K~4~Ta~4~P~4~S~24~
Gutzmann, Andreas; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section E 61 (2005) i20–i22; doi:10.1107/S1600536805001959

data_2205375
_publ_section_title
;
 K~4~Ta~4~P~4~S~24~
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i20
_journal_page_last               i22
_journal_paper_doi               10.1107/S1600536805001959
_journal_volume                  61
_journal_year                    2005
_chemical_formula_structural     'K2 ((Ta+5)2 (P S4)2 (S2) (S)2)'
_chemical_formula_sum            'K2 P2 S12 Ta2'
_chemical_formula_weight         886.76
_chemical_name_systematic
;
tetrapotassium tetratantalum tetraphosphorus tetracosasulfide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.356(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.6193(7)
_cell_length_b                   17.7307(13)
_cell_length_c                   15.8077(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     3623.0(4)
_computing_cell_refinement       'IPDS Program Package'
_computing_data_collection       'IPDS Program Package (Stoe & Cie, 1998)'
_computing_data_reduction        'IPDS Program Package'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'CIFTAB in SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34379
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.067
_exptl_absorpt_correction_T_max  0.314
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-SHAPE (Stoe & Cie, 1998) and X-RED (Stoe & Cie, 1998)]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.109
_refine_diff_density_min         -1.655
_refine_ls_extinction_coef       0.000392(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         8610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.029P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0550
_reflns_number_gt                6878
_reflns_number_total             8610
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm6048.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2205375
_cod_database_fobs_code          2205375