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_4308402
_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
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_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            'As2 Ce K7.5 O144.5 W34'
_chemical_formula_weight         9146.11
_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                   43.335(9)
_cell_length_b                   12.353(3)
_cell_length_c                   14.795(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      49.306
_cell_measurement_theta_min      4.688
_cell_volume                     7920(3)
_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      185(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  0.1364
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61436
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    25.567
_exptl_absorpt_correction_T_max  0.070973
_exptl_absorpt_correction_T_min  0.020050
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    3.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             7877
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.571
_refine_diff_density_min         -1.959
_refine_diff_density_rms         0.430
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         11048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0636P)^2^+206.3231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                8516
_reflns_number_total             11048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048920wsi20040806_104519_1.cif
_cod_data_source_block           c:\mike\work04~1\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 
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_cod_original_formula_sum        'As2 Ce K7.50 O144.50 W34'
_cod_database_code               4308402