Potassium‒sodium double salt of decavanadate, K~4~Na~2~[V~10~O~28~]·10H~2~O
Lee, Uk; Joo, Hea-Chung; Acta Crystallographica Section E 59 (2003) i122–i124; doi:10.1107/S1600536803016453

data_2202295
_publ_section_title
;
 Potassium--sodium double salt of decavanadate,
 K~4~Na~2~[V~10~O~28~]&#x00B7;10H~2~O
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i122
_journal_page_last               i124
_journal_paper_doi               10.1107/S1600536803016453
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'Na2 K4 (V10 O28), 10H2 O'
_chemical_formula_moiety         'O28 V10 6-, 10(H2 O), 4(K) 4+, 2(Na) 2+'
_chemical_formula_structural     'Na2 K4 (V10 O28) (H2 O)10'
_chemical_formula_sum            'H20 K4 Na2 O38 V10'
_chemical_formula_weight         1339.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.220(10)
_cell_angle_beta                 87.140(10)
_cell_angle_gamma                66.120(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6200(10)
_cell_length_b                   10.3870(10)
_cell_length_c                   11.017(2)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.5
_cell_measurement_theta_min      9.5
_cell_volume                     838.2(2)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1996)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       \w/2-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3845
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        3.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.302
_exptl_absorpt_correction_T_max  0.534
_exptl_absorpt_correction_T_min  0.317
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    2.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.8027P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                3393
_reflns_number_total             3845
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br6109.cif
_cod_data_source_block           I
_cod_database_code               2202295
_cod_database_fobs_code          2202295