Polyoxometalate-based Catalysts for Visible-Light Driven Hydrolytic Hydrogen Production: Coordinatively Unsaturated Cu-based Active Sites Enhance Performance
Wang, Quan Quan; Ren, Rong-Xian; Gong, Rui Jie; Zhao, Shao Da; Yan, Pinfang; Xu, Yan; Dalton Transactions  (2026) –; doi:10.1039/D5DT02675J

data_7719981
_publ_section_title
;
 Polyoxometalate-based Catalysts for Visible-Light Driven Hydrolytic
 Hydrogen Production: Coordinatively Unsaturated Cu-based Active Sites
 Enhance Performance
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02675J
_journal_year                    2026
_chemical_formula_sum            'C72 H64 Cu8.5 N24 Na O50 P W11.5'
_chemical_formula_weight         4773.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-10-06 deposited with the CCDC.	2025-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.361(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.447(3)
_cell_length_b                   12.6282(11)
_cell_length_c                   28.313(2)
_cell_measurement_reflns_used    18339
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      53.797
_cell_measurement_theta_min      3.319
_cell_volume                     10170.8(16)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            64351
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.764
_diffrn_source                   '\w scans'
_exptl_absorpt_coefficient_mu    14.804
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.118
_exptl_crystal_description       block
_exptl_crystal_F_000             8750
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         5.713
_refine_diff_density_min         -2.408
_refine_diff_density_rms         0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         8944
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0914
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1533P)^2^+731.2932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2568
_refine_ls_wR_factor_ref         0.2708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6868
_reflns_number_total             8944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02675j2.cif
_cod_data_source_block           a01
_cod_original_cell_volume        10171.0(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C72 H64 Cu8.50 N24 Na O50 P W11.50'
_cod_database_code               7719981
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.451
_shelx_estimated_absorpt_t_max   0.506
_exptl_absorpt_special_details   '(SADABS; Sheldrick, 2003)'
_shelx_res_checksum              67808
_shelx_hkl_checksum              91592