Redox-Mediator-Assisted Electrocatalytic Hydrogen Evolution from Water by a Molybdenum Sulfide-Functionalized Metal‒Organic Framework
Noh, Hyunho; Kung, Chung-Wei; Otake, Ken-ichi; Peters, Aaron W.; Li, Zhanyong; Liao, Yijun; Gong, Xinyi; Farha, Omar K.; Hupp, Joseph T.; ACS Catalysis 8 (2018) 9848–; doi:10.1021/acscatal.8b02921

data_4515540
_publ_section_title
;
 Redox-Mediator-Assisted Electrocatalytic Hydrogen Evolution from Water by
 a Molybdenum Sulfide-Functionalized Metal--Organic Framework
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              9848
_journal_paper_doi               10.1021/acscatal.8b02921
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C88 H44 O32 Zr6 (Mo O2)1.84 (Mo O3)0.40'
_chemical_formula_sum            'C88 H44 Mo2.24 O36.88 Zr6'
_chemical_formula_weight         2453.53
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-01-18 deposited with the CCDC.
2018-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   39.4657(12)
_cell_length_b                   39.4657(12)
_cell_length_c                   16.3953(5)
_cell_measurement_reflns_used    3584
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.38
_cell_volume                     22115.1(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1767
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            76098
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.921
_diffrn_reflns_theta_max         23.921
_diffrn_reflns_theta_min         0.596
_diffrn_source                   'MoK\a I\mS microfocus source with MX Optics'
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS-2014/5; Krause et al., 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3673
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.798
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         6396
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0763
_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^)+(0.1347P)^2^+28.7160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4471
_reflns_number_total             6396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02921_si_002.cif
_cod_data_source_block           NU1000-MoOx-SIM
_cod_original_cell_volume        22115.1(15)
_cod_database_code               4515540
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              47455
_shelx_hkl_checksum              69516
_shelx_fab_checksum              68597