687(17) 0.0324(10) Uani 1 1 d . . . H44A H 0.0382 1.2600 -0.0056 0.039 Uiso 1 1 calc R . . H44B H 0.0750 1.2277 -0.0180 0.039 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 0.02347(9) 0.02365(8) 0.02251(8) 0.00036(6) 0.01017(7) 0.00133(7) Th2 0.02111(9) 0.02366(8) 0.02238(8) -0.00077(6) 0.01121(6) 0.00007(7) K 0.0242(5) 0.0293(5) 0.0296(5) -0.0028(4) 0.0108(4) -0.0014(4) O1 0.0288(17) 0.0223(15) 0.0308(15) 0.0028(12) 0.0129(14) 0.0014(13) O2 0.0253(17) 0.0224(16) 0.0351(15) -0.0036(13) 0.0136(14) -0.0036(13) O3 0.0287(18) 0.0352(17) 0.0314(16) -0.0064(13) 0.0150(14) 0.0010(15) O4 0.0268(17) 0.0306(17) 0.0267(15) -0.0003(12) 0.0080(13) 0.0001(14) O5 0.0249(17) 0.0307(17) 0.0278(15) -0.0022(13) 0.0104(13) -0.0018(14) O6 0.0310(18) 0.0303(16) 0.0290(15) -0.0049(12) 0.0149(14) 0.0008(14) C1 0.044(3) 0.019(2) 0.028(2) 0.0006(18) 0.003(2) 0.004(2) C2 0.029(3) 0.044(3) 0.039(3) 0.019(2) 0.006(2) -0.009(2) C3 0.027(3) 0.081(4) 0.042(3) 0.036(3) 0.024(2) 0.014(3) C4 0.056(4) 0.061(4) 0.023(2) 0.007(2) 0.022(2) 0.022(3) C5 0.050(3) 0.038(3) 0.018(2) -0.0040(19) 0.006(2) 0.005(3) C6 0.022(3) 0.038(3) 0.030(2) 0.005(2) -0.005(2) -0.012(2) C7 0.020(3) 0.051(3) 0.033(2) 0.015(2) 0.009(2) 0.004(2) C8 0.035(3) 0.041(3) 0.030(2) 0.004(2) 0.016(2) 0.022(2) C9 0.070(4) 0.024(3) 0.024(2) 0.0093(19) 0.009(3) 0.015(3) C10 0.026(3) 0.033(3) 0.045(3) 0.007(2) -0.006(2) 0.003(2) C11 0.035(3) 0.037(3) 0.061(3) 0.014(3) 0.027(3) 0.017(2) C12 0.057(4) 0.027(3) 0.053(3) -0.003(2) 0.033(3) 0.015(3) C13 0.052(4) 0.014(2) 0.049(3) -0.006(2) 0.014(3) 0.004(2) C14 0.035(3) 0.025(3) 0.059(3) 0.010(2) 0.018(3) -0.005(2) C15 0.059(4) 0.024(3) 0.065(3) 0.018(2) 0.042(3) 0.010(3) C16 0.073(4) 0.029(3) 0.039(3) 0.009(2) 0.040(3) 0.009(3) C17 0.033(3) 0.054(3) 0.055(3) -0.029(3) 0.033(3) -0.020(3) C18 0.012(2) 0.066(3) 0.035(2) -0.010(2) 0.0074(19) 0.010(2) C19 0.050(3) 0.046(3) 0.041(3) 0.014(2) 0.033(3) 0.032(3) C20 0.054(3) 0.018(2) 0.062(3) -0.004(2) 0.044(3) 0.004(2) C21 0.039(3) 0.037(3) 0.044(3) -0.023(2) 0.026(2) -0.012(2) C22 0.028(3) 0.075(4) 0.012(2) -0.008(2) 0.0091(19) 0.005(3) C23 0.058(4) 0.056(3) 0.030(3) 0.019(2) 0.034(3) 0.026(3) C24 0.059(4) 0.032(3) 0.058(3) -0.006(2) 0.048(3) -0.011(3) C25 0.026(3) 0.043(3) 0.044(3) -0.016(2) 0.024(2) -0.002(2) C26 0.028(3) 0.054(3) 0.020(2) -0.007(2) 0.0147(19) -0.007(2) C27 0.032(3) 0.046(3) 0.033(2) 0.014(2) 0.023(2) 0.004(2) C28 0.035(3) 0.024(2) 0.054(3) 0.010(2) 0.030(2) -0.001(2) C29 0.026(3) 0.034(3) 0.046(3) -0.012(2) 0.021(2) -0.016(2) C30 0.017(2) 0.047(3) 0.029(2) -0.007(2) 0.0084(19) -0.012(2) C31 0.017(2) 0.043(3) 0.028(2) 0.003(2) 0.0077(19) 0.003(2) C32 0.022(2) 0.023(2) 0.042(3) 0.004(2) 0.017(2) 0.0093(19) C33 0.023(2) 0.032(3) 0.033(2) 0.001(2) 0.010(2) 0.004(2) C34 0.025(3) 0.039(3) 0.031(2) -0.003(2) 0.010(2) -0.001(2) C35 0.030(3) 0.041(3) 0.031(2) -0.006(2) 0.011(2) -0.004(2) C36 0.043(3) 0.028(3) 0.035(3) -0.011(2) 0.018(2) -0.009(2) C37 0.038(3) 0.020(2) 0.042(3) -0.0009(19) 0.025(2) 0.001(2) C38 0.038(3) 0.020(2) 0.043(3) 0.0087(19) 0.021(2) 0.006(2) C39 0.030(3) 0.037(3) 0.028(2) 0.006(2) 0.009(2) 0.007(2) C40 0.025(3) 0.044(3) 0.032(2) -0.003(2) 0.010(2) 0.001(2) C41 0.030(3) 0.039(3) 0.027(2) -0.002(2) 0.009(2) -0.005(2) C42 0.048(3) 0.025(2) 0.028(2) -0.0028(18) 0.018(2) -0.009(2) C43 0.040(3) 0.026(2) 0.042(3) -0.001(2) 0.027(2) 0.003(2) C44 0.028(3) 0.031(3) 0.038(2) 0.008(2) 0.016(2) 0.005(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 Th1 H1 2.2633 . ? Th1 C7 2.750(4) . ? Th1 C3 2.757(4) . ? Th1 C16 2.763(4) . ? Th1 C11 2.765(4) . ? Th1 C8 2.765(4) . ? Th1 C15 2.769(4) . ? Th1 C12 2.775(4) . ? Th1 C4 2.783(4) . ? Th1 C9 2.787(4) . ? Th1 C10 2.793(4) . ? Th1 C2 2.795(4) . ? Th1 C6 2.805(4) . ? Th1 C1 2.811(4) . ? Th1 C5 2.822(4) . ? Th1 C14 2.853(4) . ? Th1 C13 2.860(4) . ? Th2 H1 2.3381 . ? Th2 C28 2.747(4) . ? Th2 C19 2.752(4) . ? Th2 C27 2.752(4) . ? Th2 C23 2.758(4) . ? Th2 C24 2.763(4) . ? Th2 C18 2.770(4) . ? Th2 C31 2.773(4) . ? Th2 C32 2.778(4) . ? Th2 C20 2.780(4) . ? Th2 C17 2.786(4) . ? Th2 C22 2.801(4) . ? Th2 C26 2.804(4) . ? Th2 C29 2.807(4) . ? Th2 C25 2.814(4) . ? Th2 C30 2.821(4) . ? Th2 C21 2.832(4) . ? K O2 2.721(3) . ? K O1 2.787(3) . ? K O4 2.827(3) . ? K O6 2.833(3) . ? K O5 2.866(3) . ? K O3 2.913(3) . ? K C22 3.068(4) 6_575 ? K C21 3.119(4) 6_575 ? K C3 3.447(4) . ? K C23 3.479(4) 6_575 ? O1 C44 1.419(4) . ? O1 C33 1.442(4) . ? O2 C35 1.415(5) . ? O2 C34 1.429(5) . ? O3 C37 1.425(5) . ? O3 C36 1.426(4) . ? O4 C38 1.421(4) . ? O4 C39 1.426(4) . ? O5 C41 1.423(5) . ? O5 C40 1.432(5) . ? O6 C43 1.419(4) . ? O6 C42 1.427(4) . ? C1 C8 1.388(6) . ? C1 C2 1.397(6) . ? C1 H1A 0.9300 . ? C2 C3 1.415(6) . ? C2 H2 0.9300 . ? C3 C4 1.409(6) . ? C3 H3 0.9300 . ? C4 C5 1.376(6) . ? C4 H4 0.9300 . ? C5 C6 1.393(6) . ? C5 H5 0.9300 . ? C6 C7 1.402(6) . ? C6 H6 0.9300 . ? C7 C8 1.391(6) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C16 1.385(7) . ? C9 C10 1.418(7) . ? C9 H9 0.9300 . ? C10 C11 1.395(6) . ? C10 H10 0.9300 . ? C11 C12 1.394(6) . ? C11 H11 0.9300 . ? C12 C13 1.397(6) . ? C12 H12 0.9300 . ? C13 C14 1.389(6) . ? C13 H13 0.9300 . ? C14 C15 1.401(6) . ? C14 H14 0.9300 . ? C15 C16 1.385(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C24 1.388(6) . ? C17 C18 1.387(6) . ? C17 H17 0.9300 . ? C18 C19 1.408(6) . ? C18 H18 0.9300 . ? C19 C20 1.400(6) . ? C19 H19 0.9300 . ? C20 C21 1.395(6) . ? C20 H20 0.9300 . ? C21 C22 1.387(6) . ? C21 H21 0.9300 . ? C22 C23 1.392(6) . ? C22 H22 0.9300 . ? C23 C24 1.380(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.398(6) . ? C25 C32 1.406(5) . ? C25 H25 0.9300 . ? C26 C27 1.395(6) . ? C26 H26 0.9300 . ? C27 C28 1.403(6) . ? C27 H27 0.9300 . ? C28 C29 1.401(5) . ? C28 H28 0.9300 . ? C29 C30 1.399(6) . ? C29 H29 0.9300 . ? C30 C31 1.397(6) . ? C30 H30 0.9300 . ? C31 C32 1.405(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.484(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.498(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.493(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.503(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.499(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.499(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Th1 C3 83.51(13) . . ? C7 Th1 C16 104.37(15) . . ? C3 Th1 C16 171.30(16) . . ? C7 Th1 C11 154.59(15) . . ? C3 Th1 C11 98.31(14) . . ? C16 Th1 C11 76.22(14) . . ? C7 Th1 C8 29.22(12) . . ? C3 Th1 C8 75.76(14) . . ? C16 Th1 C8 109.29(14) . . ? C11 Th1 C8 173.33(14) . . ? C7 Th1 C15 85.96(14) . . ? C3 Th1 C15 158.44(16) . . ? C16 Th1 C15 29.00(13) . . ? C11 Th1 C15 83.44(14) . . ? C8 Th1 C15 103.20(14) . . ? C7 Th1 C12 125.50(15) . . ? C3 Th1 C12 95.93(15) . . ? C16 Th1 C12 82.59(13) . . ? C11 Th1 C12 29.14(13) . . ? C8 Th1 C12 152.97(14) . . ? C15 Th1 C12 75.12(14) . . ? C7 Th1 C4 75.51(14) . . ? C3 Th1 C4 29.47(14) . . ? C16 Th1 C4 155.69(15) . . ? C11 Th1 C4 93.58(14) . . ? C8 Th1 C4 82.73(12) . . ? C15 Th1 C4 129.21(16) . . ? C12 Th1 C4 78.30(14) . . ? C7 Th1 C9 132.06(15) . . ? C3 Th1 C9 142.52(16) . . ? C16 Th1 C9 28.90(14) . . ? C11 Th1 C9 55.75(14) . . ? C8 Th1 C9 127.74(13) . . ? C15 Th1 C9 54.57(15) . . ? C12 Th1 C9 73.91(13) . . ? C4 Th1 C9 149.34(15) . . ? C7 Th1 C10 160.13(14) . . ? C3 Th1 C10 116.31(14) . . ? C16 Th1 C10 55.97(15) . . ? C11 Th1 C10 29.05(13) . . ? C8 Th1 C10 151.91(13) . . ? C15 Th1 C10 74.83(15) . . ? C12 Th1 C10 54.65(14) . . ? C4 Th1 C10 120.77(15) . . ? C9 Th1 C10 29.44(14) . . ? C7 Th1 C2 74.92(13) . . ? C3 Th1 C2 29.52(13) . . ? C16 Th1 C2 148.54(14) . . ? C11 Th1 C2 118.01(14) . . ? C8 Th1 C2 55.33(14) . . ? C15 Th1 C2 158.49(15) . . ? C12 Th1 C2 124.14(15) . . ? C4 Th1 C2 55.59(14) . . ? C9 Th1 C2 134.91(14) . . ? C10 Th1 C2 122.87(14) . . ? C28 Th2 C19 89.04(14) . . ? C28 Th2 C27 29.56(12) . . ? C19 Th2 C27 98.22(13) . . ? C28 Th2 C23 137.21(15) . . ? C19 Th2 C23 83.53(13) . . ? C27 Th2 C23 165.97(15) . . ? C28 Th2 C24 159.40(13) . . ? C19 Th2 C24 75.60(14) . . ? C27 Th2 C24 164.66(14) . . ? C23 Th2 C24 28.96(13) . . ? C28 Th2 C18 114.72(14) . . ? C19 Th2 C18 29.54(13) . . ? C27 Th2 C18 113.05(13) . . ? C23 Th2 C18 75.01(14) . . ? C24 Th2 C18 55.35(14) . . ? C28 Th2 C31 76.33(13) . . ? C19 Th2 C31 146.59(14) . . ? C27 Th2 C31 83.77(12) . . ? C23 Th2 C31 87.18(13) . . ? C24 Th2 C31 109.22(14) . . ? C18 Th2 C31 161.89(12) . . ? C28 Th2 C32 83.89(12) . . ? C19 Th2 C32 172.77(14) . . ? C27 Th2 C32 76.30(12) . . ? C23 Th2 C32 100.64(12) . . ? C24 Th2 C32 110.88(13) . . ? C18 Th2 C32 157.31(13) . . ? C31 Th2 C32 29.32(11) . . ? C28 Th2 C20 77.87(13) . . ? C19 Th2 C20 29.31(13) . . ? C27 Th2 C20 99.43(13) . . ? C23 Th2 C20 75.29(13) . . ? C24 Th2 C20 82.11(13) . . ? C18 Th2 C20 55.39(13) . . ? C31 Th2 C20 117.31(13) . . ? C32 Th2 C20 146.00(13) . . ? C28 Th2 C17 143.59(14) . . ? C19 Th2 C17 55.63(15) . . ? C27 Th2 C17 136.73(14) . . ? C23 Th2 C17 55.05(15) . . ? C24 Th2 C17 28.97(13) . . ? C18 Th2 C17 28.91(13) . . ? C31 Th2 C17 137.84(14) . . ? C32 Th2 C17 131.59(14) . . ? C20 Th2 C17 74.19(13) . . ? C28 Th2 C22 108.62(14) . . ? C19 Th2 C22 74.71(13) . . ? C27 Th2 C22 138.15(14) . . ? C23 Th2 C22 29.00(13) . . ? C24 Th2 C22 54.48(14) . . ? C18 Th2 C22 81.09(12) . . ? C31 Th2 C22 81.70(12) . . ? C32 Th2 C22 106.11(12) . . ? C20 Th2 C22 54.94(13) . . ? C17 Th2 C22 73.14(13) . . ? O2 K O1 61.64(8) . . ? O2 K O4 118.52(8) . . ? O1 K O4 160.75(8) . . ? O2 K O6 121.63(8) . . ? O1 K O6 60.30(8) . . ? O4 K O6 118.05(8) . . ? O2 K O5 163.57(8) . . ? O1 K O5 115.11(8) . . ? O4 K O5 58.60(8) . . ? O6 K O5 59.55(8) . . ? O2 K O3 60.60(8) . . ? O1 K O3 118.25(8) . . ? O4 K O3 57.93(8) . . ? O6 K O3 165.65(8) . . ? O5 K O3 113.86(8) . . ? C44 O1 C33 111.8(3) . . ? C44 O1 K 113.1(2) . . ? C33 O1 K 110.4(2) . . ? C35 O2 C34 111.8(3) . . ? C35 O2 K 119.0(2) . . ? C34 O2 K 117.2(2) . . ? C37 O3 C36 112.3(3) . . ? C37 O3 K 110.4(2) . . ? C36 O3 K 107.1(2) . . ? C38 O4 C39 112.5(3) . . ? C38 O4 K 120.6(2) . . ? C39 O4 K 119.5(2) . . ? C41 O5 C40 111.2(3) . . ? C41 O5 K 111.7(2) . . ? C40 O5 K 114.5(2) . . ? C43 O6 C42 112.3(3) . . ? C43 O6 K 114.5(2) . . ? C42 O6 K 116.7(2) . . ? C8 C1 C2 135.9(4) . . ? C8 C1 H1A 112.0 . . ? C2 C1 H1A 112.0 . . ? C1 C2 C3 134.7(4) . . ? C1 C2 H2 112.6 . . ? C3 C2 H2 112.6 . . ? C4 C3 C2 134.2(4) . . ? C4 C3 H3 112.9 . . ? C2 C3 H3 112.9 . . ? C5 C4 C3 133.7(5) . . ? C5 C4 H4 113.2 . . ? C3 C4 H4 113.2 . . ? C4 C5 C6 137.0(4) . . ? C4 C5 H5 111.5 . . ? C6 C5 H5 111.5 . . ? C5 C6 C7 134.8(4) . . ? C5 C6 H6 112.6 . . ? C7 C6 H6 112.6 . . ? C8 C7 C6 134.2(4) . . ? C8 C7 H7 112.9 . . ? C6 C7 H7 112.9 . . ? C1 C8 C7 134.7(4) . . ? C1 C8 H8 112.6 . . ? C7 C8 H8 112.6 . . ? C16 C9 C10 136.9(4) . . ? C16 C9 H9 111.5 . . ? C10 C9 H9 111.5 . . ? C11 C10 C9 134.7(5) . . ? C11 C10 H10 112.6 . . ? C9 C10 H10 112.6 . . ? C12 C11 C10 132.9(5) . . ? C12 C11 H11 113.5 . . ? C10 C11 H11 113.5 . . ? C11 C12 C13 135.0(4) . . ? C11 C12 H12 112.5 . . ? C13 C12 H12 112.5 . . ? C14 C13 C12 136.7(4) . . ? C14 C13 H13 111.7 . . ? C12 C13 H13 111.7 . . ? C13 C14 C15 134.0(5) . . ? C13 C14 H14 113.0 . . ? C15 C14 H14 113.0 . . ? C16 C15 C14 134.9(5) . . ? C16 C15 H15 112.5 . . ? C14 C15 H15 112.5 . . ? C9 C16 C15 133.7(4) . . ? C9 C16 H16 113.2 . . ? C15 C16 H16 113.2 . . ? C24 C17 C18 135.7(4) . . ? C24 C17 H17 112.2 . . ? C18 C17 H17 112.2 . . ? C17 C18 C19 135.3(4) . . ? C17 C18 H18 112.4 . . ? C19 C18 H18 112.4 . . ? C20 C19 C18 133.4(4) . . ? C20 C19 H19 113.3 . . ? C18 C19 H19 113.3 . . ? C21 C20 C19 134.7(4) . . ? C21 C20 H20 112.6 . . ? C19 C20 H20 112.6 . . ? C22 C21 C20 135.4(4) . . ? C22 C21 H21 112.3 . . ? C20 C21 H21 112.3 . . ? C21 C22 C23 136.0(4) . . ? C21 C22 H22 112.0 . . ? C23 C22 H22 112.0 . . ? C24 C23 C22 133.4(4) . . ? C24 C23 H23 113.3 . . ? C22 C23 H23 113.3 . . ? C23 C24 C17 135.5(4) . . ? C23 C24 H24 112.2 . . ? C17 C24 H24 112.2 . . ? C26 C25 C32 136.4(4) . . ? C26 C25 H25 111.8 . . ? C32 C25 H25 111.8 . . ? C27 C26 C25 135.8(4) . . ? C27 C26 H26 112.1 . . ? C25 C26 H26 112.1 . . ? C26 C27 C28 133.9(4) . . ? C26 C27 H27 113.0 . . ? C28 C27 H27 113.0 . . ? C29 C28 C27 133.3(4) . . ? C29 C28 H28 113.3 . . ? C27 C28 H28 113.3 . . ? C30 C29 C28 136.8(4) . . ? C30 C29 H29 111.6 . . ? C28 C29 H29 111.6 . . ? C31 C30 C29 135.1(4) . . ? C31 C30 H30 112.4 . . ? C29 C30 H30 112.4 . . ? C30 C31 C32 134.3(4) . . ? C30 C31 H31 112.8 . . ? C32 C31 H31 112.8 . . ? C31 C32 C25 133.2(4) . . ? C31 C32 H32 113.4 . . ? C25 C32 H32 113.4 . . ? O1 C33 C34 109.1(3) . . ? O1 C33 H33A 109.9 . . ? C34 C33 H33A 109.9 . . ? O1 C33 H33B 109.9 . . ? C34 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O2 C34 C33 109.0(3) . . ? O2 C34 H34A 109.9 . . ? C33 C34 H34A 109.9 . . ? O2 C34 H34B 109.9 . . ? C33 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? O2 C35 C36 109.3(4) . . ? O2 C35 H35A 109.8 . . ? C36 C35 H35A 109.8 . . ? O2 C35 H35B 109.8 . . ? C36 C35 H35B 109.8 . . ? H35A C35 H35B 108.3 . . ? O3 C36 C35 109.0(3) . . ? O3 C36 H36A 109.9 . . ? C35 C36 H36A 109.9 . . ? O3 C36 H36B 109.9 . . ? C35 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? O3 C37 C38 107.8(3) . . ? O3 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O3 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.5 . . ? O4 C38 C37 109.4(3) . . ? O4 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? O4 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? O4 C39 C40 108.8(3) . . ? O4 C39 H39A 109.9 . . ? C40 C39 H39A 109.9 . . ? O4 C39 H39B 109.9 . . ? C40 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? O5 C40 C39 108.8(3) . . ? O5 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? O5 C40 H40B 109.9 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O5 C41 C42 108.0(3) . . ? O5 C41 H41A 110.1 . . ? C42 C41 H41A 110.1 . . ? O5 C41 H41B 110.1 . . ? C42 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? O6 C42 C41 109.8(3) . . ? O6 C42 H42A 109.7 . . ? C41 C42 H42A 109.7 . . ? O6 C42 H42B 109.7 . . ? C41 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? O6 C43 C44 108.9(3) . . ? O6 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? O6 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? O1 C44 C43 107.9(3) . . ? O1 C44 H44A 110.1 . . ? C43 C44 H44A 110.1 . . ? O1 C44 H44B 110.1 . . ? C43 C44 H44B 110.1 . . ? H44A C44 H44B 108.4 . . ? _database_code_depnum_ccdc_archive 'CCDC 918805'