A uranium-bridged dimeric Keggin-type polyoxometalate and its proton conductive properties.
Wei, Yuting; Du, Weixin; Wang, Haiying; Wang, Xiaoyue; Shen, Keqin; Xiong, Minghui; Zhang, Dongdi; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16826–16829; doi:10.1039/d4dt02077d

data_7717165
_publ_section_title
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 A uranium-bridged dimeric Keggin-type polyoxometalate and its proton
 conductive properties.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16826
_journal_page_last               16829
_journal_paper_doi               10.1039/d4dt02077d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'H5 O74 Sb4 U2 W18, 2(H2 O), 10[NH4+], 16[H2O]'
_chemical_formula_sum            'H81 N10 O92 Sb4 U2 W18'
_chemical_formula_weight         5965.905
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2024-09-19
_audit_creation_method
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Olex2 1.5-dev
(compiled 2024.09.12 svn.r2332d2e9 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-09-26 deposited with the CCDC.	2024-10-04 downloaded from the CCDC.
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_cell_angle_alpha                89.198(1)
_cell_angle_beta                 89.561(1)
_cell_angle_gamma                83.944(1)
_cell_formula_units_Z            2
_cell_length_a                   11.5231(4)
_cell_length_b                   19.0495(6)
_cell_length_c                   21.0886(7)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.344
_cell_measurement_theta_min      2.617
_cell_volume                     4602.8(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_device_type  'Bruker, D8'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.9994
_diffrn_reflns_Laue_measured_fraction_max 0.9961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            118876
_diffrn_reflns_point_group_measured_fraction_full 0.9994
_diffrn_reflns_point_group_measured_fraction_max 0.9961
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    27.163
_exptl_absorpt_correction_T_max  0.0214
_exptl_absorpt_correction_T_min  0.0035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1384 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.1636.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    4.305
_exptl_crystal_description       block
_exptl_crystal_F_000             5160.520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.8916
_refine_diff_density_min         -1.5779
_refine_diff_density_rms         0.3352
_refine_ls_d_res_high            0.7479
_refine_ls_d_res_low             10.2966
_refine_ls_goodness_of_fit_ref   1.0269
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    14
_refine_ls_number_parameters     906
_refine_ls_number_reflns         22956
_refine_ls_number_restraints     1472
_refine_ls_restrained_S_all      0.9942
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+13.6020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                20387
_reflns_number_total             22956
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02077d2.cif
_cod_data_source_block           m9116_0m_sq
_cod_depositor_comments          'Adding full bibliography for 7717165.cif.'
_cod_database_code               7717165
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4.a Riding coordinates:
 O68(H68), O2(H2a,H2b)
4.b Free rotating group:
 O1(H1a,H1b)
4.c Rotating group:
 O27(H27a,H27b), O63(H63a,H63b)
;
_platon_squeeze_special_details
;
A solvent mask was calculated and 520 electrons were 
found in a volume of 1605\%A^3^ in 1 void per unit cell.
This is slightly different from the presence of
1[10NH4+;7H2O] per Asymmetric Unit which account for
170 electrons per unit cell due to the loss of crystallization
water when drying at room temperature.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'