Na~6~(H~2~O)~20~(V~10~O~28~)·4H~2~O, a novel polyvanadate(V) with a three-dimensional framework
Guo, Hong-Xu; Yao, Zhong-Liang; Acta Crystallographica Section C 63 (2007) i51–i53; doi:10.1107/S0108270107025395

data_2016018
_publ_section_title
;
 Na~6~(H~2~O)~20~(V~10~O~28~)&#x00B7;4H~2~O, a novel polyvanadate(V)
 with a three-dimensional framework
;
_journal_coeditor_code           BC3048
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i51
_journal_page_last               i53
_journal_paper_doi               10.1107/S0108270107025395
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Na6 (H2 O)20 (V10 O28), 4H2 O'
_chemical_formula_moiety         'O28 V10, 24(H2 O), 6(Na )'
_chemical_formula_sum            'H48 Na6 O52 V10'
_chemical_formula_weight         1527.72
_chemical_name_common            'sodium decavanadate(V) tetrahydrate'
_chemical_name_systematic
;
poly[[octa-\m-aqua-dodecaaqua-\m-octacosaoxidodecavanadato-hexasodium]
tetrahydrate]
;
_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                108.682(4)
_cell_angle_beta                 103.775(2)
_cell_angle_gamma                111.674(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5834(3)
_cell_length_b                   11.3803(3)
_cell_length_c                   11.6367(3)
_cell_measurement_reflns_used    4336
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.0631
_cell_volume                     1128.19(8)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11109
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.458
_refine_ls_extinction_coef       0.0033(8)
_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   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                3529
_reflns_number_total             4088
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bc3048.cif
_cod_data_source_block           I
_cod_original_cell_volume        1128.19(5)
_cod_database_code               2016018
_cod_database_fobs_code          2016018