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_4108300
_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         'C12 H24 Fe2 N O4 P2 S2, B F4, C H2 Cl2'
_chemical_formula_sum            'C13 H26 B Cl2 F4 Fe2 N O4 P2 S2'
_chemical_formula_weight         655.82
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2008-01-31  text and data added, mto 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.054(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6325(3)
_cell_length_b                   20.7126(8)
_cell_length_c                   9.5998(4)
_cell_measurement_reflns_used    7650
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.34
_cell_volume                     1316.91(10)
_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 (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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  ga29xas
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21574
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.9007
_exptl_absorpt_correction_T_min  0.6885
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       tabular
_exptl_crystal_F_000             664
_exptl_crystal_id                ga29xas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 -6 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack (1983),  3128 Friedels'
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6583
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                5864
_reflns_number_total             6583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802268p_si_002_5.cif
_cod_data_source_block           ga29xas
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               4108300