Crystal structure of hexakis(μ~3~-hydroxo)-tetra(μ~2~-hydroxo)-octadeca(μ~2~-oxo)-tetradecaoxo-disodium(I) dodecatungsten dodecahydrate, [Na(H2O)4]2(H10W12O42) · 12H2O
Zhang, Bi-Song; Zeitschrift für Kristallographie - New Crystal Structures 223 (2008) 317–318; doi:10.1524/ncrs.2008.0136

data_8102987
_publ_section_title
;
 Crystal structure of
 hexakis(\m~3~-hydroxo)-tetra(\m~2~-hydroxo)-octadeca(\m~2~-oxo)-tetradecaoxo-disodium(I)
 dodecatungsten dodecahydrate, [Na(H2O)4]2(H10W12O42) &#x00B7; 12H2O
;
_journal_coden_ASTM              ZKNSFT
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              317
_journal_page_last               318
_journal_paper_doi               10.1524/ncrs.2008.0136
_journal_volume                  223
_journal_year                    2008
_chemical_formula_sum            'H50 Na2 O62 W12'
_chemical_formula_weight         3294.58
_space_group_IT_number           61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.105(3)
_cell_length_b                   15.729(3)
_cell_length_c                   22.892(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5078.8(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0983
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45916
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    27.209
_exptl_crystal_density_diffrn    4.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5824
_refine_diff_density_max         3.074
_refine_diff_density_min         -4.434
_refine_diff_density_rms         0.561
_refine_ls_extinction_coef       0.000181(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         5807
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+45.7159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                4930
_reflns_number_total             5807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            409947.cff
_cod_data_source_block           shx97
_cod_original_cell_volume        5078.8(17)
_cod_database_code               8102987