Efficient homogeneous electrocatalytic hydrogen evolution using a Ni-containing polyoxometalate catalyst.
Jana, Debu; Kolli, Hema Kumari; Sabnam, Subhashree; Das, Samar K.; Chemical communications (Cambridge, England) 57 (2021) 9910–9913; doi:10.1039/d1cc03605j

data_7128911
_publ_section_title
;
 Efficient homogeneous electrocatalytic hydrogen evolution using a
 Ni-containing polyoxometalate catalyst.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9910
_journal_page_last               9913
_journal_paper_doi               10.1039/d1cc03605j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'H32 K2 Ni2 O44 V10'
_chemical_formula_weight         1441.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-08-16 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                65.037(4)
_cell_angle_beta                 75.059(4)
_cell_angle_gamma                70.540(4)
_cell_formula_units_Z            1
_cell_length_a                   8.7397(4)
_cell_length_b                   10.7629(5)
_cell_length_c                   11.1283(5)
_cell_measurement_reflns_used    2709
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.998
_cell_measurement_theta_min      2.038
_cell_volume                     886.32(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.038
_exptl_absorpt_coefficient_mu    3.914
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_exptl_crystal_colour            Brownish-Orange
_exptl_crystal_density_diffrn    2.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.495
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1589P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2709
_reflns_number_total             3113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03605j2.cif
_cod_data_source_block           s1
_cod_depositor_comments          'Adding full bibliography for 7128911.cif.'
_cod_database_code               7128911
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.407
_shelx_estimated_absorpt_t_max   0.539
_shelx_res_checksum              74627