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_4333610
_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         Cs10[U10(HPO3)4(HPO4)14(PO4)5]
_chemical_formula_sum            'Cs10 H0 O88 P23 U10'
_chemical_formula_weight         5829.71
_chemical_name_common            'Cesium Uranium(IV) Phosphate-Phosphite'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.8390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.2966(4)
_cell_length_b                   20.2914(5)
_cell_length_c                   13.9293(3)
_cell_measurement_reflns_used    4787
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      1.66
_cell_volume                     4365.03(18)
_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      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29210
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    23.143
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            'Dark Green'
_exptl_crystal_density_diffrn    4.435
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5038
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.701
_refine_diff_density_min         -4.168
_refine_diff_density_rms         0.327
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         4787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0228P)^2^+258.2321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                3920
_reflns_number_total             4787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302198w_si_002_4.cif
_cod_data_source_block           Cs_U(IV)_HPO3/HPO4_PO4
_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_original_cell_volume        4365.03(17)
_cod_database_code               4333610