Phase formation in the Ni2±WO42‒H±H2O system (Z = 1.00). Crystal structure and properties of sodium heteropolyhexatungsten nickelate(2+) Na4[Ni(OH)6W8O18].16H2O
G. M. Rozantsev; S. V. Radio; N. I. Gumerova; V. N. Baumev; O. B. Shishkin; Journal of Structural Chemistry 50 (2009) 296–305; doi:

data_1519109
_publ_section_title
;
 Phase formation in the Ni2+-WO42--H+-H2O system (Z = 1.00). Crystal
 structure and properties of sodium heteropolyhexatungsten nickelate(2+)
 Na4[Ni(OH)6W8O18].16H2O
;
_journal_name_full               'Journal of Structural Chemistry'
_journal_page_first              296
_journal_page_last               305
_journal_volume                  50
_journal_year                    2009
_chemical_formula_moiety         'H6 Ni O24 W6, 16(H2 O), 4(Na) '
_chemical_formula_sum            'H38 Na4 Ni O40 W6'
_chemical_formula_weight         1932.07
_chemical_name_systematic
; 
Tetrasodium Hexahydroxonickelohexatungstate-octadecaoxide hexadecahydrate 
;
_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
_cell_angle_alpha                69.268(13)
_cell_angle_beta                 71.069(12)
_cell_angle_gamma                83.816(11)
_cell_formula_units_Z            1
_cell_length_a                   8.0089(11)
_cell_length_b                   10.5758(14)
_cell_length_c                   12.1987(16)
_cell_measurement_reflns_used    24842
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.5593
_cell_measurement_theta_min      2.6813
_cell_volume                     914.0(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  Xcalibur-3
_diffrn_measurement_method       \w/\q-scans
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71487
_diffrn_reflns_theta_full        45.00
_diffrn_reflns_theta_max         45.71
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    19.470
_exptl_absorpt_correction_T_max  0.3427
_exptl_absorpt_correction_T_min  0.1582
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         6.445
_refine_diff_density_min         -3.268
_refine_diff_density_rms         0.325
_refine_ls_extinction_coef       0.00675(3)
_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   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         15220
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                9339
_reflns_number_total             15220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSC-2009-50-296-305.cif
_cod_data_source_block           d2d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 
;
_cod_database_code               1519109