#------------------------------------------------------------------------------ #$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/00/4000090.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000090 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_formula_sum 'Cl Cs3 H12 O25 U6' _chemical_formula_weight 2274.46 _space_group_IT_number 5 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 127.929(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 19.615(5) _cell_length_b 7.239(2) _cell_length_c 12.064(3) _cell_measurement_reflns_used 1099 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.28 _cell_measurement_theta_min 2.14 _cell_volume 1351.2(6) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.930 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_device_type 'Bruker 1K CCD' _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1170 _diffrn_reflns_av_sigmaI/netI 0.1532 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3750 _diffrn_reflns_theta_full 28.28 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 2.14 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 40.000 _exptl_absorpt_correction_type semi-empirical _exptl_crystal_colour green-yellow _exptl_crystal_density_diffrn 5.590 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1892 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _refine_diff_density_max 4.938 _refine_diff_density_min -4.162 _refine_diff_density_rms 0.957 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(3) _refine_ls_extinction_coef 0.00000(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 98 _refine_ls_number_reflns 2462 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0720 _refine_ls_shift/su_max 1.776 _refine_ls_shift/su_mean 0.020 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1596 _refine_ls_wR_factor_ref 0.1705 _reflns_number_gt 1800 _reflns_number_total 2462 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M 'C 2' _cod_original_formula_sum 'H12 Cl Cs3 O25 U6' _cod_database_code 4000090 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' 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 0.75876(9) 0.2139(2) 0.94977(16) 0.0088(4) Uani 1 1 d . . . U2 U 0.75869(9) 0.2139(2) 0.56766(15) 0.0088(3) Uani 1 1 d . . . U3 U 0.77972(10) 0.6426(2) 0.77975(16) 0.0092(4) Uani 1 1 d . . . Cs1 Cs 0.0000(2) 0.5127(5) 0.7817(4) 0.0253(8) Uani 1 1 d . . . Cs2 Cs 0.5000 0.3792(9) 0.5000 0.0449(16) Uani 1 2 d S . . Cl1 Cl 0.0000 0.205(3) 0.0000 0.036(5) Uani 1 2 d S . . O1 O 0.6482(18) 0.204(5) 0.506(3) 0.024(7) Uiso 1 1 d . . . O2 O 0.8959(19) 0.637(5) 0.892(3) 0.021(7) Uiso 1 1 d . . . O3 O 0.8661(19) 0.201(5) 0.628(3) 0.028(7) Uiso 1 1 d . . . O4 O 0.664(2) 0.664(6) 0.661(4) 0.044(11) Uiso 1 1 d . . . O5 O 0.867(2) 0.200(5) 0.103(3) 0.032(8) Uiso 1 1 d . . . O6 O 0.6519(19) 0.208(5) 0.791(3) 0.028(7) Uiso 1 1 d . . . O7 O 0.774(2) 0.520(5) 0.607(3) 0.019(7) Uiso 1 1 d . . . O8 O 0.772(2) 0.526(5) 0.937(3) 0.021(8) Uiso 1 1 d . . . OH9 O 0.7903(19) 0.891(4) 0.656(3) 0.015(7) Uiso 1 1 d . . . OH10 O 0.7955(19) 0.885(4) 0.938(3) 0.013(7) Uiso 1 1 d . . . OH11 O 0.8039(18) 0.276(4) 0.802(3) 0.011(6) Uiso 1 1 d . . . OW12 O 0.004(4) 0.917(9) 0.189(6) 0.09(2) Uiso 1 1 d . . . OW13 O 0.5000 0.926(11) 0.5000 0.08(2) Uiso 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 0.0131(8) 0.0056(7) 0.0107(7) 0.0002(8) 0.0088(6) -0.0005(8) U2 0.0138(8) 0.0053(7) 0.0082(7) -0.0020(8) 0.0072(6) -0.0012(8) U3 0.0125(8) 0.0081(7) 0.0091(8) -0.0026(7) 0.0077(7) -0.0020(7) Cs1 0.0169(16) 0.0226(17) 0.030(2) 0.0056(14) 0.0116(15) 0.0018(13) Cs2 0.019(3) 0.052(4) 0.050(4) 0.000 0.014(3) 0.000 Cl1 0.010(7) 0.061(13) 0.022(8) 0.000 0.002(6) 0.000