Synthesis and structural characterization of a hydrated sodium–caesium tetracosatungstate(VI), Na5Cs19[W24O84]·21H2O
Deblonde, Gauthier; Colliard, Ian; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 667–670; doi:10.1107/S2056989024004778

data_2023143
_publ_section_title
;
 Synthesis and structural characterization of a hydrated sodium--caesium
 tetracosatungstate(VI), Na5Cs19[W24O84]&#x00B7;21H2O
;
_journal_coeditor_code           WM5717
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              667
_journal_page_last               670
_journal_paper_doi               10.1107/S2056989024004778
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'Na5 Cs19 [W24 O84], 21H2 O'
_chemical_formula_moiety         '5(Na +), 19(Cs +), W24 O84 24 -, 21(H2 O)'
_chemical_formula_sum            'Cs19 H42 Na5 O105 W24'
_chemical_formula_weight         8774.97
_chemical_name_systematic
;
Pentasodium nonadecacesium tetracosatungstate(VI) heneikosahydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.0071(3)
_cell_length_b                   18.0071(3)
_cell_length_c                   62.9142(9)
_cell_measurement_reflns_used    12610
_cell_measurement_temperature    298
_cell_measurement_theta_max      31.5780
_cell_measurement_theta_min      3.4700
_cell_volume                     17667.2(5)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      298.00
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            30484
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.459
_exptl_absorpt_coefficient_mu    29.242
_exptl_absorpt_correction_T_max  0.00728
_exptl_absorpt_correction_T_min  0.00093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    4.949
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             22548
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.283
_refine_diff_density_min         -1.527
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1323P)^2^+146.9834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1704
_reflns_number_gt                7262
_reflns_number_total             8019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5717.cif
_cod_data_source_block           I
_cod_original_cell_volume        17667.1(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2023143
_shelx_estimated_absorpt_t_min   0.668
_shelx_estimated_absorpt_t_max   0.759
_shelx_hkl_checksum              24023
_shelx_res_checksum              98029