Confirmation of the Semivacant Wells–Dawson Polyoxotungstate Skeleton. The Structures of [Ce{X(H4)W17O61}2]19- (X = P, As) Indicate the Probable Location of Internal Protons
Belai, Nebebech; Dickman, Michael H.; Pope, Michael T.; Contant, Roland; Keita, Bineta; Mbomekalle, Israel-Martyr; Nadjo, Louis; Inorganic Chemistry 44 (2005) 169–171; doi:10.1021/ic048920w

data_4308403
_publ_section_title
;
 Confirmation of the Semivacant Wells--Dawson Polyoxotungstate Skeleton.
 The Structures of [Ce{X(H4)W17O61}2]19- (X = P, As) Indicate the Probable
 Location of Internal Protons
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              169
_journal_page_last               171
_journal_paper_doi               10.1021/ic048920w
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'Ce K10 O141.6 P2 W34'
_chemical_formula_weight         9109.56
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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            2
_cell_length_a                   43.477(16)
_cell_length_b                   12.427(5)
_cell_length_c                   14.861(6)
_cell_measurement_reflns_used    979
_cell_measurement_temperature    182(2)
_cell_measurement_theta_max      55.778
_cell_measurement_theta_min      5.113
_cell_volume                     8029(5)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'X-SEED, L .Barbour(1999);http://x-seed.net/'
_computing_publication_material  'X-SEED, L .Barbour(1999);http://x-seed.net/'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      182(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.1034
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            74016
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    24.895
_exptl_absorpt_correction_T_max  0.070425
_exptl_absorpt_correction_T_min  0.020880
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7854
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.855
_refine_diff_density_min         -2.374
_refine_diff_density_rms         0.773
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(2)
_refine_ls_extinction_coef       0.00052(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_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         14161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0950P)^2^+350.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1738
_reflns_number_gt                12387
_reflns_number_total             14161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048920wsi20040806_104519_2.cif
_cod_data_source_block           c:\mike\work04~2\p21212
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_formula_sum        'Ce K10 O141.60 P2 W34'
_cod_database_code               4308403