From Order to Disorder and Back Again: In Situ Hydrothermal Redox Reactions of Uranium Phosphites and Phosphates
Eric M. Villa; Connor J. Marr; Juan Diwu; Evgeny V. Alekseev; Wulf Depmeier; Thomas E. Albrecht-Schmitt; Inorganic Chemistry 52 (2013) 965–973; doi:10.1021/ic302198w

data_4333607
_publ_section_title
;
 From Order to Disorder and Back Again: In Situ Hydrothermal Redox
 Reactions of Uranium Phosphites and Phosphates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              965
_journal_page_last               973
_journal_paper_doi               10.1021/ic302198w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         Cs4[(UO2)8(HPO4)5(HPO3)5]*4H2O
_chemical_formula_sum            'Cs4 H4 O55 P10 U8'
_chemical_formula_weight         3629.61
_chemical_name_common            'Cesium Uranium(VI) Phosphate-Phosphite'
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.513(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.5005(7)
_cell_length_b                   10.9710(4)
_cell_length_c                   14.4752(6)
_cell_measurement_reflns_used    4276
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      3.85
_cell_volume                     2844.27(19)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'Imus microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16086
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    25.610
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            Light-Yellow
_exptl_crystal_density_diffrn    4.238
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3100
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.982
_refine_diff_density_min         -2.841
_refine_diff_density_rms         0.434
_refine_ls_extinction_coef       0.00013(2)
_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   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+20.3839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                2980
_reflns_number_total             4276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302198w_si_002_1.cif
_cod_data_source_block           Cs_U(IV)_PO4/PO3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'N/A' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4333607