KNb~1.75~V~0.25~PS~10~
Yu, Jaemin; Yun, Hoseop; Acta Crystallographica Section E 67 (2011) i24–; doi:10.1107/S1600536811004430

data_2229374
_publ_section_title
;
 KNb~1.75~V~0.25~PS~10~
;
_journal_coeditor_code           FJ2392
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i24
_journal_paper_doi               10.1107/S1600536811004430
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'K Nb1.75 V0.25 P S10'
_chemical_formula_moiety         'Nb7 P4 S40 V, 4(K)'
_chemical_formula_sum            'K4 Nb7 P4 S40 V'
_chemical_formula_weight         2264.39
_chemical_name_systematic
;
potassium diniobium vanadium phosphorus decasulfide
;
_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            1
_cell_length_a                   12.9696(3)
_cell_length_b                   7.5229(2)
_cell_length_c                   13.3248(4)
_cell_measurement_reflns_used    11171
_cell_measurement_temperature    290.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.06
_cell_volume                     1300.09(6)
_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
'STRUCTURE TIDY (Gelato & Parth\'e, 1987) and WinGX (Farrugia, 1999)'
_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'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_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            11855
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.725
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.284
_refine_ls_abs_structure_details 'Flack (1983), <b>1417 Friedel pairs</b>'
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2970
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_gt           0.019
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0125P)^2^+1.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0424
_reflns_number_gt                2859
_reflns_number_total             2970
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fj2392.cif
_cod_data_source_block           I
_cod_database_code               2229374
_cod_database_fobs_code          2229374