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_4118903
_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            'C57 H51 Cl2 Fe2 N O2 P4 S2'
_chemical_formula_weight         1152.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.091(2)
_cell_angle_beta                 97.712(2)
_cell_angle_gamma                106.3740(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6092(14)
_cell_length_b                   12.5906(17)
_cell_length_c                   21.136(3)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.22
_cell_volume                     2626.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1561
_diffrn_reflns_av_sigmaI/netI    0.1101
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30526
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.9123
_exptl_absorpt_correction_T_min  0.8442
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       prism
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0261P)^2^+0.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                8068
_reflns_number_total             10362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309216v_si_002_1.cif
_cod_data_source_block           fm62t_0mg
_cod_database_code               4118903