Polyoxothiometalate-Derivatized Silicon Photocathodes for Sunlight-Driven Hydrogen Evolution Reaction.
Fu, Dong; Fabre, Bruno; Loget, Gabriel; Mériadec, Cristelle; Ababou-Girard, Soraya; Cadot, Emmanuel; Leclerc-Laronze, Nathalie; Marrot, Jérôme; de Ponfilly, Quentin; ACS omega 3 (2018) 13837–13849; doi:10.1021/acsomega.8b01734

data_4515874
_publ_section_title
;
 Polyoxothiometalate-Derivatized Silicon Photocathodes for Sunlight-Driven
 Hydrogen Evolution Reaction.
;
_journal_issue                   10
_journal_name_full               'ACS omega'
_journal_page_first              13837
_journal_page_last               13849
_journal_paper_doi               10.1021/acsomega.8b01734
_journal_volume                  3
_journal_year                    2018
_chemical_formula_sum            'C27 H45 Cl Mo3 O10 S4'
_chemical_formula_weight         981.14
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   20.702(2)
_cell_length_b                   20.702(2)
_cell_length_c                   16.158(2)
_cell_measurement_reflns_used    9597
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.87
_cell_measurement_theta_min      2.27
_cell_volume                     5997.1(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            234315
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.030
_diffrn_reflns_theta_min         1.697
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2008/1)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       needle
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7460
_exptl_transmission_factor_min   0.6348
_refine_diff_density_max         1.885
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6008
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0567P)^2^+18.3378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1353
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5391
_reflns_number_total             6008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b01734_si_002.cif
_cod_data_source_block           am01
_cod_original_cell_volume        5997.1(16)
_cod_database_code               4515874
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.706
_shelx_estimated_absorpt_t_max   0.885
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'
_shelx_res_checksum              98400
_shelx_hkl_checksum              15122