A mixed metallic and mixed valence MoV4VIV2VIII2 complex as an electron transfer photo-catalyst for the hydrogen evolution reaction
Morla, Kalyankumar S.; Thakre, Dewendra; Mourya, Adarsh K.; Singh, Piyush; Karnamkkott, Harsha S.; Ahamed, Subuhan; Sahoo, Subham; Bhattacharya, Ishita; Banerjee, Siddhartha; Sarma, Debajit; Mondal, Kartik Chandra; Ghosh, Sujit Kumar; Wankhade, Atul V.; Banerjee, Abhishek; Chemical Communications 61 (2025) 8919–8922; doi:10.1039/D5CC00117J

data_7134541
_publ_section_title
;
 A mixed metallic and mixed valence MoV4VIV2VIII2 complex as an electron
 transfer photo-catalyst for the hydrogen evolution reaction
;
_journal_issue                   49
_journal_name_full               'Chemical Communications'
_journal_page_first              8919
_journal_page_last               8922
_journal_paper_doi               10.1039/D5CC00117J
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C14 H46 Mo4 N2 O42 P4 V'
_chemical_formula_weight         1473.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-04-28 deposited with the CCDC.	2025-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4325(4)
_cell_length_b                   10.9812(4)
_cell_length_c                   17.2749(6)
_cell_measurement_reflns_used    53575
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.699
_cell_measurement_theta_min      2.207
_cell_volume                     2323.46(14)
_computing_cell_refinement       APEX-5
_computing_data_collection       APEX-5
_computing_data_reduction        APEX-5
_computing_molecular_graphics    Mercury
_computing_publication_material  enCIFer
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53564
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.207
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.501
_exptl_absorpt_correction_T_max  0.671
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_description       block
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.289
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         11344
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+6.9310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                11038
_reflns_number_total             11344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00117j2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7134540--7134541.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7134541
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.597
_shelx_estimated_absorpt_t_max   0.671
_shelx_res_checksum              17298
_shelx_hkl_checksum              66930