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_1562323
_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            'H8 O12 P4 Th'
_chemical_formula_weight         555.98
_chemical_name_systematic
; 
Alpha-Thorium (IV) tetra(hydrogenphosphanate)  
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 99.466(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.896(3)
_cell_length_b                   13.631(5)
_cell_length_c                   12.518(5)
_cell_measurement_temperature    296(2)
_cell_volume                     1160.7(8)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'CrystalMaker(R) (Palmer, 2011)'
_computing_publication_material  .
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13388
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    13.454
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1016
_refine_diff_density_max         1.886
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0410
_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+(0.0395P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                1944
_reflns_number_total             2735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-215-50.cif
_cod_data_source_block           thhp
_cod_original_cell_volume        1160.6(8)
_cod_original_sg_symbol_Hall     '-P 2yac'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1562323