Polyoxometalates from heteropoly “brown” precursors. A new structural class of mixed valence heteropolytungstates, [(XO4)WIV3WVI17O62Hx]n−
Dickman, Michael H.; Ozeki, Tomoji; Evans, Jr., Howard T.; Rong, Chaoying; Jameson, Geoffrey B.; Pope, Michael T.; Journal of the Chemical Society, Dalton Transactions  (2000) 149–; doi:10.1039/a905539h

data_7008884
_publ_section_title
;
 Polyoxometalates from heteropoly &#x201C;brown&#x201D; precursors. A
 new structural class of mixed valence heteropolytungstates,
 [(XO4)WIV3WVI17O62Hx]n&#x2212;
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              149
_journal_paper_doi               10.1039/a905539h
_journal_year                    2000
_chemical_formula_sum            'K10 Na O84 W20'
_chemical_formula_weight         5434.99
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                66.833(1)
_cell_angle_beta                 85.364(1)
_cell_angle_gamma                76.265(1)
_cell_formula_units_Z            2
_cell_length_a                   12.2390(3)
_cell_length_b                   18.0490(4)
_cell_length_c                   20.5090(5)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      1.26
_cell_volume                     4045.64(17)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1339
_diffrn_reflns_av_sigmaI/netI    0.1750
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43951
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    28.937
_exptl_absorpt_correction_T_max  0.152
_exptl_absorpt_correction_T_min  0.0349
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4706
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.04
_refine_diff_density_max         8.065
_refine_diff_density_min         -6.994
_refine_diff_density_rms         1.036
_refine_ls_extinction_coef       0.00047(2)
_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_all   0.978
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         18738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_obs          0.0751
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1910
_refine_ls_wR_factor_obs         0.1744
_reflns_number_observed          12116
_reflns_number_total             18738
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a905539h.txt
_cod_data_source_block           oji2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4045.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008884