Mild Redox Complementation Enables H2 Activation by [FeFe]-Hydrogenase Models
James M. Camara; Thomas B. Rauchfuss; Journal of the American Chemical Society 133 (2011) 8098–8101; doi:10.1021/ja201731q

data_4106184
_publ_section_title
;
 Mild Redox Complementation Enables H2 Activation by [FeFe]-Hydrogenase
 Models
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8098
_journal_page_last               8101
_journal_paper_doi               10.1021/ja201731q
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C47 H37 Fe2 N O4 P2 S2, C32 H12 B F24 '
_chemical_formula_sum            'C79 H49 B F24 Fe2 N O4 P2 S2'
_chemical_formula_weight         1780.76
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_update_record
; 
? 
;
_cell_angle_alpha                112.125(2)
_cell_angle_beta                 103.554(2)
_cell_angle_gamma                96.384(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7224(6)
_cell_length_b                   17.4566(8)
_cell_length_c                   20.4323(9)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.35
_cell_volume                     4298.3(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ba41lasq
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68738
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.8498
_exptl_absorpt_correction_T_min  0.7255
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       prism
_exptl_crystal_F_000             1794
_exptl_crystal_id                ba41lasq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2 1 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.747
_exptl_crystal_size_mid          0.394
_exptl_crystal_size_min          0.368
_platon_squeeze_details
; 
The positions for the three dichloromethane solvate molecules were 
poorly determined. Therefore, a second structural model was refined 
with contributions from the solvate molecules removed from the 
diffraction data using the bypass procedure in PLATON (Spek, 1990). 
The electron count from the "squeeze" model was consistent with 
three molecules of dichloromethane. This model converged in good agreement 
with the number of solvate molecules predicted by the complete refinement. 
;
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1291
_refine_ls_number_reflns         15916
_refine_ls_number_restraints     2377
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                11474
_reflns_number_total             15916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201731q_si_002.cif
_cod_data_source_block           ba41lasq
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4106184