# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jaqueline Kiplinger' _publ_contact_author_email KIPLINGER@LANL.GOV _publ_section_title ; Convenient access to the anhydrous thorium tetrachloride complexes ThCl4(DME)2, ThCl4(1,4-dioxane)2 and ThCl4(THF)3.5 using commercially available and inexpensive starting materials ; loop_ _publ_author_name 'Jaqueline Kiplinger' 'Thibault Cantat' 'Brian L. Scott' # Attachment 'Kiplinger_B923558B_CIF_Re-revised_12-14-09.cif' data_apx876s _database_code_depnum_ccdc_archive 'CCDC 753730' #TrackingRef 'Kiplinger_B923558B_CIF_Re-revised_12-14-09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H48 Cl4 O9 Th' _chemical_formula_weight 806.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.744(5) _cell_length_b 10.896(5) _cell_length_c 13.900(6) _cell_angle_alpha 99.515(5) _cell_angle_beta 107.115(5) _cell_angle_gamma 92.690(5) _cell_volume 1525.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 1639 _cell_measurement_theta_min 5.2 _cell_measurement_theta_max 36.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 5.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4501 _exptl_absorpt_correction_T_max 0.7425 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _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 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14789 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.1126 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.42 _reflns_number_total 5562 _reflns_number_gt 3912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atom postions for water ligands were not included in the refinement. ; _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^)+(0.1305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5562 _refine_ls_number_parameters 233 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.661 _refine_ls_restrained_S_all 0.660 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 1.10711(3) 1.43390(3) 0.30245(2) 0.03025(15) Uani 1 1 d . . . Cl1 Cl 1.1124(2) 1.2876(2) 0.44655(17) 0.0313(5) Uani 1 1 d . . . Cl2 Cl 1.2664(2) 1.2925(2) 0.21910(18) 0.0421(6) Uani 1 1 d . . . Cl3 Cl 1.2180(2) 1.6424(2) 0.26182(17) 0.0348(5) Uani 1 1 d . . . Cl4 Cl 0.8637(2) 1.5118(2) 0.26425(18) 0.0364(6) Uani 1 1 d . . . O1 O 0.9695(6) 1.2339(6) 0.2167(5) 0.0437(18) Uani 1 1 d . . . O2 O 1.0142(6) 1.4226(6) 0.1140(5) 0.0368(16) Uani 1 1 d . . . O3 O 1.0976(6) 1.5878(6) 0.4523(5) 0.0364(16) Uani 1 1 d . . . O4 O 1.3258(5) 1.4899(5) 0.4327(4) 0.0242(13) Uani 1 1 d . . . O5 O 0.1257(6) 0.8490(6) -0.0125(5) 0.0398(17) Uani 1 1 d . . . O6 O 0.8516(7) 0.5880(7) 0.0242(5) 0.050(2) Uani 1 1 d . . . C1 C 0.2312(9) 0.7808(9) 0.0301(8) 0.041(2) Uani 1 1 d . . . H1A H 0.2531 0.7264 -0.0239 0.049 Uiso 1 1 calc R . . H1B H 0.2074 0.7297 0.0741 0.049 Uiso 1 1 calc R . . C2 C 0.3440(10) 0.8728(10) 0.0900(8) 0.042(2) Uani 1 1 d . . . H2A H 0.4266 0.8402 0.0906 0.050 Uiso 1 1 calc R . . H2B H 0.3431 0.9000 0.1599 0.050 Uiso 1 1 calc R . . C3 C 0.3171(11) 0.9769(14) 0.0286(10) 0.068(4) Uani 1 1 d . . . H3A H 0.3608 1.0567 0.0696 0.082 Uiso 1 1 calc R . . H3B H 0.3452 0.9594 -0.0321 0.082 Uiso 1 1 calc R . . C4 C 0.1724(9) 0.9766(9) 0.0007(7) 0.035(2) Uani 1 1 d . . . H4A H 0.1474 1.0273 0.0549 0.043 Uiso 1 1 calc R . . H4B H 0.1382 1.0083 -0.0621 0.043 Uiso 1 1 calc R . . C5 C 0.8782(10) 0.7153(9) 0.0824(7) 0.042(3) Uani 1 1 d . . . H5A H 0.8998 0.7733 0.0424 0.051 Uiso 1 1 calc R . . H5B H 0.9500 0.7215 0.1452 0.051 Uiso 1 1 calc R . . C6 C 0.7499(11) 0.7428(11) 0.1060(8) 0.053(3) Uani 1 1 d U . . H6A H 0.7463 0.7137 0.1675 0.064 Uiso 1 1 calc R . . H6B H 0.7392 0.8314 0.1138 0.064 Uiso 1 1 calc R . . C7 C 0.6470(10) 0.6685(10) 0.0112(9) 0.052(3) Uani 1 1 d . . . H7A H 0.6333 0.7114 -0.0463 0.062 Uiso 1 1 calc R . . H7B H 0.5643 0.6538 0.0243 0.062 Uiso 1 1 calc R . . C8 C 0.7076(10) 0.5450(11) -0.0089(8) 0.056(3) Uani 1 1 d . . . H8A H 0.6763 0.5062 -0.0809 0.067 Uiso 1 1 calc R . . H8B H 0.6884 0.4865 0.0316 0.067 Uiso 1 1 calc R . . O8 O 0.7063(17) 1.2863(14) 0.3921(12) 0.029(3) Uani 0.50 1 d PD A 1 C9 C 0.7015(18) 1.2288(17) 0.2883(13) 0.036(3) Uani 0.50 1 d PDU A 1 H9A H 0.7841 1.1973 0.2872 0.043 Uiso 0.50 1 calc PR A 1 H9B H 0.6810 1.2880 0.2423 0.043 Uiso 0.50 1 calc PR A 1 C10 C 0.595(2) 1.125(2) 0.2596(15) 0.040(5) Uani 0.50 1 d PDU A 1 H10A H 0.5160 1.1465 0.2129 0.048 Uiso 0.50 1 calc PR A 1 H10B H 0.6208 1.0492 0.2264 0.048 Uiso 0.50 1 calc PR A 1 C11 C 0.5715(18) 1.1057(14) 0.3555(12) 0.030(3) Uani 0.50 1 d PD A 1 H11A H 0.6312 1.0508 0.3892 0.036 Uiso 0.50 1 calc PR A 1 H11B H 0.4822 1.0712 0.3433 0.036 Uiso 0.50 1 calc PR A 1 C12 C 0.5974(15) 1.2353(13) 0.4167(12) 0.024(3) Uani 0.50 1 d PD A 1 H12A H 0.5224 1.2821 0.3966 0.028 Uiso 0.50 1 calc PR A 1 H12B H 0.6193 1.2346 0.4895 0.028 Uiso 0.50 1 calc PR A 1 O8' C 0.6240(16) 1.3117(15) 0.3286(12) 0.029(3) Uani 0.50 1 d PD B 2 C9' C 0.624(2) 1.2296(15) 0.2325(13) 0.036(3) Uani 0.50 1 d PDU B 2 H9'1 H 0.5377 1.2209 0.1820 0.043 Uiso 0.50 1 calc PR B 2 H9'2 H 0.6871 1.2643 0.2046 0.043 Uiso 0.50 1 calc PR B 2 C10' C 0.658(2) 1.1075(19) 0.2591(14) 0.040(5) Uani 0.50 1 d PDU B 2 H10C H 0.5806 1.0555 0.2565 0.048 Uiso 0.50 1 calc PR B 2 H10D H 0.7006 1.0636 0.2132 0.048 Uiso 0.50 1 calc PR B 2 C11' C 0.7475(17) 1.1415(15) 0.3645(12) 0.030(3) Uani 0.50 1 d PD B 2 H11C H 0.8375 1.1521 0.3641 0.036 Uiso 0.50 1 calc PR B 2 H11D H 0.7393 1.0772 0.4035 0.036 Uiso 0.50 1 calc PR B 2 C12' C 0.709(3) 1.2585(19) 0.4085(16) 0.024(3) Uani 0.50 1 d PD B 2 H12C H 0.6643 1.2436 0.4573 0.028 Uiso 0.50 1 calc PR B 2 H12D H 0.7864 1.3166 0.4445 0.028 Uiso 0.50 1 calc PR B 2 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 0.0198(2) 0.0314(2) 0.0275(2) -0.00847(14) -0.00437(14) 0.00886(14) Cl1 0.0236(11) 0.0287(12) 0.0352(12) -0.0036(10) 0.0050(9) 0.0017(9) Cl2 0.0303(13) 0.0482(15) 0.0335(13) -0.0132(11) -0.0027(10) 0.0178(11) Cl3 0.0318(12) 0.0332(13) 0.0281(12) -0.0014(10) -0.0050(10) 0.0098(10) Cl4 0.0187(11) 0.0381(13) 0.0419(14) -0.0055(11) -0.0011(10) 0.0116(9) O1 0.028(4) 0.035(4) 0.046(4) -0.014(3) -0.010(3) 0.014(3) O2 0.027(3) 0.042(4) 0.025(3) -0.013(3) -0.007(3) 0.016(3) O3 0.023(3) 0.037(4) 0.040(4) -0.008(3) 0.004(3) 0.010(3) O4 0.015(3) 0.030(3) 0.021(3) -0.002(3) 0.001(2) -0.001(2) O5 0.020(3) 0.036(4) 0.041(4) -0.017(3) -0.011(3) 0.003(3) O6 0.035(4) 0.067(5) 0.033(4) -0.010(4) -0.005(3) 0.030(4) C1 0.032(5) 0.035(6) 0.044(6) -0.001(5) -0.004(5) 0.006(4) C2 0.042(6) 0.048(6) 0.035(6) 0.015(5) 0.008(5) 0.003(5) C3 0.037(7) 0.105(11) 0.070(9) 0.058(8) 0.005(6) 0.010(7) C4 0.036(5) 0.032(5) 0.023(5) -0.001(4) -0.010(4) 0.002(4) C5 0.041(6) 0.045(6) 0.027(5) -0.005(5) -0.006(4) 0.020(5) C6 0.057(7) 0.052(7) 0.041(6) -0.011(5) 0.008(5) 0.031(6) C7 0.035(6) 0.049(7) 0.054(7) -0.011(5) -0.003(5) 0.021(5) C8 0.044(7) 0.070(8) 0.037(6) -0.013(6) -0.007(5) 0.035(6) O8 0.020(6) 0.025(7) 0.038(8) -0.011(5) 0.012(5) 0.006(5) C9 0.035(8) 0.029(7) 0.031(8) -0.022(7) 0.011(6) -0.012(7) C10 0.042(12) 0.039(8) 0.030(6) -0.008(6) 0.008(9) -0.014(9) C11 0.030(7) 0.020(7) 0.037(8) 0.000(6) 0.009(6) -0.002(5) C12 0.026(6) 0.021(7) 0.013(6) -0.014(5) -0.003(5) 0.000(6) O8' 0.020(6) 0.025(7) 0.038(8) -0.011(5) 0.012(5) 0.006(5) C9' 0.035(8) 0.029(7) 0.031(8) -0.022(7) 0.011(6) -0.012(7) C10' 0.042(12) 0.039(8) 0.030(6) -0.008(6) 0.008(9) -0.014(9) C11' 0.030(7) 0.020(7) 0.037(8) 0.000(6) 0.009(6) -0.002(5) C12' 0.026(6) 0.021(7) 0.013(6) -0.014(5) -0.003(5) 0.000(6) _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 O1 2.481(6) . ? Th1 O4 2.483(5) . ? Th1 O2 2.493(6) . ? Th1 O3 2.479(6) . ? Th1 Cl4 2.717(2) . ? Th1 Cl2 2.733(2) . ? Th1 Cl3 2.732(3) . ? Th1 Cl1 2.748(3) . ? O5 C1 1.421(11) . ? O5 C4 1.418(11) . ? O6 C5 1.455(11) . ? O6 C8 1.506(13) . ? C1 C2 1.477(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.518(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.487(14) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.539(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.523(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.541(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O8 C12 1.426(16) . ? O8 C9 1.459(16) . ? C9 C10 1.490(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.472(17) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.491(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? O8' C12' 1.439(17) . ? O8' C9' 1.477(15) . ? C9' C10' 1.473(17) . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C10' C11' 1.473(17) . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C11' C12' 1.452(17) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12' H12C 0.9700 . ? C12' H12D 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 O1 Th1 O4 134.2(2) . . ? O1 Th1 O2 68.2(2) . . ? O4 Th1 O2 136.3(2) . . ? O1 Th1 O3 129.7(2) . . ? O4 Th1 O3 68.31(18) . . ? O2 Th1 O3 132.6(2) . . ? O1 Th1 Cl4 79.14(15) . . ? O4 Th1 Cl4 138.41(14) . . ? O2 Th1 Cl4 71.88(14) . . ? O3 Th1 Cl4 70.62(15) . . ? O1 Th1 Cl2 75.91(16) . . ? O4 Th1 Cl2 76.61(14) . . ? O2 Th1 Cl2 75.19(14) . . ? O3 Th1 Cl2 144.92(15) . . ? Cl4 Th1 Cl2 144.20(7) . . ? O1 Th1 Cl3 141.99(18) . . ? O4 Th1 Cl3 72.76(14) . . ? O2 Th1 Cl3 74.27(16) . . ? O3 Th1 Cl3 81.05(17) . . ? Cl4 Th1 Cl3 94.85(8) . . ? Cl2 Th1 Cl3 89.38(8) . . ? O1 Th1 Cl1 71.23(18) . . ? O4 Th1 Cl1 74.53(14) . . ? O2 Th1 Cl1 139.34(16) . . ? O3 Th1 Cl1 77.26(17) . . ? Cl4 Th1 Cl1 102.63(7) . . ? Cl2 Th1 Cl1 93.22(8) . . ? Cl3 Th1 Cl1 145.59(7) . . ? C1 O5 C4 109.6(7) . . ? C5 O6 C8 110.9(7) . . ? O5 C1 C2 107.3(8) . . ? O5 C1 H1A 110.3 . . ? C2 C1 H1A 110.3 . . ? O5 C1 H1B 110.3 . . ? C2 C1 H1B 110.3 . . ? H1A C1 H1B 108.5 . . ? C1 C2 C3 99.9(9) . . ? C1 C2 H2A 111.8 . . ? C3 C2 H2A 111.8 . . ? C1 C2 H2B 111.8 . . ? C3 C2 H2B 111.8 . . ? H2A C2 H2B 109.5 . . ? C4 C3 C2 103.0(9) . . ? C4 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? C4 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? O5 C4 C3 104.4(8) . . ? O5 C4 H4A 110.9 . . ? C3 C4 H4A 110.9 . . ? O5 C4 H4B 110.9 . . ? C3 C4 H4B 110.9 . . ? H4A C4 H4B 108.9 . . ? O6 C5 C6 104.4(8) . . ? O6 C5 H5A 110.9 . . ? C6 C5 H5A 110.9 . . ? O6 C5 H5B 110.9 . . ? C6 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? C7 C6 C5 102.1(8) . . ? C7 C6 H6A 111.3 . . ? C5 C6 H6A 111.3 . . ? C7 C6 H6B 111.3 . . ? C5 C6 H6B 111.3 . . ? H6A C6 H6B 109.2 . . ? C6 C7 C8 102.9(8) . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7B 111.2 . . ? C8 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? C7 C8 O6 102.3(9) . . ? C7 C8 H8A 111.3 . . ? O6 C8 H8A 111.3 . . ? C7 C8 H8B 111.3 . . ? O6 C8 H8B 111.3 . . ? H8A C8 H8B 109.2 . . ? C12 O8 C9 110.0(14) . . ? O8 C9 C10 103.4(14) . . ? O8 C9 H9A 111.1 . . ? C10 C9 H9A 111.1 . . ? O8 C9 H9B 111.1 . . ? C10 C9 H9B 111.1 . . ? H9A C9 H9B 109.0 . . ? C11 C10 C9 106.5(15) . . ? C11 C10 H10A 110.4 . . ? C9 C10 H10A 110.4 . . ? C11 C10 H10B 110.4 . . ? C9 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C10 C11 C12 102.2(14) . . ? C10 C11 H11A 111.3 . . ? C12 C11 H11A 111.3 . . ? C10 C11 H11B 111.3 . . ? C12 C11 H11B 111.3 . . ? H11A C11 H11B 109.2 . . ? O8 C12 C11 102.8(12) . . ? O8 C12 H12A 111.2 . . ? C11 C12 H12A 111.2 . . ? O8 C12 H12B 111.2 . . ? C11 C12 H12B 111.2 . . ? H12A C12 H12B 109.1 . . ? C12' O8' C9' 104.5(15) . . ? C10' C9' O8' 106.4(16) . . ? C10' C9' H9'1 110.4 . . ? O8' C9' H9'1 110.4 . . ? C10' C9' H9'2 110.4 . . ? O8' C9' H9'2 110.4 . . ? H9'1 C9' H9'2 108.6 . . ? C11' C10' C9' 103.1(16) . . ? C11' C10' H10C 111.1 . . ? C9' C10' H10C 111.1 . . ? C11' C10' H10D 111.1 . . ? C9' C10' H10D 111.1 . . ? H10C C10' H10D 109.1 . . ? C10' C11' C12' 105.6(16) . . ? C10' C11' H11C 110.6 . . ? C12' C11' H11C 110.6 . . ? C10' C11' H11D 110.6 . . ? C12' C11' H11D 110.6 . . ? H11C C11' H11D 108.7 . . ? O8' C12' C11' 109.8(16) . . ? O8' C12' H12C 109.7 . . ? C11' C12' H12C 109.7 . . ? O8' C12' H12D 109.7 . . ? C11' C12' H12D 109.7 . . ? H12C C12' H12D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.079 _refine_diff_density_min -1.639 _refine_diff_density_rms 0.178 #===============END================= #compound 2dot3(1,4-dioxane) data_apx912a _database_code_depnum_ccdc_archive 'CCDC 753731' #TrackingRef 'Kiplinger_B923558B_CIF_Re-revised_12-14-09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Cl4 O10 Th' _chemical_formula_weight 710.22 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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M 'P bna' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 10.2963(13) _cell_length_b 12.3952(15) _cell_length_c 18.491(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2359.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 6195 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 54.8 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 6.813 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3156 _exptl_absorpt_correction_T_max 0.7723 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _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 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24922 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.40 _reflns_number_total 2861 _reflns_number_gt 2107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atom postions for water ligands were not included in the refinement. ; _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^)+(0.0347P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2861 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_restrained_S_all 1.204 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 0.912706(18) 0.7500 0.5000 0.01192(8) Uani 1 2 d S . . Cl1 Cl 1.11225(10) 0.64303(9) 0.56998(6) 0.0209(2) Uani 1 1 d . . . Cl2 Cl 0.72581(10) 0.74340(8) 0.39523(6) 0.0196(2) Uani 1 1 d . . . O1 O 0.9949(3) 0.8743(2) 0.59373(14) 0.0156(6) Uani 1 1 d . . . O2 O 0.8250(3) 0.9333(2) 0.48104(16) 0.0188(7) Uani 1 1 d . . . O3 O 0.0944(3) 0.4269(2) 0.72472(16) 0.0226(7) Uani 1 1 d . . . O4 O 0.2774(3) 0.3992(2) 0.83623(16) 0.0243(7) Uani 1 1 d . . . O5 O 0.5834(3) -0.0065(3) 0.44013(17) 0.0230(7) Uani 1 1 d . . . C1 C 0.1505(4) 0.5179(4) 0.7610(2) 0.0264(11) Uani 1 1 d . . . H1A H 0.0949 0.5393 0.8009 0.032 Uiso 1 1 calc R . . H1B H 0.1565 0.5781 0.7277 0.032 Uiso 1 1 calc R . . C2 C 0.2821(4) 0.4911(4) 0.7890(3) 0.0274(11) Uani 1 1 d . . . H2A H 0.3396 0.4759 0.7487 0.033 Uiso 1 1 calc R . . H2B H 0.3168 0.5526 0.8151 0.033 Uiso 1 1 calc R . . C3 C 0.2226(5) 0.3089(4) 0.7989(2) 0.0266(11) Uani 1 1 d . . . H3A H 0.2171 0.2477 0.8315 0.032 Uiso 1 1 calc R . . H3B H 0.2782 0.2890 0.7587 0.032 Uiso 1 1 calc R . . C4 C 0.0893(4) 0.3363(4) 0.7712(3) 0.0282(11) Uani 1 1 d . . . H4A H 0.0539 0.2751 0.7453 0.034 Uiso 1 1 calc R . . H4B H 0.0323 0.3519 0.8117 0.034 Uiso 1 1 calc R . . C5 C 0.5639(4) 0.0935(4) 0.4772(3) 0.0241(10) Uani 1 1 d . . . H5A H 0.4941 0.1334 0.4542 0.029 Uiso 1 1 calc R . . H5B H 0.6423 0.1367 0.4744 0.029 Uiso 1 1 calc R . . C6 C 0.4697(4) -0.0729(4) 0.4446(3) 0.0265(11) Uani 1 1 d . . . H6A H 0.4854 -0.1409 0.4202 0.032 Uiso 1 1 calc R . . H6B H 0.3976 -0.0372 0.4207 0.032 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 0.01021(12) 0.01218(12) 0.01337(13) -0.00093(9) 0.000 0.000 Cl1 0.0207(5) 0.0176(5) 0.0243(6) -0.0032(5) -0.0072(5) 0.0046(4) Cl2 0.0160(5) 0.0227(5) 0.0201(5) -0.0031(4) -0.0042(4) 0.0011(4) O1 0.0139(15) 0.0160(15) 0.0169(15) -0.0027(12) -0.0009(12) -0.0015(12) O2 0.0164(16) 0.0165(16) 0.0235(17) -0.0005(12) -0.0004(12) 0.0016(13) O3 0.0265(18) 0.0233(17) 0.0182(17) -0.0009(13) -0.0089(13) 0.0023(13) O4 0.0217(17) 0.0291(17) 0.0219(17) -0.0005(14) -0.0082(14) 0.0016(13) O5 0.0172(16) 0.0265(18) 0.0253(18) -0.0031(15) 0.0035(13) 0.0010(12) C1 0.029(3) 0.024(3) 0.026(3) -0.001(2) -0.001(2) 0.005(2) C2 0.025(3) 0.025(3) 0.031(3) -0.001(2) -0.006(2) -0.002(2) C3 0.028(3) 0.027(3) 0.024(3) -0.001(2) -0.004(2) 0.005(2) C4 0.029(3) 0.029(3) 0.027(3) 0.001(2) -0.007(2) -0.005(2) C5 0.015(2) 0.022(3) 0.035(3) 0.004(2) -0.002(2) 0.0024(19) C6 0.015(2) 0.030(3) 0.035(3) -0.009(2) -0.002(2) 0.000(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 O2 2.470(3) . ? Th1 O2 2.470(3) 3_566 ? Th1 O1 2.469(3) . ? Th1 O1 2.469(3) 3_566 ? Th1 Cl2 2.7318(11) 3_566 ? Th1 Cl2 2.7318(11) . ? Th1 Cl1 2.7665(11) 3_566 ? Th1 Cl1 2.7665(11) . ? O3 C4 1.416(6) . ? O3 C1 1.433(5) . ? O4 C3 1.431(5) . ? O4 C2 1.437(5) . ? O5 C5 1.430(6) . ? O5 C6 1.433(5) . ? C1 C2 1.488(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.504(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.509(7) 5_656 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.509(7) 5_656 ? C6 H6A 0.9700 . ? C6 H6B 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 O2 Th1 O2 137.10(14) . 3_566 ? O2 Th1 O1 69.56(9) . . ? O2 Th1 O1 126.87(9) 3_566 . ? O2 Th1 O1 126.87(9) . 3_566 ? O2 Th1 O1 69.56(9) 3_566 3_566 ? O1 Th1 O1 139.90(13) . 3_566 ? O2 Th1 Cl2 79.37(7) . 3_566 ? O2 Th1 Cl2 70.69(7) 3_566 3_566 ? O1 Th1 Cl2 74.04(7) . 3_566 ? O1 Th1 Cl2 139.29(7) 3_566 3_566 ? O2 Th1 Cl2 70.69(7) . . ? O2 Th1 Cl2 79.37(7) 3_566 . ? O1 Th1 Cl2 139.29(7) . . ? O1 Th1 Cl2 74.04(7) 3_566 . ? Cl2 Th1 Cl2 90.43(5) 3_566 . ? O2 Th1 Cl1 76.37(7) . 3_566 ? O2 Th1 Cl1 141.15(7) 3_566 3_566 ? O1 Th1 Cl1 76.97(7) . 3_566 ? O1 Th1 Cl1 73.51(7) 3_566 3_566 ? Cl2 Th1 Cl1 147.19(3) 3_566 3_566 ? Cl2 Th1 Cl1 101.88(3) . 3_566 ? O2 Th1 Cl1 141.15(7) . . ? O2 Th1 Cl1 76.37(7) 3_566 . ? O1 Th1 Cl1 73.51(7) . . ? O1 Th1 Cl1 76.97(7) 3_566 . ? Cl2 Th1 Cl1 101.88(3) 3_566 . ? Cl2 Th1 Cl1 147.19(3) . . ? Cl1 Th1 Cl1 84.09(5) 3_566 . ? C4 O3 C1 110.8(3) . . ? C3 O4 C2 109.9(3) . . ? C5 O5 C6 110.8(3) . . ? O3 C1 C2 110.7(4) . . ? O3 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? O3 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O4 C2 C1 111.0(4) . . ? O4 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? O4 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? O4 C3 C4 110.3(4) . . ? O4 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? O4 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O3 C4 C3 110.6(4) . . ? O3 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? O3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? O5 C5 C6 110.2(4) . 5_656 ? O5 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 5_656 . ? O5 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 5_656 . ? H5A C5 H5B 108.1 . . ? O5 C6 C5 109.9(4) . 5_656 ? O5 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 5_656 . ? O5 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 5_656 . ? H6A C6 H6B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.923 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.157 #==============END==================== #Compound 3 data_apx915a _database_code_depnum_ccdc_archive 'CCDC 753732' #TrackingRef 'Kiplinger_B923558B_CIF_Re-revised_12-14-09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Cl4 O4 Th' _chemical_formula_weight 554.08 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 16.644(3) _cell_length_b 7.3263(15) _cell_length_c 14.877(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.356(2) _cell_angle_gamma 90.00 _cell_volume 1639.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 6954 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 54.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 9.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2729 _exptl_absorpt_correction_T_max 0.5094 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17216 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 28.24 _reflns_number_total 3819 _reflns_number_gt 3272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3819 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 0.247821(11) 0.03026(2) 0.280684(12) 0.01432(8) Uani 1 1 d . . . Cl1 Cl 0.11081(9) 0.23096(17) 0.15246(9) 0.0230(3) Uani 1 1 d . . . Cl2 Cl 0.16713(9) -0.27781(17) 0.29360(9) 0.0230(3) Uani 1 1 d . . . Cl3 Cl 0.36292(9) -0.04596(17) 0.46968(9) 0.0217(3) Uani 1 1 d . . . Cl4 Cl 0.34674(9) 0.20870(18) 0.20553(9) 0.0235(3) Uani 1 1 d . . . O1 O 0.1972(2) -0.1482(5) 0.1130(2) 0.0197(7) Uani 1 1 d . . . O2 O 0.3613(2) -0.1991(5) 0.2674(2) 0.0188(7) Uani 1 1 d . . . O3 O 0.1510(2) 0.1168(5) 0.3729(3) 0.0231(8) Uani 1 1 d . . . O4 O 0.2887(2) 0.3329(5) 0.3768(2) 0.0224(8) Uani 1 1 d . . . C1 C 0.1044(3) -0.1797(8) 0.0460(4) 0.0267(12) Uani 1 1 d . . . H1A H 0.0984 -0.1920 -0.0208 0.040 Uiso 1 1 calc R . . H1B H 0.0692 -0.0785 0.0495 0.040 Uiso 1 1 calc R . . H1C H 0.0843 -0.2895 0.0651 0.040 Uiso 1 1 calc R . . C2 C 0.2468(3) -0.3129(7) 0.1173(4) 0.0227(11) Uani 1 1 d . . . H2A H 0.2323 -0.3567 0.0506 0.027 Uiso 1 1 calc R . . H2B H 0.2318 -0.4074 0.1531 0.027 Uiso 1 1 calc R . . C3 C 0.3436(4) -0.2693(7) 0.1694(4) 0.0224(11) Uani 1 1 d . . . H3A H 0.3786 -0.3782 0.1753 0.027 Uiso 1 1 calc R . . H3B H 0.3593 -0.1787 0.1320 0.027 Uiso 1 1 calc R . . C4 C 0.4565(3) -0.1751(8) 0.3224(4) 0.0273(12) Uani 1 1 d . . . H4A H 0.4857 -0.2905 0.3284 0.041 Uiso 1 1 calc R . . H4B H 0.4695 -0.1285 0.3875 0.041 Uiso 1 1 calc R . . H4C H 0.4773 -0.0906 0.2878 0.041 Uiso 1 1 calc R . . C5 C 0.0605(4) 0.0572(8) 0.3451(5) 0.0340(15) Uani 1 1 d . . . H5A H 0.0479 0.0611 0.4023 0.051 Uiso 1 1 calc R . . H5B H 0.0534 -0.0654 0.3201 0.051 Uiso 1 1 calc R . . H5C H 0.0202 0.1365 0.2945 0.051 Uiso 1 1 calc R . . C6 C 0.1586(4) 0.3047(7) 0.4057(4) 0.0310(14) Uani 1 1 d . . . H6A H 0.1352 0.3174 0.4549 0.037 Uiso 1 1 calc R . . H6B H 0.1245 0.3832 0.3498 0.037 Uiso 1 1 calc R . . C7 C 0.2539(4) 0.3592(8) 0.4496(4) 0.0309(14) Uani 1 1 d . . . H7A H 0.2597 0.4863 0.4696 0.037 Uiso 1 1 calc R . . H7B H 0.2873 0.2858 0.5081 0.037 Uiso 1 1 calc R . . C8 C 0.3756(4) 0.4184(8) 0.4130(4) 0.0318(13) Uani 1 1 d . . . H8A H 0.3705 0.5455 0.4252 0.048 Uiso 1 1 calc R . . H8B H 0.3985 0.4058 0.3640 0.048 Uiso 1 1 calc R . . H8C H 0.4153 0.3602 0.4736 0.048 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 0.01569(12) 0.01736(12) 0.01162(11) 0.00040(6) 0.00747(8) -0.00063(6) Cl1 0.0231(7) 0.0245(7) 0.0188(6) 0.0004(5) 0.0065(5) 0.0049(5) Cl2 0.0244(7) 0.0203(6) 0.0289(7) 0.0006(5) 0.0158(6) -0.0029(5) Cl3 0.0244(7) 0.0279(7) 0.0128(6) 0.0028(4) 0.0079(5) 0.0009(5) Cl4 0.0273(7) 0.0272(7) 0.0214(6) 0.0013(5) 0.0156(6) -0.0056(5) O1 0.0169(18) 0.026(2) 0.0162(17) -0.0024(14) 0.0066(15) 0.0016(15) O2 0.0178(19) 0.029(2) 0.0138(17) -0.0021(14) 0.0106(15) 0.0012(14) O3 0.027(2) 0.023(2) 0.027(2) 0.0025(15) 0.0185(17) 0.0032(16) O4 0.031(2) 0.0193(19) 0.0175(18) -0.0032(14) 0.0112(16) -0.0007(16) C1 0.020(3) 0.031(3) 0.024(3) -0.008(2) 0.004(2) 0.000(2) C2 0.026(3) 0.022(3) 0.020(3) -0.008(2) 0.009(2) 0.002(2) C3 0.030(3) 0.024(3) 0.019(3) -0.002(2) 0.015(2) 0.005(2) C4 0.015(3) 0.044(4) 0.023(3) -0.004(2) 0.008(2) 0.003(2) C5 0.029(3) 0.037(4) 0.049(4) 0.008(3) 0.029(3) 0.008(3) C6 0.056(4) 0.020(3) 0.032(3) -0.001(2) 0.032(3) 0.005(3) C7 0.056(4) 0.022(3) 0.023(3) -0.001(2) 0.024(3) 0.009(3) C8 0.032(3) 0.030(3) 0.023(3) -0.003(2) 0.002(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 O4 2.567(3) . ? Th1 O2 2.598(3) . ? Th1 O3 2.603(3) . ? Th1 O1 2.616(3) . ? Th1 Cl2 2.6751(13) . ? Th1 Cl4 2.6919(12) . ? Th1 Cl3 2.6970(13) . ? Th1 Cl1 2.6972(13) . ? O1 C2 1.448(6) . ? O1 C1 1.454(6) . ? O2 C4 1.450(6) . ? O2 C3 1.452(6) . ? O3 C6 1.448(6) . ? O3 C5 1.448(7) . ? O4 C7 1.443(6) . ? O4 C8 1.452(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.492(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.488(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Th1 O2 124.99(11) . . ? O4 Th1 O3 64.67(11) . . ? O2 Th1 O3 146.31(11) . . ? O4 Th1 O1 149.66(11) . . ? O2 Th1 O1 63.37(10) . . ? O3 Th1 O1 127.25(11) . . ? O4 Th1 Cl2 135.25(8) . . ? O2 Th1 Cl2 82.15(8) . . ? O3 Th1 Cl2 74.00(9) . . ? O1 Th1 Cl2 71.36(8) . . ? O4 Th1 Cl4 75.44(8) . . ? O2 Th1 Cl4 71.86(8) . . ? O3 Th1 Cl4 136.68(8) . . ? O1 Th1 Cl4 81.43(8) . . ? Cl2 Th1 Cl4 148.73(4) . . ? O4 Th1 Cl3 72.41(8) . . ? O2 Th1 Cl3 74.37(8) . . ? O3 Th1 Cl3 79.90(9) . . ? O1 Th1 Cl3 133.29(8) . . ? Cl2 Th1 Cl3 84.53(4) . . ? Cl4 Th1 Cl3 104.23(4) . . ? O4 Th1 Cl1 82.24(8) . . ? O2 Th1 Cl1 136.11(7) . . ? O3 Th1 Cl1 73.33(8) . . ? O1 Th1 Cl1 76.61(8) . . ? Cl2 Th1 Cl1 102.26(4) . . ? Cl4 Th1 Cl1 85.63(4) . . ? Cl3 Th1 Cl1 149.10(4) . . ? C2 O1 C1 108.4(4) . . ? C2 O1 Th1 115.4(3) . . ? C1 O1 Th1 123.1(3) . . ? C4 O2 C3 108.2(4) . . ? C4 O2 Th1 122.2(3) . . ? C3 O2 Th1 117.6(3) . . ? C6 O3 C5 108.3(4) . . ? C6 O3 Th1 115.1(3) . . ? C5 O3 Th1 125.4(3) . . ? C7 O4 C8 108.7(4) . . ? C7 O4 Th1 115.9(3) . . ? C8 O4 Th1 124.3(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 108.2(4) . . ? O1 C2 H2A 110.1 . . ? C3 C2 H2A 110.1 . . ? O1 C2 H2B 110.1 . . ? C3 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O2 C3 C2 107.9(4) . . ? O2 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? O2 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O2 C4 H4A 109.5 . . ? O2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 H5A 109.5 . . ? O3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 C7 109.0(4) . . ? O3 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? O3 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O4 C7 C6 109.2(4) . . ? O4 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? O4 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? O4 C8 H8A 109.5 . . ? O4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.010 _refine_diff_density_min -2.616 _refine_diff_density_rms 0.214 #=================END==================