Solvothermal Synthesis and Structure of a New Selenium-Rich Selenophosphate K3PSe4.2Se6
Christine A. Dickerson; Mary J. Fisher; Richard E. Sykora; Thomas E. Albrecht-Schmitt; Jason A. Cody; Inorganic Chemistry 41 (2002) 640–642; doi:10.1021/ic015602d

data_4317612
_publ_section_title
;
 Solvothermal Synthesis and Structure of a New Selenium-Rich
 Selenophosphate K3PSe4.2Se6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              640
_journal_page_last               642
_journal_paper_doi               10.1021/ic015602d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'K3 P Se16'
_chemical_formula_sum            'K3 P Se16'
_chemical_formula_weight         1411.63
_chemical_name_systematic
; 
 potassium selenophosphate bishexaselenium(0)
;
_space_group_IT_number           203
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 2uv 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.4151(19)
_cell_length_b                   16.4151(19)
_cell_length_c                   16.4151(19)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.15
_cell_volume                     4423.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10487
_diffrn_reflns_theta_full        28.15
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    27.007
_exptl_absorpt_correction_T_max  '0.668548 ratio of min/max'
_exptl_absorpt_correction_T_min  '0.668548 ratio of min/max'
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    4.240
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             4928
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+12.1651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0420
_reflns_number_gt                445
_reflns_number_total             467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015602d_s1.cif
_cod_data_source_block           K3PSe4.2Se6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_sg_symbol_H-M      'F d -3'
_cod_database_code               4317612