Discovery of two Na<sup>+</sup>-centered Silverton-type polyoxometalates {NaM<sub>12</sub>O<sub>42</sub>} (M = Mo, W).
Wan, Rong; Liu, Zhen; Ma, Xinyi; Li, Huafeng; Ma, Pengtao; Zhang, Chao; Niu, Jingyang; Wang, Jingping; Chemical communications (Cambridge, England) 57 (2021) 2172–2175; doi:10.1039/d0cc07590f

data_7127891
_publ_section_title
;
 Discovery of two Na<sup>+</sup>-centered Silverton-type polyoxometalates
 {NaM<sub>12</sub>O<sub>42</sub>} (M = Mo, W).
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2172
_journal_page_last               2175
_journal_paper_doi               10.1039/d0cc07590f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '0.5(C48 H144 Na8 O108 Ru8 S24 W24), 3(O)'
_chemical_formula_sum            'C24 H72 Na4 O57 Ru4 S12 W12'
_chemical_formula_weight         4359.97
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2020-03-30 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9539(9)
_cell_length_b                   17.9539(9)
_cell_length_c                   17.9539(9)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.78
_cell_volume                     5787.3(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0277
_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       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.604
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.675
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0938 before and 0.0643 after correction. The Ratio of minimum to maximum transmission is 0.8077. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_description       block
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.008
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+2.0371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2029
_reflns_number_total             2398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07590f2.cif
_cod_data_source_block           njy1
_cod_depositor_comments
'Adding full bibliography for 7127890--7127891.cif.'
_cod_original_cell_volume        5787.3(9)
_cod_database_code               7127891
_shelx_estimated_absorpt_t_max   0.252
_shelx_estimated_absorpt_t_min   0.167
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.01(2) -0.01(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: Na2(0.25)
4.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'