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_7134540
_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            'C28 H77.19 Mo4 N4 O64.59 P8 V4'
_chemical_formula_weight         2338.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-05-04 deposited with the CCDC.	2025-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.9860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3825(4)
_cell_length_b                   14.0926(3)
_cell_length_c                   16.5564(4)
_cell_measurement_reflns_used    45666
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.072
_cell_volume                     3857.54(15)
_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 0.957
_diffrn_measured_fraction_theta_max 0.971
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45666
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.072
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.817
_refine_diff_density_min         -1.829
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5240
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0468P)^2^+25.7891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             5240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00117j2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7134540--7134541.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7134540
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.841
_shelx_res_checksum              20807
_shelx_hkl_checksum              19876