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_7249778
_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
'0.1(Cu0.18 O40 W12), 0.59(C7 H10 N2), 0.29(H2 O)'
_chemical_formula_sum            'C0.02 H0.02 Cu N0.02 O W'
_chemical_formula_weight         264.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2025-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            41
_cell_length_a                   13.7848(5)
_cell_length_b                   20.9048(7)
_cell_length_c                   26.7438(9)
_cell_measurement_reflns_used    9645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.104
_cell_measurement_theta_min      2.224
_cell_volume                     7644.5(5)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0757
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46576
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    18.135
_exptl_absorpt_correction_T_max  0.0452
_exptl_absorpt_correction_T_min  0.0102
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1518 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.2257.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4565
_refine_diff_density_max         7.106
_refine_diff_density_min         -2.784
_refine_diff_density_rms         0.471
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         15549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1291P)^2^+38.3531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.2059
_reflns_number_gt                12000
_reflns_number_total             15549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4ce00945b2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7249777--7249778.cif.'
_cod_database_code               7249778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O41(H41D,H41E), O42(H42D,H42E), O43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24), C26(H26),
  C28(H28), C30(H30), C32(H32), C35(H35), C37(H37), C38(H38), C40(H40)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'