Three-dimensional 14-core manganese-sodium-based polyoxometalate with unique channels as bifunctional electrocatalysts for overall water splitting
Gong, Lige; Wang, Meijia; Wang, Jihua; Dong, Limin; Gu, Yunhao; Yang, Binghe; Li, Hui; CrystEngComm 27 (2025) 974–988; doi:10.1039/D4CE00945B

data_7249777
_publ_section_title
;
 Three-dimensional 14-core manganese-sodium-based polyoxometalate with
 unique channels as bifunctional electrocatalysts for overall water
 splitting
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              974
_journal_page_last               988
_journal_paper_doi               10.1039/D4CE00945B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'H8 Mn4 O56 W12, 8(O), 4(H2 O), 8(Na)'
_chemical_formula_sum            'H16 Mn4 Na8 O68 W12'
_chemical_formula_weight         3713.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-08 deposited with the CCDC.	2025-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.2970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.3531(4)
_cell_length_b                   11.7391(3)
_cell_length_c                   18.1384(5)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.30
_cell_volume                     3085.45(14)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35001
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    23.233
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.0890
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1532 before and 0.0815 after correction.
The Ratio of minimum to maximum transmission is 0.3420.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    3.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3272.0
_refine_diff_density_max         3.645
_refine_diff_density_min         -4.768
_refine_diff_density_rms         0.563
_refine_ls_extinction_coef       0.00045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+139.3466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                5659
_reflns_number_total             6338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4ce00945b2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7249777--7249778.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7249777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O30) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(O24) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(O21) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(O5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(O27) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(O26) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O15) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O16) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(W3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
Uanis(W1) \\sim Ueq: with sigma of 0.0002 and sigma for terminal atoms of 0.0001
3.a Rotating group:
 O5(H5A,H5B), O7(H7A,H7B), O11(H11A,H11B), O14(H14A,H14B)
;
_olex2_submission_special_instructions 'No special instructions were received'