Synthetic Models for the Active Site of the [FeFe]-Hydrogenase: Catalytic Proton Reduction and the Structure of the Doubly Protonated Intermediate
Maria E. Carroll; Bryan E. Barton; Thomas B. Rauchfuss; Patrick J. Carroll; Journal of the American Chemical Society 134 (2012) 18843–18852; doi:10.1021/ja309216v

data_4118904
_publ_section_title
;
 Synthetic Models for the Active Site of the [FeFe]-Hydrogenase: Catalytic
 Proton Reduction and the Structure of the Doubly Protonated Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18843
_journal_page_last               18852
_journal_paper_doi               10.1021/ja309216v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C56 H51 B2 F8 Fe2 N O2 P4 S2'
_chemical_formula_weight         1243.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.021(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.328(4)
_cell_length_b                   22.073(5)
_cell_length_c                   18.286(4)
_cell_measurement_temperature    193(1)
_cell_volume                     6092(2)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1354
_diffrn_reflns_av_sigmaI/netI    0.1021
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65032
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         11192
_refine_ls_number_restraints     1704
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                7031
_reflns_number_total             11192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309216v_si_002_2.cif
_cod_data_source_block           bm63ssq2b
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4118904