# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Trevor W Hayton' _publ_contact_author_email hayton@chem.ucsb.edu _publ_section_title ; Reactivity of UH3 with Mild Oxidants ; loop_ _publ_author_name 'David D. Schnaars' 'Guang Wu.' 'Trevor W. Hayton' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 690032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; uranium(IV)tetraiodobis(diethyl ether) ; _chemical_name_common 'uranium(IV)tetraiodobis(diethyl ether)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 I4 O2 U' _chemical_formula_weight 893.87 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' 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' U U -9.6767 9.6646 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/acd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 12.912(3) _cell_length_b 12.912 _cell_length_c 22.993(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3833.4(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Deep_Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 14.898 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.086 _exptl_absorpt_correction_T_max 0.413 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4546 _diffrn_reflns_av_R_equivalents 0.1406 _diffrn_reflns_av_sigmaI/netI 0.1234 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.37 _reflns_number_total 937 _reflns_number_gt 516 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Because of the significant absorption (mu > 10mm^-1) due to the presence of heavy atoms, the empirical absorption correction based on psi-scan may not perfectly correct for the absorption effect. This probably results in the relatively high Rint value. ; _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^)+(0.0166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000077(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 937 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 0.828 _refine_ls_restrained_S_all 0.828 _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 U1 U 0.5000 0.2500 0.8750 0.0228(3) Uani 1 4 d S . . I1 I 0.40203(7) 0.37828(8) 0.96666(4) 0.0344(3) Uani 1 1 d . . . C2 C 0.1903(10) 0.1601(11) 0.9027(7) 0.039(4) Uani 1 1 d . . . H2A H 0.2031 0.2300 0.8903 0.059 Uiso 1 1 calc R . . H2B H 0.1444 0.1605 0.9355 0.059 Uiso 1 1 calc R . . H2C H 0.1592 0.1220 0.8714 0.059 Uiso 1 1 calc R . . C1 C 0.2921(10) 0.1093(10) 0.9197(6) 0.031(4) Uani 1 1 d . . . H1A H 0.3173 0.1405 0.9554 0.037 Uiso 1 1 calc R . . H1B H 0.2802 0.0363 0.9272 0.037 Uiso 1 1 calc R . . O1 O 0.3700(6) 0.1200(6) 0.8750 0.029(3) Uani 1 2 d S . . 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 U1 0.0202(4) 0.0202(4) 0.0280(6) 0.000 0.000 -0.0004(5) I1 0.0343(6) 0.0318(6) 0.0371(6) -0.0059(4) 0.0065(5) 0.0030(5) C2 0.020(8) 0.054(11) 0.043(11) 0.005(8) -0.001(7) -0.006(7) C1 0.026(8) 0.030(8) 0.037(11) -0.006(7) 0.006(7) -0.010(7) O1 0.033(5) 0.033(5) 0.021(8) -0.001(5) 0.001(5) -0.018(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 U1 O1 2.374(11) 10_554 ? U1 O1 2.374(11) . ? U1 I1 2.9639(10) . ? U1 I1 2.9639(11) 16_556 ? U1 I1 2.9639(10) 10_554 ? U1 I1 2.9639(11) 7_546 ? C2 C1 1.521(17) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C1 O1 1.445(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? O1 C1 1.445(13) 7_546 ? 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 U1 O1 180.0 10_554 . ? O1 U1 I1 84.64(2) 10_554 . ? O1 U1 I1 95.36(2) . . ? O1 U1 I1 95.36(2) 10_554 16_556 ? O1 U1 I1 84.64(2) . 16_556 ? I1 U1 I1 91.64(4) . 16_556 ? O1 U1 I1 95.36(2) 10_554 10_554 ? O1 U1 I1 84.64(2) . 10_554 ? I1 U1 I1 89.36(4) . 10_554 ? I1 U1 I1 169.29(4) 16_556 10_554 ? O1 U1 I1 84.64(2) 10_554 7_546 ? O1 U1 I1 95.36(2) . 7_546 ? I1 U1 I1 169.29(4) . 7_546 ? I1 U1 I1 89.36(4) 16_556 7_546 ? I1 U1 I1 91.64(4) 10_554 7_546 ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C1 C2 112.1(11) . . ? O1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? O1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 O1 C1 111.9(12) 7_546 . ? C1 O1 U1 124.0(6) 7_546 . ? C1 O1 U1 124.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 O1 C1 -82.9(10) . . . 7_546 ? C2 C1 O1 U1 97.1(10) . . . . ? O1 U1 O1 C1 0(100) 10_554 . . 7_546 ? I1 U1 O1 C1 166.4(7) . . . 7_546 ? I1 U1 O1 C1 75.2(7) 16_556 . . 7_546 ? I1 U1 O1 C1 -104.8(7) 10_554 . . 7_546 ? I1 U1 O1 C1 -13.6(7) 7_546 . . 7_546 ? O1 U1 O1 C1 0(100) 10_554 . . . ? I1 U1 O1 C1 -13.6(7) . . . . ? I1 U1 O1 C1 -104.8(7) 16_556 . . . ? I1 U1 O1 C1 75.2(7) 10_554 . . . ? I1 U1 O1 C1 166.4(7) 7_546 . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.879 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.269 #===END=== data_compound2 _database_code_depnum_ccdc_archive 'CCDC 690033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; uranium(III)tribromobis(dimethoxyethane) ; _chemical_name_common uranium(iii)tribromobis(dimethoxyethane) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H22 Br3 Cl2 O4 U' _chemical_formula_weight 742.93 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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' _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 8.779(5) _cell_length_b 9.475(5) _cell_length_c 13.156(7) _cell_angle_alpha 83.526(9) _cell_angle_beta 76.700(9) _cell_angle_gamma 65.579(8) _cell_volume 969.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Maroon _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 678 _exptl_absorpt_coefficient_mu 14.833 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.27572 _exptl_absorpt_correction_T_max 0.69173 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7697 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3592 _reflns_number_gt 2687 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was refined using SIMU keyword to constrain all terminal C-O bond groups having same Uij along C-O bonding directions. ; _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^)+(0.0389P)^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 3592 _refine_ls_number_parameters 176 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.964 _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 Cl2 Cl 0.5962(4) 0.6402(4) 0.9350(2) 0.0383(8) Uani 1 1 d . . . U1 U 0.91551(5) 0.09682(5) 0.32860(3) 0.01773(13) Uani 1 1 d . . . Br2 Br 1.07002(13) 0.31628(13) 0.31515(9) 0.0259(3) Uani 1 1 d . . . Br3 Br 1.21560(13) -0.10136(13) 0.43832(9) 0.0260(3) Uani 1 1 d . . . Br1 Br 0.82407(14) 0.21404(14) 0.12832(9) 0.0306(3) Uani 1 1 d . . . O4 O 1.1796(8) -0.0597(8) 0.1915(5) 0.0237(17) Uani 1 1 d U . . O1 O 0.6360(8) 0.0536(8) 0.3469(6) 0.0254(17) Uani 1 1 d U . . O2 O 0.6228(8) 0.3437(8) 0.3719(6) 0.0234(17) Uani 1 1 d U . . C3 C 0.4695(12) 0.3259(12) 0.3649(9) 0.024(3) Uani 1 1 d . . . H3A H 0.4562 0.3378 0.2928 0.029 Uiso 1 1 calc R . . H3B H 0.3699 0.4042 0.4058 0.029 Uiso 1 1 calc R . . C8 C 1.2716(13) 0.0075(13) 0.1094(9) 0.030(3) Uani 1 1 d U . . H8A H 1.3907 -0.0602 0.0958 0.045 Uiso 1 1 calc R . . H8B H 1.2579 0.1063 0.1310 0.045 Uiso 1 1 calc R . . H8C H 1.2273 0.0211 0.0471 0.045 Uiso 1 1 calc R . . C4 C 0.6071(14) 0.5004(12) 0.3431(10) 0.034(3) Uani 1 1 d U . . H4A H 0.6032 0.5189 0.2703 0.051 Uiso 1 1 calc R . . H4B H 0.7037 0.5137 0.3559 0.051 Uiso 1 1 calc R . . H4C H 0.5041 0.5725 0.3840 0.051 Uiso 1 1 calc R . . C1 C 0.6029(13) -0.0090(13) 0.2613(9) 0.029(2) Uani 1 1 d U . . H1A H 0.5245 -0.0571 0.2891 0.043 Uiso 1 1 calc R . . H1B H 0.7082 -0.0845 0.2250 0.043 Uiso 1 1 calc R . . H1C H 0.5545 0.0736 0.2138 0.043 Uiso 1 1 calc R . . C2 C 0.4865(13) 0.1670(13) 0.4062(9) 0.030(3) Uani 1 1 d . . . H2A H 0.4946 0.1574 0.4791 0.036 Uiso 1 1 calc R . . H2B H 0.3864 0.1507 0.4011 0.036 Uiso 1 1 calc R . . C7 C 1.1684(15) -0.1905(14) 0.1501(9) 0.034(3) Uani 1 1 d . . . H7A H 1.2760 -0.2514 0.1055 0.041 Uiso 1 1 calc R . . H7B H 1.0794 -0.1544 0.1096 0.041 Uiso 1 1 calc R . . C6 C 1.1270(15) -0.2857(13) 0.2430(10) 0.037(3) Uani 1 1 d . . . H6A H 1.1098 -0.3710 0.2205 0.045 Uiso 1 1 calc R . . H6B H 1.2206 -0.3281 0.2801 0.045 Uiso 1 1 calc R . . C5 C 0.9217(15) -0.2714(13) 0.3991(9) 0.038(3) Uani 1 1 d U . . H5A H 0.8859 -0.3435 0.3763 0.058 Uiso 1 1 calc R . . H5B H 0.8283 -0.2000 0.4466 0.058 Uiso 1 1 calc R . . H5C H 1.0155 -0.3268 0.4336 0.058 Uiso 1 1 calc R . . O3 O 0.9748(8) -0.1872(8) 0.3101(6) 0.0241(17) Uani 1 1 d U . . Cl1 Cl 0.7648(4) 0.6831(4) 1.0890(3) 0.0436(8) Uani 1 1 d . . . C9 C 0.7940(14) 0.5828(14) 0.9777(9) 0.035(3) Uani 1 1 d . . . H9A H 0.8387 0.4722 0.9932 0.042 Uiso 1 1 calc R . . H9B H 0.8768 0.6033 0.9222 0.042 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 Cl2 0.0333(16) 0.045(2) 0.0353(19) -0.0009(15) -0.0044(14) -0.0158(15) U1 0.0175(2) 0.0177(2) 0.0187(2) -0.00067(16) -0.00485(16) -0.00705(17) Br2 0.0263(6) 0.0228(6) 0.0327(7) 0.0005(5) -0.0079(5) -0.0132(5) Br3 0.0227(6) 0.0298(7) 0.0228(6) -0.0007(5) -0.0057(5) -0.0071(5) Br1 0.0311(6) 0.0366(7) 0.0214(7) 0.0035(5) -0.0096(5) -0.0096(6) O4 0.027(4) 0.024(4) 0.019(4) 0.001(3) 0.001(3) -0.011(3) O1 0.016(3) 0.028(4) 0.037(5) -0.006(3) -0.002(3) -0.015(3) O2 0.020(3) 0.023(4) 0.027(4) 0.006(3) -0.006(3) -0.009(3) C3 0.016(5) 0.021(6) 0.027(7) 0.001(5) -0.005(5) 0.001(5) C8 0.025(5) 0.036(6) 0.026(6) -0.003(5) 0.002(5) -0.013(5) C4 0.030(5) 0.014(5) 0.048(7) -0.004(5) -0.001(5) -0.003(5) C1 0.027(5) 0.036(6) 0.036(6) -0.010(5) -0.013(5) -0.019(5) C2 0.029(6) 0.040(8) 0.019(7) -0.006(5) 0.001(5) -0.014(6) C7 0.033(7) 0.047(8) 0.020(7) -0.012(6) 0.005(5) -0.015(6) C6 0.035(7) 0.021(7) 0.052(9) -0.006(6) -0.001(6) -0.010(6) C5 0.047(6) 0.023(6) 0.040(7) 0.001(5) 0.001(5) -0.014(5) O3 0.025(4) 0.025(4) 0.023(4) -0.005(3) 0.002(3) -0.013(3) Cl1 0.057(2) 0.040(2) 0.0329(19) -0.0033(15) -0.0082(16) -0.0186(17) C9 0.042(7) 0.029(7) 0.032(7) 0.002(6) -0.006(6) -0.014(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 Cl2 C9 1.796(12) . ? U1 O3 2.550(7) . ? U1 O4 2.582(7) . ? U1 O1 2.605(6) . ? U1 O2 2.656(7) . ? U1 Br2 2.8869(16) . ? U1 Br1 2.8978(18) . ? U1 Br3 3.0157(19) 2_756 ? U1 Br3 3.0980(16) . ? Br3 U1 3.016(2) 2_756 ? O4 C8 1.447(11) . ? O4 C7 1.455(13) . ? O1 C2 1.427(12) . ? O1 C1 1.466(12) . ? O2 C4 1.447(12) . ? O2 C3 1.449(11) . ? C3 C2 1.500(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C7 C6 1.503(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C6 O3 1.431(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5 O3 1.438(12) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? Cl1 C9 1.747(12) . ? C9 H9A 0.9700 . ? C9 H9B 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 O3 U1 O4 63.1(2) . . ? O3 U1 O1 67.8(2) . . ? O4 U1 O1 118.6(2) . . ? O3 U1 O2 130.9(2) . . ? O4 U1 O2 148.3(2) . . ? O1 U1 O2 63.2(2) . . ? O3 U1 Br2 144.71(15) . . ? O4 U1 Br2 86.23(15) . . ? O1 U1 Br2 147.23(16) . . ? O2 U1 Br2 84.38(15) . . ? O3 U1 Br1 98.83(17) . . ? O4 U1 Br1 74.93(16) . . ? O1 U1 Br1 78.66(17) . . ? O2 U1 Br1 74.70(16) . . ? Br2 U1 Br1 88.70(4) . . ? O3 U1 Br3 95.01(16) . 2_756 ? O4 U1 Br3 139.56(16) . 2_756 ? O1 U1 Br3 77.03(17) . 2_756 ? O2 U1 Br3 71.85(15) . 2_756 ? Br2 U1 Br3 98.31(4) . 2_756 ? Br1 U1 Br3 144.88(4) . 2_756 ? O3 U1 Br3 72.50(16) . . ? O4 U1 Br3 70.34(16) . . ? O1 U1 Br3 125.41(17) . . ? O2 U1 Br3 137.26(16) . . ? Br2 U1 Br3 81.35(5) . . ? Br1 U1 Br3 144.36(3) . . ? Br3 U1 Br3 70.70(4) 2_756 . ? U1 Br3 U1 109.30(4) 2_756 . ? C8 O4 C7 109.0(8) . . ? C8 O4 U1 124.8(6) . . ? C7 O4 U1 114.5(5) . . ? C2 O1 C1 113.7(8) . . ? C2 O1 U1 115.2(6) . . ? C1 O1 U1 121.4(5) . . ? C4 O2 C3 110.5(8) . . ? C4 O2 U1 123.1(6) . . ? C3 O2 U1 116.8(6) . . ? O2 C3 C2 107.8(8) . . ? O2 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? O2 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.5 . . ? 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 . . ? 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 . . ? 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 109.4(8) . . ? O1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? O1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O4 C7 C6 106.3(9) . . ? O4 C7 H7A 110.5 . . ? C6 C7 H7A 110.5 . . ? O4 C7 H7B 110.5 . . ? C6 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? O3 C6 C7 108.1(9) . . ? O3 C6 H6A 110.1 . . ? C7 C6 H6A 110.1 . . ? O3 C6 H6B 110.1 . . ? C7 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? 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 . . ? C6 O3 C5 111.7(8) . . ? C6 O3 U1 120.4(6) . . ? C5 O3 U1 119.4(6) . . ? Cl1 C9 Cl2 111.0(6) . . ? Cl1 C9 H9A 109.4 . . ? Cl2 C9 H9A 109.4 . . ? Cl1 C9 H9B 109.4 . . ? Cl2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 U1 Br3 U1 -101.97(16) . . . 2_756 ? O4 U1 Br3 U1 -168.92(16) . . . 2_756 ? O1 U1 Br3 U1 -57.3(2) . . . 2_756 ? O2 U1 Br3 U1 30.1(2) . . . 2_756 ? Br2 U1 Br3 U1 102.01(4) . . . 2_756 ? Br1 U1 Br3 U1 177.45(5) . . . 2_756 ? Br3 U1 Br3 U1 0.0 2_756 . . 2_756 ? O3 U1 O4 C8 165.0(8) . . . . ? O1 U1 O4 C8 124.5(7) . . . . ? O2 U1 O4 C8 39.9(9) . . . . ? Br2 U1 O4 C8 -33.0(7) . . . . ? Br1 U1 O4 C8 56.7(7) . . . . ? Br3 U1 O4 C8 -131.4(7) 2_756 . . . ? Br3 U1 O4 C8 -115.1(7) . . . . ? O3 U1 O4 C7 26.2(6) . . . . ? O1 U1 O4 C7 -14.3(7) . . . . ? O2 U1 O4 C7 -98.9(7) . . . . ? Br2 U1 O4 C7 -171.8(7) . . . . ? Br1 U1 O4 C7 -82.1(7) . . . . ? Br3 U1 O4 C7 89.8(7) 2_756 . . . ? Br3 U1 O4 C7 106.1(7) . . . . ? O3 U1 O1 C2 154.8(7) . . . . ? O4 U1 O1 C2 -166.4(6) . . . . ? O2 U1 O1 C2 -22.3(6) . . . . ? Br2 U1 O1 C2 -31.5(8) . . . . ? Br1 U1 O1 C2 -100.7(7) . . . . ? Br3 U1 O1 C2 53.7(6) 2_756 . . . ? Br3 U1 O1 C2 108.3(6) . . . . ? O3 U1 O1 C1 -61.3(7) . . . . ? O4 U1 O1 C1 -22.5(8) . . . . ? O2 U1 O1 C1 121.7(8) . . . . ? Br2 U1 O1 C1 112.5(7) . . . . ? Br1 U1 O1 C1 43.2(7) . . . . ? Br3 U1 O1 C1 -162.3(7) 2_756 . . . ? Br3 U1 O1 C1 -107.8(7) . . . . ? O3 U1 O2 C4 -156.6(8) . . . . ? O4 U1 O2 C4 -51.3(9) . . . . ? O1 U1 O2 C4 -152.9(9) . . . . ? Br2 U1 O2 C4 22.1(8) . . . . ? Br1 U1 O2 C4 -68.1(8) . . . . ? Br3 U1 O2 C4 122.7(8) 2_756 . . . ? Br3 U1 O2 C4 92.9(8) . . . . ? O3 U1 O2 C3 -13.7(7) . . . . ? O4 U1 O2 C3 91.6(7) . . . . ? O1 U1 O2 C3 -10.0(6) . . . . ? Br2 U1 O2 C3 165.0(6) . . . . ? Br1 U1 O2 C3 74.8(6) . . . . ? Br3 U1 O2 C3 -94.3(6) 2_756 . . . ? Br3 U1 O2 C3 -124.2(6) . . . . ? C4 O2 C3 C2 -174.2(9) . . . . ? U1 O2 C3 C2 38.4(10) . . . . ? C1 O1 C2 C3 -95.1(10) . . . . ? U1 O1 C2 C3 51.6(10) . . . . ? O2 C3 C2 O1 -58.2(11) . . . . ? C8 O4 C7 C6 161.5(9) . . . . ? U1 O4 C7 C6 -53.4(10) . . . . ? O4 C7 C6 O3 55.6(11) . . . . ? C7 C6 O3 C5 177.3(10) . . . . ? C7 C6 O3 U1 -34.9(12) . . . . ? O4 U1 O3 C6 5.9(7) . . . . ? O1 U1 O3 C6 147.8(8) . . . . ? O2 U1 O3 C6 151.3(7) . . . . ? Br2 U1 O3 C6 -26.4(9) . . . . ? Br1 U1 O3 C6 73.9(8) . . . . ? Br3 U1 O3 C6 -138.5(8) 2_756 . . . ? Br3 U1 O3 C6 -70.5(8) . . . . ? O4 U1 O3 C5 151.2(8) . . . . ? O1 U1 O3 C5 -67.0(7) . . . . ? O2 U1 O3 C5 -63.4(8) . . . . ? Br2 U1 O3 C5 118.9(7) . . . . ? Br1 U1 O3 C5 -140.8(7) . . . . ? Br3 U1 O3 C5 6.8(7) 2_756 . . . ? Br3 U1 O3 C5 74.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.610 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.271 #===END=== data_compound3 _database_code_depnum_ccdc_archive 'CCDC 690034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; uranium(IV)tetrabromobis(dimethoxyethane) ; _chemical_name_common uranium(IV)tetrabromobis(dimethoxyethane) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Br4 O4 U' _chemical_formula_weight 737.91 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.5816(6) _cell_length_b 14.4919(11) _cell_length_c 15.7753(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.242(2) _cell_angle_gamma 90.00 _cell_volume 1693.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 19.018 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.20319 _exptl_absorpt_correction_T_max 0.40775 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; As the crystals did not have a regular shape, it would be difficult to determine the individual faces and corresponding center-face distances precisely. Thus, we used empirical absorption correction instead of numeric correction ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13595 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.09 _reflns_number_total 3551 _reflns_number_gt 2414 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Because of the significant absorption (mu > 10 mm^-1) due to the presence of heavy atoms, the empirical absorption correction based on psi-scan may not perfectly correct for the absorption effect. This probably results in the relatively high Rint value. ; _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^)+(0.0437P)^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 3551 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 U1 U 0.02780(5) 0.25525(2) 0.60659(2) 0.01622(13) Uani 1 1 d . . . Br2 Br 0.18470(14) 0.32076(7) 0.47261(7) 0.0254(3) Uani 1 1 d . . . Br3 Br 0.24891(14) 0.39090(7) 0.70101(7) 0.0255(3) Uani 1 1 d . . . Br1 Br -0.31235(13) 0.19352(8) 0.52304(8) 0.0299(3) Uani 1 1 d . . . Br4 Br -0.01518(15) 0.11432(7) 0.72238(8) 0.0299(3) Uani 1 1 d . . . O1 O 0.0813(9) 0.1148(4) 0.5130(5) 0.0204(16) Uani 1 1 d . . . O2 O 0.3336(9) 0.1756(5) 0.6555(5) 0.0211(16) Uani 1 1 d . . . O4 O -0.1432(9) 0.3266(5) 0.7142(5) 0.0217(16) Uani 1 1 d . . . O3 O -0.1667(9) 0.3966(5) 0.5499(5) 0.0240(17) Uani 1 1 d . . . C1 C -0.0014(14) 0.1032(8) 0.4225(7) 0.026(3) Uani 1 1 d . . . H1A H 0.0475 0.1477 0.3887 0.039 Uiso 1 1 calc R . . H1B H -0.1294 0.1121 0.4143 0.039 Uiso 1 1 calc R . . H1C H 0.0225 0.0421 0.4043 0.039 Uiso 1 1 calc R . . C2 C 0.2676(13) 0.0852(7) 0.5264(7) 0.024(3) Uani 1 1 d . . . H2A H 0.3338 0.1267 0.4963 0.028 Uiso 1 1 calc R . . H2B H 0.2728 0.0238 0.5025 0.028 Uiso 1 1 calc R . . C3 C 0.3503(14) 0.0842(7) 0.6180(8) 0.029(3) Uani 1 1 d . . . H3A H 0.4768 0.0678 0.6259 0.035 Uiso 1 1 calc R . . H3B H 0.2915 0.0385 0.6474 0.035 Uiso 1 1 calc R . . C8 C -0.0847(16) 0.3202(9) 0.8057(8) 0.037(3) Uani 1 1 d . . . H8A H -0.0016 0.3694 0.8261 0.055 Uiso 1 1 calc R . . H8B H -0.0261 0.2620 0.8205 0.055 Uiso 1 1 calc R . . H8C H -0.1870 0.3251 0.8323 0.055 Uiso 1 1 calc R . . C4 C 0.4446(16) 0.1794(8) 0.7424(8) 0.037(3) Uani 1 1 d . . . H4A H 0.3901 0.1429 0.7807 0.056 Uiso 1 1 calc R . . H4B H 0.4546 0.2422 0.7622 0.056 Uiso 1 1 calc R . . H4C H 0.5626 0.1556 0.7418 0.056 Uiso 1 1 calc R . . C6 C -0.3014(16) 0.4225(9) 0.5974(9) 0.041(3) Uani 1 1 d . . . H6A H -0.4038 0.3810 0.5832 0.050 Uiso 1 1 calc R . . H6B H -0.3434 0.4847 0.5816 0.050 Uiso 1 1 calc R . . C5 C -0.2343(16) 0.4175(9) 0.4597(8) 0.038(3) Uani 1 1 d . . . H5A H -0.3463 0.3856 0.4394 0.057 Uiso 1 1 calc R . . H5B H -0.1481 0.3981 0.4267 0.057 Uiso 1 1 calc R . . H5C H -0.2536 0.4828 0.4529 0.057 Uiso 1 1 calc R . . C7 C -0.2229(17) 0.4182(9) 0.6907(8) 0.040(3) Uani 1 1 d . . . H7A H -0.1306 0.4652 0.7058 0.048 Uiso 1 1 calc R . . H7B H -0.3159 0.4302 0.7231 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 U1 0.01550(19) 0.0182(2) 0.0154(2) 0.00002(17) 0.00427(14) -0.00145(16) Br2 0.0291(6) 0.0259(6) 0.0235(6) 0.0022(5) 0.0111(5) -0.0031(4) Br3 0.0265(6) 0.0243(6) 0.0243(6) -0.0039(5) 0.0024(5) -0.0057(4) Br1 0.0174(5) 0.0341(7) 0.0371(7) -0.0073(5) 0.0032(5) -0.0043(5) Br4 0.0382(6) 0.0256(6) 0.0307(7) 0.0080(5) 0.0180(5) 0.0056(5) O1 0.020(4) 0.017(4) 0.026(4) 0.002(3) 0.009(3) 0.000(3) O2 0.020(4) 0.025(4) 0.018(4) 0.001(3) 0.003(3) 0.001(3) O4 0.022(4) 0.021(4) 0.026(4) -0.005(3) 0.014(3) 0.003(3) O3 0.017(4) 0.027(4) 0.028(5) 0.008(3) 0.004(3) 0.006(3) C1 0.024(6) 0.040(7) 0.018(6) -0.010(5) 0.011(5) -0.009(5) C2 0.027(6) 0.022(6) 0.028(7) 0.001(5) 0.021(5) 0.006(4) C3 0.024(6) 0.020(6) 0.046(8) -0.008(5) 0.014(5) 0.006(4) C8 0.041(7) 0.045(8) 0.028(7) -0.012(6) 0.014(6) -0.009(6) C4 0.041(7) 0.035(7) 0.026(7) -0.001(6) -0.013(6) 0.006(6) C6 0.033(7) 0.042(8) 0.049(9) -0.002(7) 0.009(6) 0.008(6) C5 0.036(7) 0.042(8) 0.036(8) 0.013(6) 0.009(6) 0.005(6) C7 0.042(7) 0.049(8) 0.034(8) -0.006(6) 0.019(6) 0.014(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 U1 O2 2.558(7) . ? U1 O4 2.562(7) . ? U1 O3 2.571(7) . ? U1 O1 2.596(7) . ? U1 Br1 2.7833(11) . ? U1 Br3 2.7990(11) . ? U1 Br2 2.8017(11) . ? U1 Br4 2.8047(12) . ? O1 C1 1.441(12) . ? O1 C2 1.448(11) . ? O2 C4 1.450(12) . ? O2 C3 1.467(12) . ? O4 C8 1.420(13) . ? O4 C7 1.472(14) . ? O3 C6 1.440(13) . ? O3 C5 1.438(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.449(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 C7 1.467(18) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C7 H7A 0.9700 . ? C7 H7B 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 U1 O4 122.4(2) . . ? O2 U1 O3 151.7(2) . . ? O4 U1 O3 64.9(2) . . ? O2 U1 O1 65.0(2) . . ? O4 U1 O1 148.8(2) . . ? O3 U1 O1 125.0(2) . . ? O2 U1 Br1 133.43(16) . . ? O4 U1 Br1 84.00(16) . . ? O3 U1 Br1 71.69(16) . . ? O1 U1 Br1 73.71(14) . . ? O2 U1 Br3 75.76(16) . . ? O4 U1 Br3 72.17(15) . . ? O3 U1 Br3 81.97(16) . . ? O1 U1 Br3 134.83(14) . . ? Br1 U1 Br3 150.22(4) . . ? O2 U1 Br2 82.96(16) . . ? O4 U1 Br2 135.91(16) . . ? O3 U1 Br2 76.79(16) . . ? O1 U1 Br2 72.18(15) . . ? Br1 U1 Br2 104.52(4) . . ? Br3 U1 Br2 82.02(3) . . ? O2 U1 Br4 72.44(16) . . ? O4 U1 Br4 73.60(16) . . ? O3 U1 Br4 132.03(16) . . ? O1 U1 Br4 81.57(16) . . ? Br1 U1 Br4 81.40(4) . . ? Br3 U1 Br4 107.70(4) . . ? Br2 U1 Br4 149.84(4) . . ? C1 O1 C2 108.4(8) . . ? C1 O1 U1 124.5(6) . . ? C2 O1 U1 114.5(6) . . ? C4 O2 C3 109.4(8) . . ? C4 O2 U1 125.1(6) . . ? C3 O2 U1 115.8(6) . . ? C8 O4 C7 109.8(8) . . ? C8 O4 U1 123.7(6) . . ? C7 O4 U1 115.8(6) . . ? C6 O3 C5 108.4(8) . . ? C6 O3 U1 116.4(7) . . ? C5 O3 U1 124.8(6) . . ? 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 110.5(8) . . ? O1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 O2 109.7(9) . . ? C2 C3 H3A 109.7 . . ? O2 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? O2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? 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 . . ? 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 C6 C7 109.2(10) . . ? O3 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? O3 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? 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 . . ? O4 C7 C6 110.4(10) . . ? O4 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? O4 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 U1 O1 C1 -152.4(7) . . . . ? O4 U1 O1 C1 95.8(8) . . . . ? O3 U1 O1 C1 -3.2(7) . . . . ? Br1 U1 O1 C1 49.6(6) . . . . ? Br3 U1 O1 C1 -120.3(6) . . . . ? Br2 U1 O1 C1 -62.0(6) . . . . ? Br4 U1 O1 C1 133.1(7) . . . . ? O2 U1 O1 C2 -15.1(6) . . . . ? O4 U1 O1 C2 -126.9(6) . . . . ? O3 U1 O1 C2 134.1(6) . . . . ? Br1 U1 O1 C2 -173.1(6) . . . . ? Br3 U1 O1 C2 17.0(7) . . . . ? Br2 U1 O1 C2 75.3(6) . . . . ? Br4 U1 O1 C2 -89.6(6) . . . . ? O4 U1 O2 C4 -11.6(9) . . . . ? O3 U1 O2 C4 85.2(9) . . . . ? O1 U1 O2 C4 -156.9(8) . . . . ? Br1 U1 O2 C4 -127.1(7) . . . . ? Br3 U1 O2 C4 46.0(8) . . . . ? Br2 U1 O2 C4 129.6(8) . . . . ? Br4 U1 O2 C4 -68.1(8) . . . . ? O4 U1 O2 C3 130.8(7) . . . . ? O3 U1 O2 C3 -132.3(7) . . . . ? O1 U1 O2 C3 -14.4(6) . . . . ? Br1 U1 O2 C3 15.4(8) . . . . ? Br3 U1 O2 C3 -171.5(7) . . . . ? Br2 U1 O2 C3 -88.0(7) . . . . ? Br4 U1 O2 C3 74.3(7) . . . . ? O2 U1 O4 C8 -4.6(8) . . . . ? O3 U1 O4 C8 -153.3(8) . . . . ? O1 U1 O4 C8 90.0(8) . . . . ? Br1 U1 O4 C8 134.1(7) . . . . ? Br3 U1 O4 C8 -64.0(7) . . . . ? Br2 U1 O4 C8 -121.2(7) . . . . ? Br4 U1 O4 C8 51.4(7) . . . . ? O2 U1 O4 C7 136.0(7) . . . . ? O3 U1 O4 C7 -12.7(7) . . . . ? O1 U1 O4 C7 -129.4(7) . . . . ? Br1 U1 O4 C7 -85.3(7) . . . . ? Br3 U1 O4 C7 76.7(7) . . . . ? Br2 U1 O4 C7 19.4(8) . . . . ? Br4 U1 O4 C7 -168.0(7) . . . . ? O2 U1 O3 C6 -129.0(7) . . . . ? O4 U1 O3 C6 -16.8(7) . . . . ? O1 U1 O3 C6 128.8(7) . . . . ? Br1 U1 O3 C6 75.1(7) . . . . ? Br3 U1 O3 C6 -90.8(7) . . . . ? Br2 U1 O3 C6 -174.4(7) . . . . ? Br4 U1 O3 C6 15.8(8) . . . . ? O2 U1 O3 C5 90.2(9) . . . . ? O4 U1 O3 C5 -157.6(8) . . . . ? O1 U1 O3 C5 -12.0(8) . . . . ? Br1 U1 O3 C5 -65.7(7) . . . . ? Br3 U1 O3 C5 128.4(8) . . . . ? Br2 U1 O3 C5 44.8(7) . . . . ? Br4 U1 O3 C5 -125.0(7) . . . . ? C1 O1 C2 C3 -172.7(9) . . . . ? U1 O1 C2 C3 43.4(10) . . . . ? O1 C2 C3 O2 -56.0(11) . . . . ? C4 O2 C3 C2 -169.5(9) . . . . ? U1 O2 C3 C2 42.4(10) . . . . ? C5 O3 C6 C7 -169.4(10) . . . . ? U1 O3 C6 C7 43.7(12) . . . . ? C8 O4 C7 C6 -174.0(10) . . . . ? U1 O4 C7 C6 40.2(12) . . . . ? O3 C6 C7 O4 -54.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 2.833 _refine_diff_density_min -2.322 _refine_diff_density_rms 0.319 #===END=== data_compound4 _database_code_depnum_ccdc_archive 'CCDC 690035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; uranium(IV)tetrachlorobis(dimethoxyethane) ; _chemical_name_common uranium(IV)tetrachlorobis(dimethoxyethane) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Cl4 O4 U' _chemical_formula_weight 560.07 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.493(9) _cell_length_b 7.274(4) _cell_length_c 14.821(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.538(11) _cell_angle_gamma 90.00 _cell_volume 1604.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 10.782 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.15813 _exptl_absorpt_correction_T_max 0.89537 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; As the crystals did not have a regular shape, it would be difficult to determine the individual faces and corresponding center-face distances precisely. Thus, we used empirical absorption correction instead of numeric correction ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11183 _diffrn_reflns_av_R_equivalents 0.1494 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.62 _reflns_number_total 3168 _reflns_number_gt 2615 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure has a highest residual peak of 6.63 at 0.2513 0.5946 0.2196 (0.88 \%A from U1) and a lowest residual peak -4.51 at 0.2303 0.5513 0.2581 (0.96 \%A from U1), and because of their close proximity to the heavy uranium atom they are likely 'ghost peaks'. Because of the significant absorption (mu > 10 mm^-1) due to the presence of heavy atoms, the empirical absorption correction based on psi-scan may not perfectly correct for the absorption effect. This probably results in the relatively high Rint value. ; _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^)+(0.1038P)^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 3168 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1673 _refine_ls_wR_factor_gt 0.1580 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _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 U1 U 0.74851(3) 0.97312(6) 0.27920(3) 0.0202(2) Uani 1 1 d . . . Cl1 Cl 0.6683(2) 1.2728(4) 0.2919(2) 0.0321(7) Uani 1 1 d . . . Cl3 Cl 0.8623(2) 1.0510(4) 0.4639(2) 0.0300(7) Uani 1 1 d . . . Cl4 Cl 0.8428(2) 0.7969(4) 0.2034(2) 0.0326(7) Uani 1 1 d . . . O3 O 0.6542(6) 0.8826(10) 0.3723(6) 0.0312(19) Uani 1 1 d . . . O4 O 0.7925(5) 0.6702(10) 0.3737(5) 0.0292(18) Uani 1 1 d . . . Cl2 Cl 0.6142(2) 0.7755(4) 0.1541(2) 0.0320(7) Uani 1 1 d . . . O1 O 0.6961(5) 1.1494(10) 0.1111(5) 0.0251(17) Uani 1 1 d . . . O2 O 0.8612(5) 1.2015(10) 0.2647(5) 0.0243(17) Uani 1 1 d . . . C1 C 0.6036(9) 1.1817(18) 0.0431(9) 0.043(3) Uani 1 1 d . . . H1A H 0.5839 1.2950 0.0602 0.065 Uiso 1 1 calc R . . H1B H 0.5673 1.0824 0.0477 0.065 Uiso 1 1 calc R . . H1C H 0.5981 1.1893 -0.0240 0.065 Uiso 1 1 calc R . . C3 C 0.8423(8) 1.2706(18) 0.1669(9) 0.032(3) Uani 1 1 d . . . H3A H 0.8578 1.1789 0.1295 0.039 Uiso 1 1 calc R . . H3B H 0.8777 1.3801 0.1725 0.039 Uiso 1 1 calc R . . C7 C 0.7596(12) 0.6454(19) 0.4473(10) 0.051(4) Uani 1 1 d . . . H7A H 0.7936 0.7216 0.5051 0.061 Uiso 1 1 calc R . . H7B H 0.7669 0.5181 0.4688 0.061 Uiso 1 1 calc R . . C6 C 0.6634(11) 0.6964(16) 0.4049(10) 0.045(4) Uani 1 1 d . . . H6A H 0.6288 0.6166 0.3490 0.054 Uiso 1 1 calc R . . H6B H 0.6411 0.6823 0.4553 0.054 Uiso 1 1 calc R . . C2 C 0.7471(9) 1.3139(16) 0.1153(9) 0.034(3) Uani 1 1 d . . . H2A H 0.7321 1.4102 0.1508 0.041 Uiso 1 1 calc R . . H2B H 0.7327 1.3571 0.0482 0.041 Uiso 1 1 calc R . . C5 C 0.5621(10) 0.938(2) 0.3413(13) 0.048(4) Uani 1 1 d . . . H5A H 0.5242 0.8709 0.2822 0.073 Uiso 1 1 calc R . . H5B H 0.5564 1.0671 0.3272 0.073 Uiso 1 1 calc R . . H5C H 0.5445 0.9119 0.3938 0.073 Uiso 1 1 calc R . . C8 C 0.8802(10) 0.588(2) 0.4105(11) 0.050(4) Uani 1 1 d . . . H8A H 0.9193 0.6451 0.4725 0.075 Uiso 1 1 calc R . . H8B H 0.9042 0.6051 0.3624 0.075 Uiso 1 1 calc R . . H8C H 0.8758 0.4589 0.4211 0.075 Uiso 1 1 calc R . . C4 C 0.9559(8) 1.1771(18) 0.3196(9) 0.038(3) Uani 1 1 d . . . H4A H 0.9758 1.0820 0.2890 0.057 Uiso 1 1 calc R . . H4B H 0.9695 1.1428 0.3872 0.057 Uiso 1 1 calc R . . H4C H 0.9860 1.2900 0.3197 0.057 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 U1 0.0240(3) 0.0245(3) 0.0131(3) -0.00103(13) 0.0090(2) 0.00073(15) Cl1 0.0362(17) 0.0275(14) 0.0374(16) -0.0006(11) 0.0204(14) 0.0054(12) Cl3 0.0324(17) 0.0404(17) 0.0151(14) -0.0046(10) 0.0083(12) -0.0027(13) Cl4 0.0426(18) 0.0371(16) 0.0260(15) -0.0029(11) 0.0223(14) 0.0072(13) O3 0.043(5) 0.026(4) 0.034(5) -0.001(3) 0.025(4) -0.002(4) O4 0.038(5) 0.033(4) 0.011(4) 0.008(3) 0.006(4) 0.005(4) Cl2 0.0349(17) 0.0326(14) 0.0229(14) -0.0013(11) 0.0072(13) -0.0091(12) O1 0.034(5) 0.026(4) 0.011(3) 0.006(3) 0.005(3) -0.002(3) O2 0.019(4) 0.033(4) 0.022(4) 0.004(3) 0.010(3) -0.002(3) C1 0.040(8) 0.044(8) 0.031(7) 0.010(5) 0.001(6) 0.001(6) C3 0.031(7) 0.048(7) 0.027(6) 0.000(5) 0.021(6) -0.011(6) C7 0.096(13) 0.034(7) 0.030(7) 0.003(5) 0.034(8) -0.004(8) C6 0.085(12) 0.028(7) 0.044(8) 0.004(5) 0.050(9) -0.008(7) C2 0.042(8) 0.036(7) 0.027(6) 0.007(5) 0.016(6) -0.006(6) C5 0.047(9) 0.050(8) 0.061(10) -0.008(7) 0.036(8) -0.008(7) C8 0.058(10) 0.041(8) 0.036(8) 0.007(6) 0.006(7) 0.025(7) C4 0.028(7) 0.054(8) 0.031(7) 0.002(6) 0.011(6) -0.001(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 U1 O4 2.543(7) . ? U1 O2 2.570(7) . ? U1 O3 2.570(8) . ? U1 O1 2.596(7) . ? U1 Cl1 2.598(3) . ? U1 Cl4 2.614(3) . ? U1 Cl2 2.621(3) . ? U1 Cl3 2.628(3) . ? O3 C6 1.424(14) . ? O3 C5 1.441(17) . ? O4 C7 1.423(15) . ? O4 C8 1.438(15) . ? O1 C1 1.440(14) . ? O1 C2 1.448(14) . ? O2 C4 1.426(14) . ? O2 C3 1.435(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C3 C2 1.453(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C7 C6 1.48(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 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 U1 O2 124.1(2) . . ? O4 U1 O3 65.0(3) . . ? O2 U1 O3 146.9(2) . . ? O4 U1 O1 148.7(2) . . ? O2 U1 O1 63.5(2) . . ? O3 U1 O1 127.8(3) . . ? O4 U1 Cl1 136.08(18) . . ? O2 U1 Cl1 82.69(18) . . ? O3 U1 Cl1 74.43(18) . . ? O1 U1 Cl1 71.70(18) . . ? O4 U1 Cl4 74.37(19) . . ? O2 U1 Cl4 72.26(18) . . ? O3 U1 Cl4 135.64(18) . . ? O1 U1 Cl4 80.98(18) . . ? Cl1 U1 Cl4 149.13(9) . . ? O4 U1 Cl2 82.40(19) . . ? O2 U1 Cl2 135.81(17) . . ? O3 U1 Cl2 73.51(19) . . ? O1 U1 Cl2 76.24(18) . . ? Cl1 U1 Cl2 102.11(11) . . ? Cl4 U1 Cl2 84.57(11) . . ? O4 U1 Cl3 72.96(18) . . ? O2 U1 Cl3 74.33(17) . . ? O3 U1 Cl3 79.8(2) . . ? O1 U1 Cl3 133.29(17) . . ? Cl1 U1 Cl3 84.32(10) . . ? Cl4 U1 Cl3 105.26(10) . . ? Cl2 U1 Cl3 149.45(9) . . ? C6 O3 C5 108.5(10) . . ? C6 O3 U1 115.2(7) . . ? C5 O3 U1 123.8(8) . . ? C7 O4 C8 108.1(10) . . ? C7 O4 U1 114.8(7) . . ? C8 O4 U1 124.8(8) . . ? C1 O1 C2 108.4(9) . . ? C1 O1 U1 124.5(7) . . ? C2 O1 U1 114.8(6) . . ? C4 O2 C3 109.2(8) . . ? C4 O2 U1 121.7(7) . . ? C3 O2 U1 117.4(6) . . ? 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 . . ? O2 C3 C2 108.9(9) . . ? O2 C3 H3A 109.9 . . ? C2 C3 H3A 109.9 . . ? O2 C3 H3B 109.9 . . ? C2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? O4 C7 C6 109.7(10) . . ? O4 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? O4 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O3 C6 C7 108.7(11) . . ? O3 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? O3 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? O1 C2 C3 108.6(10) . . ? O1 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? O1 C2 H2B 110.0 . . ? C3 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? 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 . . ? 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 . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 U1 O3 C6 -14.3(8) . . . . ? O2 U1 O3 C6 -129.0(8) . . . . ? O1 U1 O3 C6 131.9(8) . . . . ? Cl1 U1 O3 C6 -177.1(9) . . . . ? Cl4 U1 O3 C6 11.2(9) . . . . ? Cl2 U1 O3 C6 74.9(8) . . . . ? Cl3 U1 O3 C6 -90.2(8) . . . . ? O4 U1 O3 C5 -151.7(9) . . . . ? O2 U1 O3 C5 93.6(10) . . . . ? O1 U1 O3 C5 -5.4(10) . . . . ? Cl1 U1 O3 C5 45.6(9) . . . . ? Cl4 U1 O3 C5 -126.1(8) . . . . ? Cl2 U1 O3 C5 -62.5(9) . . . . ? Cl3 U1 O3 C5 132.5(9) . . . . ? O2 U1 O4 C7 125.7(8) . . . . ? O3 U1 O4 C7 -17.4(8) . . . . ? O1 U1 O4 C7 -139.8(8) . . . . ? Cl1 U1 O4 C7 6.9(9) . . . . ? Cl4 U1 O4 C7 -179.1(9) . . . . ? Cl2 U1 O4 C7 -92.7(8) . . . . ? Cl3 U1 O4 C7 69.0(8) . . . . ? O2 U1 O4 C8 -11.8(10) . . . . ? O3 U1 O4 C8 -154.9(9) . . . . ? O1 U1 O4 C8 82.7(10) . . . . ? Cl1 U1 O4 C8 -130.6(8) . . . . ? Cl4 U1 O4 C8 43.3(9) . . . . ? Cl2 U1 O4 C8 129.8(9) . . . . ? Cl3 U1 O4 C8 -68.5(9) . . . . ? O4 U1 O1 C1 91.1(10) . . . . ? O2 U1 O1 C1 -156.1(9) . . . . ? O3 U1 O1 C1 -13.2(9) . . . . ? Cl1 U1 O1 C1 -65.3(8) . . . . ? Cl4 U1 O1 C1 129.3(8) . . . . ? Cl2 U1 O1 C1 42.7(8) . . . . ? Cl3 U1 O1 C1 -128.2(8) . . . . ? O4 U1 O1 C2 -131.3(7) . . . . ? O2 U1 O1 C2 -18.5(7) . . . . ? O3 U1 O1 C2 124.4(7) . . . . ? Cl1 U1 O1 C2 72.4(7) . . . . ? Cl4 U1 O1 C2 -93.1(7) . . . . ? Cl2 U1 O1 C2 -179.7(8) . . . . ? Cl3 U1 O1 C2 9.4(8) . . . . ? O4 U1 O2 C4 -7.3(9) . . . . ? O3 U1 O2 C4 88.6(9) . . . . ? O1 U1 O2 C4 -152.0(8) . . . . ? Cl1 U1 O2 C4 134.9(8) . . . . ? Cl4 U1 O2 C4 -63.4(7) . . . . ? Cl2 U1 O2 C4 -125.2(7) . . . . ? Cl3 U1 O2 C4 48.8(7) . . . . ? O4 U1 O2 C3 131.6(7) . . . . ? O3 U1 O2 C3 -132.5(7) . . . . ? O1 U1 O2 C3 -13.0(7) . . . . ? Cl1 U1 O2 C3 -86.2(7) . . . . ? Cl4 U1 O2 C3 75.5(7) . . . . ? Cl2 U1 O2 C3 13.7(8) . . . . ? Cl3 U1 O2 C3 -172.3(8) . . . . ? C4 O2 C3 C2 -173.9(10) . . . . ? U1 O2 C3 C2 42.4(12) . . . . ? C8 O4 C7 C6 -169.4(11) . . . . ? U1 O4 C7 C6 46.3(12) . . . . ? C5 O3 C6 C7 -173.8(11) . . . . ? U1 O3 C6 C7 42.6(12) . . . . ? O4 C7 C6 O3 -58.3(13) . . . . ? C1 O1 C2 C3 -168.4(10) . . . . ? U1 O1 C2 C3 47.4(11) . . . . ? O2 C3 C2 O1 -57.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 26.62 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 6.627 _refine_diff_density_min -4.512 _refine_diff_density_rms 0.403 #===END=== data_compound5 _database_code_depnum_ccdc_archive 'CCDC 690036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; uranium(IV)tetratriflatebis(dimethoxyethane) ; _chemical_name_common uranium(IV)tetratriflatebis(dimethoxyethane) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 F12 O16 S4 U' _chemical_formula_weight 1014.55 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2627(14) _cell_length_b 25.521(4) _cell_length_c 13.285(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.908(4) _cell_angle_gamma 90.00 _cell_volume 2970.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 5.886 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.277 _exptl_absorpt_correction_T_max 0.423 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24272 _diffrn_reflns_av_R_equivalents 0.1511 _diffrn_reflns_av_sigmaI/netI 0.2412 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.91 _reflns_number_total 6077 _reflns_number_gt 2817 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was refined using SIMU keyword to constrain all C-F bond groups having same Uij along C-F bonding directions, and to constrain C6 and C7 having same Uij along C6-C7 bonding direction. Because of the significant absorption (mu > 10mm^-1) due to the presence of heavy atoms, the empirical absorption correction based on psi-scan may not perfectly correct for the absorption effect. This probably results in the relatively high Rint value. ; _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^)+(0.0228P)^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 6077 _refine_ls_number_parameters 410 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 0.779 _refine_ls_restrained_S_all 0.788 _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 C2 C 0.5257(16) 0.6670(6) 1.0450(11) 0.059(3) Uani 1 1 d U . . C1 C -0.2641(16) 0.4714(5) 0.6990(11) 0.045(3) Uani 1 1 d U . . C4 C -0.149(2) 0.6522(7) 0.3928(14) 0.082(4) Uani 1 1 d U . . U1 U 0.09064(5) 0.614211(18) 0.75598(3) 0.02160(13) Uani 1 1 d . . . S1 S -0.2277(3) 0.53294(11) 0.7713(2) 0.0247(7) Uani 1 1 d . . . S2 S 0.4873(3) 0.62987(11) 0.9238(2) 0.0279(8) Uani 1 1 d . . . S3 S 0.1290(3) 0.75170(11) 0.6837(2) 0.0319(8) Uani 1 1 d . . . S4 S -0.1308(3) 0.59480(12) 0.4742(2) 0.0336(8) Uani 1 1 d . . . O1 O -0.0962(8) 0.5531(2) 0.7449(6) 0.0298(18) Uani 1 1 d . . . O13 O -0.1286(8) 0.6647(3) 0.7524(6) 0.027(2) Uani 1 1 d . . . C9 C 0.3060(13) 0.6284(4) 0.5838(8) 0.038(3) Uani 1 1 d . . . H9A H 0.4100 0.6232 0.5869 0.057 Uiso 1 1 calc R . . H9B H 0.2908 0.6645 0.5981 0.057 Uiso 1 1 calc R . . H9C H 0.2391 0.6192 0.5143 0.057 Uiso 1 1 calc R . . O10 O -0.0445(7) 0.6163(3) 0.5804(5) 0.0265(16) Uani 1 1 d . . . O14 O 0.0486(7) 0.6258(2) 0.9284(5) 0.0228(18) Uani 1 1 d . . . O3 O -0.1839(9) 0.5192(3) 0.8801(6) 0.038(2) Uani 1 1 d . . . O15 O 0.2729(8) 0.5956(3) 0.6626(5) 0.0275(19) Uani 1 1 d . . . O16 O 0.1989(8) 0.5259(3) 0.7837(5) 0.0284(19) Uani 1 1 d . . . F1 F -0.3017(9) 0.4783(3) 0.5976(5) 0.064(2) Uani 1 1 d U . . O4 O 0.3172(7) 0.6259(3) 0.8888(5) 0.032(2) Uani 1 1 d . . . O7 O 0.1506(8) 0.6975(3) 0.7276(5) 0.032(2) Uani 1 1 d . . . F3 F -0.1420(8) 0.4409(2) 0.7296(5) 0.0518(19) Uani 1 1 d U . . F7 F 0.2647(9) 0.7783(3) 0.8792(6) 0.071(2) Uani 1 1 d U . . O6 O 0.5396(8) 0.6622(3) 0.8566(6) 0.043(2) Uani 1 1 d . . . O9 O 0.1649(9) 0.7560(3) 0.5882(6) 0.042(2) Uani 1 1 d . . . O8 O -0.0073(8) 0.7736(3) 0.6874(6) 0.045(2) Uani 1 1 d . . . O11 O -0.2817(9) 0.5810(3) 0.4669(6) 0.051(2) Uani 1 1 d . . . F8 F 0.4111(8) 0.7682(3) 0.7883(6) 0.066(2) Uani 1 1 d U . . O2 O -0.3580(7) 0.5638(3) 0.7278(6) 0.036(2) Uani 1 1 d . . . F2 F -0.3751(8) 0.4463(3) 0.7202(6) 0.059(2) Uani 1 1 d U . . O12 O -0.0431(9) 0.5597(3) 0.4359(6) 0.048(2) Uani 1 1 d . . . F5 F 0.6705(8) 0.6761(3) 1.0856(5) 0.067(2) Uani 1 1 d U . . F9 F 0.2713(9) 0.8357(3) 0.7628(6) 0.073(2) Uani 1 1 d U . . O5 O 0.5576(8) 0.5814(3) 0.9572(6) 0.046(2) Uani 1 1 d . . . F6 F 0.4819(8) 0.6407(3) 1.1144(5) 0.074(2) Uani 1 1 d U . . F11 F -0.0181(10) 0.6718(3) 0.3969(6) 0.080(3) Uani 1 1 d U . . C11 C 0.3205(11) 0.5126(4) 0.7424(8) 0.028(3) Uani 1 1 d . . . H11A H 0.3226 0.4751 0.7314 0.034 Uiso 1 1 calc R . . H11B H 0.4182 0.5232 0.7921 0.034 Uiso 1 1 calc R . . F10 F -0.2225(10) 0.6896(3) 0.4218(7) 0.096(3) Uani 1 1 d U . . F4 F 0.4536(9) 0.7122(3) 1.0276(6) 0.080(2) Uani 1 1 d U . . C8 C 0.1189(13) 0.5952(4) 1.0232(9) 0.046(4) Uani 1 1 d . . . H8A H 0.1554 0.6181 1.0834 0.069 Uiso 1 1 calc R . . H8B H 0.2029 0.5756 1.0148 0.069 Uiso 1 1 calc R . . H8C H 0.0451 0.5714 1.0342 0.069 Uiso 1 1 calc R . . C7 C -0.0796(11) 0.6530(4) 0.9338(8) 0.030(3) Uani 1 1 d U . . H7A H -0.0571 0.6695 1.0030 0.036 Uiso 1 1 calc R . . H7B H -0.1638 0.6289 0.9245 0.036 Uiso 1 1 calc R . . C10 C 0.2904(12) 0.5407(4) 0.6400(9) 0.029(3) Uani 1 1 d . . . H10A H 0.3748 0.5361 0.6127 0.035 Uiso 1 1 calc R . . H10B H 0.1981 0.5275 0.5877 0.035 Uiso 1 1 calc R . . F12 F -0.2230(11) 0.6415(3) 0.2947(6) 0.106(3) Uani 1 1 d U . . C6 C -0.1220(13) 0.6931(4) 0.8498(9) 0.038(3) Uani 1 1 d U . . H6A H -0.2202 0.7085 0.8438 0.046 Uiso 1 1 calc R . . H6B H -0.0460 0.7208 0.8644 0.046 Uiso 1 1 calc R . . C12 C 0.1994(13) 0.4922(5) 0.8690(9) 0.041(3) Uani 1 1 d . . . H12A H 0.1832 0.4567 0.8438 0.062 Uiso 1 1 calc R . . H12B H 0.1192 0.5024 0.8962 0.062 Uiso 1 1 calc R . . H12C H 0.2959 0.4947 0.9246 0.062 Uiso 1 1 calc R . . C5 C -0.2714(12) 0.6796(5) 0.6659(9) 0.045(3) Uani 1 1 d . . . H5A H -0.3560 0.6786 0.6926 0.067 Uiso 1 1 calc R . . H5B H -0.2892 0.6555 0.6077 0.067 Uiso 1 1 calc R . . H5C H -0.2608 0.7144 0.6416 0.067 Uiso 1 1 calc R . . C3 C 0.2769(17) 0.7849(5) 0.7823(12) 0.059(3) Uani 1 1 d U . . 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 C2 0.050(6) 0.097(6) 0.034(5) -0.015(5) 0.018(5) -0.013(6) C1 0.058(6) 0.037(5) 0.048(5) 0.000(5) 0.027(5) -0.013(5) C4 0.098(7) 0.077(7) 0.056(6) 0.020(6) 0.002(6) -0.017(6) U1 0.0172(2) 0.0262(2) 0.0204(2) 0.0018(3) 0.00457(15) -0.0017(3) S1 0.0178(17) 0.0264(17) 0.0332(19) -0.0014(14) 0.0128(14) -0.0040(14) S2 0.0170(17) 0.039(2) 0.0257(17) -0.0006(14) 0.0039(14) 0.0010(14) S3 0.0318(19) 0.0244(18) 0.038(2) 0.0041(15) 0.0088(16) -0.0018(15) S4 0.0295(19) 0.040(2) 0.0248(18) 0.0030(14) 0.0001(15) -0.0081(15) O1 0.020(4) 0.024(4) 0.044(5) 0.014(4) 0.009(4) 0.008(4) O13 0.034(5) 0.017(4) 0.024(4) 0.004(4) 0.001(4) -0.012(4) C9 0.048(8) 0.038(8) 0.032(7) -0.002(6) 0.018(6) -0.017(6) O10 0.022(4) 0.028(4) 0.026(4) 0.000(4) 0.003(3) -0.004(4) O14 0.019(4) 0.027(5) 0.029(4) 0.011(3) 0.017(3) 0.004(3) O3 0.052(6) 0.043(5) 0.024(5) -0.002(4) 0.021(4) -0.002(4) O15 0.031(4) 0.033(5) 0.018(4) -0.009(3) 0.007(4) -0.005(4) O16 0.022(4) 0.033(5) 0.031(5) 0.002(4) 0.011(4) 0.002(4) F1 0.091(5) 0.055(5) 0.038(4) -0.013(4) 0.012(4) -0.010(4) O4 0.026(4) 0.057(6) 0.015(4) -0.005(4) 0.011(3) 0.006(4) O7 0.037(5) 0.027(5) 0.033(5) -0.003(4) 0.014(4) 0.007(4) F3 0.066(5) 0.028(4) 0.069(5) -0.007(4) 0.033(4) 0.005(3) F7 0.087(5) 0.061(5) 0.056(5) -0.012(4) 0.011(5) -0.003(4) O6 0.039(5) 0.052(6) 0.040(5) 0.003(4) 0.014(4) -0.007(4) O9 0.058(6) 0.040(5) 0.038(5) 0.012(4) 0.028(5) -0.002(4) O8 0.032(5) 0.037(5) 0.068(6) 0.007(4) 0.017(5) 0.006(4) O11 0.044(6) 0.063(6) 0.039(6) 0.007(5) 0.004(5) -0.015(5) F8 0.035(4) 0.051(5) 0.099(6) 0.003(4) 0.002(5) -0.007(4) O2 0.016(4) 0.038(5) 0.053(6) 0.001(4) 0.008(4) 0.002(4) F2 0.057(5) 0.047(4) 0.079(5) -0.016(4) 0.030(4) -0.025(4) O12 0.052(6) 0.052(6) 0.034(5) -0.015(4) 0.003(5) -0.004(5) F5 0.043(4) 0.111(6) 0.036(4) -0.017(4) -0.001(4) -0.034(4) F9 0.082(5) 0.031(4) 0.083(5) 0.003(4) -0.005(4) -0.010(4) O5 0.038(5) 0.050(6) 0.038(5) 0.007(4) -0.004(4) 0.013(4) F6 0.066(5) 0.127(6) 0.033(4) -0.020(4) 0.021(4) -0.027(5) F11 0.090(6) 0.088(6) 0.060(5) 0.029(4) 0.021(5) -0.027(5) C11 0.016(6) 0.033(7) 0.037(8) -0.013(6) 0.010(6) 0.002(5) F10 0.104(7) 0.069(6) 0.095(6) 0.033(5) 0.005(5) -0.001(5) F4 0.088(6) 0.084(6) 0.059(5) -0.034(4) 0.012(4) 0.023(5) C8 0.043(8) 0.075(10) 0.025(7) 0.006(7) 0.016(7) -0.006(7) C7 0.014(6) 0.050(7) 0.027(6) -0.013(5) 0.008(5) -0.005(5) C10 0.023(7) 0.032(7) 0.037(8) -0.014(6) 0.014(6) -0.008(6) F12 0.134(7) 0.110(6) 0.041(5) 0.027(5) -0.017(5) -0.030(6) C6 0.024(6) 0.039(7) 0.047(7) -0.008(6) 0.006(6) 0.005(5) C12 0.039(8) 0.053(9) 0.039(8) 0.015(7) 0.023(7) 0.008(7) C5 0.024(7) 0.056(9) 0.048(8) 0.007(7) 0.003(7) 0.008(7) C3 0.060(5) 0.036(5) 0.071(6) 0.008(5) 0.008(6) -0.003(5) _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 C2 F5 1.294(14) . ? C2 F6 1.309(14) . ? C2 F4 1.315(15) . ? C2 S2 1.802(14) . ? C1 F1 1.290(13) . ? C1 F2 1.317(13) . ? C1 F3 1.324(14) . ? C1 S1 1.815(13) . ? C4 F12 1.291(17) . ? C4 F11 1.294(18) . ? C4 F10 1.303(18) . ? C4 S4 1.795(16) . ? U1 O7 2.258(7) . ? U1 O10 2.262(6) . ? U1 O4 2.282(6) . ? U1 O1 2.299(7) . ? U1 O13 2.392(7) . ? U1 O15 2.444(7) . ? U1 O16 2.445(7) . ? U1 O14 2.462(6) . ? S1 O2 1.399(7) . ? S1 O3 1.413(7) . ? S1 O1 1.466(7) . ? S2 O5 1.401(8) . ? S2 O6 1.412(7) . ? S2 O4 1.494(7) . ? S3 O8 1.396(7) . ? S3 O9 1.416(7) . ? S3 O7 1.490(7) . ? S3 C3 1.775(14) . ? S4 O12 1.410(8) . ? S4 O11 1.414(8) . ? S4 O10 1.484(7) . ? O13 C6 1.468(12) . ? O13 C5 1.494(11) . ? C9 O15 1.448(11) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? O14 C7 1.398(11) . ? O14 C8 1.446(11) . ? O15 C10 1.452(11) . ? O16 C12 1.422(11) . ? O16 C11 1.444(11) . ? F7 C3 1.338(15) . ? F8 C3 1.292(15) . ? F9 C3 1.319(14) . ? C11 C10 1.481(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7 C6 1.470(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 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 F5 C2 F6 108.4(12) . . ? F5 C2 F4 108.4(13) . . ? F6 C2 F4 108.6(12) . . ? F5 C2 S2 110.1(10) . . ? F6 C2 S2 110.0(10) . . ? F4 C2 S2 111.2(10) . . ? F1 C1 F2 108.9(11) . . ? F1 C1 F3 108.5(11) . . ? F2 C1 F3 107.3(10) . . ? F1 C1 S1 112.0(9) . . ? F2 C1 S1 109.3(9) . . ? F3 C1 S1 110.7(9) . . ? F12 C4 F11 108.0(15) . . ? F12 C4 F10 107.1(15) . . ? F11 C4 F10 106.1(14) . . ? F12 C4 S4 110.5(12) . . ? F11 C4 S4 112.8(12) . . ? F10 C4 S4 112.0(13) . . ? O7 U1 O10 83.6(2) . . ? O7 U1 O4 78.0(2) . . ? O10 U1 O4 149.0(2) . . ? O7 U1 O1 148.0(2) . . ? O10 U1 O1 78.3(3) . . ? O4 U1 O1 128.5(3) . . ? O7 U1 O13 75.1(2) . . ? O10 U1 O13 77.5(2) . . ? O4 U1 O13 120.5(2) . . ? O1 U1 O13 75.3(2) . . ? O7 U1 O15 81.4(2) . . ? O10 U1 O15 74.0(2) . . ? O4 U1 O15 78.7(2) . . ? O1 U1 O15 117.7(2) . . ? O13 U1 O15 144.7(2) . . ? O7 U1 O16 141.4(2) . . ? O10 U1 O16 103.9(2) . . ? O4 U1 O16 76.9(2) . . ? O1 U1 O16 69.4(2) . . ? O13 U1 O16 143.4(2) . . ? O15 U1 O16 65.2(2) . . ? O7 U1 O14 99.4(2) . . ? O10 U1 O14 139.0(2) . . ? O4 U1 O14 69.4(2) . . ? O1 U1 O14 78.4(2) . . ? O13 U1 O14 64.2(2) . . ? O15 U1 O14 147.0(2) . . ? O16 U1 O14 98.7(2) . . ? O2 S1 O3 119.0(5) . . ? O2 S1 O1 112.1(4) . . ? O3 S1 O1 110.3(5) . . ? O2 S1 C1 106.3(6) . . ? O3 S1 C1 105.6(5) . . ? O1 S1 C1 101.7(5) . . ? O5 S2 O6 119.8(5) . . ? O5 S2 O4 111.9(5) . . ? O6 S2 O4 112.7(4) . . ? O5 S2 C2 104.1(6) . . ? O6 S2 C2 104.4(6) . . ? O4 S2 C2 101.3(5) . . ? O8 S3 O9 118.5(5) . . ? O8 S3 O7 111.5(5) . . ? O9 S3 O7 112.5(4) . . ? O8 S3 C3 105.8(6) . . ? O9 S3 C3 105.9(6) . . ? O7 S3 C3 100.4(6) . . ? O12 S4 O11 119.3(5) . . ? O12 S4 O10 112.5(4) . . ? O11 S4 O10 111.9(5) . . ? O12 S4 C4 104.6(8) . . ? O11 S4 C4 105.4(7) . . ? O10 S4 C4 100.8(7) . . ? S1 O1 U1 152.8(5) . . ? C6 O13 C5 109.0(8) . . ? C6 O13 U1 117.1(6) . . ? C5 O13 U1 133.4(6) . . ? O15 C9 H9A 109.5 . . ? O15 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O15 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? S4 O10 U1 156.8(5) . . ? C7 O14 C8 112.0(8) . . ? C7 O14 U1 120.1(6) . . ? C8 O14 U1 125.6(6) . . ? C9 O15 C10 110.2(7) . . ? C9 O15 U1 126.7(6) . . ? C10 O15 U1 115.7(6) . . ? C12 O16 C11 111.0(8) . . ? C12 O16 U1 125.0(6) . . ? C11 O16 U1 119.5(6) . . ? S2 O4 U1 149.5(4) . . ? S3 O7 U1 158.5(4) . . ? O16 C11 C10 107.3(8) . . ? O16 C11 H11A 110.3 . . ? C10 C11 H11A 110.3 . . ? O16 C11 H11B 110.3 . . ? C10 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? O14 C8 H8A 109.5 . . ? O14 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O14 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O14 C7 C6 109.2(9) . . ? O14 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? O14 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? O15 C10 C11 106.1(8) . . ? O15 C10 H10A 110.5 . . ? C11 C10 H10A 110.5 . . ? O15 C10 H10B 110.5 . . ? C11 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? O13 C6 C7 104.4(9) . . ? O13 C6 H6A 110.9 . . ? C7 C6 H6A 110.9 . . ? O13 C6 H6B 110.9 . . ? C7 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? O16 C12 H12A 109.5 . . ? O16 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O16 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O13 C5 H5A 109.5 . . ? O13 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O13 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? F8 C3 F9 108.2(12) . . ? F8 C3 F7 106.1(12) . . ? F9 C3 F7 107.6(12) . . ? F8 C3 S3 112.6(11) . . ? F9 C3 S3 110.6(10) . . ? F7 C3 S3 111.4(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 C1 S1 O2 54.3(11) . . . . ? F2 C1 S1 O2 -66.5(10) . . . . ? F3 C1 S1 O2 175.5(8) . . . . ? F1 C1 S1 O3 -178.3(9) . . . . ? F2 C1 S1 O3 60.8(10) . . . . ? F3 C1 S1 O3 -57.1(10) . . . . ? F1 C1 S1 O1 -63.2(11) . . . . ? F2 C1 S1 O1 176.0(9) . . . . ? F3 C1 S1 O1 58.0(9) . . . . ? F5 C2 S2 O5 65.9(12) . . . . ? F6 C2 S2 O5 -53.5(11) . . . . ? F4 C2 S2 O5 -173.8(10) . . . . ? F5 C2 S2 O6 -60.5(12) . . . . ? F6 C2 S2 O6 -179.8(10) . . . . ? F4 C2 S2 O6 59.8(11) . . . . ? F5 C2 S2 O4 -177.7(10) . . . . ? F6 C2 S2 O4 62.9(11) . . . . ? F4 C2 S2 O4 -57.5(11) . . . . ? F12 C4 S4 O12 63.4(15) . . . . ? F11 C4 S4 O12 -57.7(14) . . . . ? F10 C4 S4 O12 -177.3(11) . . . . ? F12 C4 S4 O11 -63.2(15) . . . . ? F11 C4 S4 O11 175.7(12) . . . . ? F10 C4 S4 O11 56.1(14) . . . . ? F12 C4 S4 O10 -179.7(13) . . . . ? F11 C4 S4 O10 59.2(14) . . . . ? F10 C4 S4 O10 -60.4(13) . . . . ? O2 S1 O1 U1 67.9(11) . . . . ? O3 S1 O1 U1 -67.2(11) . . . . ? C1 S1 O1 U1 -178.9(10) . . . . ? O7 U1 O1 S1 -61.3(12) . . . . ? O10 U1 O1 S1 -118.1(10) . . . . ? O4 U1 O1 S1 79.4(10) . . . . ? O13 U1 O1 S1 -38.1(9) . . . . ? O15 U1 O1 S1 177.2(9) . . . . ? O16 U1 O1 S1 131.9(10) . . . . ? O14 U1 O1 S1 27.9(10) . . . . ? O7 U1 O13 C6 -80.4(7) . . . . ? O10 U1 O13 C6 -167.0(7) . . . . ? O4 U1 O13 C6 -14.3(7) . . . . ? O1 U1 O13 C6 112.1(7) . . . . ? O15 U1 O13 C6 -130.3(6) . . . . ? O16 U1 O13 C6 96.4(7) . . . . ? O14 U1 O13 C6 28.1(6) . . . . ? O7 U1 O13 C5 90.9(8) . . . . ? O10 U1 O13 C5 4.3(8) . . . . ? O4 U1 O13 C5 157.0(8) . . . . ? O1 U1 O13 C5 -76.6(8) . . . . ? O15 U1 O13 C5 40.9(9) . . . . ? O16 U1 O13 C5 -92.4(9) . . . . ? O14 U1 O13 C5 -160.6(9) . . . . ? O12 S4 O10 U1 -59.2(11) . . . . ? O11 S4 O10 U1 78.4(11) . . . . ? C4 S4 O10 U1 -170.1(11) . . . . ? O7 U1 O10 S4 164.7(10) . . . . ? O4 U1 O10 S4 111.0(10) . . . . ? O1 U1 O10 S4 -41.8(10) . . . . ? O13 U1 O10 S4 -119.2(10) . . . . ? O15 U1 O10 S4 81.8(10) . . . . ? O16 U1 O10 S4 23.3(11) . . . . ? O14 U1 O10 S4 -98.3(10) . . . . ? O7 U1 O14 C7 70.7(7) . . . . ? O10 U1 O14 C7 -20.4(8) . . . . ? O4 U1 O14 C7 144.0(7) . . . . ? O1 U1 O14 C7 -76.8(6) . . . . ? O13 U1 O14 C7 2.4(6) . . . . ? O15 U1 O14 C7 159.4(6) . . . . ? O16 U1 O14 C7 -143.6(6) . . . . ? O7 U1 O14 C8 -128.0(7) . . . . ? O10 U1 O14 C8 140.9(7) . . . . ? O4 U1 O14 C8 -54.7(7) . . . . ? O1 U1 O14 C8 84.5(7) . . . . ? O13 U1 O14 C8 163.7(8) . . . . ? O15 U1 O14 C8 -39.3(9) . . . . ? O16 U1 O14 C8 17.7(7) . . . . ? O7 U1 O15 C9 -28.6(7) . . . . ? O10 U1 O15 C9 57.2(7) . . . . ? O4 U1 O15 C9 -108.0(7) . . . . ? O1 U1 O15 C9 124.2(7) . . . . ? O13 U1 O15 C9 19.9(9) . . . . ? O16 U1 O15 C9 171.3(8) . . . . ? O14 U1 O15 C9 -122.7(7) . . . . ? O7 U1 O15 C10 -175.2(6) . . . . ? O10 U1 O15 C10 -89.5(6) . . . . ? O4 U1 O15 C10 105.4(6) . . . . ? O1 U1 O15 C10 -22.4(7) . . . . ? O13 U1 O15 C10 -126.8(6) . . . . ? O16 U1 O15 C10 24.7(6) . . . . ? O14 U1 O15 C10 90.7(7) . . . . ? O7 U1 O16 C12 128.4(7) . . . . ? O10 U1 O16 C12 -134.3(7) . . . . ? O4 U1 O16 C12 77.6(8) . . . . ? O1 U1 O16 C12 -62.8(8) . . . . ? O13 U1 O16 C12 -46.6(9) . . . . ? O15 U1 O16 C12 161.0(8) . . . . ? O14 U1 O16 C12 11.2(8) . . . . ? O7 U1 O16 C11 -25.6(8) . . . . ? O10 U1 O16 C11 71.7(7) . . . . ? O4 U1 O16 C11 -76.4(6) . . . . ? O1 U1 O16 C11 143.2(7) . . . . ? O13 U1 O16 C11 159.4(6) . . . . ? O15 U1 O16 C11 7.0(6) . . . . ? O14 U1 O16 C11 -142.8(6) . . . . ? O5 S2 O4 U1 -93.0(9) . . . . ? O6 S2 O4 U1 45.6(10) . . . . ? C2 S2 O4 U1 156.6(9) . . . . ? O7 U1 O4 S2 -75.5(9) . . . . ? O10 U1 O4 S2 -20.6(12) . . . . ? O1 U1 O4 S2 124.6(9) . . . . ? O13 U1 O4 S2 -140.1(8) . . . . ? O15 U1 O4 S2 8.0(9) . . . . ? O16 U1 O4 S2 74.8(9) . . . . ? O14 U1 O4 S2 179.5(10) . . . . ? O8 S3 O7 U1 44.4(13) . . . . ? O9 S3 O7 U1 -91.6(12) . . . . ? C3 S3 O7 U1 156.2(12) . . . . ? O10 U1 O7 S3 39.4(12) . . . . ? O4 U1 O7 S3 -165.7(12) . . . . ? O1 U1 O7 S3 -16.2(15) . . . . ? O13 U1 O7 S3 -39.4(12) . . . . ? O15 U1 O7 S3 114.1(12) . . . . ? O16 U1 O7 S3 143.8(11) . . . . ? O14 U1 O7 S3 -99.3(12) . . . . ? C12 O16 C11 C10 167.1(9) . . . . ? U1 O16 C11 C10 -35.5(10) . . . . ? C8 O14 C7 C6 165.7(9) . . . . ? U1 O14 C7 C6 -30.6(10) . . . . ? C9 O15 C10 C11 156.4(8) . . . . ? U1 O15 C10 C11 -51.7(9) . . . . ? O16 C11 C10 O15 53.9(10) . . . . ? C5 O13 C6 C7 133.7(8) . . . . ? U1 O13 C6 C7 -53.0(9) . . . . ? O14 C7 C6 O13 50.7(11) . . . . ? O8 S3 C3 F8 179.6(10) . . . . ? O9 S3 C3 F8 -53.7(11) . . . . ? O7 S3 C3 F8 63.5(11) . . . . ? O8 S3 C3 F9 -59.2(12) . . . . ? O9 S3 C3 F9 67.5(12) . . . . ? O7 S3 C3 F9 -175.3(10) . . . . ? O8 S3 C3 F7 60.5(11) . . . . ? O9 S3 C3 F7 -172.8(9) . . . . ? O7 S3 C3 F7 -55.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 26.91 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 2.210 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.196