[Fe2(SR)2(μ-CO)(CNMe)6]2+ and Analogues: A New Class of Diiron Dithiolates as Structural Models for the Hox Air State of the Fe-Only Hydrogenase
Christine A. Boyke; Thomas B. Rauchfuss; Scott R. Wilson; Marie-Madeleine Rohmer; Marc Bénard; Journal of the American Chemical Society 126 (2004) 15151–15160; doi:10.1021/ja049050k

data_4113209
_publ_contact_author_address
;
Department of Chemistry
University of Illinois at Urbana-Champaign
600 South Matthews Avenue
Urbana
IL 61801
USA
;
_publ_contact_author_email       rauchfuz@uiuc.edu
_publ_contact_author_fax         '1 217 333 2685'
_publ_contact_author_name        'Prof. Thomas B. Rauchfuss'
_publ_contact_author_phone       '1 217 333 7355'
_publ_section_title
;
 [Fe2(SR)2(\m-CO)(CNMe)6]2+ and Analogues: A New Class of Diiron
 Dithiolates as Structural Models for the Hox Air State of the Fe-Only
 Hydrogenase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15151
_journal_page_last               15160
_journal_paper_doi               10.1021/ja049050k
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         '2(C33 H58 Fe2 N6 O1 S2), 4(F6 P), C2 H3 N'
_chemical_formula_sum            'C68 H119 F24 Fe4 N13 O2 P4 S4'
_chemical_formula_weight         2082.28
_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
; 
2003-09-02   text and data added, cad 
;
_cell_angle_alpha                85.149(10)
_cell_angle_beta                 63.442(9)
_cell_angle_gamma                69.038(9)
_cell_formula_units_Z            1
_cell_length_a                   14.343(8)
_cell_length_b                   14.660(9)
_cell_length_c                   14.927(9)
_cell_measurement_reflns_used    982
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.6
_cell_volume                     2611(3)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  p66vas
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27576
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        1.4
_diffrn_standards_interval_time  245
_diffrn_standards_number         277
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.8713
_exptl_absorpt_correction_T_min  0.7120
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1078
_exptl_crystal_id                p66vas
_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 0 2) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         9509
_refine_ls_number_restraints     636
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+1.3586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                7764
_reflns_number_total             9509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049050ksi20040219_042726.cif
_cod_data_source_block           p66vas
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113209