Oxygen-Tolerant H<sub>2</sub> Production by [FeFe]-H<sub>2</sub>ase Active Site Mimics Aided by Second Sphere Proton Shuttle.
Ahmed, Md Estak; Dey, Subal; Darensbourg, Marcetta Y.; Dey, Abhishek; Journal of the American Chemical Society 140 (2018) 12457–12468; doi:10.1021/jacs.8b05983

data_4132745
_publ_section_title
;
 Oxygen-Tolerant H<sub>2</sub> Production by [FeFe]-H<sub>2</sub>ase
 Active Site Mimics Aided by Second Sphere Proton Shuttle.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12457
_journal_page_last               12468
_journal_paper_doi               10.1021/jacs.8b05983
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C18 H15 Fe2 N O8 S2'
_chemical_formula_weight         549.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 111.147(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0292(8)
_cell_length_b                   11.9367(7)
_cell_length_c                   16.3521(10)
_cell_measurement_reflns_used    8760
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.27
_cell_measurement_theta_min      2.49
_cell_volume                     2189.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'mercury 3.8'
_computing_publication_material  'ortep 3v.2'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(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  0.0629
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14334
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.491
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0421P)^2^+13.0065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2883
_reflns_number_total             3832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05983_si_004.cif
_cod_data_source_block           test9_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132745
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              235
_shelx_hkl_checksum              42381