Crown-type tetranuclear Ag-POM exhibits excellent proton conductivity performance.
Sun, Yahao; Cai, Minzhen; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11953–11957; doi:10.1039/d5dt01141h

data_7719095
_publ_section_title
;
 Crown-type tetranuclear Ag-POM exhibits excellent proton conductivity
 performance.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11953
_journal_page_last               11957
_journal_paper_doi               10.1039/d5dt01141h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Ag3.4 As4 Na24.6 O198 W40, 8[H2O], 4[H2O]'
_chemical_formula_sum            'Ag3.4 As4 H24 Na24.6 O210 W40'
_chemical_formula_weight         11970.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-04 deposited with the CCDC.	2025-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.3853(3)
_cell_length_b                   19.3853(3)
_cell_length_c                   26.1587(5)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.285
_cell_measurement_theta_min      2.481
_cell_volume                     9830.2(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTO II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35792
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.095
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              Microfocus
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    24.471
_exptl_absorpt_correction_T_max  0.0298
_exptl_absorpt_correction_T_min  0.0066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1605 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.2215.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.044
_exptl_crystal_description       block
_exptl_crystal_F_000             10453
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details
;
 Flack x determined using 3858 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8753
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+13.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8412
_reflns_number_total             8753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01141h2.cif
_cod_data_source_block           m13393_0m_a
_cod_depositor_comments          'Adding full bibliography for 7719095.cif.'
_cod_original_cell_volume        9830.2(4)
_cod_original_formula_sum        'Ag3.40 H24 As4 Na24.60 O210 W40'
_cod_database_code               7719095
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.111
_shelx_estimated_absorpt_t_min   0.090
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(O14W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ag1) = Uanis(Na1A)
2. Others
 Fixed Sof: Ag1(0.85) Na3(0.75) Na7(0.75) Na8(0.75) Na1A(0.15)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 246 electrons were 
found in a volume of 786\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
8[H2O], 4[H2O] per formula unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97883
_shelx_hkl_checksum              35246
_shelx_fab_checksum              38732
_olex2_submission_special_instructions 'No special instructions were received'