Polyoxometalate-based coordination polymers enhance electrocatalytic hydrogen evolution in trimetallic sulfides
Zhang, Shuyuan; Wang, Guangning; Liu, Jie; Wang, Qian; Zhang, Chunjing; Pang, Haijun; Li, Xiaoyi; Wang, Shiming; Chen, Tingting; New Journal of Chemistry 49 (2025) 1091–1099; doi:10.1039/D4NJ04347B

data_7063601
_publ_section_title
;
 Polyoxometalate-based coordination polymers enhance electrocatalytic
 hydrogen evolution in trimetallic sulfides
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1091
_journal_page_last               1099
_journal_paper_doi               10.1039/D4NJ04347B
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C20 H25 Mo12 N4 O41 P1'
_chemical_formula_sum            'C20 H25 Mo12 N4 O41 P'
_chemical_formula_weight         2172.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-07 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6283(16)
_cell_length_b                   20.910(2)
_cell_length_c                   14.0123(14)
_cell_measurement_reflns_used    116730
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.19
_cell_volume                     4872.0(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            111748
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.722
_exptl_absorpt_coefficient_mu    3.128
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.962
_exptl_crystal_description       block
_exptl_crystal_F_000             4100
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6211
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.305
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0263P)^2^+51.6941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4681
_reflns_number_total             6211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04347b2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7063601.cif.'
_cod_original_cell_volume        4872.1(8)
_cod_original_formula_sum        'C20 H25 Mo12 N4 O41 P1'
_cod_database_code               7063601
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O16-Mo14
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O12B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O6B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O8B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 1*[Sof(O3)]+1*[Sof(O4)]=1 with esd of 0.0001
 Sof(O8B)=1-FVAR(1)
 Sof(O8A)=FVAR(1)
 Sof(O6B)=1-FVAR(2)
 Sof(O6A)=FVAR(2)
 Sof(O4B)=1-FVAR(3)
 Sof(O4A)=FVAR(3)
 Sof(O12B)=1-FVAR(4)
 Sof(O12A)=FVAR(4)
 Sof(O47B)=1-FVAR(7)
 Sof(O47A)=FVAR(7)
 Fixed Sof: O76(0.5) O77(0.5) O79(0.5) O82(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C32(H32), C37(H37), C40(H40), C46(H46), C20(H20), N1(H1), C3(H3),
 C6(H6), C17(H17), C28(H28)
;
_shelx_res_checksum              98957
_olex2_submission_special_instructions 'No special instructions were received'