# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jaqueline Kiplinger' _publ_contact_author_email kiplinger@lanl.gov loop_ _publ_author_name 'Nicholas Travia' 'Marisa Monreal' 'Brian Scott' 'Jaqueline Kiplinger' #==============END================== data_apx1274 _database_code_depnum_ccdc_archive 'CCDC 871914' #TrackingRef '- REVISED DT-ART-07-2012-031676 Kiplinger_corrected.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H40 I4 O4 Th' _chemical_formula_weight 1120.19 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 15.7866(16) _cell_length_b 12.9801(13) _cell_length_c 16.7168(17) _cell_angle_alpha 90.00 _cell_angle_beta 108.0200(10) _cell_angle_gamma 90.00 _cell_volume 3257.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 4.41 _cell_measurement_theta_max 56.31 _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 2.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 8.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3135 _exptl_absorpt_correction_T_max 0.6329 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _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 36043 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.40 _reflns_number_total 7743 _reflns_number_gt 6417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (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^)+(0.0243P)^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 7743 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.190784(11) 0.616923(12) 0.219771(9) 0.01593(5) Uani 1 1 d . . . I1 I 0.35369(2) 0.77000(3) 0.288562(19) 0.02890(8) Uani 1 1 d . . . I2 I -0.01764(2) 0.59696(3) 0.132328(19) 0.02860(8) Uani 1 1 d . . . I3 I 0.14381(2) 0.61668(2) 0.387972(18) 0.02301(7) Uani 1 1 d . . . I4 I 0.53672(2) 0.56361(3) 0.12416(2) 0.03691(9) Uani 1 1 d . . . O1 O 0.1625(2) 0.4298(2) 0.19228(19) 0.0240(7) Uani 1 1 d . . . O2 O 0.3195(2) 0.5074(2) 0.29920(18) 0.0257(7) Uani 1 1 d . . . O3 O 0.1327(2) 0.7908(2) 0.18521(18) 0.0219(7) Uani 1 1 d . . . O4 O 0.2111(2) 0.6095(2) 0.10424(18) 0.0186(6) Uani 1 1 d . . . C1 C 0.1309(4) 0.3842(4) 0.1073(3) 0.0316(12) Uani 1 1 d . . . H1A H 0.1805 0.3688 0.0866 0.038 Uiso 1 1 calc R . . H1B H 0.0904 0.4306 0.0682 0.038 Uiso 1 1 calc R . . C2 C 0.0838(4) 0.2871(4) 0.1187(3) 0.0437(15) Uani 1 1 d . . . H2A H 0.0866 0.2350 0.0780 0.052 Uiso 1 1 calc R . . H2B H 0.0219 0.3005 0.1138 0.052 Uiso 1 1 calc R . . C3 C 0.1362(5) 0.2544(4) 0.2076(4) 0.0507(17) Uani 1 1 d . . . H3A H 0.1014 0.2085 0.2310 0.061 Uiso 1 1 calc R . . H3B H 0.1913 0.2203 0.2088 0.061 Uiso 1 1 calc R . . C4 C 0.1541(4) 0.3543(4) 0.2543(3) 0.0317(12) Uani 1 1 d . . . H4A H 0.1053 0.3721 0.2756 0.038 Uiso 1 1 calc R . . H4B H 0.2087 0.3504 0.3012 0.038 Uiso 1 1 calc R . . C5 C 0.3721(4) 0.5076(4) 0.3890(3) 0.0402(14) Uani 1 1 d . . . H5A H 0.3941 0.5765 0.4064 0.048 Uiso 1 1 calc R . . H5B H 0.3354 0.4859 0.4229 0.048 Uiso 1 1 calc R . . C6 C 0.4453(5) 0.4380(7) 0.4002(4) 0.085(3) Uani 1 1 d . . . H6A H 0.4472 0.3887 0.4444 0.102 Uiso 1 1 calc R . . H6B H 0.5012 0.4754 0.4154 0.102 Uiso 1 1 calc R . . C7 C 0.4295(5) 0.3824(5) 0.3153(4) 0.0523(18) Uani 1 1 d . . . H7A H 0.4853 0.3698 0.3041 0.063 Uiso 1 1 calc R . . H7B H 0.3989 0.3174 0.3145 0.063 Uiso 1 1 calc R . . C8 C 0.3731(3) 0.4556(4) 0.2536(3) 0.0339(12) Uani 1 1 d . . . H8A H 0.4095 0.5049 0.2353 0.041 Uiso 1 1 calc R . . H8B H 0.3353 0.4194 0.2048 0.041 Uiso 1 1 calc R . . C9 C 0.1161(4) 0.8328(4) 0.1004(3) 0.0313(11) Uani 1 1 d . . . H9A H 0.0813 0.7851 0.0584 0.038 Uiso 1 1 calc R . . H9B H 0.1717 0.8469 0.0892 0.038 Uiso 1 1 calc R . . C10 C 0.0651(4) 0.9307(4) 0.1000(4) 0.0498(17) Uani 1 1 d . . . H10A H 0.0015 0.9177 0.0841 0.060 Uiso 1 1 calc R . . H10B H 0.0767 0.9809 0.0617 0.060 Uiso 1 1 calc R . . C11 C 0.1010(4) 0.9669(4) 0.1909(4) 0.0470(15) Uani 1 1 d . . . H11A H 0.1575 1.0024 0.2012 0.056 Uiso 1 1 calc R . . H11B H 0.0591 1.0123 0.2052 0.056 Uiso 1 1 calc R . . C12 C 0.1123(4) 0.8675(4) 0.2396(3) 0.0343(12) Uani 1 1 d . . . H12A H 0.1605 0.8730 0.2921 0.041 Uiso 1 1 calc R . . H12B H 0.0580 0.8498 0.2520 0.041 Uiso 1 1 calc R . . C13 C 0.2105(3) 0.6035(3) 0.0182(3) 0.0229(10) Uani 1 1 d . . . H13A H 0.1839 0.6655 -0.0114 0.028 Uiso 1 1 calc R . . H13B H 0.1746 0.5452 -0.0090 0.028 Uiso 1 1 calc R . . C14 C 0.3046(3) 0.5916(4) 0.0137(3) 0.0235(10) Uani 1 1 d . . . H14A H 0.3324 0.5333 0.0482 0.028 Uiso 1 1 calc R . . H14B H 0.3015 0.5762 -0.0439 0.028 Uiso 1 1 calc R . . C15 C 0.3626(3) 0.6854(3) 0.0425(3) 0.0249(10) Uani 1 1 d . . . H15A H 0.3343 0.7440 0.0088 0.030 Uiso 1 1 calc R . . H15B H 0.3667 0.7000 0.1005 0.030 Uiso 1 1 calc R . . C16 C 0.4553(3) 0.6737(4) 0.0363(3) 0.0298(11) Uani 1 1 d . . . H16A H 0.4846 0.7403 0.0461 0.036 Uiso 1 1 calc R . . H16B H 0.4511 0.6524 -0.0204 0.036 Uiso 1 1 calc R . . C17 C 0.6821(4) 0.8827(4) 0.9142(4) 0.0399(14) Uani 1 1 d . . . C18 C 0.6170(4) 0.8067(5) 0.8916(4) 0.0470(15) Uani 1 1 d . . . H18 H 0.5659 0.8174 0.8464 0.056 Uiso 1 1 calc R . . C19 C 0.6279(4) 0.7161(5) 0.9359(4) 0.0521(17) Uani 1 1 d . . . H19 H 0.5846 0.6650 0.9198 0.063 Uiso 1 1 calc R . . C20 C 0.7024(5) 0.7004(5) 1.0042(4) 0.062(2) Uani 1 1 d . . . H20 H 0.7078 0.6404 1.0358 0.075 Uiso 1 1 calc R . . C21 C 0.7679(5) 0.7724(5) 1.0253(4) 0.063(2) Uani 1 1 d . . . H21 H 0.8196 0.7603 1.0696 0.075 Uiso 1 1 calc R . . C22 C 0.7578(4) 0.8621(5) 0.9817(4) 0.0491(16) Uani 1 1 d . . . H22 H 0.8028 0.9112 0.9974 0.059 Uiso 1 1 calc R . . C23 C 0.6710(5) 0.9828(5) 0.8681(5) 0.072(2) Uani 1 1 d . . . H23A H 0.6093 0.9928 0.8371 0.108 Uiso 1 1 calc R . . H23B H 0.7055 0.9820 0.8298 0.108 Uiso 1 1 calc R . . H23C H 0.6910 1.0380 0.9076 0.108 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 0.01699(9) 0.01874(8) 0.01204(8) -0.00101(6) 0.00447(6) -0.00014(6) I1 0.02427(17) 0.03458(18) 0.02612(16) -0.00627(13) 0.00529(13) -0.00991(14) I2 0.01880(16) 0.0439(2) 0.02091(15) -0.00407(13) 0.00299(13) -0.00422(13) I3 0.02886(17) 0.02676(16) 0.01597(14) -0.00131(11) 0.01068(12) 0.00083(13) I4 0.0320(2) 0.0498(2) 0.02860(18) 0.00255(15) 0.00897(15) 0.00501(16) O1 0.0333(19) 0.0211(16) 0.0188(16) 0.0001(13) 0.0097(14) -0.0025(14) O2 0.0249(18) 0.0355(19) 0.0159(15) 0.0017(14) 0.0051(13) 0.0092(14) O3 0.0279(18) 0.0202(16) 0.0178(15) -0.0007(12) 0.0075(13) 0.0030(13) O4 0.0223(17) 0.0218(16) 0.0122(14) 0.0002(12) 0.0062(13) 0.0000(12) C1 0.043(3) 0.029(3) 0.025(3) -0.013(2) 0.014(2) -0.009(2) C2 0.058(4) 0.037(3) 0.043(3) -0.014(3) 0.028(3) -0.022(3) C3 0.082(5) 0.024(3) 0.061(4) 0.003(3) 0.043(4) -0.007(3) C4 0.048(3) 0.023(2) 0.031(3) 0.007(2) 0.021(2) -0.004(2) C5 0.039(3) 0.055(4) 0.018(2) 0.007(2) -0.003(2) 0.013(3) C6 0.084(6) 0.113(6) 0.041(4) -0.011(4) -0.006(4) 0.074(5) C7 0.057(4) 0.058(4) 0.036(3) 0.002(3) 0.006(3) 0.033(3) C8 0.032(3) 0.044(3) 0.032(3) 0.004(2) 0.019(2) 0.014(2) C9 0.039(3) 0.028(3) 0.027(3) 0.009(2) 0.011(2) 0.005(2) C10 0.068(4) 0.046(3) 0.045(4) 0.023(3) 0.031(3) 0.035(3) C11 0.066(4) 0.029(3) 0.056(4) 0.004(3) 0.033(3) 0.014(3) C12 0.044(3) 0.030(3) 0.037(3) 0.001(2) 0.024(3) 0.012(2) C13 0.030(3) 0.026(2) 0.012(2) 0.0007(18) 0.0055(19) -0.001(2) C14 0.027(3) 0.029(2) 0.017(2) -0.0017(19) 0.010(2) 0.002(2) C15 0.032(3) 0.020(2) 0.026(2) -0.0002(19) 0.015(2) 0.001(2) C16 0.027(3) 0.035(3) 0.030(3) -0.002(2) 0.012(2) -0.005(2) C17 0.042(4) 0.043(3) 0.035(3) -0.005(2) 0.012(3) -0.008(3) C18 0.031(3) 0.053(4) 0.058(4) -0.016(3) 0.016(3) -0.012(3) C19 0.045(4) 0.050(4) 0.074(5) -0.023(3) 0.037(4) -0.014(3) C20 0.094(6) 0.049(4) 0.060(5) -0.005(3) 0.047(4) 0.013(4) C21 0.079(5) 0.066(5) 0.039(4) -0.019(3) 0.011(4) 0.033(4) C22 0.039(4) 0.048(4) 0.055(4) -0.030(3) 0.007(3) -0.010(3) C23 0.075(5) 0.075(5) 0.063(5) 0.006(4) 0.016(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 Th1 O4 2.056(3) . ? Th1 O3 2.437(3) . ? Th1 O1 2.487(3) . ? Th1 O2 2.499(3) . ? Th1 I3 3.1219(4) . ? Th1 I2 3.1709(5) . ? Th1 I1 3.1709(4) . ? I4 C16 2.164(5) . ? O1 C4 1.462(5) . ? O1 C1 1.476(5) . ? O2 C8 1.466(5) . ? O2 C5 1.474(5) . ? O3 C12 1.450(5) . ? O3 C9 1.465(5) . ? O4 C13 1.437(5) . ? C1 C2 1.505(7) . ? C2 C3 1.520(8) . ? C3 C4 1.495(7) . ? C5 C6 1.432(8) . ? C6 C7 1.542(8) . ? C7 C8 1.480(7) . ? C9 C10 1.502(7) . ? C10 C11 1.523(8) . ? C11 C12 1.507(7) . ? C13 C14 1.518(6) . ? C14 C15 1.510(6) . ? C15 C16 1.507(6) . ? C17 C18 1.389(7) . ? C17 C22 1.393(8) . ? C17 C23 1.493(8) . ? C18 C19 1.373(9) . ? C19 C20 1.377(10) . ? C20 C21 1.357(10) . ? C21 C22 1.356(9) . ? 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 O3 88.70(10) . . ? O4 Th1 O1 81.50(10) . . ? O3 Th1 O1 145.87(11) . . ? O4 Th1 O2 97.75(11) . . ? O3 Th1 O2 146.85(11) . . ? O1 Th1 O2 67.20(11) . . ? O4 Th1 I3 174.74(8) . . ? O3 Th1 I3 92.16(7) . . ? O1 Th1 I3 94.94(7) . . ? O2 Th1 I3 84.34(7) . . ? O4 Th1 I2 90.26(8) . . ? O3 Th1 I2 72.89(7) . . ? O1 Th1 I2 74.54(8) . . ? O2 Th1 I2 139.08(8) . . ? I3 Th1 I2 85.031(11) . . ? O4 Th1 I1 91.43(8) . . ? O3 Th1 I1 73.09(7) . . ? O1 Th1 I1 139.32(8) . . ? O2 Th1 I1 74.27(8) . . ? I3 Th1 I1 93.784(10) . . ? I2 Th1 I1 145.886(11) . . ? C4 O1 C1 109.7(3) . . ? C4 O1 Th1 125.0(3) . . ? C1 O1 Th1 123.9(3) . . ? C8 O2 C5 107.3(4) . . ? C8 O2 Th1 119.3(3) . . ? C5 O2 Th1 130.5(3) . . ? C12 O3 C9 110.1(3) . . ? C12 O3 Th1 128.8(3) . . ? C9 O3 Th1 121.1(3) . . ? C13 O4 Th1 171.0(3) . . ? O1 C1 C2 104.3(4) . . ? C1 C2 C3 102.5(4) . . ? C4 C3 C2 103.1(4) . . ? O1 C4 C3 104.7(4) . . ? C6 C5 O2 108.0(5) . . ? C5 C6 C7 106.3(5) . . ? C8 C7 C6 103.5(5) . . ? O2 C8 C7 104.5(4) . . ? O3 C9 C10 104.8(4) . . ? C9 C10 C11 102.9(4) . . ? C12 C11 C10 102.7(4) . . ? O3 C12 C11 105.1(4) . . ? O4 C13 C14 110.5(4) . . ? C15 C14 C13 114.1(4) . . ? C16 C15 C14 113.8(4) . . ? C15 C16 I4 113.9(3) . . ? C18 C17 C22 117.4(6) . . ? C18 C17 C23 121.2(6) . . ? C22 C17 C23 121.4(6) . . ? C19 C18 C17 120.2(6) . . ? C18 C19 C20 120.4(6) . . ? C21 C20 C19 120.0(7) . . ? C22 C21 C20 119.9(7) . . ? C21 C22 C17 122.0(6) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.859 _refine_diff_density_min -1.120 _refine_diff_density_rms 0.169 data_apx1264 _database_code_depnum_ccdc_archive 'CCDC 871928' #TrackingRef '- REVISED DT-ART-07-2012-031676 Kiplinger_corrected.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 I4 O5 Th' _chemical_formula_weight 991.98 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 16.3845(10) _cell_length_b 7.8259(5) _cell_length_c 18.6448(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.9210(1) _cell_angle_gamma 90.00 _cell_volume 2355.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 8847 _cell_measurement_theta_min 4.71 _cell_measurement_theta_max 56.72 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 11.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2295 _exptl_absorpt_correction_T_max 0.4574 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _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 25716 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.36 _reflns_number_total 5593 _reflns_number_gt 4983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (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^)+(0.0237P)^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 5593 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0508 _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 0.281577(9) 0.65106(2) 0.065503(8) 0.01102(5) Uani 1 1 d . A . I1 I 0.133078(17) 0.39490(4) 0.063628(15) 0.01637(7) Uani 1 1 d . . . I2 I 0.459559(17) 0.78040(4) 0.136722(16) 0.02062(7) Uani 1 1 d . . . I3 I 0.304908(19) 0.53036(4) -0.093125(15) 0.02182(8) Uani 1 1 d . . . I4 I -0.085255(18) 0.81766(4) 0.236488(16) 0.01985(7) Uani 1 1 d . A . O1 O 0.15477(17) 0.7781(4) -0.01807(15) 0.0150(6) Uani 1 1 d . . . O2 O 0.30388(17) 0.9369(4) -0.00671(15) 0.0158(6) Uani 1 1 d . . . O3 O 0.3685(2) 0.3654(4) 0.08044(19) 0.0290(8) Uani 1 1 d . . . O4 O 0.3106(2) 0.5068(4) 0.19242(16) 0.0237(7) Uani 1 1 d . . . O5 O 0.23178(17) 0.8200(4) 0.13132(15) 0.0140(6) Uani 1 1 d . . . C1 C 0.1029(3) 0.7124(6) -0.0832(2) 0.0205(10) Uani 1 1 d . . . H1A H 0.0459 0.7378 -0.0816 0.031 Uiso 1 1 calc R . . H1B H 0.1100 0.5909 -0.0857 0.031 Uiso 1 1 calc R . . H1C H 0.1184 0.7650 -0.1253 0.031 Uiso 1 1 calc R . . C2 C 0.1588(3) 0.9607(6) -0.0184(2) 0.0183(9) Uani 1 1 d . . . H2A H 0.1632 1.0038 0.0309 0.022 Uiso 1 1 calc R . . H2B H 0.1088 1.0070 -0.0473 0.022 Uiso 1 1 calc R . . C3 C 0.2318(3) 1.0145(6) -0.0495(2) 0.0201(10) Uani 1 1 d . . . H3A H 0.2260 0.9779 -0.0998 0.024 Uiso 1 1 calc R . . H3B H 0.2370 1.1380 -0.0479 0.024 Uiso 1 1 calc R . . C4 C 0.3755(3) 0.9765(7) -0.0394(3) 0.0242(11) Uani 1 1 d . . . H4A H 0.3734 0.9115 -0.0834 0.036 Uiso 1 1 calc R . . H4B H 0.4250 0.9482 -0.0060 0.036 Uiso 1 1 calc R . . H4C H 0.3756 1.0963 -0.0506 0.036 Uiso 1 1 calc R . . C5 C 0.4510(3) 0.3444(7) 0.0660(3) 0.0337(13) Uani 1 1 d . A . H5A H 0.4897 0.3949 0.1048 0.051 Uiso 1 1 calc R . . H5B H 0.4557 0.3993 0.0209 0.051 Uiso 1 1 calc R . . H5C H 0.4630 0.2248 0.0628 0.051 Uiso 1 1 calc R . . C6 C 0.3447(4) 0.2509(9) 0.1341(3) 0.0235(14) Uani 0.720(8) 1 d P A 1 H6A H 0.2882 0.2118 0.1184 0.028 Uiso 0.720(8) 1 calc PR A 1 H6B H 0.3809 0.1521 0.1403 0.028 Uiso 0.720(8) 1 calc PR A 1 C6' C 0.3959(11) 0.304(2) 0.1648(9) 0.0235(14) Uani 0.280(8) 1 d P A 2 H6'1 H 0.4012 0.1810 0.1659 0.028 Uiso 0.280(8) 1 calc PR A 2 H6'2 H 0.4499 0.3522 0.1837 0.028 Uiso 0.280(8) 1 calc PR A 2 C7 C 0.3511(5) 0.3434(7) 0.2020(3) 0.0472(17) Uani 1 1 d . A . H7A H 0.3262 0.2761 0.2363 0.057 Uiso 1 1 calc R B 1 H7B H 0.4091 0.3600 0.2224 0.057 Uiso 1 1 calc R B 1 C8 C 0.3220(3) 0.5980(8) 0.2598(2) 0.0334(13) Uani 1 1 d . A . H8A H 0.2883 0.5476 0.2914 0.050 Uiso 1 1 calc R . . H8B H 0.3062 0.7152 0.2508 0.050 Uiso 1 1 calc R . . H8C H 0.3792 0.5925 0.2824 0.050 Uiso 1 1 calc R . . C9 C 0.1938(3) 0.9237(6) 0.1793(2) 0.0161(9) Uani 1 1 d . A . H9A H 0.1777 1.0323 0.1560 0.019 Uiso 1 1 calc R . . H9B H 0.2335 0.9463 0.2232 0.019 Uiso 1 1 calc R . . C10 C 0.1183(3) 0.8369(6) 0.1992(2) 0.0161(9) Uani 1 1 d . . . H10A H 0.1015 0.8967 0.2398 0.019 Uiso 1 1 calc R A . H10B H 0.1325 0.7207 0.2146 0.019 Uiso 1 1 calc R . . C11 C 0.0462(3) 0.8334(6) 0.1359(2) 0.0167(9) Uani 1 1 d . A . H11A H 0.0660 0.7914 0.0931 0.020 Uiso 1 1 calc R . . H11B H 0.0268 0.9495 0.1258 0.020 Uiso 1 1 calc R . . C12 C -0.0266(3) 0.7240(6) 0.1485(2) 0.0188(9) Uani 1 1 d . . . H12A H -0.0074 0.6081 0.1595 0.023 Uiso 1 1 calc R A . H12B H -0.0673 0.7208 0.1041 0.023 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 0.01046(8) 0.01223(8) 0.01039(8) 0.00027(6) 0.00187(5) 0.00080(6) I1 0.01604(14) 0.01507(15) 0.01855(15) 0.00056(11) 0.00450(11) -0.00231(11) I2 0.01539(15) 0.02139(16) 0.02271(16) 0.00010(12) -0.00337(11) -0.00188(12) I3 0.03034(17) 0.02161(17) 0.01422(15) -0.00172(11) 0.00578(12) 0.00492(13) I4 0.01864(15) 0.01976(16) 0.02279(16) -0.00283(12) 0.00819(12) -0.00244(12) O1 0.0152(15) 0.0138(16) 0.0144(15) 0.0021(12) -0.0021(12) -0.0006(12) O2 0.0143(15) 0.0160(16) 0.0177(16) 0.0023(12) 0.0040(12) -0.0005(12) O3 0.033(2) 0.0216(19) 0.037(2) 0.0103(15) 0.0201(16) 0.0088(15) O4 0.0274(18) 0.032(2) 0.0106(16) 0.0018(14) -0.0006(13) 0.0012(15) O5 0.0116(14) 0.0178(16) 0.0128(15) -0.0036(12) 0.0022(11) 0.0014(12) C1 0.020(2) 0.019(2) 0.019(2) -0.0009(18) -0.0078(18) -0.0074(19) C2 0.018(2) 0.016(2) 0.020(2) 0.0010(18) 0.0007(18) 0.0032(18) C3 0.023(2) 0.015(2) 0.022(2) 0.0072(18) 0.0031(19) -0.0009(19) C4 0.017(2) 0.032(3) 0.024(3) 0.007(2) 0.0059(19) -0.003(2) C5 0.021(3) 0.028(3) 0.051(4) -0.006(2) 0.003(2) 0.007(2) C6 0.025(3) 0.019(3) 0.025(4) 0.005(3) 0.001(3) -0.001(3) C6' 0.025(3) 0.019(3) 0.025(4) 0.005(3) 0.001(3) -0.001(3) C7 0.084(5) 0.031(3) 0.025(3) 0.013(2) 0.005(3) 0.010(3) C8 0.035(3) 0.053(4) 0.011(2) -0.002(2) 0.001(2) 0.018(3) C9 0.021(2) 0.013(2) 0.015(2) -0.0031(17) 0.0054(17) 0.0012(18) C10 0.019(2) 0.016(2) 0.014(2) 0.0003(17) 0.0053(17) 0.0041(18) C11 0.019(2) 0.016(2) 0.015(2) 0.0013(17) 0.0035(17) 0.0014(18) C12 0.022(2) 0.016(2) 0.019(2) -0.0033(18) 0.0061(18) -0.0003(19) _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 O5 2.065(3) . ? Th1 O1 2.572(3) . ? Th1 O4 2.591(3) . ? Th1 O3 2.639(3) . ? Th1 O2 2.668(3) . ? Th1 I1 3.1481(3) . ? Th1 I2 3.1555(3) . ? Th1 I3 3.1899(4) . ? I4 C12 2.167(4) . ? O1 C2 1.431(5) . ? O1 C1 1.451(5) . ? O2 C3 1.441(5) . ? O2 C4 1.446(5) . ? O3 C5 1.432(6) . ? O3 C6 1.446(7) . ? O3 C6' 1.631(17) . ? O4 C8 1.429(5) . ? O4 C7 1.437(6) . ? O5 C9 1.427(5) . ? C2 C3 1.477(6) . ? C6 C7 1.446(9) . ? C6' C7 1.135(18) . ? C9 C10 1.513(6) . ? C10 C11 1.519(6) . ? C11 C12 1.518(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Th1 O1 75.64(10) . . ? O5 Th1 O4 76.44(11) . . ? O1 Th1 O4 136.37(10) . . ? O5 Th1 O3 137.80(11) . . ? O1 Th1 O3 139.12(10) . . ? O4 Th1 O3 61.56(10) . . ? O5 Th1 O2 82.28(10) . . ? O1 Th1 O2 62.42(9) . . ? O4 Th1 O2 143.76(10) . . ? O3 Th1 O2 130.15(9) . . ? O5 Th1 I1 91.75(8) . . ? O1 Th1 I1 72.38(7) . . ? O4 Th1 I1 75.69(7) . . ? O3 Th1 I1 82.18(8) . . ? O2 Th1 I1 134.51(6) . . ? O5 Th1 I2 88.61(8) . . ? O1 Th1 I2 136.25(7) . . ? O4 Th1 I2 75.19(7) . . ? O3 Th1 I2 77.55(8) . . ? O2 Th1 I2 75.31(6) . . ? I1 Th1 I2 149.925(9) . . ? O5 Th1 I3 149.69(8) . . ? O1 Th1 I3 76.47(6) . . ? O4 Th1 I3 133.25(7) . . ? O3 Th1 I3 72.44(8) . . ? O2 Th1 I3 74.43(6) . . ? I1 Th1 I3 90.973(9) . . ? I2 Th1 I3 103.619(9) . . ? C2 O1 C1 111.8(3) . . ? C2 O1 Th1 110.8(2) . . ? C1 O1 Th1 131.7(3) . . ? C3 O2 C4 108.9(3) . . ? C3 O2 Th1 117.5(2) . . ? C4 O2 Th1 125.8(3) . . ? C5 O3 C6 115.8(4) . . ? C5 O3 C6' 92.0(7) . . ? C6 O3 C6' 38.2(7) . . ? C5 O3 Th1 126.0(3) . . ? C6 O3 Th1 113.1(3) . . ? C6' O3 Th1 113.8(7) . . ? C8 O4 C7 110.4(4) . . ? C8 O4 Th1 124.1(3) . . ? C7 O4 Th1 120.6(3) . . ? C9 O5 Th1 174.8(3) . . ? O1 C2 C3 109.1(4) . . ? O2 C3 C2 107.7(3) . . ? C7 C6 O3 107.9(5) . . ? C7 C6' O3 114.3(13) . . ? C6' C7 O4 119.7(10) . . ? C6' C7 C6 44.6(9) . . ? O4 C7 C6 112.0(5) . . ? O5 C9 C10 111.2(3) . . ? C9 C10 C11 112.2(3) . . ? C10 C11 C12 114.6(4) . . ? C11 C12 I4 112.9(3) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.009 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.178 #==============END================= data_apx1501_hklf5 _database_code_depnum_ccdc_archive 'CCDC 880811' #TrackingRef '- REVISED DT-ART-07-2012-031676 Kiplinger_corrected.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H57 I3 N2 O2 Th' _chemical_formula_weight 1174.59 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 11.5128(11) _cell_length_b 35.767(4) _cell_length_c 20.375(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.0963(13) _cell_angle_gamma 90.00 _cell_volume 8284.6(14) _cell_formula_units_Z 8 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description slab _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 5.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4182 _exptl_absorpt_correction_T_max 0.7197 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _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 53844 _diffrn_reflns_av_R_equivalents 0.1025 _diffrn_reflns_av_sigmaI/netI 0.1523 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.01 _reflns_number_total 37831 _reflns_number_gt 22644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (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. Crystal was two component twin. Indexed with Cell_Now, integrated with APEX II, and refined with SHELXL. BASF refined to 0.4127(3). Two methylene carbons, C35 and C36, disordered over two positions. Site occupancy factors tied to one, and refined to 0.33(1). Bond distances (6) were restrained to chemically reasonable distances. Due to twinning and disorder the temperature factors on the following atoms were restrained: C20 C23 C42 C50 C53 C54 C35 C35' C36 C36' N1 C16 and N4. ; _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^)+(0.0278P)^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 37831 _refine_ls_number_parameters 851 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.846 _refine_ls_shift/su_max 0.004 _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 0.45372(2) 0.623716(7) 0.090078(14) 0.01325(7) Uani 1 1 d . . . Th2 Th 0.00679(2) 0.863877(7) 0.082329(14) 0.01375(7) Uani 1 1 d . . . I1 I 0.57968(4) 0.699801(13) 0.12431(3) 0.02804(14) Uani 1 1 d . . . I2 I 0.38485(4) 0.584293(13) -0.04695(2) 0.02208(13) Uani 1 1 d . . . I3 I 0.52758(6) 0.750265(19) 0.34318(4) 0.0745(2) Uani 1 1 d . B . I4 I 0.11619(4) 0.785414(13) 0.11936(3) 0.02482(14) Uani 1 1 d . . . I5 I -0.03013(4) 0.900384(13) -0.05782(2) 0.02360(13) Uani 1 1 d . . . I6 I 0.00798(5) 0.741305(15) 0.30835(3) 0.03340(15) Uani 1 1 d . . . N1 N 0.4396(5) 0.56232(14) 0.1403(3) 0.0108(13) Uani 1 1 d U . . N2 N 0.6540(5) 0.59603(14) 0.0953(3) 0.0147(14) Uani 1 1 d . . . N3 N 0.2146(5) 0.88670(15) 0.0933(3) 0.0149(14) Uani 1 1 d . . . N4 N 0.0013(5) 0.92710(14) 0.1260(3) 0.0130(14) Uani 1 1 d U . . O1 O 0.3243(4) 0.67035(12) 0.0202(2) 0.0182(12) Uani 1 1 d . . . O2 O 0.3447(4) 0.63758(12) 0.1579(2) 0.0212(12) Uani 1 1 d . B . O3 O -0.1395(4) 0.82100(12) 0.0145(2) 0.0194(12) Uani 1 1 d . . . O4 O -0.1057(4) 0.85435(11) 0.1504(2) 0.0183(12) Uani 1 1 d . . . C1 C 0.3538(6) 0.55689(17) 0.1856(4) 0.0171(18) Uani 1 1 d . . . C2 C 0.2332(7) 0.55428(17) 0.1602(4) 0.0196(19) Uani 1 1 d . . . C3 C 0.1551(7) 0.55125(18) 0.2064(4) 0.0217(19) Uani 1 1 d . . . H3 H 0.0747 0.5498 0.1910 0.026 Uiso 1 1 calc R . . C4 C 0.1938(7) 0.55035(19) 0.2732(4) 0.027(2) Uani 1 1 d . . . H4 H 0.1404 0.5489 0.3029 0.032 Uiso 1 1 calc R . . C5 C 0.3146(7) 0.55157(18) 0.2965(4) 0.0193(18) Uani 1 1 d . . . H5 H 0.3411 0.5508 0.3421 0.023 Uiso 1 1 calc R . . C6 C 0.3955(7) 0.55391(18) 0.2533(4) 0.0196(19) Uani 1 1 d . . . C7 C 0.1868(6) 0.55381(19) 0.0862(4) 0.025(2) Uani 1 1 d . . . H7 H 0.2546 0.5532 0.0625 0.030 Uiso 1 1 calc R . . C8 C 0.1145(6) 0.5888(2) 0.0635(4) 0.032(2) Uani 1 1 d . . . H8A H 0.0481 0.5903 0.0866 0.048 Uiso 1 1 calc R . . H8B H 0.0875 0.5874 0.0165 0.048 Uiso 1 1 calc R . . H8C H 0.1627 0.6106 0.0733 0.048 Uiso 1 1 calc R . . C9 C 0.1114(6) 0.5195(2) 0.0652(4) 0.031(2) Uani 1 1 d . . . H9A H 0.1570 0.4973 0.0766 0.047 Uiso 1 1 calc R . . H9B H 0.0856 0.5201 0.0181 0.047 Uiso 1 1 calc R . . H9C H 0.0442 0.5194 0.0878 0.047 Uiso 1 1 calc R . . C10 C 0.5260(6) 0.5552(2) 0.2816(4) 0.0234(19) Uani 1 1 d . . . H10 H 0.5690 0.5608 0.2449 0.028 Uiso 1 1 calc R . . C11 C 0.5672(7) 0.5170(2) 0.3095(5) 0.060(3) Uani 1 1 d . . . H11A H 0.5212 0.5097 0.3428 0.090 Uiso 1 1 calc R . . H11B H 0.6486 0.5184 0.3289 0.090 Uiso 1 1 calc R . . H11C H 0.5575 0.4989 0.2743 0.090 Uiso 1 1 calc R . . C12 C 0.5567(7) 0.5851(2) 0.3340(4) 0.054(3) Uani 1 1 d . . . H12A H 0.5373 0.6092 0.3148 0.081 Uiso 1 1 calc R . . H12B H 0.6393 0.5840 0.3509 0.081 Uiso 1 1 calc R . . H12C H 0.5128 0.5809 0.3697 0.081 Uiso 1 1 calc R . . C13 C 0.4886(6) 0.53167(18) 0.1168(4) 0.0197(19) Uani 1 1 d . . . C14 C 0.5878(6) 0.53200(18) 0.0884(4) 0.0199(19) Uani 1 1 d . . . H14 H 0.6032 0.5096 0.0682 0.024 Uiso 1 1 calc R . . C15 C 0.6709(6) 0.56026(19) 0.0844(3) 0.0135(17) Uani 1 1 d . . . C16 C 0.4316(6) 0.49399(18) 0.1234(4) 0.028(2) Uani 1 1 d U . . H16A H 0.3512 0.4975 0.1293 0.042 Uiso 1 1 calc R . . H16B H 0.4733 0.4810 0.1611 0.042 Uiso 1 1 calc R . . H16C H 0.4341 0.4796 0.0839 0.042 Uiso 1 1 calc R . . C17 C 0.7865(6) 0.54668(18) 0.0677(4) 0.0227(19) Uani 1 1 d . . . H17A H 0.7930 0.5538 0.0230 0.034 Uiso 1 1 calc R . . H17B H 0.7904 0.5199 0.0717 0.034 Uiso 1 1 calc R . . H17C H 0.8499 0.5577 0.0978 0.034 Uiso 1 1 calc R . . C18 C 0.7546(6) 0.62148(18) 0.0985(4) 0.0174(18) Uani 1 1 d . . . C19 C 0.7867(6) 0.63589(19) 0.0399(4) 0.0187(18) Uani 1 1 d . . . C20 C 0.8788(6) 0.66200(19) 0.0470(4) 0.0230(19) Uani 1 1 d U . . H20 H 0.9011 0.6727 0.0093 0.028 Uiso 1 1 calc R . . C21 C 0.9369(6) 0.67219(19) 0.1090(4) 0.024(2) Uani 1 1 d . . . H21 H 0.9977 0.6895 0.1122 0.029 Uiso 1 1 calc R . . C22 C 0.9061(6) 0.65701(19) 0.1663(4) 0.025(2) Uani 1 1 d . . . H22 H 0.9472 0.6636 0.2077 0.030 Uiso 1 1 calc R . . C23 C 0.8130(6) 0.63172(18) 0.1615(4) 0.0132(17) Uani 1 1 d U . . C24 C 0.7233(6) 0.6264(2) -0.0284(4) 0.025(2) Uani 1 1 d . . . H24 H 0.6657 0.6067 -0.0240 0.030 Uiso 1 1 calc R . . C25 C 0.6570(6) 0.66049(19) -0.0613(4) 0.029(2) Uani 1 1 d . . . H25A H 0.6091 0.6711 -0.0315 0.043 Uiso 1 1 calc R . . H25B H 0.6079 0.6529 -0.1016 0.043 Uiso 1 1 calc R . . H25C H 0.7125 0.6788 -0.0713 0.043 Uiso 1 1 calc R . . C26 C 0.8072(7) 0.6118(2) -0.0748(4) 0.037(2) Uani 1 1 d . . . H26A H 0.8631 0.6310 -0.0807 0.055 Uiso 1 1 calc R . . H26B H 0.7626 0.6053 -0.1171 0.055 Uiso 1 1 calc R . . H26C H 0.8481 0.5901 -0.0553 0.055 Uiso 1 1 calc R . . C27 C 0.7762(6) 0.61647(18) 0.2254(4) 0.0214(19) Uani 1 1 d . . . H27 H 0.6927 0.6100 0.2150 0.026 Uiso 1 1 calc R . . C28 C 0.8430(6) 0.58043(19) 0.2484(4) 0.030(2) Uani 1 1 d . . . H28A H 0.8217 0.5611 0.2160 0.045 Uiso 1 1 calc R . . H28B H 0.8229 0.5727 0.2903 0.045 Uiso 1 1 calc R . . H28C H 0.9261 0.5849 0.2533 0.045 Uiso 1 1 calc R . . C29 C 0.7886(6) 0.64544(18) 0.2815(3) 0.028(2) Uani 1 1 d . . . H29A H 0.8702 0.6514 0.2948 0.042 Uiso 1 1 calc R . . H29B H 0.7572 0.6354 0.3187 0.042 Uiso 1 1 calc R . . H29C H 0.7461 0.6677 0.2661 0.042 Uiso 1 1 calc R . . C30 C 0.3498(6) 0.6878(2) -0.0398(4) 0.027(2) Uani 1 1 d . . . H30A H 0.3836 0.6699 -0.0672 0.033 Uiso 1 1 calc R . . H30B H 0.4043 0.7084 -0.0294 0.033 Uiso 1 1 calc R . . C31 C 0.2338(7) 0.7015(2) -0.0746(4) 0.045(3) Uani 1 1 d . . . H31A H 0.2031 0.6848 -0.1106 0.054 Uiso 1 1 calc R . . H31B H 0.2419 0.7263 -0.0928 0.054 Uiso 1 1 calc R . . C32 C 0.1519(7) 0.7026(2) -0.0227(4) 0.047(3) Uani 1 1 d . . . H32A H 0.1175 0.7272 -0.0204 0.057 Uiso 1 1 calc R . . H32B H 0.0894 0.6843 -0.0325 0.057 Uiso 1 1 calc R . . C33 C 0.2324(7) 0.6932(2) 0.0413(4) 0.036(2) Uani 1 1 d . . . H33A H 0.2651 0.7157 0.0635 0.044 Uiso 1 1 calc R . . H33B H 0.1905 0.6794 0.0712 0.044 Uiso 1 1 calc R . . C34 C 0.2711(7) 0.64353(18) 0.2061(4) 0.030(2) Uani 1 1 d D . . H34A H 0.2651 0.6208 0.2314 0.036 Uiso 1 1 calc R A 1 H34B H 0.1929 0.6506 0.1848 0.036 Uiso 1 1 calc R A 1 C35 C 0.326(2) 0.6752(5) 0.2524(11) 0.025(7) Uani 0.328(14) 1 d PDU B 1 H35A H 0.2863 0.6761 0.2908 0.030 Uiso 0.328(14) 1 calc PR B 1 H35B H 0.4080 0.6688 0.2683 0.030 Uiso 0.328(14) 1 calc PR B 1 C36 C 0.3231(19) 0.7129(5) 0.2227(9) 0.020(7) Uani 0.328(14) 1 d PDU B 1 H36A H 0.3684 0.7134 0.1864 0.024 Uiso 0.328(14) 1 calc PR B 1 H36B H 0.2427 0.7199 0.2055 0.024 Uiso 0.328(14) 1 calc PR B 1 C35' C 0.2631(11) 0.6838(3) 0.2243(6) 0.034(4) Uani 0.672(14) 1 d PDU B 2 H35C H 0.2526 0.6992 0.1845 0.041 Uiso 0.672(14) 1 calc PR B 2 H35D H 0.1965 0.6878 0.2472 0.041 Uiso 0.672(14) 1 calc PR B 2 C36' C 0.3749(10) 0.6941(3) 0.2684(6) 0.029(4) Uani 0.672(14) 1 d PDU B 2 H36C H 0.4425 0.6860 0.2491 0.035 Uiso 0.672(14) 1 calc PR B 2 H36D H 0.3784 0.6826 0.3118 0.035 Uiso 0.672(14) 1 calc PR B 2 C37 C 0.3729(8) 0.7386(3) 0.2744(5) 0.075(4) Uani 1 1 d D . . H37A H 0.3141 0.7379 0.3036 0.090 Uiso 1 1 calc R B 1 H37B H 0.3601 0.7624 0.2514 0.090 Uiso 1 1 calc R B 1 C38 C 0.3120(6) 0.85973(18) 0.1013(4) 0.0154(17) Uani 1 1 d . . . C39 C 0.3379(6) 0.84088(19) 0.0453(4) 0.022(2) Uani 1 1 d . . . C40 C 0.4274(7) 0.8145(2) 0.0551(4) 0.029(2) Uani 1 1 d . . . H40 H 0.4459 0.8016 0.0185 0.035 Uiso 1 1 calc R . . C41 C 0.4888(6) 0.8067(2) 0.1160(5) 0.031(2) Uani 1 1 d . . . H41 H 0.5471 0.7885 0.1209 0.037 Uiso 1 1 calc R . . C42 C 0.4636(6) 0.8264(2) 0.1712(4) 0.027(2) Uani 1 1 d U . . H42 H 0.5068 0.8216 0.2129 0.032 Uiso 1 1 calc R . . C43 C 0.3745(6) 0.85317(18) 0.1647(4) 0.0169(18) Uani 1 1 d . . . C44 C 0.2732(8) 0.8474(3) -0.0230(5) 0.054(3) Uani 1 1 d . . . H44 H 0.2046 0.8629 -0.0188 0.065 Uiso 1 1 calc R . . C45 C 0.3458(12) 0.8685(3) -0.0668(5) 0.124(6) Uani 1 1 d . . . H45A H 0.3763 0.8910 -0.0447 0.187 Uiso 1 1 calc R . . H45B H 0.2973 0.8748 -0.1081 0.187 Uiso 1 1 calc R . . H45C H 0.4099 0.8531 -0.0755 0.187 Uiso 1 1 calc R . . C46 C 0.2289(8) 0.8128(3) -0.0599(4) 0.074(4) Uani 1 1 d . . . H46A H 0.2940 0.7990 -0.0717 0.111 Uiso 1 1 calc R . . H46B H 0.1761 0.8195 -0.0994 0.111 Uiso 1 1 calc R . . H46C H 0.1880 0.7976 -0.0321 0.111 Uiso 1 1 calc R . . C47 C 0.3497(7) 0.8739(2) 0.2256(4) 0.039(2) Uani 1 1 d . . . H47 H 0.2796 0.8894 0.2121 0.047 Uiso 1 1 calc R . . C48 C 0.4482(10) 0.8997(3) 0.2550(5) 0.085(4) Uani 1 1 d . . . H48A H 0.5191 0.8855 0.2671 0.127 Uiso 1 1 calc R . . H48B H 0.4279 0.9117 0.2937 0.127 Uiso 1 1 calc R . . H48C H 0.4604 0.9183 0.2227 0.127 Uiso 1 1 calc R . . C49 C 0.3225(8) 0.8474(2) 0.2794(4) 0.058(3) Uani 1 1 d . . . H49A H 0.2520 0.8336 0.2634 0.086 Uiso 1 1 calc R . . H49B H 0.3114 0.8614 0.3181 0.086 Uiso 1 1 calc R . . H49C H 0.3867 0.8303 0.2908 0.086 Uiso 1 1 calc R . . C50 C 0.2441(6) 0.92225(19) 0.0831(3) 0.0160(18) Uani 1 1 d U . . C51 C 0.1672(6) 0.95251(18) 0.0840(3) 0.0178(18) Uani 1 1 d . . . H51 H 0.1923 0.9742 0.0654 0.021 Uiso 1 1 calc R . . C52 C 0.0627(6) 0.95633(18) 0.1068(4) 0.0172(18) Uani 1 1 d . . . C53 C 0.3677(6) 0.93257(18) 0.0720(4) 0.0227(19) Uani 1 1 d U . . H53A H 0.4176 0.9354 0.1142 0.034 Uiso 1 1 calc R . . H53B H 0.3653 0.9556 0.0478 0.034 Uiso 1 1 calc R . . H53C H 0.3983 0.9131 0.0471 0.034 Uiso 1 1 calc R . . C54 C 0.0173(6) 0.99558(17) 0.1134(4) 0.029(2) Uani 1 1 d U . . H54A H -0.0539 0.9991 0.0825 0.043 Uiso 1 1 calc R . . H54B H 0.0753 1.0133 0.1041 0.043 Uiso 1 1 calc R . . H54C H 0.0017 0.9994 0.1579 0.043 Uiso 1 1 calc R . . C55 C -0.0906(7) 0.93662(18) 0.1653(4) 0.024(2) Uani 1 1 d . . . C56 C -0.2066(7) 0.94240(18) 0.1345(4) 0.023(2) Uani 1 1 d . . . C57 C -0.2894(7) 0.9503(2) 0.1740(4) 0.030(2) Uani 1 1 d . . . H57 H -0.3664 0.9546 0.1537 0.036 Uiso 1 1 calc R . . C58 C -0.2638(7) 0.9520(2) 0.2425(4) 0.031(2) Uani 1 1 d . . . H58 H -0.3225 0.9564 0.2681 0.037 Uiso 1 1 calc R . . C59 C -0.1468(7) 0.94699(19) 0.2722(4) 0.030(2) Uani 1 1 d . . . H59 H -0.1269 0.9495 0.3180 0.036 Uiso 1 1 calc R . . C60 C -0.0591(7) 0.93836(18) 0.2345(4) 0.0187(18) Uani 1 1 d . . . C61 C -0.2439(6) 0.94137(19) 0.0603(4) 0.0217(19) Uani 1 1 d . . . H61 H -0.1720 0.9409 0.0403 0.026 Uiso 1 1 calc R . . C62 C -0.3129(7) 0.9054(2) 0.0381(4) 0.037(2) Uani 1 1 d . . . H62A H -0.2688 0.8841 0.0564 0.056 Uiso 1 1 calc R . . H62B H -0.3255 0.9039 -0.0095 0.056 Uiso 1 1 calc R . . H62C H -0.3874 0.9059 0.0536 0.056 Uiso 1 1 calc R . . C63 C -0.3148(7) 0.9760(2) 0.0322(4) 0.043(3) Uani 1 1 d . . . H63A H -0.3883 0.9766 0.0489 0.065 Uiso 1 1 calc R . . H63B H -0.3296 0.9746 -0.0154 0.065 Uiso 1 1 calc R . . H63C H -0.2708 0.9982 0.0458 0.065 Uiso 1 1 calc R . . C64 C 0.0652(7) 0.9317(2) 0.2700(4) 0.031(2) Uani 1 1 d . . . H64 H 0.1113 0.9221 0.2372 0.037 Uiso 1 1 calc R . . C65 C 0.1242(8) 0.9669(2) 0.2987(5) 0.089(4) Uani 1 1 d . . . H65A H 0.0798 0.9774 0.3303 0.133 Uiso 1 1 calc R . . H65B H 0.1283 0.9845 0.2637 0.133 Uiso 1 1 calc R . . H65C H 0.2023 0.9611 0.3206 0.133 Uiso 1 1 calc R . . C66 C 0.0697(7) 0.9029(2) 0.3243(5) 0.070(4) Uani 1 1 d . . . H66A H 0.1500 0.8962 0.3401 0.105 Uiso 1 1 calc R . . H66B H 0.0269 0.8810 0.3071 0.105 Uiso 1 1 calc R . . H66C H 0.0349 0.9129 0.3603 0.105 Uiso 1 1 calc R . . C67 C -0.1136(7) 0.80087(19) -0.0431(4) 0.032(2) Uani 1 1 d . . . H67A H -0.0293 0.7996 -0.0426 0.038 Uiso 1 1 calc R . . H67B H -0.1492 0.8133 -0.0836 0.038 Uiso 1 1 calc R . . C68 C -0.1628(8) 0.7630(2) -0.0396(5) 0.059(3) Uani 1 1 d . . . H68A H -0.1008 0.7449 -0.0261 0.071 Uiso 1 1 calc R . . H68B H -0.2061 0.7556 -0.0824 0.071 Uiso 1 1 calc R . . C69 C -0.2445(9) 0.7657(2) 0.0122(5) 0.070(4) Uani 1 1 d . . . H69A H -0.3223 0.7565 -0.0057 0.084 Uiso 1 1 calc R . . H69B H -0.2139 0.7512 0.0514 0.084 Uiso 1 1 calc R . . C70 C -0.2490(7) 0.8052(2) 0.0285(4) 0.038(2) Uani 1 1 d . . . H70A H -0.2558 0.8085 0.0750 0.046 Uiso 1 1 calc R . . H70B H -0.3157 0.8172 0.0016 0.046 Uiso 1 1 calc R . . C71 C -0.1875(6) 0.85218(18) 0.1959(4) 0.023(2) Uani 1 1 d . . . H71A H -0.2665 0.8501 0.1712 0.028 Uiso 1 1 calc R . . H71B H -0.1835 0.8750 0.2218 0.028 Uiso 1 1 calc R . . C72 C -0.1633(6) 0.81887(18) 0.2429(4) 0.0232(19) Uani 1 1 d . . . H72A H -0.2172 0.8197 0.2750 0.028 Uiso 1 1 calc R . . H72B H -0.0840 0.8209 0.2672 0.028 Uiso 1 1 calc R . . C73 C -0.1764(6) 0.78118(18) 0.2070(4) 0.025(2) Uani 1 1 d . . . H73A H -0.2529 0.7804 0.1791 0.029 Uiso 1 1 calc R . . H73B H -0.1174 0.7796 0.1780 0.029 Uiso 1 1 calc R . . C74 C -0.1647(6) 0.74761(19) 0.2516(4) 0.027(2) Uani 1 1 d . . . H74A H -0.1837 0.7254 0.2248 0.033 Uiso 1 1 calc R . . H74B H -0.2215 0.7496 0.2820 0.033 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 0.01353(16) 0.01168(14) 0.01453(17) 0.00086(12) 0.00222(12) 0.00243(12) Th2 0.01453(16) 0.01175(14) 0.01527(18) -0.00045(12) 0.00325(12) -0.00139(12) I1 0.0242(3) 0.0156(3) 0.0419(4) -0.0035(2) -0.0020(3) -0.0003(2) I2 0.0269(3) 0.0220(3) 0.0160(3) -0.0029(2) -0.0007(2) 0.0044(2) I3 0.0522(5) 0.0573(5) 0.1203(7) -0.0269(4) 0.0330(5) -0.0084(4) I4 0.0224(3) 0.0160(3) 0.0375(4) 0.0047(2) 0.0092(3) 0.0023(2) I5 0.0294(3) 0.0221(3) 0.0178(3) 0.0029(2) -0.0011(2) -0.0016(2) I6 0.0289(4) 0.0366(3) 0.0330(4) 0.0066(3) -0.0003(3) -0.0032(3) N1 0.012(3) 0.013(3) 0.009(3) -0.005(2) 0.005(2) 0.005(2) N2 0.013(4) 0.013(3) 0.019(4) 0.001(3) 0.008(3) 0.001(3) N3 0.017(4) 0.015(3) 0.013(4) -0.001(3) 0.005(3) 0.001(3) N4 0.013(2) 0.013(2) 0.014(2) 0.0026(18) 0.0057(19) -0.0064(18) O1 0.014(3) 0.016(3) 0.025(3) 0.009(2) 0.006(2) 0.006(2) O2 0.033(3) 0.014(3) 0.020(3) 0.007(2) 0.015(3) 0.005(2) O3 0.025(3) 0.013(3) 0.021(3) -0.002(2) 0.008(3) -0.008(2) O4 0.027(3) 0.014(3) 0.014(3) -0.006(2) 0.006(3) -0.005(2) C1 0.014(5) 0.012(4) 0.026(5) 0.001(3) 0.008(4) 0.002(3) C2 0.022(5) 0.006(4) 0.031(6) -0.002(3) 0.006(4) -0.001(3) C3 0.023(5) 0.019(4) 0.025(5) 0.001(4) 0.007(4) -0.003(3) C4 0.028(5) 0.024(5) 0.034(6) 0.000(4) 0.026(4) -0.003(4) C5 0.026(5) 0.018(4) 0.016(5) -0.001(3) 0.009(4) -0.008(3) C6 0.026(5) 0.013(4) 0.019(5) 0.001(3) 0.001(4) 0.006(3) C7 0.009(4) 0.028(5) 0.038(6) -0.004(4) 0.003(4) -0.004(3) C8 0.032(5) 0.040(5) 0.018(5) 0.006(4) -0.014(4) -0.004(4) C9 0.026(5) 0.040(5) 0.030(6) -0.015(4) 0.009(4) -0.011(4) C10 0.019(5) 0.034(5) 0.016(5) 0.005(4) -0.001(4) 0.001(4) C11 0.041(7) 0.053(7) 0.080(9) 0.031(6) -0.009(6) 0.005(5) C12 0.039(6) 0.072(7) 0.048(7) -0.019(5) 0.000(5) -0.009(5) C13 0.023(5) 0.012(4) 0.025(5) 0.003(3) 0.005(4) 0.002(3) C14 0.022(5) 0.009(4) 0.027(5) -0.004(3) 0.001(4) 0.006(3) C15 0.014(4) 0.020(4) 0.006(4) 0.003(3) -0.001(3) 0.006(3) C16 0.029(4) 0.019(4) 0.043(5) 0.000(3) 0.025(4) -0.004(3) C17 0.021(5) 0.022(4) 0.027(5) 0.004(4) 0.009(4) 0.000(3) C18 0.013(4) 0.013(4) 0.025(5) -0.003(3) -0.003(4) 0.001(3) C19 0.012(4) 0.021(4) 0.025(5) -0.003(4) 0.010(4) 0.002(3) C20 0.009(4) 0.025(4) 0.038(5) 0.006(4) 0.013(4) -0.004(3) C21 0.015(5) 0.020(4) 0.040(6) -0.008(4) 0.014(4) -0.010(3) C22 0.015(5) 0.023(5) 0.036(6) 0.001(4) 0.006(4) -0.001(3) C23 0.004(4) 0.016(4) 0.020(4) 0.004(3) 0.004(3) 0.005(3) C24 0.020(5) 0.027(5) 0.025(5) 0.003(4) -0.002(4) -0.003(4) C25 0.025(5) 0.029(5) 0.034(6) 0.004(4) 0.005(4) 0.005(4) C26 0.034(6) 0.039(5) 0.038(6) 0.003(4) 0.010(5) 0.012(4) C27 0.020(5) 0.021(4) 0.020(5) -0.003(3) -0.007(4) 0.001(3) C28 0.034(5) 0.030(5) 0.027(6) 0.001(4) 0.007(4) 0.015(4) C29 0.043(6) 0.020(4) 0.018(5) 0.007(3) -0.004(4) 0.003(4) C30 0.026(5) 0.034(5) 0.023(5) 0.012(4) 0.011(4) 0.013(4) C31 0.024(6) 0.058(6) 0.055(7) 0.014(5) 0.017(5) 0.026(5) C32 0.028(6) 0.062(7) 0.054(7) 0.002(5) 0.015(5) 0.029(5) C33 0.041(6) 0.043(6) 0.027(6) 0.002(4) 0.012(5) 0.021(4) C34 0.041(6) 0.012(4) 0.044(6) -0.007(4) 0.031(5) -0.007(4) C35 0.027(11) 0.020(10) 0.027(11) 0.006(8) 0.004(8) 0.006(8) C36 0.020(10) 0.019(10) 0.021(10) 0.001(7) 0.004(8) 0.001(7) C35' 0.040(7) 0.023(7) 0.038(8) -0.005(5) 0.004(6) 0.001(5) C36' 0.034(7) 0.031(7) 0.024(7) -0.013(5) 0.006(5) 0.006(5) C37 0.086(9) 0.084(8) 0.064(8) -0.048(6) 0.040(7) -0.071(7) C38 0.009(4) 0.011(4) 0.026(5) 0.001(3) 0.003(4) -0.007(3) C39 0.012(5) 0.024(5) 0.027(6) -0.007(4) -0.006(4) 0.005(3) C40 0.031(5) 0.034(5) 0.024(6) -0.016(4) 0.010(4) -0.001(4) C41 0.011(5) 0.020(5) 0.061(7) 0.003(4) 0.003(5) -0.004(3) C42 0.012(4) 0.035(5) 0.032(5) 0.006(4) 0.002(4) -0.002(3) C43 0.012(4) 0.019(4) 0.019(5) -0.005(3) 0.002(4) -0.002(3) C44 0.039(7) 0.084(8) 0.036(7) -0.025(6) -0.003(5) 0.036(6) C45 0.293(18) 0.040(7) 0.021(7) 0.003(5) -0.032(9) -0.049(9) C46 0.059(8) 0.139(11) 0.024(7) -0.013(6) 0.009(5) -0.061(7) C47 0.042(6) 0.055(6) 0.019(6) 0.001(5) 0.003(4) 0.024(5) C48 0.164(12) 0.058(7) 0.042(8) -0.024(6) 0.045(8) -0.051(8) C49 0.073(8) 0.072(7) 0.030(7) -0.024(5) 0.018(6) -0.045(6) C50 0.020(4) 0.021(4) 0.007(4) -0.002(3) 0.000(3) 0.004(3) C51 0.020(5) 0.016(4) 0.020(5) -0.002(3) 0.009(4) -0.007(3) C52 0.023(5) 0.011(4) 0.021(5) 0.002(3) 0.012(4) 0.000(3) C53 0.017(4) 0.022(4) 0.031(5) -0.006(3) 0.010(4) 0.001(3) C54 0.034(5) 0.008(4) 0.048(6) 0.006(4) 0.021(4) -0.002(3) C55 0.030(5) 0.007(4) 0.034(6) -0.002(3) 0.003(4) 0.004(3) C56 0.032(5) 0.014(4) 0.026(5) 0.005(3) 0.015(4) -0.004(4) C57 0.023(5) 0.030(5) 0.040(6) -0.002(4) 0.012(4) 0.016(4) C58 0.034(6) 0.030(5) 0.034(6) -0.004(4) 0.020(5) 0.011(4) C59 0.039(6) 0.018(5) 0.034(6) -0.011(4) 0.006(5) 0.003(4) C60 0.023(5) 0.009(4) 0.028(5) 0.001(3) 0.017(4) -0.001(3) C61 0.010(4) 0.027(5) 0.030(6) 0.004(4) 0.011(4) 0.010(3) C62 0.034(6) 0.036(5) 0.037(6) 0.002(4) -0.009(5) 0.006(4) C63 0.041(6) 0.045(6) 0.046(7) 0.030(5) 0.013(5) 0.011(4) C64 0.028(5) 0.043(6) 0.020(5) -0.006(4) 0.000(4) 0.001(4) C65 0.060(8) 0.050(7) 0.141(12) -0.005(7) -0.029(8) -0.021(6) C66 0.042(7) 0.063(7) 0.092(10) 0.035(6) -0.028(6) -0.016(5) C67 0.038(6) 0.022(5) 0.036(6) -0.014(4) 0.009(4) -0.009(4) C68 0.048(7) 0.049(7) 0.088(9) -0.021(6) 0.032(6) -0.033(5) C69 0.090(9) 0.038(6) 0.098(9) -0.033(6) 0.065(7) -0.047(6) C70 0.031(6) 0.047(6) 0.039(6) -0.014(5) 0.014(5) -0.019(4) C71 0.031(5) 0.015(4) 0.027(5) -0.002(3) 0.014(4) 0.007(3) C72 0.024(5) 0.018(4) 0.034(6) 0.000(4) 0.022(4) -0.002(3) C73 0.024(5) 0.021(4) 0.024(5) -0.002(4) -0.009(4) -0.005(3) C74 0.018(5) 0.021(4) 0.044(6) 0.006(4) 0.007(4) 0.000(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 O2 2.069(5) . ? Th1 N1 2.439(5) . ? Th1 N2 2.496(5) . ? Th1 O1 2.522(4) . ? Th1 I1 3.1105(6) . ? Th1 I2 3.1164(6) . ? Th2 O4 2.070(5) . ? Th2 N4 2.434(5) . ? Th2 N3 2.504(5) . ? Th2 O3 2.522(4) . ? Th2 I5 3.1074(6) . ? Th2 I4 3.1195(6) . ? I3 C37 2.126(9) . ? I6 C74 2.148(7) . ? N1 C13 1.355(8) . ? N1 C1 1.468(8) . ? N2 C15 1.319(8) . ? N2 C18 1.467(8) . ? N3 C50 1.341(8) . ? N3 C38 1.468(8) . ? N4 C52 1.354(8) . ? N4 C55 1.464(9) . ? O1 C30 1.444(8) . ? O1 C33 1.455(8) . ? O2 C34 1.410(7) . ? O3 C67 1.448(8) . ? O3 C70 1.450(8) . ? O4 C71 1.425(7) . ? C1 C6 1.391(9) . ? C1 C2 1.406(9) . ? C2 C3 1.404(9) . ? C2 C7 1.519(10) . ? C3 C4 1.365(9) . ? C4 C5 1.397(9) . ? C5 C6 1.382(9) . ? C6 C10 1.523(9) . ? C7 C9 1.526(9) . ? C7 C8 1.533(9) . ? C10 C12 1.513(10) . ? C10 C11 1.524(9) . ? C13 C14 1.359(9) . ? C13 C16 1.514(8) . ? C14 C15 1.404(9) . ? C15 C17 1.505(9) . ? C18 C23 1.399(9) . ? C18 C19 1.402(9) . ? C19 C20 1.403(9) . ? C19 C24 1.505(9) . ? C20 C21 1.381(9) . ? C21 C22 1.383(9) . ? C22 C23 1.394(9) . ? C23 C27 1.533(9) . ? C24 C25 1.535(9) . ? C24 C26 1.545(9) . ? C27 C29 1.533(9) . ? C27 C28 1.536(9) . ? C30 C31 1.491(9) . ? C31 C32 1.524(10) . ? C32 C33 1.513(10) . ? C34 C35' 1.495(10) . ? C34 C35 1.546(16) . ? C35 C36 1.476(17) . ? C36 C37 1.447(15) . ? C35' C36' 1.495(13) . ? C36' C37 1.598(11) . ? C38 C43 1.395(9) . ? C38 C39 1.398(9) . ? C39 C40 1.388(9) . ? C39 C44 1.490(10) . ? C40 C41 1.356(10) . ? C41 C42 1.397(10) . ? C42 C43 1.393(9) . ? C43 C47 1.512(10) . ? C44 C46 1.496(11) . ? C44 C45 1.517(13) . ? C47 C48 1.510(11) . ? C47 C49 1.520(10) . ? C50 C51 1.400(9) . ? C50 C53 1.521(9) . ? C51 C52 1.363(9) . ? C52 C54 1.511(8) . ? C55 C56 1.398(10) . ? C55 C60 1.401(10) . ? C56 C57 1.371(9) . ? C56 C61 1.505(10) . ? C57 C58 1.382(10) . ? C58 C59 1.398(10) . ? C59 C60 1.397(9) . ? C60 C64 1.517(10) . ? C61 C63 1.542(9) . ? C61 C62 1.541(9) . ? C64 C65 1.503(10) . ? C64 C66 1.508(10) . ? C67 C68 1.475(9) . ? C68 C69 1.523(10) . ? C69 C70 1.454(10) . ? C71 C72 1.526(9) . ? C72 C73 1.530(9) . ? C73 C74 1.499(9) . ? 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 N1 81.24(17) . . ? O2 Th1 N2 136.10(18) . . ? N1 Th1 N2 75.38(17) . . ? O2 Th1 O1 81.49(16) . . ? N1 Th1 O1 139.43(16) . . ? N2 Th1 O1 138.23(16) . . ? O2 Th1 I1 87.19(12) . . ? N1 Th1 I1 138.89(12) . . ? N2 Th1 I1 86.71(12) . . ? O1 Th1 I1 76.17(10) . . ? O2 Th1 I2 127.71(13) . . ? N1 Th1 I2 86.79(12) . . ? N2 Th1 I2 87.77(13) . . ? O1 Th1 I2 75.49(11) . . ? I1 Th1 I2 129.816(17) . . ? O4 Th2 N4 81.55(17) . . ? O4 Th2 N3 133.15(18) . . ? N4 Th2 N3 75.19(18) . . ? O4 Th2 O3 80.36(16) . . ? N4 Th2 O3 135.33(17) . . ? N3 Th2 O3 142.46(17) . . ? O4 Th2 I5 132.51(13) . . ? N4 Th2 I5 86.42(13) . . ? N3 Th2 I5 86.28(13) . . ? O3 Th2 I5 76.69(10) . . ? O4 Th2 I4 87.78(12) . . ? N4 Th2 I4 141.29(13) . . ? N3 Th2 I4 85.88(12) . . ? O3 Th2 I4 78.14(10) . . ? I5 Th2 I4 126.276(16) . . ? C13 N1 C1 118.3(6) . . ? C13 N1 Th1 121.4(5) . . ? C1 N1 Th1 118.6(4) . . ? C15 N2 C18 118.2(6) . . ? C15 N2 Th1 122.5(4) . . ? C18 N2 Th1 118.3(4) . . ? C50 N3 C38 115.6(6) . . ? C50 N3 Th2 123.9(4) . . ? C38 N3 Th2 119.8(4) . . ? C52 N4 C55 115.7(6) . . ? C52 N4 Th2 124.6(5) . . ? C55 N4 Th2 118.6(4) . . ? C30 O1 C33 105.1(5) . . ? C30 O1 Th1 125.7(4) . . ? C33 O1 Th1 126.7(4) . . ? C34 O2 Th1 174.7(4) . . ? C67 O3 C70 105.2(5) . . ? C67 O3 Th2 122.8(4) . . ? C70 O3 Th2 130.9(4) . . ? C71 O4 Th2 173.3(4) . . ? C6 C1 C2 121.7(7) . . ? C6 C1 N1 118.2(6) . . ? C2 C1 N1 120.1(7) . . ? C3 C2 C1 117.3(7) . . ? C3 C2 C7 120.2(7) . . ? C1 C2 C7 122.5(7) . . ? C4 C3 C2 121.8(7) . . ? C3 C4 C5 119.3(7) . . ? C6 C5 C4 121.3(8) . . ? C5 C6 C1 118.4(7) . . ? C5 C6 C10 119.0(7) . . ? C1 C6 C10 122.6(7) . . ? C2 C7 C9 112.5(6) . . ? C2 C7 C8 112.2(6) . . ? C9 C7 C8 108.4(6) . . ? C12 C10 C6 113.2(6) . . ? C12 C10 C11 110.2(7) . . ? C6 C10 C11 110.1(6) . . ? N1 C13 C14 124.6(6) . . ? N1 C13 C16 118.6(7) . . ? C14 C13 C16 116.8(6) . . ? C13 C14 C15 131.2(7) . . ? N2 C15 C14 124.6(7) . . ? N2 C15 C17 120.7(6) . . ? C14 C15 C17 114.6(6) . . ? C23 C18 C19 122.1(7) . . ? C23 C18 N2 117.7(6) . . ? C19 C18 N2 120.2(6) . . ? C20 C19 C18 116.9(7) . . ? C20 C19 C24 119.6(7) . . ? C18 C19 C24 123.3(6) . . ? C21 C20 C19 121.3(7) . . ? C20 C21 C22 121.1(7) . . ? C21 C22 C23 119.5(7) . . ? C22 C23 C18 119.1(7) . . ? C22 C23 C27 118.9(6) . . ? C18 C23 C27 121.9(6) . . ? C19 C24 C25 111.0(6) . . ? C19 C24 C26 112.5(6) . . ? C25 C24 C26 108.5(6) . . ? C29 C27 C23 112.8(6) . . ? C29 C27 C28 110.9(6) . . ? C23 C27 C28 111.5(6) . . ? O1 C30 C31 104.9(6) . . ? C30 C31 C32 106.5(7) . . ? C33 C32 C31 103.3(7) . . ? O1 C33 C32 104.2(6) . . ? O2 C34 C35' 112.7(7) . . ? O2 C34 C35 107.5(11) . . ? C35' C34 C35 34.7(8) . . ? C36 C35 C34 115.9(15) . . ? C37 C36 C35 107.5(14) . . ? C36' C35' C34 107.8(9) . . ? C35' C36' C37 105.7(8) . . ? C36 C37 C36' 47.1(8) . . ? C36 C37 I3 143.0(11) . . ? C36' C37 I3 103.0(7) . . ? C43 C38 C39 122.0(7) . . ? C43 C38 N3 119.1(6) . . ? C39 C38 N3 118.9(6) . . ? C40 C39 C38 117.4(7) . . ? C40 C39 C44 119.4(7) . . ? C38 C39 C44 123.2(7) . . ? C41 C40 C39 122.6(8) . . ? C40 C41 C42 119.3(7) . . ? C43 C42 C41 120.9(7) . . ? C42 C43 C38 117.9(7) . . ? C42 C43 C47 119.4(7) . . ? C38 C43 C47 122.7(7) . . ? C39 C44 C46 114.8(8) . . ? C39 C44 C45 112.8(8) . . ? C46 C44 C45 107.1(8) . . ? C48 C47 C43 113.4(7) . . ? C48 C47 C49 108.9(7) . . ? C43 C47 C49 111.9(7) . . ? N3 C50 C51 123.7(7) . . ? N3 C50 C53 121.3(6) . . ? C51 C50 C53 115.0(6) . . ? C52 C51 C50 132.5(7) . . ? N4 C52 C51 123.4(6) . . ? N4 C52 C54 119.2(6) . . ? C51 C52 C54 117.4(6) . . ? C56 C55 C60 121.5(8) . . ? C56 C55 N4 120.7(7) . . ? C60 C55 N4 117.8(7) . . ? C57 C56 C55 118.1(8) . . ? C57 C56 C61 118.7(7) . . ? C55 C56 C61 123.2(7) . . ? C56 C57 C58 123.0(8) . . ? C57 C58 C59 117.9(8) . . ? C58 C59 C60 121.5(8) . . ? C59 C60 C55 118.0(7) . . ? C59 C60 C64 118.8(7) . . ? C55 C60 C64 123.3(7) . . ? C56 C61 C63 113.8(6) . . ? C56 C61 C62 111.6(6) . . ? C63 C61 C62 110.0(6) . . ? C65 C64 C66 109.1(8) . . ? C65 C64 C60 112.9(7) . . ? C66 C64 C60 112.2(7) . . ? O3 C67 C68 106.7(7) . . ? C67 C68 C69 105.0(7) . . ? C70 C69 C68 105.6(7) . . ? C69 C70 O3 105.7(7) . . ? O4 C71 C72 112.2(5) . . ? C71 C72 C73 113.1(6) . . ? C74 C73 C72 115.0(6) . . ? C73 C74 I6 113.4(5) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.592 _refine_diff_density_min -2.799 _refine_diff_density_rms 0.205 #==============END=====================