#------------------------------------------------------------------------------ #$Date: 2017-02-21 10:03:24 +0000 (Tue, 21 Feb 2017) $ #$Revision: 192412 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/00/4000089.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_4000089 loop_ _publ_author_name 'Li, Yaping' 'Cahill, Christopher L.' 'Burns, Peter C.' _publ_section_title ; Synthesis, Structural Characterization, and Topological Rearrangement of a Novel Open Framework U−O Material:  (NH4)3(H2O)2{[(UO2)10O10(OH)][(UO4)(H2O)2] ; _journal_issue 11 _journal_name_full 'Chemistry of Materials' _journal_page_first 4026 _journal_page_last 4031 _journal_paper_doi 10.1021/cm0008359 _journal_volume 13 _journal_year 2001 _chemical_formula_sum 'H21 N3 O39 U11' _chemical_formula_weight 3305.53 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 103.930(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.6273(18) _cell_length_b 21.161(3) _cell_length_c 14.706(2) _cell_measurement_reflns_used 1065 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.33 _cell_measurement_theta_min 1.92 _cell_volume 3512.0(9) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.964 _diffrn_measured_fraction_theta_max 0.964 _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 0.1068 _diffrn_reflns_av_sigmaI/netI 0.1892 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10920 _diffrn_reflns_theta_full 28.33 _diffrn_reflns_theta_max 28.33 _diffrn_reflns_theta_min 1.92 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 50.643 _exptl_absorpt_correction_type semi-empirical _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 6.252 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 5464 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 7.544 _refine_diff_density_min -8.344 _refine_diff_density_rms 0.922 _refine_ls_extinction_coef 0.000019(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 1.009 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 4230 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.1613 _refine_ls_R_factor_gt 0.0770 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1601 _refine_ls_wR_factor_ref 0.1812 _reflns_number_gt 2180 _reflns_number_total 4230 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M C2/c _cod_database_code 4000089 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 0.25414(12) 0.09071(6) 0.01753(10) 0.0070(3) Uani 1 1 d . . . U2 U -0.2500 0.2500 0.0000 0.0541(11) Uani 1 2 d S . . U3 U -0.05891(11) 0.07896(7) 0.02011(9) 0.0066(3) Uani 1 1 d . . . U4 U 0.57146(10) 0.07835(7) 0.02372(9) 0.0069(3) Uani 1 1 d . . . U5 U 0.81966(12) 0.07488(7) 0.22681(9) 0.0087(3) Uani 1 1 d . . . U6 U 0.05336(12) 0.25048(7) -0.00295(10) 0.0062(3) Uani 1 1 d . . . O1 O 0.222(2) 0.1144(12) -0.1075(17) 0.013(6) Uiso 1 1 d . . . O2 O 0.282(2) 0.0750(12) 0.1484(16) 0.012(5) Uiso 1 1 d . . . O3 O -0.118(3) 0.1917(13) 0.016(2) 0.030(8) Uiso 1 1 d . . . O4 O -0.120(2) 0.0914(12) -0.1038(18) 0.018(6) Uiso 1 1 d . . . O5 O -0.0035(19) 0.0747(11) 0.1600(16) 0.009(5) Uiso 1 1 d . . . O6 O 0.548(2) 0.0920(11) -0.1006(18) 0.017(6) Uiso 1 1 d . . . O7 O 0.609(2) 0.0685(12) 0.1566(18) 0.017(6) Uiso 1 1 d . . . O8 O 0.827(2) -0.0037(12) 0.2260(19) 0.017(6) Uiso 1 1 d . . . O9 O 0.809(2) 0.1621(12) 0.227(2) 0.020(7) Uiso 1 1 d . . . O10 O 0.025(3) 0.2320(14) -0.121(2) 0.032(8) Uiso 1 1 d . . . O11 O 0.085(3) 0.2688(14) 0.118(2) 0.039(9) Uiso 1 1 d . . . O12 O 0.7707(17) 0.0767(10) 0.0641(14) 0.002(4) Uiso 1 1 d . . . O13 O 0.424(2) 0.1460(12) 0.0443(18) 0.018(6) Uiso 1 1 d . . . O14 O 0.395(2) 0.0249(12) 0.0035(17) 0.012(6) Uiso 1 1 d . . . O15 O 0.096(2) 0.1468(12) 0.027(2) 0.022(7) Uiso 1 1 d . . . O16 O -0.367(3) 0.1914(13) 0.030(2) 0.026(7) Uiso 1 1 d . . . O17 O -0.101(2) -0.0247(13) 0.0038(19) 0.023(7) Uiso 1 1 d . . . OH18 O 0.2500 0.2500 0.0000 0.050(14) Uiso 1 2 d S . . OW19 O -0.176(3) 0.2820(18) 0.158(3) 0.066(12) Uiso 1 1 d . . . OW20 O 0.5000 0.160(2) 0.2500 0.036(12) Uiso 1 2 d S . . OW21 O 0.673(5) 0.227(3) 0.265(4) 0.020 Uiso 0.50 1 d P . . N1 N 0.0000 0.112(2) -0.2500 0.018(11) Uiso 1 2 d S . . N2 N 0.673(3) -0.1022(15) 0.254(2) 0.020 Uiso 1 1 d . . . 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 0.0045(6) 0.0091(7) 0.0077(7) -0.0043(6) 0.0018(5) -0.0017(6) U2 0.0099(13) 0.0156(12) 0.143(3) 0.0300(18) 0.0307(16) 0.0041(12) U3 0.0072(7) 0.0084(7) 0.0050(7) 0.0019(6) 0.0029(5) 0.0009(6) U4 0.0055(7) 0.0103(7) 0.0043(7) -0.0006(6) 0.0002(5) 0.0006(6) U5 0.0122(7) 0.0044(7) 0.0095(8) -0.0027(6) 0.0023(5) -0.0021(6) U6 0.0049(7) 0.0068(6) 0.0070(7) 0.0021(6) 0.0017(5) 0.0009(6)