The mixed-metal tris(disulfide) thiophosphate, KNb~1.77~Ta~0.23~PS~10~
Lee, Yoonjeong; Yoon, Woojin; Yun, Hoseop; Acta Crystallographica Section E 70 (2014) i8–; doi:10.1107/S1600536814000592

data_2239016
_publ_section_title
;
 The mixed-metal tris(disulfide) thiophosphate, KNb~1.77~Ta~0.23~PS~10~
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i8
_journal_paper_doi               10.1107/S1600536814000592
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'K Nb1.77 Ta0.23 P S10'
_chemical_formula_sum            'K Nb1.77 P S10 Ta0.23'
_chemical_formula_weight         596.52
_chemical_name_common
;
Potassium niobium tris(disulfide) tantalum thiophosphate
;
_chemical_name_systematic
'<i>catena</i>-Poly[potassium [tri-\m-disulfido-\m-tetrathiophosphato-di[niobate(IV)/tantalate(IV)(0.885/0.115)]]]'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0049(3)
_cell_length_b                   7.5262(2)
_cell_length_c                   13.3616(3)
_cell_measurement_reflns_used    10926
_cell_measurement_temperature    290.0(10)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.05
_cell_volume                     1307.80(5)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 2006)'
_computing_molecular_graphics
'locally modified version of ORTEP (Johnson, 1965)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID S'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12074
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.446
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.03
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1133
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.642
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.102(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2974
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.021
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+0.4965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0403
_reflns_number_gt                2842
_reflns_number_total             2974
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ru2056sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1307.81(6)
_cod_database_code               2239016
_cod_database_fobs_code          2239016