Mechanistic insights of molecular metal polyselenides for catalytic hydrogen generation
Elliott, Alexander; McAllister, James; Masaityte, Liudvika; Segado-Centellas, Mireia; Long, De-Liang; Ganin, Alexey Y.; Song, Yu-Fei; Bo, Carles; Miras, Haralampos N.; Chemical Communications  (2022) –; doi:10.1039/D2CC01226J

data_7130164
_publ_section_title
;
 Mechanistic insights of molecular metal polyselenides for catalytic
 hydrogen generation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01226J
_journal_year                    2022
_chemical_formula_moiety         'Mo4 O4 Se12.90, 2(Mo2 O2Se8), 8(C4 H12 N)'
_chemical_formula_sum            'C32 H96 Mo8 N8 O8 Se28.9'
_chemical_formula_weight         3770.63
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-28 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                78.432(4)
_cell_angle_beta                 80.140(4)
_cell_angle_gamma                86.939(4)
_cell_formula_units_Z            1
_cell_length_a                   10.098(4)
_cell_length_b                   12.766(5)
_cell_length_c                   18.713(7)
_cell_measurement_reflns_used    5011
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.241
_cell_measurement_theta_min      4.252
_cell_volume                     2328.0(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0910
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32001
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.479
_diffrn_reflns_theta_min         1.629
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.377
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5060
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.690
_exptl_crystal_description       block
_exptl_crystal_F_000             1727
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.667
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         9573
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0812
_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^)+(0.0533P)^2^+90.9215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5869
_reflns_number_total             9573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01226j2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2327.9(16)
_cod_original_formula_sum        'C32 H96 Mo8 N8 O8 Se28.90'
_cod_database_code               7130164
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.318
_shelx_estimated_absorpt_t_max   0.637
_shelx_res_checksum              64440