Nitrosyl Derivatives of Diiron(I) Dithiolates Mimic the Structure and Lewis Acidity of the [FeFe]-Hydrogenase Active Site
Matthew T. Olsen; Maurizio Bruschi; Luca De Gioia; Thomas B. Rauchfuss; Scott R. Wilson; Journal of the American Chemical Society 130 (2008) 12021–12030; doi:10.1021/ja802268p

data_4108296
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Nitrosyl Derivatives of Diiron(I) Dithiolates Mimic the Structure and
 Lewis Acidity of the [FeFe]-Hydrogenase Active Site
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12021
_journal_page_last               12030
_journal_paper_doi               10.1021/ja802268p
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C12 H24 Fe2 N O4 P2 S2), 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C25 H50 B2 Cl2 F8 Fe4 N2 O8 P4 S4'
_chemical_formula_weight         1226.71
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2008-01-18   text and data added, mto 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.380(6)
_cell_length_b                   7.175(2)
_cell_length_c                   32.098(9)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.80
_cell_measurement_theta_min      2.54
_cell_volume                     4924(2)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4 (Bruker, 2005 & 2007) 
;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  g35wasx
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            50246
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  0.9376
_exptl_absorpt_correction_T_min  0.5823
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       needle
_exptl_crystal_F_000             2488
_exptl_crystal_id                g35wasx
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 0 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack (1983),  4418 Friedels'
_refine_ls_abs_structure_Flack   -0.001(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         9019
_refine_ls_number_restraints     801
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                5520
_reflns_number_total             9019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802268p_si_002_1.cif
_cod_data_source_block           g35wasx
_cod_original_sg_symbol_Hall     'P 2c -2ac '
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_database_code               4108296