Solid-state actinide acid phosphites from phosphorous acid melts
Oh, George N.; Burns, Peter C.; Journal of Solid State Chemistry 215 (2014) 50–56; doi:10.1016/j.jssc.2014.03.029

data_1562325
_publ_section_title
;
 Solid-state actinide acid phosphites from phosphorous acid melts
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              50
_journal_page_last               56
_journal_paper_doi               10.1016/j.jssc.2014.03.029
_journal_volume                  215
_journal_year                    2014
_chemical_formula_sum            'H11 O12 P3 U'
_chemical_formula_weight         534.03
_chemical_name_systematic
; 
Uranium monophosphonate di(hydrogenphosphonate) 
monoaqua dihydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.770(5)
_cell_length_b                   9.622(4)
_cell_length_c                   17.956(7)
_cell_measurement_temperature    296(2)
_cell_volume                     2206.3(15)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'CrystalMaker(R) (Palmer, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_measurement_method       sphere
_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  0.1451
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24671
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    15.202
_exptl_absorpt_correction_T_max  0.491
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_refine_diff_density_max         2.514
_refine_diff_density_min         -1.795
_refine_diff_density_rms         0.349
_refine_ls_extinction_coef       0.00026(8)
_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   1.125
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0502
_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 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0479P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                1645
_reflns_number_total             2660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-215-50.cif
_cod_data_source_block           uhph
_cod_original_cell_volume        2206.4(16)
_cod_database_code               1562325