Synthesis and Structural Characterization of Quaternary Thorium Selenophosphates: A2ThP3Se9 (A = K, Rb) and Cs4Th2P5Se17
Paula M. Briggs Piccoli; Kent D. Abney; Jon R. Schoonover; Peter K. Dorhout; Inorganic Chemistry 39 (2000) 2970–2976; doi:10.1021/ic990767w

data_4321122
_publ_section_title
;
 Synthesis and Structural Characterization of Quaternary Thorium
 Selenophosphates: A2ThP3Se9 (A = K, Rb) and Cs4Th2P5Se17
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2970
_journal_page_last               2976
_journal_paper_doi               10.1021/ic990767w
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'Cs4 P5 Se17 Th2'
_chemical_formula_weight         2492.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.8320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2378(5)
_cell_length_b                   32.182(2)
_cell_length_c                   10.7492(6)
_cell_measurement_temperature    223(2)
_cell_volume                     3523.2(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18798
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    30.295
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.700
_exptl_crystal_description       rod
_exptl_crystal_F_000             4212
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.094
_refine_diff_density_min         -1.849
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.000418(14)
_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_all   1.148
_refine_ls_goodness_of_fit_obs   1.136
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         7056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_restrained_S_obs      1.136
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_obs          0.0262
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+19.3271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0626
_refine_ls_wR_factor_obs         0.0585
_reflns_number_observed          6308
_reflns_number_total             7056
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990767w_1.cif
_cod_data_source_block           pmb1149
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+19.3271P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+19.3271P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3523.3(3)
_cod_database_code               4321122