Computational and Experimental Study of the Mechanism of Hydrogen Generation from Water by a Molecular Molybdenum-Oxo Electrocatalyst
Eric J. Sundstrom; Xinzheng Yang; V. Sara Thoi; Hemamala I. Karunadasa; Christopher J. Chang; Jeffrey R. Long; Martin Head-Gordon; Journal of the American Chemical Society 134 (2012) 5233–5242; doi:10.1021/ja210949r

data_4117702
_publ_section_title
;
 Computational and Experimental Study of the Mechanism of Hydrogen
 Generation from Water by a Molecular Molybdenum-Oxo Electrocatalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5233
_journal_page_last               5242
_journal_paper_doi               10.1021/ja210949r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C73 H50 F12 Mo2 N16 O12 S4'
_chemical_formula_weight         1891.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.681(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4356(6)
_cell_length_b                   15.7501(8)
_cell_length_c                   20.2185(10)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      135.630
_cell_measurement_theta_min      5.611
_cell_volume                     3959.8(3)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0139
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26907
_diffrn_reflns_theta_full        68.16
_diffrn_reflns_theta_max         68.16
_diffrn_reflns_theta_min         3.56
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.448
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4802
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         6642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.139
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3049
_refine_ls_wR_factor_ref         0.3253
_reflns_number_gt                6245
_reflns_number_total             7239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210949r_si_002_2.cif
_cod_data_source_block           hk216a
_cod_database_code               4117702